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The document discusses various aspects of citrus processing including quality control, juice characteristics, and technology.

The document covers topics such as juice composition, testing methods, oils and aromas, color, rheology, and waste management.

Some of the main citrus fruits discussed include oranges, grapefruits, lemons, limes, and tangerines.

CITRUS PROCESSING

Quality Control and


Technology

Dan Kimball
Director of Qua/ity Control, Research and Development

CALIFORNIA CITRUS PRODUCERS, INC.

mSPRINGER SCIENCE+BUSINESS MEDIA, LLC


An AVI Book
Copyright © 1991 by Springer Science+Business Media New York
Originally published byVan Nostrand Reinho[d, New York, NY in [991
Softcover reprint of the hardcover 1st edition 1991

International Thomson Puhlishing Asia


221 Henderson Road #05-10
Henderson Building
Singapore 0315

AII rigl1ts reserved. No part ofthis book covered by the copyright hereon may he reproduced or used in allY form Of by any means--graphic,
electronic, Of mechanical, including photocopying, recording, tap ing, or informaticn storage and retrieval systems-~without the written
permission ofthe puhlisher.

2 3 4 5 6 7 8 9 XXX 01 00 99 98 97

Libl"a .. y of Congress Cataloging-in-Publication Data

Kimball, Dan A.
Citrus processing: quality control and technology / Dan A. Kimball.
p. cm.
Includes bibliographical references and index.
ISBN 978-94-010-5645-8 ISBN 978-94-011-3700-3 (eBook)
DOI 10.1007/978-94-011-3700-3
1. Citrus juices. 2. Citrus fruits--By-products. t Title.
TP562.K55 1991 90-25153
663' .63--dc20 CIP
Contents

Preface v

Chapter 1 Introduction
Unit 1 Citrus Juice Characteristics
Chapter 2 Brix and Soluble Solids 7
Chapter 3 Acids in Citrus Juices 34
Chapter 4 The Brixl Acid Ratio 55
Chapter 5 Testing of Fruit Samples 66
Chapter 6 Citrus Oils, Aromas, and Essences 73
Chapter 7 Citrus Juice Pulp 102
Chapter 8 Juice Cloud 117
Chapter 9 Color of Citrus Juices 126
Chapter 10 Bitterness in Citrus Juices 136
Chapter 11 Nutritional Content of Citrus Juices 162
Chapter 12 Citrus Rheology 175
Chapter 13 Citrus Processing Varieties 180
Unit 2 Citrus Juice Sanitation
Chapter 14 Inspections 213
Chapter 15 Citrus Microbiology 226
Chapter 16 Insects, Rodents, and Birds 244
Chapter 17 Physical and Chemical Contamination 254
Chapter 18 Processing Contamination 258
Chapter 19 Juice Adulteration 279
Unit 3 Citrus Juice By-Products
Chapter 20 Food-Grade Nonjuice Products 303
Chapter 21 Animal Feed and Fuel By-Products 337
Chapter 22 Wastes from Citrus Plants 353

iii
iv CONTENTS

Unit 4 Citrus Juice Management


Chapter 23 Quality Control Statistics 371
Chapter 24 Quality Control Management 388
Chapter 25 Inventory Management 397
Appendix A Acid Corrections to the Brix 412
Appendix B GWBASIC and RPG Programs 418
Appendix C HP-41C Programmable Calculator Programs 430
Appendix D Answers to Select Questions and Problems 444
Index 453
Preface

Citrus juices constitute the majority of the fruit juices consumed in the United
States and around the world. Along with the rest of the fruit juice industry, they
playa major role in the entire food industry as well. In spite of this prominence,
few texts have been written on quality control technology; and most of the texts
have been written by researchers who may possess great technical skill but
generally are less familiar with daily routine quality control problems and con-
cerns than quality control technologists are. On the other hand, quality control
technologists and managers generally do not have the time and/or the talent to
write books or communicate through scientific literature.
The author recognized the need for an updated, comprehensive, and easily
understood text on citrus quality control. This text has been designed to be used
not only by processors, bottlers, canners, and others involved in the citrus in-
dustry, but it can be of value to instructors and students of citrus technology.
Researchers also can find value in the foundations laid down by the text, es-
pecially in regard to the needs and concerns of the processing industry. Also,
consultants and marketing personnel will be greatly helped by understanding
the concepts of this volume. Persons in related industries also will find many
applications that can be easily adapted to their needs.
It may be impossible to foresee all problems and situations that can occur in
various plants at various times. It has been said that the only thing that does
not change is change itself. Constant revision of procedures, policies, and tech-
nical information should be an integral part of every quality control program.
All quality control personnel should be receiving constant training', and proce-
dures should be under continued scrutiny and development. Each company
should have a quality control manual to supplement this text. The manual should
outline procedures and policies specific to the individual plant's operation and
facilities. Reference material should be orderly, readily available, and easy to
understand.
A great lack of uniformity plagues a portion of the citrus industry, stemming

v
vi PREFACE

from a general lack of understanding of basic technical and managerial princi-


ples. The author hopes that this text will help unite the industry technologically,
in addition to functioning as a resource for persons who need up-to-date basic
information and techniques. The author welcomes comments and suggestions
about the text.
UNIT ONE

CITRUS JUICE CHARACTERISTICS


UNIT TWO

CITRUS JUICE SANITATION


UNIT THREE

CITRUS JUICE BY-PRODUCTS


UNIT FOUR

CITRUS JUICE MANAGEMENT


Chapter 1

Introduction

The commercialization of fruit juices has a long and colorful history. The first
commercial fruit juice was produced in 1869 by Welch, who began bottling
unfermented grape juice in Vineland, New Jersey. However, juice that could
be preserved for long periods of time did not emerge until after Welch intro-
duced the principles of heat sterilization. By the 1930s, flash pasteurization was
developed, and it was during this time that fruit juices gained public notice as
a significant source of vitamin C and began to increase in popularity. World
War II made new demands on the juice industry, resulting in the development
of dehydrated fruit juices and frozen concentrates. Prior to this time, California
dominated the citrus industry with its fresh markets. With the advent of frozen
concentrated orange juice and its increase in popularity, the citrus industry
moved east to Florida.
Today, Florida grows approximately twice as much citrus as California, with
about 90% of its fruit going to the processed markets. Florida's hot and humid
climate induces thin peels that are easily scarred and develop poor color, and
these cosmetic effects generally render Florida fruit inferior in the fresh mar-
kets. However, the juice flavor from such fruit is rated as superior. In Califor-
nia, the fresh markets still rule supreme, generating about ten times as much
profit for citrus growers as processed fruit. The drier Mediterranean climate of
California produces thick richly colored peels, which are more durable to scar-
ring than Florida fruit, and deep-colored juices. Culls that do not make fresh
fruit quality because of scarring, color, size, or freeze damage are sent to pro-
cessing plants in California. Thus, in spite of the fact that one-third of the U. S.
citrus is grown there, California is responsible for only about 10 to 15 % of the
juice market. Another factor that has affected the difference between California
and Florida markets is the fact that in California a wider variety of agricultural
products is produced over a much larger and more diverse geographical region
than Florida. In Florida, citrus is king, a situation that led to the development
of the Florida Department of Citrus, which has exerted great political influence
in protecting a very important industry, second only to the tourist industry.

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
2 INTRODUCTION

One Florida venture was to initiate a citrus industry in Brazil in order to avoid
the economic damage of freezes in Florida. This budding industry was later
sold to the Brazilians, who have, in recent times, emerged as a major contender
in the international citrus juice market. With a few devastating freezes in Flor-
ida, it did not take long for the Brazilian citrus empire to establish markets in
the United States and usurp Florida's previous position as king of the mountain
in the citrus industry. Brazil has the largest juice processing plants in the world
and is a leader in citrus technology in many areas.
Citrus processing consists mainly of the receiving and storage of fruit, fruit
washing and grading, juice extraction, juice finishing or screening, heat treat-
ment, packaging, and storing. Blending of previously prepared or purchased
juices is very common, along with the manufacture of by-products such as pulp
wash juices, oils and aromas, animal feeds, pectins, marmalades and jellies,
drinks, flavors, wines, vinegars, fuels, and many more. Some areas grow citrus
purely for oils or fragrances to be used in perfumes. All these products require
a degree of quality control to ensure their marketability and consumer accep-
tance. However, even though there exists a wide diversity of citrus products,
the majority of citrus products consist of 100% juices.
The chapters in this book treat the main parameters of citrus juices and some
of the main by-products and other quality-control-related topics. New emerging
technologies such as aseptic processing, debittering, reverse osmosis, and per-
haps even supercritical extraction undoubtedly will improve the quality of citrus
products but probably will have little impact on the basic principles of quality
control outlined in this book. As new technologies and research advance, greater
light is expected to be shed on citrus quality control and citrus processing. New
concepts already are slipping over the horizon, such as those regarding the po-
tential anti carcinogenic attributes of some components of citrus juices and the
potential for debittering wastes to be used as antifeedants for some agricultural
pests. Quality control personnel should be serious students of citrus research
efforts and perhaps even participate in them when possible. On the other hand,
researchers should be serious students of the industry and quality control tech-
nology and keep informed on what is happening in the industry because the
industry is the prime benefactor of their research.
Even though approximately 70% of all juices consumed in the United States
are citrus juices, it would be appropriate to mention that a significant portion
of the juice industry is comprised of noncitrus juices. Citrus juices are preferred
in an opaque form most closely resembling the natural juice. Other juices, such
as apple, grape, and berry juices, are preferred in a clarified form, involving
the use of filter presses, centrifuges, enzymatic treatments, and filters in various
stages and engineering schemes. Except for this major difference between clar-
ified and citrus juices, the quality control concepts of both are very similar, and
the principles outlined in this text can be of great benefit to all. Even persons
INTRODUCTION 3

in the sugar industry can utilize much of this information in the crystallization
of granular sugar as well as the manufacture of syrups and related products.
Bottlers and canners of any type of juice will find much of this information
valuable. Production, marketing, and other managers involved in fruit juice
processing often need a reference source regarding related technology, a role
that this text can fill.
The mission of a quality control department in a citrus juice processing fa-
cility can be divided into three main parts. The first is the measurement and
control of juice characteristics. The procedures outlined in this text can serve
as a complete guide to both the latest and traditionally accepted methods com-
monly used in the industry. Quality control goes beyond mere measurement of
these parameters. It includes comparing these characteristics to customer or in-
house specifications in determining compliance with the goals and policies of
the company. Many operations await the decision of the quality control de-
partment before proceeding. This gives quality control the ability literally to
control the quality of the products. Quality assurance is defined by some as
being even more inclusive than this, with the added responsibility of ensuring
that the products achieve a certain quality standard. This goes beyond mere
measurement and reporting of discrepancies.
The second portion of the mission of a quality control department is to ensure
the sanitation of the product. Good industrial hygiene involves a host of con-
siderations, as detailed in Unit Two of the text. Modem lifestyles demand san-
itary foods that are guaranteed to be free from any type of contaminants. Con-
tamination can come from many places-the environment, a dirty plant,
improper processing, inadequate sanitary procedures or enforcement, or even
intentional contamination. Quality control personnel are responsible for ensur-
ing a clean and healthy environment for food processing and safe, authentic,
and palatable products. In fact, quality control personnel often are held crimi-
nally negligent in a court of law if sanitation problems reach litigation.
The third portion of the quality control mission involves management-man-
agement of people, procedures, policies, specifications, inventories, and infor-
mation. Decisions have to be made on the spot, and problems must be quickly
analyzed and corrected. Consequently, information must be readily available,
and communication must be timely and thorough. The day will soon come when
quality control decisions and functions will require the use of computers. Com-
puters and programmable calculators already are widely used, and computer
applications are an intrinsic part of this text. Citrus quality control software in
GWBASIC for IBM-compatible personal computers entitled "CITQUIC" is
available from the author, including not only those programs referred to in the
text, but integration of these programs into a complete inventory management
system and quality control program. One of the advantages of such software is
that the GWBASIC programs can easily be modified to fit any commercial need.
4 INTRODUCTION

Quality control personnel must always be prepared for any eventuality. If


they wait until trouble hits, it then may be too late to gain the skills or knowl-
edge needed to handle the situation properly. They should layout concrete
procedures and communication channels well in advance and follow those plans
meticulously to avoid errors in judgment or conflicts within the company as
well as with suppliers or customers. It should always be remembered, and it
will always be true, that people are what make any quality control department
or company successful and are a company's most valuable resource. The best
thing an employee can do for the company is help it to make a profit, and the
best thing a company can do for an employee is to make a profit. This mutual
goal can be achieved only in an atmosphere of cooperation, integrity, and tech-
nical competence.
Chapter 2

Brix and Soluble Solids

Citrus juices contain a wide variety of chemical compounds, but none as prev-
alent as sugars or carbohydrates. Carbohydrates make up better than 80% of
the soluble material in citrus juices, and of these soluble carbohydrates, half are
in the form of sucrose. The sucrose molecule consists of one molecule of glu-
cose and one molecule of fructose, as shown in Fig. 2-1. The other half of the
carbohydrates in citrus juices consist of relatively even amounts of glucose and
fructose, which result from natural enzymatic breakdown of the sucrose. Other
carbohydrates playa minor role in overall juice composition. Because sucrose
consists of one molecule of glucose and one molecule of fructose, the densities
of aqueous solutions of sucrose mixed with equal portions of glucose and fruc-
tose are similar to the densities of 100 % sucrose solutions.
Juice density is one of the most important quality control parameters in the
juice industry. Juice densities are used in making conversions, back and forth,
between volume and weight parameters in performing a host of important cal-
culations in predicting juice blends and formulations and juice concentration,
standardizing laboratory results, and managing inventories and marketing. Be-
cause carbohydrates occur in such high levels in citrus juices, juice density is
detennined by using methods and scales that apply to pure sugar solutions. The
soluble material is not all in the pure form of the major carbohydrate compo-
nents; so the soluble material, including some noncarbohydrates, is referred to
as soluble solids rather than sugars. However, the soluble solids are treated as
sugars in regard to density and other quality control measurements. Also, the
soluble solids differ from the insoluble solids, such as cloud and pulp material,
which contribute little to density measurements. Organic acids and their salts
also occur in significant amounts in citrus juices and contribute to the soluble
solids content. Corrections usually are applied to density measurements in order
to account for these noncarbohydrate soluble solids as if they were carbohy-
drates, to facilitate the use of carbohydrate scales and tables.
Several scales have been developed to relate the measured specific gravity or
density to the concentration of various solutions. The API scale, selected in

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
8 CITRUS JUICE CHARACTERISTICS

H 0 4 C H ,0o H

HO OH AOH H
H OH

GLUCOSE ° 0 CH 2
OH

CH,OH H

FRUCTOSE
Fig. 2-1. A sucrose molecule. composed of a molecule of glucose and a molecule of fructose.

1921 by the American Petroleum Institute, the U.S. Bureau of Mines, and the
National Bureau of Standards, is used for petroleum products. The Balling scale
is used by the tanning and tanning extract industries. The Baume scale was
proposed in 1768 by Antoine Baume, a French chemist, to measure the con-
centrations of acids and syrups that were lighter and heavier than water by using
a different scale for each type of solution. The Quevenne scale is an abbreviated
specific gravity scale used primarily by the milk industry. The Richter, Sikes,
and Tralles scales were developed to measure the alcohol content in water via
density, and the Twaddle scale is an attempt to simplify the density measure-
ments of liquids heavier than water.
One of the best-known scales relating the concentration of sucrose solutions
to solution density was published by Balling (Balling n.d.) and served as a basis
for the development of the more complete and expanded table established by
the German mathematician Adolf Ferdinand Wenceslaus Brix (1798-1870) in
1854. The original Brix density table, used exclusively by the sugar industry
for many years, was based on the density of a sucrose solution at a standard
temperature of 17.5 ° e. This scale based on 17.5 ° e still is used by the fresh
citrus fruit industry for maturity tests. Domke (1912) proposed a table of dens-
ities of sucrose solutions according to concentration based on sucrose solution
densities at 20 o e, which has since become the standard for the processed juice
industry. At least by 1941 the Brix scale was being used by the fruit juice
industry in determining the sucrose equivalent of soluble solids; the term "Brix"
or "degrees Brix" was being used interchangeably with the % sucrose or the
% soluble solids by weight in fruit juices and was determined by using density
measurements. This usage led to the Brix scale's becoming the standard for the
measurement of juice concentration in the citrus and related industries.

BRIX BY HYDROMETER

The most economical commercial method of measuring the Brix of citrus juices
uses a weighted spindle or hydrometer, illustrated in Fig. 2-2. The buoyancy
of the hydrometer is directly proportional to the density of the solution, and the
BRIX AND SOLUBLE SOLIDS 9

Juice Level

•••••••'~;;;;;;;;;;;;;I:l~;;;;;;~.. • • • • • • • •• t>
Hydrometer
. - Cylinder

....- I f - - Hydrometer

Thermometer

Temperature
Ind.f.:'I.--II--- Correction
Scale

Fig. 2-2. Hydrometer used to measure Brix levels in single-strength juices.

degree that the hydrometer sinks into the juice can be calibrated to a Brix scale
on the neck of the hydrometer, which can be read at the level where the juice
surface strikes the hydrometer neck.
Dissolved gases affect this buoyancy, so deaeration of the juice aids in ac-
curate Brix determinations by hydrometer. Air is incorporated into the juice
during processing through agitation, mixing, and pumping.
Temperature also affects the density of the solution; therefore, many Brix
hydrometers have a built-in thermometer accompanied by a temperature correc-
10 CITRUS JUICE CHARACTERISTICS

tion scale that can be used to correct the Brix reading. In the absence of such a
scale, a thermometer and Tables 2-1 and 2-2 can be used for hydrometers based
on 17.5 °C and 20.0°C, respectively, to make the Brix correction for tempera-
ture. Hydrometers usually are used to measure the Brix of single-strength juices
where acid corrections are small. Consequently, acid corrections generally are
not used with hydrometers.

Measurement of Brix by Hydrometer

Equipment and Supplies

• Deaerating setup shown in Fig. 2-3.


• Brix hydrometer covering the Brix range of interest.
• Thermometer and Tables 2-1 or 2-2 if the hydrometer does not have a
thermometer and correction scale built in.
• Hydrometer cylinder of sufficient size to allow the hydrometer to float freely
in the juice.
• Adequate juicing apparatus if whole fruit is to be tested.

Table 2-1. Temperature corrections to the Brix using a


hydrometer based on a standard temperature of 17.5 0 C
(Florida Department of Citrus 1982).
Temp Subtract from Temp Add to
°C Brix °C Brix
5.0 0.45 18.0-18.5 0.05
6.0 0.40 19.0-19.5 0.10
7.0 0.40 20.0-20.5 0.15
8.0 0.35 21.0-21.5 0.20
9.0 0.30 22.0-22.5 0.25
10.0 0.30 23.0 0.30
11.0 0.25 23.5-24.0 0.35
12.0 0.25 24.5 0.40
13.0 0.20 25.0-25.5 0.45
14.0 0.15 26.0 0.50
15.0 0.10 26.5-27.0 0.55
15.5 0.10 27.5 0.60
16.0 0.05 28.0-28.5 0.65
16.5 0.05 29.0 0.70
17.0 0.00 29.5-30.0 0.75
17.5 0.00 30.5 0.80
31.0 0.85
31.5-32.0 0.90
Table 2-2. Temperature correction to the Brix using a hydrometer
based on a standard temperature of 20.0ac
(Charlottenberg 1900).
Observed Percentage of Sugar
Temp.
°C o 5 10 15 20 25 30 35 40 45 50 55 60 70
Subtract from Brix
o .39.49 .65 .77 .89 .99 1.08 1.16 1.24 1.31 1.37 1.41 1.44 1.49

5 .36.47 .56 .65 .73 .80 .86 .91 .97 1.01 1.05 1.08 1.10 1.14

10 .32 .38 .43 .48 .52 .57 .60 .64 .67 .70 .72 .74 .75 .77
11 .31 .35 .40 .44 .48 .51 .55 .58 .60 .63 .65 .66 .68 .70
12 .29 .32 .36 .40 .43 .46 .50 .52 .54 .56 .58 .59 .60 .62
13 .26 .29 .32 .35 .38 .41 .44 .46 .48 .49 .51 .52 .53 .55
14 .24 .26 .29 .31 .34 .36 .38 .40 .41 .42 .44 .45 .46 .47

15 .20 .22 .24 .26 .28 .30 .32 .33 .34 .36 .36 .37 .38 .39
16 .17 .18 .20 .22 .23 .25 .26 .27 .28 .28 .29 .30 .31 .32
17 .13 .14 .15 .16 .18 .19 .20 .20 .21 .21 .22 .23 .23 .24
18 .09 .10 .10 .11 .12 .13 .13 .14 .14 .14 .15 .15 .15 .16
19 .05 .05 .05 .06 .06 .06 .07 .07 .07 .07 .08 .08 .08 .08

17.5 .11 .12 .12 .14 .15 .16 .16 .17 .17 .18 .18 .19 .19 .20
Add to Brix
21 .04 .05 .06 .06 .06 .07 .07 .07 .07 .08 .08 .08 .08 .09
22 .10 .10 .11 .12 .12 .13 .14 .14 .15 .15 .16 .16 .16 .16
23 .16 .16 .17 .17 .19 .20 .21 .21 .22 .23 .24 .24 .24 .24
24 .21 .22 .23 .24 .26 .27 .28 .29 .30 .31 .32 .32 .32 .32
25 .27 .28 .30 .31 .32 .34 .35 .36 .38 .38 .39 .39 .40 .39

26 .33 .34 .36 .37 .40 .40 .42 .44 .46 .47 .47 .48 .48 .48
27 .40 .41 .42 .44 .46 .48 .50 .52 .54 .54 .55 .56 .56 .56
28 .46 .47 .49 .51 .54 .56 .58 .60 .61 .62 .63 .64 .64 .64
29 .54 .55 .56 .59 .61 .63 .66 .68 .70 .70 .71 .72 .72 .72
30 .61 .62 .63 .66 .68 .71 .73 .76 .70 .78 .79 .80 .80 .81

35 .99 1.01 1.02 1.06 1.10 1.13 1.16 1.18 1.20 1.21 1.22 1.22 1.23 1.22

40 1.42 1.45 1.47 1.51 1.54 1.58 1.60 1.62 1.64 1.65 1.65 1.65 1.66 1.65

45 1.91 1.94 1.96 2.00 2.03 2.05 2.07 2.09 2.10 2.10 2.10 2.10 2.10 2.08

50 2.46 2.48 2.50 2.53 2.56 2.57 2.58 2.59 2.59 2.58 2.58 2.57 2.56 2.52

55 3.05 3.07 3.09 3.12 3.12 3.12 3.12 3.11 3.10 3.08 3.07 3.05 3.03 2.97

60 3.69 3.72 3.73 3.73 3.72 3.70 3.67 3.65 3.62 3.60 3.57 3.54 3.50 3.43
(Calculated from data on thennal expansion of sugar solutions by Plato and assumed that the hydrometer is of
lens 16 glass. Table should be used with caution and only for approximate results when the temperature differs
much from the standard temperature or from the temperature of the surrounding air.)

11
12 CITRUS JUICE CHARACTERISTICS

500 ml
Vacuum
Flask

Juice Deaerated Juice


Fig. 2-3. Deareation setup for hydrometer Brix measurements.

Procedure

1. Extract enough juice to fill the hydrometer cylinder, and place it in the
juice beaker shown in Fig. 2-3.
2. Evacuate the vacuum flask with clamps closed. Open the clamp to the
juice beaker, and draw the juice into the flask.
3. Turn off the vacuum source, and break the vacuum by leaving the juice
beaker clamp open.
4. Open the second clamp, and allow juice to flow into the deaerated juice
beaker.
5. Fill the hydrometer cylinder with the de aerated juice, and insert the hy-
drometer into the cylinder so that the juice overflows the cylinder. This
is best done in a sink or outside.
6. Read the Brix where the level of the juice meets the Brix scale in the neck
of the hydrometer, as shown in Fig. 2-2.
7. Using the thermometer, measure the temperature, and add or subtract the
temperature correction to the Brix according to the scale in the hydrom-
eter, or use Tables 2-1 or 2-2 if no correction scale is available.
BRIX AND SOLUBLE SOLIDS 13

BRIX BY REFRACTOMETER

Even though refractometers are more expensive than hydrometers, they require
only 2 to 3 ml of sample, compared to about 200 ml or more required by the
hydrometer, and deaeration generally is not necessary. Brix measurements can
be performed much faster, and the Brix range of refractometers can be much
broader, up to 0 to 70oBrix, which is important in processing plants that man-
ufacture concentrated juices. These advantages quickly justify the use of re-
fractometers in processing plants in spite of their cost. For an instrument that
is used as often as a refractometer, with quality control, inventories, packaging,
and marketing depending on the results, the cost of the instrument is trivial; the
refractometer literally becomes the foundation of any citrus juice processing
procedure. In fact, it is wise to have at least two refractometers so that if one
needs to be repaired, the operations of the plant will not be hampered. Having
two refractometers also provides a means of checking and comparing results to
ensure accuracy.
The refractive principle that forms the basis of this type of measurement lies
in the variability of the speed of light through two mediums of different density.
To illustrate this principle, a simple analogy can be used. Suppose that a person
is drowning offshore, as shown in Fig. 2-4, and a lifeguard is trying to deter-
mine which is the fastest way to reach her. Even though the shortest distance
between two points is a straight line, it is not necessarily the fastest; in this
case, the lifeguard probably can run faster than he can swim. Thus he would
want to spend as much time as possible running and the least amount of time
swimming. The speed that he can run and the speed that he can swim are de-
termined by the density of the mediums through which he must pass, and de-
termine the ideal angle that he should take to reach the drowning victim in the
shortest possible time. It is a phenomenon of nature that light "knows" the
ideal angle that will allow it to arrive at a certain point, going from one medium
to another of different density, in the shortest possible time. As the densities of
one or both of the mediums change, so does this angle. Thus a change in the
angle of refraction permits the measurement of the density of citrus juices, as
light passes through the juice at one density and then through a glass prism at
another density, which can be translated into the concentration as degrees Brix.
The wavelength of light used with a refractometer has been shown to affect
the angle of refraction, and, for this reason, a sodium vapor lamp has been
suggested for use as a light source. However, any soft yellow lamp is sufficient
for industrial purposes. The light first enters a fogged or ground glass lens that
evenly scatters the light in all directions, as shown in Fig. 2-5. The scattered
light then enters the sample and is refracted at the surface of the prism on which
the sample lies. The critical ray is a ray that travels parallel to the surface of
the prism and represents the minimum angle at which the scattered light coming
14 CITRUS JUICE CHARACTERISTICS

-"'--

---
~
I
Shortest I
I

----i-
I
~I
i
Fastest
----------- : .....
': . '"

~ ".
. .'
" ,'.
,':" . -', .....
,',: ,'.

Fig. 2-4. Illustration suggesting why light refracts when going from one medium into another
medium of greater density, Light has a "nose" for the fastest route and bends or refracts accord-
ingly ,

through the sample can strike the prism, Of course, a ray perfectly parallel to
the surface of the prism never will strike the prism, If it changed its angle
slightly, however, it would be refracted, defining a boundary for a dark zone
or area, as shown in the figure. As perceived from the side, as illustrated, no
scattered light coming from the surface of the prism can enter the dark zone,
This dark area boundary can easily be calibrated to a Brix scale because both
the Brix and the angle of refraction are determined by the sample density,
Because the standard error for Brix readings is ±O . l°Brix, the law of sig-
nificant figures dictates that Brix values should be expressed only to the nearest
tenth of a Brix (see Chapter 23). Brix values expressed to more decimal places
than this imply deceptive accuracy. Acid corrections and temperature correc-
tions often are expressed to two decimal places . When these corrections are
applied, the final Brix value should be rounded to the nearest tenth of a Brix.
Several factors contribute to the errors in Brix readings. One of the greatest
sources of errors is the fact that citrus juices, especially concentrates, produce
an indistinct shadow or boundary between the dark and light zones of the re-
fractometer due to insoluble matter in the juice. This fuzzy shadow engenders
a wide range of opinions as to where the Brix value should be read. Whether
BRIX AND SOLUBLE SOLIDS 15

Light Source

Fogged Prism

1 " - - Light Barrier

.....- - Dark Zone

t
Prism Brix
Scale

Fig. 2-5. Illustration of the formation of the shadow in a refractometer. No light can enter the
dark zone because of refraction as the light passes from the sample into the prism at a different
density.

the shadow is adjusted to the intersection of two cross hairs or used directly on
a Brix scale itself, the Brix should be read in the middle of this fuzzy region,
where it is estimated that a perfect shadow line would appear if the fuzzy line
were clear and focused. Calibration of shadow readings can be achieved by
having lab technicians measure the Brix of several samples and comparing the
results of one lab technician to another. Those that are reading too high or too
low will easily be detected and thus can be corrected. This type of comparison
should be done as often as needed to ensure consistency and confidence in re-
sults. In fact, such multitechnician calibrations should be performed for all lab-
oratory procedures, regularly or as often as needed.
Another source of Brix reading error is the refractometer itself. Most refrac-
tometers have an adjustment screw that permits calibration of the shadow. This
can be done with standard sucrose solutions, but the use of distilled water to
calibrate the refractometer according to the refractive index is sufficient in most
cases. The refractive index is the ratio of the sine of the angle between the
incident ray and the line perpendicular to the surface of the prism to the sine of
the angle between the refracted ray and the same perpendicular line. The pro-
cedure for the calibration of a refractometer using distilled water is as follows.
16 CITRUS JUICE CHARACTERISTICS

Calibration of a Refractometer

Equipment and Supplies

• Refractometer with calibration screw.


• Distilled water.
• Dropper or plastic stirring rod.
• Wrench or screwdriver needed to adjust screw.
• Table 2-3.
• Thermometer if the refractometer does not provide for the measurement of
the temperature.

Procedure

1. Measure the temperature of the water if the refractometer does not have
a means of doing so.
2. Place a few drops of the distilled water onto the prism of the refractometer
using a dropper or plastic stirring rod, being careful not to scratch the
prism. If the temperature is to be measured by the refractometer, let the
sample sit for a few minutes for the temperature to equilibrate. Otherwise,
read the Brix right away.
3. Using Table 2-3, look up the refractive index for water at the temperature
determined above.
4. Switch the refractometer to measure the refractive index instead of the
Brix, and adjust the refractometer to read the refractive index determined
from Table 2-3 regardless of where the shadow occurs.
5. Using the wrench or screwdriver, adjust the calibration screw until the

Table 2-3. The refractive index of distilled


water at various temperatures
(Weast 1968).
°C nD °C nD
lO 1.3337 21 1.3329
11 1.3336 22 1.3328
12 1.3336 23 1.3327
13 1.3335 24 1.3326
14 1.3335 25 1.3325
15 1.3334 26 1.3324
16 1.3333 27 1.3323
17 1.3332 28 1.3322
18 1.3332 29 1.3321
19 1.3331 30 1.3320
20 1.3330
BRIX AND SOLUBLE SOLIDS 17

shadow is aligned with the cross hairs or agrees with the refractometer
reading from Table 2-3.
6. Switch the refractometer back to the Brix mode.
(The instructions may vary slightly from one instrument to another. The
manufacturer's operational manual should be consulted for details.)

Temperature Corrections

Temperature fluctuations also affect the Brix reading for refractometers, and
temperature corrections are required, as with the hydrometer. However, be-
cause the Brix is measured by using a different principle, the correction tables
are different, as can be seen by comparing Tables 2-1 and 2-2 with Table 2-4.
Many modem refractometers make this correction automatically. By applying
a double-nested least squares analysis to the data in Table 2-4, the following
equation can be constructed, which can be used in computer applications instead
of Table 2-4.

CorT = B2( +1.425 x 10- 4 - 8.605 x 1O- 6 T + 7.138 x 1O- 8 T 2 )


+ B( -2.009 X 10- 2 + 1.378 X 10- 3 T - l.857 X 10- 5 T2)
+ (-7.788 X 10- 1 + 1.700 x 1O- 2 T + 1.100 x 1O- 3 T 2 ) (2-1)

The correction calculated above from the Brix (B) and the centigrade temper-
ature (T) can be added to, if positive, or subtracted from, if negative, the Brix
reading to give a temperature-corrected Brix.

Acid Corrections

As mentioned previously, citric acid corrections are necessary as well as tem-


perature corrections. Appendix A gives the corrections that must be added to
the Brix reading according to the % titratable acidity as citric acid, determined
as described in Chapter 3. It must be remembered that other organic acids, such
as malic acid, may comprise as much as 10% of the total organic acids present
and may affect the Brix reading in a different manner from citric acid. Also,
titration does not account for salts of the organic acids, which can be present
up to about 20 % of the total salts and acids and also affect the Brix reading
(Shaw, Buslig, and Wilson 1983). The error in the Brix reading resulting from
undetected salts and organic acids other than citric acid is usually insignificant
on an industrial basis or, at least, is ignored by the industry. Again, by applying
least squares regression analysis to Appendix A the following can be obtained:

CorA = = 0.014 + 0.192A - 0.00035A2 (2-2)


~

Table 2-4. Temperature corrections to the Brix reading using a refractometer based on a standard of co
temperature of 20°C (J./ntern. Sugar 1937). n
:::j
21
Subtract from the Brix c:
(II
Brix a 5 10 15 20 25 30 35 40 45 50 55 60 65 70 c-
c:
·c 0m
10 .50 .54 .58 .61 .64 .66 .68 .70 .72 .73 .74 .75 .76 .78 .79
11 .46 .49 .53 .55 .58 .60 .62 .64 .65 .66 .67 .68 .69 .70 .71
n
J:
12 .42 .45 .48 .50 .52 .54 .56 .57 .58 .59 .60 .61 .61 .63 .63 lo
21
13 .37 .40 .42 .44 .46 .48 .49 .50 .51 .52 .53 .54 .54 .55 .55 lo
14
n-I
.33 .35 .37 .39 .40 .41 .42 .43 .44 .45 .45 .46 .46 .47 .48 m
15 .27 .29 .31 .33 .34 .34 .35 .36 .37 .37 .38 .39 .39 .40 .40 21
r;;
-I
16 .22 .24 .25 .26 .27 .28 .28 .29 .30 .30 .30 .31 .31 .32 .32 0
(II
17 .17 .18 .19 .20 .21 .21 .21 .22 .22 .23 .23 .23 .23 .24 .24
18 .12 .13 .13 .14 .14 .14 .14 .15 .15 .15 .15 .16 .16 .16 .16
19 .06 .06 .06 .. 07 .07 .07 .07 .08 .08 .08 .08 .08 .08 .08 .08

Add to the Brix


21 .06 .07 .07 .07 .07 .08 .08 .08 .08 .08 .08 .08 .08 .08 .08
22 .13 .13 .14 .14 .15 .15 .15 .15 .15 .16 .16 .16 .16 .16 .15
23 .19 .20 .21 .22 .22 .23 .23 .23 .23 .24 .24 .24 .24 .24 .24
24 .26 .27 .28 .29 .30 .30 .31 .31 .31 .31 .31 .32 .32 .32 .32
25 .33 .35 .36 .37 .38 .38 .39 .40 .40 .40 .40 .40 .40 .40 .40

26 .40 .42 .43 .44 .45 .46 .47 .48 .48 .48 .48 .48 .48 .48 .48
27 .48 .50 .52 .53 .54 .55 .55 .56 .56 .56 .56 .56 .56 .56 .56
28 .56 .57 .60 .61 .62 .63 .63 .64 .64 .64 .64 .64 .64 .64 .64
29 .64 .66 .68 .69 .71 .72 .72 .73 .73 .73 .73 .73 .73 .73 .73
30 .72. .74 .77 .78 .80 .80 .81 .81 .81 .81 .81 .81 .81 .81 .81
BRIX AND SOLUBLE SOLIDS 19

where A is the % titratable acidity. The federal code utilizes the equation:

CorA = 0.012 + 0.193A - 0.0004A2 (2-3 )

which is slightly less accurate in the acid level ranges of commercial lemon and
lime concentrations (CFR, Title 21, 146.132(a)(2) 1983).
The procedure for measuring the Brix level by refractometer is as follows.

Measurement of Brix by Refractometer

Equipment and Supplies

• Refractometer.
• Thermometer if refractometer does not provide for the measurement of the
temperature.
• Table 2-4 if the refractometer does not automatically correct for the tem-
perature.
• Appendix A and a % titratable acid value in order to make acid corrections
to the Brix.
• Dropper or plastic stirring rod.
• Water and cleaning tissue for prism.

Procedure

1. Using the water and cleaning tissue, clean and dry the prism and the sur-
face of the fogged glass used to scatter the light.
2. Prepare the sample by stirring with the plastic stirring rod and/or swirling,
and, using the plastic stirring rod or sample applicator, place a few drops
of the sample onto the prism. Care should be taken not to use metal ap-
plicators or other devices that may scratch the surface of the prism. Bub-
bles or foam also will distort the Brix reading.
3. Close the refractometer by lowering the fogged glass onto the sample, and
make sure that it is securely in place.
4. Position the light source to shine through the fogged glass, adjusting the
shadow to the cross hairs, and read the Brix, or read the Brix directly if
the shadow falls directly on the Brix scale itself. Cold samples may need
to sit a few minutes so that the temperatures can equilibrate.
5. Using Table 2-4 or Equation 2-1 and Appendix A or Equation 2-2, make
the necessary acid and temperature corrections, and round off the cor-
rected Brix to the nearest tenth of Brix. The standard Brix error is
±O.I°Brix. The Brix can be compared to the USDA grade standards de-
picted in Table 2-5.
20 CITRUS JUICE CHARACTERISTICS

Table 2-5. Minimum standards for Brix for USDA grades.


Orange Juice (47FR 12/10/82, 52.1551-52.1557)
Type of Juice Grade A Grade B
Pasteurized orange juice 11.0* 10.5*
Concentrated orange juice for 11.8* 11.8*
manufacturing
Orange juice from concentrate 11.8* 11.8*
Reduced acid orange juice 41.8* 41.8*
Reconstituted reduced acid 11.8* 11.8*
orange juice
Dehydrated orange juice 11.8* 11.8*

unsw sw unsw sw
Frozen concentrated orange 41.8 42.0 41.8 42.0
juice
Reconstituted frozen concen- 11.8* 11.8*
trated orange juice
Canned orange juice 10.5 10.5 10.0 10.5
Canned concentrated orange 41.8 42.0 41.8 42.0
juice
Reconstituted canned concen- 11.8* 11.8* 11.8* 11.8*
trated orange juice
Grapefruit Juice (48FR 9/12/83, 52.1221-52.1230)
Grade A Grade B
Type of Juice unsw sw unsw sw
Grapefruit juice 9.0 11.5 9.0 11.5
Grapefruit juice from concentrate 10.0 11.5 10.0 11.5
Frozen concentrated grapefruit 38.0 38.0 38.0 38.0
juice
Reconstituted frozen concentrated 10.6 10.6* 10.6 10.6*
grapefruit juice
Reconstituted dehydrated grape- 10.0 11.5 10.0 11.5
fruit juice
Reconstituted concentrated grape-
fruit juice for manufacturing 10.5 10.5

Grapefruit and Orange Blend (6FR 1111172, 52.1281-52.1290)


Grade A Grade B
Type of Juice unsw sw unsw sw
Single strength 10.0 11.5 9.5 11.5
Reconstituted 11.0 12.5 11.0 12.5

Tangerine Juice (2FR 7/1/69,52.2931-52.2941)


Grade A Grade B
Type of Juice unsw sw unsw sw
Concentrated tangerine juice for
manufacturing 10.6 10.6
Canned tangerine juice 10.5 12.5 10.0 12.5
*Juice solids only before or without sugar addition.
BRIX AND SOLUBLE SOLIDS 21

USE OF BRIX VALUES IN PROCESSING

Citrus juices are manufactured at a variety of concentrations or Brix levels,


which can be adjusted up or down by using commercial evaporators, blending,
or adding water. It is often more convenient to base marketing, packaging, and
inventory systems on the weight of soluble solids without the water, rather than
on the volume of the juice. Juice prices are based on so much per pound of
soluble solids, whether the product is single-strength juice or concentrate. The
weight of the soluble solids is determined by the weight or volume of the juice
and the degrees Brix or concentration. The weight of the soluble solids is de-
rived from the weight of the juice (W) and the Brix (B), by usng the following
equation.

Ws = BW/IOO (2-4 )

For example, if the net weight of a tanker of concentrate is 41,890 lb with a


Brix of 60.2°Brix, the weight of the soluble solids, using Equation 2-4, is 25,218
lb. If the price of juice is $1.30/lb soluble solids, the cost of such a tanker load
of concentrate is 25,218 x $1.30 = $32,783.
Most juice products are packaged by weight, whether they be in cans, drums,
or tankers. However, it is more convenient to use juice volumes in juice for-
mulations, blends, and other in-house processing. In order to do this, the Brix,
which is purely a weight/weight parameter, must employ a density conversion
to convert the weight parameters to volume parameters. When blending is done,
the easily measured volumes need to be converted to weight of soluble solids
by using specific gravity tables or density equations according to Brix.
Many forms of density tables for aqueous sucrose solutions as a function of
Brix have emerged in the past 140 years. The most accurate and up-to-date table
was published by Chen (1983) and provides a basis for modem citrus quality
control technology. Kimball (1986) used this table to generate regression equa-
tions that can be used instead of the table and are convenient for computer
programming. The pounds of soluble solids as sucrose per gallon of solution
(SPG) can be calculated from the Brix (B) and density (D in pounds of solution
per gallon) as follows:

SPG = BD/IOO (2-5 )

The density in grams of solution per milliliter (d) can be used to calculate D:

D = d(3785.306 ml/gal)/(453.59237 g/lb) (2-6)

Kimball's regression expression for d as a function of Brix is:

d = 0.524484e(B+330.872)2/170435 (2-7)
22 CITRUS JUICE CHARACTERISTICS

which can be used in Equations 2-5 and 2-6 to give the following:
SPG = 0.0437691Be(B+330.872)2/170435 (2-8)
D = 4.37691e(B+330.872)2/ 170435 (2-9)

The above equations, expressed as a sole function of Brix, make it possible to


use small computer subroutines in performing various quality control calcula-
tions. Some programming languages, such as RPG, cannot perform the expo-
nential functions in Equations 2-8 and 2-9. The following Taylor series expan-
sions of these equations can be used instead:

SPG = 0.0437691B(1 + :~~ (B + 330.872 t /(170435 f n!) (2-10)

D = 4.37691 (1 + :t~ (B + 330.872t /(170435 t n!) (2-11)

An example of a subroutine using RPG program language for Equation 2-10


can be found in Appendix B.
One application of the use of these equations is in calculating the amount of
water (Vw ) needed to reconstitute or dilute a given volume of citrus concentrate
(V) at an excessively high Brix (B H ) to a desired Brix (B). First, the SPGH
and the SPG desired must be calculated by using Equation 2-8 (or 2-10) above,
from the BH and B values. Then the following equation can be used:

Vw = V(SPGH - SPG)/SPG (2-12 )

For example, if we had 1000 gallons of 65.0 o Brix concentrate and wanted to
dilute it to 60.00Brix, the water needed would be:

Vw = (1000 gal) (7. 135650Brix - 6.4366QoBriJ/6.4366QoBrix

Vw = 109 gal

A particularly irritating problem occurs when a tank is full, and the Brix is
too high or too low. As there is no room for volume adjustments, some of the
juice needs to be removed and replaced with concentrate of a higher Brix or
water. The volumes involved can be calculated as explained in the following
paragraphs.

Brix Is Too Low

If the Brix is too low in a tank filled to capacity, and we need to add a higher
Brix concentrate to raise the Brix, we can use the following:

(2-13 )
BRIX AND SOLUBLE SOLIDS 23

where VH is the volume of the juice that we want to replace in the tank, V is
the volume desired or the tank capacity, SPG is calculated from the desired Brix
using Equation 2-8, SPGL is calculated from the original low Brix level in the
tank, and SPGH is calculated from the Brix of the concentrate that will be used
to bring the Brix level up. For example, if we have a WOO-gallon tank full of
60.0 oBrix concentrate that we want to raise to 62.0oBrix using 65.0 oBrix con-
centrate, using Equation 2-13 we would get:

VH = (1000 gal) (6.712 - 6.436)/(7.135 - 6.436) = 395 gal

where 6.712 is the SPG desired (62.0oBrix) calculated from B, 6.436 is the
SPGL calculated from the existing low Brix (60.0 oBrix), and 7.135 is the SPGH
calculated from the 65.0 oBrix concentrate used for the adjustment. In other
words, in this example, we would replace 395 gallons of 60 0 Brix concentrate
with 65°Brix concentrate to get a full tank of exactly 62°Brix concentrate.

Brix Is Too High

If the Brix is too high, and we want to add water to reduce the concentration,
we can use the following:

(2-14 )

where Vw is the amount of water that is needed to replace a portion of the


concentrate, VH is the desired volume or the tank capacity, SPGH is the pounds
soluble solids per gallon calculated from the overly concentrated original juice
Brix using Equation 2-8, and SPG is calculated from the desired Brix. For
example, if we have a WOO-gallon tank full of 65.0 oBrix concentrate, and we
want to drop the Brix to 62.0oBrix, Equation 2-14 can be used as follows:

Vw = (1000 gal)(7.135 - 6.712)/7.135 = 59 gal

with the SPG values calculated from the Brix values by using Equation 2-8 as
before. In other words, we would need to replace 59 gallons of the 65°Brix
with water to get a full tank of exactly 62°Brix concentrate.
We can easily see that involved computations are often required to account
for one of the many parameters of citrus juice. Not only are these and the
computations found hereafter complex, but they are often routine and must be
performed over and over again. Such situations are ideally suited for computer
applications. Computing devices range from hand-held programmable calcula-
tors to sophisticated multiterminal mainframe computers. Programming lan-
guages also differ considerably. However, the basic logic of how these equa-
24 CITRUS JUICE CHARACTERISTICS

tions can be used varies little and can be represented in the form of flow charts.
These flow charts can be used as is or modified to fit any industrial need in the
writing of programs for any computing device.
The flow charts in Fig. 2-6 through Fig. 2-9, and throughout the remainder
of this text, illustrate some computer logic that can be used in routine citrus

6rix on hand (6,)


6rix desired (6)
Volume on hand (Vc)

EQ 2-14 EQ 2-13
Vw EQ 2-18
VH
(n=2)
V,orVw

Fig_ 2-6. Flow chart for a computer program that will determine the Brix adjustment in citrus
juices.
BRIX AND SOLUBLE SOLIDS 25

Concentrate Brix (Bc)


SS Juice Brix (Bj)
Desired Brix (Bd)
Desired Volume (Vd)

EQ 2-15
Vj
Vc = Vd - Vj
Fig. 2-7. Flow chart for programming a computer to cal-
culate the volume of juice and high Brix concentrate to
make a juice product.

quality control. There are four different box shapes, which imply specific func-
tions. A rectangle with a curved or tear-sheet bottom represents input of data
or the output of results. Within these boxes you will find the data that needs to
be inputted or the variable that represents the final targeted output or answer.
Diamond-shaped boxes represent decisions that have to be made by the com-
puter or the operator. Circles represent the use of subroutines that have been
found useful in more than one program or more than once in the same program.
Plain rectangles represent computations that are unique to the program and do
not justify the formation of a subroutine.
Figure 2-6 shows a flow chart that can be used to program a computer to
calculate the amount of Brix adjustment needed in a tank with a Brix that is too
high or too low, as discussed previously. The input data includes the Brix of
the tank, the desired Brix, and the volume of the juice in the tank. The computer
26 CITRUS JUICE CHARACTERISTICS

Brix of Camp. n (Bn)


.---~~I Vol. of Camp. n (Vn)

Bf=10xSPG

B = Bf

n
Z = L: Vi (SPGi)
i=1
n
V=L: Vi
i=1
no

no

B = Bf = average Brix

EQ 2-16
SPG = ZN

Fig. 2-8. Flow chart that can be used to program computers to calculate the average Brix of a
blend.

then must detennine if the Brix on hand is too high or too low compared to the
desired Brix. It then must know if the volume of the juice can vary. If the tank
is full, the volume cannot vary. If there is room in the tank to adjust the Brix
level, then the volume can vary. Subroutines using Equation 2-8 can then be
used to detennine the SPG values needed, and Equation 2-13, 2-14, or 2-18
BRIX AND SOLUBLE SOLIDS 27

Brix of Camp. n (Bn)


Brix of 1 st Camp (B 1)
Volume of Camp. n (Vn)
(except V1)
Final desired Brix (B)

n
Z = l:
Vi (SPGi)
n=2
n
V = l: Vi
n=2

no

EQ 2 -18
V 1 = V (SPG) - Z
SPG1 -SPG Fig. 2-9. Flow chart that can be used to pro-
gram computers to calculate the volume of a
single blend component needed in a blend to
achieve a desired Brix.

can be used to detennine the final volume of water or high Brix juice needed to
achieve the desired Brix.
An example of the use of this flow chart using GWBASIC can be found in
Appendix B. A similar program for the HP-41C programmable hand-held cal-
culator can be found in Appendix C.
28 CITRUS JUICE CHARACTERISTICS

Fresh Cutback Juice

Because important volatile flavor components of the juice are lost during evap-
oration, a common, though obsolete, practice is to restore the lost flavor com-
ponents by diluting high Brix concentrates with freshly extracted juice (cutback
juice). This can be done by using the SPGc calculated from the Brix of the
concentrate in Equation 2-8, the SPGj calculated from the Brix of the single-
strength juice, the SPG calculated from the desired final Brix, and the corre-
sponding volumes (Vo lj, and V):

(2-15 )

For example, if we wanted to make 1000 gallons of 41. 8 °Brix concentrate from
12.0oBrix freshly extracted juice and 60.0 oBrix concentrate, using Equation
2-15 we would get:

v = l000(6.436 6o ,ooBrix - 4. 13341.8oBrix) = 427 gal12°Brixjuice


] ( 6 .43660 ,ooBrix - 1. 047 12.0oBrix)

To find the gallons of concentrate that would be needed, you can subtract 427
gallons of the single-strength juice from the needed 1000 gallons to get 573
gallons of concentrate ( Vc ). This method of using cutback juice has largely been
replaced by the addition of aromas recovered from commercial evaporator con-
densates and single-strength or folded citrus oils recovered from citrus peel.
In Fig. 2-7, the volume of cutback juice and concentrate needed to make a
concentrate blend can be determined. The four input values must be entered,
the subroutine using Equation 2-8 must be used to calculate the SPG values,
and Equation 2-15 can be used to calculate the final cutback juice and concen-
trate volumes. An example of a GWBASIC program using this flow chart can
be found in Appendix B.

Brix Blending

The previous example of using cutback juice to blend with high Brix concen-
trates illustrates general juice blending using only two blend components. The
sophisticated blending common in the industry today is the blending of multiple
juice components in order to achieve a desired final product. One of the main
specifications desired in the final product is the Brix value. To blend more than
one juice component to achieve a desire Brix level or range, the following equa-
tion can be used:

SPG = V1SPG1 + V2 SPG2 + V 3 SPG3 + ... + VnSPGn (2-16)


V
BRIX AND SOLUBLE SOLIDS 29

where SPG and V are the final calculated values after blending n components.
Once the final SPG has been calculated, the corresponding final Brix can be
calculated by making successive approximations using the following equation:

BI = SPG /(0.0437691 e(B + 330.872)2/170435) (2-17)

Again, the exponential expression can be replaced with the Taylor series ex-
pansion in Equation 2-10 if it is necessary to facilitate computer programming.
In using Equation 2-17, a first guess for the B value can be made by multiplying
the SPG value by 10. The BI value then can be calculated and compared to the
original B value used. If they differ by more than 0.0001 °Brix, then the BI value
can become the new B value to calculate a new BI value. The differences be-
tween the two Brix values should quickly converge to identical values, which
then can be used as the final calculated exact Brix of the blend. Again, tables
can be and have been used to convert back and forth between SPG and Brix
values, but the use of these equations makes it possible to completely automate
blend calculations.
The following example illustrates the use of these equations. Suppose that
we want to calculate the final average Brix of a blend consisting of five lots (see
tabulation below). The volumes of the given lots can be expressed in gallons
or in 52-gallon drums, and the calculation is valid as long as the same units of
volume are used throughout the calculation.

LotH Drums Brix SPG


3 58.8 6.273
2 2 61.4 6.629
3 65.3 7.178
4 11 61.4 6.491
5 8 60.1 6.450

The SPG values can be calculated from the given Brix values by using Equa-
tion 2-8 (or 2-10), or found from a table. They are given here for convenience,
to illustrate the calculation procedure for the blend. Using Equation 2-16 we
get:

SPG = _3(-,-6_.2_7_3~)_+_2-,(_6._62_9-,-}_+_1-,-(7_.1_7_8~)_+_1_1....:....{6_.4_9_1-,--}_+_8---,(,-6_.4_50-"..}
25
= 6.490

This SPG value can be used to determine the corresponding Brix by means of
tables or Equation 2-17. A first guess for B in Equation 2-17 could be lOx
6.490 or 64.9°Brix, which converges to 60.4°Brix quickly via successive ap-
proximations, which becomes the exact calculated Brix of the final blend.
30 CITRUS JUICE CHARACTERISTICS

In Fig. 2-8 the average Brix can be calculated for a blend. The Brix and the
volume of the first component are entered, the subroutine using Equation 2-8
is used to obtain the SPG value, and summations are begun to obtain the inter-
mediary values of Z and V. The computer must determine if this is the last
record. If it is not, then the computer will prompt the operator is to input the
data of the next component. This continues generating the summation values of
Z and V until the data of the last blend component is entered. Equation 2-16
then can be used to calculate the average SPG value. The first guess in the
successive approximations in Equation 2-17 is made by multiplying the SPG
value by 10, and Equation 2-17 is used until the two Brix values are within a
preset range. When the two Brix values are within range, they represent the
output as the average Brix of the blend, the desired result. In Appendix B is a
GWBASIC program example of the use of this flow chart. After entering the
Brix and volume of the last component, you enter' '0" when asked for the next
Brix. The program will list the input data and calculate and display the average
Brix and total volume. A similar program that can be used with an HP-41C
programmable hand-held calculator can be found in Appendix C.
Many procedures require that the blend target a specific Brix or Brix range.
In order to achieve the desired targeted Brix, the blend components need to be
altered or rearranged. The final Brix can be fine-tuned to a specific target, usu-
ally by adjusting the volume or the Brix of a single component. Algebraic rear-
rangement of Equation 2-16 can be used to automate this procedure.

(2-18 )

The SPG value can be determined from the desired or target Brix, and the exact
amount of component 1 needed to achieve this Brix can be calculated. If a
negative number is obtained, then you will know that you must vary another
blend component in order to achieve the desired Brix. To illustrate the use of
Equation 2-18, suppose that we wanted to know how many drums of blend
component 1 in the previous example we would need to achieve exactly
60.0 o Brix. Using the data given and Equation 2-18, we obtain:

6.436(2 + 1 + 11 + 8) - 2(6.629) - 1(7.178) - 11(6.491) - 8(6.450)


VI = ----~------------~----~--~----~--~----~----~--~--~
(6.273 - 6.436)
VI = 11 drums

The 3 drums of lot #1 given in the example would give a final Brix of 60.4,
but it would take 11 drums to bring the Brix down to exactly 60.0. Equation
BRIX AND SOLUBLE SOLIDS 31

2-16 can be rearranged in several different ways to enable the varying of the
Brix of a component rather than the volume, or the varying of serveral com-
ponents. The more components you vary, the more complex the calculation
becomes.
Figure 2-9 shows the flow chart that can be used to determine the volume
needed of one blend component in order to achieve a targeted or desired Brix
in a blend. The input data is, again, the Brix and volumes of the known blend
components (all except blend component 1 in this case), as well as the final
desired target Brix. The Brix value of the component whose volume will vary
(component 1) needs to be entered as well. The Equation 2-8 subroutine is used
to calculate the needed SPG values, and the intermediary summations are per-
formed. If this blend component is not the last blend component, then the data
from the next blend component is entered until all the blend components are
entered and the proper summations performed. Equation 2-18 can then be used
as shown in the flow chart to determine how much of blend component 1 is
needed to achieve the desired Brix. An example of the use of this flow chart is
illustrated in the GWBASIC program found in Appendix B.

Temperature Corrections to Density

The SPG values used above are based on the density of the juice at 20.0°C.
These values are generally accurate enough for industrial purposes. Chen's ta-
ble also lists densities as a function of temperature (O-50°C) at various Brix
levels. Because most juices and concentrates are processed at much colder tem-
peratures (-20 to 5°C), accounting for the effects of temperature on juice
density may be in order, provided that sufficient computer resources are avail-
able. Making manual calculations to account for these temperature effects gen-
erally is not worth the trouble involved. By performing least squares regression
analyses on Chen's data, the following equation was found to be accurate within
the range of his data (0-50°C).

D = a + bB + eB2 + T(d + e/B +f /B2) + T 2 (1/(g + hB))

a = 8.35100 e = 7.60258 x 10- 3


b = 3.12158 X 10- 2 f = -5.24849 X 10- 2
e = 1.47241 x 10- 4 g = -31481.1
d = -7.033l3 X 10- 4 h = 98.7441 (2-19 )

In the above equation, B is the Brix, T is the centigrade temperature, and D is


the density in lb / gal and can be used in Equation 2-5 to calculate the SPG
value.
32 CITRUS JUICE CHARACTERISTICS

QUESTIONS

1. Who developed the Brix scale and between what years?


2. Do both the fresh fruit industry and the processing industry use the same
Brix scale?
3. Do Brix measurements, as described in this chapter, account for all the
soluble solids in citrus juices?
4. List and compare the advantages and disadvantages of using hydrometers
and refractometers in Brix measurements.
5. List six factors that affect Brix readings using a refractometer.
6. Why do hydrometers and refractometers use different temperature cor-
rection scales?
7. In determining the weight of soluble solids of citrus juices, can the Brix
be used directly with weights of juices or with volumes of juices, and
why?
8. Under what conditions would density tables be more convenient to use
than the equations described in the chapter?
9. What is the basic inventory unit of citrus juices, and why?
10. List some reasons why you think a processor may want to blend juices.

PROBLEMS

1. If an uncorrected Brix of 10.6 were obtained from a hydrometer with a temperature


reading of 15°C, what would the final corrected Brix be according to the fresh fruit
industry? The processing industry?
2. One of the advantages of Equation 2-1 is that it can extrapolate temperatures at Brix
values between the ones listed in Table 2-4. What is the temperature correction of
a l2.0oBrix sample at lSoC according to Equation 2-1, and how does this compare
to the estimated value from Table 2-4?
3. Using Equations 2-2 and 2-3, what are the acid corrections to the Brix of samples
containing 0.76,3.83,24.76, and 37.86% acid? Compare the results to the values
obtained from Appendix A.
4. You have a Brix reading from a refractometer that does not correct for temperature
of 11.1 °Brix. The temperature reading is 23°C with an acid level of 1.08 % acid.
What is the corrected Brix?
5. You have a Brix reading of 60.2 °Brix from a refractometer that does not correct for
temperature that gives a temperature reading of 16°C with an acid level of S.23%
acid. What is the corrected Brix?
6. How much water needs to be added to 4S7 gallons of 6l.soBrix concentrate in order
to reconstitute it to ll. 8 °Brix juice? How much juice from concentrate can this
make?
7. How much 64.soBrix concentrate is needed to adjust a full 1 ISO-gallon tank con-
taining 39.6°Brix in order to obtain 41.8°Brix concentrate?
BRIX AND SOLUBLE SOLIDS 33

8. What would be the final Brix after blending the following blend components? Could
this product be used to make Grade A Frozen Concentrated Orange Juice according
to USDA standards?

Bulk Tank Gallons Brix


A 207 65.3
B 575 62.1
C 1102 12.3
D 162 39.6
E 572 59.3

9. How much 11.9°Brix cutback juice would be needed to blend with 267 gallons of
60.0 o Brix juice and 472 gallons of 64.8°Brix juice in order to make FeOJ at
41.8°Brix?
10. Suppose you want to make a concentrate with a Brix value of 41.9°Brix using 8
drums of 59.7°Brix concentrate A, 6 drums of 64.6°Brix concentrate B, and cut-
back juice at 13.3°Brix. How many gallons of cutback juice do you need? Suppose
that concentrate A is at 19 ° F, concentrate B is at 3 ° F, and the cutback juice is at
34°F. How many gallons of cutback juice do you now need in order to make the
same FCOJ at 15°F? (52 gal/drum, °C = (OF - 32)5/9)

REFERENCES

Balling, C. J. N. Gahrungschenie, 1, pt. 1, 119.


Brix, A. 1854. Z. Ver. deuf. Zucker-1nd., 4, 304.
Charlottenberg. 1900. Physikalisch-technische reichsanstalt, Wiss. Abhandl. Kaiserliche Normal-
Eichungs-Kommission,2, 140.
Chen, C. S. 1983. Accurate compilation of Brix, apparent specific gravity, apparent density, weight,
and pounds solids of sucrose solutions, Proc. Fla. State Hort. Soc., 96, 313.
Domke. 1912. Z. Ver. deuf. Zucker-Ind., 62, 302.
1967-1968. Weast, R. c., editor, Handbook of Chemisfry and Physics, 48th edition, Chemical
Rubber Co., Cleveland, OH, p. E-159, 1937.
1. Intern. Sugar, 39, 24s.
Kimball, D. A. 1986. Volumetric variations in sucrose solutions and equations that can be used to
replace specific gravity tables, J. Food Sci., 5/,529.
Shaw, P. E., Buslig, B. S., and Wilson, C. W. 1983. Total citrate content of orange and grapefruit
juices, J. Agric. Food Chern., 31,182.
Chapter 3

Acids in Citrus Juices

Acids playa vital role in the quality of citrus juices, second only to the Brix in
importance. They give the characteristic tartness or sourness of citrus products
and have been acclaimed for their effectiveness as thirst quenchers. These acids
and their salts replace many of the acids and salts lost by the body through
vigorous exercise.
Acids in citrus fruits are formed from the energy-releasing citric acid cycle
common to all life forms. This respiratory process, also known as the Krebs
cycle or tricarboxylic acid cycle, breaks down stored carbohydrates to carbon
dioxide and various organic acids, as shown in Fig. 3-1. This energy-generating
process occurs in the mitochondria of the juice cell, as shown in Fig. 3-2. The
juice cell is elongated and, when fitted together with other juice cells, forms
juice vesicles that are visible in the fruit and can be manually separated from
each other. Juice vesicles are organized into citrus sections in the fruit. As the
juice cell grows, carbohydrate-laden fluid from the sap of the tree flows into
the fruit and into the juice cell. Cell vacuoles, which have the function of stor-
ing food for the cell, absorb the aqueous carbohydrate fluid. As the fruit ma-
tures, the vacuoles grow so that they dominate the cell volume. The fluid in the
vacuoles becomes the juice of the citrus fruit. As this accumulation is taking
place, the mitochondria, the organelles next door to the vacuoles, are generating
acids in the citric acid cycle. Carbohydrates are broken down into pyruvic acid
in the membrane of the mitochondria. Once inside the mitochondria, the py-
ruvic acid enters into the citric acid cycle, generating the various acids.
As can be seen in Fig. 3-1, citric acid is the first acid formed in the cycle.
Even though much of the way that citric acid gets into the vacuole is not under-
stood, one of the most logical explanations appears to be that as soon as the
citric acid is manufactured inside the mitochondria, it migrates through the
membranes of the organelles into the juice vacuole before it can proceed with
the rest of the citric acid cycle. There is evidence that mitochondria are very
active throughout the lifetime of the fruit, indicating that not all of the citric
acid escapes the mitochondria, but some proceeds in the cycle to provide energy

34

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
ACIDS IN CITRUS JUICES 35

Pyruvate

CoA--~~
~_~
L • CO 2
NAOH. Acetyl-CoA (2C)
~COA
NAOH 70xalacetiC~

,
Acid (4C) Ci~ Acid (6C)

Aconitic Acid (6C)

Isocitric Acid (6C}


Malic Acid (4C)
I
Fumaric Acid (4C)

FAO:
~;n;c Add (4C) NAOH

otA

G~ptI J~cinYI-COA (4C)


GOP+Pi

Fig. 3-1. Krebs or citric acid cycle that occurs in the mitochondria of the juice cell. Acids pro-
duced give citrus a characteristic tart flavor.

for fruit growth and maturation. Some observers have suggested that the aco-
nitase enzyme that converts citric acid to aconitic acid may be dormant in the
early stages of fruit maturity. It is postulated that this inactivity results in the
early accumulation of citric acid in the fruit. As the fruit matures, and the aco-
nitase enzyme becomes more active, the citric acid continues in the cycle, pro-
viding much-needed energy for fruit growth resulting in a slowing or end to
citric acid accumulation in the juice cell vacuole. However, carbohydrates and
water continue to accumulate in the vacuole, causing a dilution of acid concen-
tration that gives a characteristic decrease of acid or tartness with fruit maturity.
The biological function of citric acid accumulation in citrus fruit is not only
interesting to contemplate, but it may have a direct bearing on the prediction
and understanding of citrus juice quality. There are two processes that govern
citrus growth or the growth of any plant: photosynthesis, which generates car-
bohydrates from sunlight, and respiration in the mitochondria, as already men-
tioned. The first process forms the fuel, and the second bums it. The rates of
these two processes, however, are not the same. At cooler temperatures, pho-
36 CITRUS JUICE CHARACTERISTICS

_ _ _ veSiCles in Citrus
fruit sections

Juice Cell

Juice Cells

Mitochondria
+-i-t--- Vacuole containing juice

Other organelle
+1--- Cell membrane

Fig. 3-2. Juice cell anatomy and location within the fruit. Juice accumulates in the vacuole and
occupies the majority of the volume of the mature cell.

tosynthesis is more rapid than respiration, generating an excess of carbohy-


drates. At higher temperatures, respiration is more rapid than photosynthesis,
resulting in a consumption of carbohydrate reserves, as illustrated in Fig. 3-3.
The point where these two rates intersect and are equal is called the compen-
sation point.
The compensation point temperature varies from fruit to fruit as well as with
growing conditions. However, when this temperature is exceeded, it has been
suggested that the fruit will draw on not only the carbohydrate reserve but the
citric acid reserve found in the juice cell vacuoles, causing a drop in citric acid
levels. This sudden drop of acid level is common with Valencia oranges in
California during the heat of the summer when the fruit is being harvested,
which seems to suggest that the compensation point for Valencia oranges in
California is in the neighborhood of lOO°F. Washington navels, which are har-
vested during winter months, never exhibit the same sharp drop in acid levels,
ACIDS IN CITRUS JUICES 37

Rate of Photosynthesis
...o ~
iu
:::s
'0
~
D..
>-
~
II)
c Rate of Respiration
W

Temperature - .
Fig. 3-3. Temperatures above the compensation point, where respiration exceeds photosynthesis,
cause a high demand for citric acid, which is obtained from juice cell vacuoles. This causes a
sudden drop in juice acidity.

but follow a smooth change in acid concentration characteristic of the dilution


effect mentioned previously. Figures 3-4 and 3-5 illustrate seasonal changes in
acid levels for California Washington navels and Valencia oranges where these
trends can be observed.

1.4
NAVEL
1977·78 •
1978.79 0
1.2 1979.80 x
1980.81 6
1981.82 a
1982·83 •
"0 1.0 1983·84 •
()
<i
~
0

0.8

0.6
10 12 14 16 18 20 22 24
Accumulated Temperatures from July 1st x10·3
Fig. 3-4. Changes in % acid with accumulated average temperatures from July I just after bloom
for navel orange juice. Smooth curves suggest a dilution effect in acid levels as the fruit matures
(Kimball (984). (Reprint from the Proceedings o/the Florida State Horticultural Society.)
38 CITRUS JUICE CHARACTERISTICS

1.2
VALENCIA

1.1

1.0
"0
Q
«
~
0
0.9

0
•1977-78
1978-79 o 1981-82
0.8 x 1979-80 • 1982-83
6 1980-81 • 1983-84

0.7 ~ _ _---'_ _ _---L_ _ _--'-_ _ _- I -_ _ _- ' -_ _- - - I


18 20 22 24 26 28 30
Accumulated Temperatures from July 1st x10' 3
Fig. 3-5. Changes in % acid with accumulated average temperatures from July just after bloom
for Valencia orange juice. Sudden drops in acid levels suggest temperatures exceeding the com-
pensation point (Kimball 1984). (Reprint from the Proceedings of the Florida State Horticultural
Society.)

ACID MEASUREMENTS

As mentioned in the preceding chapter, organic acids comprise a significant


portion of the soluble solids in citrus juices. The primary acid found in these
juices is the triprotic citric acid or tricarboxylic acid. Malic acid also is present,
comprising about 10% of the total acid content. Unlike citric acid, malic acid
levels remain fairly constant in the juice throughout fruit maturation. Also, as
mentioned in Chapter 2, potassium and sodium salts of citric acid comprise
about 20% of the total acid salt composition. These salts help buffer the acid,
thus preventing sudden changes in pH during a harvesting season. These salts
generally are ignored by the citrus industry, as are the differences between citric
and malic acids. A single acid titration generally is performed, and the results
are calculated as if all the acid were undissociated citric acid. In reality, all the
acid is not citric. Because of the presence of the salts, the real structure of the
citric acid in solution may be more that of a partially dissociated form, such as
dihydrogen citric acid.
ACIDS IN CITRUS JUICES 39

There are two basic ways that the acidity can be measured. Methods that
determine the pH measure only the free hydrogen ions in the solution. Acid
titrations with sodium hydroxide (NaOH) standards measure the total amount
of acid hydrogen, whether free or undissociated. The flavor of citrus juices
would be more closely associated with pH measurements because it is the free
hydrogen ions that interact with the taste receptors on the tongue. However,
maturity tests and Brix corrections preferably are determined by means of acid
titrations, which better reflect the actual citric acid present-the reason being
that pH values change very little in the acid range citrus juices and are difficult
to quantify or relate to taste and maturity differences. Acid titration, the method
used by the industry, provides a more stable and detailed scale for such mea-
surements, although the results of pH and acid titrations are of course related.
Most organic acids are weak acids that change pH when titrated with a strong
base, as illustrated in Fig. 3-6. The dashed curve represents the titration of a
pure aqueous citrus acid solution identical in amount and concentration to its
juice counterpart, which is illustrated with a solid line. The buffering action of
the weak acid can be seen by the small change of pH during the early stages of
the titrations. As the number of equivalents of base added approaches the num-
ber of equivalents of acid in the sample, or when neutralization occurs, a sharp
inflection point emerges that signals the endpoint of the titration. Because citric

12
5.9449 of CA soln made
from 3.8089 CA-H 2 0 ",. _ - - ------
in 1 00 mls water "
(3.46% aCid)-+,'
10 - I
I

.......................
8.2 I
5.9449 of 59.6 Brix,
II' 17.1 B/A ratio
8
Valencia Conc.
I
a. (3.48% acid)
6

differential analysis
4 +-- of endpoint

o
o 5 10 15 20 25 30 35 40

mls O.1562N NaOH titrated


Fig. 3-6. Titration curves for Valencia concentrate and a pure citric acid solution of the same
weight and concentration, illustrating the proper pH endpoint in acid titration of citrus juices.
40 CITRUS JUICE CHARACTERISTICS

acid is a triprotic acid, three separate inflection points would be expected, one
for each hydrogen as it comes off the molecule. However, the equilibrium con-
stants for these three dissociations are all within an order of magnitude; so a
single inflection point is observed, as seen in the figure. The equilibrium con-
stants for both of the dissociations of the diprotic malic acid are also close to
those of citric acid. Thus, malic acid becomes indistinguishable from citric acid
in these acid titrations.
There has been some controversy about what pH should be taken as an end-
point for an acid titration. The Association of Official Analytical Chemists sug-
gests a pH endpoint of 8.1 (AOAC 1980). The inflection point is somewhat
broad and slightly skewed, so that slight variations in what is taken as the end-
point can cause a significant error in the acid detennination. However, as shown
in Fig. 3-6, the pure citric acid solution gave a standard unifonn inflection point
that intersected the juice titration curve at a pH of 8.2. This value is used by
the USDA in detennining grade standards for citrus juices and concentrates,
and its use was supported by Sinclair and Bartholomew (1945). Accordingly,
this pH endpoint should be and generally is used in citrus juice acid detenni-
nations. Phenolphthalein indicator endpoints generally occur in this pH range
and can be used if a pH meter is not available.
Even though the concentration of the sodium hydroxide used in the titration
does not affect the final results, it does affect the way that the results are cal-
culated. The Association of Official Analytical Chemists (AOAC) recommends
a concentration of O.lN (N = nonnality = number of moles of H+ or OH-
ions per liter of solution) (AOAC 1980). The fresh fruit industry uses 0.1562N
NaOH because all one must do is divide the milliliters titrated by the weight of
the sample in order to obtain the % acid as citric acid. Another popular con-
centration is twice 0.1562N or 0.3125N NaOH, which is convenient in titrating
high acid juices such as lemon or lime and is used in Florida for orange juice
as well. The method used in Florida involves multiplying the nonnality (0.3125)
by a factor of 0.064, followed by mUltiplying by 100% and dividing by the
volume of the sample. The result is a w Iv percentage of acid as citric acid.
The full calculation is:

(0.3125N) ( 1 mole CA ) (192.12 g CA) ( 1 liter) ( 100% )


3 moles OH- mole 1000 ml ? ml sample
or:
(O.3125)(0.064)(loo%)/(ml sample) = w/v % citric acid

Such a w I v % cannot be used to calculate the Brix I acid ratio, however. This
value must be divided by the juice density to get the w Iw % citric acid needed
to calculate the Brix I acid ratio. The density of single-strength juice remains
ACIDS IN CITRUS JUICES 41

essentially unchanged between 11.00Brix and 13.0 o Brix at 1.04 to 1.05 gj ml,
and the w jv % can be divided by 1.04 to get the w Iw % citric acid. When
one is using the California method to determine the acid in a large number of
single-strength juice samples using a 10 ml pipette, the standard weight of 10.4
or 10.5 grams of sample can be used in calculating the acid level. If the NaOH
solution is at a concentration other than the convenient 0.1562N, the following
equations can be used to calculate the % acid:

. (Normality used) (ml titrated)


% aCldbased on sample weight = (0.1562N) (grams of sample) (3-1)

(Normality used) (ml titrated)


% acidbased on sample volume = (0.1562N) (1.04 g/ml) (ml sample) (3-2)

In routine quality control operations, large amounts of NaOH solution are


consumed, as they are during the beginning of the harvest season when fruit
maturation tests are performed. The following procedure can be used to make
a 50-gallon lot of 0.1562N NaOH solution. The procedure involves the use of
one-gallon distilled water containers that not only provide the water, but also
the containers for repackaging the NaOH solution after it is made. These one-
gallon containers of NaOH solution can then be sold to growers or packing
houses for maturation tests, in addition to being used by the processing plant.
These commercial solutions generally need to be certified by the regulatory
agency when it certifies fruit maturation tests, or when fruit is mature enough
to harvest. In Florida, maturity tests are performed by a regulatory agency, and
twice the amount of sodium hydroxide can be used to provide 0.3125N solu-
tions.

Preparation of NaOH Solution

Equipment and Supplies

• 50-gallon container with drain spigot at bottom.


• NaOH pellets (about 1200 g).
• 50 to 55 one-gallon containers of distilled water.
• 50 labels identifying the lot, including date and other information required
by local regulatory agencies as well as the customers.
• High-speed agitator for the 50-gallon container.
• 50-ml buret and stand.
• Phenolphthalein indicator ( 1 % in 1 : 1 methanol and water) or pH meter.
• Balance to weigh 1200 g of NaOH pellets.
• 25 ml volumetric pipette.
42 CITRUS JUICE CHARACTERISTICS

• 150 ml beaker or flask.


• About 1 g benzoic acid in 50 ml of ethanol or 25 ml of standard 0.1562N
HCI solution. (Acids other than benzoic acid can be used if the proper
equivalent weight is used in the caculations in the procedure.)
• 50 snap-on plastic caps that can be used to reseal one-gallon plastic con-
tainers.
• Magnetic stirrer and stirring bar (optional).

Procedure

1. Clean and dry the 50-gallon container. Empty the 50 one-gallon con-
tainers of distilled water into the 50-gallon container, discarding the used
caps.
2. Add about 1180 g of the NaOH pellets to the water and agitate until the
pellets are completely dissolved. This amount of NaOH should actually
produce a concentration of about 0.1590N. However, the excess NaOH
is needed to compensate for atmospheric carbon dioxide neutralization
during agitation.
3. Weigh between 0.4 and 0.5 g of benzoic acid into a beaker and record
the exact weight, or pipette 25 ml of the standard 0.1562N HCI solution
into the beaker. If an acid other than benzoic acid is used, the 121.13
g/mole molecular weight for benzoic acid should be replaced by the
molecular weight of the acid used, divided by the number of acid hydro-
gens per molecule of acid.
4. If benzoic acid is used, add about 50 ms of ethanol to solubilize the acid.
5. Rinse the buret with the NaOH solution from the tank, discard the rinse,
fill the buret with the NaOH solution, and zero the buret or adjust the
level to 0 ml.
6. Add 5 drops of the phenolphthalein indicator to the acid in the beaker
and/or rinse the electrode from the pH meter, carefully dry the electrode,
and insert it carefully into the acid solution so that the solution level is
above the reference wire in the electrode. These electrodes should be
kept in solution at all times when not in use, and the pH meter should
be calibrated from time to time according to the manufacturer's instruc-
tions.
7. Titrate the acid solution with the NaOH solution while stirring or swirl-
ing it until a persistent pink color of the indicator is observed, or to a
pH of 8.2 if using a pH meter.
8. Using Fig. 3-7, determine the milliliters of titrant from the buret, and
calculate the normality as follows: The Agricultural Commissioner's Of-
fice in California uses standard 0.1562N HCI to standardize the basic
solution and allows a deviation of ±0.1O ml from the exact 25.00 ml of
ACIDS IN CITRUS JUICES 43

24.1 mls -exactly 24.10 mls


24.2 mls

24.1 mls -add 0.02 mls to 24.1


24.2 mls to get 24.12 mls

24.1 mls -add 0.04 mls to 24.1


24.2 mls to get 24.14 mls

24.1 mls -add 0.06 to 24.1 mls


24.2 mls to get 24.16 mls

24.1 mls -add 0.08 to 24.1 mls


24.2 mls to get 24.18 mls

Fig. 3-7. How to read a buret properly: Place a white card with an even heavy black line behind
the buret and about,'o inch below the meniscus. The dark line of the meniscus then can be compared
to the figure.

the NaOH solution needed in the titration in order to obtain exactly


O.1562N NaOH to certify the solution. This corresponds to an error of
about ±0.01 % acid when titrating juice.

. (gramsacid)( 1 mole /122.13 g)( 103 ml/liter)


NormalIty = (3-3)
(ml titrated)
or (using HCI solution):
Normality = (0.1562N) (25 ml HCI/ml NaOH titrated) (3-4 )
For example:

(0.477 g benzoic acid) (8.188)/25.00 ml = 0.1562N NaOH


44 CITRUS JUICE CHARACTERISTICS

or:

(0. 1562N) (25.00 ml HCI/24.65 ml NaOH) = 0.1584N NaOH

9. If the normality is too high, use the following to determine the amount
of water to add where N is the high normality:

ml water = (50 gal) (3785 ml/gal) (N - 0.1562)/0.1562 (3-5)

For example:

(50) (3785) (0.1584 - 0.1562)/0.1562 = 2665 ml water

10. If the normality is too low, use the following to determine the grams of
NaOH pellets needed to add to the solution where N is the low normality:

g Na OH = (50 gal) (3.785 l/gal) (40 gNaoH/mole) (0.1562 - N)


(3-6 )
For example:

(50) (3.785)( 40)(0.1562 - 0.1544) = 13.626 g NaOH

12. With the solution at the proper concentration, using the spigot at the
bottom of the 50-gallon container, refill the one-gallon containers, snap
on new sealing lids, and apply a label to each container according to the
instructions of the inspector.

Handling NaOH Solutions


Sodium hydroxide solutions are very susceptible to two forms of contamination
from the air. One is the absorption of moisture, and the other is the absorption
of carbon dioxide. Carbon dioxide comprises about 1 to 2 % of the atmosphere
at sea level, and when dissolved in aqueous solutions undergoes the following
reaction:

(3-7)

The carbonic acid then will proceed to neutralize the NaOH solution, changing
the concentration. For this reason it is important to isolate NaOH solutions from
the atmosphere. When one is using one-gallon containers, excessive opening
and closing of the container as well as excessive agitation in the presence of air
will result in a decrease in the NaOH normality. Syphon dispensing systems
ACIDS IN CITRUS JUICES 45

thus are recommended, as shown in Fig. 3-8. As air is drawn into the NaOH
reservoir during dispensing, it passes through ascarite CO 2 absorbent and Drier-
ite moisture absorbent. Ascarite turns white upon saturation, and Drierite turns
from blue to rose red and should be changed when needed.
Both manual titration and automated titration are used in citrus processing.
The advantages of auto-titration, which uses a motor-driven buret that stops at
a preset pH, include faster analyses and the need for less effort by lab techni-
cians. Manual titrations, as depicted in Fig. 3-8, are nearly as rapid as auto-

~ thistle tube with desiccant

~ thistle tube with ascarite


carbon dioxide absorbent
'"<l1li1--- two hole stopper

4---1- bent glass tubing

+---11- NaOH solution


1+-- 5-gallon reservoir

+- latex tubing

auto zero 50 ml buret

..,.,.....- - buret refill clamp

................... pH meter
~ pH electrode
pH reference wire
waste
."--150-200 ml beaker containing
and acid or juice sample
~06 stirring bar
~ magnetic stirer

Fig. 3-8. Setup for titratable acid detennination.


46 CITRUS JUICE CHARACTERISTICS

mated methods and cost much less. Either method is suitable for industrial pur-
poses. The following titration procedure assumes a manual titration.

Acid Titration

Equipment and Supplies

• Setup shown in Fig. 3-8.


• 0.1562N NaOH.
• Phenolphthalein indicator (1 % in 1: 1 methanol and water) or pH meter.
• Lab balance for concentrate or 10 ml pipette for single-strength juice.

Procedure

1. Pipette 10 ml of single-strength juice or weight 5 to 10 g of concentrate


into a 200 ml beaker. Record the exact weight of the concentrate.
2. Add 5 drops of phenolphthalein indicator, or insert a clean dry pH elec-
trode into the solution so that the reference wire is in contact with the
solution.
3. Insert a magnetic stirring bar, and place the beaker on the magnetic stirrer,
or, if a magnetic stirrer is not available, use a 200 ml Erlenmeyer flask
and swirl it during titration.
4. Fill the buret with the 0.1562N NaOH solution (0.3125N for lemons or
limes) by opening the clamp at the base of the buret as shown in Fig. 3-8
until the buret is automatically zeroed.
5. Titrate with the NaOH solution until a slight darkening of the juice per-
sists. The combination of the orange color of the juice and the pink color
of the indicator is brown. If a pH meter is used, titrate to a pH of 8.20.
6. Read the buret to the nearest 0.02 ml as shown in Fig. 3-7 and calculate
the % acid as citric acid using one of the following equations:
• Single-strength juice:

% acid = (ml titrated) / 10.4 g (3-8)

• Orange, tangerine, or grapefruit concentrate:

% acid = (mltitrated) / ( gconc,) (3-9)

• Lemon or lime concentrate:

% acid = (mltitrated)( 0.3125N) / ((gconc,) (0.1562N)) (3-10)


ACIDS IN CITRUS JUICES 47

The USDA grade standards for acid content are generally incorporated in the
Brix/acid ratios, discussed in Chapter 4. Only canned orange juice (47FR 12/
10/82,52.1557) and lemon juice products have acid standards (CFR, Title 21,
146.114, 146.120, 146.121.). In California and Arizona sweetened or unsweet-
ened canned orange juice must have an acid level of 0.70 to 1.40 % acid for
Grade A, and 0.60 to 1.40% acid for Grade A in other areas. Grade B sweet-
ened canned orange juice requires 0.60 to 1.60% acid in any location, and
unsweetened canned orange juice requires 0.55 to 1.55 % acid for the same
grade. Lemon juice requires at least 0.70 % acid in reconstituted lemonade for-
mulations in order to meet the Standards of Identity for Frozen Concentrate for
Lemonade and Frozen Concentrate for Artificially Sweetened Lemonade. The
Standards of Identity for Lemon Juice require at least 4.5 % acid.

PROCESSING LEMON OR LIME JUICES

Concentrating Lemon (or lime) Juice

Because lemon and lime juices contain a higher percentage of organic acids by
weight than carbohydrates, lemon and lime juice concentrations are determined
as the weight of acid as anhydrous citric acid (ACA) per unit volume of juice-
grams ACA/liter or GPL (grams per liter). Instead of the sucrose equivalent
weight of soluble solids being the standard for inventories and marketing, the
weight of acid is the standard unit of measure. Even so, Brix measurements are
necessary in order to obtain densities in quality control calculations and in the
making of concentrates, as in-line refractometers are convenient to use. There
is no accurate in-line citric acid detector available for lemon evaporators, and
there are no accurate density scales available based on citric acid. Also, there
are few evaporators dedicated solely to lemon processing. The use of refrac-
tometers and the Brix scale makes it possible to process other types of citrus
fruit. The lemon or lime GPL values can be calculated from Brix data and acid
measurements.
Most lemon concentrates are evaporated to 400 or 500 ± 5 GPL. To accom-
plish this, the uncorrected observed Brix that is desired must be determined so
that the evaporator operator will know at what Brix level to operate the evap-
orator. Hence, the acid and the temperature-corrected Brix of the inbound sin-
gle-strength lemon juice must be known along with the % acid. First, the SPGj
of the single-strength juice must be found from the Brix by using Equation 2-8
(or 2-10) and the density d from Equation 2-7. The following equation then can
be used to calculate the SPGc of the final desired lemon concentrate:

SPGc = (GPLdesired)(lliter/1000 ml)(l00%)(SPGj )/Ad (3-11)


48 CITRUS JUICE CHARACTERISTICS

or:

SPGc = (GPL)( SPGJ / lOAd (3-12 )

where A is the % acid of the single-strength lemon juice. The Brix correspond-
ing to SPGc can be found by using Equation 2-17 or equivalent density tables.
This is the acid-corrected Brix, Be- Because the evaporator operator needs to
know the uncorrected observable Brix, B o ' the acid correction for this Brix must
be determined and subtracted from Bc. This can be done by finding the density,
d c from Be by using Equation 2-7, which enables the calculation of the final
acid concentration, A c ' according to:

Ac = (GPLdesired)(lliter/lOoo ml)(1oo%)/de (3-13 )

or:

(3-14 )

Next, by using Equation 2-2 or Appendix A, the acid correction to Bc according


to Ae can be determined and subtracted from Bc to give the needed uncorrected
Brix. If the temperature of the concentrate can be determined, the temperature
correction to the Brix also can be subtracted from Be by using Equation 2-1 or
Table 2-4.
For example, if we wanted to concentrate 9.7°Brix single-strength lemon
juice with 5.37% acidity to 400 GPL, using Equation 3-12, we would get:

spec = (400 GPL) (0.838 sPG @9.rBrix) = 6.0261b sol/gal


10(5.37% acid)( 1.0359 g/[email protected])

which gives 57.0 oBrix by using Equation 2-17. If we use Equation 2-7,
57.0 oBrix corresponds to a density of 1.2680 g/ml, which in tum is used in
Equation 3-14 to give:

Ae = (400 GPL)/(10(1.2680 g/ml)) = 31.55% acid

Using this value in Equation 2-2 or Appendix A gives an acid correction to the
Brix of 5. rBrix. The corrected Brix (57 .0oBrix) minus the correction
(5.7°Brix) is 51.3°Brix, which the evaporator operator should adjust the evap-
orator to produce according to an in-line refractometer. If the temperature of
the concentrate is determined to be 28°C, the temperature correction to the Brix
ofO.64°Brix also should be subtracted from the 51.3°Brix, to give 50.7°Brix,
which should be run on the evaporator according to Equation 2-1 or Table 2-4.
ACIDS IN CITRUS JUICES 49

As with the other quality control calculations discussed thus far, the above
calculation lends itself to computer application. A flow chart outlining the steps
in such a program is shown in Fig. 3-9. A suggested GWBASIC program using
Fig. 3-9 can be found in Appendix B. A similar program, which can be used
with an HP-41C programmable hand-held calculator, can be found in Appendix
C.

SS Juice Srix (Bj)


SS Juice aeid (Aj) B = Sf
Desired GPL
Cone. Temp. °C (T)

no

EO 3-14

Aeor

EO 2-1
EO 3-12
SPGe
Teor

Bo = B - Aear - Tear
Bf = 10 X SPGe

Fig. 3-9. Flow chart that can be used to program computers to calculate the uncorrected Brix
needed from an evaporator when processing lemon concentrate.
50 CITRUS JUICE CHARACTERISTICS

Determining the Concentration of Lemon (or lime) Concentrate

The actual concentration of lemon or lime concentrates can be determined by


using the following equation:

GPL = Ad( 1000 ml/liter)/loo% = lOAd (3-15 )

where A is the % acid, and d is the density calculated from the corrected Brix
by using Equation 2-7. For example, if we were to make a 56.2°Brix lemon
concentrate with an acid content of 31.50%, Equation 3-15 would become:

(10) (31.50% acid) (1.2634 g/[email protected]) = 398 GPL

which is within the standard 400 ± 5 GPL specification. Figure 3-10 shows a
flow chart that can be used to write a computer program for such a calculation,
such as the sample GWBASIC program found in Appendix B. A similar pro-
gram that can be used with a hand-held HP-41 C programmable calculator can
be found in Appendix C.
Since GPL and SPG are similar parameters, the blend equations (2-12 through
2-16) for other citrus juices can be used for lemon juice blending simply by
replacing all SPG values with GPL values. For example, suppose we want to
dilute 1000 gallons of 420 GPL concentrate to 400 GPL. The water needed can
be calculated from Equation 2-12:

If we have a full l000-gallon tank of 380 GPL concentrate, and we want to


raise the concentration to 400 GPL using 500 GPL concentrate, Equation 2-13
can be used:

VH = (1000 gal) (400 GPL - 380GPd/(5OO GPL - 380 GPL )


= 167 gal 500 GPL conc.

Thus 167 gallons of the 500 GPL concentrate would be needed to replace 167
gallons of the 380 GPL concentrate in order to bring the concentration up to the
needed 400 GPL.
Similarly, if we have a full l000-gallon tank of 418 GPL lemon concentrate
and want to dilute it to 400 GPL, using Equation 2-14 we obtain:

Vw = (1000 gal) (418 GPL - 4ooGPL)/(418GPd = 43 gal


ACIDS IN CITRUS JUICES 51

Brix (B)
% Acid (A)

EQ3-15
GPL

Fig. 3-10. Flow chart that can be used to program computers


to calculate the GPL of lemon concentrates.

This is the amount of the 418 GPL concentrate that would have to be replaced
with water to get 1000 gallons of exactly 400 GPL lemon concentrate.
In blending several lemon concentrates, the final average GPLj can be cal-
culated as follows, using the data given in the tabulation and Equation 2-16:

Lot # # of Drums GPL


9 398
2 4 409
3 3 500
4 16 404
5 5 395

GPLj = (9(398) + 4(409) + 3(500) + 16(404) + 5(395))/


(9 + 4 + 3 + 16 + 5) = 410 GPL
52 CITRUS JUICE CHARACTERISTICS

REDUCED ACID JUICES

A recent advance of citrus processing is the use of weak anionic exchange resins
to remove organic acids from citrus juices (Varsel 1980). This technique is
advantageous in situations where blending may not be so practical in reducing
acid levels. However, the use of ion exchange may be permitted only for juices
that allow such in the standards of identity, such as Reduced Acid Orange Juice.
Nineteen different types of ion exchange resins have been approved by the Food
and Drug Administration (FDA) to date for use in food processing (CFR, Title
21, 173.5-173.25.), and many more are expected to emerge. Weakly basic
resins favor the removal of stronger organic acids, such as citric acid, which is
important in citrus processing where retention of the weaker nutritional ascorbic
and folic acids is preferred. The presence of larger amounts of citric acid also
favors its removal during ion exchange. The reaction that takes place during
this process is:

(3-16)

The positive unit of the resin (R +) exchanges its hydroxide ion to neutralize
the juice acidity. Overall, citrate is removed, and water is formed. As the resin
becomes saturated with citrate, the resin efficiency declines, and regeneration
with a basic solution is required.
Two types of columns containing these resins have been considered. An up-
flow fluidized bed approach has the advantages of treating juices with normal
pulp levels and of enhancing efficiency by more vigorous and thorough contact
between the juice and the resin. The main disadvantage is the difficulty in mak-
ing resins of sufficient particle size or density that they will not be carried out
with the juice. A down-flow packed column approach has the advantage of
increased surface availability of the smaller resin, which enhances contact ef-
ficiency as well as the efficiency of regeneration. The main disadvantage is that
the juice needed to have the pulp removed to a level of at least 2 % or less in
order to avoid plugging the column. The high cost of depulping centrifuges or
UF membranes adds to the capital costs. Backwashing the column to remove
entrapped pulp may determine how often regeneration needs to be done, rather
than saturation of the resin with citrates. Overall, the down-flow process has
proved to be the preferred industrial technique. The larger the particle size is,
the less the depulping required. Insoluble solids removed in depulping can be
restored after column treatment to replenish the original character of the juice.
As explained in Chapter 15, the acids in citrus juices serve to guard against
pathogenic organisms that flourish in less acid foods. For this reason, care should
be taken in manufacturing reduced acid juices so that the pH does not remain
above 4.6 for any length of time. Timely blending of reduced acid juices with
ACIDS IN CITRUS JUICES 53

other juices is a convenient way to achieve this. The standards of identity spec-
ify that reduced acid concentrate must have a Brix/acid ratio of 21-26 (CFR,
Title 21,146.148.).
Ion exchange and its cousin, adsorption techniques, are being used to remove
bitter principles in citrus juice, and often are used in conjunction with acid
removal. A single resin can be used for both. If only debittering is desired,
saturation of the resin with commercial acids as a last step in regeneration will
prevent significant citric acid loss during resin treatment.

QUESTIONS

1. What contributions do acids make to the overall quality of citrus juices?


2. Where exactly is citric acid manufactured in citrus fruit?
3. Why does citric acid accumulate in fruit, and how and why does it change
as the fruit matures?
4. Why are pH measurements not used to measure the acid content of citrus
juices?
5. What two compounds are found in the air that can affect the concentra-
tion of NaOH solutions, and how do they?
6. In measuring the citric acid levels in lemon juices, why are solutions of
NaOH used that have a higher normality?
7. Are Brix measurements necessary for lemon juices, since concentrations,
inventories, and marketing are based on the amount of acid only?
8. What is the standard GPL error range?
9. What are the standard GPL values for lemon or lime concentrates?
10. What is the difference between SPG values and GPL values when it
comes to blend calculations?

PROBLEMS

1. What would be the % acid of a lemon concentrate sample weighing 1.684 g using
10.62 ml of a 0.781ON NaOH solution?
2. In the standardization of a 5-gallon NaOH solution, the meniscus on the buret is flat
on the 25.00 ml mark with just the tip of the meniscus below the mark, and 25 ml
of a 0.1562N Hel solution was being titrated. How much NaOH or water must be
added to get exactly 0.1562N NaOH?
3. Exactly 28.12 ml of 0.3125N NaOH solution was used to titrate 10 ml of single-
strength lemon juice. What is the % acid?
4. A 9.462 g sample of orange concentrate was titrated with a 0.1562N NaOH solution
with the meniscus on the buret just touching the 45.60 mark. What is the % acid?
5. How much water do you need to add to a 20-gallon NaOH solution standardized with
0.436 g benzoic acid using 22.42 ml of NaOH solution in the titration?
54 CITRUS JUICE CHARACTERISTICS

6. What is the GPL of a lemon concentrate containing 32.46% acid with a Brix of 51.2?
7. At what Brix would the evaporator operator run the evaporator when concentrating
an 8.9°Brix single-strength lemon juice with an acid content of 4.98% in order to
get a 500 GPL concentrate at 18°C?
8. How many gallons of water do you need for 1216 gallons of 496 GPL lemon con-
centrate in order to make 400 GPL concentrate?
9. If you have a full 3264-gallon tank of 408 GPL lime concentrate and want to change
it to a full tank of 400 GPL lime concentrate, what do you do?
10. How many gallons of 398 GPL lime concentrate do you need to blend with the
following in order to get a final 500 GPL product? How many gallons do you have
total? (Hint: See Equation 2-18.)

LotH Gallons GPL


? 398
2 520 520
3 1344 494
4 672 512
5 365 540

REFERENCES

AOAC. 1980. Official Methods of Analysis, 13th edition, 22.061.


Kimball, D. A. 1984. Factors affecting the rate of maturation of citrus fruits, Proc. Fla. State Hort.
Soc., 97, 40.
Sinclair, W. B., and Bartholomew, E. T. 1945. Analysis of organic acids of orange juice, Plant
Physiol., 20, 3.
Varsel, C. 1980. Citrus juice processing. Citrus Nutrition and Quality, S. Nagy and 1. Attaway,
eds. ACS Symposium Series 143, Washington, D.C., 237.
Chapter 4

The Brixl Acid Ratio

The empirical Brix / acid ratio, found by dividing the acid-corrected and tem-
perature-corrected Brix by the % titratable acidity w / w as citric acid (B / A
ratio), is one of the most commonly used indicators of juice quality as well as
fruit maturity. In California, the fruit harvested for the fresh fruit markets needs
a B / A ratio of at least 8: 1 or 8, whereas the fruit harvested for juice in Florida
must have a B / A ratio of at least 10: 1 or 10. Even through fruit destined for
juice in Florida requires a B / A ratio of 10, commercial Florida juices must
have a B / A ratio of at least 13, which can be achieved through blending. Con-
sumers of citrus juices generally prefer a B / A ratio of 15 to 18, depending on
the product and individual tastes.
It is generally agreed that taste is a four-dimensional phenomenon consisting
of sweet, sour, salty, and bitter. Taste is sensed by receptors about 60 microns
in diameter, which are budlike structures having numerous microvilli about 2
microns long that project into the taste pores on the tongue. Taste is detected
by a disturbance of the electrical charges on the receptor due to contact with a
food substance. These receptors are very sensitive to abuse, and are replaced
every 12 to 17 days. The receptors respond to more than one taste, in various
combinations and intensities.
In citrus products, the sourness of the organic acids and the sweetness of the
sugars compete for the same receptor sites on the tongue. Thus the actual amount
of sugar or acid is of less importance in the taste of citrus products than the
ratio of the two; and this is why the B / A ratio (or simply just the ratio) is so
important as a flavor quality indicator in citrus juices. It also means that an
overabundance of acid sourness or sugar sweetness can be blended out by using
various combinations of the high- and low-ratio juices. This is done by using
the volume (Vn ), the pounds soluble solids/gallon (SPGn ) found from the Brix

55

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
56 CITRUS JUICE CHARACTERISTICS

and Equation 2-8 and the B / A ratio (Rn) for each component of the blend of n
components, in the following equation:

V)SPG) + V2 SPG2 + V3 SPG3 + ... + VnSPGn


R = ------~--~--~~~--~--~--------~~~~--
V)SPG)/R) + V2 SPG2 /R 2 + V3 SPG3 /R 3 + ... + VnSPGn/Rn
(4-1)

If the Brix values of all the components are essentially the same, the more
compact equation below can be used instead of Equation 4-1:

For example, if we wanted to calculate the final ratio of the following compo-
nents, Equation 4-1 would be used as shown below.

Lot # # Drums BIA Ratio Brix


12 13.0 65.3
2 9 16.7 60.3
3 18 12.3 62.4
4 6 21.8 59.6
5 4 18.9 60.3

12(7.178) + 9(6.477) + 18(6.768)


R = _:--_--:-_+_6-'('-6.,-.3_82~):..__+__:_4-'-(-6.-4-77.....!.)---_:__- = 143
12(7.178)/13.0 + 9(6.477)/16.7 + 18(6.768)/12.3 .
+ 6(6.382)/21.8 + 4(6.477)/18.9

Using equation 4-2, we obtain:

R = 12 + 9 + 18 + 6 + 4 = 144
12/13.0 + 9/16.7 + 18/12.3 + 6/21.8 + 4/18.9 .

Each equation gives a slightly different answer because the Brix values are
slightly different. The wider the range of Brix values, the greater the difference
will be in the results of the two equations. Figure 4-1 shows a flow chart that
can be used to program a computer to calcuate the average B / A ratio. Appendix
B contains a sample GWBASIC program that utilizes the flow chart in Fig. 4-1.
THE BRIX/ACID RATIO 57

Brix of Camp. n (Bn)


Ratio of Camp. n (Rn)
Vol. of Camp. n (Vn)

n
Z' = 2: Vi (SPGi)
i=1
n
Z" = 2: Vi (SPGi)/Ri
i=1

no

EO 4-1
R = Z'/Z"

Fig. 4-1. Flow chart that can be used to program a computer to calculate the average Brix/acid
ratio in a blend.
58 CITRUS JUICE CHARACTERISTICS

Suppose that you want to know how much of a certain component you will
need to in order to achieve a certain desired ratio. Equations 4-1 and 4-2 can
be rearranged to the following:

v = V2 SPG2 (I/R - I/R 2 ) + V3 SPG3 (I/R - I/R 3 ) + ... + V"SPG,,(I/R - I/R,,)


) SPG)(I/R) - l/R)

(4-3)

and:

(4-4)
For example, if we wanted to calculate how much of Lot #1 we would need to
achieve the 14.3 ratio calculated in the previous example, using Equation 4-5
and 4-6 we would obtain with R = 14.3:

9(6.477) (I/R - 1/16.7) + 18(6.768) (I/R - 1/12.3) + 6(6.382)


(I/R - 1/21.8) + 4(6.477)(I/R - 1/18.9)
7.178(1/13.0 - 1/14.3)

VI = 11 drums

or:

9(I/R - 1/16.7) + 18(I/R - 1/12.3)


+ 6(I/R - 21.8) + 4(I/R - 1/18.9)
1/13.0 - I/R
VI = 14 drums

Here, the two equations again give different answers because the latter equation
does not take into account the higher Brix of the first component and thus is
less accurate than the first equation. Also, 11 instead of the original 12 drums
were calculated because of rounding-off errors. Apparently 11 or 12 drums will
give us essentially the desired 14.3 overall B / A ratio. Figure 4-2 gives a flow
chart that can be used in programming the above calculations. A sample of a
GWBASIC program using this flow chart can be found in Appendix B.
In reviewing the last three chapters and the given examples of computer ap-
THE BRIX/ACID RATIO 59

Brix of Compo n (Bn)


Ratio of Compo n (Rn)
Vol. of Compo n (Vn)
(except V1)
Desired Ratio (R)

n
Z = L Vi (SPGi) ( -R 1. )
1 -R
i=2 I

no

EQ4-3
Z
V1 = - - - - - - -
(1/R1 - 1/R)SPG1
---~

Fig. 4-2. Flow chart that can be used to program a computer to calculate the volume needed of
one blend component to achieve a desired B / A ratio.
60 CITRUS JUICE CHARACTERISTICS

Uncorrected Brix (Bi)


Weight of Sample (W)
mls titrated (mls)
Normality of NaOH (N)
Centigrade Temp. (T)

B = Bi + Acor + Teor
BAR = BfA

Fig. 4-3. Flow chart that can be used to program a computer to calculate the B / A ratio from
laboratory data.
THE BRIX/ACID RATIO 61

Brix of Compo n (Bn)


BfA Ratio of n (Rn)
Vol. of Compo n (Vn)

Bf = 10 x SPG

B = Bf

n
Z =? Vi (SPGi)
1=1
n
Zr = 2: Vi (SPGi)fRi
i=1
n
V = 2: Vi
i=1 no

no

B = Bf = average
Brix
EQ 4-1
avg BfA ratio= Z/Zr

EQ 2-16
SPG =ZN

Fig. 4-4. Flow chart that can be used to program computers to calculate the average Brix and the
Brix/acid ratio of a blend simultaneously.
Table 4-1. USDA standards for Brix/acid ratios.
Grade A Grade B
Type of Juice unsw sw unsw sw

Orange Juice (47FR 12110/82, 52.1551-52.1557)


Pasteurized orange juice
Californial Arizona 11.5-18.0 12.5-20.5 10.5-23.0
Other areas 12.5-20.5 10.5-23.0
Concentrated OJ for
manufacturing 8.0-24.0 8.0-24.0
Orange juice from concentrate
Californial Arizona 11.5-18.0 12.5-20.5 11.0-23.0
Other areas 12.5-20.5 11.0-23.0
Reduced acid orange juice 21.0-26.0 21.0-26.0
Dehydrated orange juice 12.0-18.0 10.5-19.0
Frozen concentrated OJ
Californial Arizona 11.5-19.5 12.0-19.5 10.1 +
Other areas 12.5-19.5 13.0-19.5 10.1+
Canned orange juice
Less than II. 5 °Brix 10.5-20.5 9.5-20.5
Greater than
or equal to II. 5 °Brix 9.5-20.5 9.5-20.5
Canned concentrated OJ 11.5-20.0 12.0-20.0 9.5-20.0 10.0-20.0
Grapefruit (48FR 9112/83 52.1221-52.1230)
Grade A Grade B
Type of Juice unsw sw unsw sw
GO and GO from conc. 8.0-14.0 9.0-14.0 7.0+ 9.0+
Frozen concentrated GfJ 9.0-14.0 10.0-13.0 7.0-16.0 8.0-13.0
Conc. GO for
manufacturing 6.0+ 5.5+
Dehydrated grapefruit 8.0-14.0 9.0-14.0 7.0+ 9.0+
juice
Grapefruit and Orange Blend (6FR 1111172, 52.1281-52.1290)
Grade A Grade B
Type of Juice unsw sw unsw sw
Single strength
Less than 11.5 °Brix 9.5-18.0 8.0+ 10.5+
Greater than 11.5°Brix 8.5-18.0 10.5-18.0 8.0+ 10.5+
Reconstituted
Less than 11.5 °Brix 9.5-18.0 9.0+ 10.5+
Greater than 11.5°Brix 9.5-18.0 10.5-18.0 9.0+ 10.5+
Tangerine (2FR 7/1/69,52.2931-52.2941)
Grade A Grade B
Type of Juice unsw sw unsw sw
Concentrated TJ for 9.0-21.0
maunfacturing 9.0-18.0
Canned tangerine juice 10.5-19.0 11.5-19.0* 11.5*
*Ifthe Brix is above 16.0, theBIA ratio can be below 11.5.

62
THE BRIX/ACID RATIO 63

plications, one may notice that the programs can be consolidated and used to
calculate the Brix, % acid, B / A ratio, and water needed to adjust the Brix if
necessary. Figure 4-3 is a flow chart that can be used to construct such a pro-
gram along with the sample GWBASIC program found in Appendix B.
In blending, the average Brix and the B / A ratio can be calculated by com-
bining the flow charts of Fig. 2-8 and Fig. 4-1, to create the flow chart shown
in Fig. 4-4. This flow chart can be used to generate a program such as the one
found in Appendix Busing GWBASIC language. In this program, after adding
the data of the components, you merely need to press "enter" and the results
will appear. You also can add more data after a calculation is made. A similar
program for HP-41 C programmable calculators can be found in Appendix C.
Because the standard error for B / A ratios is ± O. I, these ratios should be
expressed or rounded off to the nearest tenth of a ratio point. Table 4-1 gives
the USDA B / A ratio grade standards for citrus products.
In the fresh fruit industry, once the fruit is mature enough for harvesting,
little attention is paid to the B / A ratio. However, juice processors are concerned
about the B / A ratio throughout the season. The rate of increase is linked to the
rate of changes in the Brix and acid levels in the fruit, and of these two param-
eters, the change in the acid levels generally has the greater effect on the B / A
ratio. Brix levels range from about 9 to 15, whereas acid levels may range from
0.5% to 1.5%, a threefold increase. Smooth acid changes, as depicted in the
last chapter for Washington navel oranges, have been shown to generate linear
relationships with heat accumulation, as shown in Fig. 4-5. These linear rela-
tionships have been empirically correlated with such parameters as crop size ( C
in tons / acre), tree growth or age (Y), maximum accumulated temperatures
between May and August just after bloom (M), and accumulated heat during
the growing season (H), according to the following equation:

R = H(0.0629Y - 0.03076C + 1.237)/1000 + 6.607M/l000 - 78.42


( 4-5)
Equation 4-5 gave a confidence level of 98% in a statistical t-test comparison
between calculated and measured B / A ratios for the seven seasons illustrated
in Fig. 4-5. Even though Equation 4-5 may not be accurate with citrus growth
in other geographical areas or under different conditions, it does illustrate some
of the main influences on the B / A ratio. Further research is needed in this area.

QUESTIONS

1. What are the minimum B / A ratios required for harvesting oranges in the
United States?
64 CITRUS JUICE CHARACTERISTICS

22

NAVEL
20

18

o
......
16
ca
a:
~
CD 14 1977·78 •
1978.79 0
1979·80 lC
1980·81 ~
1981.82 0
12 1982·83 &
1983·84 •

10
12 14 16 18 20 22

Accumulated Temperatures from July 1st x10· 3


Fig. 4-5. Correlation of heat versus B / A ratio development for navel oranges from fruit samples
from three California packing houses (Kimball 1984). (Reprint from the Proceedings of the Florida
State Horticultural Society.)

2. Which of the four dimensions of taste is affected by citrus juices?


3. What actually causes taste, and what type of compounds that are found in
citrus juices are most likely to create taste sensations?
4. Is it true that if you add enough sugar to the juice it will become sweet
regardless of how much acid is present?
5. What is the major factor that influences the development of the B / A ratio
throughout a growing season?
THE BRIX/ACID RATIO 65

PROBLEMS
Blend A Blend B
Lot # # Drums Brix BfA Ratio Lot # # Drums Brix BfA Ratio
1 4 60.1 14.6 1 16 66.4 10.2
2 10 59.5 21.6 2 3 58.7 14.6
3 7 60.0 18.7 3 11 62.8 19.1
4 24 60.4 13.9 4 8 60.5 16.3
5 9 59.9 15.1 5 5 64.0 9.9

1. What is the average B / A ratio of blend A, and which equation would be best to use?
2. What is the average B / A ratio of blend B, and which equation would be best to use?
3. How many drums of 59.8°Brix 20.4 B / A ratio are needed to bring up the ratio in
blend B to 14.0?
4. How many drums of 60.1 °Brix 22.3 B / A ratio juice are needed to bring up the B / A
ratio in blend A to 16.4?
5. Suppose that it is September and you want to know if navel oranges will be mature
enough for harvesting in California by November 1. You know that the summation
of the maximum summer temperatures from May through August gave 10,879 degree
days, that the estimated crop load is about 13.5 tons/acre, and the estimated sum-
mation of daily temperatures from July 1 up until November 1 is 10,702 degree days
for the upcoming season (Y = 10). Based on this infonnation and that found in the
chapter, is it likely that navel oranges will be mature enough to harvest by November
I?
Chapter 5

Testing of Fruit Samples

When fruit is brought into a processing facility, proper procedures must be


followed in order to fairly credit the owner of the fruit for that which is pro-
cessed. The fruit owner may be a member of a cooperative or part owner of the
plant, or the fruit may have been purchased by the plant itself. In some areas,
this process is regulated by governmental agencies in order to ensure impar-
tiality, such as is done in Florida. Because it is most efficient for processors to
operate continuously, batch processing of the fruit belonging to an individual
grower generally has been replaced by the collection of a random fruit sample
from the fruit prior to processing. An analysis made from tests on this fruit
sample is used to determine the value of the load of fruit brought into the plant.
These tests include juicing the fruit sample to determine the theoretical juice
yield, as well as measuring the Brix and acid levels to determine the theoretical
weight of soluble solids that will be produced from the corresponding load of
fruit. There are many ways that this can be done. The following suggested
procedure involves the use of a weigh ticket that originates at the weigh station,
a copy of which accompanies the fruit sample so that the results can be asso-
ciated with the proper load of fruit.

Analysis of Fruit Samples

Equipment and Supplies

• Random fruit collector (preferably mechanical).


• Sample containers (you should have enough containers to hold one day's
worth of samples).
• Fruit sample conveyer (belt, rollers, hand truck, pallet, etc.).
• Scales to weigh samples (preferably washable scales).
• Fruit receipt or weigh ticket for sample identification.
• Brix measuring equipment (see Chapter 2).
• Acid measuring equipment (see Chapter 3).

66

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
TESTING OF FRUIT SAMPLES 67

• Juice container or bucket (2-3-gallon).


• Ladle and juice sample containers (numbered paper cups work well).
• Juice extractor, preferably one that is similar to or simulates commercial
extraction in the plant.

Procedure

1. Obtain a random representative sample weighing approximately 30 to 40


Ib, using a mechanical sampler and adequate sample containers. Be sure
that a fruit receipt or sample identifier is attached to each sample. Convey
the samples to the sample extracting area.
2. Weigh the sample and note the gross weight on the receipt or on a fruit
record form.
3. Extract the fruit according to the design of the extractor, preferably in a
manner similar to the commercial method used in the plant. Collect the
juice in a 2-3-gallon container or bucket.
4. Reweigh the empty fruit sample container, and subtract its weight from
the sample gross weight to get the net weight of the fruit sample.
5. Weigh the bucket of extracted juice to get the gross juice weight. Using
the ladle, stir the juice in the bucket, and fill the hydrometer tube if you
are using a hydrometer, or the juice sample container if you are using a
refractometer.
6. Discard the remaining juice in the bucket, and reweigh the empty bucket.
Subtract this weight from the gross weight to get the wet weight of the
juice.
7. If a hydrometer is used, measure the Brix as explained in Chapter 2. Once
the corrected Brix is determined, use a portion of the juice in the hydrom-
eter tube for the acid titration.
8. The juice sample can be used for Brix and acid determinations if a re-
fractometer is used.
9. The acid titration can be performed as explained in Chapter 3, and the
Brix, % acid, and Brix/acid ratio should be recorded on the fruit sample
receipt or record.

The yield can be reported as gallons of juice per ton of fruit, but the most
popular yield expression is pounds of soluble solids per ton of fruit. This can
be calculated from the fruit sample data by use of the following equation:

sol/ton = (2000 Ib/ton)(fV;) (F)(B)/(Wf )(I00%) = 20fV;FB/Wf (5-1)

where W; is the net weight of the juice, Wf is the net weight of the fruit, B is
the corrected Brix, and F is a factor applied to account for fruit loss during
68 CITRUS JUICE CHARACTERISTICS

grade-out in normal processing. The generally accepted value of this factor for
oranges, grapefruit, and tangerines is 0.85, allowing for a 15% loss of fruit,
whereas for lemons and limes the accepted factor is 0.78.
The gallons of juice per ton of fruit can be found by first obtaining the density
D (lb / gal) from the Brix by using Equation 2-9 or 2-11, and then using the
following:

gal/ton = (2000 lb /ton) (lfj)F /WfD (5-2 )

This value is helpful in estimating the size and uses of processing equipment.
Also of value in estimating the size and uses of the equipment employed in
peel processing, as well as in crediting fruit growers for the resulting profits in
the sale of peel products, is calculation of the pounds of peel per ton of fruit.
This can be done by using fruit sample data, as follows:

peel/ton = (2000 lb/ton)( Wf - lfj)/Wf (5-3 )

Each of the three above parameters can be used with the total net weight of the
fruit to give the total weight of solids, gallons, and weight of peel from a given
load of fruit. For example, if 20,172 lb of fruit were brought into a processing
plant with a random fruit sample weighing 34.11b (including a 3.8-lb container)
that yielded 14.2 lb of juice (including a 1.1-lb bucket) with a corrected Brix
of 12.6, Equations 5-1,5-2, and 5-3 would give the following results:

sol/ton = 20(13.1)(0.85)(12.6)/30.3 = 92.6 sol/ton


gal/ton = 2000 ( 13.1) (0.85) /(30.3) (8.745) = 84.0 gal/ton
peel/ton = 2000(30.3 - 13.1)/30.3 = 11351b peel/ton

As with other quality control calculations, fruit sample data processing can
be performed most efficiently on a computer. Figure 5-1 is a flow chart that can
be used to write the appropriate programs. A suggested GWBASIC program
using such a flow chart can be found in Appendix B, with a similar program
for HP-41 C programmable calculators in Appendix C.
Even though fruit sample analysis is used to credit fruit owners for the fruit
processed, processors generally are responsible for ensuring that the results of
such tests are sufficiently accurate. Also, the processors need to monitor actual
yields to ensure that they compare to the theoretical yields of the fruit samples,
so that they will not shortchange the fruit owners or themselves. For example,
if, in a given week, a processor recovers 100,000 lb of soluble solids but credits
the fruit owners with 110,000 lb of soluble solids, he will have shortchanged
himself by 10,000 lb of soluble solids, which he will have to pay for from some
TESTING OF FRUIT SAMPLES 69

Uncorrected Brix (Bi)


mls NaOH titrated (mls)
(and Normality (N»
net wt. of fruit (Wf)
net wt. of juice (Wj)
temp °C (T)

B == Bi + Acor + Tcor
R == B/A

EO 5-1 EO 5-2 EO 5-3


Ibs solids/ton gal/ton Ibs peel/ton
F == 0.85 F == 0.85 F == 0.85

Fig. 5·1. Flow chart that can be used to program a computer to calculate the fruit sample data
needed to credit a fruit owner for his or her fruit that is processed.

other funds. Conversely, if he credits the fruit owners with only 60,000 lb of
soluble solids, he will have cheated the fruit owners out of 40,000 lb of soluble
solids. This is why it is important to obtain as representative fruit samples as
possible, with results that match actual industrial yields as closely as possible.
Production efficiency can easily be measured by using:

% efficiency = Sa(iOO% )/Se (5-4 )

where Sa is the lb soluble solids of actual recovery, and Se is the lb soluble


solids estimated from the fruit sample analyses. The ideal % efficiency is 100
70 CITRUS JUICE CHARACTERISTICS

to 11 0 %, which gives the processor the freedom and the economic means to
make slight adjustments in returns to fruit owners and to remain financially
solvent. If the % efficiency is outside the ideal range and/or fruit sample results
appear out of line, the following checks should be made:

1. Check fruit sample data and calculations for errors.


2. If possible, collect another sample and redo the fruit sample test.
3. Check the sample extractor to see if it is simulating actual production,
and make legal adjustments if necessary .
4. Check the commercial extractors to see if they are producing proper yields.

LEMONS AND LIMES

Lemons (and limes) require a slightly different approach to fruit sample analysis
because their juice concentration is based on the weight of acid per unit volume.
The procedure for extraction of the juice from lemon fruit samples is the same
as with oranges, and the juice is tested in the same manner except that the NaOH
solutions used in the acid titration may be more concentrated here. Once the
fruit has been tested, the calculations of the results differ from those performed
for other citrus fruit. First, the density, D, needs to be calculated from the Brix
by means of Equation 2-9 (or density tables), and used in the yield equations
below:

. 2000 Ib/ton(llj)(% acid)F 20(% acid)lljF


Ib aCId/ton = Wi
100% ) = Wf (5-5)

gal/ton = 2000 lbs/ton (llj)F /WfD (5-6)

where llj is the net weight of the lemon juice, Wf is the net weight of the lemon
fruit, and F is the production loss factor of 0.78 for lemons and limes. For
example, a lemon fruit sample weighing 31.2 net Ib yielding 11.61b net weight
of juice with a corrected Brix of 9.7 and a % acidity of 5.37 % would give:

20(11.6)(5.37)(0.78)/(31.2) = 31.11b acid/ton


2000(11.6)(0.78)/(31.2)(8.644) = 67.1 gal/ton

The lb peel/ton is calculated the same way as for orange fruit samples, men-
tioned previously. Figure 5-2 shows a flow chart that can be used in program-
ming computers to perform these calculations, and a sample GWBASIC pro-
gram can be found in Appendix B. A similar program for the HP-41C
programmable calculator can be found in Appendix C.
TESTING OF FRUIT SAMPLES 71

Uncorrect Brix (Bi)


Fruit net weight CNf)
Juice net weight (Wi)
mls NaOH titrated (ml) I-----I~I
Normality NaOH (N)
Temp. (0C) (T)

B = Bi + Acor + Tcor

EO 5-5 EO 5-6
Ibs acid/ton gallons/ton
F = 0.78 F = 0.78

Fig. 5-2. Flow chart that can be used to program computers to calculate data from lemon or lime
fruit sample testing.

QUESTIONS

1. Why are actual yields not used to credit fruit owners for juice and by-
product yields?
2. What is the purpose of the fruit receipt or ticket?
3. Why and how often should actual yields be determined?
4. Why is a different factor, F, used with lemon fruit samples compared to
other citrus fruit?
5. What would probably be the cause of an 80% level of efficiency in pro-
cessing tangerines?
72 CITRUS JUICE CHARACTERISTICS

PROBLEMS

1. What would be the yield in sol/ton, gal/ton, and peel/ton of a fruit sample with a
weight of 27.6 Ib (including a 3.4-lb container) that yielded 13.4 Ib (including a
1. l-Ib container) of juice that had a corrected Brix of l3.4?
2. If grower A sent 19.6 tons of fruit into a processing plant that gave a yield of 106.2
Ib sol/ton, and grower B sent in 22.4 tons of fruit with a yield of 92.2 Ib sol/ton,
who would receive more money for the fruit?
3. Is the efficiency of a plant that obtains 315.6 tons of oranges in one week with a total
solids of 31,150 Ib credited to fruit growers or owners, and which produces 5073
gallons of 60.0 o Brix concentrate from that fruit, within an acceptable range?
4. What would be the yield in lb acid/ton, gal/ton, and peel/ton of a lemon fruit
sample with a net weight of 28.6 Ib yielding a net weight of 9.8 lb of juice with a
corrected Brix of 9.2 and 6.12 % acid?
5. If the fruit sample in problem 4 were grapefruit instead of lemon, what would the
fruit sample yields be?
Chapter 6

Citrus Oils, Aromas, and Essences

The sweetness of carbohydrates and the sourness of organic acids impart about
the same flavor characteristics to all citrus juices. However, the distinctive fla-
vor of an individual variety can be attributed to varying components in the oils,
aromas, and essences found within the juice. Although some compounds con-
tribute more to flavor than others, exact citrus flavor duplication would require
a delicate balance of a host of contributors. About 87% of the fresh squeezed
flavor of orange juice has been restored to freshly evaporated concentrate by
using d-limonene, ethyl butyrate, citral, and acetaldehyde (Ahmed, Dennison,
and Shaw 1978). It is well known that oxygenated hydrocarbons are major con-
tributors to citrus flavor, with d-limonene acting more as a carrier of these fla-
vors than an actual contributor itself. The excess d-limonene levels, however,
produce the characteristic "oil bum" taste that can irritate the skin or eyes. The
d-limonene in the peel will bum the edges of the mouth when one is eating fresh
fruit, and d-limonene fumes will bum the eyes during juice extraction in un-
ventilated areas. Natural variations of the delicate balance of flavor-producing
compounds are primarily responsible for vintage and off years. Processing also
has an effect on these compounds and can make or break the quality of a par-
ticular citrus product.
Not only do citrus oils, aromas, and essences contribute to juice quality, but
they can be commercially recovered and used to enhance juices and other food
products as well as be used in other industries. Because these oil products were
extracted from natural sources, the citrus fruit itself, they can be added back to
juices without violating federal standards of identity. This method of restoring
citrus flavor to concentrates generally has replaced the older method of adding
freshly squeezed cutback juice to high-Brix concentrates. Citrus oils also have
been used in the manufacture of textiles, chemicals, and other commodities.
Their toxicity to certain insects, such as houseflies, fire ants, and fleas, as well
as their herbicidal and flammable nature, suggest other promising uses.

73
D. Kimball, Citrus Processing
© Van Nostrand Reinhold, New York, NY 1991
74 CITRUS JUICE CHARACTERISTICS

OIL COMPOSITION

Citrus oils are found primarily in oval-shaped sacs in the flavedo or colored
portion of the peel, and they act as a natural toxic barrier to many microorga-
nisms and insects. Citrus oils are composed primarily (over 90%) of
d-limonene, a sesquiterpene, with other monoterperenes and sesquiterpenes
being found in trace amounts.
In orange oils, 111 volatile constituents have been found (Shaw 1977), in-
cluding 5 acids, 26 alcohols, 25 aldehydes, 16 esters, 6 ketones, and 31 hydro-
carbons. Nonvolatile constituents comprise about 1.5% of the orange oils, in-
cluding waxes, coumarins, flavonoids, carotenoids, tocopherols, fatty acids,
and sterols.
Grapefruit oil is characterized by the presence of nootkatone, which gives a
grapefruit flavor and aroma. It consists of 20 alcohols, 14 aldehydes, 13 esters,
3 ketones, and 14 monoterpenes and sesquiterpenes. The nootkatone increases
with fruit maturity. The nonvolatile portion of grapefruit oil comprises about
7 % of the oil, including coumarins, flavonoids, tocopherols, and waxes.
Tangerine oils contain the distinctive nonvolatile tangeretin in significant
amounts (4 %), along with 24 alcohols, 11 aldehydes, 4 esters, 2 ketones, 7
acids, 24 hydrocarbons, and 2 ethers.
Lemon oils are believed to contain about 2 % nonvolatiles, primarily in the
form of coumarins, along with 18 alcohols, 16 aldehydes, 11 esters, 3 ketones,
4 acids, and 23 hydrocarbons.
Lime oils have been known to contain 12 alcohols, 7 aldehydes, 4 esters, 1
ketone, and 22 hydrocarbons, with 7 % nonvolatiles, mostly in the form of cou-
marins.

OILS IN CITRUS JUICES

The hydrocabrons are the major constituents of citrus oils, primarily as


d-limonene (over 90%). In lemon and lime oils, significant amounts of a-pinene
occur (about 5%). As mentioned above, d-limonene acts as a carrier of flavor
for other oxygenated compounds and contributes little to flavor itself. However,
excess d-limonene can be detected as an oil bum on the tongue and thus should
be kept in check. For these reasons, oil levels in citrus products have been
considered important quality parameters and generally merit routine monitor-
ing.
Scott and Veldhuis (1966) developed a method of measuring the oil in citrus
juices (or any product containing citrus oils) that has been accepted by the in-
dustry, and their method (known as the Scott method) generally has replaced
the Clevenger method, which involved steam distillation and collection of the
CITRUS OILS. AROMAS. AND ESSENCES 75

oil from the product. The Scott method is much easier and faster, with greater
accuracy and precision, than the Clevenger method. Scott oil values are higher
then Clevenger levels, suggesting a more efficient analysis. The Scott method
involves bromine addition to the two double bonds in d-limonene, the mea-
surement of d-limonene as a representation of the oil level having become stan-
dard in the industry. Citral, the cis-trans mixture of neral and geranial that
occurs in lemon and lime oils in quantities up to 4 %, reacts with half as much
bromine as d-limonene. Also a-pinene reacts with the same amount of bromine
as d-limonene, even though a-pinene has only one double bond. Scott attributed
this phenomenon to some sort of secondary reactions or molecular rearrange-
ment of the a-pinene.
Because bromine is very volatile in pure form or in solution, straight standard
bromine solutions are unreliable in concentration. Scott used a bromide-bro-
mate salt solution to titrate the acidified alcoholic distillate from a juice sample,
as this salt solution was found to have a very stable concentration. As soon as
the bromide-bromate solution comes into contact with the acidified distillate,
an acid-catalyzed oxidation-reduction reaction takes place between the bromide
and the bromate to form bromine, which can react immediately with the double
bonds of d-limonene, according to the following equation:

Br03 + 6H+ + 5Br- ........ 3Br2 + 3H20


bromate acid bromide bromine
ion ion (6-1 )

The EO value for the above reaction is +0.43 V, which is indicative of the
thermodynamic favorability of the reaction. Once the bromine has been gen-
erated, it proceeds to react with d-limonene, and the other minor constituents
mentioned above, according to the following reaction:

Br

2Br2 +
bromine
(6-2 )

brominated
d-limonene
d-limonene

What makes this basic chemistry effective as a tool in routine industrial qual-
ity control is detection of the endpoint by means of methyl orange, a common
acid-base indicator. Bromine reacts preferentially with d-limonene until the
76 CITRUS JUICE CHARACTERISTICS

unbrominated terpene is exhausted. It then reacts with the pink or violet methyl
orange according to the following reaction:

Methyl Orange

Brominated Methyl Orange

(6-3 )

The conjugated resonance structure of the double bonds in methyl orange is


responsible for its color. Bromination disrupts this conjugation and results in a
loss of color, with the color loss signaling the end of the titration. Titration
beyond the endpoint causes a slight yellow color to appear, which resembles
the color of dilute unreacted bromine. Scott reported that the use of a blank in
the titration produced a value of 0.2 ml or 0.0008% oil, which generally can
be disregarded. Experience in working with blanks for specific citrus products
will facilitate their proper use.

Scott Method for % Oil

Equipment and Supplies

• Setup shown in Figs. 6-1 and 6-2.


• 10 ml auto-dispenser or graduated cylinder.
• 25 ml pipette or graduated cylinder.
• Hot pad to enable handling of hot glassware.
• Isopropyl alcohol.
• Dilute HCL solution made from equal parts concentrated HCl and water.
(Care should be taken to add the concentrated acid to water under a fume
hood or in a well-ventilated area. Never add water to concentrated acid.)
• 0.1 % methyl orange indicator (0.1 g dry methyl orange to 100 ml of dis-
tilled water).
• 0.0247NBr- -Br03 solution. (Dissolve 0.688 g ofKBr0 3 and 3 g (excess)
KBr in one liter of distilled water. This solution should be standardized.)
• Two 100 ml volumetric flasks for standardization.
• 1 ml pipette for standardization.
CITRUS OILS, AROMAS, AND ESSENCES 77

Fractionation Plate ---t"'-

water
out

Condenser

Boiling Flask

~;~C:=-"'~I-- water
Juice and in
Alcohol ---~..

Fig. 6-1.
Heater

g.~-- Distillate

Setup for distillation of citrus oil using the Scott method.

• 10 ml pipette for standardization.


• About 10 ml of pure citrus oil for standardization.

Standardization of Bromide-Bromate Solution

1. Add 10 ml of citrus oil to a 100 ml volumetric flask using a 10 ml pipette.


Fill the flask to the mark with isopropyl alcohol. Mix the solution well.
2. Withdraw 1 ml of this solution and add it to a second 100 ml volumetric
flask, and fill it to the mark with isopropyl alcohol. Mix well.
3. Pipette 10 ml of this solution into the boiling flask shown in Fig. 6-1 along
with about 25 ml of water and another 15 ml of isopropyl alcohol.
4. Proceed with the oil determination below, beginning with step number 3.
5. Divide the dilution (0.010) by the milliliters titrated (should be about 10
ml) to get the factor (about 0.0010).
78 CITRUS JUICE CHARACTERISTICS

f,Do~-- Thistle Tube With Ascarite


Carbon Dioxide Absorbent
Two Hole Stopper

+--+- Bromide-Bromate Solution

+- 5 Gallon Resevoir

.......- Latex Tubing

.:1 ....-+....... Auto Zero 25 ml Buret

.......- Buret Refill Clamp

<= .......- Distillate

~.......- Magnetic Stirer


t
Waste Container

Fig. 6-2. Setup for titration of distillate in Scott method oil detennination.

Procedure

1. Using a pipette or graduated cylinder, add 25 ml of 1l.8°Brix juice or


sample into the boiling flask in Fig. 6-1. Boiling chips may be used to
facilitate boiling.
2. Using a graduated cylinder, add 25 rnl of isopropyl alcohol and 25 rnl
CITRUS OilS, AROMAS, AND ESSENCES 79

distilled water to the boiling flask, and heat the mixture to boiling using
the setup in Fig. 6-1.
3. Distill until moisture can be seen inside the distillation apparatus in the
form of water beads. Even though 25 ml of alcohol was added to the
sample, more than 25 ml should be collected in the distillation because of
the azeotropic nature of water/alcohol mixtures. Premature termination of
the distillation will result in artificially low oil levels.
4. Using an auto-dispenser or a graduated cylinder, add about 10 ml of the
diluted acid and 1 drop of methyl orange indicator to the distillate. An
additional 25 ml of isopropyl alcohol can be added to the distillate to
provide more volume for mechanical stirring but is not necessary for the
titration.
5. Titrate the distillate, while stirring, with the bromide-bromate to a col-
orless endpoint.
6. Oil levels are reported as the % by volume in 11.8 °Brix juice. This is
found as follows:

. / _ (ml titrated) (factor) (100%)


% 011 v v - (ml o f samp1e ) (6-4 )

where the factor is found from the above standardization. For example,
if 1.5 ml of bormide-bromate were titrated, Equation 6-4 would become:

{1.5 ml)(O.OOIO)(I00% )/(25 ml) = 0.006% v /v oil

The USDA grade standards for citrus products can be found in Table 6-1.
Even through grade A orange juice is allowed up to 0.035 % oil, oil bum can
be detected below 0.020 %, depending on the juice. Commercial orange juices
generally contain about 0.015 to 0.025% oil.

OIL LEVELS IN BLENDS

It is sometimes of interest to determine the final oil in a blend so that one can
predetermine the amount of additional oil or oil-based flavors without exceeding
any maximum oil level specifications. For example, if an oil specification re-
quires the oil level to be 0.020% or lower, and you want to add as much oil-
based flavor enhancer as possible, the average oil content of the components in
a blend must be determined prior to any further oil addition. Once the oil level
of the blended components has been calculated, the amount of flavor enhancer
that can be added without exceeding oil juice specifications can be calculated.
It is important to determine these parameters prior to blending because of the
difficulty of mixing the immiscible oil with the aqueous juice. Oil addition is
80 CITRUS JUICE CHARACTERISTICS

Table 6-1. Maximum oil levels (% v /v) allowed under USDA grade
standards
Grade A Grade B

Orange (47FR 12/10/82,52.1551-52.1557)


Frozen concentrated orange juice 0.035 0.040
Orange concentrate for manufacturing none one
Orange juice from concentrate 0.035 0.045
Canned orange juice 0.035 0.055
Reduced acid orange juice 0.035 0.040
Canned concentrated orange juice 0.035 0.040
Dehydrated orange juice 0.035 0.045
Pasteurized orange juice 0.035 0.045

Grapefruit (48FR 9/12/83,52.1225-52.1227)


Grapefruit juice 0.020 0.025
Grapefruit juice from concentrate 0.020 0.025
Frozen concentrated grapefruit juice 0.020 0.025
Concentrated grapefruit juice for manufacturing none none
Dehydrated grapefruit juice 0.020 0.025
Grapefruit and orange (6FR ll/lln, 52.1288-52.1290)
Grapefruit and orange juice 0.035* 0.055
Tangerine (2FR 711169,52.2931-52.2941)
Canned tangerine juice 0.025 0.035
Concentrated tangerine juice for manufacturing none none
* Grade standards are the same for sweetened and unsweetened.

best done as the components are being added. The average oil of the blend
components can be found from the following equation:

( 6-5)

where volumes (V), % oils (0), and the pounds of solids per gallon (S) (cal-
culated from the Brix using Equations 2-8 or 2-10) of the blend components are
used to calculate the final average oil of the blend (0a). If the Brix values of
the blend components are similar, the S values may be omitted. The amount of
oil needed to raise the oil level to a certain level can be calculated by using the
following equation:

(3785.306 ml/gal)SV
mloil = (Of- 0;) 100%(1.046 sol/gal) = (Of- 0;) (36.19)(SV)
(6-6)
CITRUS OILS, AROMAS, AND ESSENCES 81

where the final desired oil level (Of), the initial oil level (0;), the pounds of
solids per gallon (S) (found from the Brix using Equation 2-8 or 2-10), and the
juice volume (V) can be used to calculate the milliliters of oil that need to be
added. In a blend, the three latter values should be the calculated average values
for the final blend. If the calculated average oil level of a blend is too high to
allow you to add as much oil or flavor enhancer as you would like, one of the
blend components can be exchanged for one with less oil to maintain the same
overall volume, or a different volume of one of the blend components can be
used. In the former case, the following equation can be used:

01 = Of+ (S2 V2(Of- O 2) + S3 V3(Of- 0 3 ) +

+ Sn Vn( Of - On) )/SI VI ( 6-7)

In the latter case, the following equation can be used:

VI = S2 V2( Of - O2) + S2 V3 (Of - 0 3) + . . . + Sn Vn (Of - On) (6-8)


OISI (1 - 0f/Od

Both of the above equations are rearrangements of Equation 6-5. Again, if the
Brix values of the components are similar, the S values can be omitted.
Let us take an example to illustrate the use of the above equations. Suppose
that we had the following blend components:

Lot # # Drums Brix Sol/Gal % Oil


1 18 65.0 7.135 0.006
2 12 62.1 6.726 0.011
3 16 59.8 6.409 0.023
4 7 60.6 6.518 0.009
5 7 64.8 7.107 0.013

Also, suppose that we want to add as much flavor enhancer as possible, not to
exceed 0.020% oil. First, Equation 6-5 would be used to determine the average
oil in the blend as follows:

18 (0.006)7 .135 + 12 (0.011 )6.726 + 16(0.023 )6.409


+ 7 (0.009 )6.518 + 7 (0.013 )7.107
18(7.135) + 12(6.726) + 16(6.409) + 7(6.518) + 7(7.107)
= 0.012% oil

As you can see, the units of volume can be anything as long as the same units
are used throughout the calculation. In order to raise the oil level from 0.012 %
82 CITRUS JUICE CHARACTERISTICS

to the desired 0.020%, Equation 2-16 can be used to find the average pounds
of solids/gallon:

SPG = _18-....:('--7_.1_35-'.)_+_12--.:('--6_.7_26....:.)_+_1_6(-,-6_.4_0_9),-+_7--'.(_6._5_18-,-)_+_7_(,-7_.1_0-,-7)
18 + 12 + 16 + 7 + 7
= 6.784

Next, Equation 6-6 can be used to calculate the milliliters of oil needed to raise
the oil level from the average of 0.012 % to 0.020%:

(0.020 - 0.012) (6.784) (36.19) (60 drums X 52 gal/drum) = 6128 ml

Because the "36.19" constant is based on gallons as a volume unit, the 60


drums had to be converted into gallons assuming 52 gallons per drum.
Now suppose that your product formulation requires at least 2.5 ml of oil-
based flavor enhancer per gallon of concentrate. For the 3120 gallons (60 drums
x 52 gal/drum) of concentrate in the example, you would need to add 7800
ml of flavor enhancer or oil, an amount greater than the 6128 ml of oil permitted
by the specification. Rearrangement of Equation 6-6 will allow us to determine
the maximum allowable oil level that will permit 7800 ml of enhancer to be
added and still maintain a final oil level of 0.020 % :

0; = Of - (rnl oil)/VS(36.19) ( 6-9)

In the example this gives:

0.020 - 7800/3120(6.784)(36.19) = 0.010%

This means that we need to reduce the 0.012 % average oil level in the blend to
0.010% by changing the blend components. Suppose that we wanted to ex-
change lot 3 for a lot with a lower oil content with a Brix of 60.1 (S = 6.450).
Equation 6-7 would become:

(18(0.010 - 0.006)7.135 + 12(0.010 - 0.011)6.726


+ 7(0.010 - 0.009)6.518 + 7(0.010 - 0.013)7.107)
0.010 + 16(6.450)

= 0.013% oil

which represents the maximum oil level that the replacement lot could contain.
If a lot with such an oil level is difficult to find, the number of drums of lot 3
CITRUS OilS. AROMAS. AND ESSENCES 83

can be changed instead of the oil level, using Equation 6-8 as follows:

18(0.010 - 0.006)7.135 + 12(0.010 - 0.011)6.726


+ 7(0.010 - 0.(09)6.518 + 7(0.010 - 0.013)7.107
0.023 (6.409)( 1 - 0.010/0.023)
= 4 drums of lot 3 instead of 16

This maze of calculations is best perfonned by computers. A flow chart il-


lustrating the programming logic is shown in Fig. 6-3. A GWBASIC program
that utilizes the flow chart can be found in Appendix B, along with a related
program for the HP-41 C programmable calculator in Appendix C. After adding
the data for the blend components using the HP-41C program, enter "0" for
the Brix and follow the prompts ofthe program. You can exchange components
as many times as you want at the end of the program.

DEOILING SINGLE-STRENGTH JUICE

During certain times of the harvesting season, freshly extracted juice reaches a
B / A ratio that is suitable for commercial juice as is without blending. This juice
can be pasteurized to stabilize the enzyme activity or packaged as is, depending
on the standard of identity employed. Freshly extracted juice, however, con-
tains high levels of citrus oils that exceed the USDA grade standard of 0.035 %.
These oils generally require deoiling using a heated vacuum technique. This
deoiling also serves as pasteurization and enzyme stabilization. New extraction
techniques are emerging that minimize the oil levels of freshly extracted juice
that may eliminate the need for deoiling in the future. During deoiling opera-
tions, the oil levels should be constantly monitored. If the oil levels are too
high, more steam or slower flow rates should be used, and vice versa. Slight
concentration of the juice during deoiling is commonly observed. The aqueous
distillate containing aroma components is commonly returned to the deoiled
juice in order to restore some of the flavor lost during deoiling as well as to
counter the slight concentration effect.

OIL AND AROMA PRODUCTION

Citrus oils and aromas are generally the major by-products of citrus processing
and are used in a variety of products. Eight types of oils and aromas are com-
monly manufactured, and their general characteristics, standards, uses, and
method of processing will be discussed hereafter. Generally speaking, the tenn
"aromas" refers to the aqueous phase separated from the oil phase in evapo-
84 CITRUS JUICE CHARACTERISTICS

Brix of Compo n (Bn) n


Zl =}: ViOiSPGi
% oil of Compo n (On) i=l
Vol. of Compo n (Vn) n
Desired final oil (Of) ~--"'I Z2 =}: ViSPGi
Max. oil enhancer i=l
allowed (M) n
Vt =}: Vi
i=l

EO 6-5
Oa = Zl/Z2

EO 6-9 EO 2-16
EO 2-16 Oe or max. Oi
SPGavg = Z2Nt allowed per SPGavg = Z2M
specification

EO 6-6
mls needed to get Of

Add calculated mls EO 6-7 EO 6-8


oil enhancer from 01 needed for V1 needed for
EO 6-6 component exchanged component exchanged

Fig. 6-3. Flow chart that can be used to program computers to calculate the milliliters of oil
needed in a blend or the maximum allowable milliliters of oil-based flavor enhancer that can be
added per specification.
CITRUS OILS, AROMAS, AND ESSENCES 85

rator and pasteurized condensates, which contains important volatile flavor and
aroma components.

Cold Pressed Aroma and Oil

Cold pressed oils are recovered from the flavedo of citrus peel by rasping or
rupturing the oil sacs close to the surface of the fruit just prior to or during juice
extraction. Because heat easily removes the valuable volatile oil components,
no heat is applied to the oil. As the oil is extracted, water is used to wash it
from the peel to form a slUrry. The use of too much water during this step causes
excess peel material to get into the slurry, which can absorb important oil con-
stituents, such as aldehydes, that are removed with the peel material. Excessive
pressure in oil sac rasping or rupturing also will cause excess peel material to
get into the slurry. The peel then is washed with water, and the washings are
conveyed to a finishing press that separates the oil slurry from pieces of peel.
Excessive finishing pressure will cause excessive insolubles to get into the oil
emulsion, making it more difficult to break during polishing.
The oil slurry is centrifuged in a desludging centrifuge (8,000-10,000 rpm)
that separates the slurry into an oil-rich emulsion, an aqueous discharge, and a
semisolid sludge material. The sludge usually is discarded, but the aqueous
discharge may be filtered and returned to wash the peel to form additional oil
slurries. In this way, any small amounts of oil remaining in the aqueous dis-
charge may be recovered through a recycle of the water. The oil-rich emulsion
may be treated with enzymes for several hours, depending on the enzyme, or
it may be placed in a freezer for about 30 days in order to help it break up for
increased oil recovery. The emulsion then is centrifuged in a two-way separator
or oil polisher (16,000-18,000 rpm) that centrifuges it into a discarded heavy
phase and a light clear oil phase. Some plants polish the emulsion immediately
after desludging. The product then can be treated enzymatically or stored in a
freezer for about 30 days to facilitate the precipitation of waxes dissolved in
the oil. After such "winterizing," the oil can be decanted and filtered and the
waxy precipitates discarded. The oil should be stored in closed-head glass, tin-
dipped, aluminum, wall-galvanized, or suitably lined drums under nitrogen or
carbon dioxide. Citrus oils absorb readily into most plastics, so plastic con-
tainers should be avoided. Refrigeration and air exclusion in the headspace of
the oil drums minimize oxidation. However, the precipitation of waxes may
continue, as precipitation slows with time but never really stops at low temper-
atures. Storage temperatures of 60 to 75°F generally are recommended to keep
the waxes in solution. Also, protection from light is advised because photo-
chemical reactions with some oil components may detract from the quality of
the oil.
86 CITRUS JUICE CHARACTERISTICS

Oil yields generally increase with maturity of the fruit but decrease right after
periods of rainfall. Soft fruit generally gives poorer yields than firm fruit be-
cause of less efficient rasping or rupturing of the oil sacs. Grapefruit oils are
best extracted from February through April and need to be cured after dew axing
for about 6 months (60-70°F). The oil starts out orange-like in nature and then
undergoes a chemical change. Waxes take longer to precipitate in grapefruit
oils than with orange oils even though 95 % of the waxes are removed in the
first two months of storage. However, waxes may continue to precipitate for up
to 2 years. The lower the temperature is, the faster the precipitation.

Cold Pressed Oil Quality Control

To obtain the highest yield possible, it is important to perform quality control


checks at different points of the oil extraction process. This can be done by
taking samples of the oil slurry, the aqueous discharge from the desludger, the
oil emulsion from the desludger, and the heavy discharge coming from the pol-
isher. If yields seem unusually high or low, whole fruit can be analyzed for the
total available oil in order to determine if yields are affected by biological or
processing parameters. Analysis of the whole fruit is difficult, however, espe-
cially on a routine basis. Analyzing the samples described above generally will
reveal processing problems, and comparison of overall oil production versus
tons of fruit run generally will show problems in the fruit and the first stages of
the oil process.
The efficiency of the desludger can be measured by taking 1.00 ml of the
inbound oil slurry, adding about 25 ml of isopropyl alcohol, and titrating, using
the Scott method described earlier in the chapter (as). Next one takes 1.00 ml
of the aqueous discharge and performs the same oil determination (0 a). Then
the following equation is used to calculate the desludger efficiency:

% oil recovery = (as - Oa) 100% / as (6-10)

The % recovery should be above 90%. The heavy aqueous discharge may be
filtered and reused to wash more oil from the peel into the oil slurry in order to
reclaim a portion of the oil remaining in the aqueous material.
The oil coming from the oil-rich emulsion from the desludger also is a pa-
rameter ofthe oil recovery efficiency. It can be measured by weighing 1-2 grams
of the emulsion into a 100 ml volumetric flask and filling the flask to the mark
with isopropyl alcohol. The weight of the sample must be recorded exactly.
Then 1 m1 of this dilution is added to 25 ml of isopropyl alcohol and titrated
CITRUS OILS, AROMAS, AND ESSENCES 87

by the Scott method. The % oil in the emulsion can be calculated by using:

o = (ml titrated) (0.001 ml oiliml titrated) (100 ml fisk) (100% )d


e (wt of emulsion)
(6-11 )

where Oe is the % oil in the emulsion, and d is the density of the oil. For orange
oil the density is 0.842 giml, and that for lemon oil is 0.853 giml. The oil
level in the emulsion should be between 70 and 80 % and can be changed by
varying the flow rate through the desludging centrifuge, the length of time be-
tween bowl flushings, and the length of time the bowl remains open during the
flush cycle. The oil emulsion then should be treated enzymatically and stored
in cold storage, or it may feed into the polisher immediately, depending on the
oil recoveries desired. Immediate treatment of the oil emulsion may result in
some oil loss during polishing because the emulsion will be more difficult to
break. The rate of flow into the polisher varies with equipment but should be
about 1 to 1.5 gallons per minute. The heavy discharge from the polisher can
be analyzed for oil by the Scott method in a manner similar to that for the oil
emulsion; and it should not contain more than 5 to 7 % oil. In larger operations
more than one polisher may be required to minimize oil losses. A 100-mesh
screen sometimes is used to remove extraneous debris from dewaxed or pol-
ished oils. Aroma oil is made from the distillation of the aqueous discharge
from polishers.

Steam-Distilled Oils and Aromas

Steam-distilled oils generally are produced by steam injection or steam distil-


lation of expressed sugar solutions (press liquor) obtained by pressing limed
peel. Steam is injected into the press liquor and carries off d-limonene even
though it has a higher boiling point than water (352°F compared to 212°F).
The condensate separates into an oil layer on the top and an aqueous layer on
the bottom. The oil layer, which is decanted, contains about 25% more alde-
hydes than cold press oil because the aldehydes are less volatile than d-limonene,
which is lost during the heat treatment. The oil slurry feeding into the desludg-
ing centrifuge in cold pressed oil operations also may undergo steam distilla-
tion. The amount of steam used, as well as the amount of cooling in the con-
densers, may be adjusted to give a maximum yield with a minimum of oil
remaining in the outgoing stripped press liquor or peel. These oils generally are
used in the manufacture of paints, rubber, and textiles.
88 CITRUS JUICE CHARACTERISTICS

Folded Oils

Some cold pressed oils are further distilled in order to remove d-limonene while
concentrating the less volatile oxygenated flavor compounds. These concen-
trated oils, referred to as folded oils, are valuable materials that may be added
back to citrus juices to enhance their flavor without increasing oil levels as much
as untreated cold pressed oils do. Some oils are stripped of all the terpenes and
are referred to as terpeneless oil-a product that is very rich in flavor. Aromas
from the aqueous layer in these steam distillations also may be recovered.

Essence Oils and Aromas

The natural fresh flavors and aromas characteristics of freshly extracted juice
are largely removed during commercial evaporation. Essence oils are recovered
from the condensate from these evaporators and differ from other citrus oils in
the content of valencene, a sesquiterpene (0.5-2.0%), which is not found ap-
preciably in other oils. Excess heat treatment during the recovery of essence oil
will result in chemical conversion from valencene to nootkatone, a character-
istic component of grapefruit oil, as well as breakdown of the esters, under the
acidic conditions of the juice, to alcohols and acids, to give an off aroma com-
monly called a "wet dog" aroma.
There are basically two types of essence oil recovery systems. One uses a
fractionation column to concentrate the volatile materials from the first effect
or first vaporization in commercial juice evaporators, and the second fraction-
ates the volatiles from both the first effect and the second effect; and then the
final products from the two systems are mixed together. The aqueous phase, or
aroma, primarily consists of alcohols and aldehydes (13 % ethanol) (Johnson
and Vora 1983). Yields are generally in the neighborhood of 0.20% of the
inbound juice (11.8°Brix) feeding into the evaporator for aroma and 0.014%
for essence oil.

Juice Oils

The term "juice oils" really has two meanings. Citrus oils not only are found
in oil sacs in the flavedo of the fruit peels, but they occur in the juice cells
themselves. About 0.005 % of the oil in fresh single-strength juice comes from
the juice cell. The juice cell oil is not exactly the same as that found in the fruit
peel, as the juice oil is higher in esters and lower in aldehydes than cold pressed
oil. The oil recovered from single-strength juice in deoiling operations also is
called juice oil even though most of this oil comes from the peel. The latter
definition is the one more commonly used in the industry. This juice oil is
CITRUS OilS. AROMAS. AND ESSENCES 89

generally of better quality than that of essence oils, as in the corresponding


aroma from the respective aqueous phases. As mentioned previously, the
aqueous phase from deoiling operations generally is added back to the deoiled
juice to restore flavor and to offset the slight concentration of the juice during
deoiling.

Quality Control of Citrus Oils

The quality of citrus oils is centered primarily around their flavor attributes,
which arises from a multitude of oil components in varying concentrations.
These delicate flavor balances are little understood; so quality control or quality
monitoring other than subjective organoleptic methods has been very difficult.
However, other methods that are easily used in routine quality control have
served as a means of estimating citrus oil quality, especially in regard to adul-
teration and oxidative tendency. Standards have been set by the United States
Pharmacopeial Convention, Inc. (USP), which first met on January 1, 1820 and
met every ten years thereafter until 1970, when the decision was made to update
its information every five years. The information given below is based on the
convention held in July, 1975. The Food Chemicals Codex (FCC), published
by the National Research Council and officially recognized by the Food and
Drug Administration, contains standards for citrus oil quality. The USP and
FCC standards are summarized in Table 6-2. For more detailed descriptions of
these standards the reader is referred to the original texts (The United States
Pharmacopeia 19th Revision 1975; Food Chemicals Codex 1981).

Optical Rotation

Many chemical compounds occur in pairs that differ from one another only in
the fact that they are mirror images and cannot be superimposed upon each
other. These pairs are referred to as enantiomers, and their difference sometimes
affects their chemical reactivity. If such a pair contains a chiral carbon (a carbon
bonded to four different entities), they will rotate plane polarized light as shown
in Fig. 6-4. If equal amounts of both enantiomers exist together, no net rotation
of polarized light will be observed, as one enantiomer rotates the light to the
right (dextrorotatory) and the other rotates the light to the left (levorotatory).
The degree that the light is rotated as it passes through a solution containing
the enantiomers is directly proportional to the concentration difference of one
enantiomer compared to the other, according to:

R = ale ( 6-12)
90 CITRUS JUICE CHARACTERISTICS

Table 6-2. Summary of citrus oil specifications according to the


United States Pharmacopeia (USP) (1975) and the Food Chemicals
Codex (FCC) (1981).
USP FCC

Lemon Cold Pressed Oil


aldehydes (as % citral) 2.2-3.8 (Cal) 2.2-3.8 (Cal)
3.0-5.5 (Ital) 3.0-5.5 (ltal)
Optical rotation ( + degrees) 57.0-65.6 57.0-65.6
Refractive index (20·C) 1.473-1.476 1.473-1.476
Specific gravity 0.849-0.855 0.849-0.855
UV absorption (315 nm) 2!0.20 (Cal) 2! 0.20 (Cal)
2!0.49 (Ital) 2! 0.49 (Ital)
Lemon Distilled Oil
Aldehydes (as % citral) none 1.0-3.5
Optical rotation ( + degrees) none 55-75
Refractive index (20·C) none 1.470-1.475
Specific gravity none 0.842-0.856
UV absorption (315 nm) none ::;;0.01
Lemon Cold Pressed Oil Desert Type
Aldehydes (as % citral) none 2! 1.7
Optical rotation ( + degrees) none 67-78
Refractive index none 1.473-1.476
Specific gravity none 0.846-0.851
UV absorption (315 nm) none 2!0.20
Lime Cold Pressed Oil
Aldehydes (as % citral) none 4.5-8.5 (Mex)
3.2-7.5 (Tahit)
Optical rotation ( + degrees) none 35-41 (Mex)
38-53 (Tahit)
Refractive index none 1.482-1.486 (Mex)
1.476-1.486 (Tahit)
Specific gravity none 0.872-0.881 (Mex)
0.858-0.876 (Tahit)
UV absoorption (315 nm) none 2!0.45 (Mex)
2! 0.24 (Tahit)
Evaporative residue ( % ) none 10.0-14.5 (Mex)
5.0-12.0 (Tahit)
Lime Distilled Oil
Aldehydes (as % citral) none 0.5-2.5
Optical rotation ( + degrees) none 34-47
Refractive index (20·C) none 1.474-1.477
Specific gravity none 0.855-0.863
CITRUS OILS, AROMAS, AND ESSENCES 91

Table 6-2. (Continued)


USP FCC

Orange Cold Pressed Oil


Aldehydes (as % decanal) 1.2-2.5 1.2-2.5
Optical rotation ( + degrees) 94-99 94-99
Refractive index (200C) 1.472-1.474 1.472-1.474
Specific gravity 0.842-0.846 0.842-0.846
UV absorption (315 nm) ~0.130 (Cal) ~0.130 (Cal)
~0.240 (Flor) ~0.240 (Flor)
Evaporative residue ~43 mg/3 ml none
Orange Bitter Cold Pressed Oil
Aldehydes (as % decanal) none 0.5-1.0
Optical rotation ( + degrees) none 88-98
Refractive index (20°C) none 1.472-1.476
Specific gravity none 0.845-0.851
Evaporative residue ( % ) none 2-5
Orange Distilled Oil
Aldehydes (as % decanal) none 1.0-2.5
Optical rotation ( + degrees) none 94-99
Refractive index (20°C) none 1.471-1.474
Specific gravity none 0.840-0.844
UV absorption (315 nm) none :$;0.01

Grapefruit Cold Pressed Oil


Optical rotation ( + degrees) none 91-96
Refractive index (20°C) none 1.475-1.478
Specific gravity none 0.848-0.856
Evaporative residue ( % ) none 5-10
Tangerine Cold Pressed Oil* (Dancy and closely related varieties)
Aldehydes (as % decanal) none 0.8-1.9
Optical rotation ( + degrees) none 88-96
Refractive index (20°C) none 1.473-1.476
Specific gravity none 0.844-0.854
Evaporative Residue ( % ) none 2.3-5.8

Mandarin Cold Pressed Oil* (Citrus reticulata Blanco var. Mandarin)


Aldehydes (as % decanal) none 0.4-1.8
Optical rotation ( + degrees) none 68-78
Refractive index (20°C) none 1.473-1.477
Specific gravity none 0.847-0.853
Evaporative residue ( % ) none 2-5
* Tangerine and mandarin oils referto essentially the same fruit because Dancy tangerines are of the same species,
C. reticulata, and there is no variety known as "mandarin" in the C. reticulata species (see Chapter 13).
92 CITRUS JUICE CHARACTERISTICS

Polarizer 1 Polarizer 2

Monochromatic
Light
.~ .. -'~-l>
EB CD
Unpolarized Plane Polarized
(])
Rotated
Light Light Light
Fig. 6-4. Measurement of the optical rotation of citrus oils. The first polarizer polarizes the light,
and the oil rotates the light. The second polarizer can be rotated to detect the degree of rotation.

where R is the observed optical rotation in degrees, a is the specific optical


rotation, I is the length of the sample cell in decimeters, and c is the concen-
tration difference between the enantiomers in g / ml.
Limonene, the primary component of citrus oils, occurs in enantiomeric pairs,
but only the dextrorotatory enantiomer (d-limonene) occurs in citrus oils. The
optical activity of d-limonene allows its measurement in citrus oils. Pure
d-limonene has an optical rotation of + 125.6° (20 0 e) using a sodium D line
as the monochromatic light source. In citrus oils, the optical rotation that is
observed ranges from +75 0 to + 100° and constitutes a fair measure of the
d-limonene content in the oil. It should be remembered the citrus oils contain
components other than d-limonene that are optically active and may affect the
optical rotation. However, this effect is believed to be small and is generally
ignored by the industry. Also, most other optically active components of citrus
oils generally occur as racemic mixtures, or mixtures containing both enantio-
mers, which result in no significant net rotation of light.
The purpose of measuring the d-limonene content in citrus oils is to estimate
adulteration of the oils by using d-limonene from noncitrus sources. Also, folded
oils can be characterized by the d-limonene content by polarimetry. Even though
the Scott method also can be used to measure the d-limonene content, polar-
imetry is a much quicker and easier method. The optical rotation, which gen-
erally will decrease with fruit maturity, can be measured by the following pro-
cedure.
CITRUS OILS. AROMAS. AND ESSENCES 93

Determination of Optical Rotation

Equipment and Supplies

• Polarimeter accurate to ±O.I ° to ±0.5°. (Homemade polarimeters that


meet these requirements can be made at much less cost than commercial
instruments. )
• 1 dm sample cell if not included with polarimeter.
• Temperature bath and thermometer.
• Sodium lamp or soft yellow lamp.

Procedure

1. Most commercial polarimeters are preset to zero rotation when no sample


is present. Polarimeters can be calibrated by filling the sample cell with
alcohol or water and using the deviation from zero to correct the final
rotation reading of the sample.
2. The oil sample is warmed to 25°C with a temperature bath and thermom-
eter.
3. The sample cell is rinsed a few times with the oil that is to be analyzed,
and then the cell is filled with the oil. One should make sure the cell is
clean, especially the optical surfaces.
4. The cell is put into the polarimeter with the operator viewing the light
source through both polarizers, with the sample cell aligned between them.
One should rotate the second polarizer until the light source appears the
darkest. This should be done with great care. The polarizer should always
be rotated to the right, with the angular rotation read to the nearest degree.
5. Generally temperature corrections are not made with optical rotation mea-
surements of citrus oils. For orange and grapefruit oils, 0.22 ° can be
added or subtracted per degree centigrade above or below 25°C, and for
lemon oils 0.14° can be similarly added or subtracted from the reading
(Kesterson, Hendrickson, and Braddock 1971).
6. The final rotational reading usually is rounded off to the nearest degree if
temperature corrections are applied.

Refractive Index

The principles behind measurement of the refractive index were discussed in


Chapter 2. The refractive index scale and the Brix scale measure essentially the
same physical parameter. It is redundant to perform a refractive index check as
well as an optical rotation measurement because they measure essentially the
94 CITRUS JUICE CHARACTERISTICS

same thing, the estimated d-limonene content of the oil. However, it would be
very difficult to adulterate citrus oils with a component that had both the same
optical rotation properties and the same optical density properties as d-limo-
nene. Both tests are relatively quick and easy, so both are worthwhile if adul-
teration is a concern. Pure d-limonene has a refractive index of 1.4727 (20°C),
and the refractive index of citrus oils ranges from 1.4720 to 1.4740 (20°C).
Most processing plants already possess a refractometer for Brix measurements,
making the refractive index of citrus oils an even easier parameter to define. In
dry years the refractive index will increase with maturity. The following pro-
cedure can be used.

Determination of Refractive Index

Equipment and Supplies

• Refractometer that can read in units of refractive index.


• Dropper or plastic stirring rod to apply oil to the refractometer.
• Light source (soft yellow) if not included with the refractometer.
• Temperature bath or circulator with thennometer if not included with the
refractometer.

Procedure

1. Carefully clean the prism of the refractometer with water or alcohol, and
dry it with tissue paper.
2. Using the dropper or plastic stirring rod, apply a few milliliters of the
sample to the prism so that it is completely covered. Care should be taken
that no hard or abrasive object comes into contact with the prism.
3. For indirect scales, adjust the shadow to the center ofthe cross hairs, and
read the refractive index on the corresponding scale. For direct scales,
read the scale where it intersects the shadow.
4. It is recommended that all samples be measured at 20°C using a temper-
ature bath and thennometer. However, if corrections are necessary, adjust
the refractive index for orange oil by adding or subtracting 0.00045/ ° C,
and for lemon oil by adding or subtracting 0.00046/ °C if the temperature
is above or below 20°C (Kesterson, Hendrickson, and Braddock 1971).

Specific Gravity

The specific gravity is the density of the material divided by the density of water
at the same temperature. This test also is redundant if used with the refractive
index and the optical rotation in estimating the d-limonene content of citrus oils
CITRUS OILS, AROMAS, AND ESSENCES 95

and the general composition. Again, however, the greater the variety of tests
perfonned, the greater the chance is of detecting adulteration. The specific grav-
ity of d-limonene is 0.8419 (21°C), compared to that of citrus oils which ranges
from 0.842 to 0.881. In determining the specific gravity, a pycnometer com-
monly is used to measure a certain volume of the oil that, along with the oil
net weight, can be used to determine the specific gravity of the oil. The specific
gravity generally will increase with fruit maturity.

Determination of Specific Gravity

Equipment and Supplies

• Pycnometer or beaker and volumetric pipette ( 10 ml or 25 ml).


• Laboratory balance.
• Temperature bath and thermometer.

Procedure

1. Rinse the pycnometer with a few portions of the oil that is to be analyzed,
and fill it with the oil without putting the cap on the pycnometer; or place
about 50 ml of the oil into a beaker.
2. Place the pycnometer or beaker in a temperature bath, and warm it to
20°C.
3. Place the cap on the pycnometer and wipe the excess oil from the exterior
until it is clean and dry; or pipette 10 or 25 ml of the oil into a clean dry
beaker. Weigh the pycnometer or beaker immediately, using the lab bal-
ance to ± 1 mg.
4. Discard the sample, and clean and dry the pycnometer or beaker and re-
weigh it. Subtract the tare weight to get the sample net weight.
5. Repeat the procedure using distilled water. Divide the density of the sam-
ple (gjml) by the density of distilled water (gjml) to get the specific
gravity. The density of the water need not be determined each time. A
standard value of 0.998203 (200C) can be used instead for the density of
water, based on a water density of exactly 1 at 3.98°C.
6. Temperature corrections, if necessary, can be made by adding or subtract-
ing 0.00078 (0.00077 for lemon oil) for each centigrade degree above or
below 20°C (Kesterson, Hendrickson, and Braddock, 1971).

Aldehydes

Unlike the optical rotation, refractive index, and specific gravity, measurement
of the aldehyde level in citrus oils is a direct measure of the flavor quality of
96 CITRUS JUICE CHARACTERISTICS

those oils. For this reason, aldehyde measurements probably are the major qual-
ity parameter used in the marketing of these oils. Even though other oil con-
stituents contribute significantly to the organoleptic characteristics, the alde-
hydes are considered the major contributor. In lemon oils the most abundant
aldehyde is citral, which is actually the cis-trans mixture of neral and geranial
and occurs at levels of about 2 to 4 % in the oil. The most abundant aldehyde
in other citrus oils is decanal, with levels ranging about 0.8 to 2.0% in the oil.
Aldehyde analyses thus are based upon the citral or decanal equivalent of al-
dehydes.
There are several ways to measure the aldehyde content of citrus oils, in-
cluding the Kebler method (Kebler 1921), the Kirsten modification of the Ke-
bIer method (Kirsten 1955), and the N-hydroxy benzene sulfonamide (or HBS)
colorimetric method (Petrus, Dougherty, and Wolford 1970), as well as several
forms of the hydroxylamine hydrochloride method (J. o/the AOAC 1953; Carter
1981). The fastest, safest, and easiest method is that of Petrus, Dougherty, and
Wolford (1970). Hydroxylamine hydrochloride is added to the oil and reacts
with the aldehyde groups as follows:

0 N-OH
II II
(NH 3 OH)+Cl- + RCH ~ RCH + HCI (6-13 )
hydroxylamine an aldehyde an oxime hydrochloric
hydrochloride acid

The resulting acid can be determined by titration with a base.


Aldehyde levels generally increase as the season progresses. Also, wet
weather will have a tendency to increase the level of aldehydes in citrus oils.
Fruit stored for a long period oftime generally will have lower aldehyde levels.
The following procedure can be used for aldehyde determination.

Determination of Oil Aldehydes

Equipment and Supplies

• 0.5N hydroxylamine hydrochloride (34.75 g of hydroxylamine hydrochlo-


ride dissolved in 40 ml warm water and filled to the mark of a I-liter
volumetric flask with isopropyl alcohol; adjust the pH of the solution to
3.5, and store it in the refrigerator).
• Setup shown in Fig. 3-8.
• 30-minute timer.
• Laboratory balance.
• 50 ml graduated cylinder.
CITRUS OILS. AROMAS. AND ESSENCES 97

Procedure

1. Weigh about 5 g of the oil to be analyzed into the beaker shown in Fig.
3-8. Record the exact weight.
2. Add 35 ml of the 0.5N hydroxylamine hydrochloride solution to the flask
using the graduated cylinder. Stir the mixture for exactly 30 minutes.
3. Using the setup in Fig. 3-8, titrate with 0.1562N NaOH solution to a pH
endpoint of 3.5.
4. Calculate the % aldehyde using:

at M(ml titrated)(0.1562N)(1Iiter/1000 ml)lOO%


ro aId = --~------~~~--~~--~------~----- (6-14 )
(g of sample)

where M is the molecular weight of the citral for lemon oils (152.23
g/mole) or for decanal for other citrus oils (156.27 g/mole).

Evaporative Residue

The residue left after evaporation of the volatile components of oil products has
a tendency to stabilize the oil toward oxidation, one of the main causes of oil
quality deterioration. For this reason, the amount of evaporative residue can
serve as an estimate of the oxidative stability of the oil, which may be of oc-
casional interest. The evaporative residue will generally increase with fruit ma-
turity as well as with storage time of the fruit before processing. The following
procedure can be used.

Determination of Evaporative Residue

Equipment and Supplies

• 100 ml Pyrex evaporating dish or equivalent.


• Steam bath or equivalent.
• Desiccator.
• Laboratory balance to ± 0.001 g.
• Bunsen burner (optional).
• Oven (optional).

Procedure

1. Using the bunsen burner or steam bath, heat the evaporating dish; then
dry and cool it in a desiccator for about 30 minutes.
98 CITRUS JUICE CHARACTERISTICS

2. Immediately weigh the dried evaporating dish as a tare weight.


3. Place 5 g (record the exact weight) of the oil into the dish, and heat it on
a steam bath for 5 hours (6 hours for lime oils). The USP procedure
requires orange oils to be heated in an oven at 105°C for an additional 2
hours (The United States Pharmacopeia 1975).
4. Cool the dish with the sample at room temperature in a dessicator, and
reweigh it.
5. The % evaporative residue can be calculated from:

%ER = (g residue)( 100 % ) / (g sample) (6-15 )

Ultraviolet Absorption

Organic compounds that possess double bonds characteristically have electronic


energy levels that correspond to the energy of ultraviolet light, so that these
compounds absorb light in the UV region. Absorption peaks generally are very
broad, making it difficult to use UV absorption as a definitive means of differ-
entiating chemical structures. However, like many of the previous tests for cit-
rus oils, UV absorption can be useful in conjunction with other tests in esti-
mating general oil quality, detecting adulteration, and helping to differentiate
between oil varieties (Kesterson, Hendrickson, and Braddock 1971). Lemon
and lime oils have UV absorption peaks around 315 nm. Grapefruit oils have
two peaks, one around 318 nm and one around 268 nm. Orange oils have a
peak around 330 nm, and tangerine oils have two peaks, at about 330 nm and
318 nm. The intensities ofthese peaks have been used as a general guide to the
quality of the oils, and the USP and FCC standards both include UV absorption
parameters. The intensity of the main absorption peak is determined by means
of the following procedure.

Determination of UV Absorption

Equipment and Supplies

• UV spectrophotometer with a 1 cm cell and graph paper or printout.


• Laboratory balance.
• 100 ml volumetric flask.
• 100+ ml isopropyl alcohol.

Procedure

1. Add 0.250 g of oil to the 100 ml volumetric flask, fill it to the mark with
isopropyl alcohol, and mix the solution.
CITRUS OILS. AROMAS. AND ESSENCES 99

2. Rinse and fill the 1 cm cell of the spectrophotometer, and measure the
absorbance between 260 nm and 400 nm at intervals of at least 5 nm to
within 12 nm of the peak. Then read the absorbance at intervals of at least
3 nm three times, and then at 1 nm intervals until 5 nm beyond the peak
maximum. Thereafter absorbance readings should be made at least every
10 nm.
3. Draw a tangent to the areas of minimum absorbance. Drop a vertical line
from the main peak maximum to the tangent line, and determine the dif-
ference in absorbance that this CD line represents (absorbance at C at the
peak minus absorbance at D or the tangent line).
4. If a sample is used that is not exactly 0.250 g, a weighted ratio can be
applied to the CD value. For example, if a 0.255 g sample is used, you
should make the following calculation:

(CD value observed)(0.250 g)/(0.255 g) CD value (6-16)

QUESTIONS

1. What imparts the majority of the flavor to citrus juices next to sugars
and acids?
2. What is the major constituent of citrus oils and at about what percent?
3. What compounds characterize grapefruit oil and tangerine oil?
4. What terpene (besides d-limonene) is found in lemon and lime oils?
5. What contribution does d-limonene make to citrus flavor?
6. What four compounds have been used to duplicate up to 87 % of fresh
orange juice flavor?
7. What are the basic principles behind the Scott method of oil analysis?
8. Why is the methyl orange indicator effective in the Scott method?
9. Why is a bromide-bromate salt solution used in the Scott method rather
than a straight bromine solution?
10. Can any condenser be used in the Scott method? Why?
11. How do you determine the end of the distillation in the Scott method,
and why?
12. What is the purpose of the HCI in the Scott method?
13. What are the industrial ranges of oil in commercial orange juices?
14. What is the difference between citrus oils, aromas, and folded oils?
15. What is "winterizing," and why is it performed?
16. Is it possible to directly distill citrus oils out of aqueous solutions?
17. What declaration must appear on citrus juice labels if citrus oils or aro-
mas are added?
18. What is the purpose of determining the optical rotation, refractive index,
and specific gravity of citrus oils?
100 CITRUS JUICE CHARACTERISTICS

19. What are the purposes of measuring the evaporative residue, ultraviolet
absorption, and aldehydes in citrus oils?
20. What is the best way to determine the quality of citrus oils and aromas?

PROBLEMS

1. If you titrate the distillate of several juice samples using the Scott method, what are
the % oils if the following quantities of the bromide-bromate solution are used?

ml bromide-bromate solution
1.67
2.72
3.11
4.76
6.01

2. What is the average oil in a blend consisting of the following blend components?

Lot # Gallons Brix Lb Sol/Gal % Oil


250 60.9 6.576 0.029
2 1675 58.7 6.259 0.005
3 1497 64.2 7.021 0.011
4 902 65.6 7.221 O.oI8
5 3676 59.9 6.423 0.015

3. Suppose that you wanted to increase the oil level in the above blend to 0.020% oil.
How much oil would you need to add?
4. Suppose that in the above blend you want to add 2.5 ml of oil flavor enhancer per
gallon of concentrate. How much would you want to add?
5. In the above blend, suppose that you wanted to add the flavor enhancer determined
in the previous problem but not to exceed 0.020% in the final blend according to
specification. What average oil level must the blend have before the addition of the
oil?
6. In comparing the answers in problems 2 and 5, we see that one of the blend com-
ponents must be changed in order to meet the 0.020% oil specification and allow
for the flavor enhancer. Suppose we could replace blend component 3 with the same
amount of 64.9°Brix concentrate with an oil level of 0.003 %. Would this solve the
problem?
7. Suppose that in the above blend you eliminate lot 5 and increase the volume of lot
2 to 3000 gallons. Would this solve the problem stated in problem 6?
8. What would be the oil extraction efficiency in the manufacture of cold pressed oils
if you titrated 4.40 ml for a heavy discharge from the desludger sample, using the
Scott method and the procedure outlined in the chapter, and 25.52 ml for a sample
from the inbound oil slurry? Would this efficiency be acceptable according to in-
formation in the chapter?
CITRUS OILS, AROMAS, AND ESSENCES 101

9. What % oil would there be in the oil emulsion discharge from the de-
sludger in a cold pressed orange oil operation if 1.984 g of oil were analyzed with
18.46 ml titrated, using the Scott method according to the procedures explained in
the chapter? According to information in the chapter, would this be an acceptable
level of efficiency?
10. In the aldehyde determination for lemon oil, suppose you weighed 4.568 g of the
oil and titrated it with 6.16 ml of O.1562N NaOH according to the procedure in the
chapter. What would the % aldehyde be, and would this be good or poor quality
oil?

REFERENCES
Ahmed, E. M., Dennison, R. A., and Shaw, P. E. 1978. Effect of selected oil and essence volatile
components on flavor quality of pumpout orange juice, 1. Agric. Food Chern., 26, 368-372.
Carter, B. 1981. Private communication. Ventura Coastal Corp.
Food Chemicals Codex, 1981. National Academy Press, Washington, D.C., 140, 168, 169, 170,
172,209,210,319.
Johnson, J. D. and Vora, J. D. 1983. Natural citrus essences, Food Tech., 12,92-93.
1953.1. of the AOAC, 119.
Kebler, 1921. 1. of the A.O.A.C., 4,474.
Kesterson, J. W., Hendrickson, R., and Braddock, R. J. 1971. Florida Citrus Oils, Bulletin 749
(technical). University of Florida, Gainesville, Fla., 24-27, 114-127.
Kirsten, 1955.1. of the A.O.A.C., 38, 738.
Petrus, D. R., Dougherty, M. H., and Wolford, R. W. 1970. A quantitative total aldehydes test
useful in evaluating and blending citrus essences and concentrated citrus products, 1. Agric. Food
Chem., 18,908-910.
Shaw, P. E. 1977. Essential oils. In Citrus Science and Technology Vol. I, Steven Nagy, Philip
Shaw, and Matthew Veldhuis, eds. The AVI Publishing Company, Inc., Westport, Conn., 430-
435.
Scott, W. C. and Veldhuis, M. K. 1966. Rapid estimation of recoverable oil in citrus juices by
bromate titration. J. of the A. O.A. c., 49, 628-633.
The United States Pharmacopeia 19th Revision, 1975. United States Pharmacopeial Convention,
Inc., Rockville, Md., 560, 563.
Chapter 7

Citrus Juice Pulp

Most juices, such as apple, grape, and berry juices, are preferred by consumers
in a filtered and clarified form. However, citrus juices are preferred in a pulpy
and opaque form. Most of the opaque nature of citrus juices is attributed to the
colloidal cloud material, which will be described in Chapter 8. The solid par-
ticles of the fruit that will eventually settle out, which are primarily juice sac
and membrane material, impart a turbidity or mouth-feel that characterizes cit-
rus juices as well as giving a natural appearance. This citrus pulp can be divided
into two main groups-sinking, or spindown, pulp and floating pulp.

SINKING PULP

Sinking or spindown pulp generally is made up of the smaller or finer pulp


particles that form a sediment on standing because of juice saturation and/or
because they have slightly higher densities than that of the juice itself. The
major contributions of sinking pulp to citrus juice quality include contributing
to an opaque appearance and increasing the juice turbidity or mouth-feel. This
sediment is readily visible in glasspack or clear pack containers of single-strength
juices. Even though this pulp imparts a desirable mouth-feel to the juice, it may
impart an undesirable sludge appearance in clear containers. This problem has
been overcome in part by using opaque containers or using wraparound labels
at the level of the sediment on clear containers. Clear containers have the ad-
vantage of portraying the brilliant natural color of citrus juices even though a
proper package design on an opaque container can enhance product appeal as
well.
Although the precise amount of sinking pulp is elusive, the following indus-
trially accepted method of measuring the % pulp can be used for routine quality
control. This procedure is somewhat empirical in nature. The diameter and the
speed of the centrifuge along with the duration of centrifuging can dramatically
affect the results. For this reason, standards have been set regarding speed ver-
sus centrifuge diameter and time of centrifuging. Also, the temperature may

102

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
CITRUS JUICE PULP 103

affect the results. In order to see how these parameters affect a particular juice,
it is recommended that tests be done that vary the speed, duration, and temper-
ature used in the procedure.

Determination of Spin down Pulp

Equipment and Supplies

• Lab centrifuge.
• Tachometer.
• Two 50 ml conical centrifuge tubes. (Clear plastic tubes are the safest and
easiest to use.)
• Temperature bath and thermometer.

Procedure

1. Using the temperature bath and thermometer, bring the 11.8 °Brix juice
sample to 78°F (26°C).
2. Pour the temperature-adjusted juice into a clean and dry 50 ml centrifuge
tube with mixing to the 50 ml mark.
3. Put the tube into the centrifuge, along with another tube filled with another
sample or water to 50 ml on the opposite side to balance the load. More
than two samples can be analyzed at once, depending on the capacity of
the centrifuge. However, samples should be properly balanced in the cen-
trifuge. Place the tubes so that the graduations are facing the direction of
rotation. This will allow an average reading of the pulp directly on the
graduations if the surface of the pulp is uneven.
4. Using the tachometer, bring the rpm to 1500 for a centrifuge measuring
II! inches from the bottom of one centrifuge tube to the bottom of the
other on the opposite side when both tubes are extended in the horizontal
position. For centrifuges with diameters that are different from II! inches,
the following equation can be used to determine the rpm needed to exert
the same centrifugal force on the sample:

rpm = 1500 .../11.5/ d (7-1 )

For example, a centrifuge measuring 12.4 inches in diameter as described


above would require an rpm value of:

1500 .../11.5/12.4 = 1445 rpm

5. Centrifuge at the proper rpm for 10 minutes.


104 CITRUS JUICE CHARACTERISTICS

6. After the centrifuge comes to a complete stop, read the pulp level on the
graduation on the centrifuge tube halfway between the highest and lowest
levels of the separated pulp sediment. If the graduations are hard to see,
use a felt-tip pen to color the raised portions of the graduations.
7. The % pulp is found from:

% pulp = (rnl pulp)(100%)/50 rnl sample (7-2)

The USDA grade standards can be found in Table 7-1. The industrial range
for orange juices is generally 8 to 12 % pulp. Grapefruit juice usually has about
2 % less pulp than orange juices have.
Pulp levels can be controlled to some extent through control of the finishing
pressure used just after extraction. Higher finisher pressures will generally re-
sult in higher pulp levels. Finishing pressures can be monitored by % pulp
measurements. If the % pulp is consistently running high, the pressure can be
lowered, and vice versa. The chapter on statistics (Chapter 23) can be used to
define how many consecutive high or low pulp levels determine a nonrandom
effect. High finisher pressures often mean higher juice yields, but juice quality
may suffer, especially in the early part of the season. Excess loss of juice yields
can be estimated by examining the moisture content of the pulp expelled by the
finisher. If it is too wet, too much juice is being lost with the pulp, and the
finisher pressure should be increased, and vice versa. A more exact way to
determine the juice content in expelled pulp is to perform a quick fiber test on
it. This test is, again, somewhat empirical but less so than the spindown pulp
procedure.

Quick Fiber Test

Equipment and Supplies

• Mechanical shaking screen (20 mesh) with drain pan.


• Large serving spoon.
• I-liter beaker.
• Magnetic stirrer.
• Lab balance or triple beam balance.
• 250 rnl graduated cylinder.

Procedure

1. Weigh 200 g of well-mixed pulp into a I-liter beaker using a large serving
spoon. Add 200 g of water and stir for I minute, let the mixture sit for 3
minutes, and then stir it for another 1 minute.
CITRUS JUICE PULP 105

Table 7-1. USDA grade standards for maximum free and suspended
pulp levels in citrus juices.
Grade A Grade B
Grapefruit Juice (48FR 9/12/8321,52.1226-52.1227)
Grapefruit juice 10 15
Grapefruit juice from concentrate 10 15
Frozen concentrated grapefruit
juice (sweetened) 10 15
Grapefruit and Orange Juice (6FR 11/1172, 52.1289) 12 18

Tangerine Juice (2FR 7/1/69,52.2931-52.2941)


Canned tangerine juice 7 10

2. Pour the contents of the beaker into the shaker screen and shake it for 3
minutes.
3. Weigh the liquid from the drain pan. The grams of liquid is a measure of
the juice content of the pulp. Optimum values depend on the commercial
machinery used and the manufacturing objective. High plant juice yields
mean high pulp levels and perhaps some loss in flavor quality, and vice
versa.
Industrial ranges are classified into three categories: tight ( < 150 g liquid),
moderate (150-180 g liquid), and loose (180-200 g liquid). In California it is
difficult to get quick fiber pulp measurements of less than 180, with 160 being
the standard target value. In Florida the quick fiber usually ranges from 90 to
140 g liquid.
The physical condition of the fruit and the variety will also have an effect on
the pulp level. Fruit has been known not only to break down and go soft after
peak maturity, but to do so during certain times of the early and mid seasons
as well. This often causes sudden shifts in pulp levels. If more than one variety
is being run, the varieties will most likely be at different stages of maturity, in
addition to differing in physical composition. Therefore, it is necessary to closely
monitor and adjust finisher pressures. For all these reasons, quality control per-
sonnel need to monitor pulp levels, juice yield, and juice quality in maintaining
the ideal finisher pressure. It should be noted that if pulp washing is being done
and added back on-line in accordance with federal standards of identity for
100% juice products, juice yields may become less important because juice lost
to the pulp expelled by finishers will be recovered in the pulp wash operation.

Processing Effects on Juice Pulp

Another consideration that is important to the pulp quality of citrus juices con-
cerns the changes that take place in the pulp during processing. The spindown
106 CITRUS JUICE CHARACTERISTICS

pulp of the juice leaving the finisher needs to be about 12 to 20% for it to be 8
to 12 % in the final 60 0 Brix concentrate. The reason for this is that the heat
applied in pasteurization and evaporation operations, as well as the chopping
action of pumps and the juice itself, induces a degree of breakdown in the pulp
particles that results in lower pulp levels after processing. Such breakdown can
be illustrated by considering the change in the pulp level in freshly extracted
juice before and after evaporation to 60 to 65°Brix. A rule of thumb is that for
each effect in the evaporator (E), the final pulp level in the concentrate (PI)
can be found from the pulp level of the freshly extracted juice (P), by using
the following equation:

PI = P (0.6973 - 0.0265E) (7-3 )

If the juice were reconstituted and reevaporated, E would be twice the number
of effects used in the evaporation, and so on. Citrus juices are rarely reconsti-
tuted and reevaporated more than once, if at all. This step is sometimes taken
to remove contaminates such as potassium citrate crystals or burnt pulp parti-
cles, to produce low-pulp products, or to debitter citrus concentrates.
It should be kept in mind that the above equation gives only approximate
results. The nature of the pulp and the empirical nature of the procedure for
measuring the pulp make it difficult to predict precise results. For example, if
the pulp level of the juice coming out of the finisher is 17 %, and it is concen-
trated to 60 0 Brix using a three-effect evaporator, the expected approximate pulp
level in the final concentrate is:

(17 % )( 0.6973 - 0.0265 (3)) = 10.5 % pulp

If this concentrate were for some reason reconstituted to lZOBrix and reevap-
orated to the same concentration in the same evaporator, the pulp level in the
second concentrate would be:

(17%)(0.6973 - 0.0265(6)) = 9.2% pulp

In normal juice processing, the finisher can be adjusted by monitoring the


pulp levels in the final concentrates. However, in the manufacturing of low-
pulp products, changes in pulp levels with evaporation become more important.

lOW-Pulp Juices

The pulp in citrus juices sometimes presents a problem for citrus processors and
their customers. The pulpy nature of the juices requires greater space between
plate heat exchangers in pasteurizers, chillers, and evaporators, not to mention
CITRUS JUICE PULP 107

nozzles in fillers, filters, and other machinery having restricted spaces that is
commonly used to process juice. The use of natural juices in various drinks is
increasing in popularity, with efforts to increase the health appeal of many bev-
erages. Also, low-pulp juices can be evaporated to higher Brix levels because
of lower viscosities that can save on storing and shipping costs. Moreover,
many dairies and other nonjuice processors are processing juices with equip-
ment designed for milk and other nonpulp products. The plugging of such
equipment has prompted many users to seek citrus juices with lower pulp levels.
Once a piece of machinery becomes a site for pulp collection, microbial spoil-
age can easily set in, as well as pulp burning in pasteurizers, not to mention the
restriction or stoppage of product flow. The increased use of ion exchange and
adsorption resins for acid reduction and debittering also has increased the de-
mand for depulping technology.
Where pulp specifications exist, predictions of final pulp levels are necessary
to control the operation of the industrial centrifuge. By using the pulp levels
desired in the final concentrate, the pulp levels required before evaporation can
be estimated, and from these values the required pulp levels before centrifu-
gation can be determined. If freshly extracted juice were to be centrifuged and
concentrated to make low-pulp products, Equation 7-3 could be used to deter-
mine the needed P value from the PI specification. However, if reconstituted
juice were to be used, Equation 7-3 would pose problems because centrifugation
takes place between the first and the second evaporations. To estimate the cen-
trifuge pulp levels needed before evaporation based on final pulp specifications,
the following alternate form of Equation 7-3 can be used:

(7-4 )

For freshly extracted juice a factor of 1.619 for k can be used, and for re-
constituted juice a factor of 1.189 has been used for a three-effect evaporator.
It should be noted that the number of effects of the evaporator is not used in
Equation 7-4 for lack of data. Because each processing system is different, good
record keeping should help you to determine the exact factors for your system.
For example, if a final pulp specification in 60 0 Brix concentrate were 2.0 to
3.0% pulp, we would want to shoot for 2.5% pulp. Using Equation 7-4, we
would want to shoot for 4.0% pulp coming out of the centrifuge for freshly
extracted juice and 3.0% pulp for reconstituted juice. Again, flow rates can be
adjusted to target these levels. Because centrifugation is a fairly rapid process,
pulp tests are best done continuously during depulping. Part of the operation of
most centrifuges is the periodic opening of the inner bowl in order to discharge
the collected heavy layer, or pulp in this case. The length of time that the bowl
is open and the length of time between bowl openings affect not only the pulp
level of the outbound juice but the amount of juice lost with the expulsion of
108 CITRUS JUICE CHARACTERISTICS

the pulp. Optimum flush cycles should be determined in order to have no more
than 10% loss of juice soluble solids, and thereafter the pulp levels are best
controlled by adjusting the flow rates through the centrifuge. The expelled pulp
can be added back downstream, collected, or added to other products in order
to minimize the loss of juice soluble solids.
In light ofthe fact that juice pulp is heterogeneous and amorphous in nature,
difficulty in predicting the exact nature and level of pulp in citrus juices should
be expected. The control of pulp in juices has been described as more an art
than a science, and periodic deviations in expected results should be considered
normal. Depulped juice is characteristically less viscous and can be concen-
trated to higher levels than conventional juices.

Blending of Pulp Levels

The blending of juices to meet pulp specifications may be of interest at times,


especially in the manufacture of low-pulp concentrates. Lots that do not meet
specification can be blended to specification by using the following equations,
which are similar to Equations 6-5, 6-7, and 6-8. The average pulp level for a
blend can be found as follows:

P = VjPjS j + V2P2S 2 + V3P3S3 + ... + VnPnSn (7-5)


VjSj + V2 S2 + V3S 3 + ... + VnSn

where P is the final average pulp level and Vn, P n, and Sn are the volumes, pulp
levels, and the pounds of solids per gallon of the various components of the
blend. As before, if the Brix levels of all the components are similar, the S
values can be eliminated from the equation. If the final pulp level is too high
or too low, a lot with a different pulp level can be substituted, or the amount
of a particular lot can be varied to get the desired pulp level. If the first lot is
substituted, the required pulp level of the new component needed to achieve a
certain final pulp level can be calculated by using the following:

(7-6)

If the volume of lot 1 is to be varied, the required volume to achieve a certain


final pulp level can be found as follows:

S2V2(Pj - P2) + S3 V3(Pj - P 3 ) + ... + SnVn(Pj - P n)


Vj = (7-7)
PjSj(l - Pj/Pj)

In blending low-pulp juices, care should be taken not to use uncentrifuged


juices to bring up the pulp levels because the higher-pulp juices contain larger
CITRUS JUICE PULP 109

pulp particles that may cause problems for low-pulp users even though the
spindown pulp levels are within specifications.
As an example of pulp blending, suppose that we wanted to blend the fol-
lowing components:

Lot 3 Gallons Brix Sol/Gal % Pulp


1 567 60.5 6.505 1.6
2 432 59.6 6.382 2.7
3 167 65.2 7.164 3.7
4 546 62.0 6.712 2.0
5 321 61.3 6.615 4.2

By using Equation 7-5, the final average pulp of this blend can be calculated as
follows:

567(6.505)1.6 + 432(6.382)2.7 + 167(7.164)3.7


+ 546(6.712)2.0 + 321(6.615)4.2 5 1
567(6.505) + 432(6.382) + 167(7.164) + 546(6.712) = 2. % pu p
+ 321(6.615)

This would fit the 2.0 to 3.0% pulp specification mentioned in the last section.
Suppose, however, that 2.8 % pulp was the desired pulp level. In order to
meet this specification, lot 1 could be substituted for a lot with a pulp level
determined as follows by using Equation 7-6:

432(6.382)(2.8 - 2.7) + 167(7.164)(2.8 - 3.7)


+ 546(6.712)(2.8 - 2.0) + 321(6.615)(2.8 - 4.2)
2.8 + )
567(6.505
= 2.6% pulp in lot 1

If, instead of exchanging lot 1 for another lot, you wanted to change the amount
of lot 1 to achieve the 2.8 % final pulp level in the blend, Equation 7-7 could
be used as follows:

432(6.382)(2.8 - 2.7) + 167(7.164)(2.8 - 3.7) + 546(6.712)


(2.8 - 2.0) + 321(6.615)(2.8 - 4.2)
108 gal
1.6(6.505)(1 - 2.8/1.6)

Again, such equations are easily programmed into computers or program-


mable calculators. You may notice that the equations for adjusting the pulp
levels in juice blends are identical to many of the equations used to adjust the
oil in citrus blends. Much of the same computer logic and programming can be
, '0 CITRUS JUICE CHARACTERISTICS

used for both. A flow chart that can be used to adjust pulp levels in citrus juice
blends is shown in Fig. 7-1. An example of the use of this flow chart can be
found in the GWBASIC program found in Appendix B. A similar HP-41C pro-
gram can be found in Appendix C.

JUICE SACS OR FLOATING PULP

Juice sacs refer to the coarse membrane material that is screened from the juice
during juice finishing operations. Citrus juices generally go through two stages
of finishing prior to evaporation. The reason for this is to prevent coarse pulp
from sticking to heated surfaces in the evaporator with resultant burning or the
formation of brown or black flakes in the juice. Coarse pulp particles also may
clog or become entrapped in the evaporator, thus restricting flow and inducing
the same type of burning. The pulp that is removed can be washed with water
in order to leach out additional juice solids to make pulp wash juice. Instead of
being washed, the juice sacs can be frozen or dried. The latter products usually
are referred to as commercial juice sacs and can be added back to juices after
evaporation to provide floating pulp or a fresh juice appearance and mouth-feel.
Juice sac material also can be used as an extender or texturizer in other food
products.

Frozen Juice Sacs

Juice sacs generally require pasteurization in order to reduce microbial activity


and, more important, to deactivate pectinase enzymes that can induce gelation
and cloud loss, which are of concern when the juice sacs are to be used in citrus
juices or concentrates. Because juice sac material, as it is expelled from juice
finishers, is viscous in nature, shell-in-tube type heat exchangers generally are
required for pasteurization. The juice sacs can be frozen at -10°F (-23°C)
in polyethylene bags inside 5-gallon cans during storage, or they can be frozen
with dry ice sprays and packaged in polyethylene bags in 5-gallon cardboard
boxes. Larger containers, such as 55-gallon drums, require longer freezing and
thawing times, which may result in the development of off colors, off flavors,
and/or spoilage as the frozen mass develops or thaws unevenly. The use of
choppers to break up frozen material can reduce the thawing times.

Dried Juice Sacs

Dried juice sacs can be made from washed pulp by using pulp expelled in pulp
wash operations as well as from pulp expelled from juice finishers. Dried juice
sacs are not usually added back to citrus juices because such actions generally
will violate standards of identity for 100% juice products. Juice sac material is
believed to be responsible for much of the air pollution in feedmill operations.
CITRUS JUICE PULP 111

Brix of Compo n (Bn) n


Vol. of Compo n (Vn) Z1 = ~ ViPiSPGi
% Pulp Compo n (Pn)t---+t i=1
Desired % Pulp (Pf) n
Z2 = ~ ViSPGi
i=1

EO 7-5 SAVE THE INPUT


Pavg = Z1/Z2 Vn, SPGn, and Pn

no
n
Z3 = ~ ViSPGi (Pavg - Pi)
i=2

EO 7-7
EO 7-8
Z3 PI = Pf + Z3N1 SPG 1

Fig. 7-1. A flow chart that can be used to program computers to calculate the average pulp and
pulp level adjustments in citrus juice blending.

If the juice sac material were dried separately, this pollution would be reduced
considerably. Unwashed juice sacs can be dried in foam mats or freeze-dried
under a vacuum. The latter method is qualitatively best but is the costliest to
perform. The sugar content of unwashed juice sacs produces a darker cara-
melized color than that of washed juice sacs upon drying. Washed juice sacs
112 CITRUS JUICE CHARACTERISTICS

can be dried in drum dryers or direct fire dryers. The final moisture content of
the dried sacs must be below 10 %. (See Chapter 21 for moisture tests on dried
citrus peels.) A third method of drying juice sacs involves the leaching of the
juice sacs with acetone. The resulting juice sacs are lighter in color and fluffier,
looking more like individual juice cells when reconstituted with water, com-
pared to juice sacs produced by the other drying methods.
Dried juice sacs can be milled to any consistency down to fine flour. The
common types are grits, flakes, and flour. Grits are milled to a mesh of -16 to
+30. Flakes are milled to pass through a -4-mesh sieve, and flour is milled
to pass through a 100-mesh screen.
The color of dried juice sacs may fade but is not an important quality param-
eter. Juice sac composition is illustrated in Table 7-2. Antioxidants may have
to be added to prevent off flavor development in the dried sacs. Ambient tem-
perature storage for longer than one year may result in weevil infestation.
The measurement of floating pulp in juices is a little less precise than the
measurement of spindown pulp. Screening of the pulp followed by weighing of
the larger screened pulp particles can provide for an estimate of the floating
pulp level. This method measures the floating pulp only and is somewhat com-
parable to the quick fiber test mentioned previously, but requires less costly
equipment, is more rapid, and thus is better suited to routine quality control.
The procedure is outlined below.

Determination of Floating Pulp or Juice Sacs

Equipment and Supplies

• 20-mesh sieve.
• Laboratory balance or triple beam balance.
• I-liter volumetric or Erlenmeyer flask.
• Stirring rod or spatula.

Table 7-2. Some characteristics of dried washed juice sacs


(Kesterson and Braddock 1973).
Parameter Orange Grapefruit
% Crude fiber 18.9
% Protein 9.0
% Ash 20.6
% Moisture 8-10 8-10
% Fat 1.2-2.1 0.7-0.8
Bulk density (lb/ft3 ) 9.3 9.3
Water holding capacity 10/1 to 13/1 14/1 to 15/1
Fat holding capacity 4/1 to 5/1 4/1 to 5/1
(Source: Food Technology 1973. 27(2): 50, 52, 54. Copyright © by the Institute of Food Technologists.)
CITRUS JUICE PULP 113

Procedure

1. Weigh 1 liter of well-mixed 11.8 °Brix juice into a I-liter flask while
swirling it so that the juice contains a representative amount of pulp.
2. While swirling, pour the juice through the 20-mesh sieve over a sink and
shake the screen until the pulp retained by the screen "balls up" and is
free of excess juice.
3. Carefully tum the ball with the spatula or stirring rod into one mass and
then onto the balance pan and weigh it. Disregard any slight amount of
pulp that may cling to the screen.
4. Divide the weight of the recovered pulp by the weight of the juice, and
multiply by 100% to get the % floating pulp. In Florida the floating pulp
is reported by use of the following:

(% floating pulp )( 7 .49) = g / 6 fi oz of FCO]


or:

(% floating pulp) ( 19.77) = g /64 fl oz carton juice

Pulp levels of 0.75 to 0.80% are ideal in most situations. This is equivalent to
roughly 4 gallons of juice sac material per 1000 gallons of single-strength juice.

PULP WASH

The pulp expelled from primary and secondary finishers contains about 80 %
juice. These juice solids can be recovered by washing and refinishing the pulp
several times. The resulting juice is commonly referred to as pulp wash or
water-extracted soluble orange or grapefruit solids (WESOS or WESGS). In the
first stage, or the first time that the juice pulp is washed and refinished, about
50% of the available juice from the expelled pulp can be recovered. If two
stages are used, 63 % of the available juice can be recovered, and if three stages
are used, 75 % of the available juice in the pulp can be recovered. A four-stage
system can recover up to 80% of the available juice from the pulp. More stages
than this generally do not recover enough juice to be economically feasible.
The efficiency of a pulp wash system depends on a balance of parameters in-
cluding the water-to-pulp ratio and the number of stages. Figure 7-2 shows the
results of a study performed by FMC using its equipment. As can be seen in
the figure, the ideal water-to-pulp ratio is between 1.5 and 2.0, with the number
of stages exceeding 3 to 4 contributing little to the % recovery of juice from
the pulp. If 100 lb of pulp can be produced per ton of fruit processed, a pulp
wash system can increase the juice yield by 5 to 8 lb of soluble solids/ton of
fruit. Usually 80 to 120 lb of soluble solids/ton can be obtained in normal juice
processing without pulp washing, depending on the time of year and the variety
114 CITRUS JUICE CHARACTERISTICS

R = 2.0

>-
a:
w 75
100
:
R = 1.0
>
0
0
w
a: 50
eft
R = 0.5
25
R = WATER
PULP

2 3 4 5 6 7
NUMBER OF STAGES
Fig. 7-2. The efficiency of an FMC pulp wash system as a function of the water-to-pulp ratio and
the number of stages (Ballentine and Ferguson 1989).

of fruit. This increase in yield due to pulp washing can represent a significant
increase in juice yield, especially when juice is in high demand.
Pulp wash juice generally is considered inferior to extracted juice in both
color and flavor. The quality control of pulp wash juice generally consists of
the measurement of limonin (see Chapter 10). The limonin content in pulp wash
juices is responsible for the major effect of pulp wash on citrus juice quality,
as pulp wash can contain as much as twice the limonin found in conventional
juices. Concerns over juice quality and excessive juice supplies have led to
restrictions on the use of pulp wash in 100% juice products. The federal stan-
dards of identity permit the adding of pulp wash on-line to freshly extracted
juice, but Florida law prohibits any adding of pulp wash to 100% juice prod-
ucts. In order to enforce this law, Florida requires the addition of a sodium
benzoate tracer to all pulp wash products made in the state so that detection of
their illegal use is easier. Florida also requires that drums of pulp wash be
clearly labeled and encircled by a 5-inch yellow band.
Pulp wash juice contains a greater amount of high molecular weight com-
pounds, such as pectin, which increase the viscosity of resulting concentrates.
The added viscosity can pose problems in conveyance during evaporation and
chilling, so enzymes sometimes are added during the first stage of pulp washing
to help break down the high molecular weight compounds. Thus these pectinase
or polygalactonase enzymes have a maximum amount of time to work to de-
crease the viscosity. Without enzyme treatment, concentrate levels of over
400Brix may present difficulty in the concentration of pure pulp wash juices.
An alternative enzyme treatment consists of enzyme addition to the final pulp
wash and holding the juice for about an hour at 115°F. The pulp wash may be
CITRUS JUICE PULP 115

pasteurized and/or centrifuged prior to evaporation if necessary. Centrifuged


and enzyme-treated pulp wash juice can be concentrated to 65°Brix. Again, the
state of Florida requires the addition of sodium benzoate as a tracer to detect
unauthorized use of pulp wash in lOO% citrus juice products, which is usually
done just prior to evaporation.
The most efficient multistage pulp wash system is a countercurrent one where
fresh water is used in the last stage and then is used in succeeding prior stages
until the first stage. This reduces the time needed for the juice in the pulp and
in the washing solution to equilibrate.
Pulp wash also is used as a carbohydrate source in drink bases and as a
clouding agent. Quality control tests sometimes used to measure the quality in
such products include % light transmission (ability to act as a clouding agent),
% spindown pulp (mouth-feel), diacetyl or plating (microbiological growth),
and viscosity (ability to reconstitute).

CORE WASH

Core wash is the same as pulp wash except that it is obtained from the core
material expelled from the orifice tubes in the FMC extractor. This core mate-
rial consists of much of the rag or membrane material and seeds formerly con-
tained inside the fruit. The rag and seed material is very high in limonin, and
successive stages of washing and finishing of this material can result in a juice
extremely high in limonin (up to three to five times more than in conventional
juices, depending on the variety and the time of the season). Core wash juice
is very opaque and is used as a clouding agent in drink bases. Core washing
methods generally employ gentle washing using fewer stages than in pulp wash-
ing and gentle treatment to avoid breaking the seeds and releasing large amounts
of limonin. Commercial debittering systems have successfully debittered such
juices, as explained in Chapter lO, with other characteristics remaining similar
to those of pulp wash concentrates.

QUESTIONS

1. What are the advantages and disadvantages of sinking or spindown pulp


in relation to juice quality?
2. If the pulp level is too low, should the finisher pressure be increased or
decreased?
3. What would be the effect on juice yield if the pulp level were too low?
4. What are some of the reasons why pulp levels change during processing?
5. What benefits would there be in manufacturing low-pulp juices? What
are the disadvantages?
6. How can the depulping efficiency be regulated in depulping operations?
116 CITRUS JUICE CHARACTERISTICS

7. What are the advantages and disadvantages of a pulp wash system?


8. What are some of the differences between sinking and floating pulp?
9. Besides using pulp wash in 100% juice products according to federal
standards, what are some other uses that may be possible for pulp wash
juice?
10. How could a quick fiber test be of use in pulp wash processing?

PROBLEMS

1. What speed, in rpm, should a lab centrifuge use if the distance from bottom to bottom
between two centrifuge tubes in the horizontal position in a lab centrifuge is 131
inches?
2. What is the % pulp in each of the following spindown pulp tests according to the
procedure in the text?
Ml Pulp in Tube

1.6
2.5
4.8
3.6
5.1

3. If the pulp level of freshly extracted juice is 19.3 %, what would be the expected
spindown pulp level after evaporation using a seven-effect evaporator? What would
be the expected pulp level if this same concentrate were reconstituted and reevapor-
ated a second time in the same evaporator?
4. If a customer wanted juice with a pulp level of 2.8 to 3.0%, what pulp level would
you want to shoot for coming out of the centrifuge using freshly extracted juice?
5. In blending pulp levels, what would be the final average pulp level using the follow-
ing blend components?

Lot # Drums Brix Sol/Gal % Pulp


5 60.2 6.464 3.6
2 19 60.1 6.450 1.0
3 6 59.8 6.409 0.4
4 8 60.4 6.491 2.8
5 15 59.6 6.382 2.3

6. In the above blend, suppose you want to exchange lot 5 for a lot with a pulp level
that would give a final pulp level of 2.0%. What is the required pulp level for this
new blend component, assuming the same Brix and volume for lot 5?
7. If the number of drums in lot 5 in problem 5 are to be changed to meet the 2.0
specification in the previous problem rather than substituting a new lot, what is the
required number of drums of lot 5?
8. What would be the % floating pulp in 1045 g of single-strength juice that yielded
8.6 g of screened pulp?
Chapter 8

Juice Cloud

In citrus juices, unlike other juices, an opaque nature is considered a desirable


characteristic. Citrus juice itself comes primarily from the juice cell food stor-
age vacuoles, where it exists in a clear cloudless form. As the juice cell is
ruptured during juice extraction, high molecular weight compounds from the
organelles and cytoplasm of the juice cell become suspended in the juice, along
with membrane and pectin material. This colloidal suspension, which gives
citrus juices its cloud, is comprised of about 30% proteins, 20% hesperidin,
15 % cellulose and hemicellulose, and 5 % pectin (Bennett 1987). The content
of the other 30% of the juice cloud remains a mystery.
Proteins come primarily from the organelles and cytoplasm in the juice cell,
such as the mitochondria. Semi soluble membrane material is believed to be
responsible for the cellulose and hemicellulose material in the cloud, in addition
to being a common component of citrus peel. Hesperidin remains in a soluble
form within the intact juice cell vacuole; however, juice extraction causes a
change to take place rendering it insoluble and inducing precipitation that con-
tributes to the juice cloud.
The suspended cloud and spindown pulp are closely related. It is believed
that the pulp breakdown discussed in the previous chapter contributes to the
suspended cloud material. It also has been shown that as pulp levels increase,
so does the amount of cloud material (Rouse, Atkins, and Huggart 1954).

PECTIN

Even though pectin comprises a small portion of the cloud material, and al-
though juice cloud stability can be achieved in its absence, the effect of pectin
on juice cloud stability is dramatic. The term "pectin" refers to a class of high
molecular weight compounds, with molecular weights of 100,000 to 200,000,
consisting of 150 to 1500 galacturonic acid units linked together via a (1 --+ 4)
glycoside bonds with side chains of rhamnose, arabinans, galactans, xylose,

117

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
118 CITRUS JUICE CHARACTERISTICS

o
I II
OCOH ••- - - - galacturonic
acid
Q~ OH 0 Co-CH 3

~W _ _ methoxy
group
OH~~O
~II
Fig. 8-1. Segment of a pectin mole-
cule showing the characteristic galac- OH~
turonic acid and esterified methoxy
groups. OH

and fucose (Stevens 1941). Many of the carboxyl groups are esterified with
methanol to form methoxy groups, as shown in Fig. 8-1. These methoxy groups
block many reactions, including polymerization or gelation; so the degree of
esterification (D. E.) is a measure of the gelling ability of the pectin or the grade
of pectin, and ranges from 1 to 100%. The grade also may be determined ac-
cording to the percentage of methoxy groups, from 0 to a maximum of 16.32 %.
See Chapter 20 for a more detailed description of commercial pectin recovery
and characteristics.

GELATION AND CLOUD LOSS

There are two basic types of reactions that result in gelation in citrus concen-
trates or cloud loss in single-strength citrus juices. One reaction is the reversible
acid- or base-catalyzed esterification of the carboxyl groups of the galacturonic
acid components of pectins, according to:

o o
II H+ orOH- II
CH 3 + R-COH • ~ R-COCH 3 + H 20 + Heat (8-1 )
H+ or OH-

The equilibrium of this reaction depends on many factors, including pH, water
content, heat, and secondary reactions. In the presence of sugars, under the
proper conditions, polymerization can occur in citrus concentrates, resulting in
gelation. Even though the methoxy groups themselves prevent such polymer-
ization, the reverse reaction in equation 8-1 allows it to occur. Such polymer-
ization is not common in citrus concentrates.
JUICE CLOUD 119

IOH

I
o
~
f:':\
OH

Q
II OH
OCO a ~ -08°~ OH
OH 0
II
~ -oc~
co-
OH~O~ 8
OOH

OH 0 OH
II
-oc O~
OH
O co - f:':\c
2+
OH~~ oII OH
OH 0 0
O ~O - f:':\c
2+ -oc I
OH~O\l ~ 0
Fig. 8-2. Calcium pectate structure
~OH
responsible for most gelation and cloud
loss in citrus juices.

A more common form of gelation occurs when there are sufficient gal act-
uronic acid groups to form pectates, which link together via divalent cations
such as calcium, as shown in Fig. 8-2. This can occur only if there are enough
deesterified carboxyl groups available. In freshly extracted citrus juices, the
D.E. values are usually over 50%. Levels below about 20% may be sufficient
to cause the formation of calcium pectates, which in tum results in gelation in
concentrates and cloud loss in single-strength juices. This precipitation in sin-
gle-strength juices seems to entrap or affect other cloud components as well,
resulting in total cloud loss. Also, the length of the pectic chain or the molecular
weight of the pectin affects the cloud stability. Juices with low molecular weight
pectins generally will not gel. If too much heat is used during lemon and lime
juice processing, the acid hydrolysis described in the reverse reaction of Equa-
tion 8-1 will occur (because these juices contain more acid than other citrus
juices), which will result in polymerization and/or calcium pectate formation
or gelation.

PECTINASE ENZYMES

Another type of deesterification that can lead to cloud loss and/or gelation
through calcium pectate formation results from the pectinase enzymes that nat-
urally occur in citrus juices. These enzymes, also referred to as pectin esterases
or pectin methylesterases, are the primary cause of gelation and cloud loss in
commercial juices. In order to prevent the removal of the methoxy groups by
this enzyme, heat treatment is used to deactivate or destroy the enzyme. In most
120 CITRUS JUICE CHARACTERISTICS

juices a temperature of 150°F (66°C) is generally sufficient for pasteurization;


but 190°F (88°C) or more for about 10 to 15 seconds is required to deactivate
most of the pectinase enzymes, with lemon and lime juices requiring only 165-
190°F (74-88°C) to deactivate the enzyme because of their higher acid con-
tent. Unpasteurized "fresh squeezed" juice products are easily recognized by
severe cloud separation, which may be partially overcome by opaque containers
or labels, or, as done in the food service industry, shaking the juice to disperse
the cloud before it is served to a customer. Heat treatment is the only commer-
cial way to prevent this cloud loss.
In monitoring the stability of juice cloud, several methods have been used.
Before 1952 the Stevens cloud test was extensively used (Rouse, Atkins, and
Huggart 1954), which involved the addition of excess pectin followed by a
period of incubation, generally a couple of days, and measurement of the vol-
ume of the clarified layer which resulted from enzymatic activity. Usually a
volume of 10 ml of clarified juice per 100 ml of single-strength juice represented
an unstable cloud. More rapid techniques have since been developed, which
are more conducive to routine quality control operations. These rapid tech-
niques center around the measurement of the rate of acid formation of the re-
verse reaction in Equation 8-1 or:

o 0
II ~;i~~~e II (8-2)
R-COCH 3 + H 20--R-COH + CH3 0H
acid

The rate of this reaction can be expressed in the form of a first-order rate law:

(volume titrated) (NaOH normality)


R = k(acid) (8-3 )
(reaction time) (sample volume)

where the rate R is expressed in terms of the acid concentration and the rate
constant k. The concentrations of other species, assuming a negligible effect on
the reaction rate, are incorporated in the rate constant. This equation suggests
that a measurement of the change of acid concentration or pH can be used as
an estimate of the reaction rate or the enzymatic activity. The absolute value of
R usually is expressed in standard scientific units. However, the enzymatic ac-
tivity, a relative value, is of interest here; so convenient units can be used to
calculate a final reaction rate, which can be expressed in arbitrary units estab-
lished by standard industrial methodology.
The change in pH of a citrus juice sample is difficult to detect with the small
amount of pectin naturally present in the juice. In order to speed up the reaction
JUICE CLOUD 121

or to render the pH change large enough to measure, excess pectin is added to


the juice sample. The pH of the juice is adjusted to near neutrality with a base;
and then either a standard amount of base is added and the time needed for the
enzymatically produced acid to restore the sample to the original pH is mea-
sured, or a standard pH is maintained and the amount of base needed to accom-
plish this is measured for a given period of time. It is important that a proper
balance of enzyme and pectin exist. Samples of 10 to 30 ml of single-strength
juice (or the equivalent weight of soluble solids) are commonly used with 40
to 100 ml of standard 1 % pectin solution. The final PEU (pectin esterase units),
or arbitrary reaction rate units, can be expressed in various units, including ml
NaOH at a certain normality per milliliter, gram, or pound soluble solids per
second or minute. Another novel method is to add methyl red pH indicator to
the pectin-juice mixture. A negative test occurs if the solution maintains color
for 30 minutes. In routine quality control, the least tedious method that pro-
duced an adequate positive/negative test follows. This PEU test is a pass/fail
test having little value in further refinement of the results.

PEU Test

Equipment and Supplies

• pH meter
• 10 ml volumetric pipette
• 100 ml beaker
• 250 ml beaker
• 50 ml graduated cylinder
• Temperature bath
• Two disposable Pasteur pipettes
• Graduated 1 ml pipette
• Stopwatch or timer
• Magnetic stirrer
• 1 % pectin-salt solution made by mixing 10 g of pectin and 15.3 g NaCI
in a one-liter container and filling it with distilled water. (Heat may be
needed to get the pectin into solution.)
• 2.0N NaOH (20 g NaOH in 250 ml distilled water) protected from at-
mospheric carbon dioxide and moisture. (See section on acid titrations in
Chapter 3.)
• 0.05N NaOH (32.0 m1 of 0.1562N NaOH mixed with 100 ml distilled
water) protected in the same way as the above basic solution.
122 CITRlJS JUICE CHARACTERISTICS

Procedure

1. Pipette 10 ml of single-strength juice (1l.8°Brix) into a 100 ml beaker.


2. Add 40 ml of 1 % pectin-salt solution to the sample using a 50 ml grad-
uated cylinder, and add a magnetic stirring bar.
3. Place the 100 ml beaker containing the sample inside a 250 ml beaker
containing enough water to insulate the inner 100 ml beaker and sample.
4. Warm the beakers in an 86°F (30°C) temperature bath until the sample
in the lOa ml beaker is at the temperature of the bath as measured by
the thermometer.
5. Place the beakers on a magnetic stirrer, along with a thermometer, and
insert a pH electrode as shown in Fig. 8-3.
6. While stirring and maintaining constant temperature, add 2.0N NaOH
solution until the pH is stable at 7.0, using a disposable Pasteur pipette.
7. Add 0.05N NaOH using a second Pasteur pipette until the pH is between
7.6 and 7.8, and record the exact pH.
8. Using a graduated 1 ml pipette, add exactly 0.10 ml of the 0.05N NaOH
solution and start and stopwatch or timer.
9. Record the time it takes to regain the pH recorded in step 7 above.
10. The rate of acid formation can be calculated in pectin esterase units as
follows:

PEU = (0.05NNaOH)(0.1O ml NaOH) (8-4)


( 10 ml sample) (minutes)

Thermome ter ~

I
250 ml beaker -+ - -
'"
L~ :(f)" :6':
pH meter

- ...
~
~ pH probe
100 ml beaker
water -e:.
F" I
pectin/juice sample
, I ,

Magnetic Stirrer ____ stop watch

Fig. 8-3. Setup for the recommended PEU determination.


JUICE CLOUD 123

where the minutes refers to the time it took to regain the pH recorded in
step 7. For example:

PEU - (0.05) (0.10) - 833 X 10- 5


- (10) (6.0) - .

Most juices processed in modem evaporators and pasteurizers have PEU val-
ues of 1 x 10- 6 to 1 X 10- 4 . Those with levels much higher than this are
susceptible to gelation and/or cloud loss, depending on pH, temperature, and
other related conditions. In routine operations, rather than having a maximum
allowable PEU level, it may be more convenient to have a minimum time in-
terval for the pH recorded in step 7 to be regained, such as 2.5 minutes. If the
recorded pH is regained in 2.5 minutes or less, the cloud should be considered
unstable, and further heat treatment should be applied. In the above process it
should be noted that with stirring of the sample during the timing of the pH
change, the incorporation of atmospheric CO 2 into the sample will result in
some drop in pH. However, this should not prevent the determination of a stable
or an unstable cloud test. It should be kept in mind, however, that even with
no enzyme activity the pH will drop because of this CO 2 effect.
It is possible to have a gelled or clarified citrus juice with low enzyme activity
because deesterification can take place prior to heat treatment. Hence, one
should be careful not to allow excess time between extraction and heat treat-
ment. Sometimes when a juice concentrate gels, measurement of the enzyme
activity is of little value because deesterification could have taken place prior
to heat treatment. In such a situation, direct measurement of gelation is in order.
For frozen concentrated orange juice (FCOJ) in 6 oz cans, the following guide
can be used in grading the degree of gel when it is poured out onto a tray at
room temperature:

#1 gel-Questionable whether gel is present or not.


#2 gel-Definite gel lumps.
#3 gel-Definite gel that holds to the shape of the can but breaks up partially
upon pouring.
#4 gel-Definite gel that retains the shape of the can upon pouring.

A #1 or #2 gel can usually be salvaged by reconstitution and centrifuging, but


a #3 or #4 gel usually cannot be salvaged and must be discarded.

VISCOSITY

Cloud and pulp material contribute strongly to the viscosity of citrus juices,
especially at high Brix levels. The cold temperatures required for storage and
124 CITRUS JUICE CHARACTERISTICS

shipping of these concentrates also add greatly to the viscosity. Excessively


viscous concentrates put a heavy burden on processing pumps, and viscosity is
usually the limiting factor in the degree of concentration of citrus juices. If the
viscosity can be reduced, higher concentration levels can be achieved with
greater savings in storage and shipping costs. However, the use of enzymes in
primary citrus products is not allowed in Florida.
The viscosity can be reduced by centrifugation and controlled enzyme treat-
ment, used to break down juice pulp and cloud material. Polygalacturonase has
been used for the latter purpose (Baker and Bruemer 1971); it cleaves primary
pectin chains between adjacent nonesterified carboxyl groups. This reaction,
which is carried out at 86°F (30°C), is terminated by heat treatment to deac-
tivate the enzyme. Enzyme addition is commonly used during the first stage of
pulp wash systems for the same purpose, and it also increases the total soluble
solids and thus the juice yield. Ultrasonic and irradiation treatments have also
been used to break down juice cloud and pulp in order to reduce the viscosity
of the concentrate (Berk 1964). Complete enzyme clarification sometimes is
desired for lemon and lime juices.

QUESTIONS

1. What is the source of most of the cloud material found in citrus cloud?
2. What is the relationship between cloud material and pulp?
3. What is the main cause of cloud loss or gelation in citrus products?
4. What role do pectinase enzymes play in cloud stability, and how can ge-
lation be prevented commercially?
5. Why is excess pectin added to juice samples in the PEU test?

PROBLEMS

1. Suppose that you open a drum of concentrate obtained from another processing plant
and notice a high viscosity. You take a sample and discover that the Brix is not
excessively high, but gel lumps are found. What is the gel number? Does this mean
that the concentrate must have a high PEU value? What can be done to correct the
situation?
2. What would be the PEU value, according to the procedure in this chapter, for a
sample that took 2 minutes and 23 seconds to return to the original pH? Would this
be considered cloud-stable juice?
3. What would be the PEU value of a juice sample that took 6 minutes and 10 seconds
to return to the original pH? Is this juice cloud stable?
4. Suppose you used 1.0 ml of 0.01562N NaOH in the procedure for 10 ml of sample,
and it took 28 minutes and 53 seconds to return to the original pH. What would be
the PEU value, and would this be considered stable juice cloud?
JUICE CLOUD 125

5. What would be the PEU value per gram of soluble solids per second using 0.5 ml of
0.0312NNaOH for 15 ml of sample (12.0oBrix) that took 25 minutes and 16 seconds
to return to the original pH? Would this be considered stable juice cloud?

REFERENCES

Baker, R. A. and Bruemer, J. H. 1971. Proc. Florida St. Hort. Soc., 84, 197.
Bennett, R. D. 1987. From presentation to the Citrus Products Technical Committee at the USDA
Fruit and Vegetable Laboratory, Pasadena, Calif., March 13, 1987.
Berk, Z. 1964. Food Tech., 18, 1811.
Rouse, A. H., Atkins, C. D., and Huggart, R. L. 1954. Effect of pulp quantity on chemical and
physical properties of citrus juices and concentrates, Food Tech., 8, 431-435.
Stevens, J. W. 1941. U.S. Patent 2,267,050, December 23, 1941.
Chapter 9

Color of Citrus Juices

The natural bright color of citrus juices has long been regarded as one of their
major qualitative advantages over other food products. Their carotenoidal pig-
mentation has been associated with the color of the sun, producing a bright and
cheerful effect that complements the sweet and tart flavors and pleasant aromas
of the juices. The yellow-to-orange-to-pink-to-red colors have been used exten-
sively in marketing through transparent packaging and the use of sliced fruit in
advertising. The USDA holds color equal to flavor in its quality scoring system,
an indication of the importance of color in the quality of commercial citrus
products.
The main carotenoids responsible for the orange color of orange and tanger-
ine juice are a-carotene, /3-carotene, zeta-antheraxanthin (yellowish), violax-
anthin (yellowish), /3-citraurin (reddish orange), and /3-cryptoxanthin (orange)
(Stewart 1980), with the red or pink color of the pigmented grapefruit juice
varieties due to the presence oflycopene (Khan and MacKinney 1953). The red
color in blood oranges and related varieties is due to the presence of anthocy-
anins (Chandler 1958).
In dry cooler Mediterranean climates, as in California, fruit pigmentation is
well developed. In hotter and/or more humid areas, such as Florida, the color-
ation appears more dilute. For this reason the measurement of juice color plays
a greater role in juice processing in Florida than it does in California.
Color enhancement can occur only through blending with juices of higher
coloration. The federal code permits the blending of up to 10% of tangerine
juice (Citrus reticulata) and its hybrids with orange juice while still allowing
the product to be called 100% orange juice, in an effort to enhance juices with
weak color.
Off colors due to Maillard oxidation (as a result of scorching or excessive
heat applied to concentrates over too long a time) detract from the color quality
of the juice and can result in lower color scores. Such browning reactions dull
the natural citrus color. However, off flavors from these reactions develop be-
fore the visible effect occurs and further render the juice inferior. Also, white

126

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
COLOR OF CITRUS JUICES 127

hesperidin flakes or brown or black flakes from evaporator bum are readily
visible in citrus juices and mar their appearance. See Chapter 18.

USDA COLOR SCORING

The USDA has established a standard for the grading of the colors of orange
juice using six plastic color tubes, 011 (lightest) to 016 (darkest). One-inch-
diameter plastic tubes matching these color standards can be obtained from a
licensed manufacturer (such as Fiper/Magnuson, P.O. Box 11427, Reno, Nev.
89510, 1-800-648-4737) or by contacting:

Processed Products Branch


Fruit and Vegetable Quality Division, AMS
U.S. Department of Agriculture
Washington, D.C. 20250
These tubes can be used for direct color comparisons or to calibrate approved
colorimeters. Like most colors, these tubes are sensitive to light and may fade
on prolonged exposure; so they should be stored in a dark place. The following
procedure should be observed in using the tubes for direct comparison to citrus
juices.

Color Tube Test


Equipment and Supplies

• USDA color tubes (011-016)


• 45 ° angle tube rack with dull gray background and space between each
standard tube for sample tube. (See Fig. 9-1.)
• One-inch-diameter screw-cap culture tube for juice samples.
• Standard light source of approximately 150 candles with a color tempera-
ture of 7500 ± 2000K or a Macbeth Color Box model EBA-220, which
approximately simulates daylight under a moderately overcast day. Sub-
dued northern daylight may be used if care is exercised to minimize the
effects of reflected light from colored objects. Ordinary incandescent or
fluorescent light is not satisfactory .
• 80°F temperature bath.
• Deaeration setup shown in Fig. 2-3.

Procedure

1. Deaerate the juice as explained in Chapter 2.


2. Place the reconstituted juice (1l.8°Brix) in a one-inch-diameter test tube,
and warm it to 80 ± 2°F (27 ± 1°C) in the temperature bath.
128 CITRUS JUICE CHARACTERISTICS

Light - 45 degree angle

Gray Background
Fig. 9-1. Proper rack arrangement for direct comparison of orange juice color with USDA stan-
dard color tubes.

3. Place the sample tube between the standard color tubes that are just lighter
than and darker than the sample tube .
4. Use Table 9-1 to determine the USDA color score. Table 9-2 gives the
corresponding USDA grade standards for citrus juices.

TRISTIMULUS TEST

The standard method of color scoring in the food industry recommended by the
International Committee of Illumination is based on the "standard observer"
or simulated standard eye and consists of three primary colors or filters, referred
to as X (amber), Y (green), and Z (blue). Table 9-3 correlates these parameters
with the wavelength of visible light usually associated with color.
In 1952 Hunter came up with a scheme that measured redness (a), yellow-
COLOR OF CITRUS JUICES 129

Table 9-1. USDA color scores from comparison with plastic USDA
color tube standards (C juice color). =
Frozen cone. Pasteurized Canned orange
orange juice, orange juice and juice and cone.
reduced acid, and orange juice from orange juice for Dehydrated
canned conc. concentrate manufacturing orange
orange juice juice
C> OJ! 40 40 40 40
012 < C < OJ! 40 40 40 40
C = 012 40 40 40 40
013 < C < 012 39 39 39 39
C = 013 39 39 39 39
014 < C < 013 38 38 38 38
C = or
slightly > 014 37 37 38 37
OJ5 < C < OJ4 36 36 37 36
C = OJ5 36* 36 37 36
016 < C < OJ5 35 36* 36 35
C =016 34 35 36* 34*
C < OJ6 33 or less 34 or less 35 or less 33 or less
*Limits for Grade A.

ness (b), and lightness (L), which can be depicted as shown in Fig. 9-2 (Hunter
1958). These Hunter parameters can be related to the tristimulus parameters
according to (Kramer and Twigg 1970):

L = 100 .JY (9-1 )


a = 175(1.20X - y)/.JY (9-2 )
b = 70(Y - 0.847Z)/.JY (9-3 )

The Hunter citrus colorimeter further simplifies the color measurement by mea-
suring the citrus redness (CR) and the citrus yellowness (CY), which are related
to the tristimulus parameters as follows:

CR = (1.277X - ~.213Z - 1) 200 (9-4 )

CY = 100 (1 - 0.847(Z/Y)) (9-5)

The Florida Department of Citrus adopted the Hunter D45 colorimeter as the
official method of color measurement, using the following procedure.
130 CITRUS JUICE CHARACTERISTICS

Table 9-2. USDA color grades for citrus juices. (No color standards
exist for concentrated grapefruit juice for manufacturing, dehydrated
grapefruit juice. tangerine juice or its hybrids, or any lemon or lime
juices.)
Grade A Grade B

Orange Juice (47FR 12/10/82, 52.1557)


Frozen concentrated orange juice 36-40 32-35
Canned concentrated orange juice 36-40 32-35
Reduced acid orange juice 36-40 32-35
Pasteurized orange juice 36-40* 32-35
Orange juice from concentrate 36-40* 32-35
Concentrated orange juice for
manufacturing 36-40 32-35
Canned orange juice 36-40 32-35
Dehydrated orange juice 34-40 33 or less

Grapefruit Juice (48FR 9/12/83,


52.1224,52.1226)

Grapefruit juice 18-20** 16-17***


Grapefruit juice from concentrate 18-20** 16-17***
Frozen concentrated grapefruit juice 18-20** 16-17***

Grapefruit and Orange Juice Blend


(6FR 11/1172, 52.1284, 52.1288)

Grapefruit and orange juice blend 18-20** 16-17***

'> OJ6.
'*Means color representative of juice from mature. well-ripened grapefruit; the juice may show fading and lack
luster.
"*Means juice may be slightly. but not materially, affected by scorching, oxidation, or caramelization.

Hunter Colorimeter Test

Equipment and Supplies

• Hunter D45 or D45D2 colorimeter or other approved colorimeter.


• Temperature bath (80°F or 27°e).
• Deaeration setup shown in Fig. 2-3.
• One-inch-diameter screw cap culture tube.
• USDA standard OJ4 color tube.
COLOR OF CITRUS JUICES 131

Table 9-3. Reflectance values for X, Y, Z of the standard observer at


various wavelengths from average daylight illumination (Kramer and
Twigg 1970).
Wavelength nm X Y Z
380 4 20
90 19 89
400 85 2 404
10 329 9 1570
20 1238 37 5949
30 2997 122 14,628
40 3975 262 19,938
450 3915 443 20,638
60 3362 694 19,299
70 2272 1058 14,972
80 1112 1618 9461
90 363 2358 5274
500 52 3401 2864
10 89 4833 1520
20 576 6462 712
30 1523 7934 388
40 2785 9149 195
550 4282 9832 86
60 5880 9841 39
70 7322 9147 20
80 8417 7992 16
90 8984 6627 10
600 8949 5316 7
10 8325 4176 2
20 7070 3153 2
30 5309 2190
40 3693 1443
650 2349 886
60 1361 504
70 708 259
80 369 134
90 171 62
700 82 29
10 39 14
20 19 6
30 8 3
40 4 2
750 2
60
70
132 CITRUS JUICE CHARACTERISTICS

L
100-white

yellow

b red

blue

-30 o 30
a

0- black
Fig. 9-2. Illustration of Hunter's color scheme based on the parameters a, b, and L.

Procedure

1. Reconstitute the juice to the following Brix values:


45°Brix FCOJ to 12.8°Brix
42°Brix FCOJ to 11.8°Brix
COJFM to 12.3°Brix
or to the standard 11.8°Brix as in other quality tests.
2. Deaerate the juice sample for at least 3 minutes using the procedure found
in Chapter 2.
3. Warm the sample in the temperature bath to 80 ± 2°F (27 ± 1°C) in the
one-inch-diameter culture tube.
4. The colorimeter should be kept on standby with the power connected at
all times. If the instrument is off, tum it on, and let it warm up for about
10 minutes.
5. Tum the sensitivity knob as far to the right as possible.
COLOR OF CITRUS JUICES 133

6. Standardize CR and CY with an OJ4 USDA color tube as indexed by the


instrument.
7. Place the culture tube containing the sample at the indexed position, and
read the CR and CY values. Orange juices yield CR values of 26 to 45
and CYvalues of 74 to 89.
8. Apply the CR and CY values to the nomograph in Fig. 9-3, or use the
following equation to calculate the equivalent color number ( CN):

CN = 0.165CR + 0.111 CY + 22.510 (9-6)

The Hunter D45D2 automatically calculates the color number.


9. The calculated color number then can be converted into the USDA color
score by using the information in Table 9-4 for the various types of orange
juices.

Other colorimeters have since been approved by the Agricultural Research


Service of the USDA in cooperation with the Florida Department of Citrus,
including the following:

• Minolta Chroma Meter IIIRejiectance/CRlOO-provided that the instru-


ment is equipped with an adapter for one-inch-diameter test tubes and is
calibrated by using an OJ4 color standard tube according to plans available
from the ARS. The color number then can be determined by using:

CN = 43.85 + 1.07X - 0.61Y - 2.74Z (9-7)

VISUAL
50
COLOR
POINTS
OJ2/40/~
45 OJ3/39 /~ ,-40.S

~'
/
Q __ / 38 / • 1 - 39.5
w 40 / I
a:
en
~
a: 35
OJ4/37
/
/~ /
,{38.S
t: /
0
OJS/36'~
/ /
,-37.S
30 / HCC
/ !. 36.5
, /
EQUIVALENT

25
~ " COLOR SCORE
70 85 90 95

Fig. 9-3. Nomograph for converting CR and CY values to USDA color scores.
134 CITRUS JUICE CHARACTERISTICS

Table 9-4. Conversions from color number to USDA color score


(Florida Dept. of Citrus 1975).
Pasteurized OJ Frozen conc. Conc. OJ and
Color and OJ from OJ and conc. conc. OJ for
number concentrate canned OJ manufacturing
32.5-33.4 33 33 35
33.5-34.4 34 34 36
34.5-35.4 35 36
34.5-34.9 35
35.0-36.4 36
35.5-36.4 36 37
36.5-37.4 37 37 38
37.5-38.4 38 38 38
38.5-39.4 39 39 39
39.5-40.4 40 40 40

• Macbeth Color-Eye Model 1500-provided that the instrument is equipped


with an adapter for one-inch-diameter test tubes, according to plans avail-
able from the ARS, and is calibrated by using a white tile. The color num-
ber then can be calculated by using:

eN = 39.35 + 1.74X - 1.28Y - 0.94Z (9-8)

• HunterLab LabScan Model LS-5100-provided that the instrument is


equipped with an adapter for one-inch-diameter test tubes, according to
plans available from the ARS, and is calibrated by using an OJ4 color
standard tube. The color number then can be calculated by using:

CN = 40.10 + 1.90X - 1.55Y - 1.45Z (9-9)

Table 9-4 can be used to convert these color numbers into USDA color scores.
There are no color grade standards for grapefruit juices or other citrus juices.
The Texas Citrus Exchange (U .S. Expressway 83 at Mayberry, Mission, Tex.
78572) has established a grapefruit color scoring system that may be of value
to other grapefruit juice processors. Pigmented citrus juices containing lycopene
(pink grapefruit) and anthocyanins (blood oranges) have a tendency to undergo
a color change during processing to a brownish or dull color. This color change
generally renders the juices inferior as processed products even through pig-
mented citrus fruits are said to be the most delicious. Decolorization of these
pigmented juices is the subject of ongoing research.
COLOR OF CITRUS JUICES 135

QUESTIONS

1. What main carotenoids are responsible for the colors observed in citrus
juices?
2. What is the difference between California and Florida orange juice color,
and why?
3. How much tangerine juice can be added to orange juice while it still may
be called 100% orange juice, and why is this done?
4. What processing problems can occur to mar or degrade the color appear-
ance of citrus juices?
5. What colorimeters are approved for measurement of the color of citrus
juices?

PROBLEMS

1. What would be the L, a, and b Hunter color parameters for orange juice reflecting
average daylight at a wavelength of 620 nm, which represents pure orange color?
2. What would be the CR and CY values for the light in problem 1, and how does this
compare to CR and CY values found from orange juice measurements?
3. What would be the USDA color score for FCOJ with a CR value of 34 and a CY
value of 78? What would be the USDA color score for COJFM with the same CR
and CY values?
4. What USDA score and grade would FCOJ have if it were slightly lighter in color
than an OJ5 USDA standard color tube?
5. What would be the color number and corresponding USDA color score and grade for
concentrated orange juice for manufacturing using the Minolta colorimeter if the
tristimulus values were X = 555, Y = 321, and Z = 148?

REFERENCES
Chandler, B. V. 1958. Anthocyanins of blood oranges, Nature, 182, 993.
Hunter, R. S. 1958. Photoelectric color difference meter, 1. Opt. Soc. Am., 48(12), 985-995.
Khan, M. U. D. and MacKinney. 1953. Carotenoids of grapefruit, Plant Physiol., 28, 550-552.
Kramer, A. and Twigg, B. A. 1970. Quality Control for the Food Industry Vol. I. The AVI Pub-
lishing Company, Inc., Westport, Conn., 28, 32.
Stewart, 1. 1980. Color as related to quality in citrus. In Citrus Nutrition and Quality, S. Nagy
and J. A. Attaway, eds. The American Chemical Society, Washington, D.C., 129-150.
Chapter 10

Bitterness in Citrus Juices

As mentioned in Chapter 4, taste is a four-dimensional phenomenon consisting


of sweet, sour, salty, and bitter sensations. Even though a single taste receptor
on the tongue can respond to three or four of these modalities, the taste sites
on the tongue can be divided up into: the filiform papillae on the front tip and
sides of the tongue, which are particularly sensitive to salty and sweet tastes;
the fungiform papillae on the middle and sides of the tongue, which are partic-
ularly sensitive to sour tastes; and the circumvallate papillae on the back of the
tongue, which are particularly sensitive to bitter tastes. A strong bitter taste is
a result of electrical stimuli of monopolar-monohydrophobic or bihydrophobic
contacts with the tongue receptor (Belitz et al. 1979). The bitter taste in foods
is sometimes a delayed reaction that "comes back" or forms an aftertaste that
can linger for long periods of time. Thus, when performing organoleptic anal-
ysis of citrus juices for bitterness, one should pay attention to poignant sensa-
tions on the back of the tongue and delayed responses. When one is tasting
more than one sample, crackers or some other tongue scrubber should be used
to remove the lingering bitterness of the previous sample.
In citrus juices, two compounds impart essentially all of the bitter taste: li-
monin and naringin. In some grapefruit juices, a degree of bitterness is some-
times desirable in order to contribute to a "wide awake" flavor along with the
sourness of the acids. However, most juices, especially orange juices, are known
for their sweetness. Bitterness thus is considered detrimental to quality in these
products.

NARINGIN

One class of compounds associated with citrus juices is the flavonoids, which
have the following characteristic molecular structure:

136

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
BITTERNESS IN CITRUS JUICES 137

R-O OH

OH 0
These flavonoids are differentiated from each other by the carbohydrate linkup,
R. In sweet oranges (Citrus sinensis (L.) Osbeck), as well as in most other
citrus species, the predominant flavonoid is the tasteless and odorless hesperi-
din. In grapefruit varieties (Citrus paradisi Macf.) the primary flavonoid is
naringin, a bitter principle. As with other flavonoids, naringin is primarily found
in the membranes and albedo of the fruit and contributes to the bitterness of
fresh fruit as well as to the juice. The taste threshold of naringin is about 50
ppm even though levels of about 500 ppm are considered ideal, and levels of
over 900 ppm can occur.
The naringin content can be measured in several ways (Ting and Rouseff
1986). However, the spectrophotometric Davis test is the method most com-
monly used. The Davis test involves the reaction of naringin, or any flavonoid,
with diethylene glycol in dilute alkali to the corresponding chalcone, which is
yellow in color. The reaction is as follows:

CH,oH CH,oH

~ ~~O
0 OH +HOCCOCCOHNaOH.I~ ~~OH
HO~ DEG H~
~ I~? OOH
H~
~~
OHO H~OHO
~~

NARINGIN CHALCONE
(yellow)

Davis Test for Naringin (Davis 1947)

Equipment and Supplies

• Spectrophotometer with necessary accessories.


• Six test tubes.
• Six 100 ml volumetric flasks.
• 0.1 ml pipette.
• 0.5 ml pipette.
• Centrifuge and accessories.
• 90% diethylene glycol (2,2'-dihydroxyethyl ether) (reagent grade) in
water.
138 CITRUS JUICE CHARACTERISTICS

• 4N sodium hydroxide.
• Graph paper and/or calculator.
• 200 mg naringin for standards in distilled water.
• 50 ml graduated cylinder.

Procedure

1. Centrifuge the juice sample, using the procedure for determining the %
pulp.
2. Add 10 ml of 90% diethylene glycol to a test tube along with 0.1 ml of
the centrifuged juice serum. Add 0.1 ml of the NaOH solution, mix the
solution, and let it stand for 10 minutes.
3. Measure the sample's absorbance on the spectrophotometer at 420 nm,
comparing it to a distilled water blank. It may be easier to measure the %
transmittance and convert it to absorbance by using:

Absorbance = log ( 100/ %T) (10-1 )

4. The naringin content can be found by comparing the absorbance to a graph


of absorbance versus naringin concentration values, C, or by calculation
using Beer's law:

Absorbance = kC (10-2 )

5. The standard graph or the factor k can be found from the following cali-
bration or standardization.

Calibration

1. Prepare a stock solution by dissolving 200 mg of naringin in 100 ml of


distilled water.
2. Make five standards by pipetting, or by using a graduated cylinder to
transfer, 5.0, 12.5, 25.0, 37.5, and 50.0 ml of the stock solution into
each of five 100 ml volumetric flasks, filling them to the mark to obtain
10,25, 50, 75, and 100 mg/ml standard solutions.
3. To each of five test tubes add 10 ml of the 90% diethylene glycol, and
then add 0.1 ml of each standard to separate glycol-containing test tubes.
4. Add 0.1 ml of the NaOH solution to each standard-containing test tube,
and after 15 minutes measure the absorbance at 420 nm using the spec-
trophotometer, or measure the % transmittance and convert that value to
absorbance using Equation 10-1.
5. Either plot the absorbance versus mg naringin /100 ml (10 mg /100 ml
of standard being equal to 100 ppm naringin in the juice sample, so that
BITTERNESS IN CITRUS JUICES 139

to get ppm one may multiply the corresponding mg naringin/100 ml by


10), or calculate the average value of k using Beer's law (Equation 10-2).
6. Another suggested approach is to use five times the concentrations of the
above chemicals and sample (Ting and Rouseff 1986).

Another method commonly used is high performance liquid chromatography


(HPLC), which can be used effectively to measure the levels of other flavonoids
separately. The benefit of HPLC analysis is that naringin can be differentiated
from other flavonoids. Usually this is not necessary because naringin predom-
inates in grapefruit juices.

HPlC Naringin Test (Fisher and Wheaton 1976)

Equipment and Supplies

• Isocratic or single pump HPLC system with UV detector and chart re-
corder. Gradient or multipump systems are useful when one is analyzing
for more than one flavonoid at one time. Integrators or computers linked
to the HPLC are helpful but not necessary.
• 20: 80 acetonitrile-water mobile phase.
• Lab centrifuge.
• Syringe filter (2 I-/m).
• 50 1-/1 HPLC syringe.
• Same naringin standards used in the Davis test.

Procedure

1. Centrifuge the reconstituted or single-strength juice ( 11.8 °Brix) by using


the procedure for the measurement of the % pulp.
2. Filter the supernatant with the syringe filter.
3. Inject 25 1-/1 of the filtered sample or standard into the HPLC system set
at 1. 5 ml / min; the UV detector should be set at 280 nm and 0.1 absor-
bance unit, full-scale range.
4. Elution times are about 12 to 16 minutes for naringin and 16 to 18 minutes
for hesperidin, depending on the CI8 column used.
5. Using 25 J-tl of the standards described in the Davis test, the mg of narin-
gin per unit peak height (usuaUy in cm) can be determined by averaging
as follows:

c~~ (Ni/P;) )/n = F (10-3 )


140 CITRUS JUICE CHARACTERISTICS

where N is the mg naringin in the five standards, n is the total number of


standards (five here), and F is the factor for calculating naringin levels.
P is the peak height.
6. A plot of N versus P can be used to compare with unknown juice samples,
or the factor F can be used to calculate the naringin concentrations (mg
naringin/1oo ml) by multiplying F times the peak height. The ppm of
naringin can be found from the mg of naringin /100 ml by multiplying by
10.

There are no USDA standards for naringin content in citrus juices. Naringin
bitterness is accounted for in flavor scores. However, Florida law (Official Rules
Affecting the Florida Citrus Industry 1975) requires grade A grapefruit juice to
have less than 600 ppm naringin and grade B juice to have less than 750 ppm
naringin.

LIMON IN

Limonin, which is the principal bitter component in most citrus juices, includ-
ing grapefruit juice, is a product of a series of reactions that originate in the
trunk of citrus trees (Hasegawa et al. 1986). These reactions generate a class
of compounds known as limonoids, which are similar to each other in chemical
structure and characteristics. The limonoid nomilin is formed in the trunk of the
tree and translocated to the fruit, where it is converted into several limonoids
including the tasteless limoninoate A-ring lactone, the open ring structure of
limonin. In most citrus varieties, this limonin precursor concentrates in the seeds
within mature citrus fruit. However, in some orange varieties, such as navel
oranges (Citrus sinensis (L.) Osbeck), the A-ring lactone remains in the neutral
environment of the juice cell cytoplasm or membrane. Upon the rupture of this
membrane during juice processing, the A-ring lactone encounters the acid en-
vironment of the juice, which gradually catalyzes the closing of the ring to form
limonin according to the following reversible reaction:

~o ~O
OH
COO-

L1MONIN A-RING LACTONE L1MONIN


(non-bitter) (bitter)
BITTERNESS IN CITRUS JUICES 141

The rate of this reaction is primarily heat-dependent, with some effect due to
the juice pH. At cold temperatures viscosity can also affect this reaction in high-
Brix concentrates. The rate of this reaction is slow enough that it does not affect
the quality of fresh fruit, which generally is consumed soon after it is cut.
However, navel juice that is stored overnight in a refrigerator will tum bitter if
it is from early or midseason fruit. Even though navel juice is considered substan-
dard because of this bitterness problem, the navel orange is excellent as a fresh
fruit. It has an early growing season, outstanding fresh flavor, and a low juice
content that makes it easy to eat as a fresh fruit. Because more money can be
made in the fresh markets than with processed products (up to 10 times as
much), both fruit variety and production are dominated by the fresh markets in
areas such as California where navel oranges can be grown of satisfactory qual-
ity. Such fresh market domination has left juice processors in such areas with
the dilemma of either selling the resulting bitter juice at a lower price or turning
to commercial debittering techniques.
Another problem associated with the delayed development of limonin has to
do with premature testing for limonin before development is complete. The rate
of limonin formation is affected primarily by acidity and heat, as mentioned
previously. Also, it has been shown that limonin solubilities range from 1 to
18 ppm in aqueous solutions containing 0 to 10% sucrose (Chandler 1971).
Pectin and other complex components of citrus juices increase this solubility,
but it is clear that high limonin levels (up to 30 ppm) can easily be affected by
the solubility equilibria of limonin in citrus juices. It also is safe to assume that
upon juice extraction not all the limonin in the juice cell membranes is leached
out into the juice at one time. The leaching has its own rate, which can affect
detectable limonin amounts during storage. Also, it is possible that continued
biochemical reactions may interfere with limonin levels, including formation
from precursors, limonin metabolism, and eqUilibria with aqueous-phase li-
monoid glucosides.
In the absence of a more thorough knowledge of these effects, a good rule of
thumb is that you should boil freshly extracted juice four minutes for every
expected ppm; reconstituted juices require about one minute of boiling for every
expected ppm. Overheating of juice has from time to time resulted in sudden
drops of limonin as well as Maillard abuse of the sample, and should be avoided.
Figure 10-1 shows some general behavior of the limonin levels in freshly ex-
tracted California Washington navel juice. From the figure it can be seen that
a significant amount of heat is required to completely develop limonin in freshly
extracted juices. Many observers have assumed that the heat applied during
normal juice processing is sufficient to fully develop the limonin in citrus juices.
However, it is common in California for early and midseason navel concen-
trates to develop significant amounts of limonin even after complete heat treat-
ment in evaporation and relatively long storage periods.
As mentioned previously, carbohydrates increase limonin solubility. This ef-
142 CITRUS JUICE CHARACTERISTICS

13


12 •
11

-
10

-
E
c. 9
C.
c: 8
c:
0
E 7
:J
6

5
4
3
2

0 200 400 600 BOD 1000 1200 1400


t (minutes)
Fig. 10-1. The development of limonin in freshly extracted Washington navel orange juice after
time t at the temperature given.

fect is a result of hydrogen bonding. Such complexing reactions also have been
shown to affect the ability of the tongue to detect limonin. Guadagni et al.
showed that increasing the sweetness of the juice decreases one's ability to taste
the limonin bitterness (Guadagni, Maier, and Turnbaugh 1974). Organic acids
also interfere with the detection of limonin by taste, primarily through pH ef-
fects. A pH of 3.8 has been shown to be the ideal pH for suppressing limonin
detection (Tatum and Berry 1973) (Maier et al. 1977).
Several methods have been developed to measure limonin levels in citrus
juices, including spectroscopy (Wilson and Crutchfield 1968), thin layer chro-
matography (TLC) (Tatum and Berry 1973), gas chromatography (GC) (Kruger
and Colter 1972), radio immunoassay (RIA) (Weiler and Mansell 1980), en-
zyme-linked immunoassay (EIA) (Jourdon et al. 1984), and high performance
liquid chromatography (HPLC) (Rouseff and Fisher 1980). The two most widely
used in commercial plants are EIA and HPLC; the EIA method has the advan-
tage of being able to analyze several samples simultaneously and thus is faster,
whereas the HPLC has the advantage of being more accurate and reliable.
BITTERNESS IN CITRUS JUICES 143

Enzyme-linked Immunoassay

EIA is based upon several reactions involving anti-limonin antibodies produced


in rabbits and limonin-alkaline phosphate tracer. The tracer is synthesized by
the manufacturer of EIA limonin test kits (Idetek, Inc., San Bruno, Calif.) by
refluxing limonin with aminooxy acetic acid to give limonin-7-0-carboxy-
methyl oxime, which then is coupled with the amino groups of the alkaline
phosphatase enzyme via carbodiimide to give a limonin-enzyme linked com-
pound. This tracer is mixed with a limonin standard or unknown juice sample
in a micro test tube, and the mixture then is pipetted into an antibody-coated
well and incubated. The free limonin and the limonin-linked enzyme tracer
compete for the fixed number of antibodies attached to the well's surface. The
more free limonin that exists from the juice or limonin standard, the less en-
zyme-linked limonin tracer there will be to react and become fixed to the im-
mobilized antibodies on the wall of the wells.
Of the other limonoids that are similar in chemical structure and character-
istics to limonin, only deoxylimonin reacts similarly to the antibodies and thus
can give artificially high limonin results. However, this limonoid occurs at lev-
els of less than 0.5 % of the limonin levels in citrus juices and generally should
not affect citrus limonin tests. Aqueous-phase limonin glucosides, on the other
hand, occur at levels as high as 500 ppm in citrus juices and have been found
to interfere with EIA results, giving artificially high limonin determinations.
This interference, failure to properly calibrate EIA test systems, and irrepro-
ducibility of results in juice samples analyzed at different Brix levels are be-
lieved to be the primary reasons for inconsistency between HPLC and EIA
determinations.
After incubation, the wells are washed free of excess nonbonded material.
Then the wells are filled withp-nitrophenyl phosphate, which acts as a substrate
for the limonin-linked enzyme conjugate. The intensity of the colored product
is directly proportional to the amount of enzyme-linked limonin bound to the
antibodies on the wall of the reaction well and inversely proportional to the
amount of dormant limonin displacing the active enzyme-linked limonin. In
other words, the lighter the color, or the less the absorbance or optical density,
the more limon in there is present.
EIA test kits require the use of standards for every test. Nonjuice limonin
standards are difficult to prepare because the complex components of the juice
give limonin its solubility. Juice limonin standards also often vary, as already
mentioned, making accurate calibration difficult. Idetek's test kit claims validity
in the 1 to 10 ppm limonin range, as higher limonin levels yield a curve instead
of a line in their Beer's Law calibration plot. This constraint poses a problem
for navel orange juice, which may contain as much as 30 ppm limonin. Idetek
suggests diluting the sample and calculating the equivalent limonin level for
11.8°Brix juice. This dilution places the sample under different limonin solu-
144 CITRUS JUICE CHARACTERISTICS

bility conditions, which can result in significant errors. The lower the Brix is,
the less soluble the limonin; and once the limonin crystallizes, it cannot be
detected by the Idetek method. In order to avoid these solubility problems, all
limonin analyses should be done with samples of at least 11.8°Brix. Higher-
Brix samples also upset the solubility equilibria and should be avoided as well.
When using standard solutions of limonin for calibration, one should check the
effect of the organic solvent used in the standard on the procedure. This can be
done by adding similar amounts of the pure solvent without limonin to a juice
sample and observing the calibration curve followed by using the standard with
the limonin. Generally, the more solvent that is used, the more distorted the
calibration will become. It is also recommended that when one is calibrating
the Idetek system, a standard should be added to a juice sample before analysis
rather than used directly. Instructions for the use of the Idetek kit are included
with it.

High Performance liquid Chromatography

HPLC has undergone dramatic development in the past several decades, having
become a major analytical tool in the food industry. It is possible to vary col-
umns, detectors, and mobile phase, and to make slight modification of the pro-
cedures, so that few compounds exist that cannot be detected by this method.
HPLC analysis can be divided into four main sections: sample preparation,
compound separation, detection, and calculation or display. Because orange
juice contains many insoluble and colloidal macromolecules and much partic-
ulate matter, sample preparation usually is mandatory to prevent column plug-
ging. This preparation can range from simple filtering to elaborate extractions
and preliminary separations.
Limonin is readily soluble in organic solvents, so the use of such solvents is
common in preliminary separations. The elimination of aqueous material sim-
plifies the HPLC procedure and provides for a cleaner chromatograph, void of
extraneous interfering peaks. Three organic solvents have a high solubilizing
power for limonin-acetone, acetonitrile, and chloroform; and chloroform is
the solvent of choice for several reasons. First, its immiscibility with aqueous
solutions makes it a strong extracter, whereas acetone and acetonitrile dissolve
in juice samples and are much weaker in pulling the limonin from the aqueous
solution. Of the three, chloroform is the most volatile, a property that facilitates
vacuum evaporation when chloroform extracts are concentrated to raise the li-
monin level so that it is high enough to detect. Also, acetonitrile and acetone
sometimes extract other compounds that interfere with limonin peaks. There are
three different ways in which the limonin can be extracted from the juice: one
way is to use a simple chloroform extraction; another is to use special diato-
maceous earth in a 60 ml coarse-porosity fritted disc funnel to extract the li-
BITTERNESS IN CITRUS JUICES 145

monin from a juice-diatamaceous earth cake using vacuum filtration; a third


method consists of the use of a C I8 "Sep-Pak" cartridge attached to a 10 ml
syringe. Whichever method is used, the final solution should be filtered prior
to injection into the HPLC system.
As with any other analytical technique, proper calibration is crucial to ac-
curate results. It is not too difficult to analyze each of the extractions above or
multiple extractions to ensure that all the limonin is being extracted. Using
diatomaceous earth (see procedure below), we found that the first extraction
removes 75% of the limonin, the second about 25%, the third about 5%, and
the fourth a trace, and the fifth gives no limon in peak. Analyzing juice samples
at various times of preheating will show how much boiling of the sample is
needed to fully develop the limonin. Also, analyzing the same sample at dif-
ferent Brix levels will clarify limonin solubility effects. Repeat analyses will
illustrate precision. Analysis of the same sample under different storage con-
ditions will reveal storage effects. All these influences may dramatically affect
limonin results and should be checked regardless of the procedure used.
For routine limonin determinations, a simple isocratic or single-pump system
usually suffices. Multiple pumps or gradient systems are useful when one wants
to look at several components at once that require different or changing mobile
phases. Cyano (CN) columns usually are used for normal phase limonin sepa-
rations because their intermediate polarity most closely matches that of limonin.
Reverse phase methods employing C I8 columns are used with the "Sep-Pak"
sample preparations mentioned above. Short precolumns can be used in addition
to or instead of regular columns to protect the longer more expensive analytical
columns or by themselves to shorten retention times. The solvent system used
in the determination must contain miscible components. The normal and reverse
phase mobile solutions commonly used contain solvents with a wide range of
polarity. The ratio of these components can be varied to resolve the limonin
peak. Degassing and filtering of the solvents helps to protect against column
plugging and/or spurious gas peaks that may interfere with limonin peaks.
The method of choice generally is ultraviolet detection. Limonin has an ab-
sorption maximum at 207 nm. However, many other compounds extracted with
limonin have significant absorption at this wavelength, causing a low signal-to-
noise ratio. For this reason, limonin HPLC determinations usually are per-
formed at higher wavelengths such as 215 or 220 nm. Because UV lamps have
a limited lifetime and can undergo degradation, monthly calibration of the HPLC
procedure is recommended. A good lamp can last indefinitely, but the usual
lifetime is about 200 hours of use. It is wise to keep a spare on hand so that
loss of a lamp will not interfere with quality control needs.
The means of displaying the detected limonin is very important. It can range
from a simple chart recorder to a sophisticated computer display. HPLC seldom
is used in routine quality control, so excessive expenditures may not be war-
ranted. For this reason, the author considers a simple chart recorder the most
'46 CITRUS JUICE CHARACTERISTICS

cost-effective device. Comparing sample peak heights to the peak heights of


standards gives acceptable results. However, chart recorder integration and
computer analysis are much more convenient to use if they are economically
feasible.
Even though HPLC is considered slower than the EIA method, many deter-
minations usually are not necessary in most quality control systems. If many
limonin determinations were required, we would recommend that both methods
be used, the HPLC to check accuracy and the EIA system to produce the bulk
of the determinations. The industry often refers to two limonin levels-the
HPLC value and the EIA value. In reality there should be only one, and proper
calibration should yield only a single value, which should lean definitively to-
ward the HPLC results. The following is a guideline for the development of an
HPLC procedure.

HPLC Limonin Determination

Equipment and Supplies

• Isocratic HPLC system, UV detector (207-230 nm), chart recorder, 25


em x 4.6 mm Zorbax CN column with a 5 cm x 4.6 mm Zorbax CN
precolumn for the normal phase or 22 mm x 2.1 mm C I8 column for the
reverse phase.
• HPLC solvent system consisting of ethylene glycol monomethyl ether,
2-propanol, and n-heptane (10: 15: 25 v Iv) or heptane, 2-propanol, and
methanol (11: 12: 2 v Iv) for the normal phase or acetonitrile, tetrahydro-
furan, and water (17.5 : 17.5 : 65 v I v) for the reverse phase (Shaw and
Wilson 1984).
• 20 p.l HPLC syringe.
• For normal phase separation, the setup shown in Fig. 10-2, including a 60
ml coarse-porosity fritted disc funnel connected to a rotary evaporator with
glass tubing, a heating source, about 30 ml diatomaceous earth (amorphous
diatomaceous silica and crystalline silica obtained from swimming pool
supply venders), and about 300 ml chloroform.
• For reverse phase separation, a C I8 "Sep-Pak" (Waters Associates, Mil-
ford, Mass.) attached to a 10 ml syringe containing a small piece of si-
lanized glass wool conditioned with about 2 rn1 acetonitrile followed by 5
rn1 water.
• 10 ml graduated cylinder.
• 10 rn1 pipette.
• Stirring rod.
• About 60 ml hexane (optional).
BITTERNESS IN CITRUS JUICES 147

Heat
Source

Fig. 10-2. Setup for sample preparation for normal phase HPLC limonin determination.

• 15 ml screw-cap test tube and 2 /-tm filter syringe (optional for the normal
phase) or a 0.45 /-tm nylon 66 Millipore filter for the reverse phase.
• Limonin chloroform standard (25 mg /100 ml).
• 1 ml graduated pipette or 0.1 ml autopipette.
• 25 ml pipette and extra 100 ml volumetric flask for reverse phase separa-
tion.

Procedure (Normal Phase)

1. Add about 30 ml of diatomaceous earth to the fritted disc funnel, pipette


10 ml of 11.8°Brix juice into the funnel, and mix the contents well with
a stirring rod. See Fig. 10-2.
2. Without removing the stirring rod, fill the funnel with hexane, stir it, and
vacuum-extract the hexane into the evaporation flask of the rotary evap-
orator. Discard the hexane extract. This step is done to remove extraneous
148 CITRUS JUICE CHARACTERISTICS

material that may interfere with the limonin peak. If there is no interfer-
ence, this step can be ignored.
3. Without removing the stirring rod, fill the funnel with chloroform, stir it,
and vacuum-extract the chloroform into the rotary evaporator, which is
already in motion with a heat source applied. A three-way stopcock, as
shown in Fig. 10-2 should be open during the extraction and closed when
one is adding new solve At and stirring.
4. Repeat step 3 four more times while concentrating the chloroform in the
rotary evaporator. Continue concentrating it until less than 2 ml of chlo-
roform remains in the evaporation flask. The rate of evaporation can be
enhanced by stronger vacuum, greater heat, and/or the use of refrigerated
coolant in the condenser. It is recommended that one use moderate heat,
compressed air, aspirated vacuum, and tap water in the condenser. Too
much heat results in hot glassware that is difficult to handle.
5. Remove the evaporation flask, rinse it with four or five 2 ml portions of
chloroform into a 10 ml graduated cylinder, and record the volume (ml
GC). Be careful not to lose any of the limonin-rich chloroform rinses.
6. Immediately filter the rinses with a syringe filter, place the chloroform
solution in a screw-cap test tube, and seal it.
7. Rinse the 20 1-'1 syringe several times with the chloroform extract, and
inject 151-'1 of the solution into the HPLC injector using the normal phase
mobile phase described above. Start the chart recorder (10 mV 5
mm/min), and inject the sample at the same time. The pump speed should
be 1.5 ml/min.
S. The peak height (P) can be combined with the ml GC, the density of the
sample, d (g/ml), and the pounds soluble solids/gal, S, in the following
equation:

limonin (ppm) = F( ml GC) P / dS (10-4 )

where F is a calibration factor. The Sand d factors are used to calculate


the limonin content in juice samples on an 11.soBrix juice basis. The d
and S values for 11.soBrix juice are 1.0446 g/ml and 1.029 lb sol/gal.
If the juice sample has a slightly different concentration, Equations 2-7
and 2-S should be used to calculate the d and S values. Figure 10-3 gives
an example of what the chromatograph should look like.

Procedure (Reverse Phase)

1. Pass 2.5 ml of 11.soBrix juice through a conditioned "Sep-Pak" car-


tridge followed by 2.5 ml of water.
2. Extract the limonin from the cartridge using 2.5 ml of acetonitrile, filter-
BITTERNESS IN CITRUS JUICES 149

o 2 4 6 8 10
Minutes
Fig. 10-3. HPLC chromatograph of limonin and nomilin peaks using the normal phase method.

ing through a 0.45 pm nylon 66 Millipore filter, place it in a screw-cap


test tube, and seal it.
3. Follow the procedure given above for the normal phase using 2.5 ml for
the ml GC and a 22 mm x 2.1 mm C I8 column and the reverse phase
mobile phase described above.

Calibration

1. Add 0.1, 0.3, 0.5, 0.8, and 1.0 ml of the standard to 10 ml each of 5
identical 11.8 °Brix juice samples for normal or reverse phase calibration,
and proceed with the analysis as explained above.
2. The pg limonin per unit of peak height h can be found as follows:

/ (0.025 g lim) (106 pg)(? ml std.)(l ml)(15 pI)


( 10-5)
pg h = (100 ml chlor)( 1 g)(? ml GC) (10 3 pl)( OP)

where OP is the difference in the peak height of the un spiked juice sample
compared to the spiked juice sample.
150 CITRUS JUICE CHARACTERISTICS

3. The average /1-g/h from the five standards can be used to calculate the
factor F used in Equation 10-5:

F = (/1-g/h)(1.029lb sol/gal @11.8°Brix) (10-6)


(15 /1-1 inject) (1 rn1 /1000 /1-1) (? ml juice sample)

5. In order to check the calibration, the factor calculated above can be used
in Equation 10-5 to determine the expected limonin levels of each of the
standard tests. This is done by first calculating the limonin level of the
unspikedjuice sample (L), using the average Fvalue from Equations 10-6
and 10-5. Then the expected limonin levels of the spiked samples can be
calculated:

E = (? rn1 std)Cs (I/? mljuice)(1/d)(106 /1-g/1 g) +L (10-7)

where Cs is the concentration of the standard (0.025 g limonin /100 ml,


the ml juice is 10 ml for the normal phase and 2.5 ml for the reverse
phase, and d is the density ofthe juice (1.0446 g/ml for 11.8°Brixjuice).
6. The expected limonin levels from Equation 10-7 and the measure limonin
levels from Equation 10-4 using the average F value are compared in the
sample calibration illustrated in Table 10-1. The validity of the calibration
can readily be seen by comparing the two sets of values.

A limonin determination can be performed in 30 to 40 minutes. The USDA


has no grade standards for limonin levels, even though bitterness is incorporated
into the flavor score. Florida law sets a maximum of 5.0 ppm limonin for Grade
A canned, chilled, and frozen concentrated grapefruit juices and a maximum of

Table 10-1. Calibration of the normal phase HPlC limonin


determination based on 11.8 0 Brix, assuming 10.0 ml GC for
each of the five spiked analyses and the unspiked analysis.
Peak ht. in Change in Expected
Sample chart units peak ht. /J-g/unit ppm lim ppm lim
Navel juice 1.65 -* -* 13.8 -*
+0.1 ml std. 1.93 0.28 0.13 16.2 16.2
+0.3 ml std. 2.55 0.90 0.13 21.4 21.0
+0.5 ml std. 3.10 1.45 0.13 26.0 25.8
+0.8 ml std. 4.03 2.38 0.13 33.7 32.9
+ 1.0 ml std. 4.50 2.85 0.13 37.7 37.7
Average = 0.13
F = 0.9
'Does not apply to unspiked sample.
BITTERNESS IN CITRUS JUICES 151

7.0 ppm limonin for Grade B (Florida Dept. of Citrus). These grade standards
apply to concentrate (not finished products) processed between December 2 and
July 31. They also apply to finished products processed from concentrate or
bulk single-strength juice between December 2 and July 31, provided that any
juice or concentrate blended with it that is processed between August 1 and
December 1 meets the permissible limits of limonin for the desired grade.

Limonin TLC Determinations

The principle of thin layer chromatography (TLC) determinations is similar to


that of HPLC. However, instead of using a packed column to separate the com-
ponents of a sample, the separation takes place on a flat silica-coated plate.
Instead of pumping an eluting solvent through a column, the eluting solvent
travels through the silica by capillary action. Instead of detecting the limonin
by means of a UV detector, the limonin is developed chemically to enable visual
comparison with standards. Most of the materials needed for TLC limonin anal-
ysis are available in most citrus laboratories with no need for major capital
investments; thus the major advantage of the method is its low cost. The main
disadvantages include the method's less objective visual comparison with stan-
dards and the somewhat tedious nature of the determination.
Several procedures exist for limonin TLC analysis. Juice samples can be
extracted with chloroform in a manner similar to that described for the HPLC
procedure or its equivalent, and the extractant can be spotted on the TLC plate
and eluted. Direct spotting of the juice onto the TLC plate has been shown to
be successful, but it requires more drying time on the plate compared to organic
extractants. Several elution solvents have been used, including: chloroform and
acetic acid in a 98: 1 ratio (Chandler and Kefford 1966); a top layer of toluene,
ethanol, distilled water, and glacial acetic acid in a 200: 40: 15: 1 ratio after
overnight standing (Hasegawa, Patel, and Snyder 1982), ethylacetate and cy-
clohexane in a 3: 2 ratio (Hasegawa 1980); and acetone elution followed by
elution with benzene, hexane, acetone, and acetic acid in a 65: 25: 10: 3 ratio
(Tatum and Berry 1973). (The last reference also contains a study of 16 other
solvent systems used for TLC analysis of limonin in citrus juices.) After elu-
tion, two main methods of development have been used. One consists of spray-
ing the dried plate with a 10% sulfuric acid solution in ethanol and heating it
to develop a dark colored spot. The other involves the use of Ehrlich's solution
(0.395 g p-dimethylamino-benzaldehyde and 0.789 g sulfuric acid in 50 ml
ethanol) and exposing the sprayed dried plate to chlorine gas, which can be
generated in a well-ventilated area by adding sulfuric acid to ammonium chlo-
ride. The result is a brownish limonin spot. Considering safety, speed, and
simplicity, the author recommends the following procedure.
152 CITRUS JUICE CHARACTERISTICS

TLC Limonin Determination (Tatum and Berry 1973)

Equipment and Supplies

• Silica-coated TLC plate approximately 12-14 cm x 8.5 cm.


• 50 J.l.1 syringe with fiat unbeveled tip.
• 10 J.l.1 syringe with fiat unbeveled tip.
• Wann air stream.
• Limonin standard solution (0.010 g limonin/100 ml in ethanol or aceto-
nitrile).
• TLC solvent tank with paper lining (second tank optional).
• Acetone for solvent tank to a depth of about ~ inch.
• Eluting solution for solvent tank to a depth of about ~ inch, consisting of
benzene, hexane, acetone, and acetic acid in a ratio of 65 : 22 : 10: 3 by
volume.
• 10% sulfuric acid solution.
• Chromist TLC sprayer.
• Oven to develop plate ( 125°C).
• UV light source (optional).
• Syringe filter ( 10 J.l.1).

Procedure

1. Filter the juice, using the syringe filter, and spot 25 J.l.1 of filtered single-
strength or reconstituted juice (11.8°Brix), using the 50 J.l.1 syringe, about
1 cm from the bottom of the TLC plate. Multiple samples can be ana-
lyzed at one time on wider plates. Spots should be about 1 cm from the
edge of the plate and/or 2 cm apart.
2. Dry the spot with a wann air stream, respot with another 25 J.l.1 sample
of the juice over the first spot, and redry the plate.
3. Using the 10 J.l.1 syringe, spot 1, 2, 3, 4, and 5 J.l.1 of the limonin standard
solution about 1 cm from the bottom and 2 cm apart on the TLC plate.
For estimated limonin levels over 10 ppm, spot 6, 8, 10, 12, and 14 J.l.1
of the standard instead.
4. Dry the TLC plate again with wann air for at least 1 minute. Incomplete
drying will result in streaked spots.
5. Place the plate in the solvent tank containing acetone with the liquid level
about halfway between the bottom of the plate and the spot. Elute until
the liquid level travels about 3 cm, remove the plate, and dry it. Uneven
liquid levels on the plate indicate insufficient drying of the sample spot.
6. Place the plate in a paper-lined solvent tank containing the benzene so-
lution, and elute to the top of the plate.
BITTERNESS IN CITRUS JUICES 153

7. Remove the plate, dry it, and repeat the elution two more times.
8. Spray the plate with the sulfuric acid solution, using the chromist sprayer,
until it is lightly wet.
9. Incubate the plate in the oven (125 °C) for 6 minutes, and then remove
and cool it.
10. The limonin spot will appear dark in color and rectangular in shape if it
was dried properly during sample preparation.
11. The unknown sample can be compared to the standards visually by view-
ing them against a light source from the back or glass side of the TLC
plate. They also can be viewed by using an ultraviolet light source under
the plate, in which case the spots appear reddish brown.
12. The limonin level can be determined by comparison with the closest
standard and multiplying the microliters of the standard by 2.

PROCESSING CONSIDERATIONS

Even though juice bitterness is induced naturally, processing can have an im-
portant effect on it. For example, it has been shown that ethylene gas, com-
monly used to degreen early-season fruit for the fresh markets, can trigger a
mechanism that reduces limonin levels (Maier, Brewster, and Hsu 1973). It has
been suggested that leaving fruit so treated in storage bins for as long as possible
will help to decrease the bitterness. Even so, early-season navel juices are usu-
ally too bitter for this precaution to have a significant effect on final juice qual-
ity.
Because both naringin and limonin enter the juice primarily from membrane
material in the fruit, extraction and finishing pressures and the length of time
that the juice is in contact with the membrane material can affect the degree of
bitterness of the resulting juice. Such variations are small, becoming important
only when the limonin and naringin levels are reduced through natural matu-
ration to levels close to the taste thresholds. Most juice extractors can be ad-
justed to give a soft or a hard squeeze, and finishers usually can be adjusted to
give a soft or a hard finish. In either case, hard extraction or finishing usually
results in greater bitterness and greater juice yield. Therefore, in the early sea-
son, extraction and finishing pressures should be set for hard squeezing, as it
gives greater yields, and the bitterness is too high for a soft squeeze to yield
good-quality juice anyway. Later in the season, when bitter taste thresholds are
approached, the squeeze should be changed to a softer squeeze in an effort to
produce a lesser or a nonbitter juice. Lesser or nonbitter juice products usually
bring in more than enough money to offset losses of yield due to softer squeezes.
Also, immediate centrifuging of the juice to remove naringin-Iaden pulp has
been shown to reduce naringin levels in grapefruit juices by as much as 10 to
20% (Berry and Tatum 1986).
1 54 CITRUS JUICE CHARACTERISTICS

The common units of bitter component levels, as mentioned previously, are


parts per million (ppm), a weight/weight parameter similar to the Brix. For this
reason, in blending limonin (or naringin) levels, equations similar to Equations
2-16 and 2-18 can be used. For example, suppose that we wanted to blend the
following lots:

Lot 3 Drums Bri.!: lb / gal ppm Limonin


5 65.1 10.983 8.1
2 10 60.2 10.737 16.2
3 4 59.8 10.717 10.5
4 3 61.7 10.811 3.6
5 8 62.4 10.846 4.7

The lb / gal can be found from the Brix by using Equation 2-8 or 2-10 or sucrose
density tables. We can find the final weighted average limonin level ofthe blend
by using the following:

( 10-8)

where Ln is the limonin level of component n in ppm, Dn is the density of


component n in lb / gal found from Equations 2-9 or 2-11 according to Brix,
and Vn is the volume of component n, in units of drums in the above example.
Substituting the data in the example into Equation 10-8 gives:

8.1(10.983)5 + 16.2(10.737)10 + 10.5(10.717)4 + 3.6(10.811)3


+ 4.7( 10.846)8
(10.983)5 + (10.737)10 + (10.717)4 + (10.811)3 + (10.846)8

= 9.7 ppm

This value is well over the 7 ppm taste threshold. Suppose you wanted to reduce
the number of drums of lot 2 so that the final blend would be at or below the
threshold. The number of drums of lot 2 needed for this could be calculated as
follows:

( 10-9)

where Lf is the desired finallimonin level in the blend.


BITTERNESS IN CITRUS JUICES 155

Using the above example gives:

5(10.983)(8.1 - 7.0) + 4(10.717)(10.5 - 7.0) + 3(10.811)(3.6 - 7.0)


+ 8(10.846)(4.7 - 7.0)
(10.737)(7.0 - 16.2)
= 1 drum

Therefore, if you use I drum of lot 2 instead of 10 drums, you will have a final
weighted average limon in level in the blend of exactly 7.0 ppm.
Rather than change the number of drums of lot 2, you may wish to exchange
lot 2 for the same number of drums with a lower limonin level in order to
achieve 7.0 ppm limonin in the blend. The limonin level needed in such a lot
can be calculated as follows:

(10-10)

which in the example gives:

5(10.983)(7.0 - 8.1) + 4(10.717)(7.0 - 10.5)


+ 3 (10.811 )(7.0 - 3.6) + 8( 10.846)(7.0 - 4.7)
7.0 +
(10.737)10

= 7.9 ppm limonin

Thus if the 10 drums of lot 2 at 16.2 ppm were exchanged for 10 drums of a
lot with 7.9 ppm and the same Brix, the weighted average limonin level in the
final blend would be the desired 7.0 ppm.
It must be remembered that the juices from all citrus varieties contain limonin
to some degree, and it cannot be assumed that they contain no limonin even if
they come from what is considered a nonbitter juice such as Valencia. It is
interesting to note that Valencia orange juice, the most popular orange juice in
the world, is considered a nonbitter juice even though early-season California
Valencia juice contains limonin levels as high as 15 ppm. However, the acid
content of this early season juice is so high that by the time the acid levels are
blended to commercial levels, the limonin levels are blended to below taste
threshold values. Hence, limonin levels, even in traditionally nonbitter juices,
should not be treated lightly in blending.
1 56 CITRUS JUICE CHARACTERISTICS

As with other citrus juice parameters, the adjustment of limonin levels lends
itself to computer application. Limonin levels usually are not determined as
often as other juice parameters, so blending or adjusting citrus juices to a spec-
ified limonin level does not have the same import as adjusting the Brix, ratio,
oil, or pulp levels. However, where debittering is not done, the use ofthe above
equations may be warranted. Figure 10-4 shows a flow chart that can be used
to program computers to make the above calculations. Also, a sample
GWBASIC program can be found in Appendix B.

DEBITTERING OF CITRUS JUICES

Methods to debitter citrus juices have been under investigation for many years,
including: ethylene gas treatment (Maier, Brewster, and Hsu 1973); the use of

Limonin camp. n (Ln) n


Brix of Camp. n (Bn) Z1 = I LiDiVi
Volume Camp. n (Vn) i=1
Maximum Limonin (Lmax) n
Z2 = I DiVi
i=1

EO 10-8 yes
Lavg = Z1/Z2

yes

EO 10-9 EO 10-10
Lavg
V1 L1

Fig. 10-4. Flow chart that can be used to program computers to adjust the limonin level in citrus
blends.
BITTERNESS IN CITRUS JUICES 157

the nonbitter flavone neodiosmin, which competes with limon in for receptor
sites on the tongue (Guadagni, Maier, and Turnbaugh 1976); the use of im-
mobilized bacteria and enzymes (Hasegawa and Maier 1983); the use of super-
critical carbon dioxide (Kimball 1987); the use of auxin sprays on trees, which
interfere with the biosynthesis of limon in in the fruit (Hasegawa et al. 1986);
and the use of adsorption and ion exchange resins (Shaw and Buslig 1986;
Maeda et al. 1984; Johnson and Chandler 1985). The last has proved to be the
only commercially feasible method (Kimball and Norman 1990a,b; Norman
and Kimball 1990). Ion exchange resins not only have the capacity to remove
limonin and naringin, but they can remove substantial quantities of organic
acids as well. Early-season bitter juice may not need to be debittered to below
the taste threshold because of the high acid content of the juice; as with the
Valencia juice mentioned above, acid blending will dilute out some of the li-
monin content. If deacidification and debittering take place simultaneously,
however, limonin levels probably will need to be reduced to below taste thresh-
old values.

Commercial Absorption Debittering

Commercial debittering of citrus juices consists of juice preparation, resin treat-


ment, and column regeneration. In preparing the juice for resin treatment, sev-
eral factors must be considered. First, freshly extracted juice must be treated
differently from reconstituted juice, which is generally low in oil and pulp con-
tent, whereas the freshly extracted juice requires temperature elevation to about
120°F and pulp removal down to about 1 %. Pulp removal can be accomplished
by using commercial centrifuges or ultrafiltration membranes. Freshly extracted
juice requires heat treatment for resin efficiency, which serves also to stabilize
pectinase enzymes and pasteurize the juice. Freshly extracted juice also must
be deoiled because the citrus essential oils are absorbed by the resin and can
decrease its efficiency; oil levels of 0.015 % or less are recommended. The
heating of the juice also increases centrifuging efficiency. Freshly extracted
juices contain almost twice the spindown pulp as pasteurized or evaporated
juices. Because efficient resins are small in size and weight, down-flow resin
beds generally are required. The use of up-flow systems results in costly resin
loss.
After resin treatment, the juice has only a trace pulp content and is lower in
oil content. Insignificant amounts of organic acids, including vitamin C, are
lost during resin treatment. Some of the vitamin C loss is due to the increased
heat applied to the juice. Acid treatment of the resin during regeneration pre-
vents acid reduction during the resin treatment. Navel juice processors prefer
high acid levels, as there is usually an overabundance of low-acid late-season
navel juice that needs the early-season high-acid juice for blending.
158 CITRUS JUICE CHARACTERISTICS

When one is using absorption or ion exchange resins, saturation of the resin
eventually requires its regeneration. In commercial debittering the entrapment
of pulp particles results in pressure buildup in the column, which necessitates
regeneration before the resin becomes saturated with limonin or naringin. Pulp
and cloud clarification by means of ultrafiltration reduces the concern for col-
umn clogging, so that regeneration can be less frequent. Regeneration generally
consists of a series of backflushes of basic solutions, clear water rinses, air
scrubs, and, if acid reduction is to be minimized, a final acid treatment. Because
of the difficulty of disposing of sodium hydroxide, potassium hydroxide or am-
monium hydroxide generally is preferred. Also, sulfuric acid is considered to
be the acid of choice as far as waste disposal is concerned. If regeneration
wastes are to be disposed of through irrigation, then sodium bases, nitric acid,
and hydrochloric acid should be avoided, as they are considered detrimental to
agricultural soils.

QUESTIONS

1. When tasting juice for bitterness, what should one look for?
2. What two compounds cause citrus juice bitterness, and in what varieties
do they occur?
3. What is the taste threshold of naringin in grapefruit juice, and what is
the ideal level?
4. What are the USDA and Florida grape standards for naringin and li-
monin?
5. Why is it that limonin bitterness does not affect the fresh fruit industry
but naringin bitterness does?
6. What affects the rate of limonin development?
7. How can you be sure that the limonin in a juice sample is completely
developed?
8. What are the advantages and disadvantages of the limonin EIA, HPLC,
and TLC methods of analysis?
9. What is the commercially accepted means of debittering citrus juices,
and why has this method been successful?
10. What are some ways of reducing bitterness in citrus juices during pro-
cessing?

PROBLEMS

1. In the HPLC nonnal phase limonin detennination, finish the calibration table (p.
159), assuming that the sample is 11.8°Brix. What is the factor F?
BITTERNESS IN CITRUS JUICES 159

Sample P mlGC OP p.g/P ppm LIM EXPT ppm LIM


Lot 1 0.85 9.4
+O.lmlstd 1.05 9.4
+ 0.3 ml std 1.35 9.4
+ 0.5 ml std 1.80 9.4
+ 0.8 ml std 2.30 9.4
+ 1.0 ml std 2.70 9.5
AVG =

2. Using the factor calculated above, what is the limonin level in a 12.1 °Brix juice
sample with a peak height of 1.56 and a GC value of 9.6 ml?
3. What would be the expected limonin level after blending the following components?
Would this be considered bitter juice?

Lot Gallons Brix Limoninppm


467 65.1 16.1
2 1102 12.6 8.2
3 136 59.6 3.7
4 48 61.9 2.1
5 2676 58.2 5.5

4. Supposed you wanted to make the same amount of juice in the blend in problem 5.
What would be the maximum limonin level of a 62.1 °Brix lot be if you exchanged
it with lot 1 to get a final limonin level of 7.0 ppm?
5. Suppose you had no other lot to exchange with the components in problems 3 and 4,
but you wanted to reduce the limonin level to 7.0 ppm. How many gallons of lot 1
would you need to pull from the blend?
6. What would be the expected naringin level after blending the following components?
What would be the Florida grade?

Lot Drums Brix Naringin ppm


16 58.2 546
2 19 57.0 772
3 5 46.4 534
4 8 62.1 817
5 10 13.6 907

7. Suppose you wanted to make the same amount of juice, exchanging lot 2 above for
another lot of the same Brix. What would be the maximum naringin content allowed
in order to get grade A juice by Florida standards?
8. Suppose you wanted to keep the number of drums of lots 1 and 3 and use one of the
other lots to adjust the naringin content to the maximum level for grade A in the state
of Florida. How many drums of lots 2, 4, or 5 would you need?
160 CITRUS JUICE CHARACTERISTICS

REFERENCES

Belitz, H. D., Chen, H., Jugel, H., Treleano, R., Wieser, H., Gasteiger, J., and Marsili, M.
1979. Sweet and bitter compounds: Structure and taste relationship. In Food Taste Chemistry,
ACS Symposium Series 115, J. C. Boudreau, ed. The American Chemical Society, Washington,
D.C., 125.
Berry, R. E. and Tatum, J. H. 1986. Bitterness and immature flavor in grapefruit: analyses and
improvement in quality, J. Food Sci., 51,1368-1369.
Chandler, B. V. 1971. Some solubility relationships of limonin. Their importance in orange juice
bitterness, CSIRO Food Res. Q., 31, 36-40.
Chandler, B. V. and Kefford, J. F. 1966. The chemical assay of limonin, the bitter principle of
oranges,J. Sci. Food Agric. , 17,193.
Davis, W. B. 1947. Determination offlavanones in citrus fruits, Anal. Chem., 19,476-478.
Fisher, J. F. and Wheaton, T. A. 1976. A high pressure liquid chromatographic method for the
resolution and quantitation of naringin and naringenin rutinoside in grapefruit juice, J. Agric.
Food Chern., 24, 898-899.
Florida Dept. of Citrus, Official Rules Affecting the Citrus Industry, Lakeland, Fla., 20-64.03(5),
20-64.09(7) .
Guadagni, D. G., Maier, V. P., and Turnbaugh, J. G. 1976. Effect of neodiosmin on threshold
and bitterness of limonin in water and orange juice. J. Food Sci., 41, 681-684.
Guadagni, D. G., Maier, V. P., and Turnbaugh, J. G. 1974. Some factors affecting sensory thresh-
olds and relative bitterness of limonin and naringin, J. Sci. Food Agric., 25, 1199-1205.
Hasegawa, S. 1980. Private communication. Biosynthesis of limonoids in Citrus: sites and trans-
location.
Hasegawa, S. and Maier, V. P. 1983. Solutions to the limonin bitterness problem of citrus juices,
Food. Tech., 37(6), 73-77.
Hasegawa, S., Herman, Z., Orme, E. D., and Ou. P. 1986. Phytochemistry, 25, 542,1323,2783.
Hasegawa, S., Patel, M. N., and Snyder, R. C. 1982. Reduction of limonin bitterness in navel
orange juice serum with bacterial cells immobilized in acrylamide gel, J. Agric. Food. Chem.,
30, 509-511.
Johnson, R. L. and Chandler, B. V. 1985. Debittering and deacidification of fruit juices, Food
Tech. in Australia, 38, 294-297.
Jourdon, P. S., Mansell, R. L., Oliver, D. G., and Weiler, E. W. 1984. Competitive solid phase
enzyme-linked immunoassay for the quantification of limonin in citrus, Anal. Biochem., 138,
19-24.
Kimball, D. A. 1987. Debittering of citrus juices using supercritical carbon dioxide, J. Food Sci.,
52, 481-482.
Kimball, D. A. and Norman, S. I. 1990a. Changes in California navel orange juice during com-
mercial debittering, J. Food Sci., 55, 273.
Kimball, D. A. and Norman, S. I. 1990b. Processing effects during commercial debittering of
California navel orange juice, J. Agric. Food Chern., 38, 1396-1400.
Kruger, A. J. and Colter, C. E. 1972. Gas chromatographic identification oflimonin in citrus juice,
Proc. Fla. State Hort. Soc., 85,206-210.
Maeda, H., Takahashi, Y., Miyake, M., and Ifuku, Y. 1984. Studies on the quality improvement
of citrus juices and utilization of peels with ion exchange resins. 1. Removal of bitterness and
reduction of acidity in Hassaku (Citrus hassaku hort. ex. Tanaka) juice with ion exchange resins
and adsorbents, Nippon Shokuin Kogyo Gakkaishi, 31, 413-420.
Maier, V. P., Bennett, R. D., and Hasegawa, S. 1977. Limonin and other limonoids. In Citrus
Science and Technology Vol. I, S. Nagy, P. E. Shaw, and M. K. Veldhuis eds. The AVI Pub-
lishing Company, Inc., Westport, Conn., 379, 382.
BITTERNESS IN CITRUS JUICES 161

Maier, V. P., Brewster, L. C., and Hsu, A. C. 1973. Debittering citrus juices, Citrograph, 58,
403-404.
Norman, S. I. and Kimball, D. A. 1990. A commercial citrus debittering system, Proc. o/the 36th
Citrus Eng. Conf., Florida section of the ASME, Lakeland, Fla., March 29, 1990, 1-31.
Official Rules Affecting the Florida Citrus Industry, January 1, 1975, State of Florida, Dept. of
Citrus, 20-65.01 to 20-65.05.
Rouseff, R. L. and Fisher, J. F. 1980. Determination of limonin and related limonoids in citrus
juices by high performance liquid chromatography, Anal. Chern., 52,1228-1233.
Shaw, P. E. and Buslig, B. S. 1986. Selective removal of bitter compounds from grapefruit juice
and from aqueous solution with cyc\odextrin polymers and with Amberlite XAD-4, J. Agric.
Food Chern., 34, 837-840.
Shaw, P. E. and Wilson, C. W. 1984. A rapid method for determination oflimonin in citrus juices
by high performance liquid chromatography, J. Food Sci., 49, 1216-1218.
Tatum, J. H. and Berry, R. E. 1973. Method for estimating limonin content of citrus juices, J.
Food Sci., 38, 1244-1246.
Ting, S. V. and Rouseff, R. L. 1986. Citrus Fruits and Their Products. Marcel Dekker, Inc., New
York, 108-113.
Weiler, E. W. and Mansell, R. L. 1980. Radioimmunoassay of limonin using a titrated tracer, J.
Agric. Food Chem., 28, 543.
Wilson, K. W. and Crutchfield, C. A. 1968. Spectrophotometric determination of limonin in or-
ange juice, J. Agric. Food Chem., 16, 118-124.
Chapter 11

Nutritional Content of Citrus Juices

Natural foods, especially citrus products, have always been highly regarded as
excellent sources of human nutrition. Nutrition is the ability to engender growth,
and many of the components of citrus products contribute to the growth and
well-being of the human body. In order to grow, the human body requires cer-
tain dietary components, and this need has given rise to the regulation of nu-
tritional labeling by many governments. Such labeling, which provides nutri-
tional information to consumers, is of great value, especially for persons who
must monitor their nutritional intake for medical or dietary purposes. Nutri-
tional labeling also gives an aura of professionalism and quality to a product,
especially one that contains significant amounts of nutrients.
There are two basic types of nutrients. The TrUlcronutrients are those that
occur as major components of the food product, such as sugars or carbohy-
drates, salts, acids, protein, and fats. These nutrients provide energy for the
body in addition to regulating the absorption rates of various body chemicals
and water retention in the body. Proteins act as catalysts for certain life-giving
chemical reactions and as building blocks for many parts of the body. The
micronutrients are those that occur in trace amounts. They either regulate spe-
cific chemical reactions, like the proteins, or they form important organome-
tallic complexes such as the iron complexes that make up the blood.
To establish a uniform way of reporting nutritional information, laws regu-
lating labeling have been passed in various countries. In the United States, the
Food and Drug Administration (FDA) first published nutritional labeling reg-
ulations in the Federal Register in March of 1973 (U .S. Food and Drug Admin-
istration 1973). Since that time, changes in the regulations have occurred, and
they continue to occur because of constant research and new understanding
about human nutrition. The current FDA regulations can be found in the Code
of Federal Regulations (CFR), Title 21, 101.9-101.13. For natural products
where no nutrients have been added, nutritional labeling is optional. About two-
thirds of the 100% citrus products on the market do not include any nutritional

162

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
NUTRITIONAL CONTENT OF CITRUS JUICES 163

labeling. If nutritional labeling is used, the rules and fonnat outlined in the
federal code must be followed.
With respect to labeling, there are two classes of nutrients. Group I nutrients
are those added to the product, which must be present at least at the levels
declared on the label. Group II nutrients are those that occur naturally, which
must be present in at least 80 % of the levels declared on the label. Excess
amounts of nutrients are allowed within good manufacturing practice except that
the calorie, carbohydrate, sodium, and fat levels cannot exceed 20% of the
value declared on the label. Official compliance with declared label values is
detennined by taking 12 samples, selected from 12 separate shipping cases at
random, and analyzing them by AOAC or other suitable methods.
Even though FDA is reviewing the commerical nutritional labeling fonnat
that will most likely contain changes; the fonnat that the nutritional infonnation
must presently follow is illustrated in Table 11-1. All nutritional levels are ex-
pressed on a per-serving basis. A serving of citrus juice usually is designated
as 6 fluid single-strength ounces (177 ml) with 113 g designated for citrus
sections. The servings per container is the number of reconstituted or consum-
able servings rounded off to the nearest whole number.

Table 11-1. Sample format for


nutritional labeling of a 6-ounce
can of frozen concentrated
orange juice. The words "per
serving" in the first line
are optional, as are the
sodium and potassium
labeling.
Nutritional Information Per Serving
Serving Size 6 fl. oz.
Servings per Container 4
Calories 90
Protein I g
Carbohydrates 21 g
Fat Og
Sodium o mg (optional)
Potassium 260 mg (optional)

Percentage of U. S. Recommended Daily Allowances


(U.S. RDA)
Vitamin C 120%
Thiamin 8%
Contains less than 2% of the U.S. RDA of Protein. Vitamin A,
Riboflavin, Niacin, Calcium, and Iron.
164 CITRUS JUICE CHARACTERISTICS

REPORTING OF MACRONUTRIENTS

Calories

Calories, in reference to nutritional labeling, represent the amount of energy


available for human metabolism. Calories can be determined by using accepted
analytical methods such as the AOAC (1980) or the Atwater method (USDA
1955). However, a more common and simple way to determine the caloric con-
tent of citrus juices is to use a mathematical approach on the basis of 4, 4, and
9 calories per gram of protein, carbohydrates, and fat, respectively. For ex-
ample, if we use the example in Table 11-1, the calories per serving could be
calculated as follows:

I g protein x 4 = 4 calories
21 g carbohydrates X 4 = 84 calories
o g fat x 9 = 0 calories
Total = 88 calories

Calorie values then are rounded off to the nearest even number up to 20 calories,
to the nearest increment of 5 from 20 to 50 calories, and to the nearest increment
of 10 from there on up. Because, in the above sample, the number of calories
is greater than 50, the calorie value is rounded off to the nearest 10, or to 90
calories, which appears on most nutrition labels of 100% orange juice.

Protein

Proteins are enzymes or biological catalysts that govern the biochemical reac-
tions occurring in the body, and provide energy like the carbohydrates. The
human body manufacturers many of the proteins it needs. However, it requires
an outside source for some of them. Some parts of the body, such as hair, are
themselves made up of proteins. Proteins are comprised of long amino acid
polymeric chains that are cross-linked in various ways. For the purposes of
nutritional labeling, the protein level is calculated by multiplying the weight
percent of total nitrogen by 6.25. The nitrogen content in citrus juices has been
reported to be 60 to 120 mg per 100 ml of single-strength juice (Ting 1967),
with higher values reported in California orange juices (Tockland 1961). The
nutritional quality of proteins should aslo be taken into consideration. This qual-
ity is dependent on the protein efficiency ratio (PER). A PER value of at least
20 % of casein is required for a food to be considered a significant source of
protein. Citrus products generally fall short of this and thus are considered to
be insignificant or poor sources of protein.
NUTRITIONAL CONTENT OF CITRUS JUICES 165

The Kjeldahl procedure is generally used to measure the total nitrogen level
in citrus juices, but it is a lengthy and involved procedure for routine quality
control work and may account for only 11 to 20% of the total juice protein
(Attaway et al. 1972). Also, at least 1 gram of protein is required for nutritional
labeling, and citrus juices just meet this requirement. Given these circum-
stances, protein analysis usually is not performed on citrus products in quality
control laboratories. When protein is reported on nutritional labels, the value
should be rounded off to the nearest gram per serving, which is usually 1 gram.
The USRDA for protein depends on the gender and age of the consumer, rang-
ing from 23 grams for children 1 to 3 years old to 56 grams for adult males 23
to 50 years old.

Carbohydrates

Carbohydrates, or sugars, are abundant in citrus juices and products, compris-


ing about 80 to 90 % of the soluble solids found in citrus juices (except lemon
and lime) and containing high levels of potential energy in their chemical bonds.
Thus citrus juices contain a high level of calories, the only nutritionally unde-
sirable characteristic of citrus products. About half of the carbohydrates are in
the fonn of sucrose, an oligosaccharide or disaccharide, consisting of one fruc-
tose "and one glucose molecule. The remaining carbohydrates are essentially
equal portions of glucose and fructose, the natural products of acid or enzymatic
hydrolysis of sucrose. The bond between the glucose and fructose molecules in
sucrose contains energy; so when the bond has been broken through hydrolysis,
some of the energy or calorie content of the sucrose is lost. For this reason, in
citrus juices, where half of the sucrose has been hydrolized, less potential en-
ergy is available, and the calorie content is reduced. Complex carbohydrates or
polysaccharides such as pectin, hemicellulose, and cellulose occur in insignif-
icant amounts in citrus juices compared to the primary sugars mentioned above.
Carbohydrates generally are measured according to Brix levels, as described
in Chapter 2. The Brix measurement includes organic acids, soluble salts, and
other soluble nitrogenous and pectic substances. Corrections are commonly
made to the Brix for acid levels as citric acid equivalents, which, for nutritional
labeling purposes, are considered part of the carbohydrates. Thus the acid-cor-
rected Brix measurement can be used to determine the nutritional carbohydrate
level in citrus juices.
Nutritional labeling laws require that the carbohydrate level be reported in
grams, rounded off to the nearest gram, per serving. In order to convert the %
sugar (Brix measurement) into grams per 6-ounce serving, the following can be
used.
gcarbohydrates!6 oz = (Brix) (177 ml per serving) (d) / 100% ( 11-1 )
166 CITRUS JUICE CHARACTERISTICS

where d is the density of the single-strength juice in g/ml. For example:

(11.8°Brix) (177 mIl serving) ( 1.0446 g/ml) 1100%


= 21.8 g carbohydrates

Rounding this off to the nearest gram gives 22 grams, which would be reported
on the nutritional label. If nutritional sweeteners are added to make sweetened
juice, they must be included in the carbohydrate level in nutritional labeling.

Fat

Fats are lipids (natural compounds that are soluble in hydrocarbons but not in
water), and are generally considered to be detrimental to health. In citrus juices
there are essentially no fats, and that can generally be declared on nutritional
labels. If fats were to exist in significant quantities, their level would be reported
to the nearest gram per serving.

Sodium and Potassium

Sodium and potassium labeling are optional under the present federal code.
When reported, the sodium or potassium level is given to the nearest milligram
per serving. Sodium generally is considered to be detrimental to health, whereas
potassium is considered to be advantageous. Citrus juices generally contain
insignificant amounts of sodium and can be so labeled. However, high levels
of potassium are common; levels of 200 mg to 2000 mg per serving can be
found in commercial juices, depending on the geographical location (Harding,
Winston, and Fisher 1940). Also, legally added water in reconstituted products
may be rich in potassium and/or sodium and contribute to the presence of these
nutrients. Again, as mentioned earlier, naturally occurring nutrients can legally
exist in levels of at least 80% of the declared value, with no maximum limit
for potassium. The natural sodium or potassium levels in water used to legally
reconstitute citrus products fall in this category. Because sodium levels are low
in citrus products, routine quality control of those levels is seldom performed.
Also, because potassium is plentiful in many foods, its presence in citrus prod-
ucts does not constitute an anomaly and rarely justifies routine monitoring. On
those infrequent occasions when it is required, professional laboratories, using
ion chromatography or atomic absorption, can be used.

REQUIRED REPORTING OF MICRONUTRIENTS

When nutritional labeling is used, seven vitamins and minerals as well as pro-
tein must be mentioned on the label: vitamin A, ascorbic acid (vitamin C),
thiamin (vitamin B 1), riboflavin (vitamin B2 ), niacin (vitamin B4), calcium, and
NUTRITIONAL CONTENT OF CITRUS JUICES 167

iron. These values must be reported as a percentage of the U.S. recommended


daily allowance (USRDA): in 2% increments up to and including 10%, in 5%
increments from 10% to 50% ofthe USRDA, and in 10% increments thereafter.
When a nutrient occurs at a level of less that 2 % of the USRDA, the product
can be labeled as containing less that 2 % of the nutrient . If five or more of
these eight nutrients occur below 2 % of the USRDA, the manufacturer can state
that collectively these nutrients occur in levels less than 2 % of the USRDA,
rather than list each of the eight nutrients separately. For citrus juices, generally
orily vitamin C and thiamin occur in levels above 2 % of the USRDA. The
federal code indicates that no food can be considered a significant source of a
particular nutrient that does not occur at least at a level of 10% of the USRDA,
and that no food can be considered a superior source of a particular nutrient
unless it contains 10% more of the USRDA than another product does.
Vitamins and minerals, other than the ones mentioned above, do not occur
in citrus juices to any significant degree and generally do not appear on citrus
nutritional labels.

Vitamin C

Vitamin C, also known as ascorbic acid, hexuronic acid, cevitamic acid, and
antiscorbutic acid, has long been associated with citrus nutrition. Limes once
were used extensively to stave off scurvy attacks on board seagoing vessels, so
much so that British sailors were labeled "Limeys." Even though other fruits
and vegetables have higher levels of vitamin C than citrus juices, few are as
attractive in color, taste, and thus popularity as citrus. A single 6-ounce serving
(177 ml) provides more than 100% of the USRDA of vitamin C; so foods
containing higher levels of the vitamin offer no real nutritional advantage over
citrus. Also, vitamin C is very stable in citrus juices and degrades very little
with storage, another nutritional advantage.
L-Ascorbic acid has the following chemical structure:

OH

H-C-H
I
H-C-OH
r C- H
I C-OH
o II
L~-OH
II
o
168 CITRUS JUICE CHARACTERISTICS

It is easily oxidized to L-dehydroascorbic acid, which has the following chem-


ical structure:

OH

H-C-H
I
H-C-OH
,C-H
I C=O
o
L C=O
C=O

L-Dehydroascorbic acid is less stable than L-ascorbic acid, but the two have
nearly the same nutritional effect. Vitamin C contributes to: iron absorption;
cold tolerance; maintenance of the adrenal cortex; antioxidizing activity; me-
tabolism oftryptophan, phenylalanine, and tyrosine; body growth; wound heal-
ing; synthesis of polysaccharides and collagen; formation of cartilage, dentine,
bones, and teeth; and capillary maintenance. Humans cannot synthesize vitamin
C, and must depend on an external source for its supply.
The vitamin C level in citrus decreases with maturity. Florida oranges go
from about 50 mg /100 ml of single-strength juice at the beginning ofthe season
to about 30 mg/IOO ml by the end of the season (Harding, Winston, and Fisher
1940). During an average marketing period, the loss of vitamin C amounts to
less than 10%, which is indicative of the stability of vitamin C in citrus juices.
Atmospheric oxygen· is responsible for most vitamin C loss during long-term
storage. Many polymeric containers readily admit oxygen, which degrades vi-
tamin C as well as contributing to the development of off colors and flavors.
Grapefruit juice generally contains slightly less vitamin C ( 45 mg /100 ml) than
orange juice (50 mg/100 ml) and lemons (60 mg/IOO mI). Tangerines and
limes contain even less vitamin C (about 30 mg/IOO ml). These vitamin C
levels represent approximate averages and indicate general relative compari-
sons. Actual vitamin C levels may vary widely, by as much as 50%.
Even though vitamin C is a major nutrient in citrus juices and is considered
to be an important quality parameter, its stability and generally consistent levels
render routine analysis unimportant. Industrially, vitamin C levels are not con-
sidered an important parameter. However, vitamin C levels can be of interest
on occasion, especially in establishing nutritional labeling; and the following
two methods of analysis can be used.
NUTRITIONAL CONTENT OF CITRUS JUICES 169

Vitamin C Indophenol Titration

Equipment and Supplies

• 50 ml buret, magnetic stirrer, and 125 ml Erlenmeyer flask for titrating.


• 100 ml volumetric flask.
• 10 ml pipette.
• 50 ml beaker.
• 150 ml beaker.
• 500 ml volumetric flask.
• Dye solution: Add 0.250 g sodium 2,6-dichlorobenzenoneindophenol or
sodium 2,6-dichlorophenolindophenol to 500 ml warm water (60°C) (or
0.050 g sodium 2,6-dichloroindophenol to 200 ml distilled water) and add
approximately 100 mg sodium bicarbonate (NaHC0 3 ). Filter the solution,
and store it in a sealed amber container in the refrigerator until it is used.
When the dye fails to give a distinct endpoint, discard it.
• Acid solution: 10 g of metaphosphoric acid (HP0 3 ) in warm distilled water
(60°C) in successive portions until the acid will not dissolve. Transfer the
solution to a 500 ml volumetric flask, cool it to room temperature, and add
40 ml glacial acetic acid. Fill the flask to the mark with distilled water.
The solution should be good for 7 to 10 days when stored in the refriger-
ator. HP0 3 slowly changes to H 3 P04 •
• Ascorbic acid standard solution: 0.100 g of pure ascorbic acid (melting
point 190-192°C) in a 50 ml beaker. Add 10 ml acid solution, and care-
fully transfer the solution to a 100 ml volumetric flask. Fill the flask to the
mark with distilled water. This solution contains 1 mg ascorbic acid / m!.
Make a fresh solution for each titrating session. Do not store it.

Standardization Procedure

1. Bring the dye solution to room temperature. Transfer 10 ml of the fresh


ascorbic acid standard solution to a 150 ml beaker, and add 10 ml of acid
solution.
2. Titrate the ascorbic acid solution rapidly with the dye solution until a light
but distinct rose pink color persists for at least 5 to 10 seconds.
3. Repeat at least once until the milliliters titrated are within 0.10 ml for
each titration.
4. The dye concentration can be calculated by using:

Dye cone. = (10 mg ascorbic acid) / (ml titrated) ( 11-2)


170 CITRUS JUICE CHARACTERISTICS

For example:

(10 mg ascorbic acid)/(21.42 ml) = 0.4669 mg/ml

Titration Procedure

1. Add 10 ml of reconstituted or single-strength juice ( 11.8 0 Brix) to 10 ml


of the acid solution.
2. Titrate immediately with the standardization dye solution until a rose pink
color persists for 5 to 10 seconds.
3. Calculate the ascorbic acid (AA) or vitamin C level by using:

mg AA / 100 ml = (dye cone. ) (ml titrated) ( 100 ml juice)


-.:.......0_ _---"-----'---_ _ _- ' - "_ _- - - ' - _ - ' -
(11-3 )
(10 ml sample)

For example:

(0.4669) (9.46 ml titrated) (100 ml)/(lO ml) = 44.2 mg AA/I00 ml

The following HPLC procedure uses ion pairing and can be used to determine
both the L-ascorbic acid level and the dehydroascorbic acid level. Dehydroas-
corbic acid is derivatized with 1,2-phenylenediamine in order to increase its
ultraviolet absorbance.

HPLC Vitamin C Determination (Keating and Haddad 1982)

Equipment and Supplies

• Isocratic or single-pump HPLC system with UV detector (290 nm and 348


nm), 30 cm X 4 mm C I8 column, 20 p.l syringe, and chart recorder (in-
tegrator is optional).
• 0.45 p.m filter.
• 100 ml volumetric flask.
• 200 ml methanol.
• Standard solution: Dissolve 25 mg ascorbic acid, 5 mg dehydroascorbic
acid, and 180 mg 1,2-phenylenediamine dihydrochloride (PDA . 2HCI)
in 50 m1 of methanol in a 100 ml volumetric flask, and fill the flask to the
mark with methanol. Let it stand in the dark for 80 minutes in order to
complete the derivatization.
• Mobile phase: methanol in water (60:40 v Iv) containing 2.5 x 11- 4 M
hexadecyItrimethylammonium bromide ion pairing agent.
• Lab centrifuge.
NUTRITIONAL CONTENT OF CITRUS JUICES 171

Procedure

1. Add 200 mg of PDA . 2HCl to 70 ml of reconstituted or single-strength


juice (1l.8°Brix) or standard solution to a 100 ml volumetic flask. Dis-
solve it, and fill the flask to the mark with methanol.
2. Centrifuge for 5 minutes, filter, and allow the solution to stand in the dark
for 1 hour. Filter it with a 0.45 ttm filter.
3. Inject 15 ttl of this solution into the HPLC system with a pump flow rate
of 1.0 ml/min after conditioning the column with the mobile phase for 3
hours.
4. Set the wavelength of the detector to 348 nm initially, and change it to
290 nm after the dehydroascorbic acid peak has eluted. Detector atten-
uation is 0.1 aufs throughout the run.
5. The ascorbic acid and dehydroascorbic acid level can be calculated by
using:
(11-4)
where Pj and P s are the peak heights (or areas under the peak if an inte-
grator is used) of the juice and standard samples, respectively, and ~ and
Cs are the concentrations of the vitamin C in the juice and standard sam-
ples, respectively. In the standard, the ascorbic acid concentration is 25
mg/100 ml and the dehydroascorbic acid concentration is 5 mg/lOO ml.

Nearly 75% of the vitamin C in oranges and over 80% of the vitamin C in
grapefruit can be found in the peel. The USRDA for vitamin C is 60 mg.

Thiamin

This vitamin is also known as vitamin B\, aneurin, antineuritic factor, antiber-
iberi factor, and oryzamin. The metabolically acitve form of thiamin is thiamin

Y
pyrophosphate.

NyNH2
o 0

I ~/s cc-o-r-O-r- OH
N~ ~ "';/ OH OH
~ ""C-N
+
This molecule acts as a coenzyme which participates in decarboxylation of
a-keto acids in the initial phases of the citric acid cycle. Thiamin deficiency is
responsible for the development of beriberi.
172 CITRUS JUICE CHARACTERISTICS

Orange juice has the highest level of thiamin ( 170 I-tg /6 oz serving or 11 %
of the USRDA), followed by tangerine juice (100 I-tg/6 oz serving or 7% of
the USRDA) and grapefruit juice (70 I-tg/6 oz serving or 5% of the USRDA).
Unlike vitamin C, thiamin levels increase with fruit maturity, expanding from
as low as 45 I-tg/ 100 g of single-strength juice to 90 I-tg/100 g of juice through-
out a given season. The USRDA for thiamin is 1.5 mg.
Thiamin determinations are commonly performed by using a combination of
enzymes, packed open columns, and fluorimeters (Ting and Rouseff 1986). This
procedure is generally too tedious and complex for routine quality control anal-
ysis. Because thiamin determinations are performed infrequently, professional
laboratories usually are consulted.

Calcium

Even though calcium occurs in very small amounts naturally in citrus juices,
calcium-added products have increased in popularity. Any nutrient that is added
must be declared on the nutritional label, and nutritional labeling becomes man-
datory. As mentioned earlier, most minerals are determined by using ion ex-
change or atomic absorption. This is usually best done in professional labora-
tories because of the infrequent need for such determinations and the cost of
the instrumentation. The USRDA for calcium is 1 gram. Calcium hydroxide is
easily added to citrus juices and neutralizes the acidity, producing a sweeter
juice at the same time. However, it should be remembered that such calcium
additions violate the standards of identity for 100% juice products, rendering
them "drinks" rather than "juices."

Pectin and Flavonoids

Even though there are no labeling requirements or formats in the federal code
regarding pectins and flavonoids, it should be noted that these compounds, found
abundantly in citrus products, are believed to be linked to the reduction of serum
cholesterol, a rare and important characteristic in foods. Like many natural
products, the nutritional label, as outlined in the federal code, falls far short of
completely describing the nutritional advantages of citrus products. Many such
advantages have yet to be discovered and understood. Even though nutritional
analysis plays a minor role in overall citrus quality control, it should be remem-
bered that the nutritional value of citrus products is one of their major selling
points, and quality control personnel should properly represent it as such to the
industry and to the consumer.
NUTRITIONAL CONTENT OF CITRUS JUICES 173

QUESTIONS

1. What is the difference between macronutrients and micronutrients?


2. What is the difference between class I and II nutrients?
3. If no nutritional labeling appears on a 6-ounce can of frozen concentrated
orange juice, is the law being violated? Why or why not?
4. What are some of the advantages and disadvantages of using nutritional
labeling on 100% citrus juice products?
5. What nutrient must appear on the label twice?
6. What is the most abundant nutrient in single-strength juices?
7. How do the acids in citrus juices fit into nutritional labeling?
8. What micronutrients must be reported when nutritional labeling is used?
9. Which fruit has the most vitamin C and thiamin, and does the vitamin
C and/or thiamin increase or decrease as the season progresses?
10. How much of the USRDA of vitamin C and thiamin is commonly de-
clared on most 100% orange juice products?

PROBLEMS

1. Suppose that super citrus scientist Dr. VanOhjay has discovered a new orange variety
that produced juice of a higher nutritional quality. This new juice contains 11 grams
of protein, 8 grams of carbohydrates, and 1 gram of fat per 6 ounces (177 ml). What
calorie level would be declared on the label?
2. In the indophenol titration for vitamin C, suppose that you titrated 19.64 ml in the
standardization and 11.46 ml in the sample titration. What would be the dye concen-
tration, the vitamin C level (mg/lOO ml juice), and the highest declarable % US-
RDA value on the label?
3. How many grams of carbohydrates would be declared on a label of product whose
serving size is 100 ml of single-strength juice at 12.0oBrix?
4. What would be the maximum declarable amounts on a nutritional label (serving 6
ounces or 177 ml) for a juice with the following analysis results. Assume USRDA
levels for an adult male.
• 0.501 g protein
• 20.4 g carbohydrates
• 35.6 mg/100 ml vitamin C
• 52.3 J.(g/l00 g thiamin
• 63. 1 mg / serving calcium added to the juice
5. If the peak height of a standard ascorbic acid solution, using the HPLC method, were
1.46 and the dehydroascorbic acid peak height 0.32, what would be the resulting
levels of the two if the juice sample peaks were 2.23 for ascorbic acid and 0.36 for
dehydroascorbic acid? What would be declared on the label?
174 CITRUS JUICE CHARACTERISTICS

REFERENCES

Attaway, J. A. et al. 1972. Some new analytical indicators of processed orange juice quality, Proc.
Fla. State Hort. Soc., 85, 192-203.
AOAC. 1980. Official Methods of Analysis, 13th Edition, 10.031, Association of Official Analyt-
ical Chemists, Washington, D.C.
Harding, P. L., Winston, J. R., and Fisher, D. F. 1940. Seasonal changes in Florida oranges.
USDA Tech. Bulletin, 753.
Keating, R. W. and Haddad, P. R. 1982. Simultaneous determination of ascorbic acid and dehy-
droascorbic acid by reverse phase ion-pair high performance liquid chromatography with pre-
column derivatization, J. Chromatography, 245, 249-255.
Ting, S. V. 1967. Nitrogen content of Florida orange juice and Florida orange concentrate, Proc.
Fla. State Hort. Soc., 80, 257-261.
Ting, S. V. and Rouseff, R. L. 1986. Citrus Fruits and Their Products. Marcel Dekker, Inc., New
York, 128-129.
Tockland, L. B. 1961. Nitrogenous constituents. In The Orange: Its Biochemistry and Physiology,
W. B. Sinclair, ed. University of California Press, Berkeley, Calif.
USDA. 1955. Energy Values of Foods-Basis and Derivation, A. L. Merrill and B. K. Watt, eds.
Government Printing Office, Washington, D.C.
U.S. Food and Drug Administration. 1973. Food: nutritional labeling, Federal Register, 38, No.
49, 6959-6961. U.S. Government Printing Office, Washington, D.C.
Chapter 12

Citrus Rheology

"Rheo" comes from the Greek word meaning "to flow," thus rheology is the
study of flow or, in the citrus industry, the study of the flow of citrus juices and
concentrates. Fluids are divided into two basic types in rheology. Newtonian
fluids are chemically pure homogenous fluids whose viscosity, or resistance to
deformation, does not change with shear rate. (Shear rate can be described as
the flow rate, the stirring rate, or the rate at which one surface passes over
another.) Non-Newtonian fluids have different apparent viscosities at different
shear rates. The latter description generally characterizes heterogeneous solu-
tions such as citrus juices and concentrates. The non-Newtonian nature of citrus
juices is primarily due to pulp and cloud material within the juice. Removal of
these components renders the resulting serum Newtonian in nature. The term
"consistency" or "apparent viscosity" is generally used with non-Newtonian
fluids, while "viscosity" is generally used with Newtonian fluids.
Citrus juices at concentrations above 200Brix are considered to be pseudo-
plastic; that is, their apparent viscosity decreases with an increase in shear rate.
In other words, as the concentrate moves more rapidly through a pipe or during
mixing in a tank, its apparent viscosity decreases. In order to start flowing,
citrus concentrates require an extra amount of energy, which is called the yield
stress.
Citrus concentrates are also thixotropic: when flow begins just after the yield
stress is applied, there is a breakup of the forces that hold the concentrate to-
gether. When the flow is stopped, these forces are restored. In rheology this
behavior is called going from a gel to a sol and then back to a gel condition.
The opposites of pseudoplastic and thixotropic are dilatent and rheopectic, re-
spectively.
In summary, citrus concentrates are non-Newtonian, pseudoplastic, thixo-
tropic fluids.

175

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
176 CITRUS JUICE CHARACTERISTICS

Significance of Citrus Rheology

Citrus juice and concentrate consistency plays an important role in the quality
of citrus products. It has an important impact on the operation of every piece
of equipment used in citrus processing, as well as on consumer acceptance and
satisfaction. Even though routine measurements of the apparent viscosity gen-
erally are not necessary, consistency becomes an important parameter in de-
signing equipment for new products. Although this usually is a problem for
engineers, quality control personnel often are consulted about product consis-
tency, especially in small processing plants.

Equipment Sizing

Citrus processing plants are often referred to as just a bunch of tanks, pipes,
and pumps. Even though there may be a little more to processing plants than
that characterization implies, juice conveyance and storage are involved in nearly
every step of citrus processing. Thus flow rates, which are a function of pump-
ing power and pipe or orifice size, are of vital interest in integrating all the
processing steps and in transporting juice products in a timely manner.
Citrus concentrates exist at a wide range of temperatures, concentrations, and
compositions during their processing, and fluctuations in their apparent viscos-
ities can be dramatic. A pump, pipe, or other piece of equipment that is too
small can become a lethal bottleneck in processing, blending, packaging, and
shipping. A pump, pipe, or other piece of equipment that is too large can turn
out to be an excessive and costly expenditure or even an electrical tapeworm,
consuming large amounts of unnecessary energy. Single-strength juices gener-
ally have the same apparent viscosity as water for engineering purposes, or
about 18 centipoise. For 42°Brix frozen concentrated orange juice (FCOJ), the
apparent viscosities range from 430 to 2749 centipoise at 26.7°C, with grape-
fruit concentrate ranging from 150 to 1885 centipoise (Ezell 1959). For 60 to
65 °Brix concentrates the apparent viscosities range from 400 to 1000 centipoise
at 25°C and 3000 to 7000 centipoise at -10°C, all with a shear rate of 115.5
sec-I (Crandall, Chen, and Carter 1982). Bulk storage and shipping viscosities
generally are close to the latter extreme.
The apparent viscosity increases dramatically at commercial freezer temper-
atures, so care should be taken not to drop the temperature of bulk freezers or
tank farms much below -10°C (15°F). Quality control personnel generally
have to monitor freezer temperatures. As mentioned in Chapter 18, the increase
in fluidity that occurs with increased temperatures, compared to drum freezer
temperatures of about -20°C or about OaF, is responsible for the formation of
potassium citrate crystals in lower Brix / acid ratio concentrates.
CITRUS RHEOLOGY 177

Processing Considerations

During processing, product consistency can playa major role. As described in


Chapter 8, failure to deactivate the naturally occurring pectinase enzymes found
in the juice can result in gellation and/or a significant increase in the product's
consistency; however, most, if not all, modem evaporators heat juice suffi-
ciently to deactivate the pectinase enzymes. High pulp levels also contribute to
product viscosity. Juice sac material added to concentrates to give a floating
pulp or "just squeezed" appearance adds significantly to product consistency,
whereas centrifuged low-pulp concentrates are very fluid. Pulp wash concen-
trates generally are relatively viscous because of the additional insoluble ma-
terial contained therein, and can pose serious consistency problems. Enzymes
are often used to break up suspended and insoluble material in pulp wash juices.
Also, monitoring of the apparent viscosity during pulp wash processing is war-
ranted. Often pulp wash juices are immediately combined with freshly extracted
juices to diminish the problem of excessive pulp wash consistency.
In addition to the suspended and insoluble material in citrus juices, the sol-
uble components can significantly contribute to the apparent viscosities. Early-
season high-acid concentrates are more fluid than late-season sweeter concen-
trates. Evaporators employing plate heat exchangers generally can concentrate
early-season orange juices to 65°Brix, but late-season juices containing more
sugar cannot be concentrated to the same level because of their excessive vis-
cosity. It has been shown that sucrose solutions above 22°Brix involve sucrose-
sucrose molecular interactions that strengthen hydrogen bonding (Kimball
1986). These interactions are the major contributors to this type of apparent
viscosity. The use of pectinase enzymes or homongenization has been suggested
as a way to reduce the apparent viscosity of citrus concentrates so that higher
Brix levels can be achieved (Crandall et al. 1988). This will result in a reduction
in storage and shipping costs.

Consumer Considerations

Besides cloud loss and gellation, mentioned in Chapter 8, another parameter of


citrus juice quality exists that is related to rheology-the mouth-feel. This is
especially important in the formulation of juice drinks. Natural juices set the
standard for the mouth-feel or consistency desired by consumers of citrus drinks.
Various gums and pectins have been used in an attempt to duplicate the mouth-
feel or apparent viscosity of natural juices. Also, the use of gel agents is of
primary interest in the manufacture of citrus jams and jellies. In such cases,
rheological measurements can help quality control personnel to maintain the
proper conditions and product components in order to make a successful, good-
quality product.
178 CITRUS JUICE CHARACTERISTICS

Rheology Measurement

Many instruments and methods are used to measure viscosities and apparent
viscosities. To compare results from one method or instrument with another, it
must be remembered that for non-Newtonian fluids the apparent viscosity is
characterized by the temperature and the shear rate. The apparent viscosity gen-
erally is expressed as centipoise ( 100 g / sec cm) and shear rate (sec - , ). Among
the methods used are procedures that measure the flow through a capillary tube
or orifice, the rate of a falling weight through the sample, the power consumed
in stirring, the penetration into a test sample, the rate and degree of spread on
a flat surface, ultrasonic vibration, and radioactive density measurements. For
non-Newtonian fluids, the most applicable and most commonly used method is
the rotation of a spindle or a cylinder within a coaxial cylindrical tube. These
instruments generally provide a consistent shear rate or rotational speed for
selected spindles, from which the torque needed to maintain that speed is mea-
sured and correlated with the apparent viscosity. The shear rate in such mea-
surements can be found by using:

( 12-1)

where R, is the radius of the cylindrical spindle, R2 is the radius of the cylin-
drical tube containing the sample, and a is the angular velocity of the spindle
(rpm) (Loncin and Merson 1979). The procedure outlined by the manufacturer
of each instrument should be followed in making apparent viscosity measure-
ments.
Newtonian methods of measuring apparent viscosities, such as measuring the
rate of fall of a heavy object through a sample or the rate of flow through a tube
or an orifice, generally involve varying shear rates throughout a single mea-
surement. For Newtonian fluids where the viscosity does not change with shear
rate, these methods are acceptable, but with non-Newtonian solutions, such as
citrus concentrates, the varying shear rates can give misleading results. Never-
theless, Newtonian methods can have value when applied to non-Newtonian
solutions in some cases. For example, if all that is desired is a pass/fail result,
Newtonian methods may suffice. Also, analysts developing in-house standards
can employ Newtonian methods if the product composition remains sufficiently
consistent.

QUESTIONS AND PROBLEMS

1. Define rheology, Newtonian fluid, non-Newtonian fluid, pseudoplastic, dilatent,


thixotropic, and rheopectic solutions.
2. How would citrus concentrates be defined in rheology?
CITRUS RHEOLOGY 179

3. How do pulp levels, Brixj acid ratio, pectinase enzyme actIvity, and temperature
affect the apparent viscosity of citrus concentrates?
4. Which piece of equipment is not generally affected by juice consistency: pipes, evap-
orators, extractors, chillers, bulk storage, or pumps?
5. What would be the shear rate of a rotary viscometer using a spindle with a radius of
1.0 cm and a sample container with a radius of 1.2 cm with an angular velocity of
100 rpm?

REFERENCES

Crandall, P. G., Chen, C. S., and Carter, R. D. 1982. Models for predicting viscosity of orange
juice concentrate, Food Tech., 36(5), 245-251.
Crandall, P. G., Davis, K. C., Carter, R. D., and Sadler, G. D. 1988. Viscosity reduction by
homogenization of orange juice concentrate in a pilot plant taste evaporator, J. Food Sci., 53(5),
1477-1481.
Ezell, G. H. 1959. Viscosity of concentrated orange and grapefruit juices, Food Tech., 13,9-13.
Kimball, D. A. 1986. Volumetric variations in sucrose solutions and equations that can be used to
replace specific gravity tables, J. Food Sci., 51 (2), 529-530.
Loncin, M. and Merson, R. L. 1979. Food Engineering, Principles and Select Applications. Ac-
ademic Press, New York, 34.
Chapter 13

Citrus Processing Varieties

Many factors affect the quality of citrus juices, including industrial practices,
fruit maturity, climate, soil conditions, rootstock, and fruit variety. Industrial
practices and fruit maturity have been discussed in detail in this text. Climate,
soil conditions, and rootstock are generally beyond the control of the processing
quality control department and/or processing plant. The variety of inbound juices
used in blending and/or product manufacture, however, is of interest and is
controlled to some degree by the processor, especially in regard to juices re-
ceived from outside the local area. Therefore, this chapter has been included to
give the processor a global picture of citrus varieties. Taxonomy that is related
to rootstocks, ornamentals, or other areas not directly relevant to citrus pro-
cessing has been omitted. Only those taxonomical parameters that concern cit-
rus products are considered.
For many years the diversity of citrus species and varieties was unknown.
Citrus species always have been and always will be undergoing natural and
manmade changes, which make classification an ongoing and controversial task.
Also, the effort to compare varieties grown in distant geographical areas and to
separate the effects of local conditions from varietal differences added to the
confusion. In addition, the separation of hybrids from true species remains
largely a matter of opinion and accepted practice. In 1967 Swingle and Reece
proposed 16 species of the Citrus subgenus that have generally been accepted
by the industry (Swingle and Reece 1967). Tanaka proposed 159 species of the
Citrus subgenus (Tanaka 1954). Tanaka's species may be of benefit to the hor-
ticulturist, but it is considered too complex for industrial use, especially to pro-
cessors. The author of this text also utilizes extensively the opinions and infor-
mation supplied by Hodgson (1967), Rangama, Govindarajan, and Raman
(1983), and Considine (1982).
Table 13-1 presents a taxonomical description ofthe commercially important
citrus species. The order in which the species appear represents general impor-
tance by groups of species that are similar. The commercial importance is a
relative and seasonal term that may vary from time to time. Other members of

180

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
CITRUS PROCESSING VARIETIES 181

Table 13-1. Taxonomy of edible citrus fruits.


Kingdom- Plant
Order-Geraniales
Suborder-Geraniineae
Class-Dicoty ledoneae
Subclass-Archichalmydeae
Division-Embryophyta
Subdivision-Angiospermeae
Family-Rutaceae
Subfamily-Aurantiodeae
Tribe-Citreae
Subtribe-Citrinae
Genus-Citus L.
Subgenus-Citrus
Species-Citrus sinensis (L.) Osbeck-Sweet Orange
Citrus aurantium L.-Sour or Seville Orange
Citrus paradisi Macfadyen-Grapefruit
Citrus grandis (L.) Osbeck-Pummelo
Citrus maxima (Burm.) Merrill-Pummelo
Citrus decumana L.-Pummelo
Citrus limon L. Burm. f.-Lemon
Citrus aurantifolia (Christm.) Swing.-Lime
Citrus reticulata Blanco-common Mandarin/Tangerine
Citrus unshiu Marc.-Satsuma Mandarin/Tangerine
Citrus deliciosa Tenore-Mediterranean Mandarin/Tangerine
Citrus nobilis Lourerio-King Mandarin/Tangerine
Citrus madurensis (Lourerio)-Calamondin Mandarin/Tangerine
Citrus medica L.-Citron
Main Varietal Groups
Citrus sinensis (L.) Osbeck-Sweet Orange
Common Orange
Acidless Orange
Pigmented or Blood Orange
Navel Orange
Citrus paradisi Macfadyen-Grapefruit
White or Common Grapefruit
Pigmented or Pink Grapefruit
Citrus grandis (L.) Osbeck, maxima (Burm.) Merrill, or decumana L.-Pummelos
White or Common
Pigmented or Pink
Acidless
182 CITRUS JUICE CHARACTERISTICS

the Rutaceae family are sometimes used for food products, such as the kumquats
of the Fortunella genus in the Citreae tribe. However, these products are of
minor importance compared to those found in the Citrus L. genus.

Sweet Oranges I Citrus sinensis IL.1 Osbeckl

This species constitutes by far the most important class of commercial citrus,
with about two-thirds of the citrus produced worldwide falling into this cate-
gory. Sweet oranges are known by different names around the world, including
"naranja" in Spain, "aranico" in Italy, "laranja" in Portugal, "malta" in
India, and "kan" in Japan. Sweet oranges rank behind only sour oranges and
mandarins for hardiness, except that mandarins are more susceptible to frost
injury to the fruit. Sweet oranges are used extensively for fresh fruit, but in the
United States and Brazil they are used primarily for juice products. Sweet or-
anges can be classified into four categories, including the common orange, na-
vel orange, blood orange, and acidless or sugar orange.

Common Oranges

About two-thirds of all sweet oranges fall into the common orange category.
Common oranges are referred to as white or blond oranges. In Spain they are
called' 'blanca," in Italy' 'biondo," and in France' 'blonde. " The predominant
variety in this group is the Valencia orange, which constitutes about half of all
the oranges grown in the United States. Valencia oranges are also the predom-
inant commercial variety of any type of citrus, one reason for this dominance
being their long growing season and their resulting ability to adapt to a wide
range of growing conditions. Therefore, this orange is grown in every major
orange-producing country in the world. Contrary to popular belief, the Valencia
orange came from the Azores Islands and perhaps from Portugal, not from the
well-known city of Valencia in southern Spain, which is also known for its
citrus production. This variety should not be confused with the Valencia Tem-
prana variety in Spain, which matures earlier than the Valencia and is a smaller
fruit.
Table 13-2 lists the major varieties found in the common orange group. Main
budlines and related strains are generally classified together under one variety,
especially when the literature describes them as indistinguishable. Synonyms,
as well as countries where the literature has reported that the variety is of com-
mercial importance, are listed alphabetically, along with subjective and relative
descriptions of flavor and color. This relative rating system attempts to provide
the processor with a comparison of varieties within a given species according
to the literature and should not be construed as absolute. Also, some varieties
may be of local use and interest only, and so are not listed here.
CITRUS PROCESSING VARIETIES 183

Table 13-2. General attributes of the common orange varieties of the


Citrus sinensis (l.) Osbeck or sweet orange species.
Variety Other Names Location (s) Flavor Color
Balta Pakistan
Belladonna Italy pleasant
Biondo Commune Beledi N. Africa pleasant
Communa- Egypt
Spain Greece
Koines-Greece Italy
Liscio Spain
Nostrale
Biondo Riccio Italy pleasant
Cadenera Cadena Fina Algeria excellent
Cadena sin Morocco
Jueso Spain
Precoce de
Valence
Precoce des
Canaries
Valence san
Pepins
Calabrese Calabrese Italy well flavored
Ovale
Ovale
Carvalhal Portugal
Castellana Spain sweet-low acid pale
Clanor Clan William S. Africa good
Don Jao Portugal
Fukuhara Japan
Hamlin Norris S. Africa sweet-low acid well colored
Algeria
Argentina
Brazil
Florida
India
Iran
Mexico
Homosasa Florida good
Joppa S. Africa light orange
Texas
Khettmali Katmali Israel excellent
Hitmali Lebanon
Macetera Spain unique
Maltaise Maltaise N. Africa mild medium well colored
Blonde Petite Jaffa
Portugaise
Blonde

(Table continued on p. /84)


184 CITRUS JUICE CHARACTERISTICS

Table 13-2. (Continued)


Variety Other Names Location(s) Flavor Color
Maltaise Ovale Maltaise Oval S. Africa mild pale
Garey's or California
California
Mediterra-
nean
Sweet
Marrs Marrs Early California sweet-lacking acid well colored
Iran
Texas
Mosambi Bombay-Dec- India insipid-low acid straw yellow
can Pakistan
Mosambique
Musami
Parson Brown Florida well flavored dull orange
Mexico
Turkey
Pera Rio Brazil good good
Pera Coroa Brazil good good
Pera Brazil rich well colored
Pera Natal Brazil rich deep color
Pineapple S. Africa rich-sweet light orange
Argentina
Brazil
Florida
India
Mexico
Premier S. Africa good
Queen S. Africa rich red-orange
Salustiana Salus Algeria rich-sweet
Iran
Morocco
Spain
Sathgudi Chini of S. S. India fair-sweet
India
Seleta Selecta Australia acidy
Siletta Brazil
Shamouti Chamouti N. Africa sweet light orange
Jaffoui S. Africa
Jaffa Egypt
Jaffoui China
Palestine Cyprus
Jaffa Greece
India
Iran
Israel
Lebanon
Syria
Turkey
CITRUS PROCESSING VARIETIES 185

Table 13-2. (Continued)


Variety Other Names Location(s) Flavor Color

Shamouti Masry Khalily White Egypt rich-sweet well colored


Egyptian
Shamouti
Tomango S. Africa
Valencia Valencia Late S. Africa good-acid
Hart's Tardiff Algeria
Hart Late Argentina
same as Arizona
Lou Gim Australia
Gong Brazil
Natal of California
Brazil China
Pope Egypt
Calderon Florida
Delta India
Midknight Iran
Tajamur Iraq
Israel
Jamaica
Lebonan
Mexico
Morocco
Spain
Pakistan
Turkey
Vema Bema Algeria sweet well colored
Bernia Mexico
Vernia Morocco
Bedmar Spain
Vicieda Viciedo Algeria well flavored pale
Morocco
Spain
Westin Brazil rich well colored

The literature cited early in this chapter also includes some information that
may be of interest to the processor. One can learn, for example, that the Bel-
ladonna variety may be the same as the Shamouti orange. The Calabrese variety
is the most important common orange in Italy. The Hamlin orange is the world's
principal early-season common orange. The Homosasa is one of Florida's old-
est varieties. The Macetera is considered excellent for processing because of its
high juice content and unique flavor. The Maltaise blonde closely resembles
the Shamouti and Shamouti Masry oranges. The Parson Brown is the earliest-
season common orange. The Sathgudi is the principal common orange in India.
186 CITRUS JUICE CHARACTERISTICS

Because the Shamouti orange is the most common sweet orange in North Africa
and the Near East, it sometimes is simply referred to as the "beledi" or com-
mon orange. This designation probably is misleading because other common
oranges are grown in the area as well. The Shamouti orange generally is not
considered to be a good processing orange because it lacks juice and has a
relatively poor color. The development of bitter compounds has also been re-
ported in the Shamouti oranges (Levi et al. 1974), as well as in the Balta,
Mosambi, and Pakistan Valencia. The varieties described as early-season in-
clude the Balta, Biondo Commune, Hamlin, Marrs, and Mosambi, with the
Parson Brown described as very early. Early to midseason fruits include the
Premier, Vicieda, and Westin. Midseason fruits include the Khettmali, Mace-
tera, Maltaise Blonde, Pera Rio, Pera Coroa, Pineapple, Queen, and Sathgudi.
The late mid season varieties include the Maltaise Ovale and the Seleta. The
late-season fruits include the Calabrese, Pera, Pera Natal, and Valencia.

Navel Oranges

Navel oranges are characterized by a rudimentary secondary fruit in the apex


of the primary fruit that resembles a navel. This feature is sometimes found in
some mandarins but occurs regularly only in navel oranges. Navel oranges are
the most popular eating oranges in the world, primarily because they are not
very juicy, the flesh has an excellent and rich flavor, and they are crisp, seed-
less, and easy to peel. However, a delayed limonin bitterness develops upon
processing, as described in Chapter 10.
Table 13-3 presents a general description of navel orange varieties in a man-
ner similar to that of Table 13-2. The flavor descriptions in the table do not
account for the delayed bitterness mentioned above because those descriptions
are intended for fresh fruit products. Debittered or late-season navel juices rival
common oranges in juice quality but take a back seat with respect to juice yield
and perhaps juice color. Also, navel trees are sensitive to unfavorable condi-
tions and/or neglect. The principal navel variety and the second most popular
all-around citrus variety is the Washington navel, which is quite unstable hor-
ticulturally and has given rise to all other navel varieties except the Australian
navel varieties and their derivatives. The Australian navels, grown to some
extent in California and South Africa, are later-season and juicier than Wash-
ington navels, with a tart flavor that lingers longer into the season. In Florida,
Washington navels produce poorly, leaving Florida to local navel varieties
(Summerfield, Glen, and Dream) that are of minor commercial and processing
importance. Very early-season varieties include the Bonanza, Leng, and Na-
velina. Early-season varieties include the Bajaninha Piracicaba, Oberholzer, Rio
Grande, and Thomson. Lane's Late is the only variety classified as late-season.
CITRUS PROCESSING VARIETIES 187

Table 13-3. General attributes of the navel orange varieties of the


Citrus sinensis (L.) Os beck or sweet orange species.
Variety Other Names Location(s) Flavor Color
Baianinha Bahianinha Brazil
Piracicaba California
Bonanza California sweet pale yellow
Bourouhaine Iran
Tunisia
Frost Arizona
Washington California
Morocco
Fukumotto Japan
Gillette California rich deep color
Lane's Late Australia
California
Leng Australia fair well colored
Navelate Spain less sprightly pale
Navelina Dalmau Morocco sweet deep color
Portugal
Spain
Oberholzer Oberholzer S. Africa
Palmer
Rio Grande California
Thomson Thomson Algeria good well colored
Improved California
Chile
Iran
Spain
Washington Atwood S. Africa rich deep color
Bahia Algeria
Baia Argentina Florida Morocco
Baiana Australia Iran Portugal
Fisher Brazil Iraq Spain
Riverside California Israel Turkey
China Lebanon
Egypt Mexico

Blood Oranges

Blood oranges are characterized by their reddish pigmentation, which is due


primarily to the presence of anthocyanins in the flesh of the fruit. In Spain,
blood oranges are referred to as "sanguin," in Italy as "sanguigna" or "san-
guinella," and in French-speaking countries as "sanguine." Blood oranges
make up about 40% of the oranges grown in Spain and a slightly higher per-
centage of those grown in Italy. Blood orange juice has a unique and highly
188 CITRUS JUICE CHARACTERISTICS

favored flavor and is considered the most delicious of all citrus juices. However,
the anthocyan ins have a tendency to fade during processing and storage that
gives the juice an undesirable muddy color. Activated charcoal has been used
commercially in Italy to remove the anthocyanins, restoring a healthy color to
the juice. This activated charcoal also removes limonin, which imparts a de-
layed bitterness to many blood varieties similar to that of navel juice. However,
the activated charcoal also removes significant amounts of vitamin C, which
cannot be replenished in the United States in 100% juice products without vi-
olating federal standards of identity. The color development in blood oranges
is directly proportional to the heat applied during the season. High temperatures
deepen the pigmentation.
Table 13-4 lists the main blood orange varieties. Blood oranges can be clas-
sified into three regional groups. The oldest group is the ordinary blood orange,
which is similar to the common orange in every way except the pigmentation.
It includes the Sanguinello Commune, Maltaise Sanguine, and other light blood
varieties such as the younger Moro and Tarocco varieties. The Doblefina group
includes the Doblefina of Spain, Entrefina, Spanish Sanguinelli, and Doblefina
Amelioree. The smallest group is the Shamouti or Palestine Jaffa Blood Orange
group, including the Shamouti Mawadri and the Mawadri Beledi. The latter is
the earliest-season blood orange. The Maltaise Sanguine and the Sanguinello
Commune are similar to the Sanguinello Moscato, the latter being the most
important commercial blood orange, which is grown primarily in Sicily. The
oldest blood orange is the Sanguigno Semplice. The Moro blood orange matures
very early, with midseason blood oranges including the Ruby, Sanguigno
Semplice, Sanguinello Commune, Sanguinello Moscato, Tarocco, and To-
mango. Late midseason blood oranges include the Doblefina, Doblefina Ame-
lioree, Maltaise Sanguine, Mutera, and Spanish Sanguinelli.

Acidless Oranges

Acidless or sugar oranges are characterized by their low or nonexistent acid


levels. In France they are called "douceatre" or "douce." In Spain they are
referred to as "sucrena," in Italy as "maltese" or "dolce," in North Africa
and the Near East as "meski," in Turkey as "lokkum" or "tounsi," in Egypt
as "succari," and in Brazil as "lima." Acidless oranges are generally too de-
void of acid to be processed without risk of the growth of pathogenic micro-
organisms. Some varieties, shown in Table 13-5, such as the Succari of Egypt,
reach Brix/ acid ratios of up to 100, too sweet to process. The sucrena of Spain
is the oldest acidless orange. The Vainiglia of Italy is generally of only local
use and interest. Acidless oranges are generally early-season fruits.
Table 13-4. General attributes of the blood orange varieties of the
Citrus sinensis (L.) Osbeck or sweet orange species.
Variety Other Names Location(s) Flavor Color
Blood Red Blood Red India very good variable
Malta W. Pakistan
Doblefina Ovale Sangre Algeria mild-pleasant variable
Sanguina Oval Morocco
Rojo Oval Spain
Sanguine Ovale
Morlotte
Blood Oval
Doblefina Grosse Algeria good variable
Amelioree Sanguine Morocco
Washington Spain
Sanguine
Washington
Sangre
Pedro Veyrat
Entrefina Inglesa Spain
Malta Blood Algeria
Maltaise Portugaise Algeria excellent good blood
Sanguine Iran variable
Tunisia
Mawadria Damawi Lebanon light blood
Beledi Mawadri Beladi Syria
Moro Belladonna California pleasant deep almost
Sanguigno Iraq violet red
Sicily
Mutera Spain rich-sweet lacks red
Ruby Ruby Blood California rich sometimes
Florida streaked red
Sanguigno Italy pleasant red streaks
Semplice
Sanguinello Italy pleasant deep red
Commune
Sanguinello Iran well flavored good blood
Moscato Sicily
Shamouti Shamouti Lebanon light blood
Mawadri Maouardi Syria
Spanish Sanguinelli Spain deep red and
Sanguinelli Sanguinella constant
Negra
Tarocco Tarocco dal Italy rich and well pig-
Muso Iraq sprightly mented
Tarocco di
Francofonte
Tarocco Liscio Calabrese Morocco rich and well pig-
Sanguigno Sicily sprightly mented
Tarocco Ovale Spain
Tomango S. Africa excellent red only in
cold winters

189
190 CITRUS JUICE CHARACTERISTICS

Table 13-5. General attirbutes of the acidless orange of the Citrus


sinensis (L.) Os beck or sweet orange species.
Variety Other Names Location(s) Flavor Color
Lima Brazil insipid light yellow
Succari Sukkari Egypt overly sweet pale
Sucrena Imperial Spain insipid good
Grano de Oro
Real
Canamiel
Vainiglia Vaniglia Italy sweet-
Maltaise slight
Dolce bitterness

SOUR ORANGES (Citrus aurantium L.)

Sour oranges are also referred to as bitter or Seville oranges. In Spain they are
called "naranja agria" or "amarga," in Italy "melangolo" or "arancio
amaro," in France "bigarade" or "orange amere," in Israel "khuskhash," in
West Pakistan "khatta," and in Japan "daidai." Sour oranges are generally
too bitter and sour to be processed into juice, and the oils are generally strong
and disagreeable. However, the trees are resistant to excess soil moisture, frost,
and neglect and thus are grown in areas prohibitive to other species. Sour or-
anges are used to make marmalades and, to some extent, essential oils. By
British standards, the quality of marmalades made from sour oranges surpasses
the quality of marmalades made from sweet oranges.
There are three basic types of sour oranges, the main varieties of which are
listed in Table 13-6. Common bitter oranges consist mainly of the Sevillano
variety, which is used extensively for the production of marmalades, essential
oils, and bitter juices used in drink bases in Spain and Australia, and is a late-
season fruit. The bittersweet group contains the essentially synonymous vari-
eties of the Bittersweet of Florida and the Paraguay or Apepu. This group is
grown mainly for essential oils. The variant bitter oranges are grown primarily
for perfumery and ornamentals.
Hybrids or species that closely resemble the sour orange include the Gunter
(c. maderaspatana Tan.), Bergamot (c. bergamia Risso), Sanbo (c. sulcata
Takahashi), and Myrtleleaf (c. myrtifolia Rafinesque). The Gunter is of im-
portance primarily in South India. Bergamot oil is used in Italy as a base for
cologne water. Sanbo remains popular in the Wakayama Prefecture of Japan
and the Myrtleleaf (Large Chinotto variety) is used for candied peel (marma-
lade) or crystallized whole in Italy.
CITRUS PROCESSING VARIETIES 191

Table 13-6. General attributes of the sour orange varieties of the


Citrus aurantium L. species. Other names for the sour orange are
the common bitter orange or the Seville orange.
Variety Other Names Location (s) Flavor Color
Bittersweet Bittersweet of Florida
Florida Paraguay
Paraguay Spain
Apepu
Kabusu Kabusudaidai Japan
Sevillano Agrio de Australia good for
Espana Spain marma-
Real lade
Sour Seville
(Related Hybrids that Closely Resemble the Sour Orange)
Bergamot Italy
Gunter Kitchli India pleasant pale orange
Vadlapudi with slight
bitterness
Myrtleleaf Chinotto China
Myrtle-leaf orange Florida
Italy
Sanbo Sanbokan Japan good

GRAPEFRUIT AND PUMMELOS

Grapefruit and pummelos (shaddocks) are closely related. In fact, many people
believe that the grapefruit is a hybrid or a variety of the pummelo. The grape-
fruit (so named, it is believed, because the fruit grows in clusters like grapes)
is recognized as the separate species Citrus paradisi Macfadyen. Grapefruit has
a highly distinctive flavor with a lighter color, whereas the flavor and the color
of pummelos vary widely and give rise to the three pummelo species-Citrus
grandis (L.) Osbeck, the most common, Citrus maxima (Burm.), and Citrus
decumana L. In France the pummelos are referred to as "pamplemousse," in
Italy as "pompelmo," in Spain as "pampelmus," and in Japan as "buntan"
or "zabon." Most pummelos are very thick-skinned and are worthless as a fresh
fruit or for juice. However, there are some that are of importance commercially
in the Orient. Pummelos are less cold-tolerant than grapefruit, and some of the
major varieties do not have a bitter flavor like that of grapefruit.
Tables 13-7 and 13-8 briefly describe commercially important grapefruit and
pummelo varieties. In Spain grapefruit are referred to as "toronja." They rank
third behind oranges and mandarins in world production. In processed products
the glucoside naringin imparts an immediate bitter flavor as well as delayed
192 CITRUS JUICE CHARACTERISTICS

Table 13-7. General attributes of grapefruit varieties of the Citrus


paradisi Macf. species.
Variety Other Names Location(s) Flavor Color

Common or White Grapefruit


Duncan China excellent buff-chamois
Florida
Marsh Marsh Seedless S. Africa good buff-chamois
White Marsh Argentina
Arizona
Australia
California
China
Cyprus
Egypt
Florida
Iran
Iraq
Israel
Jamaica
Spain
Texas
Triumph Jackson S. Africa lacks
bitter-
ness
Pigmented or Pink Grapefruit
Flame Florida
Henderson Ruby Red Florida slightly fades to am-
Texas sweet ber with
maturity
Ray Ruby Texas
Red Blush Ruby Argentina good slight pink
Red Marsh Arizona
Red Seedless California
Iran
Iraq
Texas
Rio Red Texas deep
Star Ruby Texas best flavor darkest
Thompson Argentina good chaimois or
China dark buff

bitterness from limonin. In Florida, a little less than half of the grapefruit that
is grown is processed. Grapefruit peel is used in the production of pectin and
essential oils. There are two basic types of grapefruit-common or white and
pigmented or pink. The late-season Marsh variety is by far the most popular
common grapefruit. The mid-early-season Duncan grapefruit is considered to
CITRUS PROCESSING VARIETIES 193

Table 13-8. General attributes of pummelo varieties of the Citrus


grandis (L.I Osbeck, Citrus maxima (Burm.). and
Citrus decumana l. species.
Variety Other Names Location(s) Flavor Color

Common or White Pummelos


Banpeiyu Pai You Japan excellent pale yellow
Pai Yau Taiwan
Hirado Hirado Buntan China pleasant, trace light greenish
Japan bitterness yellow
Kao Pan Kao Panne Thailand sweet, mildy lemon yellow
acid
Kao Phuang Siamese California acid
Mato Mato Buntan China lacking acid, light greenish
Japan sweet, trace yellow
of bitterness
Tahitian Moanalua Hawaii unique, excel- faintly amber
lent
Pigmented Pummelos
Ogami Egami Florida good deep pink al-
Japan most red
Pan dan Bener Java pleasant, red-fleshed
sweet,
slightly acid
Pandan Wangi Java pleasant, red-fleshed
sweet,
slightly acid
Siamese Pink Siam California grapefruit- pink-tinged
like, sub-
acid, trace
bitterness
Thong Dee California good pink -tinged
Florida

be the best flavored, setting the standard for all other varieties. It is a common
trend among varieties that the seedier ones (such as the Duncan) have a richer
flavor than the less seedy or seedless varieties (such as the Marsh). The Triumph
Grapefruit is another early-midseason grapefruit.
Pink grapefruit varieties are characterized by the presence of the pink to red
pigment of the carotenoid lycopene. Although attractive in a fresh fruit, this
pigmentation has a tendency to fade during processing and storage similar to
that of the anthocyanins in blood oranges. For this reason, pigmented grapefruit
juice is not popular. However, pink grapefruit juice cocktail contains pink
grapefruit juice along with sweeteners, colorants, and other ingredients de-
signed to give a pink grapefruit juice appearance without this color fading ef-
194 CITRUS JUICE CHARACTERISTICS

fect. Consequently grapefruit juice cocktail is somewhat popular. As with the


anthocyanins, heat is required during the growing season to develop the pig-
mentation. In the United States, the Red Blush variety is the most popular, with
highly pigmented varieties recently emerging (Star Ruby and Rio Red). The
Star Ruby is reported to have the best flavor among the pigmented varieties as
well as the deepest color. The Thompson grapefruit is considered a mid season
fruit.
Like grapefruit, pummelos are classified as common or white and pigmented
or pink. Common pummelos are moderately high in acid, and the pink pum-
melos range from light pink to deep red. Some pummelo varieties have a highly
distinctive and excellent flavor. A third class of pummelos is the acidless pum-
melo, which resembles the acidless orange mentioned above. Acid levels range
from less than 0.1 % to about 2.0 %, with Brixl acid ratios of up to 150. Some
varieties, such as the Tahitian pummelo of Hawaii, are of local use and interest
only. Early-season pummelos include the Kao Pan and Mato. Pummelos con-
sidered to be medium early-season fruits include the Banpeiyu, Hirado, and Kao
Phuang. The Thong Dee is a midseason fruit.
Several tangelo (tangerine x pummelo) hybrids are closely associated with
grapefruit and pummelos, along with the orangelo (orange x pummelo) variety
"chironja" of Puerto Rico, as shown in Table 13-9. The chironja hybrid is not
considered suitable for processing. The more important varieties include the
K-early of Florida, the poorman and Wheeny of New Zealand and Australia,
and the hassaku and natusdaidai of Japan. Tanaka classified the hassaku hybrid
as C. hassaku Hort. ex. Tan. (pummelo X mandarin) and the natsudaidai spe-
cies as C. natsudaidai Hayata (pummelo X sour orange or mandarin). Hassaku
juice is known to develop severe limonin bitterness with levels as high as 50
ppm. Nomilin, a known metabolic precursor of limonin, has been found to peak
about one month before limonin levels reach their maximum (Hashinaga and
Itoo 1983). It has also been found that freezing of natsudaidai juice ruptures
juice cell membranes in the juice pulp with leakage of additional bitter com-
pounds into the juice (Iwata and Ogata 1976). The melogold variety (common
grapefruit X acidless pummelo) is the most recent commercial hybrid.

MANDARINS OR TANGERINES

Mandarins or tangerines are known in Japan as "mikan, " in India as "suntura"


or "sangtra," in Italy and Spain as "mandarino," and in French-speaking
countries as "mandarine." In the Orient mandarins clearly dominate the citrus
industry, and they are important in many other parts of the world. Because the
characteristics of mandarins vary so widely, they are often regarded as exotics.
Mandarins are characterized by their loose and easily peeled rind, an open core,
and a deeper orange color than is found in most other types of citrus. The flavor
of mandarins also is unique and richer than that of most citrus species. Man-
CITRUS PROCESSING VARIETIES 195

Table 13-9. General attributes of hybrids that most closely resemble


grapefruit and pummelos.
Variety Other Names Location (s) Flavor Color

Orangelos
Chironja Puerto Rico mild, lacks yellow or-
grapefruit ange
bitterness
Tangelos
Hassaku (c. has- Hassaku Mikan Japan good, turns light yellow
saku Hort. ex. Hassaku Zubon bitter
Tanaka)
K-early Florida rather acid yellowish
orange
Melogold California good buff-chamois
Natsudaidai (c. Natsumikan Japan too acid for yellowish
natsudaidai Natsukan most orange
Hayata)
Orobanco California good buff-chamois
Poorman New Zealand Australia pleasantly reddish
Grapefruit New Zealand subacid,
Poorman Orange trace of
bitterness
Smooth Seville Smooth Flat Australia pleasantly reddish
Seville subacid, orange
trace of
bitterness
Wheeny Wheeny Australia good but straw color
Grapefruit New Zealand acid

darins rank second behind oranges in global importance and are more cold-
resistant than other types of citrus, except that freeze damage to the fruit can
be severe because of the loose nature of the rind. Increased heat during the
latter part of the season results in lower acid levels and milder juice. In Japan
about 15 % of the mandarins harvested are processed. Elsewhere, processed
mandarin juice is of less importance and is used primarily to enhance color in
light-colored orange juices. In the United States, up to 10 % mandarin juice can
be added to orange juice without declaration or violation of federal standards
of identity. There are four basic types of mandarins, which have been assigned
their own separate species classification.

Common Mandarin (C. reticulata Blanco)

The common mandarins, described in Table 13-10, are the most important
group. They are characterized by a tight rind. The Beauty variety is similar to
the Dancy, and the Campeona closely resembles the King variety in the King
196 CITRUS JUICE CHARACTERISTICS

Table 13-10. General attributes of the common mandarin varieties of


the Citrus reticulata Blanco species.
Variety Other Names Location(s) Flavor Color
Bakrai Rangurtype Iran
Beauty Beauty of Australia sprightly orange
Glen Retreat
Campeona Glen Argentina rich and orange
sprightly, me-
dium acid
Clementine N. Africa sweet, subacid deep orange
Algeria
Arizona
California
Iraq
Morocco
Spain
Tunisia
Coorg Orange India
Cravo Laranja Cravo Brazil mild deep orange
Dancy Argentina rich, sprightly, deep orange
Arizona medium high
California acid
China
Florida
Desi of Punjab India
Ellendale Ellendale Australia rich, pleasantly bright or-
Beauty subacid ange
Emperor Emperor of S. Africa pleasant light orange
Canton Australia
India
Fewtrell Fewtrell's Australia mild orange
Early
Indian Iraq
Imperial Australia pleasantly suba- pale
cid
Kashi Orange India
of Assam
Kinnow Arizona rich deep yel-
California lowish
West Pakistan orange
Lee Florida rich and sweet orange
Malvaiso Argentina pleasantly sub-
acid
Mandalina Lebanon pleasantly sub-
Syria acid
Murcott Murcott Argentina rich and sprightly high color
Honey Brazil orange
Smith Florida
Nova Florida pleasant deep orange
CITRUS PROCESSING VARIETIES 197

Table 13-10. (Continued)


Variety Other Names Location(s) Flavor Color

Ortanique Cuba rich orange


Jamaica
Reunion Island
Osceola Florida rich deep orange
Ponkan Nagpur Brazil mild and pleasant orange
Warnurco China
India
Pakistan
Philippines
Sri Lanka
Taiwan
Robinson Florida rich and sweet deep orange
Sikkim Darjeeling India
Orange
Sunburst Florida excellent
Tankan China rich and sweet deep orange
Japan
Taiwan
Wilking Brazil rich and sprightly deep orange
Morocco

mandarin group. The Lee, Robinson, Osceola, and Nova varieties are all sim-
ilar and are actually hybrids of the Clementine mandarin and the Orlando tan-
gelo. The Kinnow and Wilking varieties are hybrids of the King mandarin and
the Willow leaf. The Kinnow variety in West Pakistan is known to exhibit de-
layed limonin bitterness. The mandalina of Lebanon resembles the Dancy va-
riety. In the United States the Dancy tangerine is predominant with the Ponkan
variety dominating the Oriental markets, especially in China. In India the Pon-
kan is referred to as the "nagpur santra" and is the leading mandarin variety.
The very early-season fruits include the Cravo, Imperial, and Nova varieties.
Early-season fruits include the Clementine, Fewtrell, and Robinson varieties.
Early to midseason fruits include the Emperor, Lee, Osceola, Ponkan, and Sun-
burst. Midseason fruits include the Beauty, Dancy, and Wilking. Late midsea-
son fruits include the Ellendale, Emperor, Ortanique, and Tankan. Late-season
fruits include the Campeona and Murcott. Very late-season fruit includes the
Malvaiso variety.

Satsuma Mandarin (C. unshiu Marc.)

The Satsuma mandarin varieties are listed in Table 13-11, and, as can be seen,
dominate the Japanese citrus industry. Satsuma mandarins are also found in
198 CITRUS JUICE CHARACTERISTICS

Table 13-11. General attributes of the satsuma tangerine varieties of


the Citrus unshiu Marc. species.
Variety Other Names Location(s) Flavor Color
Aoe Wase Aoe Japan
Dobashi Beni Japan deep orange-
Spain red
Hayashi Unshiu Japan
Iseki Wase Iseki Japan
Ishikawa Ishikawa Japan excellent,
Unshiu sweet
Juuman Juman Japan rich
Kuno Unshiu Japan
Matsuyama Wase Matsuyama Japan
Miho Wase Miho Japan sweet
Mikan Japanese Mikan Japan
Miyagawa Wase Miyagawa Japan excellent
Nagahashi Japan semibright
Nankan-4 Japan
Okitsu Unshiu Japan
Okitsu Wase Japan
Owari Unshiu Owari Satsuma Japan rich but orange
subacid
Seto Unshiu Japan
Silverhill Owari Japan very sweet
Frost Owari
Sugiyama Unshiu Japan excellent,
sweet
Yonezawa Japan bright-col-
ored
(Satsuma varieties are also grown in California, China, and India but tbe exact varieties are not clear.)

significant quantities in many other parts of the world, and are considered the
hardiest of mandarins as well as the most cold-tolerant of citrus. Satsuma tan-
gerines generally are divided into five categories. The Wase Satsumas include
the early-season varieties (September-October) and represent one-fifth of all
Japanese mandarins. The oldest variety is the Aoe Wase. The Zairai group
includes old native varieties indigenous to Japan. The Owari group, the most
important, is grown in the Owari Province and is especially suited for the can-
ning of fruit sections. The Ikeda and Ikiri groups are primarily of local use and
interest only. Early-season varieties include the Aoe Wase, Iseki Wase, Mat-
suyama Wase, Miho Wase, Miyagawa Wase, Okitsu Unshiu, Okitsu Wase, and
Silverhill. The medium-early varieties include the Dobashi Beni and the Owari
Unshiu. The midseason varieties include the Nankan-4 and the Yonezawa. The
late-season varieties include the Ishikawa and the Sugiyama Unshiu.
CITRUS PROCESSING VARIETIES 199

Mediterranean Mandarin (C. deliciosa Tenore)

This group of mandarins, so named because they are primarily grown in the
Mediterranean basin, is sometimes referred to as the Willow leaf mandarins (see
Table 13-12). This group contains the broadest distribution of varieties, being
referred to as: "Ba Ahmed" in Morocco; "Blida," "Boufarik," or "Bougie"
in Algeria; "Bodrum" in Turkey; "Paterno," "Palemo," or "Avana Spe-
ciale" in Italy; "Nice" or "Provence" in France; "Valencia" in Spain; "Se-
tubal" or "Galego" in Portugal; "Baladi," "Effendi," or "Yousef" in Egypt
and the Near East; "Thorny" in Australia; "Mexirica" or "Do Rio" in Brazil;
"Chino" or Amarillo" in Mexico; and "Koina" in Greece. This group is the
second most important mandarin variety behind the common mandarin but is
being rapidly replaced by the Satsuma mandarins as well as the Clementine
mandarin. Some Chinese varieties have been reported to resemble Mediterra-
nean mandarins, including the Suhoikan variety. The Mediterranean variety is
considered a late-season fruit.

Table 13-12. General attributes of Mediterranean mandarin varieties


of the Citrus deliciosa Tenore species and the King Mandarin
varieties of the Citrus nobilis loureio species.
Variety Other Names Location (s) Flavor Color

Mediterranean Mandarins
Bergamota Argentina
Malaguina Argentina
Mediterranean Mediterranean N. Africa distinctly mild light
Common Algeria and plea- orange
Willow leaf Argentina santly aro-
Brazil matic,
Egypt sweet
Greece
Spain
Suhoikan China

King Mandarins
King Indo-China California rich deep orange
Mandarin China
Camboge Florida
Mandarin Indo-
Kunembo China
Malaysia
Okinawa
Taiwan
200 CITRUS JUICE CHARACTERISTICS

King Mandarin (C. nobilus Loureiro)

This group of mandarins includes a single commercial variety-the King variety


shown with the Mediterranean group in Table 13-12. King mandarins are among
the least cold-tolerant mandarins and are relatively unimportant as a commercial
variety. These mandarins are the largest in fruit size and the latest-maturing
among the mandarins as well.

Hybrids

Several important tangor and tangelo varieties that most closely resemble man-
darins are listed in Table 13-13. The most important hybrid in the United States
is the Temple tangor (c. sinensis X C. reticulata), which has been assigned
the species C. temple Hort. ex. Tan. and is considered a medium late-season
fruit. The Iyo mikan of Japan has been assigned the species C. iyo Hort. ex.
Tan. and is a mid season fruit. The Umatilla tangor is a cross between the Sat-

Table 13-13. General attributes of hybrids that most closely resemble


the mandarin species.
Variety Other Names Location(s) Flavor Color

Tangelos (mandarin X pummelo)


Minneola Arizona rich and tart orange
California
Florida
Orlando Arizona mildly sweet orange
California
Florida
Seminole Florida sprightly acid, rich orange
too tart
Thorton Florida mildly sweet pale OT-
Texas ange
Ugli Jamaica rich subacid orange
Tangors (mandarin x oranges)
Iyo Iyo Mikan Japan sweet orange
Sue Linda Florida smoother than orange
Temple
Temple Cuba rich and spicy orange
Florida
Jamaica
Umatilla Florida rich, acid orange
Others
Fallglo Florida pleasant excellent
Sudachi Japan
CITRUS PROCESSING VARIETIES 201

suma tangerine and the Ruby orange. The Minneola, Seminole, and Orlahdo
tangelos are all crosses of the Duncan grapefruit and the Dancy tangerine. The
Iyo tangor is known to exhibit delayed limonin bitterness. Of this group, the
Orlando tangelo is considered an early-season fruit, the Thorton tangelo is con-
sidered a mid season fruit, the Minneola is a medium late-season fruit, and the
Ugli is a late-season fruit. Other mandarin-like hybrids include the Fallgo
(Bower x Temple), an early-season fruit, and the Sudachi (c. ichangensis x
C. reticulata), the latter constituting the species C. sudachi Hort. Shirai.

LEMONS I C. limon IL.) Burm. t.)

Lemons are characterized by their light yellow color and their excessively high
acid content. Lemons once were used in the manufacture of citric acid but have
been replaced by more inexpensive methods. Lemons are referred to as "li-
mone" in Italy, "limon" in Spain, and "citron" in France, but are different
from the Mediterranean limetta (c. limeua Risso). They contain the widest
divergence of all citrus species. Lemons are primarily processed into juice and
lemonade, as well as pectin and lemon oil. Table 13-14 lists the main lemon
varieties. The Bema lemon is much like the Lisbon lemon, and the Interdonato
is the earliest-season lemon in Italy. The main varieties by far are the Eureka
and the Lisbon, with the latter generally replacing the former. The best-pro-
cessing lemon is said to be the Mesero, with the Monachello being resistant to
the mal secco disease. Lemons may have more than one crop per year and
sometimes several crops. The Bearss and Mesero are considered winter fruits,
with the Interdonato included as an early-season fruit. The Eureka lemon ma-
tures in the late winter, spring, and early summer, with the Lisbon lemon ma-
turing in the winter and early spring. The Femminello Ovale is a late winter
fruit. The sweet lemon variety dorshapo is of minor importance except in Ara-
bian countries, where it is highly favored. The related species limetta (c. li-
metta Risso) resembles the Dorshapo sweet and includes the single important
variety of Millsweet. Some evidence suggests that the elderly prefer the higher-
acidity drinks made from lemons.

LIMES

Limes are similar to lemons except that limes have a greener fruit and flesh
color than lemons and have a distinct and unique flavor and aroma. In Italy and
Spain limes are referred to as "lima," and in French-speaking countries they
are called "lime." In Arabian countries both lemons and limes are called "li-
mun," and in the Orient they are referred to as "nimbu" or "limbu." Limes
are the most tropical of all citrus and are generally preferred to lemons. India
is the largest producer of limes, which in the United States are grown almost
202 CITRUS JUICE CHARACTERISTICS

Table 13-14. General attributes of lemon varieties of the Citrus limon


(l.) Burm. f. species.
Variety Other Names Location(s) Flavor Color
Bearss Sicily Florida
Berna Verna Algeria
Bernia California
Vernia Morocco
Spain
Canton Rangpur China
Lime India
Japan
Eureka S. Africa highly greenish
Argentina acid yellow
Australia
California
China
Greece
Israel
Mexico
Pakistan
Femminello Commune Sicily high acid
Ovale Ruvittaru
Interdonato Speciale Sicily high acid greenish
slight bit- yellow
terness
Karystini Greece
Lisbon Algeria very acid pale greenish
California yellow
China
Greece
Mexico
Morocco
Mesero Fino Italy high acid
Primitiori Spain
Monachello Moscatello Italy lacking acid
Polyphoros Greece
Sicilian lemon Brazil
Vilafranca Italy high acid greenish yel-
low

entirely in southern Florida. Limes have the highest acid content of all citrus
but are lower in vitamin C and other nutrients compared to lemons. Limes are
used mainly as additives to alcoholic beverages, in limeade, and to produce
lime oil. Table 13-15 lists the main lime varieties.
Limes can be classified into three species. The small-fruited group (c. au-
rantifolia Swing.) consists of a single commercial variety, West Indian, which
is the most commercially important of all lime varieties. The large-fruited group
CITRUS PROCESSING VARIETIES 203

Table 13-15. General attributes of lime varieties, including the small-


fruited (Citrus aurantifolia Swing.), the large-fruited (Citrus latifolia
Tan.), and the sweet lime (Citrus limettoides Tan.) species. Also,
lemon(lime)-like hybrids are listed.
Variety Other Names Location(s) Flavor Color

Small Fruit Limes


West Indian Mexican Brazil highly greenish
Key California acid, distinct yellow
China aroma
Egypt
Florida
India
Iran
Malaysia
Mexico
Large Fruited
Bearss Bearss Florida
Seedless
Persian
Tahiti Persian Australia very acid, true greenish yel-
Brazil lime flavor low
California
Florida
Sweet Lime
Indian Palestine California insipidly sweet, straw yellow
Egypt slight bitter
India after taste
Latin Amer-
ica
Near East
Pakistan
Lemon/Lime-Like Hybrids
Galgal Gulgal India very sour, trace pale yellow
Kumaon lemon of bitterness
Marrakech Moroccan limetta Morocco very sour high pale yellow
limonette Limun Boussera acid
Mediterranean Tunisian Sweet Italy acidless, insip-
Sweet Lime Lime Tunisia idly sweet
Meyer N. Africa acidyand light orange
Florida lemon-like
New Zealand
Texas
204 CITRUS JUICE CHARACTERISTICS

(c. [atifolia Tan.) is second in importance, with two of the varieties, Bearss
and Tahiti, closely resembling each other. The Sahesli lime of Tunisian and the
Pond lime of Hawaii are very similar to the Bearss lime described in the table.
The sweet lime (c. limettoides Tan.) is considered too insipidly sweet in the
United States but is popular in India and the Near East. The single variety,
Indian or Palestine, is referred to as "mitha nimbu" in India and "limun helou"
or "sucarri" in Egypt. In California the dessert and coastal fruit of this variety
exhibit marked differences. Sweet limes are often used to prevent fevers and
liver complaints. The West Indian and Tahiti limes are mainly winter fruits,
along with the Meyer hybrid. Some lemon and lime-like hybrids also are de-
scribed in Table 13-15.

CITRUS GEOGRAPHY AND QUALITY CONTROL

As mentioned early in this chapter, citrus varieties grown in distant localities


become important when citrus products are brought in from those areas and
used in blending or in the making of various products. Table 13-16 is a listing
of citrus varieties grown in the different citrus-producing areas. This table can
be used by quality control personnel in explaining characteristics of juice re-
ceived from these countries, states, or localities. Even though the commercial
importance of these varieties changes, Table 13-16 will give the processor a
general idea of the citrus industry in these areas. For example, if a lot of con-
centrate from Brazil has a significantly different flavor from previous lots, in-
vestigation may reveal that the difference is due to a varietal change rather than
a processing, storage, or shipping error.

Table 13-16. Citrus varieties believed to be of commercial importance


by the author, listed by country, state, or region.
Algeria Common Mandarins Common Grapefruit
Common Oranges Clementine Marsh
Cadenera Mediterranean Mandarins Pink Grapefruit
Salustiana Mediterranean Red Blush
Valencia Lemon Thompson
Vema Bema Common Mandarins
Navel Oranges Lisbon Campeona
Thomson Dancy
Washington Argentina Murcott
Blood Oranges Common Oranges Mediterranean Mandarins
Doblefina Hamlin Bergamota
Doblefina Pineapple Malaguina
Amerlioreo Valencia Mediterranean
Maltaise Navel Oranges Lemons
Sanguine Washington Eureka
CITRUS PROCESSING VARIETIES 205

Table 13-16. (Continued)


Arizona Pera Grapefruit Hybrids
Common Oranges Pera Natal Melogold
Valencia Pineapple Orobanco
Navel Oranges Valencia Common Mandarins
Frost Westin Clementine
Washington Navel Oranges Dancy
Common Grapefruit Baianinha Kinnow
Marsh Piracicaba King Mandarins
Pink Grapefruit Washington King
Red Blush Acidless Oranges Mandarin Hybrids
Common Mandarins Lima Minneola
Clementine Common Mandarins Orlando
Dancy Carvo Lemons
Kinnow Murcott Bema
Mandarin Hybrids Ponkan Eureka
Minneola Wilking Lisbon
Orlando Mediterranean Mandarins Limes
Australia Mediterranean West Indian
Common Oranges Lemons Tahiti
Seleta Sicilian lemon Indian
Valencia Limes
West Indian China
Navel Oranges
Lane's Late Tahiti Common Oranges
Shamouti
Leng
Valencia
Washington California
Sour Oranges Navel Oranges
Common Oranges Washington
Sour Seville Maltaise Ovale Common Grapefruit
Common Grapefruit Valencia Duncan
Marsh Navel Oranges Marsh
Grapefruit-like Hybrids Baianinha Common Pummelos
Poorman Piracicaba Hirado
Smooth Bonanza Mato
Seville Frost Common Mandarins
Wheeny Washington Ponkan
Common Mandarins Gillette Tankan
Beauty Rio Grande King Mandarins
Ellendale Thomson King
Emperor Washington
Fewtrell Mediterranean Mandarins
Blood Oranges Suhoikan
Imperial Moro Lemons
Limes Ruby
Tahiti Eureka
Common Grapefruit Lisbon
Brazil Marsh Limes
Common Oranges Pink Grapefruit West Indian
Barao Red Blush
Hamlin Pink Pummelos Cuba
Pera Rio Siamese Pil)k Common Mandarins
Pera Coroa Thong Dee Shamouti
206 CITRUS JUICE CHARACTERISTICS

Table 13-16. (Continued)


Cuba (Con!.) Osceola Kinnow
Common Grapefruit Robinson Ponkan
Marsh Sunburst Sikkim
Egypt King Mandarins Lemons
Common Oranges King Canton
Biondo Commune Mandarin Hybrids Limes
Shamouti Minneola West Indian
Shamouti Masry Orlando Indian
Valencia Seminole Lemon Hybrids
Navel Oranges Thorton Galgal
Washington Sue Linda
Acidless Oranges Temple Iran
Succari Umatilla Common Oranges
Common Grapefruit Fallglo Shamouti
Marsh Lemons Valencia
Mediterranean Mandarins Bearss Navel Oranges
Mediterranean Limes Bourouhaine
Limes West Indian Thomson
West Indian Bearss Washillgton
Indian Tahiti Blood Oranges
Florida Greece Maltaise
Common Oranges Common Oranges Sanguine
Hamlin Biondo Sanguinello
Homosasa Commune Moscato
Parson Brown Shamouti Common Grapefruit
Pineapple Mediterranean Mandarins Marsh
Valencia Mediterranean Pink Grapefruit
Navel Oranges Lemons Red Blush
Washington Eureka Common Mandarins
Blood Oranges Karystini Bakrai
Ruby Lisbon Limes
Sour Oranges Polyphoros West Indian
Bittersweet India
Common Grapefruit Common Oranges Iraq
Duncan Hamlin Common Oranges
Marsh Mosambi Valencia
Pink Grapefruit Pineapple Navel Oranges
Flame Sathgudi Washington
Henderson Shamouti Blood Oranges
Pink Pummelos Valencia Moro
Ogami Blood Oranges Tarocco
Thong Dee Blood Red Common Grapefruit
Grapefruit Hybrids Common Mandarins Marsh
K-early Coorg Orange Pink Grapefruit
Common Mandarins Desi of Punjab Red Blush
Lee Emperor Common Mandarins
Murcott Kahsi Orange Clementine
Nova Of Assam Indian
CITRUS PROCESSING VARIETIES 207

Table 13-16. (Continued)


Israel Common Mandarin Java
Common Oranges Ortanique Pink Pummelos
Khettmali Mandarin Hybrids Pandan Bener
Shamouti Ugli Pandan Wangi
Valencia Temple Lebanon
Navel Oranges Common Oranges
Japan
Washington Khettmali
Navel Oranges
Common Grapefruit Valencia
Marsh Fukumotto
Sour Oranges Navel Oranges
Lemons Washington
Eureka Sanbo
Common Pummelos Blood Oranges
Italy Banpeiyu Mawadri Beledi
Common Oranges Hirado Shamouti
Belladonna Mato Mawadri
Biondo Grapefruit Hybrids Common Mandarins
Commune Hassaku Mandalina
Biondo Riccio Natsudaidai Malaysia
Calabrese Common Mandarins King Mandarins
Blood Oranges Tankan King
Moro Satsuma Mandarins Limes
Sanguigno Aoe Wase West Indian
Semplice Dobashi Beni
Sanguinello Hayashi Mexico
Commune Unshiu Common Oranges
Sanguinelio Iseki Wase Hamlin
Moscato Ishikawa Parson Brown
Tarocco Unshiu Pineapple
Tarocco Juuman Valencia
Liscio Kuno Unshiu Vema
Sour Oranges Matsuyama Wase Navel Oranges
Bergamot Miho Wase Washington
Acidless Oranges Mikan Lemons
Vainiglia Miyagawa Wase Eureka
Mediterranean Mandarins Nagahashi Lisbon
Mediterranean Nankan-4 Limes
Lemons Okitsu Unshiu West Indian
Femminello Okitsu Wase Morocco
Ovale Owari Unshiu Common Oranges
Interdonato Seto Unshiu Cadenera
Mesero Silverhill Salustiana
Monachello Sugiyama Valencia
Vilafranca Unshiu Vema
Lemon Hybrids Yonezawa Vicieda
Mediterranean Mandarin Hybrids Navel Oranges
Sweet Lime Iyo Frost
Jamaica Sudachi Washington
Common Grapefruit Lemon Navelina
Marsh Canton Washington
208 CITRUS JUICE CHARACTERISTICS

Table 13-16. (Continued)


Morocco (Cont.) Common Mandarins Salustiana
Blood Oranges Ponkan Valencia
Doblefina Portugal Vema
Doblefina Common Oranges Vicieda
Amelioree Carvalhal Navel Oranges
Tarocco Don Jao Navelate
Liscio Navel Oranges Navelina
Common Mandarins Washington Thomson
Clementine Washington
Wilking Puerto Rico Blood Oranges
Lemons Grapefruit Hybrids Doblefina
Berna Chironja Doblefina
Lisbon Reunion Island Amelioree
Lemon Hybrids Common Mandarins Entrefina
Marrakech Ortanique Mutera
Ii monette Spanish
Sri Lanka
New Zealand Sanguinelli
Common Mandarins
Grapefruit Hybrids Tarocco Liscio
Ponkan
Poorman Sour Oranges
Wheeny South Africa Bittersweet
Lemon Hybrids Common Oranges Sevillano
Meyer Clanor Acidless Oranges
Hamlin Sucrena
North Africa
Joppa Common Grapefruit
Common Oranges
Maltaise Marsh
Biondo Commune
Ovale Common Mandarins
Maltaise
Pineapple Clementine
Blonde
Premier Satsuma Mandarins
Shamouti
Queen Dobashi Beni
Common Mandarins
Shamouti Mediterranean Mandarins
Clementine
Tomango Mediterranean
Mediterranean Mandarins
Valencia Lemons
Mediterranean
Navel Oranges Berna
Lemon Hybrids
Oberholzer Mesero
Meyer
Washington
Okinawa Common Grapefruit Syria
King Mandarin Marsh Navel Oranges
King Triumph Washington
Pakistan Common Mandarins Blood Oranges
Common Oranges Emperor Mawadri
Malta Lemons Beledi
Blood Oranges Eureka Shamouti
Blood Red Spain Mawadri
Common Mandarins Common Oranges Common Mandarins
Kinnow Biondo Mandalina
Pokan Commune
Philippines Cadenera Taiwan
Pink Pummelos Castellana Common Pummelos
Siamese Pink Macetera Banpeiyu
CITRUS PROCESSING VARIETIES 209

Table 13-16. (Continued)


Common Mandarins Ray Ruby Common Mandarins
Ponkan Red Blush Clementine
Tankan Rio Red Lemon Hybrids
King Mandarins Star Ruby Mediterranean
King Thailand Sweet Lime

Texas Common Pummelos


Common Oranges Kao Pan Turkey
Marrs Kao Phuang Common Oranges
Common Grapefruit Tunisia Parson Brown
Marsh Blood Oranges Valencia
Pink Grapefruit Maltaise Navel Oranges
Henderson Sanguine Washington

QUESTIONS

1. What is the most commercially important citrus species?


2. What are the two most important varieties commercially among all spe-
cies?
3. What are the main differences between common and navel sweet or-
anges?
4. What is the main pigment in blood oranges, and what effect does pro-
cessing have on it?
5. Which citrus juice species is believed to have the best flavor? The best
color?
6. Which citrus variety makes the best marmalades?
7. Which of each pair generally has the better flavor: (a) seedy or seedless
varieties; (b) light or dark pigmented varieties?
8. What is the main pigment found in grapefruit and pummelos, and what
is the effect of processing on this pigment?
9. What are the two main lemon varieties?
10. Which citrus species is the most tropical?

REFERENCES
Considine, G. D. 1982. Foods and Food Production Encyclopedia. Van Nostrand Reinhold Com-
pany, New York, 410-414.
Hashinaga, F. and Itoo, S. 1983. Seasonal changes in limonoids in Hassaku and pummelo fruits.
l. lap. Soc. Hort. Sci., 51 (4), 485-492.
Hodgson, R. W. 1967. Horticultural varieties of citrus. In The Citrus Industry I, W. Rether, H. J.
Webber, and L. D. Batchelor, eds. Division of Ag. Sciences, University of California, Berkeley,
Calif., 431-580.
Iwata, T. and Ogata, K. 1976. l. lap. Soc. Hort. Sci., 45(2),187-191.
210 CITRUS JUICE CHARACTERISTICS

Levi, A. et al. 1974. The bitter principle in Shamouti orange juice. 1. Seasonal changes and dis-
tribution in different parts of the fruit, Lebensm.-Wiss. Techno!', 7,234-235.
Rangama, S., Govindarajan, V. S., and Raman, K. V. R. 1983. Citrus fruit varieties, chemistry,
technology, quality evaluation, and analytical chemistry II (Review), Chemical Rubber Company
Critical Reviews in Food Science and Nutrition, 18(4),313-386.
Swingle, W. T. and Reece, P. C. 1967. The botany of citrus and its wild relatives. In The Citrus
Industry. Division of Ag. Sciences, University of California, Berkeley, Calif., publication 4012.
Tanaka, T. 1954. Species problems in citrus (Revisio Aurantiacearium, IX), Japan Soc. Prom.
Sci., Ueno, Tokyo, Japan.
Chapter 14

Inspections

Several basic factors affect or contribute to the sanitary condition or standing


of a citrus processing or bottling plant. One is geographic location. Rural, sub-
urban, and metropolitan areas each have different sanitation problems. Insect
and rodent habitats as well as waste disposal facilities exert an influence on
plant sanitation. Weather conditions and climate also playa significant role in
sanitation problems. Temperatures, humidity, and precipitation affect insect and
rodent fauna and activity, which vary throughout the year as well as from one
geographical location to another. Also, sanitation methods and precautions fol-
lowed during daylight hours differ from those used at night when insects and
rodents are most active and attracted to lights.
The engineering of the plant is an important factor. Construction, location,
and cleaning facilities for equipment can make a dramatic impact on plant san-
itation. Leaks and drainage problems can cause unsightly accumulations. An-
other important consideration in the effectiveness of a sanitation program is the
attitude and capability of plant management regarding plant sanitation. The
"sanitation quotient" of a plant must start at the top. Even so, the attitudes of
employees must be inbred, along with follow-through, in the observance of
company policies and procedures, in order for any sanitation program to be
successful. The foundation of any sanitation program is a good system of in-
spections. These inspections ensure sanitation awareness as well as implemen-
tation of the existing program.
There are several reasons why sanitation is important. In the citrus industry,
product quality assurance is essential. Contaminated or spoiled products gen-
erally do not pose health concerns because of the nonpathogenic characteristics
of microorganisms in citrus juices, but broken glass or pieces of metal in the
product can be dangerous to the consumer. Also, if flavor and appearance are
irrevocably marred, serious financial losses are possible. Because constant sur-
veillance of processing operations generally is not feasible, the concerns of a
sanitation program must go beyond visible contamination and spoilage of citrus
products. The program must eliminate or minimize "potential" contamination

213

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
214 CITRUS JUICE SANITATION

and spoilage. Another objective of a sanitation program is to facilitate a healthy


and attractive appearance not only in citrus products, but in citrus processing
equipment. Customer and public confidence is enhanced by a plant that looks
clean. Also, employees work better in a clean and healthy environment, just as
athletes compete better in clean and attractive uniforms. The final reason for a
sanitation program is simple: it is a legal requirement.

ROLE OF THE FOOD AND DRUG ADMINISTRATION

The United States Food and Drug Administration (FDA) has the responsibility
for regulating and ensuring the sanitation and safety of all foods and drugs
produced or imported into the United States according to the Federal Food,
Drug, and Cosmetic Act enacted on June 25, 1938. This Act has since been
modified and incorporated into the Code of Federal Regulations (CFR). In this
code, Title 21 part 110 refers to sanitation and defines the "good manufacturing
practice" that is required of all food processors. Some of the main features of
good manufacturing practice as outlined in the code are the following:

1. No person infected by a communicable disease can work in a food plant.


2. Food plant employees must wear clean clothes, wash their hands, re-
move jewelry or other items that cannot be sanitized as well as loose
items that could fall into the food, keep their gloves sanitary, and wear
hair restraints.
3. No eating, drinking, or use of any tobacco products is permitted in food
plants or where processing utensils or equipment is stored. Personal be-
longings should be kept out of food processing areas.
4. Food plant grounds should be kept so as not to contaminate the food
product (there should be no dusty roads or yards, poor drainage, or har-
borages for rodents, insects, or other pests).
5. Food plants should be designed and constructed to allow sufficient space
for processing and storage, in order to avoid food contamination.
6. In food plants, extraneous material or chemicals should not be stored or
used so as to cause contamination.
7. Food plants should provide adequate lighting for handwashing areas,
locker rooms, restrooms, and where food ingredients are stored and used,
as well as adequate handwashing facilities. Light bulbs should be cov-
ered so that breakage will not contaminate the food.
8. Adequate ventilation should be provided to minimize off odors or fumes
that could contaminate the food.
9. There should be adequate screening to protect against birds, animals,
and other vermin. No animals of any kind should be allowed into a food
plant other than those that must be used as raw material.
INSPECTION 215

10. There should be an ample potable water supply for proper cleaning, of
sufficient quality that it will not contaminate the food.
11. Sewage and refuse disposal should be done in an adequate manner to
avoid food contamination.
12. Doors to restrooms should be self-closing and not open directly into pro-
cessing areas. Double doors should be used if necessary.
13. All equipment and utensils used in processing should be cleaned suffi-
ciently and often enough that they will not contaminate the food, and
they should be stored in a sanitary fashion.
14. All ingredients or raw materials should be inspected to ensure that they
are clean, wholesome, and fit for human consumption.
15. The food processing should be monitored in such a way as to ensure the
sanitation of the product, by procedures including, but not limited to,
container inspections, temperature monitoring, sanitary inspections, and
microbial monitoring.
16. Food products should be so labeled as to allow proper product identifi-
cation, and records concerning product quality should be retained for at
least the shelf life of the product, or no more than two years. The ad-
dition of any defective lot renders the final product defective, regardless
of the degree of the defect.
17. Storage and shipment of food products should be done in such a way as
not to contaminate the food.

FDA Inspections

To enforce the federal regulations regarding good manufacturing practice, the


FDA conducts periodic inspections of food plants. These inspections generally
are unannounced, and can range from general surveillance to investigation of a
complaint or a specific problem. FDA inspectors should always be treated with
respect and courtesy, as they are ambassadors of the public, the ultimate con-
sumers of citrus products. Such courteous treatment also produces the best
working relationship. Three phases constitute a proper and effective FDA in-
spection.

Preinspection Phase
When an FDA representative appears at the plant, the first thing one should do
is arrange for a preinspection conference. Those persons who should attend
include the quality control manager, the chief executive officer of the company
(CEO), and the FDA inspector. FDA inspectors are required to inspect plants
at reasonable times and not during weekends, holidays, or off shifts. Each com-
pany should maintain an FDA file. The inspector should be required to show
216 CITRUS JUICE SANITATION

his or her credentials, and these credentials should be recorded in the file along
with the inspector's name and the date and time of the inspection. FDA in-
spectors do not have unlimited authority to access company records except for
shipping documents of interstate commerce under section 703 of the Act and
processing records of low acid foods. They also are not granted authority to
take photographs. It must be remembered that volunteered information can be
used against a processor in a court oflaw. However, the best policy is to always
be prepared for an FDA inspection through a proper sanitation program. Then
full cooperation with FDA inspectors can be a pleasant experience for all con-
cerned, perhaps even a time to show off a little.
The preinspection conference is a good time for processors to review the
results of the last inspection and clarify any questions they or the inspector may
have. The FDA file should include information on all cleaners and additives
used in the plant as well as all paperwork from previous inspections. Also, the
file may include informative pamphlets and brochures such as "FDA Inspection
Authority" (NFPA Bulletin 39-L, NFPA, 1133-20th Street, Northwest, Wash-
ington, D.C. 20036) or "Good Manufacturing Practice in Manufacturing, Pro-
cessing, Packing, or Holding Human Food" (U.S. Department of Health, Ed-
ucation, and Welfare, Public Health Service, Food and Drug Administration,
HFF-326, 200 C Street, Southwest, Washington, D.C. 20204). Some compa-
nies have a form letter that they give to the inspector on arrival that outlines
company policy about what the inspector will or will not be allowed to do
beyond his or her inherent authority. The preinspection conference presents a
good opportunity for those involved to go over these policies.

Inspection Phase
FDA inspectors should always be accompanied while inspecting the plant, pref-
erably by the quality control manager. The names and titles of those persons
who accompany the inspector should be recorded in the file. If a USDA in-
spector is present, he or she may wish to accompany the inspector as well. The
FDA inspector has authority to inspect all areas of the plant without warrant
and should be allowed to do so. During the inspection the inspector will fill out
form FD-482, shown in Fig. 14-1, a copy of which should be kept with the
FDA file. If the inspector takes any samples, he or she should issue a receipt
for them, which also is kept in the file. It is recommended that the company
take duplicate samples. The form used by the FDA inspector as a sample receipt
is shown in Fig. 14-2. If any problems are found, the inspector is required to
notify the company promptly by using FD-483, shown in Fig. 14-3.

Postinspection Phase
After the inspection, a postinspection conference should be held by the same
people who attended the preinspection conference. If any of the above forms
INSPECTION 217

DEPARTMENT OF HEAL TH AND HUMAN SERVICES


PUBLIC HEALTH SERVICE

Notice of Ins on it hereby given pursuant to Section 704{a) & (e' of the Federal Food~ Orug~ and Cosmetic Act [21
U.S.C. 374(01 8. (olJ'and/or Part F or G, Title III of the Public Hoalth S.",ice Act [42 U.S.C. 262·264)2

purpose, may dUring all reasonable hours enter and Inspect any estab·
Iishment for the propagation or manufacture and preparation of any
VirUS, serum, tOXin, antllOXtn, vaccme, blood. blood component ordenv-
lSec. 704. (a) FOf" purposes of enforcement of this Act, officers or em- atlve. allergenic product or other product aforesaId for sale. barter, or
plovees dul.,. designated bV the Secretary, upon presenting approp- exchange m the D,stTict of Columbia. or to be sent, carTied. or brought
r1"le credentials and wfltten notice to the owner. ope rat Of. or agent In from any State or possession Into any other State or posesslon or Into
charge, are iluthorlzed (1) to enter, at reasonable times. any lactory any foreign country, or from any foreign country Into any State or
warehouse. or establishment In which luod. drugs. devices, or cosmet posseSSion
ICS are manufactured, processed. packed. or held. for Introduction Into
mterstate commerce or after such introduction. or to enter any vehicle
being used to transport or hold sucb food. drugs, devices, or cosmetiCs In Part F - •• " Control of Radiation
Interstate commerce. and (2) to Inspect. at reasonable limes and wlthm
reasonable tlmlts and In a reasonable manner. such factory, ware· Sec 360 A(eI) '"If the Secretary finds for good cause that tbe methods,
house, establishment. or vehicle and all perTment eqUipment. finished tests, or programs related to electroniC product radiation safey In a
onel unfinished millerlals containers, and labeling therein In thp ril<;e particular factory, warehouse, or establishment In whIch electronic
of any factory, warehouse, establishment, or consulting laboratory in products are manufactured or held. may not be adequate or reliable,
which prescription drugs or restricted devices are manufactured, proc- officers or employees duly designated by the Secretary, upon presenting
essed, packed, or held, inspection shall extend to all things therein approprlBte credentials and a written notice to the owner. operator, or
(including records, files, papers, processes, controls, and fiICilities) agent III cbarge, are thereafter authOrized (1) to enter. at reasonable
bearing on whether prescription drugs or restricted devices which are times any area In such factory, warehouse. or establishment In which
adulterated or misbranded within the meaning of this Act, or which the manufacturers tests (Of resting programs) reqUired by sectIon
may not be manufactured, introduc:ed into interstate commerce, or 358(h) are carTied out and (2) to Inspect. at reasonable times and WIthIn
sold, or offered for sale by reason of any provision of this Act, have reasonable limits and In a reasonable manner. the facilities and proce·
been or are being manufactured, processed, packed. transported, or dures wllilin such area wblch are related to electroniC product radla1lon
held in an.,. such place, or otherwise bearing on violation of this Act. safety Each such Inspection sh;]11 be commenced and completed With
No inspection authorized by the preceding sentence shall extend to reasonable promptness In addition to otber grounds upon whIch good
financial data, sales data other than shipment data, pricing data, cause may be found for purposes of thiS subsection. good cause Will be
personnel data (other than data as to qulllHications of technical and conSidered to eXist In any case wllere the manufacturer has Introduced
professional personnel performing functions subject to this Act), and Into commerce any electroniC product which does not comply With an
research data (other than data, relating to new drugs and antibiotic applicable standard prescnbed under thiS subpart and With respect to
drugs and devices anc., subject to reporting IJnd inspection under regu- which no exempllon Irom the notificatIOn requirements has been
lations lawfully issued pursuant to section 505(i) or (j), section SOl(d} granted by Ole Secretary under sectIOn 359(a~2) or 359(e) ..
or (g), sections 512(1} or (m), section 519, or 520(g}, and data relating
to other drugs or devices which in the case of a new drug would be (b) Every manufacturer of electroniC products shall establish and
subject to reporting or inspection under lawful regulations issued pur- maintain such records (mc/udmg restmg records). make such reports.
suant to section 505(j)). A separate notice shall be given for each such and proVide such mlormatlon, as the Secretary may reasonably requITe
inspection, but a notice shall not be required for each entry made to enable him to determine whether such manufacturer has acted or IS
during the period covered by the inspection. Each such inspection shall acting In compliance With thiS subpart and standards preSCribed pursu'
be commenced and completed with reasonable promptness. ant to thiS subpart and shall. upon request of an officer or employee duly
deSignated by the Secretary, perml! sucb officer or employee!O Inspect
Sec 704(e) Every person reqUired under section 519 or 520(g) to main·
appropriate books, papers, records and documents relevant to deter
lam records and every person who IS In charge or custody of such
ITllnlng wllether such manufacturer has acted or IS actIng In complIance
recorris shall upon request of an officer or employee deSIgnated by the
With standards prescTlbed pursuant to section 359(a)
Secretary. permit such officer or employee at all reasonable times to
have access to and to copy and verify, such records
(f) , The Secretary may by regulation (1) require dealers and dlstflb·
2Applicable sections of Pans F and G of Title III Public Health Service
utors of electroniC products to which there are applicable standards
Act f42 U.S.C. 262-264J are quoted below:
prescnbed under 011S subpart and the relall pnces of whlcb IS not less
Pari F LicenSing - Biological Products and Clinical Laboratories than $50, to furnish manufacturers of such products SUCll InformatIOn
and"'" •• as may be necessary to Identify and locate. for purposes of seclJon 359,
Ihe first purchasers of such products for purposes other than resale. and
Sec 351(c) "Any officer, agent, or employee of the Department of (2) reqUire manufacturers lapreserve such informatIOn Any regulation
Health, EducatIOn, and Welfare, autllorlzed by the Secretary for the establlsblng a reqUirement pursuant to clause (1) of the preceding

FORM FDA 412 (11/80) PREVIOUS EDITION IS OBSOLETE


NOTICE OF INSPECTION

Fig. 14-1. Form FD-482, filled out by the FDA inspector during an FDA inspection.
218 CITRUS JUICE SANITATION

DEPART"'EI'IT OF HEALTH, EDUCAT IOH. AND wELFARE


PuBLIC MEAt.. TI-I SERVICE

FOOD AH D DAUe; AOM-INISTRATtON

Thr follo ... !n" ",.,....,,1 ...... ,,.. (,ClII"'iI'"lf'~1 I» th!l' F"oCod IoI\I! DIU, ,ir, dllllll'll.tnlllliOft.1Id Ii!CiI!.pt ,. Iltul'br 1o["lu!.o ... lf"dacd pu r tu. "110
8,.".110/'0 :0. ((') o f 11lI,. Pri .. , .. , PIDold , Orull:. MId CO.fM'lIcA~1 CZI U.S.C. l7"Ccl:: .nJ oilorP.rt ..... Sub P.rt J. $rclllJlll'~(bJ ",f
'rh .. Put;.ll~ H.-01111'" $,.,,,j.:,. A C~ - .1' U.S.C. ~6J..J- Io"d/OI' 2 1 COd .. <Ol F.-It ... ,., R,. ... h.U_. !CF R j IJ07.0'1. EltClupn or Ih,u e
. , .... ..al<l'·d ot\ \hit 'f'WIU' of Ih ... (<0_.

Fig. 14-2. FDA sample receipt, used if samples are taken during an FDA inspection.
INSPECTION 219

DEPARTMENT OF HeAL TH, EDUCATIOH, AHD WEL FARE


puel.lC HEAL TH SERVice
FOOD AND ORua AO"'IN I'STRATIO N'
D.8TRICT AooRr; • •

) V (ifl.......W/'f)' :J::&...C'fJ.~
'&l., ~ '1'110 -
&.r
1C.
97.A.i>1..<',Vl(it<
NAM e; 0" INDIVIDUAl. T O WH O ,.. "IiPOR' ' .... ulEe CAT I' 0" Ult ... eCT ION' fl . N U MDCR

TO: -f>fvll ~ lii£1iJ!. ItIi"'-U(. M.iI....,.. _"'fill


mLI 0' ~,:o~r; I'>r) (lft'J>.-'ly/\.... TYPE ETAIiI..I 'H"" E.NT IN.PEeTeo ( , ... ,

1' 1" 1'14 NAM" NAME 0" '1ft ... , BRANCH OR UNIT IN.~I[CTI.D
(' I. /~
.TAIlCTlAODAI; ••
,'in (,j., " jl, rvrI ' f',)
"'fAIEET AOORE.• • OF" PRE."U&E8 IN&PECTt:D

,=,~:l. 2 t:ad- i.t:l'..rl.ilM1R Q.u.t


e'''}NO '~TI f71l/(/,J
CITY AND .TATIE:

DURI NG AN INJ:l I',o1"IO N OF YOUR 'lAM (I' (W E) OU5ItAYI;O:

(jj ~."'l cvo ..d ..L.U1''-~;:oL'fL:.{l'/' ~/)

Q ~..dL,"Y'1 J..u-a:h.1l 0-<..[}.()ui." J.~;J


~ Cu)"...J..,>rN.j-:.J ~:..<tl..arno.

~£F. P.f.l'&R51.
or fillS PAC;'
", .11'
~1!~Tlzk:£
( •• ,
ri;;." ~ ~
, ;~T~' ii.
' 0,
J:..¥1-, •

';, ,-p:. \
A
. I < "P~C<:'::' nj7r7~
11)1\: '" ri 1~ ' ... _... . ~. 7 ~
T'r ....
"' • "r.~" ,
INSPECT,O ...... l OBSER V " T' 0 ... S

Fig. 14..3. Fonn FD-483, filled out by the FDA inspector during an FDA inspection.
220 CITRUS JUICE SANITATION

have not been filled out, this is a good time to complete them. Any problems
found during the inspection are discussed, and the FDA inspector outlines a
plan for correcting the problems. Notes should be taken on these conversations
and any decisions made, and included in the FDA file.
After the inspector leaves, plant management should meet to decide how any
requested corrections will be made, in accordance with the FDA inspector's
instructions including specific assignments.

Imported Products

Whenever citrus products are imported into the United States, both customs and
FDA clearances must be obtained before any product can be further processed
or sold. Custom inspectors are primarily concerned with proper representation
of the product, contraband, disease, and contamination brought in from foreign
countries. FDA officials are concerned with adulteration and proper identifica-
tion of products. Most citrus importers identify the products they import into
the United States by using the U.S. federal standards of identity found in Chap-
ter 19. These standards of identity sufficiently describe imported products for
identification by the FDA officials, who then issue form FD-702, shown in Fig.
14-4.

USDA INSPECTIONS

Unlike the FDA inspections, inspections by the U. S. Department of Agriculture


(USDA) are a voluntary service to food processors in grading various food
commodities. For a food to obtain a USDA grade certification, certain require-
ments must be met, one of them being sanitation. Failure to meet USDA san-
itation requirements can, at worst, lead to a loss of this service.
The USDA is paid by user companies for its service, which can be provided
on an occasional basis or continuously, using laboratory facilities provided by
the user company. Sanitation requirements are always in force when the USDA
issues grades. However, if continuous inspection is desired, a special plant san-
itation survey must be performed to determine whether a plant's sanitation pro-
gram qualifies for USDA grading. Thereafter, routine sanitation inspections are
performed.
The plant survey covers plant organization, facilities, and operation. Some
of the main concerns of this inspection are as follows:

1. Weeds, trash, rubbish, rodent and insect harborages around the plant,
and protection from such in food storage areas.
2. Offensive odors, dust, soot, or inadequate drainage.
INSPECTION 221

form API'f'tJvrv,UMlI l't D. 4'~/'lo l/j "'.


E~pl,.tM" D.tt: J,""V't J I . 198o.
DEPARTMENT OF

o
ENTRY DATA TAKEN FROM HEALTH AND HUMAN SERVICES
Number FOOD AND DRUG AOMtNIST"ATfON
IOAd.I"""
Notice

o Mlnifet!
39-M10127-0
0 ..006/14/88 439-0010127-0 06/14/88
D
I
IT Ad"anct
=~[ ENTRY NO. AND DATE
N01;ee
BII...L OF" LADING NO. POAT OF LADING COUNTRY OR ORIGIN
Mexico
PORT OF UNLOADING
Hidalgo, Texas
I Hidalgo, Tx
PORT OF ENTRY

8ROKER'S REF NO.


I-4638
Veracruz
e ,H, BOX NO.
493
VALUE OF ENTRV IN
$100300.00
u.s. S ICONTAINER NO. IMPORTING VESSEL
2 Trucks
I06/14/88ARRIVAL DATE

FOR THE 'Ntme. A~r",. IMPORTER IName, Add,e... , MANUFACTVAER/SH'''ER (NIIM., AddrtSs,

.,
ACCOUNT OF I CONiI..- ZOp Codol OF RECORD Zip Code) ZIp Code)
Tropical Bf"Verllgea Inc Smne Ju~uera Veracruzana SA
700 Jackson Ave, Apt 134 Kill 297 Carrt Mexico-TUltpa
HcAllen, Texas 78501 POM Rica, Ver .• H exlco
SROKER fllltOt.."..,Ibo.,.' LOCAT ION OF LOT (FOr" FOA DATE
.1tM"I1".,'otI) AVAIL

N._
J1IIIny Santoa Inc
J1,=.1
T~~~ Citrua Excha~ .e
~~~i I I same
mw~. LUD.-u II I I PHONE NO. 5B5 4503

(FOA 8AOKER' S USE'


GeNERAL DESCRIPTION Of SHIPMENT
THIS IMPORTATION OTY. PACKAGED ITO::'[:;::k~~lJ;o':.?:'c.FfE.

MAY PROCEED
Without FDA Extmlnltlon 216 Dltu1l\s Frozen cn-"nge Juice
Concentrate
This notlQe does not Pf't'cludt tction should
the mereh.ndi .. In!t be found ....iol .. tive •

• " lLlDONLY,FSlGNED

SlG~~ FDA R"P~Nrtw


(,~ Darll

IMPORTANT NOTiCe - An Imoon shlp","n' mUft be


IItld Intoct 1000lly pondlng 'unlltr no.ice from FDA.
With the idvlnCII notlCll', or otherwl-se. Brok.r 0( Impomr
mult inform FDA of tho 'allowing:

1. EarliHt d.te "the ilhipmem will be .1fI1I.ble for


samp1i~.

I!
2. loatlon in 10001.re, of the Ihipment on that dlte.

3. Bre.kdown .. stIown on the Invoice-number Ind sl ••


0' units 01"" 10•• and S .. I... e"'" 10'.
~~-

FORM FDA 102(6/85) p.ey,ous EDITION MAY 8! USED. MAY PROCEED NOTICE

Fig. 14-4. Fonn 702, used by the FDA to clear an imported product.
222 CITRUS JUICE SANITATION

3. Wall construction and cleanliness, as well as the number of floors and


floor materials and their cleanliness.
4. Proper screening of all openings in the plant and adequate shielding of
light bulbs.
5. Sanitizing systems, including chlorination facilities and proper cleanup
facilities.
6. Separate storage areas for cleaning compounds away from food process-
ing areas.
7. Sufficient lighting for proper operations and cleaning.
8. Sufficient ventilation to prevent excessive heat, steam, condensation, va-
pors, smoke, or fumes.
9. Leaking roofs, pipes, valves, or other equipment, as well as covered
tanks, catwalks, and cross belts.
10. Flaking paint or rust.
11. Material used to make equipment and containers, which should be non-
absorbent so as not to contaminate the product, and should not come into
contact with unsanitary surfaces.
12. Oil and grease from motors that could contaminate the product.
13. Slime and mold buildup on plant facilities or equipment, as well as the
placement of loose items such as lunchboxes or personal gear.
14. Quality of the water used in the plant.
15. Restroom doors, which should not open directly into the food processing
area and should be self-closing; the proper number of waste receptacles;
handwashing signs; handwashing facilities, including soap, hot water,
and hand drying facilities.
16. Adequate lighting for color scoring and sufficient facilities, environment,
and equipment for inspection.
17. Protection of food containers from dust and dirt.
18. Cleanliness of employees, including hair restraints, as well as employees
with infectious diseases, gum chewing, tobacco use, or other unsanitary
personal habits or facilities.

During continuous inspections, the USDA inspector will perform periodic


sanitation inspections, using the form shown in Fig. 14-5. When infractions
occur, one of three levels of seriousness will be assigned to the problem. A
minor infraction (MN) constitutes a problem that it is desirable to correct, which
must be corrected within 24 hours. A major infraction (MJ) may result in prod-
uct contamination and must be corrected by the next shift change. A critical
infraction (CR) means that the product is being contaminaated, and the infrac-
tion must be corrected immediately. Copies of the sanitary score sheet should
be given to plant management promptly. If unsatisfactory or unusual conditions
exist, copies must be sent to area, regional, and national USDA offices. If an
INSPECTION 223

FORM FV-41o_3
15-76)
U.S. DEPARTMENT OF AGRICULTURE
AGRICULTURAL MARKETING SERVICE

SANITATION SCORE SHEET FOR


CITRUS PROCESSING PLANTS

NAME OF PLANT LOCATION DATE D.I.R NO.

5({V1~y faVLd C ;+rus 1/11) Ie IlJj.s-jrlo 3;


RATING SYMBOLS (JI S.",f.ofo" l' ~ ~ ~
SJGNATURElrl:E:O~~
.-
--. ti
MN _ Minor MJ _ Major TIME ();; r<
CR - Critical U _ Unsatisfactory ~ 0 MlTATION DEFICIENCIES -- SHOW !TEM, NO. AND DESCRIBE

PREMISES
<1) O,Mrs Le-?+ "pelll - ;VO-t ;·n~4 ~G ""5 ....
1. Outside areas \I V~"
A
2. Waste disposal fMI V IV ~ peel +'rItSftI ".., jr"u",j
3.
RECEIVING AREA
1. Unloading pit ./ V- i/'
2. Grading V VIV
B
3.
4.
Conveyors and chutes
Bins
V
M:r V V
VV'
B:> .fIles SWl1vw-'JI\.J /':"'.5 - +# iJ -f.o yeW\", IJ
5.
6.
7.
PROCESSING AREAS
1. Washing and grading V (fiN II' (i) c./" loy: \1\ ..."ibl-" vu"'f W DvK •' : ;
2. Sizers and leads
3. Extractors V .... V
/.-.
4. Troughs and lines V' '-""' II.
5. Finishers ./ V
6. Valves and lines V v
7. Blend and storage tanks l/ V
C 8. Disposal screw conveyors V' ...... V'
9. Fillers & closing machines V L; V
10. Stabilizer V V V
11. Floors, gutters & walls V'-"
12. Waste storaQe ..... V
13.
14.
15.
16.
WAREHOUSE OR COLD STORAGE
1. General housekeeping V- V L..
V 1/ L-
....
2. Sugar storage
D 3. Can storage V V
4.
5.
6.
REST ROOMS
1. Supplies V frV\ V ~ No 5bo..{/ .for- Wtl-ski~ ha..ds
2. Wash basins L- V. ...
E
3. T oi lets & urinals V' V
4. Floors & walls V 0/ 20
5.
PERSONNEL
1. Cleanliness V V ~

2. Head covering V V V
F
3. Smokil]9 V V ......
4. I" )" Iv V '1/
5. "'" ..l"

Fig. 14-5. Inspection fonn used by USDA inspectors during continuous inspection.
224 CITRUS JUICE SANITATION

unsatisfactory condition persists for three successive days or three days in one
week, the inspector is required to contact his or her supervisor and/or other
USDA officials as needed. Again, failure to resolve sanitation problems can
result in the withdrawal of grading services.

IN-HOUSE INSPECTIONS

Some good guidelines for in-house inspections can be found in the FDA and
USDA inspections. Performing FDA-like and USDA-like inspections is the best
way to prepare for such inspections. A good pamphlet that can be used as an
additional guide is "Do Your Own Establishment Inspection-A Guide to Self
Inspection for the Smaller Food Processor and Warehouse" (U.S. Department
of Health and Human Services, Public Health Service, Food and Drug Admin-
istration, 200 C Street, Southwest, Washington, D.C. 20204).
Even though the legal requirements of sanitation must be kept in mind, san-
itation programs in citrus processing plants should be based on product quality.
If proper care is taken to ensure the quality of the products in-house, no serious
problems should ever occur with FDA or USDA inspections. A loss of repu-
tation and profits is usually much more devastating than conflicts with regUla-
tory agencies. In-house personnel also are more knowledgeable about equip-
ment and procedures and can implement a more effective sanitation program
than outside inspectors. This knowledge of products and equipment should be
constantly used in designing and redesigning sanitation programs so that pro-
duction time and cleaning materials will not be wasted during the production
of high-quality products.
There are two types of in-house inspections. One is based on solving a spe-
cific problem that has occurred. For example, the presence of a large number
of Drosophila fruit flies may require the periodic inspection of peel residue
accumulations in certain areas of the plant. Once these accumulations are being
removed on a regular basis, or when the weather gets cooler and the flies be-
come less active, the procedure can be modified or eliminated. If a particular
procedure or inspection system does not solve the problem, new procedures
should be tried until the problem is solved. At least on a weekly basis, the entire
plant should be shut down for a complete cleanup, and an FDA- or USDA-like
inspection should be performed. It is important that those individuals doing the
inspecting are not those doing the cleaning. Otherwise, shortcuts will be taken
in the inspection. Also, management should always be aware of and supportive
of monitoring the sanitation condition of the plant, especially in construction
and reconstruction within the plant. Quality control personnel should always be
consulted in such modifications.
Inspections form just the foundation for a good sanitation program. The sub-
sequent chapters go into greater detail about the many facets of citrus sanitation.
INSPECTION 225

QUESTIONS

1. What are some of the factors that affect sanitation in processing or bot-
tling plants?
2. What is the foundation of any sanitation program?
3. What are some of the reasons why sanitation is important?
4. What is the law regarding chewing tobacco in processing areas?
5. What is the law regarding restroom doors that open directly into pro-
cessing areas?
6. Who should attend the preinspection conference when an FDA inspector
appears at the plant?
7. What forms will an FDA inspector fill out, and why?
8. What records does an FDA inspector have the authority to access?
9. Can a processor go to jail for failing a USDA inspection?
10. Why is a survey taken prior to USDA continuous inspection?
11. Give examples of minor, major, and critical USDA sanitation infrac-
tions.
12. What should be the basis of in-house sanitation programs?
13. What are the two types of basic in-house inspections?
14. How should FDA and USDA inspectors be treated, and why?
15. When is it okay to leave an FDA inspector alone in the plant?
Chapter 15

Citrus Microbiology

One of the major means of contamination of citrus products is by the growth of


single-celled microogranisms. Some microorganisms are pathogenic (disease-
causing) in humans and are of primary concern to food processors. Other mi-
croorganisms, although not pathogenic, destroy the quality of foods and make
them unpalatable or undesirable. Microorganisms found in citrus products fall
into the latter category. The high acid content of citrus juices prevents the growth
of pathogenic microbes while allowing certain acid-tolerant bacteria, yeasts,
and molds to flourish. The wastes generated by this biological activity produces
undesirable flavors and odors that degrade the quality of citrus products. An
understanding of the factors that affect the growth of these microorganisms en-
ables the development of procedures to prevent it. Some of these factors are
light, temperature, air availability, pH, moisture, and osmotic pressure.

BACTERIA

Single-cell organisms are divided into two types according to cellular structure.
One type is the eucaryotes ("eu" means true; "karyo" is the combining fonn
for nucleus), or microorganisms with a true nucleus. The other category is the
procaryotes, which are microbes that lack a true nucleus and usually have their
DNA in a single molecule. Procaryotes include bacteria and bluegreen algae,
whereas eucaryotes contain all other algae, molds, yeasts, and protozoans. There
are three types of bacteria, which differ in their shape or morphology. Bacillus
bacteria are elongated or rod-shaped, coccus bacteria are spherical, and spirillus
bacteria are spiral or corkscrew-shaped. Bacteria are classified by many param-
eters, including growth conditions, size, and wastes produced. Even though
other acid-producing bacteria have been isolated from citrus juices from the
genera of Aerobacter and Xanthomonas (Faville and Hill 1951a), only lactic
acid bacteria from the genera Lactobacillus and Leuconostoc have been found
to significantly affect citrus products.

226

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
CITRUS MICROBIOLOGY 227

Lactobacillus

Lactobacillus bacteria (Buchanan and Gibbons 1974) are gram positive rod-
shaped bacteria from the Lactobacillaceae family, which derives its name from
the fact that at least half of the carbon produced from carbohydrate metabolism
is in the form of lactate. Other products from Lactobacillus growth are diacetyl,
acetate, formate, succinate, carbon dioxide, ethanol, and other one- or
two-carbon acids. Diacetyl (2,3-butanedione), which is synthesized by the bac-
teria from citric acid, imparts an undesirable buttermilk-like flavor and odor to
citrus juices and is the major cause of product rejection of single-strength juices
due to spoilage.
These nonpathogenic organisms grow at temperatures of 5 to 53°C (41-
12rF) with optimal temperatures generally 30 to 40°C (86-104°F). They are
very acid-tolerant, with an optimal pH range of usually 5.5 to 5.8 with signif-
icant growth below this pH range. Lactobacillus bacteria also are very sensitive
to osmotic pressure or juice concentration, with slow growth at 35 to 38°Brix
and no growth over 45°Brix. The main species found in citrus juices are Lac-
tobacillus plantarum and Lactobacillus brevis (Hays and Riester 1952). L.
planarum has an optimal temperature range of 30 to 35°C (86-95°F), with
growth at 15°C (59°F) but generally not at 45°C (l13°F). L. brevis has an
optimal growth temperature of about 30°C (86°F), with growth at 15°C (59°F)
but no growth at 45°C (113°F). Some strains are pigmeted from orange to red,
but most are white in color.

Leuconostoc

Leuconostoc (Buchanan and Gibbons 1974) are gram positive spherical coc-
coids, usually in pairs or in chains. Leuconostoc is a nonpathogenic member of
the Streptococcaceae family, which normally produces lactic acid, ethanol, car-
bon dioxide, and diacetyl with the same buttermilk-like off flavors and odors as
produced with Lactobacillus bacteria. Optimal temperatures for growth are in
the range of 20 to 30°C (68-86°F), which is cooler than the range for Lacto-
bacillus bacteria. Most species will grow in media with a pH of 5.5 to 6.5. One
species, Leuconostoc oenos, will grow in the range of 4.2 to 4.8 and even lower
but probably not higher. Generally Leuconostoc bacteria grow very slowly at
pH levels of around 3.6 compared to Lactobacillus, but they grow faster at a
pH of 4.0 and above. Most species are facultative anaerobes, which means they
can grow in the presence or absence of air. The main species found in citrus
are Leuconostoc mesenteroids and Leuconostoc dextranicum (Hays and Riester
1952). L. mesenteroids grows in the 10 to 37°C (50-99°F) range, with an
optimal range of 20 to 30°C (68-86°F), but these bacteria cannot withstand
228 CITRUS JUICE SANITATION

55°C (131°F) for 30 minutes. Some strains, however, may withstand temper-
atures of 80 to 85°C (176-185°F) for shorter periods of time. L. mesenteroids
forms a slime of dextran metabolized from sucrose and/or levano polymers from
fructose. L. dextranicum also produces slimy dextran growth, though not as
actively as L. mesenteroids. The growth temperature range and the optimal
range for L. dextranicum are the same as for L. mesenteroids.

Bacillus subtilis and Bacillus pumilus

A problem that is sometimes encountered in plating is the formation of large


colonies that swell with gas formation and then burst, forming a colony that
resembles a volcano or has a wrinkled texture. These aerobic colonies spread
rapidly on the plate and can obliterate the other colonies, rendering the counting
of colonies impossible. The microorganisms responsible for this behavior are
Bacillus subtilis and/or Bacillus pumilus, both aerobic spore formers (York
1988). These bacteria sometimes are found on the surface of citrus fruit and get
into the juice during extraction. The pH range for their growth has not been
reported. They may be thermophilic or grow at high temperatures, and they can
survive the heat treatment of pasteurization or evaporation of citrus juices. The
formation of these bacteria on agar plates is enhanced by the presence of mois-
ture. That is why plates are inverted during incubation-inversion keeps the
moisture away from the agar surface. These organisms are not pathogenic but
can make the counting of colonies on a plate very difficult if not impossible.

YEASTS

Yeasts belong to the eucaryote (true nucleus) category of microorganisms. Tax-


onomically, yeasts belong to the class Ascomycetes (sac fungi) and to the fungi
subclass of the phylum Thallophyta, or plants that have no true roots, stems,
or leaves. Yeasts usually can be differentiated under a microscope by the fact
that most of them reproduce by budding, as shown below.

Yeast cells are generally larger than bacteria, as illustrated in Fig. 15-1 by
bacteria and yeasts that have been isolated from citrus juices. Generally yeasts
grow much more slowly than bacteria, with optimum temperatures for growth
of 20 to 30°C (68-86°F), the same as for Leuconostoc bacteria. Yeasts gen-
erally are more tolerant of high temperatures (65-70°C or 149-158°F) than
CITRUS MICROBIOLOGY 229

SMALLEST YEAST c:::>


LARGEST
LACTOBACILLUS
I I
SMALLEST LACTOBACILLUS c:::J
LARGEST LEUCONOSTOC <::::>
SMALLEST LEUCONOSTOC 0
Fig. IS-I. Relative size ranges for bacteria and yeasts that have been isolated from citrus juices.

bacteria or molds. They also have a much higher tolerance for preservatives,
cold temperatures, and osmotic pressures than bacteria. In fact, yeasts are some-
times referred to as osmiophilic or osmiotolerant. Within a microorganism there
is a delicate balance of aqueous life-giving solutions. If the cell wall comes into
contact with a medium that is more concentrated in soluble material than the
cell is, the water from these life-giving solutions will migrate out of the cell
into the more concentrated solution in an effort to equalize the two concentra-
tions. This osmotic effect is generally lethal to bacteria and is one reason for
the use of concentrated syrups in the canning of fruits. However, yeasts are
more resistant to osmotic pressures than bacteria and can easily survive in citrus
concentrates of 58 to 65°Brix. Yeasts have been shown to remain more viable
at 50 0 Brix than at 12 to 30 0 Brix after heating at 60°C (140°F) for up to 8
minutes (Juven, Kanner, and Weisslovicz 1978), so they are of primary concern
in the microbiology of citrus concentrates. If yeasts are predominant in the juice
flora, the juice most likely came from reconstituted concentrate. If bacteria
dominate the flora, the juice most likely came from single-strength juice or was
contaminated in a single-strength form. Yeasts also grow in media with a pH
as low as 1.5, well within the acidity range that is common to citrus juices.
It is interesting to observe that even though yeast can be found in nearly every
concentrate that has not been aseptically treated, fermentation occurs incon-
sistently in lots of citrus concentrates. This phenomenon may be partially due
to the number of viable microbes prior to spoilage, but that does not account
for such fermentation in samples with lower microbial counts. In the fermen-
tation process, there is oxidation by a microbe in the absence of an electron
230 CITRUS JUICE SANITATION

receptor such as oxygen. This results in the production of more oxidized cabron
dioxide gas and more reduced ethanol, as follows:

C 6 H 12 0 6 -> 2CH 2 CH 20H + 2C02 (g) 57 kilocalories / mole


glucose ethanol
( 15-1)

Not all of the 57 kilocalories thus produced is released as heat. Some of this
energy is stored in high-energy phosphate bonds in ATP within the microbe.
One reason for the inconsistent fermentation in citrus concentrates is that not
all species that have been found in citrus juices are capable of fermentation. As
seen in Table 15-1, the six most commonly found species in one study will not
ferment at all (Rhodotorula and Cryptococcus species). The next eight species
ferment only glucose, which comprises only one-fourth of the carbohydrates in
citrus juices. The next three species (Trichosporan) will not ferment at all,
whereas two others that were among the least common yeasts in this study are
capable of fermenting both glucose and sucrose. (Note: The eight species at the
bottom of the table were isolated from citrus concentrates in separate studies;
thus their percent of incidence in relation to the others is unknown.) It is evident
that the species present may significantly affect whether or not fermentation will
occur. A more recent study documents that the most prominent yeast in pas-
teurized citrus juices is probably Sacchromyces cerevisiae, followed by Rho-
dotorula species (commonly called pink yeast) and Zygosaccharomyces species
(an osmophile) (Parish 1988). Rhodotorula species are not thought to be spoil-
age yeasts and may indicate post-pasteurization contamination.

Mold

Most of the molds of concern to the food industry belong to the same class as
yeasts-Ascomycetes (sac fungi). The major contributing factor to mold growth
is the availability of moisture. Molds have been known to grow in any location
where moisture is found, ranging from air with a relative humidity of 70% to
water reservoirs. In addition to moisture, air availability is important. Also,
molds generally require an environment free from agitation or disturbance. Idle
concentrate tanks exposed to mold spore contamination from the air have been
known to accumulate mold growth if not cleaned out or flushed out with fresh
concentrate. Mold colonies found in standard plate counts generally indicate
that there has been undisturbed concentrate exposed to the air for a period of
time up to several days, or that the plate has been exposed in the air. An upper
temperature limit for mold growth would be about 60°C (140°F), with a pH
tolerance down to as low as zero.
Molds that get into citrus juices from the surfaces of fruit generally are ho-
CITRUS MICROBIOLOGY 231

Table 15-1. Yeast isolated from commercial citrus


concentrates (Kobatake, Kurata, and Komagata
1978).
% of Isolation Out
Genus Species of 24 Samples
Rhodotorula glutinis 83.3
minuta
rubra
Cryptococcus albidus 37.5
injirm-miniatus
laurentii
Candida lambica* 33.3
diddensii*
freyschussii*
intermedia*
parapsilosis*
sake*
santamariae*
valida *
Trichosporan cutaneum 25.0
pullulans
variabile
Debarymoyces hansenii** 12.5
Kloeckela apiculata* 4.2
Pichia etchellsii* 4.2
Hansenula anomala** 4.2
Cephaloascus fragrans 4.2
Candida*** magnoliae**
Saccharomyces'" chevalieri**
Candida**** maltosa**
Hanseniaspora**** guilliermondii*
Pichiu**** membranaefaciens*
Saccharomyces**** cerevisiae*
Schwanniomyces * * * * occidentalis* *
Torulaspora**** delbrueckii*
*Known to fennent glucose only.
**Known to ferment glucose and sucrose.
***Juven. Kanner, and Weisslowicz 1978.
****Found in unpasteurized orange juices (Parish and Higgins \989).

mogenized and destroyed by the juice acidity, and usually are not likely to affect
the quality of the juice, except perhaps for carton juice. Freshly squeezed juice
obtained from the processing of moldy fruit may also contain high levels of
mold, most of which can be destroyed through proper pasteurization. Black
mold growing on the surfaces of moist processing equipment or buildings may
break off and create an unsightly cosmetic contamination. However, molds
found in citrus juices have not been known to be pathogenic or produce off
232 CITRUS JUICE SANITATION

flavor or odors in citrus products under nonnal conditions. Some of the molds
that have been isolated from citrus juices include, in order of prevalence, Au-
reobasidium pullulans, Aspergillus niger, Botrytis species, Phoma species, Mu-
cor species, Aspergillus Jumigatus, Cladosporium sphaerospermum, and Pen-
icillium species (Kobatake, Kurata, and Komagata 1978). A more recent study
found the following in commercial pasteurized orange juices: Aureobasidium
pullulans (a black yeast), Penicillium species (black yeasts), and Cladosporium
species. Also the following were found in unpasteurized laboratory samples:
Fusarium species, Geotrichum species, and Penicillium species (Parish and
Higgins 1989).

DETERMINATIVE TECHNIQUES

Detenninations of the number and type of microorganisms are important in any


food processing operation. In the citrus industry, several methods are being
used, the most rapid one being the direct microscope count. The major disad-
vantage of this method is that it does not differentiate between living and dead
microorganisms. Periodic microscope counts have been used to estimate sig-
nificant changes in the number of microbes. One must be careful to take a
representative sample and perfonn a unifonn count.

Diacetyl

Another method sometimes used to estimate microbial growth is the measure-


ment of diacetyl or 2,3-butanedione levels. As mentioned earlier, diacetyl is
produced by lactic acid bacteria, which impart a buttennilk flavor and odor to
single-strength juices. Diacetyl reacts with creatine in the presence of naphthol
under alkaline conditions to produce a dark brownish-purple dye:

+HN=C
NH2

~-6H
I 2
oII
C-OH
06
----.~ Dye (15-2)
40% KOH

Diacetyl CH 3
Creatine

Acetylmethylcarbinol (3-hydroxy, 2-butanone) also is a fennentation prod-


uct, as well as a derivative of diacetyl in the presence of strong alkali and
oxygen. However, it is less volatile than diacetyl and is distilled off at a more
CITRUS MICROBIOLOGY 233

constant rate throughout the distillation in the procedure given below. Acetyl-
methylcarbinol also reacts with the creatine to give the same color as produced
with diacetyl; so a correction must be applied to the diacetyl distillate to account
for the acetylmethylcarbinol. Reconsituted concentrates result in much less dye
formation than freshly extracted juices, because of volatile losses during evap-
oration.

Diacetyl Test (Hill, Wenzel, and Barreto 1954)

Equipment and Supplies

• Spectrophotometer set at 530 nm.


• Distillation setup shown in Fig. 5-1, as used in the Scott oil determination.
• I-Naphthol (or alpha naphthol) (5 gin 100 ml of 99% isopropyl alcohol).
• Creatine solution (100 g KOH or 71.3 g NaOH in about 150 ml distilled
water in 250 ml volumetric flask. Cool the solution and add 0.75 g crea-
tine, and fill the flask to the mark with distilled water.)
• Timer.
• Three 25 ml graduated cylinders.
• 10 ml pipette.
• 5 ml pipette with bulb or equivalent.
• 2 ml pipette with bulb or equivalent.
• 50 ml beakers or flasks. for samples and blank.
• 300 ml graduated cylinder.
• Diacetyl standards in distilled water at 0.5, 1,2, 3, 5, 7, and 10 ppm.

Procedure

1. Standardize the Brix of the sample of 1l.8°Brix.


2. Add 300 ml of the sample to the distillation apparatus shown in Fig. 5-1
(without the alcohol shown in the figure), and distill off three 25 ml por-
tions, discarding the second portion. The first portion contains most of
the diacetyl, while the third contains approximately the same amount of
acetylmethylcarbinol as in the first portion because it distills off at a steady
rate.
3. Pipette 10 ml of the first portion and 10 ml of the third portion into sep-
arate 50 ml beakers, and 10 ml of distilled water into a third beaker to
serve as a blank.
4. Pipette 5 ml of the naphthol solution into each beaker, using a bulb or
pipettor.
5. Pipette 2 ml of the creatine solution into each beaker at 2-minute intervals
according to the timer.
234 CITRUS JUICE SANITATION

6. After 5 minutes of contact time with the creatine solution, measure the %
light transmission or absorbance, using a spectrophotometer set at 530 nm
(Abs = log (lOO/%Trans).
7. Subtract the absorbance of the third 25 ml portion from that of the first,
which contains most of the diacetyl. This step corrects for the acetyl-
methylcarbinol in the first diacetyl portion. Compare the corrected ab-
sorbance with the absorbance of diacetyl standards.

Diacetyl values can be plotted on a control chart, and when those values
increase dramatically, a cleanup should be performed immediately. A range of
0.6 to 6 ppm has been suggested for the maximum diacetyllevel, depending on
the particular operation and desired specifications.

Standard Plate Counts

Standard plate counts comprise the primary method used in monitoring micro-
bial growth in citrus products. Plate counts account only for viable organisms
but take 2 to 3 days to get results. The plate count is performed by mixing a
juice sample with an agar medium and incubating the resulting gel. Each or-
ganism in the sample reproduces to form a visible colony that can be easily
counted. The location in the plate, shape, color, and texture of the colonies
generally can be used to identify the type of organism that created the colony.
Lactobacillus organisms form small white to red circular colonies about the size
of a pinhead and can be embedded throughout the agar, not on the surface.
Leuconostoc colonies are large domelike circular colonies, appearing only on
the surface ofthe agar, with a smooth translucent color and texture. One species
of Leuconostoc produces colonies that appear as a thin film on the bottom of
the medium under anaerobic conditions. Yeast colonies generally are recog-
nized by their star shape, formed by two flat circular colonies intersecting at
right angles. These colonies are generally between Lactobacillus and Leucon-
ostoc in size and grow throughout the medium. Surface yeast colonies may
resemble Leuconostoc colonies but usually are flatter on the surface. Mold col-
onies are always on the surface and consist of a very fibrous or cottonlike ma-
terial. Some mold colonies may result from air contamination rather than the
sample. A blank plate containing no juice sample aids in the monitoring of
sterilization procedures as well as air contamination.
Plate counts usually are expressed as the number of colony forming units
(cfu) per milliliters of single-strength juice ( 11.8 °Brix). This allows the com-
parison of juice products that may vary in concentration. When the number of
colonies per plate exceeds 300, a dilution should be performed until the number
of colonies per plate is less than 300. Trying to count over 300 colonies may
result in counting errors, and too many colonies on a plate may result in the
CITRUS MICROBIOLOGY 235

blending together of colonies that are difficult to differentiate. Using a standard


dilution, over 300 colonies are usually considered "too many to count" (TMTC)
or "too numerous to count" (TNTC).
There is a wide divergence of opinion about what constitutes microbial growth
limits or specifications for a contaminated product. The detection of off flavors
or fermentative gas production is a clear indicator that microbial growth has
gone too far. Maximum microbial levels accepted in the industry range from
500 to 100,000 cfu/ml of single-strength juice (SSJ). Some commercial spec-
ifications allow less than 1000 to 5000 bacteria / ml SSJ while limiting yeast
and mold levels to less than lO / ml SSJ. Such specifications may be appropriate
for pasteurized or "not from concentrate" juices, as bacteria are the main flora
in such products. However, for concentrates or products made from concen-
trates, yeasts are the dominating flora. For such products a more appropriate
specification would be the reverse of the above: 1000 to 5000 yeasts / ml SSJ
and less than a 10 mold count and bacteria / ml SSJ. Manufacturers of fresh
squeezed, lightly pasteurized, or pasteurized juices or those who still use the
archaic method of adding cutback juice to concentrates to make FCGJ risk mi-
crobial contamination in order to provide a better-tasting product. The shelf life
of such products usually is very short, and appropriate limits may be in the
neighborhood of 30,000 cfu/ml SSF.
Most processing plants that manufacture citrus concentrates, regardless of the
equipment they use or the cleaning procedures employed, should be able to keep
microbial plate counts below 5000 cfu / ml SSJ. Higher counts than this gen-
erally indicate that a problem exists that, if not corrected, can lead to much
higher plate counts and eventual spoilage. It generally is not known what the
minimum plate count is that will produce off flavors and odors. Quality dete-
rioration depends again on the temperature, viscosity, and type of microorgan-
ism present. However, with citrus concentrates, off flavors and odors probably
will not develop until the total viable plate counts reach the tens of thousands
or higher.

Standard Plate Count Method

Equipment and Supplies

• Incubator set at about 25°C (80°F).


• Autoclave sterilizer (I21-l32°C or 250-270°F).
• Sterile I ml wide-mouth pipettes (disposable or sterilized glass pipettes).
• Sterile 99 ml dilution bottles containing excess sterile distilled water.
• Sterile 10 ml screw cap test tubes for sample collection (optional if samples
are to be taken from retail containers).
236 CITRUS JUICE SANITATION

• Sterile orange serum agar. (Dissolve 45.5 g of dehydrated orange serum


agar in 1 liter of cold water, heat the solution to 28°C (82 OF), pour 20 ml
in each screw cap test tube of appropriate size, and sterilize in the auto-
clave. Orange serum agar also can be made by mixing 200 ml of orange
juice serum, filtered at 200°F with about 6 g filter aid, with 10 g Tryptone
and 3 g yeast extract,S g dextrose, 2.5 g K 2 HP0 4 , 20 g Bacto-agar, and
800 ml water.)
• Sterile lemon serum agar for plate counts of lemon juices. (Mix 50 ml of
lemon juice serum, filtered at 200°F with about 6 g filter aid, with 10 g
Tryptone, 3 g yeast extract, 10 g dextrose, 4 g K 2HP0 4 , 20 g Bacto-agar,
and 950 ml water.)
• Sterile petri dishes.
• Quebec Colony Counter.
• Mechanical hand counter.
• Melting bath with thermometer.

Sterilization

1. Dry glassware can be sterilized in ovens at 132°C (250°F) for several


hours. Glass pipettes can be sterilized in canisters, a practice that allows
them to remain in a sterile environment until use.
2. Presterilized pipettes and petri dishes can be purchased. Care should be
taken to avoid contamination in partially used packages.
3. Dilution bottles containing dilution water and test tubes containing orange
or lemon serum agar or for use to take samples can be sterilized in the
autoclave at 15 lb pressure for 15 minutes. It is important that the caps
are loosened during sterilization to avoid pressure breakage of the glass-
ware. Also, gradual cooling is necessary after sterilization to avoid boiling
of the liquids in the glassware, causing spillage and desterilization.
4. Before use, you should adjust the volume of water in the 99 ml dilution
bottles to exactly 99 ml taking care to keep the openings covered as much
as possible to avoid air contamination.
5. Plating should be done in an area that is free of extraneous drafts or other
contamination.

Procedure

1. Samples can be collected from bulk containers and tanks in sterile 10 ml


screw cap test tubes or directly from retail containers. Samples should be
used as is, without dilution, to avoid contamination. A factor can be ap-
plied to give all results on an 11.8 °Brix basis.
2. One milliliter ofthe sample is pipetted into the 99 rn1 dilution bottle, with
the bottle opening kept covered as much as possible. It is important that
CITRUS MICROBIOLOGY 237

the 99 ml dilution bottles contain exactly 99 ml of sterile water. A com-


mon practice is to sterilize the bottles with slightly less than 99 ml water.
A separate bottle containing sterile water then can be used to adjust the
water level in these bottles. You should be careful not to contaminate the
water. Do not flame the neck of the bottle as it draws nonsterile air into
the bottle. For concentrate samples, rinse the concentrate from the inside
of the pipette using the sterile water in the bottle, by repetitively with-
drawing and expelling the water, into and out of the pipette.
3. All equipment and solutions should be at room temperature to avoid kill-
ing the flora in the sample.
4. The dilution bottles containing the sample should be sealed and shaken
well until fully mixed. Using another sterile 1 ml pipette, pipette 1 ml of
the dilution into a petri dish, keeping the dish covered as much as possi-
ble.
5. The presterilized agar test tubes, containing about 20 ml of agar, should
be melted in a hot water bath and cooled to at least 45°C (113°F) before
the agar is poured into the petri dish, with care again taken to keep the
dish covered as much as possible.
6. The dish must be swirled gently so that the agar and sample are mixed
and just cover the bottom of the dish. Allow the dish to cool until the agar
sets up or gels.
7. The petri dish is labeled and placed in the incubator (2SoC or 75°F) in
an inverted (gel side up) position in the dark for 48 hours. Lights in the
incubator during incubation will inhibit growth.
8. After incubation, the top cover of the dish is removed and the bottom part
of the dish placed on the Quebec Colony Counter. The colonies are
counted by using the mechanical hand counter or its equivalent. Separate
counts for Lactobacillus, Leuconostoc, yeast, and mold can be done if
desired. The number of colonies per 1 ml of 1l.8°Brix equivalent can be
calculated from:

c = PD(1.0291b soluble solids/gal @11.8°Brix)


(15-3 )
S

where C is the count / ml SS] or the number of colony forming units (cfu) ,
P is the number of colonies counted on the plate, D is the dilution or 100
in the procedure above, and S is the pounds soluble solids/gallon accord-
ing to the Brix of the original sample, using Equation 2-8 or 2-10. If
greater dilution is required in order to keep the number of colonies counted
below 300, then 1 ml from the first dilution bottle can be added to a second
99 ml dilution bottle to give a dilution of 10,000 instead of 100. This
value then can be used for D above.
238 CITRUS JUICE SANITATION

Automated Methods

Recently developed computerized methods of rapid microbial analysis, involv-


ing measurement of the change of conductance of samples with microbial ac-
tivity, are being used in some parts of the industry. These methods provide
rapid results, sometimes in hours, as well as the ability to measure many sam-
ples at once. The high cost of the equipment can be justified only if numerous
microbial determinations are required. For this reason generally only larger pro-
cessing plants with special applications, such as aseptic processing, are em-
ploying these methods. These automated systems are the closest thing available
to timely and accurate microbial determinations. Standard plate counts often are
used to calibrate and check results from these methods.

PROCESSING CONSIDERATIONS

Fruit

The peel of citrus fruit is a natural barrier to most microbial contamination.


Surface molds eventually will cause fruit to decompose, but once a fruit is
broken, microbial decay can occur rapidly. For this reason, under USDA in-
spection, only 10% or less of the fruit leaving the grading table is allowed to
be broken, and only 2 % or less can show visible evidence of decay (off color
or spongy texture). Also, inbound fruit traditionally undergoes some form of
trash elimination and washing prior to grading. In California, where most of
the fruit has undergone washing and waxing in a packing house prior to its
arrival at the processing plant, fruit washing is done more to enhance the con-
veyance of the fruit than to clean it. Such washing removes waxes applied at
packing houses, which cause the fruit to stick to belts and other conveyance
equipment. Surface microbial counts of the fruit generally cannot be correlated
to the plate counts of the resulting juice (Faville and Hill 1951b). One study
involving over 300 commercial lots of orange juice gave a pure random corre-
lation between the percent broken and decayed fruit and the final plate counts
of the juice (Kimball 1982).
Because most juices undergo pasteurization in modem evaporators or pas-
teurizers, the microbial flora of freshly extracted juice rarely correlates with the
flora in the processed juice. However, overly decayed fruit can easily produce
a juice with off flavors and odors developed prior to processing. This becomes
a greater problem in areas dominated by fresh fruit markets, where processing
plants are considered to have top priority for getting rid of fruit regardless of
its condition. Many processors, however, set standards regarding the degree of
broken and decayed fruit that is permissible before fruit is processed.
Water containing 15 to 20 ppm chlorine is often used for fruit rinsing or for
flushing of equipment that may be vulnerable to microbial growth or accumu-
CITRUS MICROBIOLOGY 239

lation. Chlorine levels are easily determined by using locally available swim-
ming pool test kits, which involve the yellow color development of chlorine
with o-tolidine. Dilution of water samples may be required in order to keep
within the chlorine concentration range on the color comparison chart included
with such a kit. Fruit grading, washing, and the use of chlorinated water is
generally more important in warmer humid climates or seasons. It should be
remembered that fruit that has undergone spoilage prior to chlorinated washings
may still impart off flavors and odors to the resultant juice.

Pasteurization

Heat treatment is the most common method of reducing microbial activity in


foods. Bacteria, the fastest-growing microorganisms in freshly extracted citrus
juices, undergo cell division about once very 30 minutes, depending on the
temperature and growing conditions. This means that in 6 hours over 4000
microbes can be produced from one bacterium. Unpasteurized juice can easily
contain thousands or tens of thousands of bacteria per milliliter, which can
result in significant spoilage if the juice is held for several hours without pas-
teurization. Pasteurization temperatures as low as 65.6°C (150°F) have been
shown to be adequate in the control of microbial growth (Berry and Veldhuis
1977). However, temperatures of at least 91°C (195°F) are required to deac-
tivate pectinase enzymes, which can cause cloud loss and/or gelation. Pasteur-
ization time can be as long as 40 seconds, but modem evaporators elevate juice
temperature to pasteurization levels for only about 10 to 15 seconds. Aseptic
systems sterilize the juice with similar pasteurizers, and use hydrogen peroxide
to sterilize juice containers prior to filling. Aseptic packaging for citrus juices
is not as popular as with other juices because of the higher amino acid content
of citrus juices, which results in the development of browning and off flavors.
The main objective of aseptic packaging is to minimize or eliminate the need
for refrigeration. Even though aseptically treated juices have no microbial ac-
tivity, refrigeration still is required for citrus juices in order to prevent the de-
velopment of off flavors and colors from the oxidation of amino acids, ascorbic
acid, and sugars.

Cooling Effects

Immediate chilling of pasteurized juices or concentrates not only inhibits the


growth of surviving microbes, but reduces the rate of oxidative reactions as
well. Single-strength juices should be kept close to O°C (32°F), and concen-
trates should be packaged and stored at -4°C (25 OF) or lower. Concentrations
stored at these temperatures consistently show a reduction of microbial flora
with time. Concentrates with plate counts in the tens of thousands can experi-
240 CITRUS JUICE SANITATION

ence a reduction of contamination with prolonged storage in freezers, usually


in a matter of months. This is due not only to cold temperatures but also to the
osmotic effects mentioned earlier. Single-strength juices usually have a limited
shelf life (weeks) regardless of their storage temperature, but concentrates can
often be stored for years.

Cleanup and Water Effects

Both bacteria and yeasts have difficulty growing in concentrates of 60 0 Brix and
higher; so the careful control of water addition to concentrate lines and tanks
has been found to be of great importance in controlling the growth of micro-
organisms in citrus concentrates. Partial rinsing of a concentrate line or tank is
one of the major causes of high microbial plate counts in concentrate lots be-
cause the microbes grow much more rapidly under the more dilute conditions.
Also, a constant flow of fresh concentrate through the lines and tanks minimizes
the time available for growth and reduces contamination. The only growth that
can occur is on the inner surface of the pipes where yeast may adhere and feed
on the flow of juice passing by, and this is why light yellowish yeast slime can
be found on the inner surfaces of contaminated lines. This buildup should be
cleaned immediately. During busy times of the year when fresh concentrate
constantly flows through the lines and the weather is cooler, the number of
cleanups can be reduced. Hot summer temperatures and infrequent processing
usually require a frequent-cleanup program. Cleanups may occur at various in-
tervals, from daily to monthly. Incomplete cleanups run the risk of inducing
microbial growth through dilution of the concentrate; therefore, partial cleaning
is worse than no cleaning at all for citrus concentrates.
Contamination of the lines from other sources also may cause spoilage. For
example, condensate may form inside the concentrate tank, diluting the con-
centrate and then spoiling it when left for a long period of time such as over
the weekend. Another source is blending with contaminated product, which
contaminates the entire blend. Another is blockage in plate heat exchangers or
lines, which provides a site for the accumulation of proudct that is not removed
during cleanups, and then spoils when left for long periods of time in what is
mistakenly thought to be clean equipment. Entrapped debris also provides a site
for microbial growth, and dead spaces in product lines present another hazard
where microbial growth may thrive. Such dead spaces should be taken apart
and checked regularly or removed altogether. A buildup of pressure from car-
bon dioxide production during fermentation literally can cause product hoses,
lines, containers, and even steel drums to explode, creating a safety as well as
a quality hazard.
Juice lines, tanks, evaporators, extractors, fillers, and packagers can all be
cleaned by using automated CIP (Cleaning In Place) systems. They also can be
CITRUS MICROBIOLOGY 241

taken apart manually and cleaned. Manual cleaning is the easiest and surest
method to inspect, but permanent lines are difficult or impossible to take apart
and inspect completely. However, most processing plants have enough equip-
ment to justify the use of an automated CIP system for at least part of it. Prop-
erly programmed CIP systems provide a more efficient and consistent cleanup
even though they are more difficult to inspect than manual cleaning systems.
Because citrus juices are acidic, 2 % caustic solutions are often used for clean-
ups. After the juice is removed, it is common practice to use a chlorine or
iodophor sanitizer rinse to reduce surface contamination of the equipment.
However, a rule of thumb may be that if a piece of equipment can be totally
inspected (all surfaces can be seen), such as a tank, and it looks clean to the
eye and there are no off odors, it can be considered clean. Equipment that can-
not be totally inspected, such as process lines, must be inspected by indirect
methods such as observance of clear water rinses and the presence of off odors.
Laboratory plate counts, however, are the surest means of determining the level
of product microbial contamination.

QUESTIONS

1. What is the main by-product of lactic acid bacteria that degrades citrus
juices?
2. What other genera of bacteria have been found in citrus juices besides
Lactobacillus and Leuconostoc?
3. What microorganisms are considered pathogenic to humans that are found
in citrus juices?
4. How can you recognize yeast cells under the microscope?
5. Why do yeasts survive better in citrus concentrates than bacteria?
6. To what eucaryotic class of microorganisms do the yeasts and molds
commonly found in citrus juices belong?
7. How can mold contaminate citrus juices?
8. What can be deduced from each of the following statements about sam-
ples?
• "A" has a high level of bacteria.
• "B" has a high level of yeasts.
• "C" has a high level of mold.
9. What is the minimum plate count before off flavors and odors will de-
velop from microbial spoilage?
10. Cite evidence from the chapter that the growth of microorganisms found
in citrus products is inhibited by light.
11. What is the maximum allowable % broken and % decayed fruit leaving
the grading table under USDA inspection?
242 CITRUS JUICE SANITATION

12. How does the condition of fruit correlate with the microbial plate counts
of the resulting processed juice?
13. What is the minimum temperature that has been shown to adequately
control microbial growth?
14. About how long does a concentrate juice lot with a high microbial count
need to be stored in a commercial freezer before the counts are reduced
to acceptable levels?
15. What are some of the most likely causes of high plate counts in citrus
concentrates?

PROBLEMS

1. What is the cfu of a 65°Brix sample that resulted in 316 colonies appearing on the
plate?
2. What is the cfu of a 60 Brix sample yielding 146 colonies of yeasts, 4 colonies of
0

Lactobacillus, and 1 colony of Leuconostoc?


3. If a 12.3°Brix sample yielded 25 colonies when plated, would it be more or less
contaminated than the concentrate sample in problem 2 using the same 100 dilution
factor?
4. Suppose that a linear relation was found between absorbance and the concentration
of diacetyl, using the procedure in the chapter, which was:

Absorbance = (Concentration in ppm) (0.0623 ) (15-4 )

What would be the diacetyl value of a sample with an absorbance of 0.7 for the
sample and 0.5 for the blank?
5. Identify the following plates:

,
1.
.. & D • 0 0 1 iPS \C'tc=n rmnl

REFERENCES

Berry, R. E. and Ve1dhuis, M. K. 1977. Processing of oranges, grapefruit and tangerines. In Citrus
Science and Technology II, S. Nagy, P. E. Shaw, and M. K. Velduis, eds. The AVI Publishing
Company, Inc., Westport, Conn., 202.
CITRUS MICROBIOLOGY 243

Buchanan, R. E. and Gibbons, N. E., eds. 1974. Bergey's Manual of Determinative Bacteriology.
The Williams & Wilkins Company, Baltimore, Md., 510-513, 576-593.
Faville, L. W. and Hill, E. C. 1951a. Recent investigations pertaining to acid-tolerant bacteria in
citrus juices. Second Annual Citrus Processors Meeting, Citrus Experiment Station, Lake Alfred,
Fla., October 9, 1951.
FaviUe, L. W. and Hill, E. C. 1951b. Incidence and significance of microorganisms in citrus
juices, Food Tech., 10, 423-425.
Hays, G. L., Riester, D. W. 1052. The control of "off odor" spoilage in frozen concentrated
orange juice, Food Tech., 6(8),386-389.
Hill, E. C., Wenzel, F. W., and Barreto, A. 1954. Colormetric method for detection of micro-
biological spoilage in citrus juices, Food Tech., 3, 168-171.
Juven, B. J., Kanner, J., and Weisslowicz, H. 1978. Influence of orange juice composition on the
thermal resistance of spoilage yeasts, J. Food Sci., 43, 1074-1080.
Kimball, D. A. 1982. Unpublished.
Kobatake, M., Kurata, H., and Komagata, K. 1978. Microbiological studies of fruit juices I & II,
J. Food Hygenic Sci. of Japan (Shokuin Eiseigaku Zasshi) , 19,449-461.
Parish, M. E. 1988. Microbiological aspects of fresh squeezed citrus juice. In Ready (0 Serve Citrus
Juices and Juice Added Beverages, R. F. Matthews, ed. Univ. of Florida, Gainsville, Fla., 79-
96.
Parish, M. E. and Higgins, D. P. 1989. Yeasts and molds isolated from spoilage citrus products
and by-products, J. of Food Protection, 52(4), 261-263.
York, G. K. 1988. Private communication with microbiologist, University of California, Davis,
Calif.
Chapter 16

Insects, Rodents, and Birds

Citrus processing plants generally are located in areas with mild climates, which
offer ideal living and growing conditions for many insects, rodents, and birds.
However, citrus juices may be processed and packaged in nearly every climate,
each with its own problems in regard to animal infestation. Regardless of the
processing conditions, the same basic principles of pest control are generally
applicable and important in producing a good-quality citrus product.

INSECTS

Even though the insects are a specific taxonomical class, the term "insect" is
generally applied to any creature that one would colloquially refer to as a' 'bug."
Insects are known for having six legs and three separate body sections. Such
creatures as spiders, mites, ticks, chiggers, millipedes, centipedes, snails, slugs,
and so on, are not insects, but for the purposes of food sanitation they can be
considered as such because of the methods used for their containment and con-
trol. Insects are the most abundant animal form on earth, with three to four
times as many species as the rest of the animal kingdom has put together. As
many as 700,000 species are known, with about two new species being added
each year. There is much that we do not know about them, but one thing we
do know is that insects cost the agricultural industry billions of dollars each
year. With respect to agricultural growth, insects are a concern because of their
effects on the quality and yield of certain crops. In the citrus processing indus-
try, however, the concern is with insects being embedded in fruit or being at-
tracted to the processing areas and entering the product during processing or
storage. Insect fragments in citrus products do not pose a health danger because
the acids of the juices kill any pathogenic microbes, but visible insect fragments
constitute a serious quality infraction, rendering the juice unpalatable. Also,
insect fragments and eggs that are visible only under a microscope can result
in lower defects scores upon USDA inspection; and citrus products contami-
nation by insects can lead to FDA action, up to costly fines or worse.

244

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
INSECTS. RODENTS. AND BIRDS 245

Insects are able to readily adapt to a wide range of environments. It can be


safely assumed that anywhere humans can live, so can insects. It may be next
to impossible to completely purge a processing plant of all insects, but, by using
basic techniques, processors can control insects sufficiently to produce a good-
quality product. The war on insects is too vast for processors to rely on merely
one or two battle plans. They need an integrated system, using all available
resources and tactics, to stay on top of an insect invasion. This requires a
knowledge of insects, including what factors affect them and how.

Food and Water

Hunger and thirst are the greatest motivators on earth, and insects are constantly
seeking food and water. Processing plants have a tendency not only to exist by
large bodies of war, but to have a large amount of water scattered around the
premises. Water, clean or dirty, has a tendency to draw insects, expecially
crawlers, some of which can detect water from long distances; and crickets and
cockroaches are especially attracted to wet areas. The field cricket (Gryllus
assimilis) (Fabricius)) is found in many parts of the world and across the United
States. The most common types of cockroaches are the Croton bug or the Blat-
tella germanica (German cockroach) (Fig. 16-1) and the Blatta orienta lis (ori-
ental cockroach); these cockroaches can hatch up to 50 offspring at one time.
These insects congregate around sinks, ditches, and wherever water collects.
They are most active at night or in the dark, but they often can be seen during
daylight hours. Crickets are generally easy to locate because of the noise they
make with their legs. Puddles of water not only attract insects, but they look
messy, and if they are in walkways or roadways, they become unpleasant ob-
stacles for people to wade through. Water should be drained or removed by
squeegee in such areas, and long ditches or waterways should be covered or
shortened to minimize insect attraction.
Insects feed on a variety of materials, especially those that humans consider
to be trash, such as paper. Trash receptacles should be well placed and used,
and should be emptied regularly. Floors in processing and eating areas should
be swept andlor mopped often. Fruit residue common around fruit conveyers
should be routinely removed, and juice spillage should not be left very long
before cleanup. Fruit waste that must be stored should be stored away from the
plant, and, if an insect infestation is noticed, the waste should be sprayed.
Weeds should not be allowed to grow near the plant, and landscaping should
be well cared for and sprayed if necessary. Unnecessary piles of parts, equip-
ment, or pallets provide excellent insect breeding and hiding areas, and should
be eliminated or removed from the plant. If the food and water are taken away,
insects will go somewhere else, not into your plant or your products.
The natural oils found in the outer peel of citrus fruit act as a natural barrier
246 CITRUS JUICE SANITATION

Mediterranean Fruit Fly Mexican Fruit Fly Oriental Fruit Fly


(Epochra canadenis) (Anastrepha ludens) (Dacus dorsalis)

Common Fruit Fly


(Drosophi la
Adult Female melangaster)
Adult Male German Cockroach
German Cockroach (81attella germanica)
(81attella germanica)
Fig. 16-1. Insects of common concern to citrus processing plants (USDA drawings). The Dro-
sophila is much smaller than the other insects in the figure.

to most insects. Also, the acidity of the juice inside the fruit is unpalatable to
insects, as a rule. However, there are some insects that thrive in citrus fruit,
namely, the Mediterranean fruit fly, the Mexican fruit fly, the Oriental fruit fly ,
and a few others that are less common. These pests have been essentially erad-
icated from the continental United States but flourish in citrus processing areas
in other parts of the world. These insects enter the fruit and lay their eggs within
the fruit itself. This not only damages the fruit but provides unsightly contam-
ination when it is processed. Grade-out of infested fruit is not always 100%
efficient, and centrifuging of contaminated citrus juices is commonly used to
remove insect fragments. Imported juices often will have lower pulp levels be-
cause centrifuging to remove insect fragments also removes pulp. Other insects
grow only on the surface of citrus fruit and generally do not contaminate juice
INSECTS. RODENTS. AND BIRDS 247

extracted from the fruit. Lemons are not considered a host for the Mediterranean
fruit fly.

Drosophila

Even though the natrual aromas and essential oils of citrus repel most insects,
the common fruit fly or Drosophila (Insecta, diptera-also known as vinegar
flies or pomace flies) seems attracted by them. The genus Drosophila has up to
50 different species, with the predominant species being Drosophila melano-
gaster, which thrives in mild weather during the late summer and early fall (see
Fig. 16-1). Drosophila simulans also becomes abundant in areas such as central
California but does not thrive in hot weather. Drosophila pseudobscura pre-
dominates in cooler weather.
Drosophila melanogaster are 1.5 to 2.5 mm long with red eyes and a black
abdomen, the first three segments having a yellow band. They convey spoilage
organisms from fruit to fruit and are strong fliers, flying over 6 miles in one
day, although they become immobilized in wind over 5 miles per hour and a
light intensity greater than 150 foot-candles. They are day fliers with very rapid
reproductive cycles. Although the flies spend only 24 hours in the egg, the egg
may remain in the female to within an hour of hatching. The larva and pupa
stages take three days each, giving a reproductive cycle of about seven days.
Females may lay up to 2000 eggs at one time but average only about 1000.
Adults live from 40 to 70 days, depending on the temperature. Thus, if two
Drosophila mate on June 1, assuming an average life span and two days be-
tween reproductive cycles, by mid-July, when the original parents die, there
will have been over 30 quadrillion (3.125 x 10 16 ) fruit flies produced. If this
many fruit flies were placed end to end (assuming an average 2 mm length),
they would extend out into space nearly 2! light days or the distance that light
traveling at 186,000 miles per second would go in 2~ days. Within a few days
after this, the average rate of production from the time of original mating would
have exceeded the speed of light in placing the flies end to end as they were
born. If the parents were to remate during the larva and pupa stages of the last
generation, the reproduction rate would be two to three times faster. These
staggering statistics suggest the importance of insect control and the need for
action early in the season before the numbers get out of control. Vigorous re-
production also produces sex odors that drift in the wind and attract even more
insects-another reason why breeding areas should be removed and cleaned.

Temperature

Insects are cold-blooded animals; that is, they require an outside source for
body heat. The ideal temperature for insects is generally 28.0°C (82.4°F),
248 CITRUS JUICE SANITATION

which is very close to humans' ideal temperature. Therefore, insects will always
try to invade the human environment. The comfort range for insects is also very
narrow, generally 21 to 32°C (70-90°F); temperature outside this range seri-
ously diminish insect activity. Solar heat stored in cement and metals provides
a heat source for insects after sunset. The abundance of cement surfaces, brick
or stone buildings, metal buildings, vehicles, equipment, or railroad rails com-
monly found at processing plants provide a comfortable habitat for insects. Once
activated by temperature, they begin their search. for food and water, which are
generally plentiful around processing plants. When the climate is cooler or dur-
ing the winter, insects like to move indoors, where they can vacation for the
winter. Some like it so much that they never bother to go home, especially if
temperature controls are left on all the time. Turning off the temperature con-
trols over the weekend, especially during cold weather, inhibits insect activity
and growth. Insects also like to inhabit electrical control boxes and equipment
because of the warmth of the electronics. As no processing plant can operate
without these devices, the sealing of cracks and crevices and the use of chem-
icals (see below) are needed to control infestations in these areas. Insects often
cause damage to such equipment, especially sensitive laboratory equipment.

Light

All insects are attracted to light to some extent, a characteristic that is of great
importance to night operations where nocturnal (night-active) insects are at-
tracted to processing lighting. Some insects, such as moths, can see for hundreds
of yards, whereas others, such as Drosophila, can see only a few yards. The
compound eye structure that is common to insects prevents them from seeing
linearly, so they usually approach lighting in a wandering fashion.
Insect are particularly sensitive to the ultraviolet light range, just outside hu-
mans' visible region. Mercury vapor lights attract over 100 times as many in-
sects as softer yellow sodium vapor lights, which emit a smaller amount of
ultraviolet light. For this reason, the use of mercury vapor lights should always
be discouraged at food processing plants, especially in rural areas. When out-
side lighting is necessary, it should be placed away from entries into the plant
or locations where product is exposed to the air, such as tanker loading areas.
Tankers always need air access to the tanker during filling or emptying, which
usually means that insects have access as well. If these areas are well lit at
night, insects usually will congregate there. Lights within the plant are best
placed where they cannot be viewed directly from outside the plant. Blinds and
curtains should be closed at night to avoid attracting insects, and screens should
be used to cover windows that must remain open. In rural areas where a pro-
cessing plant is the only light source for miles around, insects especially can be
a problem, but in a city where there are many lights, the problem may be less
INSECTS, RODENTS, AND BIRDS 249

severe. Using lights with a lower wattage will also diminish insect attraction.
Again, once they are inside the plant, they may decide to stay there and repro-
duce.
The attraction insects have for light can also be used to the advantage of the
quality control department. Ultraviolet light traps, consisting of an ultraviolet
light surrounded by an electrified screen, attracts insects. When they land on
the screen, they are electrocuted and fall into a collecting tray at the bottom of
the trap. These trays, which should be changed often, will give a good indi-
cation of what kind of insects are infesting an area. These lights should be
placed in areas that draw the insects away from processing areas, and where
they cannot be seen from the outside-you would not want a light trap to lure
insects in from the outside. Most flying insects fly only about 5 feet from the
floor or less, so the light traps are best used at these heights. However, higher
processing areas that have attractive debris will lure insects higher off the
ground. Ultraviolet bulbs lose their ability to emit ultraviolet light with time
and should be changed periodically (at least annually), even if no visible change
is observed in their light.

Insecticides

Due to their obvious toxicity, most insecticides are not permitted for use in food
processing plants. The federal code (Title 21 11O.37(b)) states: "The use of
insecticides or rodenticides is permitted only under such precautions and restric-
tions as will prevent the contamination of food or packing materials with illegal
residues." The pesticide tolerances that define "illegal residues" are in a con-
stant state of change, so that only by subscribing to the Federal Register can
one be assured of staying on top of changes in the law, but this generally is not
required of citrus processors. The use of pyrethrin insecticides is permitted by
the Food and Drug Administration and has been shown to be effective against
Drosophila and many crawling insects. Pyrethrins have been used orally for the
treatment of intestinal worms in humans and thus pose a smaller toxic threat
than other chemicals used to control pests. Extracted from pyrethrin plants in
Africa and South America, pyrethrins consist basically of four compounds,
known as pyrethrin I and II and cinerin I (allethrin) and II; and they are effective
against a wide variety of insects including Drosophila, aphids, bettles, cabbage
worm, housefly, leaf hooper, louse, mealybug, mosquito, sod webworm, thrip,
and mare. These insecticides also work quickly, with a quick kill rate. Sunlight
quickly breaks pyrethrins down, making them a contact insecticide that must
be sprayed directly on the insect rather than a residual insecticide that will kill
the insect at a later time. This breakdown of pyrethrins prevents the buildup of
insecticides in the plant, but it also necessitates cyclic application. Pyrethrins
should never be used with alkaline materials, as they would thereby lose their
250 CITRUS JUICE SANITATION

effectiveness. Similar pyrethrin-containing compounds are Drione, Foliafume,


Prentox Pyronyl, Pyrenone, and Tri-Excel DS (Considine 1982). In particularly
difficult situations, professional exterminators with experience in food process-
ing plants can be consulted and retained.
Whenever insect buildup is observed, the areas should be sprayed as soon as
possible, both inside the plant and outside. Foggers are very effective in killing
flying insects such as Drosophila. Care should be taken that no one is in the
plant during fogging. The use of timers will allow the use of foggers at night
or over the weekend. Doors to laboratories or lunchrooms should be left open
so that the insecticide can reach those areas. Care should be taken that all areas
of the plant be fogged. If one room is neglected, the flies will resort to that
room until the air clears, and then will reinfest the plant. Processors should also
be careful to close all product tanks and vessels and to cover any surface that
may come into contact with the food product. Carrier gases associated with the
insecticides can cause illness and can contaminate citrus products. The fumi-
gated rooms should be left vacant for several hours after fogging, again pref-
erably overnight or over the weekend. If a particular area is found to contain
insects, hand sparying also can be done.
Even though many crawling insects may be killed in fogging operations,
many will escape because crawlers are well adapted to hiding in places that the
fog cannot reach. Roach powders made of borax or boric acid, sulfur, or pyr-
ethrum can be used in electrical boxes, in cracks and crevices, under or behind
equipment or fixtures, or wherever there is not much water. Care should be
taken not to place these powders where they may fall or get into the product.
Roach traps consisting of sticky surfaces also can be used, not only to kill
roaches but to monitor their activity. Again, in particularly difficult situations,
a professional exterminator can be employed.
Outside the plant, harsher chemicals can be used. A chemically treated pe-
rimeter around the plant will prevent many crawlers from entering the plant.
All insecticides should be stored in isolated areas away from food ingredients
in order to avoid the accidental incorporation of these dangerous chemicals as
food additives.

Physical Barriers

An open door or product tank is an invitation to dinner for an insect that is best
canceled. All doors to processing areas should be closed when not in use and
equipped with automatic closing arms if necessary. Few insects can fly through
a closed door. Those doors that must remain open for long periods of time
should be equipped with properly functioning air screens. As shown in Fig.
16-2, air screens should not blow insects into the plant. Air flow should be
uniform across the entire door area without quiet "holes" where insects can
INSECTS. RODENTS. AND BIRDS 251

PROCESSING AREA

PROCESSING AREA

BAD!

Fig. 16-2. Proper and improper air screens over doorways that must be open for long periods of
time, showing good air flow and bad air flow. Care should be taken not to blow the insects into
the processing area.

slip through. Also, ventilation systems used to remove peel oil volatiles that
bum the eyes in extraction areas can disrupt air curtain flow, a situation that
must be avoided. Because fruit must be conveyed into the plant and the wastes
removed, there usually are openings in plant walls that can allow the entry of
insects. These should be as small as possible and covered with plastic strips or
other suitable barriers. Windows that open should always be screened. Also,
windows should be caulked, thresholds sealed, and other holes and cracks re-
paired. Even a solid wall a few feet high around the plant can be a significant
barrier to a crawling insect infestation.
Product tanks should always be closed except when it is absolutely necessary
that they be open. Some tanks require air vents during filling and emptying,
which should be screened to avoid the entrance of insects. Drum, can, or bottle
filling stations should be entirely free of insects. Filling is usually the most
vulnerable time in the process for product contamination by insects.
252 CITRUS JUICE SANITATION

Education

Often, in order for the previous methods to work, plant personnel need to be
educated on what the plant is doing for the control of insect contamination.
Purchased or home-made slide or video presentations can be used as a part of
new-employee orientations. Unlike microorganisms, insect problems are some-
thing that everyone can see and do something about, not just the quality control
department.
The important thing to remember is that all of these methds need to be used.
No one or two methods are sufficient. In fact, using all of these methods does
not guarantee that you will not have insect problems. As with many quality
control parameters, however, the consumer demands a sanitary product regard-
less of the problems involved.

RODENTS AND BIRDS

It is contrary to the Code of Federal Regulations (CFR, Title 21 11O.37(b)) to


permit any animals or birds into any area of a food processing plant except
those that are essential as a raw material. As with insecticides, the chemicals
used to control animals in food processing plants are limited to those that will
not leave illegal residues on any food products. Rats, mice, and squirrels are
the most common types of rodents that infest citrus processing plants. Squirrels
are less bold than rats or mice and generally live in outlying areas away from
the bulk of plant activity. Rats and mice readily move inside the plant and live
in ceilings, walls, control panels, equipment, offices, laboratories, lunchrooms,
and so on. Rodents are generally nocturnal in nature and thus are most often
seen at night. They are more visible than insects, and sightings should be re-
ported right away. The exact location and direction of movement should be
noted so that breeding areas can be located. Evidence of chewing or feces, as
well as grease streaks along walls that rats may rub against, also are important.
Rat urine will fluoresce under long ultraviolet light, emitting a greenish color.
Poisoned bait should be set out in areas suspected as hiding or breeding areas
but never where it can contaminate food products or containers. Each day the
bait should be checked for feeding. When the feeding has stopped, the rodents
usually have been killed. Pallet and drum storage areas and old abandonded
equipment or structures are ideal habitats for rats and mice, and usually a change
in season will drive rodents into plant areas. All holes, cracks, or other openings
that rodents can use to enter the plant should be sealed off as much as possible.
Birds are attracted to high structures where they can nest out of reach of
predators. They generally like quiet places free from vibration and noise. Thus
they generally shy away from tall evaporators that are constantly in use, but
idle tall structures away from processing noise are vulnerable to nesting. Com-
INSECTS. RODENTS. AND BIRDS 253

mercial ultrasonic or chemical repellants or avicides can be used to discourage


infestation, according to good manufacturing pmctice.

DETECTION OF CONTAMINATION

Detection of an insect or an animal presence in the plant is discussed above.


However, the detection of animal contamination in the product requires differ-
ent methods from those previously described. The best way to detect this type
of filth in citrus products is to alert production and quality control personnel
who routinely inspect the product. Any type of off-colored specks observed
against the bright colors of citrus juices should be reported immediately. Find-
ing one insect fragment in a product must mean that the rest of the insect is
somewhere else. Filth of any kind should be removed from the product and
separated by using sieves. The filth must be identified visually or under a mi-
croscope as an insect fmgment, hair, and so forth, so that steps can be taken to
prevent further contamination. Imported or purchased products should be in-
spected for evidence of insect contamination upon their arrival at the plant.
Severe problems usually can be seen through plastic liners without their being
opened. Lots severely contaminated with such filth are nearly impossible to
salvage and should be discarded or rejected. The economic loss of so doing
should be sufficient incentive to impose a proper sanitation program on the
process. Accepting and/or selling contaminated products can cost processors
their reputations and a portion, if not all, of their customers and business.

QUESTIONS

1. How many species of insects are known?


2. What can attmct insects to a processing plant?
3. What is the main concern of processing plants regarding insects?
4. Why is it that more insects do not infest the interior of citrus fruit?
5. What insect is attmcted to the citrus aromas common in citrus processing
plants?
6. What can be done to prevent Drosophila infestation in a processing plant?
7. How many Drosophila can be produced from two flies during an average
life span?
8. What is the comfort temperature mnge for insects?
9. What is the difference in insect attmction for mercury vapor lights and
sodium vapor lights?
10. Why are pyrethrins just contact insecticides?

REFERENCES
Considine, D. M. 1982. Foods and Food Production Encyclopedia. Van Nostrand Reinhold Com-
pany, New York, 1626.
Chapter 17

Physical and Chemical Contamination

The sanitary production of foods as outlined in the federal code for good man-
ufacturing practice includes restrictions that prevent contamination by physical
or nonliving objects or chemicals. The physical objects range from dust parti-
cles to hammers, and the chemicals range from toxic lubricants to juices of
another variety. Most of these objects and chemicals are necessary for the op-
eration of a citrus processing plant. However, regardless of their value, they all
have the potential for misuse and can damage the quality of the plant's products.
Such misuse can range from accidental or careless contamination to intentional
adulteration, and, unlike the contamination discussed in previous chapters, can
be lethal to product consumers. For this reason, prevention of such contami-
nation should be a vital part of any sanitation or quality control system in citrus
processing plants.

PHYSICAL CONTAMINATION

Product containers, whether they be cans, bottles, cartons, drums, tanks, or


tankers, usually are protected from physical contamination by lids or covers.
However, during processing, there is always a time when this protection is
removed or not in place, so that there is some risk of objects other than the
intended product getting into the container. Common sense dictates that these
containers should be clean and sanitary before use. Also, during processing,
the containers should be protected from falling objects or airborne contamina-
tion. Production personnel, who are usually the first line of defense, should be
trained and held responsible for this type of contamination. Loose items, such
as tools, bolts, nuts, lunch boxes, clothing, jewelry, pens, and so on, should
not be placed near open product containers where they may accidentally get
into the product. Loose items in shirt pockets pose a serious risk when one
bends over an open product tank. Hair protection is required by federal law,
including beard covers as well as hair nets or hats. Hair longer than shoulder
length should be kept up inside a hair cover because long hair poses a safety as

254

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
PHYSICAL AND CHEMICAL CONTAMINATION 255

wall as a sanitary hazard. Even visitors should wear hair protection when they
tour proudct areas. Also, good personal hygiene should be practiced by food
handlers, including clean clothes and hands.
Insulation near product containers, commonly used to insulate product and
refrigeration lines, may become worn and break off, causing unsightly or even
dangerous contamination. Dust and dirt inside the plant should be removed as
much as possible, and cleaned equipment should not be placed on the ground
or in any location where it may pick up dust or dirt. Dusty roads or travel ways
should not be allowed near or inside the plant, especially in tanker and tank
loading and unloading areas. After a tanker has been cleaned, it should never
travel any distance without all openings closed tightly. Condensate water that
commonly accumulates on cold surfaces, such as refrigerated lines and tanks,
should not fall in or near product containers, as this water picks up dust and
dirt from the air and the exterior surfaces of processing equipment.
Citrus products should never come into contact with unsanitary surfaces such
as wood or rusty steel. Drums and drum lids used to package citrus concentrates
should contain an inner baked enamel finish that is free from rust, dirt, or chip-
ping paint. Plastic containers should be free from plastic dust and residue. Pa-
perboard containers should be checked for dust and dirt accumulation prior to
use. During barreling, two plastic liners should be used, and the innermost liner
should not be opened until just before filling and should be closed just after
filling. Before barrel dumpers are used, all extraneous material, such as labels,
liner fasteners, and so on, should be removed so that it will not fall into the
product as it empties.
If glass objects are dropped into a tank full of product, there is no sanitary
way to get them out, and the potential for breakage could result in the total
rejection of the entire lot of juice. Plastic or metal containers should be used to
take samples, and bimetal thermometers should be used to take temperature
readings. Similarly, the Food and Drug Administration requires all glass light-
ing over product vessels or containers to have plastic covers or sleeves in order
to avoid contamination if the glass should break. Because debris from eating,
drinking, smoking, or chewing gum or tabacco often finds its way into product
containers, the FDA prohibits these activities in processing areas. Food ma-
chines should be placed in lunchrooms and not in processing areas, and em-
ployees should be provided a time and place for meals and breaks.

CHEMICAL CONTAMINATION

The processing of citrus juices always requires the use of chemicals in one form
or another. Water itself is a chemical, and is used not only for cleaning but to
adjust the concentration of concentrates and juices from concentrate. It should
go without saying that only potable water should be used in citrus products and
256 CITRUS JUICE SANITATION

for cleaning surfaces that come into contact with citrus products. Recycled or
reuse water should never be used for such purposes. Even though the water so
used in potable, that does not guarantee that the minerals, salts, or other chem-
icals (such as chlorine) in the water will not affect the quality of the citrus
product. Dilution water should be checked for off flavors and odors prior to use
or whenever contamination is suspected. Water used for cleanups also should
be potable and should not contain any extraneous debris. Many beverage man-
ufacturers go to great lengths to treat the water they use in the making of their
products.
Only food-grade caustics and sanitizers should be used for cleanups, and
FDA inspectors generally require information on the cleaners used in process-
ing. After cleanups, equipment should be thoroughly rinsed and drained in order
to avoid contamination the next time that it is used. Some mixing of the
FDA-approved cleaning agents may not pose much of a health hazard for con-
sumers; however, off flavors or odors may arise with such mixing, the acid
nature of the juice may change, and/or the federal standards of identity will
most likely be violated.
Citrus processing sometimes also includes the use of food additives, pesti-
cides, lubricants, and other chemicals. Nonfood and food chemicals should be
stored separately so that toxic materials will not be added accidentally to food
products. Care should be taken not to add the wrong food additive because so
doing not only could affect the quality of the product, but it could also violate
standards of identity. If polychlorinated biphenyls (PCBs) are used in any trans-
formers, in capacitors, as heat transfer or hydraulic fluids, or in lubricants,
coatings, inks, and so on, the federal code should be consulted (Title 21 110.40).
These compounds are considered toxic, and their use is regulated in food plants.
The many moving parts of citrus machinery require lubricants, and care should
be taken that these chemicals not drip into product containers or anyplace where
they could result in product contamination. Also, refrigerants used to chill citrus
juices and concentrates have the potential of leaking into the product, which
would diminish their chilling capacity in addition to contaminating the product.
Containers, such as drums, that have been previously used for nonfood pur-
poses, such as petroleum, should never be used for food products.
A good rule of thumb regarding physical or chemical contamination is some-
times referred to as Murphy's law: If anything has the possibility of getting into
a food product, most likely it will. Eliminate the possibility, and you will elim-
inate the contamination.

QUESTIONS

1. Who should be responsible for it if containers are contaminated during


processing?
PHYSICAL AND CHEMICAL CONTAMINATION 257

2. Who should be responsible for inspecting containers prior to their use?


3. What loose items are allowed to be placed near open product vessels or
containers?
4. Why is it that glass objects cannot be used to take samples from product
vessels?
5. Why is eating, drinking, smoking, or chewing prohibited in processing
areas?
6. Why should food and nonfood chemicals or materials be stored in separate
areas?
Chapter 18

Processing Contamination

Besides microbial, insect, animal, physical, and chemical contamination, there


is also contamination due to processing errors. As with many types of contam-
ination mentioned before, this type of contamination does not produce any kind
of health dangers; only the product quality is affected. The detrimental effects
range from cosmetic or appearance changes to texture and flavor changes. Be-
cause processing errors are the source ofthis type of problem, proper processing
can be the cure. A good quality control program can virtually eliminate all of
the problems discussed in this chapter.

HESPERIDIN

Hesperidin belongs to the group of compounds called flavonoids, like naringin,


which was discussed in Chapter 10. Unlike naringin, hesperidin imparts no
flavor to citrus juices, and it exists as the predominant flavonoid in orange and
tangerine juices. Its chemical structure is:

HESPERIDIN
OH
OH ~OCH

~o-~w)g ,
OH HO OH ~
I
OH 0
f3-Rutinosyl

Like other flavonoids, hesperidin is found primarily in the membrane and


peel material of the fruit. It is not soluble in neutral aqueous solutions and is
only slightly soluble in acidic solutions such as citrus juices. Upon extraction

258

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
PROCESSING CONTAMINATION 259

of the juice from the fruit, hesperidin comes into contact with the acidic juice
and will begin to form crystals. Under the microscope, these crystals are long
and needlelike. On processing equipment, they appear as a white scale or film
that can build up until it breaks off as white flakes. Hesperidin also contributes
to about 10 to 20% of the juice cloud. Its crystals can clog finishing screens,
thereby decreasing juice yield. Also, during evaporation concentration of the
juice accelerates hesperidin crystallization, producing white flakes that appear
in the concentrate or reconstituted juice.
Hesperidin levels within the fruit generally decrease with maturity because
as the fruit matures, it accumulates moisture, which dilutes the hesperidin con-
centration. In spite of this, the appearance of hesperidin flakes in citrus juices
increases with fruit maturity and may become an acute problem in the late sea-
son, especially in Valencia juice. This is probably due to lower acid levels,
which reduce the solubility of the hesperidin. Also, greater breakdown of the
peel in late-season fruit may cause increased amounts of hesperidin to get into
the juice. The USDA has set an arbitrary standard for the number of hesperidin
flakes permitted for various defects scores, as shown in Fig. 18-1. Hesperidin
flakes can be observed (USDA method) using 710 ml of 11.8 °Brix reconstituted
juice that has sat undisturbed for 5 minutes in a 1000 ml beaker with a 4-inch-
diameter bottom. White hesperidin flakes are apparent on the bottom of the
beaker, as observed from below with the aid of a flashlight.
Even though hesperidin formation cannot be prevented, routine hot caustic
cleanups can keep finisher screens and processing equipment free from hesper-
idin buildup. Again, late-season processing requires more frequent hot caustic
cleanups.

SCORING GUIDE

FOR HESPERIDIN
FROZEN CONCENTRATED ORANGE JUICE
AND CONCENTRATED ORANGE FOR MFG.

18 SCORE POINTS 19 SCORE POINTS 20 SCORE POINTS

Fig. 18-1. Arbitrary defects scoring guide for hesperidin flakes used by the USDA.
260 CITRUS JUICE SANITATION

BLACK FLAKES

Whenever heat is used during processing, as in evaporation or pasteurization,


there is risk of product overheating, scorching, or bum. (Off flavors and colors
produced from heat abuse are discussed in the next section.) If the flow of the
juice through such heating equipment is obstructed, excessive heat can be ap-
plied, which may result in product bum. Plate heat exchangers used in evapo-
ration or pasteurization are especially susceptible because they have very small
orifices that are easily blocked. The main purpose of finishing operations is to
remove pulp and other particles that may block the openings and passageways
in the evaporators or adhere to heated surfaces. Once a pulp or hesperidin par-
ticle is trapped and begins to bum, other particles will become attached to it,
and the bum area can spread until the entire flow of juice is blocked. Super-
concentration of the juice results in solidified sugars or "candy" formation, so
that the evaporator must be shut down and cleaned. The first evidence of this
problem is the appearance of black flakes in processed concentrate. Evaporators
with plate heat exchangers should be shut down and taken apart immediately if
black flakes appear in the concentrate because the bum area will only spread
and increase. TASTE evaporators should be cleaned right away if more than a
few black flakes appear. Small amounts of very tiny black flakes are commonly
found in concentrates processed in TASTE evaporators and generally are of no
concern. If juice sac material is to be added, the addition should be made after
heat treatment, especially if plate heat exchangers are used.
Black flake formation usually can be attributed to holes worn into finisher
screens or excessive hesperidin buildup due to insufficient cleanups. Because
black flakes are highly visible against the bright colors of citrus juices, they can
be easily recognized and perhaps even removed by using a sanitary ladle. If the
contamination is not too severe, the problem can be diminished by blending
with uncontaminated lots. However, it should be remembered that, unlike hes-
peridin flakes, most specifications require a zero level of black flakes or specks
because of their high visibility.

JUICE OXIDATION

Any food that contains highly oxidizable components, such as carbohydrates


and ascorbic acid, is vulnerable to oxidation. Oxidation can occur in many
ways, but catalyzed oxidation is usually the most rapid and therefore of greatest
concern to food processors. Citrus juice oxidation produces both off colors and
off flavors, but generally off flavors develop before off colors and are of greater
concern than the off colors.
In flavor oxidation, there are three basic catalysts. One is the naturally oc-
curring enzymes-nature's catalysts-that cause chemical changes in all living
things. These enzymes are generally deactivated through heat processing and
PROCESSING CONTAMINATION 261

cause no further changes in the juice. The organic acids present in citrus juices
also are catalysts and can assist in breaking up carbohydrate chains through acid
hydrolysis. However, the amine-assisted breakdown of carbohydrates has been
shown to be the major cause of the development of cooked off flavors (Hand-
werk and Coleman 1988). The mechanism for the amine catalysis is similar to
that of acid catalysis, but has been shown to occur under milder conditions of
heat and acidity than acid catalysis. Also, the oxidation of ascorbic acid or
vitamin C has been shown to be a significant factor in the development of off
flavors in citrus juices.
Citrus juices contain greater amounts of amino acids than other juices such
as apple or grape, which make citrus juices more vulnerable than other juices
to oxidation involving amino acids and the plentiful carbohydrates. These sugar-
amino acid reactions were first studied by Louis-Camille Maillard (1878-1935)
and have since taken his name as nonenzymatic Maillard reactions. The Mail-
lard reactions involve the reaction of the aldehyde group of the sugar with the
amino group of the amino acid, according to the following condensation reac-
tion:

HC =N-R
R'-CHO + R-NH z ...... I
R' (18-1 )
sugar amino Schiff base
acid

Further reactions can occur from the Schiff base, including various condensa-
tion reactions and Strecker degradations. At least 20 products of oxidation of
citrus juices have been isolated, and many more exist. However, only six have
been shown to contribute significantly to the quality of heat-abused citrus juices
(Handwerk and Coleman 1988).

1-Ethyl-2-formylpyrrole

CHO

This compound, also known as N-ethylpyrrole-2-carbaldehyde, is formed from


hexose-amino acid reactions followed by a Strecker degradation. It has a taste
threshold of only 2 ppm compared to a typical level of 0.5 ppm in dehydrated
262 CITRUS JUICE SANITATION

orange juice, which generally contains larger amounts of oxidative products due
to the additional heat required in processing. No data are available for other
citrus juices, but the levels would be expected to be much less. Excess amounts
of this compound impart a piney stale odor and flavor to heat-abused juices. Of
the six heat-abuse products that affect citrus juice quality, this is the only one
that actually incorporates the nitrogen from the amino acid into its structure,
illustrative of the role of amino acids in the oxidative process. Its boiling point
is 48 to 53°C.

2-Hydroxy-3-methyl-2-cyclopenten-1-one

HO

Other common names associated with this compound are methylcyclopenteno-


lene, hydroxymethylcyclopentenone, and cyclotene. Cyclotene is considered a
major contributor to the off flavor of citrus juices because of its low taste thresh-
old of 5 ppm, compared to levels of 1 ppm commonly found in dehydrated
orange juice. This compound most likely results from the acidic degradation of
ascorbic acid because the chemical structures are similar. However, acid-cata-
lyzed hexose degradation also is possible. Excessive amounts of cyclotene pro-
duce a maple or caramel-like odor and flavor.

5-Methyl-2-furaldehyde

Also known as 5-methylfurfural, this compound is formed from amino acid-


catalyzed oxidation of hexoses such as glucose or fructose. It has a boiling point
of 187°C, a specific gravity of 1.1072!8, and an index of refraction of 1.5263 2°,
and is soluble in water, very soluble in alcohol, and infinitely soluble in ether.
PROCESSING CONTAMINATION 263

It can be detected at 10 ppm, compared to less than O.S ppm found in dehy-
drated orange juice. Adding a hydroxy group to the methyl group to give
5-hydroxymethyl-2-furaldehyde results in a compound with a taste threshold in
canned orange juice of over 200 ppm with a typical level of 14 ppm. Grapefruit
juice held at SO°C for 12 weeks can exceed this taste threshold. This hydroxy
compound is virtually absent in fresh juices and may serve as a general measure
of product oxidation. It has a boiling point of 114 to 116°C, a melting point of
32 to 3SoC, and an index of refraction of I.S627 20 .

2, 5-Dimethyl-4-hydroxy-3( 2H )-furanone

o
o
This compound is also known as furaneol, and is also produced from hexoses
and amino acids. It has a taste threshold of O.OS ppm in orange juice and imparts
a pineapple-like flavor when it occurs in excessive amounts.

2-Methoxy-4-etheneylphenol

OH

This compound is also known as 4-vinyl guaiacol or guaiacol ethylene ether. It


is one of the only two compounds from citrus juice oxidation that produce de-
tectable quality changes but do not come from sugar-amino acid reactions or
ascorbic acid oxidation. It is formed from ferulic acid, which occurs in small
amounts in most plants. Ferulic acid has been found to occur in single-strength
orange juice at levels of 0.18 ppm, which increase to 0.30 ppm upon pasteur-
ization. When exposed to air, 4-vinyl guaiacol is converted to vanillin (Nairn
264 CITRUS JUICE SANITATION

et al. 1988). It has a melting point of 138 to 139°C and is slightly soluble in
water and soluble in ethanol. It has a taste threshold of only 0.05 ppm, with a
typical canned orange juice level of 1 ppm (which is over the taste threshold).
Excessive amounts impart an old fruit or rotten flavor and odor.

(1- Terpineol

This compound is a derivative of d-limonene, the primary constituent in citrus


oils, and d-limonene is commonly found in citrus juices. a-Terpineol is a col-
orless liquid with a lilac odor, which has a boiling point of 210 to 218°C and
a density of 0.935 g/ml. It is volatile with steam but is insoluble in water and
soluble in alcohol or ether. It has a taste threshold of 2.0 ppm, with a typical
level of 4 ppm in canned orange juice, and in excessive amounts it imparts a
stale, musty, or piney aroma to heat-abused juice.

General Observations

All these compounds have very low taste thresholds, and some of them have
been shown to impart off flavors below their thresholds when combined with
other heat-abuse products. For example, 5-hydroxymethyl-2-furaldehyde, hy-
droxymethylcyclopentenone, and N-ethylpyrrole-2-carboxaldehyde will impart
an off flavor even though each exists at only half of its taste threshold. Also,
2,5-dimethyl-4-hydroxy-3(2H)-furanone, a-terpineol, and 4-vinyl guaiacol im-
part off flavors even though they occur at only half of their individual taste
thresholds.
Additional amounts of citric acid also have been shown to enhance Maillard
oxidation, an effect attributed to the buffering action of the citrate ion because
the rates of these oxidative reactions are pH-sensitive. Also, the methyl groups
of citric acid assist in catalyzing oxidation to some extent, and phosphate ad-
dition accelerates oxidation regardless of buffering effects.
Restricting the amount of available oxygen obviously reduces the rate of ox-
PROCESSING CONTAMINATION 265

idation of citrus products. Steam injection or vacuum filling minimizes off flavor
development. Deaeration of citrus juices has not been shown to significantly
reduce oxidation because there is always enough air in the juice to facilitate
oxidation. Increasing the dissolved oxygen increased the rate of browning in
lemon juice but did not affect the rate of ascorbic acid degradation (Robertson
and Samaniego 1986). In another study, raising the initial levels of dissolved
oxygen increased browning and ascorbic acid degradation in orange juice, but
reducing the initial dissolved oxygen levels did not extend the taste-panel-de-
termined shelf life of pasteurized orange juice (Trammell, Dalsis, and Malone
1986).
Even though large amounts of heat are used during most citrus processing,
the majority of heat abuse occurs during storage. Shelf-life studies of 66°Brix
orange concentrate have shown that a reduction of storage temperature to 5.5 ° C
(4.4°C to -1.1 °C) can increase the shelf life by 4 months (5 months to 9
months) (Marcy et a1. 1984). With storage temperatures of -6.6°C (20°F) or
below, orange concentrate can be stored for at least a year. These results are
comparable to what is found industrially. Juices being evaporated are generally
held at 90 to 95°C (195-205°F) for about 10 to 20 seconds, with a total reten-
tion time in the evaporator of about 10 minutes, depending on the evaporator.
Most of this time the temperature of the juice is around 35 to 70°C (100-
150°F). Processed concentrate can withstand maximum evaporator tempera-
tures for about 30 minutes. Aseptic juices and concentrates are known for their
burnt-off flavors, most of which occur during unrefrigerated or prolonged stor-
age.

Analytical Techniques

Citrus juice oxidation products, like most chemicals, can be measured by using
sophisticated or time-consuming analytical techniques, including mass spec-
trometry, gas chromatography, and so forth. These methods are generally too
expensive and involved for routine quality control, and are generally not found
in quality control laboratories. For quality control purposes, the general degree
of oxidation and the shelf-life determination are the main factors of interest.
The simplest method for measuring the general heat abuse of citrus juices is the
formol or formaldehyde test, which measures the level of primary amino acids.
Most of the amino acids in citrus juices are primary amino acids, the exception
being proline, which is a secondary amino acid. Proline occurs in significant
amounts in citrus juices and even constitutes the major amino acid in many
varieties. Because amino acids are consumed during Maillard oxidation, the
loss of amino acids can be used as an indicator of heat abuse. The formol test
involves a Strecker degradation of the amino acids, generating acidity according
266 CITRUS JUICE SANITATION

to the following equation:


H H
"C/
NH+ 0 o II 0
1
3 11 II N II
R-C-CO- + C -> R- C -CO-
amino acid HH
(except proline) fonnol
(18-2 )
The acidity generated can then be titrated with a standard base.
The advantage of this method is its simplicity, speed, and convenience, as it
can be done at the same time as a routine acid titration. Its disadvantages include
a lack of specificity as to which amino acid is being measured and the fact that
oxidation can occur without consuming any amino acids. Also, because the
decrease of amino acids is what is important, two tests must be done, one before
and one after heat abuse or storage. Still, the formol test can provide a quick
estimate of heat abuse, and studies in the author's laboratories have shown that
a decrease of about 0.10 meq/ 100 ml of a single-strength juice equivalent con-
stitutes a detectable flavor change in California orange juices. Formol values
generally range from 1 to 3 meq/ 100 ml of single-strength juice. The following
procedure can be used.

Formol Test

Equipment and Supplies

• Same as for acid titration (see Chapter 3).


• 37 % formaldehyde neutralized to a pH of 8.4 within the hour.
• 10 ml graduated cylinder.

Procedure

1. Proceed to the endpoint (8.2 pH) as described in the section on acid ti-
tration (see Chapter 3), and continue titrating to a pH of 8.4.
2. Add 10 ml of the neutralized formaldehyde solution. The pH will drop.
Rezero the buret containing the NaOH solution.
3. Again titrate to a pH of 8.4, and read the ml of NaOH needed to do so.
The total amino acids (except proline) can be calculated by using:

(ml titrated) (N) ( 100 ml juice) (Sj)


meq AA/100 ml = ( )( ) (18-3)
ml sample Ss
PROCESSING CONTAMINATION 267

where N is the normality of the base (0.1562N) and Ss and Sj are the Ib
solids/gal of the sample and 1l.8°Brix juice. Ss and Sj are the same if
the sample has been reconstituted or adjusted to 11.8°Brix. Sj is equal to
1.029 lb solids / gal. The amino acid level is usually expressed as milli-
equivalents amino acids per 100 ml of juice. Equation 18-3 can be con-
densed to:

meq AA/lOO ml = 16.07(ml titrated)/(ml sample )Ss (18-4)

Another method suggested for the monitoring of heat abuse in citrus juice
products is the measurement of the furfural level. Furfural is a product of as-
corbic acid degradation, but it does not contribute directly to off flavor devel-
opment in the juice. Even though some oxidation reactions occur at different
rates, the rate of furfural development is believed to be an adequate indicator
of heat abuse for quality control purposes. The advantages of this method in-
clude the measurement of a specific oxidative product, and the fact that because
furfural is essentially nonexistent in fresh juice, only one test is needed to es-
timate the heat abuse of the juice. Also, furfural is easily distilled from the juice
by using an apparatus common in citrus quality control laboratories and is con-
centrated sixfold in so doing. The main disadvantage is that it involves the use
of aniline, a toxic chemical that can cause intoxication when inhaled, ingested,
or absorbed through the skin. Consumption of 0.25 ml of aniline can cause
serious poisoning. Acute symptoms include cyanosis, methemoglobinemia,
vertigo, headache, and mental confusion. Chronic symptoms include anemia,
anorexia, weight loss, skin lesions, and bladder tumors. The maximum safe
level is only 5 ppm. Analysis using aniline should be done under expert super-
vision.
The furfural procedure involves the following reaction:

o CHO
01 + +
FURFURAL ANILINE

This is a form of the Strecker degradation that results in a highly colored con-
jugated product that can be detected with a spectrophotometer. The procedure
uses SnCl2 to stabilize the color formation as well as to decrease interference
from codistilled compounds.
268 CITRUS JUICE SANITATION

Furfural Test (Ting and Rouseff 1986)

Equipment and Supplies

• Spectrophotometer.
• Oil distillation apparatus used in oil determination plus boiling chips or
anti foaming agent.
• 10 ml ground glass stoppered graduated cylinder.
• 2 ml pipette.
• One 13 x 150 mm test tube.
• 1 ml pipette.
• Furfural standards (0.5, 1.0, 2.0 p.g/ml in distilled water; make a 1: 100
dilution of a 1 mg/ml stock solution, and use 5, 10, and 20 ml of this
solution, diluting each to 100 ml).
• 95 % ethanol.
• Aniline / acetic acid solution. (Mix 2 ml of purified aniline with 1 ml 20 %
SnCl z • 2H zO in concentrated HCI. Mix and add glacial acetic acid to 20
ml.) Observe necessary safety precautions in working with aniline.

Procedure

1. Add 200 ml of reconstituted (11.8 °Brix) or single-strength juice to the


500 ml boiling flask in the distillation setup, along with a drop of anti-
foaming agent or boiling chips.
2. Collect 10 ml of distillate in the graduated cylinder, and stopper it tightly.
3. Mix the distillate and pipette 2 ml of it into the test tube; then add 2 ml
of ethanol and 1 ml of aniline/acetic acid solution to it. If analyzing
grapefruit juices, add 10 ml of distilled water.
4. Allow the tube to stand for 10 minutes, and then read the absorbance at
515 nm on the spectrophotometer.
5. Compare to standards, and calculate the p.g/liter of the furfural accord-
ingly. Standards should be added to fresh juice and distilled in order to
account for the distillation efficiency. The following equation can be used:

/1 _ (10 ml distillate) (1000 ml/liter) (2 ml std) (J1.g/ml std)


p.g - (200 rn1 juice) (2 ml distillate)
(18-6 )
or:
J1.g/liter furfural = 50/( p.g/ml standard) ( 18-7)

For grapefruit juices, multiply the furfural level by 3. Off flavor detection
correlates with furfural levels of about 50 to 70 J1.g/liter in canned and glass-
PROCESSING CONTAMINATION 269

packed orange juice and 150 to 175 ILg/liter in canned or glass-packed grape-
fruit juice. Grapefruit juice has a greater tendency to mask the off flavors formed
from product oxidation and thus has a higher taste threshold.
If the equipment is available, HPLC can be used to measure the amount of
furfural, which would eliminate the need to handle the toxic aniline.

HPLC Furfural Test (Marcy and Rouseff 1984)

Equipment and Supplies

• Isocratic HPLC system with a 4.6 mm x 25 mm Zorbax ODS column and


a UV detector set at 280 nm with a solvent system of 35 : 65 methanol and
water.
• Furfural standards prepared in the same way as in the previous procedure.
• Distillation apparatus used in the previous procedure with anti foam agent
and boiling chips.
• 10 ml graduated cylinder.

Procedure

1. Add 200 ml of reconstituted (11.8°Brix) or single-strength juice to the


500 ml flask in the distillation setup, and add 1 drop anti foam and boiling
chips. The standards used in the previous procedure should be used with
fresh juice here as well, in order to account for distillation efficiency.
2. Collect 10 ml of the distillate in the graduated cylinder and inject 15 ILl
into the HPLC system with a flow rate of 1.0 ml/min.
3. The elution time is about 8.5 minutes. Use the same calculations as in the
previous procedure.

If a gas chromatograph is available, some of the oxidative products that di-


rectly affect off flavors can be measured. The main drawback to the determi-
nation of some of these compounds is that they cannot be purchased in pure
fonn for standard preparation and must be synthesized in the laboratory. The
synthesis of these compounds is usually the difficult or prohibitive step, rather
than the analysis itself.

GLC Oxidation Products Test (Tatum, Nagy, and Berry 1975)

Equipment and Supplies

• Rotary evaporator.
• 100 g NaC!.
270 CITRUS JUICE SANITATION

• 1500 ml beaker.
• Two I-liter separatory funnels.
• 1 liter methylene chloride.
• Na2S04 desiccant.
• 10 ml volumetric flask or graduated cylinder.
• GLC with a 9' x 0.25" Carbowax 20M pack stainless steel column (20%
on 60-80 mesh Gas Chrom P) with a helium flow rate of 200 ml/min.
The temperature is programmed at 80°C for 6 min., and increased to 130°C
for 6 min., 135°C for 14 min., 140°C for 24 min., 155°C for 30 min.,
180°C for 46 min., 190°C for 56 min., 200°C for 64 min., and 220°C
for 76 min.
• 100 ILl syringe for injection into GLC system.

Procedure

1. Add 100 g NaCI to 1 liter of reconstituted (II.8°Brix) or single-strength


juice in the 1500 ml beaker, and stir it for 5 minutes to dissolve the salt.
2. Separate the sample into two I-liter separatory funnels, and extract each
portion 5 times with 200 ml of methylene chloride.
3. Dry the extracts over Na2S04, combine them, and evaporate them in a
rotary evaporator at 30°C.
4. Transfer the concentrate and washings into a 10 ml volumetric flask, and
fill it to the mark with methylene chloride.
5. Inject 100 ILl of the concentrated extract into the GLC system, and com-
pare the peaks to standards. The retention time and source of synthesis
have been reported for the relevant compounds shown in the table:

Standard
Compound Source GLC Ret. Time (min.)
a-Terpineol c 21.0
2,5-Dimethy l-4-hydroxy-3(2H)-furanone x 43.0
4-Vinyl guaiacol a 54.5
5-Hydroxymethyl furfural c 75.0
5-Methyl-2-furaldehyde c *
l-Ethyl-2-formylpyrrole b *
2-hydroxy-3-methyl-2-cyclopenten-1-one c *
Furfural c 12.5
a-Synthesized as described in references (Tatum et al. 1975).
b-Synthesized as described in references (Tatum et al. 1967).
c-Commercially available.
x-Not commercially available and no reported synthesis.
'-Not reported using this method.
PROCESSING CONTAMINATION 271

Brown Color

As mentioned earlier, during the oxidation of citrus juices browning follows off
flavor development. Browning with heat is common in nearly all foods. The
development of brown compounds in crude plantation white sugars has been
attributed to the development of humic acids, caramel, 5-hydroxymethyl fur-
fural, and melanoidins (Cheng, Lin, and Wang 1983). 5-Hydroxymethyl fur-
fural has already been mentioned as a remote participator in off flavor devel-
opment in oxidized citrus juices. The dark pigment in caramel is probably related
to the melanoidins, as is the pigments found in humic acids (Benzing-Purdie,
Ripmeester, and Preston 1983). Melanoidins have long been associated with
Maillard reactions (Spark 1969) and are the result of a slow polymerization of
reducing sugars along with inorganic salts. Melanoidins also are what consti-
tutes the brown pigment in skin. Even though the chemical structures of mel-
anoidins have not been determined, the related compound melanin has been
shown to be a complex quinoidal compound consisting of the following units:

Melanin is formed from the oxidation of tyrosine, which occurs at levels of up


to 3 mg /100 ml of single-strength juice and below 1 mg /100 ml in single-
strength grapefruit and lemon juices. As with many chemical reactions that
occur in citrus juices, the formation of melanin is commonly found in nature.
This oxidation product is found in feathers, hair, eyes, and skin, with albinos
lacking the enzyme needed to convert tyrosine to melanin.
The browning of citrus juices has been linked to ascorbic acid degradation,
which is at least partially responsible for the off color development in citrus
juices. Increased citrate concentrations enhance browning reactions by increas-
ing the buffering of the pH. Increased phosphate levels enhance browning re-
gardless of any buffering effect (Spark 1969).
Chemical measurement of the off colors found in heat-abused juices generally
is not done. Visual observations, along with color scoring and taste confirma-
tion, are usually sufficient for one to conclude that the shelf life of the juice has
expired. The actual amount of browning usually is not important, especially to
the pass/fail shelf-life tests. Heat-abused juice can be carefully reblended to
dilute the browning effect to below detection levels. Otherwise, browned juice
272 CITRUS JUICE SANITATION

should be discarded as unmarketable. Even though sulfites, thiols, mercaptans,


and other sulfur-containing amino acids have been shown to inhibit browning,
addition of these compounds might pose a health risk to consumers and most
likely would violate most federal standards of identity. The most viable means
of preventing both off flavor and off color formation in citrus juices is to min-
imize oxygen contact and reduce the temperature as much as possible during
processing and storage. In other words, do not heat-abuse the juice.

POTASSIUM CITRATE CRYSTALLIZATION

When high Brix (58-65°Brix), low Brix/ acid ratio citrus concentrates are stored
in commercial freezers, crystallization of some of their organic salts may occur.
These crystals generally have a negative effect on the citrus juice, resulting in
lower USDA defects scores as well as clogging plate heat exchangers and other
processing equipment that have restricted flow areas. These crystals also do not
reconstitute as easily as citrus concentrates. Larger crystals usually are laced
with insoluble hesperidin, which further hampers reconstitution attempts.
The crystals are hard and have a characteristic acid taste. They range in size
from fine sand up to 3 mm in diameter, depending on how long the crystalli-
zation has been allowed to proceed. The composition of the crystals from Cal-
ifornia and Brazilian concentrates is illustrated in Table 18-1. As can be seen,
the Brazil concentrate and crystals have higher levels of potassium than the
California counterparts. The higher potassium levels resulted in higher acid
levels in the Brazilian crystals as well. This predominance of potassium and
citric acid in the crystals agrees with other studies (Hils 1973; Koch 1980;

Table 18-1. Composition of MPC crystals and the composition


typical of orange juice concentrate for comparison
(Kimball 1985).
60 Brix Concentrate MPC Crystals
wlw % of" Kimball Bielig Kimball Koch
Total acid (as citric) 4-7 4-5 30-40 68.7
Reducing sugars 20-30 31.1-36.2 <0.5 0.09
Sucrose 16.1-27.1 0.06
Glucose 13.2-17 .1 0.03
Fructose 13.5-18.1 0.06
Potassium 0.51-0.71 1.09-1.46 9.15 13.78
Sodium 0.03-0.04 0.002-0.006 0.133
Ascorbic acid 1.23-1.54 1.01-1.78 0.Q2
Hesperidin 0.37-0.46 0.38
Pulp 8-12 (v Iv) 6-8 (v Iv) 4.75
Water 40 40 13.00
PROCESSING CONTAMINATION 273

Bielig et al. 1983). The stoichiometric relationship between potassium and citric
acid suggests that monopotassium citrate (MPC) is the primary species of salt
in the crystals. The citrate ion has so many sites for internal rotations that it
takes on a variety of shapes, leading to an amorphous or irregular crystal lattice
that gives rise to amorphous crystals. Also, other juice components, especially
cloud material, pulp, and hesperidin, become entrapped in or adhere to the
crystals, adding to their amorphous nature.
There are three main factors that affect the appearance of these crystals, one
being the thermodynamic favorability of the crystallization. Solubility tests have
shown that the Ksp of MPC in sucrose solutions follows this relationship:

(CA)(K+) = Ksp (moles/lited = 9.47 x lOIO e -806o/T (18-8)

where (CA) and (K+) are the concentrations of the citric acid and potassium
ions in moles/liter, and T is the absolute temperature between 253 OK ( - 20°C
or -4°F) and 293°K (+20°C or 68°F) (Kimball 1985). If the product of the
molar concentrations of citric acid and potassium ion exceeds the Ksp value,
crystallization is thermodynamically favored. It should be remembered that cit-
rus juices, like most other fruit juices, contain excess amounts of citrate beyond
that measured by acid titrations-up to 20% more citrate (Shaw, Buslig, and
Wilson 1983). Measurements of the citric acid and potassium levels for navel
and Valencia concentrate throughout a season in California are shown in Fig.
18-2 (Kimball 1985). The dashed line at the bottom is the Ksp value calculated
from Equation 18-8 at O°C. As can be seen, throughout the entire season for
both varieties of orange concentrate the Ksp value was exceeded, a situation
that would strongly favor MPC crystallization. This suggests that the high-Brix

--
'"> . 0.10
.....
("(S
0

-E •
0
-50 o 50 100 150 200 250 300

Day Processed
Fig. 18-2. The product of the citric acid and potassium concentrations for California navel and
Valencia concentrates during a processing season. The dashed line represents the Ksp value cal-
culated from Equation \8-8 for O°C (Kimball 1985). (Reprint from Food Technology 1985, 39(9),
79-8\, copyright © by the Institute of Food Technologists.)
274 CITRUS JUICE SANITATION

citrus concentrates are always susceptible to MPC crystallization and can be


considered to be supersaturated solutions of MPC. Using the relationships in
Fig. 18-2 and the Ksp relationship in Equation 18-8, Fig. 18-3, can be con-
structed, giving the estimated MPC saturation curves in orange juice as a func-
tion of Brix and temperature. Early-season and mid season navel and Valencia
curves were essentially the same; separate late-season navel and Valencia curves
are given. In Fig. 18-3, if concentrated orange juice is diluted and warmed, it
passes to the right and down in the figure, passing through the saturation curve
until it reaches the unsaturated area. In this area, MPC crystallization is no
longer thermodynamically favorable, and the crystals will begin to dissolve.
Another factor that affects this crystallization significantly is the juice pH. In
aqueous solutions, the highly polarized water molecule solubilizes the ionic
species-here potassium ions, citrate ions, and hydrogen ions. As water is re-
moved through evaporation, the ions begin to compete for available water mol-
ecules. The small size of the hydrogen ion and its ability to hydrogen-bond
make it an easy winner. This means that increased hydrogen ion or acid levels
exclude the potassium ions from the solubilizing water molecules, leading to
crystallization between potassium and citrate ions as shown in Fig. 18-4. This

70
65 ° Brix Concentrate

60 Supersaturated
in MPC

50

40
x
.;:: Unsaturated
in MPC
~ 30
Frozen
Juice \
\
20 \
\
\
\ Single Strength Juice

10 \
\
\
\
OL-----~--~~--~~--~~--~~----~--~~--~----~
·20 ·15 ·10 ·5 o 5 10 15 20

Temperature (0C)
Fig. 18-3. Saturation curves for California navel and Valencia orange juices for MPC crystalli-
zation as a function ofBrix and temperature (Kimball 1985). (Reprint from Food Technology 1985,
39(9),79-81, copyright © by the Institute of Food Technologists.)
+lV>+
PROCESSING CONTAMINATION 275

SO'in~i~~ty
Uti7 ~~~~id

o
&-
\utions

ffi
crystalization in
concentrated solutions
and/or acid solutions Fig. 18-4. The effect of acid on MPC

o
crystallization. The solubilizing water mol-
ecules favor the hydrogen ion. leaving the
potassium to crystallize with citrate (Kim-
ball 1985). (Reprint from Food Technology
1985,39(9),79-81, copyright © by the In-
Citrate stitute of Food Technologists.)

explains why early-season high-acid concentrates produce more crystals than


their sweeter late-season counterparts. High-acid tangerine and tangelo concen-
trates are especially susceptible to MPC crystallization. Lemon juices usually
are not so concentrated, and MPC crystallization thus has not been so much of
a concern with them.
The final factor affecting this crystallization is the rate of crystal formation.
Even if crystallization is thermodynamically favorable, if it does not occur
within a significant period of time, the thermodynamic favorability becomes
less important. A general equation that describes crystal formation is:

rate = .J(2DV( C - S)t)j q (18-9)

where D is the diffusivity factor, V is the ionic volume, C is the ionic concen-
tration, S is the ionic solubility, t is the time, and q is the charge of the ionic
species. The diffusivity factor is generally constant in dilute solutions, but here
this factor is significantly affected by the Brix, temperature, and acid content
of the concentrate. The acid levels can be reduced by ion exchange or blending.
It is desirable to keep the Brix as high as possible in order to minimize storage
and shipping costs. The temperature can be controlled somewhat. Bulk storage
tanks cannot be kept much below -lOoC (about 15°F) because if the temper-
ature is too low, the concentrate becomes too viscous to be pumped in and out
of the storage tank, but drum freezers are kept much colder (-20°C or O°F).
The higher heat needed by bulk storage systems increases the ion mobility in
276 CITRUS JUICE SANITATION

the concentrate, permitting thermodynamically favorable MPC crystallization.


Some bulk freezers are allowed to warm up to -4°C (25°F), which would
favor MPC crystallization even more. Reduction of bulk freezer temperatures
as low as possible would minimize MPC crystallization. Also, increased agi-
tation, which is common in the handling of bulk concentrates, increases the
formation of seed crystals. The result is the initial formation of many small
crystals that later aggregate into larger crystals.
Because the exact relationship of the D factor in Equation 18-9 to the Brix,
acid level, and temperature is unknown, it is not useful in predicting the actual
crystal growth. A regression equation has been found that does a better job of
this when compared to experimental data:

t = 648do. 334 (r2 = 0.91) (18-10)

where t is the time in days of storage in an industrial freezer at about -10°C


(about 15°F), and d is the diameter of the crystals in millimeters. Usually a
Brix/acid ratio of about 15.0 or less and a Brix of at least 60 0 Brix are required
for Equation 18-10 to be effective in crystallization prediction. Concentrates
with higher Brix levels will form crystals more slowly.
As large MPC crystals can cause processing quality problems, care should
be taken not to store low Brix/acid ratio concentrates in bulk freezers for more
than a few months. Such early-season concentrates should be barreled or blended
soon after production to avoid crystallization. This precaution and minimizing
bulk freezer temperatures are generally the best ways to control MPC crystal
formation.

QUESTIONS

1. What quality problem does hesperidin produce in citrus juices, and how
can this problem be eliminated?
2. During what part of the season is hesperidin contamination the biggest
problem, and why?
3. What causes black flakes to form, and how can this contamination be
eliminated?
4. How many black flakes are generally acceptable in citrus concentrates?
5. What compounds in citrus juices are mostly responsible for off flavor
development during excessive heating?
6. Which of the six heat-abuse products mentioned in the chapter imparts
a pineapple-like flavor?
7. Which two of the six heat-abuse products mentioned in the chapter that
affect flavor are not produced by Maillard reactions between sugars and
amino acids or from ascorbic acid degradation?
PROCESSING CONTAMINATION 277

8. When is the most heat abuse generally applied to citrus juices?


9. What are some of the advantages and disadvantages of the formol test
and the furfural test as mentioned in the chapter?
lO. Which occurs first, browning or flavor change during juice oxidation?
11. What causes the brown coloring in heat-abused citrus juices?
12. Does the fact that citrus concentrates are supersaturated in MPC mean
that MPC crystals will definitely form during normal industrial storage?
Why?
13. How does the acid level affect MPC crystallization?
14. What is the most feasible way to prevent MPC crystallization?
15. What varieties of concentrate are the most vulnerable to MPC crystalli-
zation?

PROBLEMS

1. In the formol test, using 9.83 ml of 60.2°Brix concentrate for both tests, would the
concentrate be expected to have developed off flavors if the initial test titrated 9.82
ml of the base and the test after heat abuse titrated 9.51 ml of the base?
2. In the furfural test, suppose that the absorbance matched the 1.02 Ilg/ml standard.
Would this orange juice be expected to have off flavors from heat abuse?
3. What would be the Ksp value for MPC at O°C, the freezing point of water? (O°C =
273°K)
4. Would a concentrate containing 0.15M citric acid and O.IOM potassium ion be fa-
vored to form MPC crystals at the same temperature mentioned in problem 3?
5. About how long would it take to form 2 mm crystals in 60 Brix concentrate with a
0

Brix/acid ratio of less than 15.0?

REFERENCES

Benzing-Purdie, L., Ripmeester, J. A., and Preston, C. M. 1983. Elucidation of the nitrogen forms
in melanoidins and humic acid by nitrogen-IS cross polarization-magic angle spinning nuclear
magnetic resonance spectroscopy, 1. Agric. Food Chern., 31, 913-915.
Bielig, H. 1., Hofsommer, H. J., Fischer-Ayloff-Cook, K. P., and Bakke, K. J. 1983. Crystalline
precipitation in frozen orange juice concentrates, Flussiges Obst, 50(3), 105.
Cheng, H. T., Lin, W. F., and Wang, C. P. 1983. Studies on the color development in stored
plantation white sugars. In The Maillard Reaction in Foods and Nutrition, G. R., Waller and
M. S. Feather, eds. ACS Symposium Series 215, American Chemical Society, Washington,
DC., 91-102.
Handwerk, R. L. and Coleman, R. L. 1988. Approaches to the citrus browning problem, J. Agric.
Food Chern., 36, 231-236.
Hils, A. 1973. Identification of a crystalline substance (K-citrate) in orange concentrate, Flussiges
Obst, 40(12), 496.
Kimball, D. A. 1985. Crystallization of potassium citrate salts in citrus concentrates, Food Tech.,
39(9),76-81,97.
278 CITRUS JUICE SANITATION

Koch, J. 1980. Formation of monopotassium citrate (MPC) in frozen concentrated orange juice
(FCOJ) at 65°Brix. Presented at the 31 st Annual Citrus Processors' Meeting, Lake Alfred, Fla.,
September 10, 1980.
Marcy, J. E. and Rouseff, R. L. 1984. HPLC determination of furfural in orange juice, J. Agric.
Food Chern., 32, 979-981.
Marcy, 1. E., Graumlich, T. R., Crandall, P. G., and Marshall, M. R. 1984. Factors affecting
storage of orange concentrate, J. Food Sci., 49, 1628-1629.
Nairn, M., Striem, B. 1., Kanner, J., and Peleg, H. 1988. Potential offerulic acid as a precurser
to off-ftavors in stored orange juice, J. Food Sci., 53(2), 500-504.
Robertson, G. L. and Samaniego, C. M. L. 1986. Effect of initial dissolved oxygen levels on
degradation of ascorbic acid and the browning of lemon juice during storage, J. Food Sci., 51 (I),
184-187, 192.
Shaw, P. E., Buslig, B. S., and Wilson, C. W. III. 1983. Total citrate content of orange and
grapefruit juices, J. Agric. Food Chern., 31(1),182-184.
Spark, A. A. 1969. Role of amino acids in non-enzymatic browning, J. Sci. Food Agric., 20, 308-
316.
Tatum, J. H., Nagy, S., and Berry, R. E. 1975. Degradation products formed in canned single
strength orange juice during storage, J. Food Sci., 40, 707-709.
Tatum, J. H., Shaw, P. E., and Berry, R. E. 1967. Some compounds formed during nonenzymatic
browning of orange powder. J. Agric. Food Chern., 15, 773.
Ting, S. V. and Rouseff, R. L. 1986. Citrus Fruits and Their Products. Marcel Dekker, Inc., New
York, 177-178.
Trammell, D. J., Dalsis, D. E., and Malone, C. T. 1986. Effect of oxygen of the taste, ascorbic
acid loss, and browning for high-temperature-short-time pasteurized single strength orange juice,
J. Food Sci., 51(4), 1021-1023.
Chapter 19

Juice Adulteration

Fraudulent representation of foods and medicines has a long history. In the days
of the wild west, snake oils and medicinal tonics were sold to gullible passersby
at a price that was hard to tum down. These concoctions were consumed in the
hope of there being at least a remote possibility that some of their claims would
be valid but many of these "cure-aIls" caused more damage than they reme-
died.
In 1938, the United States Congress enacted the Federal Food, Drug, and
Cosmetic Act. Even though there was an earlier law, and the Act has been
modified somewhat since, it remains essentially intact today. This law gave
definition to the term "adulteration," which is described in section 402 of the
Act. The Food and Drug Administration (FDA) has the responsibility for en-
forcing this law, which requires different emphases and methods depending on
which type of adulteration is involved. The four basic types of adulteration are:
(1) filthy, putrid, decomposed, or harmful; (2) unsafe or unsanitary; (3) statu-
torily unsafe; and (4) economic (Stutsman 1988).
The first kind of adulteration is a concern for the manufacturers of any prod-
uct. Chapter 17 covers a portion of this type of contamination. There is no
product made that cannot be dangerous in the wrong situation. The production
process for any consumable food, such as citrus juices, is not totally invulner-
able to the possible addition of poisons or harmful materials. In recent times a
great deal of attention has been paid to packaging that prevents the addition of
dangerous substances by persons other than the manufacturer. Citrus juices often
are packaged in cans, plastic containers, or cartons that are difficult to tamper
with in retail stores. Industrial processing and storage areas should maintain a
security system to prevent outsiders from roaming around the plant. Processing
records should be detailed enough that any problems can be traced back to
specific employees. This way employees can be held accountable for their own
actions, in addition to serving as watch dogs for the product during processing.
The second type of adulteration involves processing in such a manner that
the food may become adulterated. Because the FDA cannot continually inspect

279
D. Kimball, Citrus Processing
© Van Nostrand Reinhold, New York, NY 1991
280 CITRUS JUICE SANITATION

a processing area, it needs the flexibility of preventing adulteration by prevent-


ing the conditions that would cause adulteration as much as possible. For ex-
ample, if there are many insects in the plant, their presence would constitute an
unsanitary condition because the insects would be likely to cause contamination
even if they were not actually found in the product.
The third type of adulteration involves substances that are declared by law to
be unsafe, which usually are excluded from the group referred to as "food
additives." Food additives must undergo thorough screening in order to deter-
mine if they can be safely added or used in food products. In order for a sub-
stance to be used in a food, it must be "generally recognized as safe" or achieve
GRAS status. Food additives that are considered safe because of common usage
prior to January 1, 1958 have GRAS status (Title 21 CFR 170.30(c» without
extensive additional testing. Food additives developed since then must undergo
a rigorous screening process. Detailed descriptions of those substances that can
be used in foods or come into contact with foods can be found in the Code of
Federal Regulations, Title 21 170-189. This list continues to be augmented with
the development of new food additives and processes.
The last type of adulteration is economic adulteration. Laws relating to this
type of adulteration do not permit the use of materials that are not described or
implied on the label. Because a full description of how a product, such as orange
juice, was manufactured would be lengthy and confusing, standards of identity
have been invoked to simplify the identification of foods and beverages. As a
result, the federal standards of identity for citrus juices have evolved. These
standards of identity go far beyond descriptions of the other forms of adulter-
ation in stating exactly how a citrus juice can be made and/or formulated. Many
acceptable food additives that have achieved GRAS status and are acceptable
with respect to the first three forms of adulteration are not acceptable in regard
to the standards of identity. It should be remembered that the standards of iden-
tity and the Food, Drug, and Cosmetic Act are designed to prevent contami-
nation, fraud, or a decrease in the value of food products. New technologies
that legitimately enhance the quality of food products, such as debittering, gen-
erally do not come under restriction according to the intent of the Act.

STANDARDS OF IDENTITY

The standards of identity for various citrus products are contained in the Code
of Federal Regulations and the Federal Register. These standards and their
interpretation may change from time to time, and the current status of such
standards should be monitored by quality control management with the aid of
legal counsel if necessary. With this charge in mind, the following constitutes
a brief description of the most current standards of identity for citrus products
available:
Orange Juice (CFR Title 21 146.135). This product contains juice from un-
JUICE ADULTERATION 281

fermented fruit of sweet orange varieties (c. sinensis) with seeds and excess
pulp removed. The product may be chilled but not frozen.
Frozen Orange Juice (CFR Title 21 146.137). This product is the same as
orange juice except that it is frozen.
Pasteurized Orange Juice (CFR Title 21 146.140). This product is the same
as orange juice except that pasteurized orange juice can contain up to 10% of
tangerine juice (c. reticulata) or its hybrids. Also, oil and pulp (not washed or
spent pulp) can be added. Concentrated orange juice, sugar, invert sugar, dex-
trose dried com sirup, or dried glucose sirup can be added to raise the Brix to
a normal range for orange juice, but such addition must be declared on the label.
The juice can be heat-treated to reduce enzyme activity and the number of viable
microorganisms. This juice can be frozen and must have a Brix of at least 10.5,
not including added sweeteners. The B / A ratio must be at least 10.
Canned Orange Juice (CPR Title 21 146.141). This product is the same as
pasteurized orange juice with certain additional characteristics: the condensate
water from deoiling may be added, the minimum Brix is 10, and the minimum
B / A ratio is 9. Also, if the juice is not refrigerated, the word "canned" can be
omitted from the label.
Orange Juice from Concentrate (CPR Title 21 146.145). Orange juice from
concentrate contains reconstituted frozen concentrated orange juice or orange
concentrate for manufacturing and may contain orange juice, pasteurized orange
juice, orange juice for manufacturing that has been preserved by freezing and
not canning, orange oil, unwashed pulp, and water. It may contain the same
declared sweeteners as pasteurized orange juice, and may be heated or pasteur-
ized. It must contain at least 11.8°Brix exclusive of any added sweeteners.
Frozen Concentrated Orange Juice (CPR Title 21 146.146). This product
may contain 10% tangerine juice or its hybrids (c. reticulata) and/or 5 % sour
orange juice (c. aurantium). It may contain water, orange oil, orange essence,
unwashed pulp, and the same declared sweeteners as above. The product can
be heat-treated. In order to reconstitute this product to not less than 11. 8 °Brix,
the dilution ratio should be not less than 3 parts water to 1 part concentrate.
Reduced Acid Orange Juice (CPR Title 21 146.148). This product is the
same as frozen concentrate orange juice except that it must employ the use of
anionic ion exchange as permitted in 173.25 of Title 21 in reducing the acid
levels, and the B / A ratio must be between 21 and 26.
Canned Concentrated Orange Juice (CPR Title 21 146.150). This product
is the same as frozen concentrated orange juice except that it is not frozen, and
it is canned and heat-treated so as to prevent spoilage.
Orange Juice for Manufacturing (CFR Title 21 146.151). This product is the
same as orange juice except that it can have a lower Brix and B / A ratio than
required for orange juice and can contain up to 10% tangerine juice or its hy-
brids (c. reticulata). Unwashed pulp and orange oil also may be added, and it
may be heat-treated, chilled, and/or frozen.
282 CITRUS JUICE SANITATION

Orange Juice with a Preservative (CFR Title 21 146.152). This product is


the same as orange juice for manufacturing except that a declared preservative
has been added.
Concentrated Orange Juice for Manufacturing (CFR Title 21 146.153). This
product is the same as frozen concentrated orange juice except that the Brix and
B / A ratio may be less than that required for frozen concentrated orange juice.
However, this product must be concentrated to at least 20oBrix.
Concentrated Orange Juice with a Preservative (CFR Title 21 146.154).
This product is the same as concentrated orange juice for manufacturing except
that it contains a declared preservative.
Grapefruit Juice (CFR Title 21 146.132). This standard is similar to the
orange juice standard except that the use of a mechanical means of juice ex-
traction is mentioned, and it must come from fruit of the C. paradisi species.
Only 10% by volume ofthis product can come from grapefruit hybrids, and no
more than 15 % can come from grapefruit concentrate. Grapefruit pulp, oil, and
essence can be added, as well as the same declared sweeteners mentioned in
the pasteurized orange juice standard. A minimum of lO oBrix exclusive of added
sweeteners is required, with the Brix corrected for acid by adding 0.012 +
0.193x - 0.0004x2, where x is the % acid. The product may be heat-treated,
canned, or frozen.
Lemon Juice (CFR Title 21 146.114). This product is made from fruit of the
C. limon (L.) Burm. f. species and has a similar standard to those for orange
and grapefruit juices. Acceptable additives include reconstituted lemon concen-
trate so as not to increase the acidity by more than 15 % of the finished food,
water, lemon oil, and preservatives. The juice can be manufactured from lemon
concentrate, but it must have a temperature-, but not acid-, corrected Brix of at
least 6, and a titratable acidity of 4.5 % if this is done. Lemon juice can be heat-
treated, canned, chilled, or frozen. It also must fill 90% of a standard container
unfrozen.
Frozen Concentrate for Lemonade (CFR Title 21 146.120). This product is
made from lemon juice along with any combination of suitable nutritive car-
bohydrate sweeteners. It must have a corrected Brix of at least 48.0, with the
acidity in the final product being at least 0.70 g /100 ml with a concentration
of at least 1O.5°Brix. Acceptable additives include lemon pulp and lemon oil.
Frozen Concentrate for Artificially Sweetened Lemonade (CFR Title 21
146.121). This standard is the same as that for frozen concentrate for lemonade
except that in lieu of nutritive sweeteners it is sweetened with one or more of
the artificial sweeteners listed in sections 172, 180, or 184 of Title 21, such as
Aspartame. If such artificial sweeteners are used, the Brix requirement men-
tioned in the previous standard does not apply. Dispersing agents can be used
to disperse the lemon oil, as well as thickening agents, as long as they are not
food additives as defined in section 102(s) of Title 21. Ifthe thickening agents
JUICE ADULTERATION 283

are defined as food additives, they can be used, provided that they comply with
section 409 of Title 21.

Economic Fraud

As mentioned in Chapter 15, citrus juices pose no health risk to consumers


because no pathogenic organisms can survive the juice acidity. However, eco-
nomic fraud is a very real concern to citrus processors. Economic fraud basi-
cally consists of the use of a cheaper material to formulate a juice without
declaring it on the label, and selling it as if it contained the more expensive but
authentic juice. Greed among manufacturers of citrus products has led to eco-
nomic fraud in the industry, and such fraud drives prices down and hurts the
honest citrus juice manufacturer besides deceiving consumers. Some consumers
have allergic reactions when certain changes are made in juice composition,
and ifthese changes are not declared on the label, a serious health problem may
arise in those rare but very real circumstances. If a processor purchases adul-
terated juice, even in ignorance, and uses it to formulate its own products, both
of the companies involved become legally liable for the adulteration. For this
reason, it behooves every citrus processor to be vigilant in the detection of juice
adulteration. Failure to do so can be very costly. Those companies convicted
of adulteration face millions of dollars in fines, including the costs of the in-
vestigations, costly recalls, and years of prison terms for management personnel
so involved (see "3 Charged in Sale of Phony Orange Juice," Los Angeles
Times, Thursday, July 27, 1989, page 14 of part I).
Besides the specific descriptions found in the standards of identity, section
402(b) of the Food, Drug, and Cosmetic Act gives four charges that can be
used to describe adulteration (Stutsman 1988):

I. If any valuable constituent has been in whole or in part omitted or ab-


stracted therefrom.
2. If any substance has been substituted wholly or in part therefor.
3. If damage or inferiority has been concealed in any manner.
4. If any substance has been added thereto or mixed or packed therewith so
as to increase its bulk or weight, or reduce its quality or strength, or make
it appear better or of greater value than it is.

An example of violation of the first charge would be the removal of vitamin


C using activated charcoal. Activated charcoal has long been known to remove
limonin bitterness from citrus juices as well as sensitive anthocyanin pigments
that may tum brown and produce off flavors. However, activated charcoal also
removes significant amounts of vitamin C. The addition of undeclared vitamin
C to make up for this would constitute a violation of the second charge. Adding
284 CITRUS JUICE SANITATION

artificial colors to mask poor juice color would be a violation of the third charge.
The addition of cheaper carbohydrates would be a clear violation of the fourth
charge.

TYPES OF ECONOMIC ADULTERATION

There are many types of economic adulteration. However, nearly every type of
adulteration that has been known to occur in the industry falls into one of four
different categories: water addition, carbohydrate addition, cover-up, and
blending of unauthorized juices or juice products.

Water Addition

Some of the standards of identity exclude the addition of water. These standards
involve single-strength juices that are neither concentrated nor made from con-
centrate. These juices include lemon juice, grapefruit juice, orange juice, frozen
orange juice, pasteurized orange juice, canned orange juice, orange juice for
manufacturing, orange juice with preservative, and canned tangerine juice. The
last is defined under USDA grade standards rather than as a separate standard
of identity. On the other hand, the citrus juice products whose standard of iden-
tity allows for the addition of water include orange juice from concentrate,
frozen concentrated orange juice, reduced acid frozen concentrated orange juice,
concentrated orange juice for manufacturing, and concentrated orange juice with
a preservative.
Water comprises over 80% of the composition of natural juices, so detection
of its illicit addition can be difficult; but it can be done in one of two ways.
One method is to monitor the mineral content of the juice. Natural juices have
a certain range of mineral levels as follows:

Orange Grapefruit
Sodium <50 ppm <50 ppm
Potassium > 1400 ppm 300-500 ppm
Calcium 65-120 ppm 100-150 ppm
Magnesium 95-170 ppm 90-140 ppm
Phosphorous 120-310 ppm

Potable water from the city, which is used in many plants, may contain much
higher levels of these minerals, and high mineral levels would indicate illicit
water addition. Because pulp washing utilizes plant water, high mineral levels
also may be indicative of pulp wash addition although legal water addition can
occur in citrus concentrates without the addition of pulp wash. Minerals can be
determined by using a variety of methods, which usually involve instrumenta-
JUICE ADULTERATION 285

tion beyond the resources of most quality control laboratories. Professional lab-
oratories provide an economic means of determining mineral levels.
Treated water naturally low in minerals could not be detected through mineral
analyses. However, a method has been developed that can distinguish between
water that is natural to the juice and water added from other sources (Winters
et al. 1988; Brause et al. 1984). This method involves the measurement of the
oxygen isotope ratios. When water is absorbed into the plant through the root
system, it has a tendency to lose the lighter IH and 160 isotopes through eva-
potranspiration and to keep the heavier deuterium eH) and 18 0 isotopes. The
oxygen isotope ratios are determined by using a complex procedure, also rec-
ommended for professional laboratories, and the results are reported as 0 180 by
use of the following equation:

0 180 (ppt) = (Rsample - Rstandard) (1000) I Rstandard ( 19-1 )

In this equation the R values are the 180 / 6 0 isotope ratios. For concentrated
orange juice above 60 o Brix, the 0 180 value should be above + 10. For authentic
single-strength orange juice the 0 18 0 value should be positive. Anything less
than these values is indicative of water addition.

Carbohydrate Addition

Because citrus juices are comprised primarily of carbohydrates and water, the
addition of cheaper carbohydrates to authentic juices has been a lucrative way
to falsify citrus products. Citrus juices are sold by the weight of the soluble
solid equivalent of carbohydrates. When commercial sugars are sold as low as
5C lIb, and the equivalent orange juice price is up to $2.00 lIb soluble solids,
one can see how much the profit margin can be increased with substitution of
commercial sugars or similar products.
Several methods can be used to detect carbohydrate adulteration. One of the
simplest is based on the sugar composition of the juice itself. Citrus juices
contain sucrose, glucose, and fructose, in a ratio of about 2: 1 : 1. Glucose and
fructose are known as reducing sugars because they can be oxidized by using
mild oxidizing agents. Sucrose, however, cannot be oxidized by mild oxidizing
agents because its anomeric carbon forms the bond between its glucose and
fructose monomers. Thus a measure of the reducing sugars, a relatively easy
determination, should result in the determination of about half of the carbohy-
drates, which in tum constitutes about 80 to 90% of the total soluble solids of
the Brix value. The use of high-fructose com syrup or cane sugars (predomi-
nately sucrose) can be detected quickly by the following method. However,
invert beet sugars or special combinations of reducing and nonreducing sugars
286 CITRUS JUICE SANITATION

cannot be detected from a reducing sugar test; so this method should constitute
a preliminary screening and not serve as a verification of authenticity.
The following reducing sugar test is based on the reduction of Cu 2 + to Cu I +
by the reducing sugar. The Cu 2 + ions usually form a light blue color in aqueous
solution, when they are reduced to Cu 1+, an orange-colored oxide precipitate
is formed, according to the following equation:

blue sugar orange

The reaction is catalyzed by tartrate, and methylene blue dye is used as an


indicator. When the copper has all been reduced, the dye indicator is quickly
reduced, resulting in a dramatic color change from the deep navy blue of the
indicator to the bright orange of the copper oxide.

Reducing Sugars Test (AOAC 1984)

Equipment and Supplies

• 10 ml buret, 125 ml Erlenmeyer flask or beaker, and magnetic stirrer/


heater for titration.
• Copper solution. (Dissolve exactly 69.278 g of CUS04 . H 2 0 in 1 liter of
distilled water.)
• Tartrate solution. (Dissolve 346 g of potassium sodium tartrate (Rochelle
salt) and 100 g of NaOH in 1 liter of distilled water.)
• 1 % methylene blue indicator. (Dissolve about 1 g in 100 ml of distilled
water.)
• Two 2 ml pipettes.
• Lab centrifuge.
• Boiling chips.
• 10 ml graduated cylinder.

Procedure

1. Centrifuge reconstituted or single-strength juice (l1.8°Brix) for 10 min-


utes as outlined in Chapter 7. Add 1 ml of the serum to the 10 ml grad-
uated cylinder, and fill it to 10 ml with water.
2. Pipette 2 ml of the copper solution and 2 ml of the tartrate solution into
the 125 ml Erlenmeyer flask, and fill the flask to about 50 ml with distilled
water. Add a few boiling chips, and heat this solution to boiling.
3. Pour the centrifuged juice sample serum into the 10 ml buret, and zero it.
JUICE ADULTERATION 287

4. Titrate the copper solution while stirring with the sample serum until a
dark orange color is observed. Add 3 drops of the indicator, and continue
titrating until the bright orange of the copper oxide is fully restored.
5. The % reducing sugars (RS) can be calculated from the following:

(0.002 liter Cu) (69.278g/1 Cu) (180.16g/mole sugar)


(100%) (IO-fold dilution)
%RS (19-3 )
(249.68g/mole Cu)(4 moles Cu/mole sugar)
( 1.0446g/ ml juice) (ml titrated)
or:
%RS = 23.93/( ml titrated) (19-4)

For example:
23.93/4.77 ml titrated = 5.02 % reducing sugars

Levels below 4.5 or above 5.5 might be suspect in regards to carbohydrate


adulteration.
A surer way of determining the amount of nonjuice carbohydrates in citrus
juices involves the use of \3C / 12C ratios (Bricout and Koziet 1987). These
ratios usually are expressed in the same manner as the 15 180, as follows:

(19-5)

It has been found that there is a difference in this ratio for different plants in
nature. Simpler C4 plants, such as com and sugar cane, have O\3C values around
-10, whereas higher C 3 plants, such as flowers and trees (citrus), have a O\3C
value below -22. Therefore, if sugar from cane or com is used in citrus juices,
a higher D\3C value will be observed. The analytical methods required for such
a determination are, again, expensive and complex and best left to professional
laboratories.
Another procedure has been developed (Low 1989) to detect invert beet sugar
down as low as 1 %, and perhaps even as low as 0.1 %. This method employs
the use of HPLC with a pulse amperometric detector that is several orders of
magnitude more sensitive than refractive index detectors. The method detects
the adulterating carbohydrates by determining the oligosaccharide pattern. With
this new technique, any illicit carbohydrate adulteration can be detected.

Cover-Up

When juice has been adulterated, it often becomes necessary to add something
else in order to cover up the adulteration. For example, one of the simplest tests
288 CITRUS JUICE SANITATION

used in detecting the illicit addition of pulp wash has been the formol or for-
maldehyde test, which measures the amount of primary amines. Pulp wash has
a lower concentration of amino acids than authentic juice has, and its illicit
addition may be detected by this very fast and simple technique. However, it
is possible to get around the test with the addition of very cheap amino salts-
the addition of the amino salts being a second adulteration used to cover up the
first adulteration. Because it is so easily circumvented, the formol test has be-
come a weak test for juice adulteration. However, it is useful in other parts of
citrus quality control, as mentioned in the preceding chapter, and as a prelim-
inary adulteration screening.
Another common cover-up technique is the addition of colors. When a juice
is adulterated with something other than juice, it must become more dilute in
authentic components including colors. The addition of turmeric, annatto, or
other dyes (FD&C dyes), which makes the juice a darker orange, has been used
in adulteration cover-ups. However, these dyes can be easily tested for by any
quality control laboratory using the following techniques.
Turmeric is prepared from the dried roots of the tuberous rhizomes of Cur-
cuma tonga L., a member of the ginger family. It is native to southern and
southeastern Asia and is commercially cultivated in Malaysia. The color com-
ponent of turmeric is curcumin, also known as turmeric yellow, with the fol-
lowing chemical structure:

<OCH 3

rCH=CH-<O/OH
CH 2

~OCH=CH-<0 (-OH
OCH 3
Annatto dyes are natural carotenoid colorants derived from the seed of the
tropical annatto tree or Bixa orellana. The primary color component is bixin, a
carotenoid with the following chemical structure:

CH 3 CH 3 H H CH 3
I I I I I
H COOC-CH C CH C C~ Ct-i C=C C CH 3COOH
3 ~/~/ ~/~/ ,/" \//\//
CH CH CH CH CH C CH CH
I
CH 3
JUICE ADULTERATION 289

The water-soluble fonn of bixin is norbixin, which is fonned from the sa-
ponication of the methyl ester group. A single test can be used to detect either
annatto or tunneric. Even though you can continue the test to detennine which
dye has been added, the presence of either dye indicates adulteration.

Turmeric and Annatto Determination (AOAC 1980)

Equipment and Supplies

• I-liter Erlenmeyer flask.


• 100 ml graduated cy tinder.
• 500 ml graduated cylinder.
• Magnetic stirrer.
• Rotary evaporator or equivalent.
• 500 ml separatory funnel.
• Two 150 ml Erlenmeyer flasks or beakers.
• 600 ml of 95 % ethanol.
• Vacuum filter apparatus.
• Ammonium hydroxide (reagent grade).
• About 400 ml hexane.
• Glacial acetic acid.
• Curcumin and annatto for color comparison.

Procedure

1. Place 100 ml of reconstituted or single-strength orange juice ( 11.8 °Brix)


in the I-liter Erlenmeyer flask.
2. Add 600 ml of 95 % ethanol, stir the mixture occasionally, and let it stand
for several hours. Then filter it.
3. Evaporate the filtrate to 100 ml using a rotary evaporator or the equiva-
lent, and pour it into a 500 ml separatory funnel.
4. Add 25 ml of 25% NaCI and enough ammonium hydroxide to make the
solution alkaline.
5. Extract the lipids and oily pigments from the solution using 200 ml of
hexane.
6. Immediately acidify the bottom aqueous layer with acetic, and extract it
with hexane. If the hexane layer is colored, then tunneric or annatto is
present. To see the difference between the presence and the absence of
tunneric or annatto, add enough curcumin or annatto to the juice sample
to see a detectable color change. Then repeat the test. The presence of
tunneric or annatto should be readily discernible by comparison with sam-
ples with no dyes present.
290 CITRUS JUICE SANITATION

This test is a pass/fail test. Any discernible deepening of the color in the last
hexane layer indicates the presence of these dyes.
The Food and Drug Act of 1906 certified 7 dyes that could be used in foods.
By 1938, when the Food, Drug, and Cosmetic Act was passed, 11 more dyes
were included, and thereafter these dyes were referred to as FD&C dyes by
number. The azo dyes, FD&C Yellow No.5 and FD&C Yellow No.6, have
been used to restore diluted orange juice color. FD&C No. 5 is also called
tartrazine or hydrazine yellow. It has the following chemical structure:

In 1856 dyes from coal tar were discovered, and for the next 80 years these
dyes were used extensively in food products. More modem synthetic techniques
generally have replaced the extraction of these dyes from coal tar. The presence
of coal tar dyes and of FD&C dyes can be detected simultaneously using the
following simple test. Again this is a pass/fail test. Any detection of these dyes
would constitute adulteration in 100% orange juice products.

FD&C and Coal Tar Dyes (Ting and Rouseff 1986)

Equipment and Supplies

• 1 g of calcium carbonate.
• Acetone and petroleum ether in the ratio of 1 : 3.
• 500 ml separatory funnel.
JUICE ADULTERATION 291

Procedure

1. Add 1 g of calcium carbonate to 5 ml of reconstituted or single-strength


orange juice (l1.8°Brix).
2. Add 30 ml of the acetone/petroleum ether solution, shake the mixture for
3 minutes, and allow the layers to separate.
3. If the aqueous layer is orange-yellow, it has FD&C or coal tar dyes added.
A slight yellow color is acceptable. Just enough FD&C colors should be
added to a juice sample to cause a noticeable color change, which should
be compared to the color of authentic samples.
Other colorants and cover-up compounds can be and have been used to cover
up citrus juice adulteration. Because any adulteration involves juice dilution,
the measurement of authentic juice components that are too expensive or im-
possible to falsify can be used to detect juice dilution rather than adulterant
addition. One such component is isocitric acid, for which there is no commer-
cial source. If the isocitric acid content falls below 44 ppm, one can be assured
that the authentic juice has been diluted. Affordable test kits are available for
the determination of isocitric acid, which can be used routinely in any quality
control laboratory (Boehringer Mannheim Biochemicals, Indianapolis, Ind.).

Addition to Unauthorized Juices or Juice Products

Most orange juice products are allowed to contain up to 10% tangerine or tan-
gerine hybrids while still being called 100% orange juice. The high color of
tangerine juice is used to enhance the appearance of orange juices of weaker
color, primarily in Florida. However, other fruit juices usually are less expen-
sive than tangerine juice and have been illegally added to orange juices in direct
violation of the standards of identity. Apple, pear, white grape, orange pulp
wash, and grapefruit juices usually are sold at lower prices than that of orange
juice, and when they are blended into orange juice products, their economical
returns are augmented greatly. Apple, pear, and white grape can be detected by
using isocitric tests or other more complex testing schemes based on composi-
tional differences. Grapefruit juice contains the characteristic compound narin-
gin, so naringin determinations can be used to detect grapefruit adulteration in
orange juice (see Chapter 10 for analytical methods).
Federal law allows pulp wash to be added to citrus juices on-line in an amount
that constitutes about 5 to 10% of the juice, but if the pulp wash is separated
and packaged separately, it can no longer be legally added to other citrus prod-
ucts. Florida law prohibits any addition of pulp wash to any 100% citrus juices,
and in order to detect illicit pulp wash addition, Florida requires the addition
of sodium benzoate to all pulp wash juices to act as a tracer. If sodium benzoate
is found in 100% orange juice products, it is assumed that Florida pulp wash
292 CITRUS JUICE SANITATION

was used as an adulterant. However, failure to find the benzoate tracer is no


guarantee that the product does not contain illicit pulp wash. Pulp wash is gen-
erally used in drink bases that add preservatives, such as benzoates, and the
pulp wash product itself is not damaged by the benzoate addition.

ADULTERATION SCREENING PROCEDURES

Several adulteration screening procedures are used around the world, ranging
from special computerized packages available from a single manufacturer to
specialized techniques developed by individual laboratories to government-reg-
ulated procedures and criteria. These procedures are constantly in a state of
development and change, and new methods and technologies are constantly
appearing (Nagy, Attaway, and Rhodes 1988; Fruit Juice Adulteration Work-
shop 1989). However, most of these techniques are beyond the scope and re-
sources of most industrial quality control laboratories; so professional labora-
tories usually are consulted regarding the analytical work. However, a
knowledge of the standard methods can be helpful to any citrus quality control
facility.

Europe

Northern Europe has seen the establishment of some of the most sophisticated
adulteration procedures in the world, and presently three standards are being
used in Europe: the German RSK (Hofsommer 1989; Association of the Ger-
man Fruit Juice Industry 1987), the French AFNOR (Hofsommer 1989; Union
Nationale des Producteurs de Jus de Fruits 1989), and a criterion used by the
Netherlands and Belgium, referred to here as the Dutch standard (Hofsommer
1989; Warenwet P.B.O.-voorschriften (E-17a) 1977). The European Commu-
nity is working toward a single EC standard but has encountered some diffi-
culty. One problem, for example, is that many different products are of concern
to these countries. The following listing shows the juice products that each
standard covers:
RSK
AFNOR (French) (German) Dutch
Apple Apple Apple
Grape Apricot Grape
Grapefruit Black currant Grapefruit
Lemon Grape Orange
Orange Grapefruit
Pineapple Lemon
Tomato Orange
Passion fruit
Pear
Raspberry
Sour Cherry
JUICE ADUL TERA TION 293

With so many different products, it is difficult to establish a single unified stan-


dard. Also, the use of standards does not guarantee the absence of adulteration,
as standards can be circumvented. However, properly used standards can con-
stitute a significant deterrent to juice falsification. Tables 19-1 through 19-3
show the ranges of juice components that characterize each of the three Euro-
pean standards. Juices entering the affected countries must meet these stan-
dards.

United States

As yet, the United States does not have an official standard for authentic juices
that compares with the European standards. The standards of identity simply
declare that the juice must be authentic and describe the natural components
permitted in it, such as pulp, citrus oils, and so on. When citrus juices are
imported into the United States, or when a commercial product is suspected of
adulteration, any and all means can be used to prove such adulterations, in-
cluding employee depositions, chemical tests, and/or inspection of company
records. Imported juices usually go through a screening process by customs and
FDA officials that is somewhat easy to monitor, even though it is impossible to
thoroughly analyze every imported lot. However, the inspection of domestic
juice is not required, and the monitoring of adulteration is much more difficult
domestically. The most likely person to detect domestic adulteration is a com-
petitor or a customer of the juice adulterator. Adulteration may be suspected if
a product is selling for too Iowa price, or an in-house screening procedure may
unearth suspect material. A competitor may wish to notify the FDA and pursue
criminal prosecution of the adulterator, while a customer may wish just to cease
doing business with a suspected supplier. The latter does not require as much
rigorous proof.
Even a rumor that a company is adulterating its juices can cause it difficulty
in marketing its products. Even if a company purchases blend components from
a suspected company, the purchaser's reputation may be on the line. Not only
are reputations of companies at stake, but also the reputations of management
personnel, especially quality control management. It would be difficult to con-
vince a judge that quality control personnel were entirely ignorant of adultera-
tion that was going on within the company because it is their specific job to
monitor the composition of the company's products.
The adulteration tests are quite numerous and complex, including sophisti-
cated computerized systems that are now on the market. However, the resources
of most quality control facilities are usually quite limited and exclude the bulk
of these techniques. Professional laboratories have tried to find an economic
and thorough method of adulteration detection that can be of use to any citrus
quality control laboratory. One such method is the matrix method of detecting
juice adulteration (Brause et al. 1984), which consists of the measurement of
294 CITRUS JUICE SANITATION

Table 19-1. French orange juice authenticity


standards (AFNOR) (Hofsommer 1989; Union
Nationale des Producteurs de Jus de Fruits 1989).
Parameter Acceptable Range
Density at 20°C ~ 1.040
Total solids (g/IOO g) ~10.5
Titratable acidity (mmoI/L) 100-250
Refractometer dry extract ( % ) ~ 10.2
Ash (giL) 2.8-5.5
Ethanol (giL) ,;:;3
Sulfur dioxide (mg/L) ,;:;10
d-Limonene number (milL) ,;:;0.3
Copper (mg/L) ,;:;5
Zinc (mg/L) ,;:;5
Iron (mg/L) ,;:; 15
Lead (mg/L) ,;:;0.3
Arsenic (mg/L) ,;:;0.2
Cadmium (mg/L) ,;:;0.05
Tin (mg/L) ,;:; 100
Mercury (mg/L) ,;:;0.01
Sodium (mg IL) ,;:;40
Potassium (mg/L) 1100-2500
Calcium (mg/L) 50-240
Magnesium (mg/L) 70-170
Phosphorus (mg/L P) 100-225
Pulp(%v/v) ,;:; 15
Total carotenoids (mg/L) 3-26
~-carotene (mg/L) ,;:; 1.8
Naringin (mg/L) ,;:;10
Hesperidin (mg/L) 150-1000
Sucrose (giL) 5-50
Glucose (giL) 20-50
Fructose (giL) 20-50
Maltose (giL) o
Glucose I fructose ratio 0.8-1.2
Total sugars (giL) 80-115%
L-Malic (giL) 0.6-4
Tartaric acid o
Citric acid (giL) 6-16
Isocitric acid (mg/L) 60-200
Ascorbic acid and dehydroascorbic acid (mg/L) ~200
Aspartic acid (mg/L) 100-500
Threonine (mg I L) 10-60
Serine (mg/L) 80-250
Asparagine (mg/L) 180-1000
Glutamic acid (mg/L) 50-200
Proline (mg/L) 400-2500
Glycine (mg/L) 10-40
Alanine (mg/L) 45-200
Valine (mg/L) 10-40
JUICE ADULTERATION 295

Table 19-1. (Continued)


Parameter Acceptable Range
Methionine (rng/L) 1-5
Isoleucine (rng/L) 2-15
Leucine (rng/L) 2-15
Tyrosine (rng/L) 15-20
Pheny lalanine (rng / L ) 15-50
-y-Arninobutryric acid (rng/L) 150-800
Ornithine (rng/L) 5-20
Lysine (rng/L) 20-80
Histidine (rng/L) 5-30
Arginine (rng/L) 400-1400
Total free amino acids (mg/L) 2000-5000

21 parameters, as shown in Table 19-4. Many of these tests can be perfonned


in a citrus quality control laboratory , but, as with any set of standards, analysts
should be careful in interpreting the results. The FDA has established a pattern
recognition method, involving many juice parameters and using specialized

Table 19-2. Dutch orange juice standards


(Hofsommer 1989; Warenwet
P.B.O.-voorschriften (E-17a) 1976).
Parameter Acceptable Range
(Sugar?) extract (g/L) ~25
(Acid?) (g/L) ~3.3
Potassium (mg/L) ~ 1500
Phosphorous (mg/L) ~ 120
Hesperidin (mg/L) :s 1000
Proline (mg/L) ~575
Pectin (mg/L) :s700
D- Isocitric acid (mg / L ) ~70
Ratio citric acid / D-isocitric acid :s 130
Ratio glucose / fructose :s 1.00
Pulp (%) :s1O
(Formol number?) (ml / 100 ml) ~ 15.0
Aspartic acid (mmol /L) ~ 1.7
Serine (mmol/L) ~ 1.0
Asparagine (mmol/L) ~ 1.7
Glutamic acid (mmol/L) ~0.5
Alanine (mmol/L) ~0.7
Aminobutyric acid (mmol /L) ~ 1.7
Arginine (mmol/L) ~2.5
Glycine (mmol/L) :s0.3
Glutamine (mmol/L) :s0.5
Acid-corrected sugar extract ~ 11.2°Brix
296 CITRUS JUICE SANITATION

Table 19-3. German orange juice standards (RSK)


(Hofsommer 1989; Association of the German Fruit
Juice Industry 1987).
Parameter Acceptable Range
Color (points) ~3
Aroma (points) ~3
Flavor (points) ~5
Relative density (g/ml 20 0 /20°C) ~ 1.0450
Corrected Brix ~11.l8
Soluble solids (g /L) ~ 116.8
Titratable acids (pH 7.0)
as tartaric acid (g/L) ~8.0
Sulfurous acid (mg/L) slO
Ethanol (g/L) s3.0
Volatile acids as acetic acid (g/L) sOA
Lactic acid (g /L) sO.5
L-Malic acid (g/L) s2.5
Citric acid (g/L) ~8.0
D-Isocitric acid (mg/L) ~70
Citric acid/D-isocitric acid ratio s 130
Tartaric acid (g/L) o
Glucose (g/L) ~22
Fructose (g/L) ~24
Glucose/fructose ratio sl.O
Sucrose (g/L) s45
Sucrose ( % in total sugar) s50
Reduction free extract (g/L) ~26
Ash (g/L) ~3.5
Alkalinity number ~11.0
Potassium (mg/L) ~ 1700
Sodium (mg/L) s30
Magnesium (mg/L) ~90
Calcium (mg/L) sIlO
Chloride (mg/L) s60
Nitrate (mg/L) slO.0
Phosphate (mg/L) ~400
Sulfate (mg/L) s 150
Formol number
(ml 0.1 mol NaOH/loo ml) ~18
Corrected formol number ~90% of formol no.
Proline (mg/L) ~575
L-Ascorbic acid (mg/L) ~2oo
Flavonoid glycosides
as hesperidin (mg/L) slOoo
Water-soluble pectins expressed as
galacturonic acid anhydride (mg/L) s500
Aspartic acid (mmol/L) 1.7-3.0
Threonine (mmol/L) 0.10-0.30
Serine (mmol/L) 1.0-1.8
Asparagine (mmol/L) 1.7-4.5
JUICE ADULTERATION 297

Table 19-3. (Continued)


Parameter Acceptable Range
Glutamic acid (mmol/L) 0.5-1.1
Glutamine (mmol/L) :5 0.5
Proline (mmol/L) 3.9-11.3
Glycine (mmol /L) 0.15-0.30
Alanine (mmol /L) 0.7-1.5
Valine (mmol/L) 0.07-0.23
Methionine (mmol/L) trace-0.03
Iso-leucine (mmol /L) 0.025--0.065
Leucine (mmol/L) 0.020-0.060
Tyrosine (mmol/L) 0.025-0.10
Phenylalanine (mmol/L) 0.8-0.30
-y-Aminobutyric acid (mmol /L) 1.7-3.5
Ornithine (mmol/L) 0.025-0.10
Lysine (mmol/L) 0.15-0.40
Histidine (mmol/L) 0.03-0.12
Arginine (mmol/L) 2.5-6.0
Ammonia (mmol/L) :51.5
Ethanolamine (mmol/L) :50.6
Total carotenoids (mg/L) :515
iJ-Carotene as % total carotenoids :55
Cryptoxanthinester
as % total carotenoids :515
Pectic substances as galacturonic acid
anhydride
oxalate-soluble pectin (mg /L) :5200
alkali-soluble pectin (mg/L) :5300

computer software called ARTHUR (Page 1986), which enables investigators


to determine when a juice does not fit the normal composition.

In-house Methods

The purpose of this chapter is to acquaint citrus quality control personnel with
the problem of citrus juice adulteration and some of the things that have been
and are being done to correct the problem. Every quality control laboratory
should have some sort of screening system for all inbound products used in the
formulation of its products. Simple chemical tests such as those mentioned here
can constitute preliminary screenings. If these tests or information gathered from
other sources suggest the possibility of adulteration, more elaborate tests should
be performed. Periodic testing by professional laboratories is highly advisable,
and such spot checks are best done randomly.
Some observers have suggested the establishment of in-house or company
standards for the products the company purchases. The establishment of spec-
ifications is a common practice, but it rarely if ever includes standards specifi-
298 CITRUS JUICE SANITATION

Table 19-4. Specifications for orange juice


according to the matrix method of determining
authenticity used commercially in the United States
(Brause et al. 1984).
Parameter Acceptable Ranges
Fructose ( % ) 2-3
Glucose (%) 2-3
Sucrose (%) 3-5.5
Total sugars ( % ) 7.2-10.8
Glucose / fructose ratio 1.00
Total sugar of Brix ( % ) 61-91.5
Sucrose of total sugars ( % ) 30-60
Sodium (ppm) ::;50
Potassium (ppm) ;;", 1400
Calcium (ppm) 65-120
Magnesium (ppm) 95-170
Phosphorous (ppm) 120-310
Naringin (ppm) <2
Sodium benzoate o
Sorbitol o
Isocitric acid (ppm) ;;",44
UV-VIS-fluorescence (A443/ A 325 ) ;;",0.100
Fluorescence 2 peaks @ 270-306 nm
Stable isotope ratio ;;", + 10.0 (at 63°Brix)
as 5'80 (OSIRA) (%) ;;",0 (at 42°Brix)
;;",0 (fresh juice)
::;0 (recon juice)
::; -22.0

cally designed to prevent juice adulteration. The concept behind establishing


adulteration standards is the idea of rejecting a product on the basis of violation
of specifications, rather than having to prove that the product was adulterated.
On the other hand, if the supplier were unaware of the exact adulteration screen-
ing that was being used, it would be more difficult to cover up any falsification.
An appropriate screening program will consist of a blend of tests that can be
performed easily and economically, the use of professional laboratories for more
expensive and complex tests, cooperation from upper management including
purchasing and marketing, thoroughness, and common sense.

QUESTIONS

1. When was the Food, Drug, and Cosmetic Act enacted, and in what sec-
tion of the Act is adulteration specifically mentioned?
JUICE ADULTERATION 299

2. What are the four types of adulteration according to the FDA? Give an
example of each.
3. What are the four charges or descriptions of adulteration according to
Section 402(b) of the Act? Give an example of each.
4. What are the four main types of economic adulteration that occurs in the
citrus industry?
5. What citrus products can one legally add water to?
6. What is the surest way to detect water addition to citrus juices? Then
why are other methods used?
7. Why are sugar or sugar products added to citrus juices?
8. What limitations does the carbon isotope ratio determination have in de-
tecting illicit carbohydrate addition to citrus juices?
9. What is the surest method to detect adulteration cover-up, and why is it
so definitive?
10. How much grapefruit juice can one blend with concentrated orange juice
for manufacturing? How much tangerine juice?
11. How much pulp wash (%) can be contained in orange juice according
to Florida standards? U.S. standards?
12. What are the 3 standards used in Europe, and to which countries do they
apply?
13. What is the procedure used by the U.S. government (FDA)?
14. Who does most of the policing of adulteration in the United States?
15. What is the adulteration screening system used by your company? What
feasible screening process would you recommend?

PROBLEMS

1. What could you say for an orange juice sample that had the following mineral com-
position?
Na: 55 ppm
Ca: 126 ppm
K: 1565 ppm
Mg: 165 ppm
P: 306 ppm
2. Suppose that in three reducing sugar tests you titrated the following volumes (ml).
Give the % reducing sugars and interpret the results. What would be the appropriate
action in each case?

ml Titrated % Reducing Sugars Action


5.21
6.03
3.12
300 CITRUS JUICE SANITATION

3. What would 0 180 value of -0.15 indicate? What would a ol3e value of -20.5 in-
dicate?
4. A typical analysis of single-strength orange juice in the United States might be 0.65 %
w /w acid as citric acid, with a Brix/acid ratio of 18.2. Would this product pass the
RSK screening? Explain why or why not, and give reasons why the RSK may be
faulty in some circumstances.
5. Would the product in problem 4 meet the Dutch standards? How about the AFNOR
standards?

REFERENCES

AOAC 1980. Official Methods of Analysis, 13th Edition, 14.154. Association of Official Analytical
Chemists, Washington, D.C.
AOAC. 1984. Official Methods of Analysis, 14th Edition, 31.034-31.036. Association of Official
Analytical Chemists, Washington, D.C.
Association of the German Fruit Juice Industry. 1987. RSK Values, The Complete Manual. Fliis-
siges Obst GmbH, Bonn, Federal Republic of Germany, 1987.
Brause, A. R., Ratennan, J. M., Petrus, D. R., and Doner, L. W. 1984. Verification of authen-
ticity of orange juice, J. of the A. O.A. C., 67, 535.
Bricout, J. and Koziet, 1. 1987. Control of the authenticity of orange juice by isotopic analysis, J.
Agric. Food Chern., 35,758-760.
Fruit Juice Adulteration Workshop, August 9-10, 1989, Herndon, Va. Sponsored by General Phys-
ics Corporation, Columbia, Md.
Hofsommer, H. 1989. Analytical methodologies of detection as practiced in Europe. Presented at
the Fruit Juice Adulteration Workshop, August 9-10, 1989, Herndon, Va. Sponsored by General
Physics Corporation, Columbia, Md.
Low, N. 1989. Detection of beet medium invert sugar adulteration in high carbohydrate foods.
Presented at the Fruit Juice Adulteration Workshop, August 9-10, 1989, Herndon, Va. Spon-
sored by General Physics Corporation, Columbia, Md.
Nagy, S., Attaway, J. A., and Rhodes, M. E. eds. 1988. Adulteration of Fruit Juice Beverages.
Marcel Dekker, Inc., New York.
Page, S. W. 1986. Pattern recognition methods for the determination of food composition, Food
Tech., 40(1/) , 140-109.
Stutsman, M. J. 1988. Fruit juice adulteration, an overview of compliance and regulatory issues.
Presented at the Fruit Juice Adulteration Workshop, July 21, 1988, Herndon, Va. Sponsored by
General Physics Corporation, Columbia, Md.
Ting, S. V. and Rouseff, R. L. 1986. Citrus Fruits and Their Products. Marcel Dekker, Inc., New
York, 188.
Union Nationa1e des Producteurs de Jus de Fruits. AFNOR-UNPJF Fruit Juices Specifications.
Association Francaise de Normalisation, 1989.
Warenwet P. B. O.-voorschriften (E-17a), Verordening van 9 December 1976, Vb.Be.aft. 9, d.d.
7 -3-1977 van bei Produkischap van Groenten en Fruit.
Winters, K., Scalan, R. S., and Parker, P. L. Detection of orange juice adulteration by stable
isotope analyses. Presented at the Fruit Juice Adulteration Workshop, July 21, 1988, Herndon,
Va. Sponsored by General Physics Corporation, Columbia, Md.
Chapter 20

Food-Grade Nonjuice Products

Besides citrus juices, other food-grade products are manufactured from citrus
fruits. The most common among them are the citrus oils and essences, discussed
in Chapter 6. Pulp products also are very common, and were discussed in Chap-
ter 7. These flavoring and texturizing materials are used extensively in juice
products themselves, as well as in other foods. Other food-grade by-products
will be discussed in this chapter, including pectin, jellies, jams, fruit sections,
juice drinks, and purees. Peel extracts are commonly used as beverage bases in
many parts of the world, mainly as a result of improved debittering techniques.
Citrus flavors, including encapsulated flavors, are popular, but their production
involves technology beyond the scope of this book. Much of this product in-
formation is proprietary, as confidentiality is necessary in order to maintain a
healthy competitive climate. However, basic principles and products common
to the industry are discussed here.

PECTIN, JelLIES, AND JAMS

The manufacturing of jellies and jams using pectins has been in existence since
the French chemist Braconnat used pectins to make jellies as early as 1820.
However, it was not until the 1900s that large-scale pectin production emerged,
with the first pectin plant being built in Corona, California by the California
Fruit Growers Exchange.

Pectin Production

Pectin has been called "nature's glue." It consists of long and complex chains
primarily in the form of polygalacturonic acid units (a linear galacturonglycan
of a-(1-4 )-linked D-galactopyranosyl-uronic acid) with molecular weights of
100,000 to 200,000 (see Chapter 8). Pectin has a solubility in hot water of about
2 to 3 %, yielding a pH of 2.0 to 3.5. It belongs to a group of related compounds

303
D. Kimball, Citrus Processing
© Van Nostrand Reinhold, New York, NY 1991
304 CITRUS JUICE BY-PRODUCTS

such as protopectin, the water-soluble parent or precursor that becomes pectin


upon hydrolysis. Also, related to pectin are pectinic acid, with a higher degree
of methoxylation, and pectric acid, with fewer or no methoxy groups. Pectins
are classified as high ester (7-8% methoxy groups) or low ester (3-5% meth-
oxy groups). Citrus pectins are used as thickening agents in a large variety of
food, pharmaceutical, and cosmetic products, but 75 % of the pectin produced
is used in the manufacture of jams, jellies, marmalades, and similar products.
Pectin blends better than other texturizers such as gums, starches, and carbo-
hydrate derivatives, and exceeds gelatin in firmness up to temperatures of 120°F
(49°C). Most pectin is produced in the United States, Europe, and Israel.
Most of the pectin in citrus pulp is generally found in juice sac material, with
large amounts occurring in the albedo of the peel. Lemon peel is the most
common source of commercial pectin. Several methods for pectin extraction
have been used, including the procedure discussed in the following paragraphs.
Peel used for pectin extraction usually must undergo extraction of peel oils
prior to or during juice extraction. The peel then is shredded in order to enhance
pectin extraction efficiency, and the shredded peel is washed with water to re-
move sugars, glycosides, and other water-soluble material. Some pectin may
be lost in this washing, but that amount is usually insignificant and oflow grade.
If the peel is not to be processed right away, it should be heated at 95 to 98°C
(203-208°F) for 10 minutes in order to deactivate the pectinase enzymes that
cleave the cx( 1-4) linkage and degrade the pectin. The peel then is extracted
with hot dilute acid (hydrochloric or sulfuric acid at a pH of about 2.0 at 40-
lOO°C (104-212°F) for 45-60 minutes). Lower pH values and hotter temper-
atures shorten the time needed for extraction. Multiple extractions under milder
conditions produce higher-grade pectin. Care should be taken in monitoring and
removing heavy metals, which are common impurities in technical grade acids.
This acid extraction aids in the conversion of protopectins in the peel to the
water-soluble pectins. The acidic solution is filtered from the peel by using
shredded paper, diatomaceous earth, or the equivalent, with the aid of filter
presses or similar equipment. The filtrate contains about 1 % pectin and should
be concentrated to about 3 to 4% pectin. Isopropyl alcohol, ethanol, methanol,
or isobutanol then is added to the solution, to 50 to 70% by weight, resulting
in a precipitation of the pectin in a gelatinous mass. A hydraulic press usually
is used to separate the pectin from the solution. Several 50 to 70% alcohol-in-
water solutions are used to wash the pectin, followed by a final 80 to 90%
alcohol aqueous washing. These washings remove about 50% of the alcohol
and water. Final drying involves the use of warm air, which results in a mois-
ture content of about 6 to 10%. The solid pectin then is pulverized and packaged
as a yellowish white powder. Rapid-set pectin can be made by rinsing the pectin
with an acid solution prior to drying, whereas a slow-set pectin requires stand-
ing in an acidified alcoholic bath for 10 to 20 hours. Common yields of pectin
FOOD-GRADE NONJUICE PRODUCTS 305

Table 20-1_ Food Chemicals Codex specifications


for commercial pectins (Food Chemicals Codex
1931 ).
Acid-insoluble ash sl%
Arsenic (as As) s3%
Total ash slO%
Degree of esterification of high-ester pectin ~50%
Degree of esterification of low-ester pectin s50%
Degree of amide substitution of low-ester pectin s40%
Heavy metals (as Pb) sO.004%
Lead s 10 ppm
Loss on drying s12%
Sodium methyl sulfate sO.1 %
Total anhydrogalactouronides ~70%

are in the neighborhood of 3 % of the peel weight. The high cost of the solvents
used in pectin extraction justify the recovery and reuse of the wash solutions.
The Food Chemicals Codex (FCC) has established specifications for com-
mercial pectin along with procedures for measuring the required parameters
(Food Chemicals Codex 1931), and these specifications are illustrated in Table
20-1. As mentioned earlier, one of the quality problems of using technical grades
of acids in processing is the presence of heavy metal contaminants. The FCC
specifications for acid-insoluble ash, total ash, heavy metals, and lead are de-
signed to account for these contaminants and keep them at safe levels. Arsenic
contamination also must be accounted for in processing acids. The solvent con-
tent and the degree of esterification are parameters of the pectin itself, and the
sodium methyl sulfate specification provides for measuring the degree of de-
methoxylation that has occurred in the pectin as a result of pectinase enzymes
or acid hydrolysis. The FCC procedures for the determination of arsenic, lead,
and sodium methyl sulfate are not given here because they involve the use of
highly toxic chemicals or complex procedures not suited to routine quality con-
trol use by laboratory technicians. It is recommended that atomic absorption or
ion chromatography be used instead of FCC procedures. Sending spot samples
to professional laboratories also is a viable alternative if adequate in-house fa-
cilities do not exist. The following procedures are given by the FCC (Food
Chemicals Codex 1931).

Total Ash

Equipment and Supplies

• Crucible .
• Crucible tongs.
306 CITRUS JUICE BY-PRODUCTS

• Heat source (550°C or 1022°F).


• Desiccating chamber.
• Balance.
• Ethanol (15 ml).
• Glass stirring rod.

Procedure

1. Weigh 3 g of pectin in a tared crucible.


2. Ignite the heater, and heat the sample at around 550°C (1022°F), not to
exceed a dull redness, until evidence of carbon (lumps) has been removed
by combustion.
3. If carbonaceous material still remains, wet the charred mass with hot
water, filter it with ashless filter paper, and ignite the paper and charred
mass. Add the filtrate to the ash, evaporate it to dryness, and heat to dull
redness.
4. If carbonaceous material still persists, cool the crucible and add 15 mlof
ethanol, break up the lumps with a glass stirring rod, and then bum off
the alcohol. Heat to dull redness.
5. Cool the crucible in a dessicator, and weigh it.
6. The % total ash is found by using:

Wash ( 100%)
Ash = ----"""--'-----'-- (20-1)
t Wsample

For example:

(0.301 gash) (100%)


10.1 % ash
(2.977 g sample)

Acid-Soluble Ash

Equipment and Supplies

• Same as with the previous ash test.


• Boiling flask and heat source.
• Dilute HCI (25 ml).
• Gooch crucible or ashless filter paper.
• Hot water.
• Ignitor.
FOOD-GRADE NONJUICE PRODUCTS 307

Procedure

1. Add the ash remaining from the total ash detennination to a boiling flask,
and add 25 ml of dilute HCl. Boil the mixture for 5 minutes.
2. Collect the insoluble material on a tared ashless filter paper or in a Gooch
crucible, and wash it with hot water.
3. Ignite the solid material, and after complete combustion cool it in a des-
iccator.
4. Weigh the remaining ash, and calculate the acid-soluble ash in the same
way as done with the total ash in the previous procedure.

Degree of Esterification

Equipment and Supplies

• 250 ml beaker.
• Magnetic stirrer.
• 250 ml Erlenmeyer flask.
• 100 ml graduated cylinder.
• 500 ml distillation flask with a Kjeldahl trap and a water-cooled condenser.
• Acid titration setup shown in Fig. 3-8.
• Balance.
• Drying oven (105°C or 221 OF).
• 30 to 60 ml fritted disc filter funnel of coarse porosity and vacuum source.
• About 50: 50 HCl, ethanol washing solution.
• 60% isopropyl alcohol (lPA) solution in water (about 100 ml).
• Anhydrous isopropyl alcohol (20 ml).
• Ethanol (2 ml).
• Phenolphthalein indicator solution (l % in IPA).
• Methyl red indicator solution (1 % in IPA).
• O.IN NaOH solution.
• 0.5N NaOH solution.
• 2.5N NaOH solution.
• O.IN HCl solution.
• 0.5N HCl solution.
• Concentrated HCl.

Procedure

1. Weigh 5 g of the pectin sample into a 250 ml beaker, add 5 ml of con-


centrated HCl and 100 ml of 60% IPA, and stir the sample for 10 min-
utes.
308 CITRUS JUICE BY-PRODUCTS

2. Vacuum-filter the solution through a fritted disc filter funnel, washing


with six 15 ml portions of HCl: ethanol solution, followed by a rinse of
60 % IP A solution until no further dissolution is observed (or the chloride
is removed). Wash with 20 ml of anhydrous IPA, dry the pectin in an
oven (105°C or 221 OF) for 2.5 hours, cool it, and weigh it.
3. Transfer 500.0 mg of the dried filtrate to a 250 ml Erlenmeyer flask, and
add 2 ml of ethanol followed by 100 ml of boiled (C0 2 -free) water.
Stopper the flask, and swirl it until the pectin is evenly dispersed or
hydration is complete.
4. Add 5 drops of phenolphthalein indicator solution, titrate with O.IN
NaOH, and record the volume titrated as VI or the initial titer.
S. Add 20.0 ml of O.SN NaOH to the flask, stopper it, shake it vigorously,
and allow it to stand for 15 minutes.
6. Add 20.0 ml of O.SN HCI and shake the flask until the pink color dis-
appears. Add 3 drops of phenolphthalein indicator, and titrate with O.IN
NaOH to a faint pink color that persists on vigorous shaking. Record the
titrated volume as V2 • If the pectin is thought to contain amide groups,
continue with steps 7, 8, and 9. Otherwise, skip to step 10.
7. Transfer the flask contents to a boiling flask fitted to a Kjedahl trap, filled
with 150 ml of boiled (COz-free) water and 20.0 ml of O.IN HCl, and
a condenser. Add 20 ml of 2.SN NaOH solution to the boiling flask, and
heat it carefully to avoid foaming until 80 to 120 ml of distillate has been
collected.
8. Add a few drops of the methyl red indicator to the receiving flask, and
titrate with O.IN NaOH solution. Record the volume titrated as S.
9. Repeat the titration using the same indicator in 20.0 ml of O.IN HCI as
a blank, and record the volume titrated as B. The amide titer (B - S)
should be recorded as V3 •
10. Add VI + V2 + V3 (V3 = 0 if no amide groups are determined) to get
Vr • The degree of esterification can be calculated by using:

V2 ( 100%)
EO = ~-'-----'- (20-2 )
Vr

11. The degree of amide substitution can be calculated by using:

(20-3 )

12. The % by weight of the anhydrogalacturonides can be calculated by


using:

TAGO = 3.S2VI + 3.80V2 + 3.SV3 (20-4 )


FOOD-GRADE NONJUICE PRODUCTS 309

Heavy Metals

Equipment and Supplies

• Two 50 ml color comparison tubes.


• 50 ml graduated cylinder.
• 10 ml graduated cylinder.
• Filter funnel and vacuum source and trap.
• Crucible.
• Crucible tongs.
• Ignitor.
• Lead acetate standard solution. (Make a stock solution of lead nitrate
[159.8 mg ACS Pb (N0 3 h in 100 ml water and 1 ml nitric acid diluted to
1000.0 ml in lead-free glass containers with water], and dilute 10 ml of
the stock solution on the day of use to 100 ml with water.)
• Dilute acetic acid.
• Dilute ammonium hydroxide solution (dilution of 400 ml of ACS reagent
grade ammonium hydroxide with water to 1000 mI.)
• H2 S solution. (Pass H 2 S into cold water to saturate the solution, and store
it in small, dark, amber bottles with little head space in a cold dark place.
The solution is good only if it has a strong odor and forms a sulfur precip-
itate when added to an equal volume of ferric chloride (9 g ferric chloride
hexahydrate /100 ml water).)
• Concentrated H 2 S04 •
• Concentrated HN0 3 .
• HCl solution (one-half concentrated HCI and one-half water).
• Freshly prepared hydrogen sulfide.
• Steam bath.
• Litmus paper or equivalent.
• Short-range pH paper (3.0-4.0 pH) .
• Muffle furnace (500-600°C or 932-11 I2°F) (preferred).

Procedure

1. Prepare a lead solution by adding 2.0 ml of the lead acetate standard


solution to a 50 ml color comparison tube along with enough water to
make 25 m!. Adjust the pH with dilute acetic acid or dilute ammonium
hydroxide to a pH of 3.0 to 4.0, using short-range pH paper. Dilute the
solution with water to 40 m!. This is solution A.
2. Place 500 mg of pectin in a crucible with the lid loosely on it, add enough
sulfuric acid to wet the sample, and heat it at a low temperature (about
550°C or 1022°F) until the pectin is thoroughly charred or carbonized.
310 CITRUS JUICE BY-PRODUCTS

3. Add 2 ml of nitric acid and 5 drops of sulfuric acid, and heat the crucible
until dense white sulfuric acid fumes evolve.
4. Ignite the sample, preferably in a muffle furnace (500-600 o e or 932-
1112°F), until complete combustion ofthe organic material occurs, and
cool it.
5. Add 4 ml of dilute hydrochloric acid, cover the sample, and heat it on a
steam bath for 10 to 15 minutes.
6. Uncover the sample, and evaporate it to dryness on the steam bath.
7. Moisten the residue with 1 drop of hydrochloric acid, add 10 ml of hot
water, and heat it for 2 minutes.
8. Add ammonium hydroxide dropwise until the sample is just alkaline to
litmus, dilute it to 25 ml with water, and adjust the pH to 3.0 to 4.0,
using short-range pH paper and dilute acetic acid.
9. Filter the sample if a solid or suspended material exists, rinse the cru-
cible and filter with 10 ml of water, and transfer the washings to a 50
ml color comparison tube, diluting the solution to 40 m!. Mix the solu-
tion to a uniform consistency. This is solution B.
10. Add 10 ml of freshly prepared hydrogen sulfide to each tube (solutions
A and B), and allow the tubes to stand for 5 minutes.
11. View the sample tube (B) and the lead standard tube (A), looking down-
ward from the top over a white surface. If the sample solution is darker
than the lead standard, then the pectin exceeds the 10 ppm lead or heavy
metal specification, and vice versa.

Solvent Content

Equipment and Supplies

• Glass-stoppered weighing bottle.


• Balance.
• Drying chamber or oven (105°e or 221°F).
• Desiccator.

Procedure

1. Heat the empty dry weighing bottle and stopper in a drying chamber for
30 minutes, and weigh the bottle and stopper.
2. Place 1 to 2 g of pectin, accurately weighed, in the weighing bottle, and
evenly distribute the pectin to a depth of about 10 mm.
3. Place the opened bottle and stopper in the same drying chamber ( 105°e
or 221°F) for 2 hours.
4. After drying, stopper the bottle immediately, cool it in a desiccator, and
weigh it.
FOOD-GRADE NONJUICE PRODUCTS 311

5. The % solvent can be calculated from:

wt after drying )
% solvent = ( 1 - wt b" d.
elore rymg
100% (20-5)

For example:

( 1 - 1.102 g) 100% = 10.0% solvent


1.224 g

The most common quality control parameter of pectins, however, is the jelly
grade or the pounds of sugar that one pound of pectin will support. The maxi-
mum jelly grade of pectin from lemon peel is about 300 to 350; from grapefruit
peel, 250 to 300; and from orange peel about 150 to 250. Most pectins used
for the commercial production of jams and jellies have a jelly grade of about
150. The Institute of Food Technologists has established a standard procedure
to measure the jelly grade, which has been officially accepted by the industry
(1FT Committee on Pectin Standardization 1959).

Jelly Grade of Pectin

Equipment and Supplies

• Exchange Ridgelimeter with square plate glass accessories and Hazel-Atlas


No. 35 glass tumblers ground down to a height of 3.125 inches with lids
and spatula.
• Glass stirring rod.
• 3/4" masking tape.
• Sugar (three times as many grams as the estimated jelly grade).
• Tartaric acid solution (48-80 g in distilled water to 100 ml).
• 3 qt stainless steel saucepan (e.g., Ekcoware pan No. 7323, Flintware pan
No. 7623, or Revere copper-clad pan No. 1403).
• Potato masher (e.g., Flint No. 1905).
• Heat source to boil mixture.
• Refractometer.
• Thermometer.
• 25 ± 3.0°C storage area.
• 2 ml pipette.
• 150 ml beaker and balance.

Procedure

1. Determine the grams of pectin needed by dividing 650 by the assumed


jelly grade. Subtract this number from 650 to get the grams of sugar
312 CITRUS JUICE BY-PRODUCTS

needed. For example, for an estimated jelly grade of 150, 650/150


equals 4.33 g of pectin, and 650 - 4.33 or 646 g of sugar would be
needed.
2. Add about 20 to 30 g of the needed sugar to a clean and dry 150 ml
beaker, and add the pectin. Mix the two solid materials with a stirring
rod.
3. Tare the saucepan and potato masher, and then add 410 ml of distilled
water. Pour the contents of the beaker into the pan all at once, and gently
stir the mixture for 2 minutes. Try to get the solid material under the
surface of the water as quickly as possible. Place the pan on the heat
source, and heat it until the solution is fully boiling, while stirring the
solution the entire time.
4. Add the remaining needed sugar and stir until all of the solid material
has dissolved. Boiling should continue until the net weight of the jelly
batch is 1015.0 g. Ifthe net weight is less than this, add excess distilled
water, and reboil down to the proper weight. The entire heating time
should be about 5 to 8 minutes.
5. After the final weighing, let the solution sit undisturbed on a flat surface
for about one minute.
6. Tip the pan, skim off the floating material, and place a thermometer in
the solution. When the temperature reaches 95°C, pour the solution
quickly into three previously prepared Ridgelimeter glasses. These tum-
blers are prepared by extending the height of the glasses, which is done
by encircling the rim of the glass with masking tape extending exactly
one-half inch above the rim. Also, pipette 2.0 ml of the tartaric acid
solution into each tumbler. (See Fig. 20-1.) Stir each solution gently
with the glass stirring rod to remove bubbles. Exactly 15 minutes after
pouring, cover the jars with lids that fit snugly on the masking tape rim,
and store them at 25 ± 3.0°C for 20 to 24 hours.
7. Remove the lids and the masking tape around the rim of the tumblers.
A clean and wetted wire furnished with the Ridgelimeter is used to sep-
arate the excess jelly above the rim of the tumbler by drawing it across
the surface. Turning the tumbler during this separation ensures an even
and uniform jelly surface.
8. The remaining jelly is removed from the tumbler onto a square glass
plate by inverting the tumbler at about a 45° angle, as shown in Fig.
20-1, and carefully separating the jelly from the top of the rim of the
tumbler with a spatula. Thereafter the jelly should slide out of the tum-
bler onto the glass plate on its own. One should be careful not to drop
the jelly onto the glass plate or rupture the jelly. A timer is started as
soon as the jelly in on the glass plate. If the jelly leans, the plate should
be tilted away from the lean to position the jelly upright. Place the glass
plate in the Ridgelimeter as shown in Fig. 20-1.
FOOD-GRADE NONJUICE PRODUCTS 313

~With masking tape rim

..
Hazel-Atlas No. 35
glass tumblers removal of jelly
from tumbler

micrometer
R..Ii.---'----
Ridgelimeter

lass plate

Fig. 20-1. Equipment used to measure the jelly grade of pectins.

9. Using the micrometer, lower the screw to just above the surface of the
jelly. After 2 minutes adjust the screw to just contact the top of the jelly
with the micrometer tip. The lowest line on the vertical scale is the per-
cent sag, with the micrometer reading giving tenths of a percent sag.
Repeat this step for each of the two remaining triplicate samples. If the
percent sag differs by more than 0.6 %, the jelly should be remade and
the test repeated.
10. Remove a portion of the jelly from the center, place it on the prism of a
refractometer, and read the Brix after about a minute. The temperature-
corrected Brix (see Chapter 2) must be 65.0 ± 1.0oBrix. A 1.0oBrix
error can mean an error of 3 to 4 jelly grade points.
11. The jelly grade is found by calculating a correction factor to the assumed
or estimated jelly grade. The factor (Fj) is found from:

Fj = 2 - (% sag)/23.5 (20-6 )

12. This factor is used to get the true jelly grade as follows:

JG = Fj ( estimated jelly grade) (20-7 )


314 CITRUS JUICE BY-PRODUCTS

For example:

Fj = 2 - (24.1)/23.5 = 0.97

JG = (0.97)( 150) = 146 jelly grade

Production of Jams. Jellies. and Preserves

Gelation has long been used as a means of preserving various fruits; the resul-
tant increased viscosity or decrease in water activity inhibits microbial growth
and spoilage. Jams and jellies usually can be stored at room temperature until
they are opened. Thereafter, the surface becomes subject to airborne molds,
which literally grow on the surface of almost any food product, especially one
as rich in carbohydrates and nutrients as fruit jams and jellies are.
Jellies can be defined as a clear jelled fruit product that retains its shape when
cut by a knife. The federal standards of identity describe jellies as a mixture of
fruit ingredients containing not less than 45 parts of fruit juice by weight to each
55 parts of saccharine ingredient (CFR Title 21 150.140). (The word "sac-
charine" is defined as a sweetening material.) For example, if you used 2.5
pounds of 65.0 o Brix orange concentrate, the amount of saccharine ingredient
that you could use while still calling the product fruit jelly would be:

65.0 0 BriX) (55 parts sach.)


(2.5'bconcJ ( 00% (8.0factor) 5 .. = 16 lb sach.
1 0 4 parts JUIce
If saccharine ingredients were used, another 16 pounds of sugar would be re-
quired to make the jelly. The 8.0 factor is from the federal code for orange
juice. The factor for grapefruit juice would be 11.0. There is also a federal
standard of identity for artificially sweetened fruit jelly, which requires at least
55 % of the final weight of the jelly to be fruit juices. For this artificially
sweetened product, the allowable ingredients are more restricted, especially the
sweeteners used. Only saccharine ingredients that are not sugar can be used.
Jams or preserves contain unclarified juice, usually containing thicker or larger
portions of the solid material of the fruit than found in jellies. The federal code
defines fruit jams or preserves as containing 47 parts of fruit ingredients by
weight to 55 parts of saccharine ingredient for citrus products (CFR Title 21
150.160). Artificially sweetened fruit preserves and jams have standards of
identity that are similar to those of jellies except that the term "fruit" is used
instead of "fruit juice."
The process of gelation of jams and jellies depends on the hydrogen bonding
balance or water activity in the solution. It is believed that the negatively
charged, highly hydrated pectin chains are bound together by hydrogen bonds.
Sugar molecules compete for the hydrogen bonding with water molecules, while
FOOD-GRADE NONJUICE PRODUCTS 315

acids are used to control the negatively charged pectin chains. By combining
the right proportions of pectin, sugar, water, and acid, gelation will occur, even
at temperatures as high as the boiling point of water (Joseph 1955). Also, the
mineral content will affect the balance and thus the gelation. Divalent cations
may act as linking agents between pectin chains, resulting in gelation. In fact,
low-methoxy pectins require polyvalent cations in order to gel. For the reason,
the mineral content of the water used in processing should be considered. Also,
the natural pectins, sugars, acids, buffering salts, and other soluble material
inherent in the juices or fruit used should be taken into consideration.
Slow-set pectins require the pH to be less than 3.30, whereas rapid-set pectins
require a pH ofless than 3.55. The slow-set pectins, however, are more tolerant
of excess acid levels than the rapid-set pectins. Jellies generally utilize slow-
set pectins so that gelation does not occur until the product is in the container.
Also, jellies generally use more pectin than jams to obtain a firmer gel. For
jams it is better to use a rapid-set pectin in order to avoid floating pieces of fruit
that separate if gelation is too slow. Most jellies and jams are made from a
standard 150 jelly grade pectin.
The general process of making jams or jellies involves premixing the pectin
with about three to five times as much sugar as pectin to help disperse the
pectin, and then dissolving this mixture in the fruit juice or pulp. When this
mixture is dissolved in fruit juice concentrates, the amount of sugar to be pre-
mixed with the pectin should not exceed about 20 to 25 % of the total solution.
This mixture is cooked or evaporated until it reaches an acid- and temperature-
corrected Brix of 65 to 68. The acid is added just before filling in order to
postpone the gelation as long as possible. Two examples of fruit jellies and
jams are presented in Tables 20-2 and 20-3.
The USDA divides the grade standards for fruitjeUy into two areas. Standard
fruit jelly meets the FDA standards of identity (CFR Title 21 150.140.), whereas
unstandardized jelly includes fruit ingredients not allowed in the same standards

Table 20-2. Orange jelly formulation (Swisher and Swisher 1977).


Slow-set pectin ( 150 jelly grade) 11.0 Ib
65.0 o Brix concentrated orange juice 2.5 gal
Water 7.0 gal
Sugar 100.llb
Acid solution (7.9 Ib citric acid monohydrate in 1.0 gal of water) 591 ml
Orange oil 44 ml

Procedure
I. Mix pectin with 5 pounds of sugar, and add the mixture to warm water with stirring and bring
to a boil. Boil for 30 seconds.
2. Add the rest of the sugar, dissolve it, and add orange concentrate without further heating.
3. Add acid solution and orange oil and fill the container. Makes about 165 pounds of jelly.
316 CITRUS JUICE BY-PRODUCTS

Table 20-3. Orange marmalade formulation (Swisher and Swisher


1977).
Rapid-set pectin ( 150 jelly grade) 0.51b
65.0 o Brix concentrated orange juice 0.51b
Commercially prepared orange peel strips 20.91b
Water 30.0 gal
Sugar 100.1 Ib
Acid solution (7.9 Ib citric acid monohydrate in 1.0 gal of water) 414 ml
Orange oil 30 ml

Procedure
1. Mix pectin with about 5 pounds of sugar, and add the mixture to warm water with stirring
and bring to a boil. Boil for 30 seconds.
2. Add the rest of the sugar and peel strips, boil to dissolve, and then turn off the heat source.
3. Add the concentrated orange juice, oil, and acid solution. Yields about 152 pounds of mar-
malade.

of identity. Also, an unstandardized jelly can contain as much as 27 parts of


black currant juice to 55 parts of sugar, whereas standardized jelly cannot con-
tain any black currant juice.
The USDA further classifies jellies into four types: Type I jellies are stan-
dardized jellies containing fruit juice from a single variety of fruit, Type II
jellies are standardized jellies that contain juices from more than one fruit va-
riety, Type III jellies are unstandardized jellies containing juices from one va-
riety of fruit, and Type IV jellies are unstandardized jellies that are made from
more than one fruit variety.
The USDA scoring system is shown in Table 20-4. Grade A texture is de-
scribed as tender to slightly firm and retains a compact shape without excessive
weeping. Grade B may lack firmness but cannot be syrupy; it also can be more
than slightly firm but not tough or rubbery. Grade A color is described as in-
cluding a sparkling luster and is no more than slightly cloudy. Grade B color
may range from slightly cloudy to slight dullness. Grade A flavor must be free

Table 20-4. USDA scoring system for grades of


fruit jelly.
Minimum
Consistency Color Flavor Score
Maximum points 40 20 40
Grade A 36-40 18-20 36-40 90
Grade B* 32-35 16-17 32-35 80
Substandard* 0-31 0-15 0-31
'If the fruit jelly falls into this category in anyone area, it cannot receive a higher
grade regardless of the total score.
FOOD-GRADE NONJUICE PRODUCTS 317

from any caramelized or other objectionable flavor, whereas Grade B may have
only a slight caramel-like flavor.

FRUIT SECTIONS

The canning and the bottling of fruit sections have become a popular means of
preserving citrus fruit. Grapefruit sections have found acceptance in the United
States, and mandarin sections are well accepted in the Far East. Canned and
bottled citrus fruit sections have the advantage of long shelf lives and retention
of most of the whole-fruit nutrition, and can be conveyed to noncitrus or off-
season geographical areas that otherwise might not be able to partake of the
benefits of citrus.

Fruit Preparation

Prior to processing, citrus fruit should be held in storage bins for 4 to 6 days to
allow it to soften. A prescaling of the fruit may shorten this holding time to 2
to 3 days. The fruit then is scalded in hot water (90-100°C or 196-2100F) for
5 to 8 minutes for grapefruit or 4 minutes for oranges, which further softens the
fruit. Then the fruit is sprayed with low pressure steam that penetrates the peel,
which is followed by additional bin storage until the fruit is ready for peeling.
The softened fruit requires gentle handling, but the additional holding time can
reduce scalding requirements by 30 %. It also results in less fruit spoilage and
less cooked off flavors.

Peeling

About 5 % of sectionized fruit is peeled by hand, and the rest by mechanical


means. Hand peeling generates greater amounts of juice in waste streams than
mechanical peeling, which may be diverted to juice processing. Hand peeling
also generally requires less scalding and thus gives better quality. The mechan-
ically or hand-peeled fruit then undergoes a hot caustic spray (0.5-2.5 % NaOH
or Na2C03) at 88 to lOO°C (190-212 OF) for 12 to 25 seconds. (These lye
solutions can be recycled, but must be replenished daily because of the leaching
of fruit-soluble solids.) The fruit then is allowed about a 15- to 25-minute re-
action time, followed by water sprays to remove the basic solutions. The peeled
fruit is chilled in water baths or sprays at 2 to 5°C (35-40°F), a step that
facilitates sectionizing of the fruit.

Sectionizing

Manual sectionizing is done by placing the fruit against a spindle, and the sep-
arated sections are tapped or brushed against each other to remove the seeds.
318 CITRUS JUICE BY-PRODUCTS

Mechanical sectionizing may be done in various ways. Pruit generally is placed


in a cup with the blossom end up, and aligned automatically or by hand using
a light beam guide. The sectionizing blades break apart the segments, and shak-
ers are used to remove the seeds. The separated sections usually are graded by
hand prior to filling.

Filling

After the sections are placed in the container, a liquid sweetener is added, which
can be a mixture of water, juices, and sugar at vaious concentrations. Allowable
filling solutions include water, grapefruit juice and water, grapefruit juice,
slightly sweetened sirup or slightly sweetened water (12.0-15.9°Brix), light
sirup (16.0-17.9°Brix), heavy sirup (~18.0oBrix), slightly sweetened
grapefruit juice and water (12.0-15.9°Brix), lightly sweetened grapefruit juice
and water (16.0-17.9°Brix), heavily sweetened grapefruit juice and water
(~18.0oBrix), slightly sweetened grapefruit juice (12.0-15.9°Brix), lightly
sweetened grapefruit juice (16.0-17.9°Brix), and heavily sweetened grapefruit
juice ( ~ 18.0 oBrix). Usually sections from grapefruit that pack 70 to 80 to a
box in fresh fruit packaging are packed in 8-ounce and 303 cans, and larger
grapefruit that pack 54 or 64 to a box are packaged in 26-ounce glass containers.
There are two basic methods of filling citrus sections into containers. One is
cold fill, where the container is chilled after sealing in a 35 to 40 0 P (2-4°C)
water bath. The container then is dried by an air stream, and dry ice sometimes
is sprinkled on it to maintain its temperature on the way to cold storage at 36
± 2°P. About 0.04 to 0.05% sodium benzoate sometimes is added as a pre-
servative, along with less than 0.035 % calcium chloride or calcium lactate to
enhance the firmness of the sections.
Hot-fill packaging includes heating the sealed container to 149 to 190 0 P (63-
88°C) for 20 to 45 minutes, depending on its size. Larger containers require
more heat for a longer time. The heat-treated container then is passed through
a 60 to 75°P (16-24 °C) water bath, which cools the contents to about 90 to
lOOoP (32-38°C). The residual heat dries the can.

Analytical Procedures

The Brix and acid levels of the sirup used in canning or bottling citrus fruit
sections are measured as explained in Chapters 2 and 3. The integrity of the
fruit sections themselves generally is determined by direct inspection. If the
section maintains its form when suspended above the liquid, it can be consid-
ered firm. The main quality parameter is the drain weight, which is determined
by using the following procedure.
FOOD-GRADE NONJUICE PRODUCTS 319

Drain Weight

Equipment and Supplies

• No.8 circular sieve (8" diameter).


• Collection pan at least as large as the sieve.
• Scale or balance.

Procedure

1. Pour the contents of the container through the sieve, collecting the liquid
in the pan or tray under the sieve.
2. Drain for 2 minutes, and tap the sieve to remove adhering liquid.
3. Weigh the liquid and the screened fruit sections separately.
4. Calculate the percent drain weight by using:

% drain wt = (Wfruit ) ( 100 % ) / (Wfruit + ~iqUid) (20-8)

For example:

(125 gfruit)( 100 % ) / (125 gfruit + 102 gliquid) = 55 % drain wt

Standards of Identity (CFR Title 21 145.145)

The federal standards of identity require that at least 50 % of the drain weight
be in the form of whole sections in order for the product to be called fruit
sections or segments. If less than 50% of the drain weight is whole sections,
the product must be called broken sections or broken segments. Also, they must
have less than 20 square centimeters (3.1 square inches) of tough membrane
or albedo on the segments per 500 grams ( 17.6 ounces) of the product. Also,
there can be no more than four developed seeds (9.0 mm or 0.35 inch or larger),
and no more than 15 % of the drain weight can contain injured, discolored, or
otherwise blemished fruit.

USDA Grade Standards (CFR Title 21 52.1141-52.1151)

Grade A canned grapefruit sections must have at least 53 % of the water capacity
of the container in the form of fruit, with at least 65 % of the fruit being in the
form of whole sections. Grade B also requires that 53% of the water capacity
of the container be in the form of fruit, with only 50% or more of the fruit being
in the form of whole sections. Substandard canned grapefruit fails the above
requirements. The fill of the container or the composition of the liquid medium
320 CITRUS JUICE BY-PRODUCTS

is not considered in USDA grades. Table 20-5 illustrates the USDA scoring
system for canned grapefruit.

JUICE DRINKS, BASES, AND PUREES

Citrus juice drinks can be defined as beverages that contain less than 100 % fruit
juices. They usually contain varying amounts of sweeteners and organic acids,
and perhaps also carbonation, flavors, colors, emulsifiers, texturizers, or other
components designed to enhance the beverage. A drink base can be defined as
the concentrated components of a drink minus the major portion of water,
sweetener, and perhaps even the acid, although many drink bases already con-
tain the needed acid. In the United Kingdom, drink bases are called squashes;
in Australia they are known as cordials and usually contain about 20 to 50%
juice. The main consumer appeal of juice drinks is their low cost. Drinks and
drink bases can be used for nonbeverage products as well, such as popsic1es
and purees. Purees are a type of fruit juice base used as a flavoring material for
sherbets, candy, baking products, and many other products. Purees once were
made from macerated whole fruit but now are made from juice concentrate in
a manner similar to that used for drink bases. Also included in puree bases are

Table 20-5. USDA grades for canned or bottled grapefruit sections.


Minimum
Wholeness Color Defects** Character Score
Maximum 25 25 25 25
Grade A 21-25 23-25 23-25 23-25 90
Grade B* 17-20 21-22 21-22 21-22 80
Broken* 0-16 21-25 21-25 21-25 70
Substandard* 0-20 0-20 0-20
*Sections falling in this classification in anyone parameter cannot receive a grade higher regardless of total
score.
* *Defects are determined according to the scheme below.
Extraneous Total Large Damaged
Veg. Matter* Seeds * Seeds * Albedo and Membrane* Units
8 oz can336 ml
Grade A 0.25(1) piece 1.6(3) 0.4 (l ) !(l)in. 2 ~ oz.
Grade B 0.50(2) piece 4.8 (6) 1.2(2) ~(1!)in'> ~ oz.
No. 303 can492 ml
Grade A 0.50(1) piece 3.2(4) 0.8(2) 1.0(2.0) in. 2 ! oz.
Grade B 0.75(2) piece 9.6(12) 2.4(3) 2(3) in.2 1! oz.
No.3 Cyl.1455 ml
Grade A 0.75 (l) piece ( 10) (3) 4(5) in. 2 I! oz.
Grade B 1(2) (20) (5) 6(7!) in. 2 4 oz.
*The first number is the maximum allowed average for all samples. The second number in parentheses is the
maximum allowed per sample.
FOOD-GRADE NONJUICE PRODUCTS 321

juice sacs, sugar, color, flavors, citrus oils, essences, and citric acid to adjust
the pH to about 3.0. Sherbet bases generally are manufactured as 50-fold con-
centrates and are required by law to contain at least 2 % juice. Sugar and color
usually are added by the food processor using the puree base. Oil levels of puree
bases usually occur in the range of 0.030 to 0.035 %, as measured by the pro-
cedure outlined in Chapter 6. The pulp level ranges from 6 to 12.5 %, as deter-
mined by procedures mentioned in Chapter 7.
The most popular beverages in the United States are carbonated soft drinks,
and the increased concern in the late 1900s for healthful beverages has made
juice-added soft drinks especially appealing. Also, juice drinks with high levels
of juice have been developed that emphasize added nutrients such as calcium
and low calorie sweeteners. The flavor and the color quality of the juices used
in these drinks playa lesser role in the overall quality of the drink than they do
in citrus juices; so a lower quality can be used in these drink bases, such as
pulp wash juices or bitter juices as well as high-acid juices such as lemon and
lime juices. Components that make up citrus drinks can be broken down into
11 groups: juice, sweeteners, acids, colorants, flavors, texturizers, clouding
agents, nutrients, foaming agents, de foaming agents, and preservatives; but
these components may not all be contained in an individual juice drink or base.

Juices

Juices are used for several reasons, the main one being to enhance the health
appeal of the product. Depending on the amount of juice used, color and flavor
enhancement are the next most important contributions the juices make to the
drink. Cost often determines which juices are used in a drink, with cheaper
juices such as apple, pear, or white grape juices frequently used. Some highly
colored juices, such as pomegranate or cranberry juice, can add a desirable
deepening of the citrus color at around the 1 % level, but greater amounts impart
an unsightly brownish tinge to the product. Lemon and lime juices have been
used as citric acid sources for drinks, enhancing their citrusy flavor at the same
time. Pulp wash juices and peel extracts are ideal juice sources for citrus drinks,
which provide a use for these products that would be difficult to market other-
wise.
With the advent of debittering techniques, the use of bitter juices in drinks is
expected to decline. The most bitter navel juice can contain limonin levels as
high as 40 ppm, well over the 6 to 7 ppm generally accepted taste threshold. A
tenfold dilution in making a 10% juice drink would dilute the limonin level to
4 ppm maximum, below the taste threshold. Care must be taken in using bitter
juices with nonbitter citrus juices because even non bitter citrus juices contain
some limonin. Because pulp wash juice (or the juice produced from washing
the core material recovered from FMC-like juice extractors), and peel extracts
322 CITRUS JUICE BY-PRODUCTS

are highly bitter, they may require debittering before significant quantities can
be used in juice drinks.

Sweeteners

Sugar (sucrose), or its equivalent in high fructose com syrup (HFCS) or low
calorie sweeteners, is a major component in most juice drink formulations.
Commercial sugars generally cost only 5 to 15% as much as the sugars or sol-
uble solids found naturally in citrus juices, a difference that makes juice drinks
a more economical product for consumers. The only known nutritional disad-
vantage of citrus juices is their high calorie content, which can be largely over-
come by using low calorie sweeteners in juice-based drinks. The Federal Reg-
ister allows sugar (sucrose), invert sugar, fructose, com syrup, glucose syrup
sorbitol, or any combination of these ingredients to be used as sweeteners in
carbonated soft drinks (FR June 26, 1969,9867). Because sugar is readily avail-
able and comprises the major portion of most juice drinks, it is not added until
just prior to packaging of the final drink, along with the necessary water. This
procedure saves a considerable amount of money in shipping, storage, and con-
veying.

Acids

Acids are another major component of citrus juices and juice drinks, and give
the beverage a citrusy tangy taste. Because the hydronium ion is what imparts
this taste, theoretically most acids can be used; but not all acids are approved
for food use. Citric acid, which is the most common acid found in fruits and
juices, is considered to be one of the best acids to use in foods. One reason for
this is that it is easily buffered, being a triprotic weak acid. Also, citrus pro-
cessors who have quality control programs based on citric acid (citric acid cor-
rections to the Brix and lemon and lime inventories based on the weight of citric
acid) are better equipped to handle citric acid than other acids. However, the
Federal Register permits the use of acetic acid, adipic acid, fumaric acid, glu-
conic acid, lactic acid, malic acid, phosphoric acid, or tartaric acid in addition
to citric acid in carbonated soft drinks (FR June 26, 1969, 9867). Citric acid
can be buffered by adding tricalcium phosphate, sodium citrate, and citric acid
in the ratio of 1 : 5: 30 by weight. Again, the Federal Register allows acetate,
bicarbonate, carbonate, chloride, citrate, gluconate, lactate, orthophosphate, or
sulfate salts of calcium, magnesium, potassium, or sodium to be used as buff-
ering agents in carbonated soft drinks (FR June 26, 1969, 9867).

Colorants

Colorants play a minor role in regard to the Brix, but they have a significant
influence on the drink's overall appeal and therefore can be formulated inde-
FOOD-GRADE NONJUICE PRODUCTS 323

pendently of the sugar and the acid. Highly pigmented juices from other vari-
eties of fruit offer a natural and nutritional way to produce desirable colors in
fruit juice drinks. As mentioned above, the addition of 1 % of pomegranate or
cranberry juice to citrus juice drinks can deepen the color. Also, tangerine juices
are known for their deep orange color, as is juice produced in dry Mediterranean
climates such as that in California, Australia, and South Africa and around the
Mediterranean basin. Natural pigments can be used such as turmeric and anatto
(see Chapter 19).
Other common natural pigments used in citrus drinks include the carotenoids.
One of the most common carotenoids is iJ-carotene, which is extracted from
citrus peels or other natural sources. iJ-Carotene imparts a light yellow to orange
color to citrus juice drinks. It is not very soluble in water but is more soluble
in fats and oils. Its molecular structure is as follows:

FD&C dyes, described in the Chapter 19, also can be used to enhance the
color of citrus drinks. FD&C No.5 is used in lemon drinks in the range of 10
to 15 ppm, in lime drinks at 20 to 30 ppm, and in grapefruit drinks at 5 to 10
ppm. In orange drinks FD&C No.5 and FD&C No.6 can be used together,
each at about 0.008 to 0.2 %, depending on the amount of juice used in the
drink. Packaging also has an effect on the need for color. Generally, the bright
colors of citrus juices are a good selling point. However, if opaque cans or
containers are used, color enhancement becomes less important.

Flavors

Citrus flavors come in various forms. Natural citrus oils and essences extracted
from the peel of the fruit and recovered during juice evaporation or pasteur-
ization are the most common source of citrus flavors. Citrus oils can be con-
centrated or folded in order to strengthen the citrus flavor by concentrating the
oxygenated compounds in the oils. Again, the addition of these flavors has little
effect on the Brix measurements and can be formulated independently of the
324 CITRUS JUICE BY-PRODUCTS

sugars and acids. The most prevalent component of citrus oils is d-limonene,
which is easily measured by using the Scott method, described in Chapter 6.
Ideal oil ranges are 0.015 to 0.020% by volume. Other compounds that con-
tribute to the citrus-like taste of juice drinks include ethyl butyrate and various
aldehydes, such as decanal, citral, acetaldehyde, and octanal.

Texturizers

Texture or mouth-feel is important in attempts to duplicate the sensation of


authentic citrus juices. Natural juices contain pectins and proteins that act as
natural emulsifiers. Pulp and other solid material also contribute to the general
viscosity and mouth-feel of the juice. Juice sac material can be added to citrus
drinks to give a fresh squeezed juice appearance and mouth-feel. Some textur-
izing agents used in the industry include glycerol, ester of wood rosin, guar
gum, hydroxylated lecithin, lecithin, methyl cellulose, mono- and diglycerides
of fat-forming fatty acids, polyglycerol esters of fatty acids, propylene glycol
alginate, sodium alginate, sodium metaphosphate (sodium hexametaphos-
phate), gum acacia, gum arabic, xanthan gum, vegetable gums and brominated
oils, gum tragacanth, carbo bean gum (locust bean gum), carrageenan, ester
gum, sodium carboxymethy1cellulose, cottonseed oil, or even pectin in a range
of around 0.1 to 0.3 %. The texturizer of choice depends on the desired texture,
price, and availability. Even though texturizers appear to have a significant
effect on the density of the juice, their contribution to the Brix measurement is
generally insignificant.

Clouding Agents

Clouding agents give citrus drinks the opaque appearance of juice. This is es-
pecially important in lemonades and limeades, where the natural cloud levels
in the juices must be extensively diluted in order to bring the acid levels in the
juice down to the desired levels. About 30 % of the natural cloud in juice is
made up of proteins, which come primarily from the cytoplasm and organelles
of the juice cells during extraction. About 10 to 15 % of the cloud is made up
of hemic ell uloses from the membrane material of the fruit, and about 5 % of the
juice cloud is composed of pectin (Bennett 1985). Natural flavonoids, such as
hesperidin and naringin, also contribute to the cloud material. Protein/pectin
combinations have been shown to produce cloud similar to that found in citrus
juices. Casein, a common protein, has been found to produce cloud with highly
methoxylated pectin in a ratio of about 500 to 1000 /kg/mg pectin (Bennett
1988). Soy flour or other suitable protein sources can be used with pectins as a
starting point in most drink cloud formulations.
FOOD-GRADE NONJUICE PRODUCTS 325

Nutrients

As explained in Chapter 11, natural juices contain a healthy supply of certain


nutrients, especially vitamin C. Because vitamin C is associated with citrus
juices, consumers usually expect to find levels of the vitamin equal to that found
naturally in juices in citrus drinks. The average content of vitamin C in pure
juices is about 0.05 % or 50 mg/ 100 ml. To calculate the amount of vitamin C
that must be added to these drinks to equal the levels found in pure juices, the
following equation can be used:

wt vitamin C = 0.0005 (1 - p /100) W (20-9 )

where p is the percent of juice soluble solids in the final drink compared to the
total soluble solids in the drink, and W is the total weight of the drink. The
weight of the drink can be found from the gallons by multiplying by the density
found from the Brix, using Equation 2-9 or 2-11. For example, if we had 1000
gallons of an 11.8 °Brix juice drink that contained 10 % orange juice soluble
solids, the weight of drink after converting the 1000 gallons of drink to pounds
would be 8717 pounds drink (d = 8.717 lb/gal). Equation 20-9 then would
give:

0.0005(1 - 1O%/100)8717lb = 3.9 lbofvitamin C

Calcium addition to juice drinks containing high levels of citrus juices has
recently become a popular way to increase the nutritional value of citrus prod-
ucts. The USRDA for calcium is 1 gram. Assuming a serving size of 6 ounces
( 177 ml), a maximum of 24 grams per gallon of drink or 53 pounds per 1000
gallons of drink should constitute the maximum level of calcium needed to
enhance the drink's nutrition. Because most people consume other foods that
are high in calcium (such as milk), an amount that is less than this maximum
level should be adequate. It must be remembered, as explained in Chapter 11,
that whenever nutrients are added, nutritional labeling is mandated by law.

Preservatives

Unlike nutrients, the presence of preservatives has a negative connotation in


foods. Concentrated drink bases naturally inhibit microbial growth by osmotic
pressures and cold temperatures. Single-strength drinks often are packaged in
aseptic bottles, cans, or paperboard or fiberboard containers using hot-fill tech-
nologies and/or hydrogen peroxide sterilization. In order to minimize the risk
of contamination and the heat required for sterilization, preservatives are often
added. Sulfites act not only as preservatives but as antioxidants that help inhibit
326 CITRUS JUICE BY-PRODUCTS

Maillard oxidative reactions, which can cause off flavors and colors to develop.
Ascorbic acid or vitamin C is sometimes used as an antioxidant as well. How-
ever, the use of sulfites is becoming more restricted, and they have been banned
in many areas offood processing. Some ofthe most common preservatives used
in citrus juices and beverages are benzoates and sorbates. These preservatives
are more effective against bacteria in single-strength juices and are less effective
against the slower-growing yeasts, with the effectiveness of sodium benzoate
against yeast depending on the pH of the juice. For pH values of 2.5 to 3.5, a
sodium benzoate level of 0.05 % is effective against yeasts; at pH values of up
to 4.5, 0.10% sodium benzoate is required. Common sodium benzoate levels
of 0.15 % are found in many juice drinks, as well as levels of 0.05 % potassium
sorbate.
The Federal Register permits the following preservatives to be used in car-
bonated soft drinks: ascorbic acid, benzoic acid, BHA, BHT, calcium disodium
EDT A, erythorbic acid, glucose-oxidase-catalase enzyme, methylparaben or
propylparaben, propylgallate, potassium or sodium benzoate, potassium or so-
dium bisulfite, potassium or sodium metabisulfite, potassium or sodium sorbate,
sorbic acid, sulfur dioxide, tocopherols, and, in the case of canned soft drinks,
stannous chloride at less than 11 ppm as tin (FR June 26, 1969,9867).

Foaming and Defoaming Agents

Some drinks have a greater appeal when associated with foam, such as some
soft drinks, but others do not. Foaming and defoaming agents can be used to
control this characteristic. The Federal Register permits the use of glycyrrhizin,
gum ghatti, licorice or glycyrrhiza, yucca (Joshua tree or Mojave), and guillaia
(soap bark) as foaming agents in carbonated soft drinks (FR June 26, 1969,
9867). Dimethylpolysiloxane can be used as a defoaming agent in carbonated
soft drinks at levels equal to or below 10 ppm.

Juice Base Formulation

Fruit drinks usually are made in steps. Microcomponents can be preblended in


the laboratory by experts to help protect proprietary combinations. Preblending
also makes the addition of juice drink components easier by reducing the num-
ber of components needed during batch processing. Flavor extracts utilize water,
ethanol, propylene glycol, glycerol, and/or other surfactive agents as solvents.
Flavor emulsions are made by adjusting the right density combinations of citrus
oils (about 0.84 g/ml) with the heavier oils (about 1.33 g/ml) to obtain about
1.02 glml so that the emulsion will mix with the other aqueous-phase com-
ponents ofthe drink. Water-soluble acids, buffers, preservatives, colorants, tex-
turizers, clouding agents, nutrients, and other components can be preblended
FOOD-GRADE NONJUICE PRODUCTS 327

as well. The blending of these aqueous and nonaqueous components with juice
concentrates constitutes a drink base, which can be used by a bottler to make a
finished drink by the addition of sugar and water. However, the amounts of
sugar, acid, juice, and water significantly affect each other's concentrations; so
determining the right amount of these macrocomponents in relation to one an-
other can become confusing.
In order to determine how the four main macrocomponents of juice drinks
affect each other, their relationship must be defined. The sugar or soluble solid
balance in juice-like solutions can be defined as follows:

(20-10 )

where Vc' Dc, and Be are the volume, density, and Brix of the concentrate used
in making the base or drink, Ws and Wa are the weights of sugar and acid to be
added to the drink, and B, V, and D are the Brix, volume, and density of the
final juice drink. The 1.19 factor is used to obtain the sugar equivalent of the
added acid correction to the Brix as calculated by Equation 2-2. The first and
last terms in Equation 2-2 dropped because they are negligible in acid correc-
tions to juice drinks. To understand the validity of this assumption, consider
making 1000 gallons of drink at 11.8 °Brix and 1 % acid using 10% soluble
solids as orange juice concentrate with a Brix of 65.0 and an acid level of 3.0.
The error in calculating the amount of sugar needed would be about a third of
a pound of sugar out of 828 pounds needed. This suggests that the first and last
terms in Equation 2-2 are negligible. The percent of acid plus the correction is
I + O. 19, so that 1. 19 times the weight of the citric acid is equal to the sugar
contribution to the Brix or soluble solids.
The acid balance is:

(20-11 )

with Vo DC' and Ac being the volume, density, and acidity of the juice concen-
trate used in the drink and V, D, and A the volume, density, and acidity desired
in the final drink, with Wa again being the weight of the acid needed. Unlike
the Brix, which includes acid levels in its value, the percent acid does not in-
clude any sugar concentrations or sugar corrections. Therefore, the weight of
the sugar is not included in Equation 20-11.
The percent juice in the drink is an important parameter, which is defined as:

(20-12 )

using the same variables as above.


By using Equations 20-10, 20-11, and 20-12, other equations can be derived
328 CITRUS JUICE BY -PRODUCTS

that enable the calculation of the amount of sugar and acid needed in a particular
drink:

Ws = VD(B - 1.19A - PB(1 - 1.19AjBJ/100)/100 (20-13)

Wa = VD(A - PBA c /l00B c )/100 (20-14)

To find the volume of water needed, we can utilize a simple weight balance
equation as follows:

(20-15)

where Vw and Dw are the volume and density of water. Using Equations 20-12
through 20-15, we can obtain:

VD ( PB ( 100 + 0.19A ) ) (20-16)


Vw = 100D w 100 + 100 1 - Be e - B + 0.19A

The volume of concentrate needed in a base is easily derived from Equation


20-12:
(20-17)

Equations 20-13, 20-14, 20-16, and 20-17 are all independent equations based
on the same drink parameters, which are usually known prior to formulation.
Care must be taken to use consistent units for densities, volumes, and weights.
We use mainly pounds and gallons here.
Let us consider an example to illustrate how these equations can be used.
Suppose that we want to make 1000 gallons of a 10% juice drink with a final
Brix of 11.8 and a final acid level of 1.0% from a 65.0 o Brix concentrate with
an acid level of 3.0%. How much concentrate, water, sugar, and acid are needed
to make the drink? Because Equations 20-13,20-14,20-16, and 20-17 are in-
dependent equations, we can calculate any of the four parameters in any order.
The densities can be obtained from Equation 2-9 or 2-11 from the Brix. Using
Equation 20-17 to get the volume of concentrate needed, we obtain:

(10% )( 1000 gal) (8.717 lb / gal)( 11.8°Brix)


(100) (65.0 oBrix)( 10.977 lb / gal) = 14.4 gal conc.

The amount of acid needed, using Equation 20-14, is found as follows:

(1000 gal) (8.717 lb / gal) ( 10% (11.8)(3.0% ))


100 1.0% - l00(65.0oBrix.)
= 82.4 lb citric acid
FOOD-GRADE NONJUICE PRODUCTS 329

The amount of sugar can be calculated from Equation 20-13:

(1000)(8.717) ( () 10%(11.8) ( 1.19(3.0)))


100 11.8 - 1.19 1.0 - 100 1 - 65.0

= 827.7 lb sugar

The needed water can be found from Equation 20-16:

1000(8.717) ( 10(11.8) ( 100 + 0.19(3.0))


100(8.322) 100 + 100 1 - 65.0

- 11.8 + 0.19(1.0)) = 919.1 gal water

Although it may be handy to calculate the needed parameters in any order,


especially if only some of them must be calculated, it often is sufficient to
calculate the parameters in sequence by using dependent equations. These de-
pendent equations are simpler to use and easier to program into computers than
the above equations. Using the above example, we must begin with Equation
20-14 to obtain the 82.4 pounds of citric acid needed and Equation 20-17 to get
the 14.4 gallons of concentrate needed. We then can use the following depen-
dent equation to get the amount of sugar needed:

(20-18 )

For example:

(lOO0( 8.717) (11.8) - (14.4)( 10.977)( 65.0)) / 100 - 1.19 (82.4)


= 827.8 lb sugar

compared to the 827.7 pounds of sugar calculated by Equation 20-13. The vol-
ume of water needed can be calculated by using a form of Equation 20-15:

(20-19 )

In the example problem this dependent equation gives:

(1000(8.717) - (14.4)(10.977) - 827.8 - 82.4)/8.322 = 919.1 gal water

It should be remembered that the weight of citric acid determined above is


the weight of pure anhydrous citric acid. If other acids are used, their effect on
the Brix must be determined and substituted into the equations accordingly.
330 CITRUS JUICE BY-PRODUCTS

Citric acid has a solubility in water of 54.0% at 10°C (50°F) to 84.0% at


100°C (212°F). Usually citric acid monohydrate is added to juice drink bases
because it is easier to dissolve than anhydrous citric acid. The weight of citric
acid calculated above can be converted to the weight of citric acid monohydrate
by multiplying by 1.0938. In the above example, this would give 90.1 pounds
of citric acid monohydrate instead of 82.4 pounds of citric acid. The water
added in hydrate form with citric acid monohydrate amounts to less than a gal-
lon in the example and is generally negligible in regard to the amount of water
needed in the drink. Volumetric measurements in large tanks generally have an
error in measurement that is larger than this.
In the manufacture of drink bases, all or part of the citric acid can be added
to the base. In order to do this, it is necessary to add some water to predissolve
the citric acid and perhaps other water-soluble drink base components. Too
much water addition will overly dilute the drink base, and not using enough
water will prevent solubilizing of the citric acid. It may be important to know
what effect this acid and water addition will have on the concentration of the
base. The Brix of the base after the addition of a 50% solution of citric acid
can be calculated as follows:

(20-20)

where V' is the volume of water used to dissolve the acid. This value can be
calculated by using:

(20-21)

where X is the fraction of acid used in predissolving the acid. In the above
example, if we want to dissolve 82.4 pounds of citric acid to make a 50% (X
= 0.50) acid solution, Equation 20-21 becomes:

V' = 82.4(1 - 0.5)/8.322(0.5) = 9.9 gal water

To calculate the fraction of citric acid in a predissolving solution, one can use
the following equation:

(20-22)

Using Equations 20-20 and 20-21 in the above example gives:

~~(714-;-.4~)~(~10~.9_7_7~)(~6_5.~0)~+~1_19~(_82~.4~)~
,. = 59.3°Brix for drink base
(14.4) (10.977) + 1.19(82.4) + 9.9(8.322)
FOOD-GRADE NONJUICE PRODUCTS 331

More water may be needed to dissolve the citric acid. The volume of the base
also needs to be known, and can be calculated by using the following equation:

(20-23 )

where the density of the base, Db' can be found from Equation 2-9 or 2-11
according to the Brix, B b . In the above example, Equation 20-23 becomes:

(14.4)( 10.977)( 65.0) + 119(82.4)


(59.3) (10.693) = 31.7 gal of drink base

The user of the base then would need to use 31.7 gallons of base with 919.1
9.9 or 909.2 gallons of water and 827.7 pounds of sugar. This formulation can
be converted to the use of one 52-gallon drum of base by means of simple
proportions, to give 1 drum of drink base + 1491 gallons of water + 1358
pounds of sugar to make 1640 gallons of finished drink.
As you may have surmised, these calculations can become complex and te-
dious if performed often. Here again, computer programming can be used to
automate the calculations. Figure 20-2 shows a flow chart that can be used to
write a program to automate this procedure.
One problem that emerges from time to time is that the Brix and/or % acid
of the final drink does not come out right. Suppose, in our example, that for
some reason the Brix came out to 1l.5°Brix instead of the needed 1l.8°Brix
and with 0.9 % acid instead of the needed 1.0% acid. If citric acid were added,
the Brix would be affected; so addition of sugar and water would be required
to achieve the proper balance of components. To find the amounts of acid and
sugar needed to correct the situation, the following equations could be used:

(20-24 )

(20-25 )

where the subscript i refers to the parameters for the initial erroneous condi-
tions, and absence of a subscript indicates the desired final conditions. In the
example above we do not want to add water to the final drink; so the last term
332 CITRUS JUICE BY-PRODUCTS

Brix of Cone. (Be)


% Acid Cone. (Ae)
% Juice in Drink (P)
Final Brix (B)
Final % Acid (A) EQ 20-20, 20-23
Final Volume (V) Bb,Vb

EQ 20-21 V'
x=% acid desired in
predissolved
solution

EQUATIONS
20-13,20-14,20-16
20-17
Ws, Wa, Vw, Ve

yes
Ws, Wa, Vw, Ve

Fig. 20-2. Flow chart that can be used to program computers to formulate drink bases.

in the numerator of the two equations above goes to zero, and we get:

(1000)(8.707)(1.0 - 0.8 + (1.0(11.8 - 11.5)/(100 - 11.8)) + 0


100 - 1.0
17.9 Ib citric acid
FOOD-GRADE NONJUICE PRODUCTS 333

(1000)(8.707)(11.8 - 11.5) + 11.8(17.9 + 0)


100 - 11.8
= 32.0 Ib sugar

The total volume of the resulting drink becomes:


(20-26)

Initial Drink Brix (Bi)


Initial Drink Acid (Ai)
Initial Volume (Vi)
Final Brix (8) 1--+1
Final Acid (A)

Vi=Vi+Vw

Vw = Vi(Ai/A-1)
(add Vw to drink)
EO 20-24
Wa

EO 2-14
V'w

EO 20-26 EO 20-25
V Ws

Vi=Vi+V'w

Fig. 20-3. Flow chart that can be used to program computers to calculate the sugar and acid
needed to adjust errors in any type of drink.
334 CITRUS JUICE BY-PRODUCTS

or, in the example:

(1000) (8.707) + 32.0 + 17.9 + 0


1005 gal of total drink
8.717

Again, computer programming can simplify the use of these equations. Figure
20-3 shows a flow chart that can be used to program computers to automate the
adjustment of sugar and acid in citrus or any type of drink.
Because a great amount of water is used in making juice drinks, it is impor-
tant to monitor it so that contaminants do not enter drinks through the water.
The alkalinity of the water is one of the major problems, as it can neutralize
some of the added acids as well as affect the drink flavor. Chemicals such as

Table 20-6. Sample formulation of a 10%


juice citrus drink.
Oil emulsion (296 gal)
Citric acid 7.4 lb
Orange oil 23.71b
Cottonseed oil 308.91b
J3-Carotene 23.71b
Gum 355.61b
FD&C Yellow #5 1.2lb
FD&C Yelloc #6 0.91b
BHT 0.31b
Acid solution (736 gal)
Citric acid 753.6Ib*
Trica\cium phosphate 28.31b
Sodium citrate 127.3 lb
Thiamine hydrochloride 95.6 g
Water 650.0 gal

Drink base
Orange pulp wash concentrate** 274.0 gal
Tangerine concentrate*** 7.4 gal
Lime concentrate 7.4 gal
Acid solution 736.0 gal
Oil emulsion 296.0 gal
Potassium sorbate 74.11b
Orange oil flavor 2.8 gal
*This value is the amount calculated in Equation 20-14 minus the citric
acid added in the oil emulsion and minus the acid in the lime concentrate,
assuming 400 GPL lime concentrate.
**60.0 o Brix and 25 B I A ratio or 2.40% acid.
"*60.0 o Brix and 10.0 B I A ratio or 6.00% acid.
Note: 1000 gal of base makes 17,38\ gal of drink, requiring 15,I691b of
sugar and 15,282 gal of water in addition to the 650 gal of water used to
make the acid solution. The final drink should have a Brix of 11.8 and
0.56% acid.
FOOD-GRADE NONJUICE PRODUCTS 335

chlorine also may influence the final product. In severe cases, water treatment
may be required in citrus drink production.
Table 20-6 shows a complete sample formulation.

QUESTIONS

1. How long has pectin been used to make jellies?


2. What function does pectin serve in fruit?
3. What is the solubility of pectin in hot water?
4. In what foods are pectins mainly used?
5. What variety of fruit is the best source of pectin?
6. What are some common contaminants of pectins, and what are generally
their sources?
7. What is the difference between jams and jellies?
8. What are the four main ingredients of jellies?
9. What do low-methoxy pectins require in order to gel?
10. Why is some of the sugar premixed with the pectin before water is added?
11. What is the primary quality control parameter of citrus sections?
12. What percent of the drain weight must be whole sections in order to meet
a USDA Grade A standard?
13. What are puree bases primarily used for?
14. What are the 11 main components used in making juice drinks?
15. What are two advantages of making juice drinks compared to 100 %
juices?
16. What are some of the main advantages of using citric acid over other
acids in juice drinks?
17. What is the basic composition of juice cloud?

PROBLEMS

1. In making 1000 gallons of a 50% orange juice drink, how much vitamin C do you
need to add in order to have about the same level of vitamin C as found in 100 %
orange juice?
2. Suppose you wanted to make a 60% juice drink base that was 23.0 oBrix, and that
would make 10,000 gallons of final drink at 11.8°Brix and 0.53 acid, using 62.0oBrix
orange concentrate with an acid level of 2. 12 %. How much citric acid, water, and
orange juice concentrate would be needed to make the base, and how much water,
base, and sugar would be needed to make the final drink? (Hint: You can use Equa-
tion 20-21 to find the volume of water V' needed to get the desired 23.0 oBrix.)
3. Suppose that you wanted to make a 30% juice drink, using pasteurized single-strength
juice (12.4°Brix and 0.95% acid) to make 20,000 gallons of 12.0oBrix, 0.67% acid
drink. How much citric acid, water, sugar, and juice would you need? (Hint: Treat
the pasteurized juice in the same way as concentrate.)
336 CITRUS JUICE BY -PRODUCTS

4. In making a 25,DOO-gallon juice drink, it was found that the Brix came out to 11.1
instead of the desired 11. 9 °Brix, but the acid level came out correct at 0.72%. How
much sugar and acid would be needed to correct the Brix, and what would the final
volume of the drink be?
S. In making a 1O,ODO-gallon drink, it was found that the Brix came out to 12.6 instead
of the desired 11.8°Brix with an acid level of 1.60% instead of the desired 1.00%.
How much acid, water, and sugar will be needed to correct the situation? (Hint:
Consider setting the Wa or Ws to zero and use Equation 20-24 and/or Equation 20-25
to solve for Vw ' )

REFERENCES

Bennett, R. D. 1985. From presentation to the Citrus Products Technical Committee at the USDA
Fruit and Vegetable Laboratory, Pasadena, Calif., December 16, 1985.
Bennett, R. D. 1988. From presentation to the Citrus Products Technical Committee at the USDA
Fruit and Vegetable Laboratory, Pasadena, Calif., June 9, 1988.
Food Chemicals Codex, 1931. National Academy Press, Washington, D.C., 215-217.
1FT Committee on Pectin Standardization. 1959. Pectin standardization, final report of the 1FT
committee, Food Tech., 13,496-500.
Joseph, G. H. 1955. Pectic substances, Adv. Chern. Ser., 12,49-56.
Swisher, H. E. and Swisher, L. H. 1977. Specialty citrus products. Citrus Science and Technology
Vol JI, S. Nagy, P. E. Shaw, and M. K. Veldhuis, eds. The AVI Publishing Company, Inc.,
Westport, Conn., 321-322.
Chapter 21

Animal Feed and Fuel By-Products

The waste products of the agricultural and food industry have long been used
as fertilizers and animal feeds, and to make special nonfood products such as
fuels, in the form of methane gas and alcohols. Methane gas production usually
is generated from waste water and will be discussed in Chapter 22. Fuel-grade
alcohols usually are manufactured from peel products and are discussed in this
chapter. Citrus peel and peel products have been and continue to be used as a
source of high-quality animal feeds, which require careful quality control.

FEEDS FROM CITRUS PEEL

Citrus peel often is viewed as a waste product even though some citrus proces-
sors are able to make substantial profits from it. The most popular peel products
are those used in animal feeds. Citrus plants frequently are located in rural areas
where livestock are raised that can use the citrus wastes as feed or a feed sup-
plement. Fertilizers from livestock or pOUltry wastes, in tum, are often used in
citrus groves, creating a compatible symbiotic relationship. Dried peel products
can be conveyed to distant markets as well, which provide the juice processor
with numerous opportunities for disposing of waste products economically.
Many factors affect the quality control of feeds, such as the type and breed
of animal, the desired end results or animal products, the effect of these prod-
ucts on humans, supplemental feeds, the complexities of animal nutrition, the
economics involved, and the storage capabilities of the feed. Many of these
parameters are too complex for routine quality control. Also, the processor has
control over only a few of them. Most of these characteristics are naturally
inherent in the feed, and once the general characteristics of the feed have been
established, it is up to the quality control department to guard against excessive
contamination or alteration of the basic attributes of the feed.
Most citrus processors guarantee their feeds to have at least a minimum
amount of protein, crude fiber, fat, and ash. Another important parameter is the

337
D. Kimball, Citrus Processing
© Van Nostrand Reinhold, New York, NY 1991
338 CITRUS JUICE BY -PRODUCTS

amount of nitrogen-free extract, primarily carbohydrates, which varies some-


what and usually is not guaranteed. Even so, these parameters rarely need rou-
tine monitoring, and the analyses are best performed by professionallaborato-
ries when they are required. A general estimate of the total quality of the feed
can be expressed in several ways, the most common method being the total
digestible nutrients (TDN) of the feed. This is determined by adding the %
nitrogen-free extract, % protein, % crude fiber, and the % fat times 2.25. For
example:
N-free extract 15.9%
Protein (N X 6.25) 1.7%
Crude fiber 2.7 %
Fat (0.2 x 2.25) 0.5%
TDN = 20.8
Although the TDN is a simple number to determine, the proportions of the
four components that actually contribute to animal nutrition varies. Also, these
proportions are based upon humans and dogs, and do not apply directly to ru-
minants. However, the TDN still is commonly used to estimate the general
quality of citrus feeds.

Unprocessed Peel

The use of unprocessed or wet peel as a cattle feed is a widespread practice,


which usually requires that the animals be located relatively close to the citrus
processor. The acidic nature of the wet peel is corrosive to the metal in most
trailers, inevitably resulting in messy leaks. This characteristic, combined with
the wetness ofthe peel, limits the distance that the peel can be transported. Wet
peel generally contains anywhere from 78% to 90% moisture, depending on
the juice extraction procedure used. Because this product usually is sold "as
is," moisture tests or other routine tests rarely are performed. An example of
the nutrient guarantee of wet peel is as follows:
Protein: not less than 1.1 %.
Crude fat: not less than 2.3%.
Crude fiber: not less than 2.6%.
Ash: not less than 1. 3 %.
Transportation costs are the main costs of processing wet peel. They usually
determine the price and the need for additional quality control.

Pressed Peel

Peel that has been shredded, limed, and pressed to remove about 10% of the
moisture has the advantages of lower transportation costs and a more appealing
ANIMAL FEED AND FUEL BY-PRODUCTS 339

and unifonn texture and composition. Such treatment provides for the produc-
tion of press liquor and/or citric molasses, and allows the feed to be transported
longer distances because of a reduction in trailer leaks. Typical nutrient levels
of pressed peel are shown in Table 21-1. Little to no routine quality control is
perfonned on this lightly processed peel product.

Dried Citrus Peel or Pulp

Dried citrus peel, one of the most common feeds manufactured from citrus peel,
is second only to com in nutritive value for dairy and beef cattle and sheep
(Kirk and Davis 1954). The drying of citrus peel is somewhat involved, re-
quiring more quality control monitoring than does production of unprocessed
or pressed peel. Dried citrus peel is made by passing pressed peel through a
rotary dryer, with the consistency and speed of the peel through the dryer de-
tennining the drying efficiency. Studies have been made of the rate of drying
at various temperatures (Braddock and Miller 1978).
Citric molasses is often added to the pressed peel to aid in the drying process
and to help prevent burning of the peel. Too much molasses will cause the peel
to stick to the edges of the dryer, which will also cause burning. Molasses
addition also darkens the color of the feed. Some investigators have even used
the feed color to detennine the amount of molasses that has been added (Bissett
1950). When molasses is used in the drying process, the dried pulp is referred
to as sweetened dried citrus pulp. In wanner drier weather, wet or pressed peel
can be spread on the ground and solar-dried. This is a common and economical
practice in areas with a dry Mediterranean climate such as California. Even
though most peel dryers are equipped with dust collectors, dried citrus peel
usually is associated with fine dried particles. FMC juice extractors break up
more juice cells than other juice extractors, causing an increase in this fine dust
material in the dried feed.
The most important parameter to monitor in dried peel manufacturing is the
moisture content. Moisture levels must be below 10%, or micorbiological spoil-
age can set in along with a buildup of heat. This heat can reach a point where

Table 21-1. Typical nutrient levels for pressed peel.


California Florida Florida
Nutrient Orange Orange * Grapefruit *
Protein (N X 6.25) (%) 1.7 2.01 2.24
Crude Fat ( % ) 0.2** 2.65 1.18
Crude fiber ( % ) 2.7 4.36 4.61
Ash (%) 1.5 1.45 1.46
Moisture ( % ) 78 72 75
Nitrogen-free extract ( % ) 15.9 17.80 15.7
'Kesterson and Braddock 1976.
**ether extract
340 CITRUS JUICE BY·PRODUCTS

the dried peel will spontaneously combust, not only causing a fire hazard but
destroying the product. Smoldering peel that has not been dried sufficiently can
create a serious disposal problem. Unless the peel is spread out and air- or solar-
dried immediately, it will continue to bum until it becomes ash. Some bulk
dried peel warehouses have thermocouple monitors with air vents in the floor
to adjust the temperature and correct moisture problems. The relative humidity
in storage areas should be kept at 52 % or less in order to avoid reabsorption of
moisture by the peel (Braddock and Miller 1978). Oil recovery systems some-
times add moisture to the peel through peel washings, which should be ac-
counted for in drying operations. Grapefruit peel generally contains more mois-
ture than orange peel and thus would require more drying. There are several
ways to perform moisture tests, and one of the simplest follows:

Peel Moisture Test

Equipment and Supplies

• Triple beam balance.


• Heat lamp.
• Drying pan or dish.
• Shredder (blender, food processor, or knife and cutting board).

Procedure

1. If the peel has not been shredded or chopped fine, this needs to be done
with a shredder. Peel particles should be about 20 to 30 mesh or about
1 /81/ in diameter or smaller.
2. Place the empty drying pan or dish on the triple beam balance, and record
the weight ( Wpan ).
3. Place the shredded peel in the drying pan so as to just cover the bottom
of the pan, and record the weight (Wb ).
4. Leaving the drying pan on the balance, radiate the pan with a heat lamp
until no further change in weight is noticed. Record the weight ( Wa ). Care
should be taken not to overheat or scorch the sample.
5. The % moisture can be calculated from:

(21-1 )

For example:

100%(1 - (184.54 - 179.10)/(185.10 - 179.10)) = 9.3% moisture


This procedure can be used with wet, pressed, or dried peel. Dried citrus peel
has the general nutrient values shown in Table 21-2. Dried pulp is slightly
ANIMAL FEED AND FUEL BY-PRODUCTS 341

Table 21-2. Typical nutrient levels of dried citrus peel (Kesterson


and Braddock 1976).
Unsweetened Sweetened
Nutrient Orange Orange Grapefruit
Protein (%) 5.9-6.2 5.3 6.4-7.0
Fat (%) 3.1-4.9 2.8 5.5-5.9
Crude fiber ( % ) 11.5-12.0 9.3 12.1-15.3
Ash (%) 4.9-6.9 8.0 6.5
Nitrogen-free extract ( % ) 62.7-64.0 66.6 56.9

higher in fiber, nitrogen-free extract, and ash than wet peel, but it is lower in
fat (Kirk and Davis 1954).

Pellets

Because of the dusty nature of dried citrus pulp and its low bulk density, many
processors pelletize the dried pulp. This compacting of the dried pulp volume
cuts shipping and storage costs about in half and facilitates a cleaner and more
efficiently conveyed product. The higher-density pellets are more easily con-
sumed by ruminants as well. Pellets made from dried pulp fines are generally
about! inch in diameter and about 1 to I! inches long. Whole dried citrus pulp
is made into pellets about ~ inch in diameter and about ~ to ~ inch long in order
to retain the pulp fiber and seeds (Kesterson and Braddock 1976).
Several factors affect the mechanical durability of the pellets, including the
thickness of the die, holding time, pellet size, energy used in pelletizing, and
bonding agents used. Citrus molasses has been found to be an excellent bonding
agent when used in the proportions of about 5 to 15 % of the total weight.
However, molasses usually is added before the peel is dried instead of during
pelletizing in order to aid in the drying process, as mentioned previously. The
extrusion rate and the bulk density of the pellets vary inversely with the die
length, and the energy needed during the extrusion is inversely proportional to
the die thickness.
Some additional advantages of pelletizing dried citrus peel include the re-
duction of microbial spoilage. It has been found that pellets with twice the
moisture content of dried pulp still are resistant to microbial deterioration (Dean
1966). However, pellets wetter than this lose their mechanical stability. Be-
cause pelletizing involves friction that can heat the product, and thus dry the
pellets, dried citrus pulp destined to become pellets must be dried to only 10 to
12 % moisture levels. After pelletizing, the moisture levels will drop to below
the needed 10% level. Like dried citrus pulp, pellets should be kept in areas
with 52 % or less humidity to avoid reabsorption of moisture into the peel. A
relative humidity of 90% for 30 days has been shown to induce mold growth
(Braddock and Miller 1978).
342 CITRUS JUICE BY-PRODUCTS

Insect Infestation

Another problem in the stomge of dried citrus pulp or pellets is the occurrence
of insect infestation. The almond moth, Cadra cautella (Walker) (Hagstrum
and Sharp 1975) and the saw-toothed gmin beetle, Oryzaephilus surinameusis
(L.), have been associated with dried citrus pulp, with the latter found in coarse
pulp (Laudens and Davis 1956). Pellets and fine meals have been found to
contain the cigarette beetle, Lasioderina serricorne (F.) (Laudens and Davis
1956). Other insects have also been found in dried citrus material and justify
thorough cleaning of warehouses as often as possible. Residual insecticides,
traps, and barriers should be used, as well as professional services if needed.
(See Chapter 16.)

Press liquor

Press liquor is the solution expressed from shredded and limed peel. Unlimed
peel is very slimy and retains moisture. To remove moisture, about 0.15 to
0.25 % lime is added to shredded peel, and is allowed to react for at least 15
minutes. The exact mechanism by which the lime helps to release water and
remove the slimy texture of the peel is not known, but probably the basicity of
the lime demethoxylates the pectins in the peel in a manner similar to the action
of pectinase enzymes:

o o
II ow II (21-2 )
R- COCH 3 - R- CO- + CH3 0H
which is similar to Equation 8-1. The divalent cations, Ca + 2 , from the lime
probably combine with the demethoxylated pectin in a manner similar to that
illustrated in Fig. 8-2. The end result is syneresis, or the natuml expression of
fluid, which is not unexpected considering that 80 to 85 % of the peel is water.
The slimy nature of the unlimed peel is probably due to hydrogen bonding of
the ;:!ster groups of the pectin with water. Lime demethoxylation increases the
ionic strength of these bonds, producing a less slimy texture. About 10% of the
peel moisture can be removed in primary presses. Secondary presses generally
can remove only about another 2 % of the moisture from the peel.
Press liquor usually contains about 9 to 15 % soluble solids expressed as °Brix,
with about 60 to 70% of these soluble solids being in the form of sugars. Peel
oil levels mnge from 0.2% to 0.5% in Florida press liquor and up to 0.8% in
California press liquor made from orange peel. The drier climate in California
produces peel with a higher oil content. Typical press liquor constituents are
shown in Table 21-3. Press liquor is occasionally sold as is for animal feed
production, or fermented to produce fuel-gmde alcohols, or concentrated to
citric molasses, the last being its most common use.
ANIMAL FEED AND FUEL BY-PRODUCTS 343

Table 21-3. Typical composition of citrus press liquor (Nolte, von


Loesedke, and Pulley 1942).
Constituent Range Average
pH 5.4-6.4 5.7
Brix (17.5°C) 6.1-12.6 10.1
Sucrose (%) 1.20-3.09 2.40
Reducing sugars ( % ) 2.82-5.81 4.23
Protein (N x 6.25) 0.40-0.59 0.47
Pectin (alcohol ppt, %) 0.27-0.88 0.66
Ash (%) 0.43-0.94 0.72
Acid as citric acid ( % ) 0.15-0.30 0.21
Alcohol (% by volume) 0.00-0.39 0.22
Peel oil (% by volume) 0.12-0.58 0.23

Citric Molasses

The manufacture of citric molasses offers several advantages over the manufac-
ture of press liquor alone. Storage and shipping costs are greatly reduced be-
cause molasses takes up less space; concentrated sugar solutions are more re-
sistant to microbial spoilage; and citric molasses can be mixed with pressed
peel to aid in peel drying, as mentioned previously, in addition to acting as a
bonding agent when pellets are made from dried pulp. The use of evaporators
that utilize waste heat from peel dryers can greatly reduce the cost of molasses
production. An example of the composition of citric molasses is given in Table
21-4.
Citric molasses generally has about the same characteristics as Blackstrap
molasses except that it contains half as much ash and twice as much protein.
Florida requires that at least 45 % of the total sugars be invert sugars (glucose

Table 21-4. Typical analysis of Florida citric molasses (Kesterson


and Braddock 1976).
Constituent % Constituent %
Brix 72.0 Calcium 0.8
Sucrose 20.5 Sodium 0.3
Reducing sugars 23.5 Magnesium 0.1
Protein (N x 6.25) 4.1 Iron 0.04
N-free extract 62.0 Phosphorus 0.06
Fat 0.2 Manganese 0.002
Fiber 0 Copper 0.003
Ash 4.7 Niacin 35 ppm
Pectin 1.0 Riboflavin 11 ppm
Potassium l.l Pantothenic acid 10 ppm
pH 5.0 Viscosity (25°C) 2000 cps
344 CITRUS JUICE BY-PRODUCTS

and fructose) with a Brix of at least 35.5 after mixing with an equal weight of
water (Florida State Dept. of Agriculture 1950).
Two common problems in the manufacture of citric molasses are foaming
and scale formation. Commercial antifoaming agents can be used to minimize
foaming problems; and in addition to foaming agents, removal of the suspended
solids through centrifuging or other suitable means can reduce foam formation.
Foaming can be due to microbial spoilage, alkaline processing, or the mixing
of old and new molasses (Hendrickson and Kesterson 1971). Scale formation
is due to calcium from the lime used to treat pressed peel, which often precip-
itates on evaporator surfaces as calcium citrate. Using preheaters will provide
a site for the precipitation of this scale in an area that is easier to clean, and the
use of two such preheaters allows the use of one while the other is being cleaned.
The scale can be removed by using a 5 to 15 % hot caustic solution containing
2 to 3 % chelating agents such as alkaline ethylene diaminetetraacetic acid (Kes-
terson and Braddock 1976).
Most citric molasses has been sold as a feed supplement for animal feeds.
Storage of the molasses usually will decrease the pH by about 0.4 unit per
season (Hendrickson and Kesterson 1950), and viscosity will increase with stor-
age. Vigorous agitation generally will restore fluidity, but prolonged storage
can result in solidification of the molasses. Molasses that is increasing its vis-
cosity at a rate of less than 500 cps per day can be stored for at least 3 months
(Hendrickson and Kesterson 1952).
The microbial flora of citric molasses would be expected to resemble that of
juice concentrates. Various species of Lactobacillus and Leuconostoc have been
isolated from citric molasses including L. Jermentum, Le. mesenteroides subsp.
mesenteroides, and Le. paramesenteroides (Parish and Higgins 1988).
A final footnote on citric molasses concerns the suspended matter. Citric
molasses manufactured in California generally contains a large amount of set-
tleable sludge material, which has been linked to the commercial waxes applied
in the fresh fruit packing houses. In Florida, where most citrus fruit is processed
directly from the field, this waxy sludge is less common. Also, the waxes used
in Florida and California are not the same. In California, juice fruit usually is
heavily coated with these waxes, which find their way into the press liquor and
then into the molasses. Commercial centrifuging to remove this sediment has
proved ill advised because sand impurities from the lime end up in the press
liquor and produce excessive wear in centrifuges. This sediment adds to the
viscosity of the molasses and may cause a conveyance problem if allowed to
settle out in storage tanks.

FUEL-GRADE ALCOHOL

With the increase in price of fossil fuels over the past several decades, alter-
native sources for fuels have been sought; and some of the more promising
ANIMAL FEED AND FUEL BY-PRODUCTS 345

sources are found in renewable agricultural products and waste materials. The
food industry has always tried to achieve economical recovery of waste mate-
rials. Now anhydrous ethanol is being used in premium unleaded gasolines, as
ethanol is an efficient fuel that can be used to enhance octane ratings.
Citrus press liquor and reconstituted citric molasses have been used as a feed-
stock for commercial alcoholic fermentations. A major problem encountered in
such fermentations is the presence of citrus peel oil, which is toxic to most
microorganisms. As mentioned previously, press liquor contains at least 0.2 %
oil (based on 1I.8°Brix). Citric molasses usually contains much less oil, as
most of it has been stripped out during evaporation. Oil levels must be 0.08 %
or less for a successful alcoholic fermentation; so the oil in citrus press liquor
must be removed before fermentation can take place. A common way to do this
is to use direct steam injection into press liquor (see Chapter 6 and section on
stripper oil). The viscosity of citric molasses also can inhibit fermentation, in-
cluding the contribution of waxy sludge material found in California citric mo-
lasses, as mentioned. Citric molasses usually is diluted to about 200Brix or less
prior to fermentation.
Like most microorganisms, yeasts undergo four main stages of growth, as
shown in Fig. 21-1. In the initial phase, they begin adjusting to conditions and
start to grow. Growth is rapid during the log phase, where reproduction occurs
exponentially. As the feedstock is depleted and the yeast waste material (alcohol
here) is concentrated, growth slows until fermentation reaches a steady state. It
is in the lag phase that fermentation is the most efficient. If fresh feedstock is

r
z
0 lag phase

~
::> death
a.. phase
0
a.. log phase
.....
en
L5
>-
TIME •
Fig. 21-1. The four stages of microbial growth. Alcoholic fermentation is most effective when
the yeasts are in the lag phase.
346 CITRUS JUICE BY-PRODUCTS

not introduced, the growth will eventually begin to decrease, resulting in the
death phase.
There are basically two types of fermentation, continuous and batch. Contin-
uous fermentation requires that yeast be kept in the lag phase by constantly
replenishing the feedstock while bleeding off the alcoholic solution without
changing the yeast population or activity. A popular and efficient continuous
fermentor is the Wick fermentor, shown in Fig. 21-2 (Wick 1980). The gas
generated in the fermentation causes a circular flow in the solution; and this
circular current not only mixes the solution to make it uniform, but it keeps the
yeast within it, providing a "dead zone" that contains little yeast in the comers
where the alcoholic solution can be bled off without significantly changing the
yeast population. Commercial use of the Wick fermentor has proved successful
(Eastman 1981). Continuous fermentation also is easier to monitor as far as
quality control is concerned because its conditions do not change as much as
those of batch operations. Batch fermentation requires greater tank space to
produce alcohol as rapidly as the continuous methods do. Also, the constant
starting and stopping of batches is very time-consuming and requires close at-
tention to ensure a successful fermentation.
Other factors also affect the rate of fermentation, including the type of yeast
used. Distiller's yeast has been found to grow faster in reconstituted citric mo-
lasses or steam-treated press liquor in California than do the natural yeasts or
Montrachet yeast. Excessive bacterial growth can destroy a fermentation, pro-

Carbon
Dioxide
Vent
Outbound
Alcoholic
Solution

,,--........
Currents Caused ! f -;; '\ )
By Gas Bubbles ~ Iff '/ J
From I
Fermentation tIL I;
t I...~ /
,-,.,

Fig. 21-2. Wick continuous fennentor used commercially to produce fuel-grade alcohol (Wick
\980).
ANIMAL FEED AND FUEL BY-PRODUCTS 347

ducing acetic acid rather than alcohol. Because bacteria grow much faster than
yeast, bacterial growth can quickly take over a fermentation. However, bacteria
are more sensitive than yeast to the osmotic effects in concentrated molasses,
as well as to benzoates and penicillin. Steam treatment of press liquor and pas-
teurization of molasses during evaporation are generally sufficient to prevent
bacterial contamination. Small amounts of benzoate or veterinary grade peni-
cillin can be used to inhibit bacterial growth as well. A good cleanup and san-
itation program is the best way to prevent bacterial spoilage.
In order to start up a fermentation process, using either a batch or a contin-
uous method, the feedstock must be diluted to 12 to 30 oBrix. Also, fermenta-
tion is more rapid with warm solutions. The peel oil level should be checked
to ensure that it is below the 0.08% v Iv limit (based on 1l.8°Brix). As the
container is filling with feedstock, one should add about 120 ml of veterinary
grade penicillin, 3 gallons of FMC defoamer or the equivalent, and 1 gallon of
pectinase if needed to reduce the viscosity of the solution, assuming a
1O,OOO-gallon fermentation volume. One should mix about 20 pounds of dis-
tiller's yeast in a 5-gallon bucket of lukewarm water to paint consistency, and
when gas evolves, add the mixture to a fermentation vessel containing about
half of the feedstock (5000 gallons here). It is important to allow a vent for
evolving carbon dioxide gas. The 20.0oBrix feedstock should decrease in Brix
down to about 13.0 oBrix after fermentation in batch processing. Fermentation
of 10,000 gallons takes up to 24 hours or so to really get under way and about
36 to 48 hours for completion, depending on feedstock, yeasts, and tempera-
ture.
To determine when fermentation is complete, a reducing sugar test can be
used. The Brix alone is insufficient because alcohol and other components of
the solution will contribute to it. Although the reducing sugars account for only
about half of the sugars present, their disappearance can be used as an indication
that all the sugars have been consumed in the fermentation. Reducing sugar
levels of 1 to 2 % usually indicate that the fermentation is complete. A method
that can be used to measure the reducing sugars is given in Chapter 19.
After fermentation, the beer is distilled in commercial stills. Aqueous alcohol
forms an azeotropic mixture upon distillation that prevents more than 95.6%
ethanol from being distilled at atmospheric pressure. Further heating cannot
result in any enrichment of the ethanol solution. Commercial plate column stills
can produce 90% ethanol solutions but generally achieve around 80% ethanol.
An 80% ethanol solution is sufficiently enriched to be used directly as a fuel in
automobiles with enlarged air intake jets, but 100% or anhydrous ethanol is
required for blending with gasoline. Alcohol bums hotter than gasoline and thus
requires a higher air mixture in the carburetor. Pure ethanol can be obtained by
further drying of the 80 % solution using absorbents, such as cornstarch or dried
citrus peel, or by the use of a vacuum (95 torr, 0.125 atm, or 26 inches of Hg)
during distillation that will shift the azeotropic composition up to as high as
348 CITRUS JUICE BY-PRODUCTS

99.5% ethanol. When an absorbent is used to dehydrate the alcohol solution,


dry carbon dioxide from the fermentation process can be used to redry the ab-
sorbent so it can be reused. A typical continuous plate alcohol still is shown in
Fig. 21-3. Some of the alcohol solution is refluxed back into the top of the
second column in order to maintain the proper temperature.
The quality control of distillation involves the measurement of alcohol levels
at various points. The distillage can be concentrated and added back to the peel
like citric molasses, as a high-protein supplement to the feed. This distillage
should not contain more than 5% alcohol; otherwise, too much alcohol is being
lost. The temperature of the first column should be about 245°F (118°C) in
order to remove 95 % of the alcohol. If water builds up in the bottom of the
second column, it can be pumped back into the first column. The temperature
in the second column should stabilize at about 173°F (78.2°C). In order to
avoid federal liquor license requirements, the alcohol produced needs to be
denatured or poisoned by adding methanol or a similar toxic chemical that will

Thermometer
Vapors

Beer --+

oo
:s
a.
CD
:s
...
~

Reflux
~-- Tank

Product
Tank
Distillage

Fig. 21-3. Commercial still used in production of alcohol from citric molasses or press liquor.
ANIMAL FEED AND FUEL BY-PRODUCTS 349

not affect its perfonnance as a fuel. Adequate signs and labeling must be used,
warning that the alcohol is toxic and is not intended for human consumption.
In order to measure the alcohol level in the distill age and the final product,
several methods can be used. One method involves measurement of the chem-
ical oxygen demand (COD) and is lengthy compared to other methods (AOAC
1984); another involves measurement of the specific gravity (AOAC 1984); a
third method involves the direct fractional distillation of the alcohol from the
sample. The latter two methods have proved sufficient for routine quality con-
trol. The specific gravity method is best for measuring the ethanol in the distil-
late or final product, and the distillation method works best for measuring the
ethanol in the distillage.

Ethanol by Specific Gravity (AOAC 1984)

Equipment and Supplies

• Balance.
• 25 ml pipette.
• 25 ml beaker or flask.
• 25 ml of distilled water.
• Thennometer.
• AOAC table 52.003 (optional).

Procedure

1. Pipette 25 ml of distilled water at 20°C into a clean and dry beaker or


flask, and weigh it. If the same pipette and container are used each time,
the same weight of the container and water can be used for each test.
2. Using the same pipette and container, pipette 25 ml of the alcoholic dis-
tillate (70% or more in ethanol) at 20°C into the container, and weigh it.
3. Divide the weight of the sample by the weight of the water to get the
specific gravity.
4. Use AOAC table 52.003 to find the % alcohol according to specific grav-
ity, or use the following regression equation, which can be easily pro-
grammed into hand-held programmable calculators or computers:

%A = -1176 + 1895/Sg - 701/S; (21-3 )

where Sg is the specific gravity, and A is alcohol. For example:

-1176 + 1895/0.839 - 701/(0.839? = 87% alcohol


350 CITRUS JUICE BY-PRODUCTS

Commercial ethanol from citrus products contains a slight off coloration. In


citrus alcohol produced in California, small amounts of isopropyl alcohol and
ethyl esters have been found (Bennett 1981). These ethyl esters probably are
coupled with inorganic salts such as phosphates or sulfates.

Ethanol by Distillation

Equipment and Supplies

• Setup shown in Fig. 21-4.


• 100 ml graduated cylinder.

Procedure

1. Add 100 ml of the sample to the boiling flask in Fig. 21-4, and apply
heat. The temperature at the top of the column should reach 78.2°C
( 173 ° F) when the fractionating ethanol reaches the thermometer. This
temperature should remain steady until toward the end of the distillation.
2. When no more ethanol can be seen coming over into the condenser, or
when water beads are noticed in the column or condenser, record the
milliliters distilled as the % v I v of alcohol. For further accuracy, multi-
ply the milliliters of distillate by 0.95 to get the approximate true % al-
cohol in the sample, or use the specific gravity method on the distillate.

It should be readily apparent that the distillate cannot contain more than the
95.6% ethanol azeotropic limit. This is the reason for using the 0.95 factor in
step 2 above and for the suggestion that the specific gravity method be used on
the distillate. However, the % v Iv of ethanol measured by using this method
is adequate for most routine quality control.

QUESTIONS

1. What are the main nutritional parameters of citrus peel animal feeds?
2. What is the most common feed produced from citrus peel?
3. Why is citric molasses added back to pressed peel before peel drying?
4. What is the most important quality control parameter in the manufacture
of dried citrus peel, and why?
5. What are the advantages of pelletizing dried citrus pulp?
6. Why is lime added to press peel?
7. What is the major use of citric molasses?
ANIMAL FEED AND FUEL BY-PRODUCTS 351

Thermometer --.Il

Packing Material

Condenser
- - - - (No Water)
Condenser-' Water

Water-.

' ....f---100 mls Sample


10 ml
Graduated ---I'"
Cylinder Variable Heat
Source

8. What basic citrus peel component inhibits alcoholic fermentation of peel


extracts?
9. Why is bacterial growth a problem in alcoholic fermentations?
10. What two solutions require quality control monitoring during distillation
of fermented citrus beers?
352 CITRUS JUICE BY-PRODUCTS

PROBLEMS
1. What is the TDN for wet peel that just meets a typical nutrient guarantee as men-
tioned in the chapter, assuming a nitrogen-free extract of 1O.3%?
2. What would be the TDN of pressed California orange peel, sweetened dried citrus
pulp, and citric molasses, according to the data in the chapter?
3. Is dried citrus pulp dry enough if a 6.832 g sample in a 165.132 g pan weighed
171.178 g (pan and sample) after drying under a heat lamp?
4. What would be the % alcohol in a distillate with a specific gravity of 0.832?
5. What would be the exact % alcohol in the distillage if 6.7 ml were distilled off in
the alcohol determination described in the chapter, yielding a distillate with a specific
gravity of 0.812? Would this be considered an acceptable distillation efficiency?

REFERENCES

AOAC. 1984. Official Methods of Analysis, 13th Edition, 9.012, 9.014, 10.024, 11.005, 11.007,
11.008. Association of Official Analytical Chemists, Washington, D.C.
Bennett, R. D. 1981. Private communication.
Bissett, O. W. 1950. A method for estimating soluble solids in dried citrus pulp, Proc. Fla. State
Hort. Soc., 63, 174-179.
Braddock, R. 1. and Miller, W. M. 1978. Some moisture properties of dried citrus peel, Proc.
Fla. State Hort. Soc., 91,106-109.
Dean, W. W. JT. Pelleting Wet Citrus Pulp with the Aid ofa Bonding Agent. M.S. Thesis. Uni-
versity of Florida, August 1965, University of Florida Agriculture and Engineering Mimeo Re-
port EG66-1, February 1966.
Eastman, R. 1981. Private communication.
Florida State Dept. of Agriculture. Lett. of December 8, 1950, Supplementary Feed Bull., 97.
Hagstrum, D. W. and Sharp, J. E. 1975. Population studies of Cadra cautella in citrus pulp ware-
house with particular reference to Diapause, 1. Econ. Entomol., 68(1), 11-14.
Hendrickson, R. and Kesterson, J. W. 1950. Storage changes in citrus molasses, Proc. Fla. State
Hort. Soc., 63, 154-162.
Hendrickson, R. and Kesterson, J. W. 1952. Viscosity of citrus molasses, Proc. Fla. State Hort.
Soc., 65, 226-228.
Hendrickson, R. and Kesterson, J. W. 1971. Citrus molasses, Fla. Agr. Exp. Sta. Bull., 677,
3-27.
Kesterson, J. W. and Braddock, R. 1. 1976. Byproducts and Specialty Products of Florida Citrus.
University of Florida, Gainsville, Fla., 10,22,31.
Kirk, W. G. and Davis, G. K. 1954. Citrus products for beef cattle, Fla. Agr. Exp. Sta. Bull.:
538,5-16.
Laudens, H. and Davis, D. F. 1956. Dried citrus pulp insect problem and its possible solution with
insecticides-coated paper bags, Proc. Fla. State Hort. Soc., 69, 191-195.
Nolte, A. J., von Loesedke, H. W. and Pulley, G. N. 1942. Feed yeast and industrial alcohol from
citrus wastes press juice, Ind. Eng. Chern., 34, 670-673.
Parish, M. and Higgins, D. 1988. Isolation and identification or lactic acid bacteria from samples
of citrus molasses and unpasteurized orange juice, 1. Food Sci., 53(2), 645-646.
Wick, E. 1980. New vessel design for rapid, continuous, fermentation. USDA Science and Edu-
cation Administration, Advances in Agricultural Technology, AAT-W-10/February.
Chapter 22

Wastes from Citrus Plants

Citrus processing plants, like most other plants, generate materials of little or
no commercial value that generally need to be removed from the processing
site. It usually is the responsibility of the quality control department to monitor
and manage waste accumulation and treatment, especially in small processing
plants. These materials, which can be classified as solid, liquid, gaseous, or
hazardous wastes, can be conveyed from the plant through waste streams, by
air flow into the atmosphere, or by vehicle. Because these materials affect per-
sons in the vicinity of the plant, and because federal, state, and local regulations
apply to the disposal of these wastes, the quality control of wastes is an impor-
tant function.
The degree of pollution regulation depends largely upon the type and amount
of pollution as well as the surrounding environment. Citrus processing plants
and bottlers exist in a variety of locations, from rural to metropolitan, with a
wide range of existing pollution. Many plants are located next to large bodies
of water, which often act as disposal sites for wastes. Rural sites include large
land areas, which also may serve as disposal sites. Metropolitan plants often
take advantage of municpal disposal facilities, whereas plants located in sub-
urban areas must treat their own wastes or convey them long distances. The
federal government has passed several laws to control the pollution of the en-
vironment, including the Clean Air Act of 1977, the Clean Water Act, the Safe
Drinking Water Act, the Resource Conservation and Recovery Act, and the
Toxic Substance Control Act. State and local governments are likely to have
even stricter requirements and to act as watchdogs for the standards of the fed-
eral Environmental Protection Agency (EPA). It is estimated that except for
preconstruction environmental impact reports, a properly running citrus pro-
cessing plant that processes under 500,000 tons of fruit a year probably will not
need to deal with EPA on a continual basis. With good waste management,
even larger plants can escape close regulatory scrutiny.

353
D. Kimball, Citrus Processing
© Van Nostrand Reinhold, New York, NY 1991
354 CITRUS JUICE BY-PRODUCTS

AIR POLLUTION

Citrus processors and bottlers are not considered nationally to be major polluters
of the atmosphere. However, as with all manufacturers, their pollutant emis-
sions are significant enough to require some form of monitoring. Some of the
main sources of air pollution include boilers, evaporators, and furnaces, as well
as minor sources such as storage tanks, cooling equipment, and dried peel con-
veyance equipment. Rotting refuse and waste water are another source of off
odors that can contribute to atmospheric pollution.
The EPA has issued standards for ambient air quality, as summarized in Ta-
ble 22-1. Primary emissions are those that immediately escape the processing
equipment. Secondary emissions are those formed from primary emissions in
the air, which are of less importance to citrus processors than primary emis-
sions. Pollution problems often arise from errors in the feedmill where peel is
burned or volatile organic compounds (VOCs) are not sufficiently scrubbed. A
bluish gray smoke is indicative of d-limonene emission. Many local regulations
limit the VOCs that can be emitted, including the VOC content of paints and
thinners. For example, in Tulare County, California, only 420 grams of
VOC /liter of paint (excluding water) is allowed during drying below 194 OF
(90 ° C). The stringency of local regulations can be seen by comparing this
value to the federal maximum of 1470 grams VOC /liter of paint used in paint-
ing automobiles (45 FR 85414, December 24, 1980).
Sulfur compounds are considered one of the major pollutants in the combus-

Table 22-1. Primary ambient air quality standards set by EPA as of


1983 (Perry and Green 1984).
Pollutant Maximum Primary Emission Per Time Period
0.03 ppm Annual mean**
0.14 ppm* 24 hours
co 8.7 ppm* 8 hours
35 ppm* I hour
0 3 (corrected for N0 2
and S02) 0.12 ppm* I hour
NO" 0.05 ppm Annual mean**
Lead 0.08 ppb* I hour
Hydrocarbons
(corrected for CH 3 ) 0.24 ppm* 3 hours
Particulate matter 0.04 ppm Annual geometric mean***
0.13 ppm* 24 hours
Photochemical oxidants
(expressed as 0 3 ) 0.08 ppm* I hour
'Not to be exceeded more than once per year.
**(E7~ 1 lin
***nth root of (II;'~ 1 l.
WASTES FROM CITRUS PLANTS 355

tion of fossil fuels. In citrus processing, natural gas and oils, which contain
some sulfur, are the most common sources of energy. In Tulare County, Cali-
fornia, a rural area, the sulfur content must be below 0.7% in fuels. In Met-
ropolitan Los Angeles, the sulfur content must be 0.5 % or less in fuels. These
maximum values change from time to time, depending on existing conditions.
Local authorities generally require notification of changes from one fuel to an-
other or any other changes that may affect the pollution of the area. Good com-
munication and consideration for one's neighbors and the environment gener-
ally will prevent pollution regulation from becoming a serious issue.

SOLID WASTES

Even though citrus peel generally is sold as an animal feed, it sometimes is


referred to as a major solid waste from citrus processing plants. Discarded peel,
rot bins, and even pooled waste streams can cause a stench and should be re-
moved. Piles of discarded peel are an unsightly, reeking mess. Other forms of
solid wastes may include broken glass that can be shipped back to the glass
factory; shipping cartons, crates, fiber containers, and so on which can be burned
or sent to recycling stations or municipal disposal sites; and discarded equip-
ment, drums, metal cans, and so forth, which usually can be sold as scrap
metal. Collections of these solid wastes provide harborages for rodents and
insects that may spread to processing areas.

L1aUID WASTES

The primary waste from citrus processing plants and bottlers is in the form of
liquid or aqueous wastes. Aqueous wastes assume a variety of forms, from
relatively clean refrigeration water to highly organic discharges from oil cen-
trifuges. Regardless of the source, citrus waste streams basically contain four
types of contaminants: suspended and settleable solids (such as juice sac ma-
terial, pulp, and waxes), soluble organics (primarily sugars and acids), soluble
inorganics (caustic sodas), and volatile organics (d-limonene from peel oils,
etc.). Various methods and method combinations can be used to treat this type
of waste, depending on the need and the resources available.

Filtration

All waste treatment methods list filtration as the initial step. Self-cleaning grav-
ity-fed screens or shaker screens remove particulate matter, which can clog
equipment or lines as well as prove difficult to treat. Solid material thus re-
moved can be added to citrus pulp and processed in the feedmill, or collected
and transported to a remote disposal site.
356 CITRUS JUICE BY -PRODUCTS

Reuse Water

Waste effluents can be greatly reduced by reusing some of the waste streams.
For example, the relatively clean refrigeration water can easily be recycled
within the refrigeration system itself. Condensate water from the first effect in
evaporators can be reused in boilers as makeup water. Other condensate streams
from cooling towers can be used in belt sprayers to facilitate fruit conveyance,
as well as in some clean up hoses. This water may not be suitable for other
drinking or food processing purposes and should be so labeled, but potable
water that has been completely treated can be used anywhere in the plant. Be-
cause juice evaporators produces water, the waste water effluents will always
exceed water usage.

Dissolved Air Flotation (OAF)

The introduction of fine air bubbles into static waste water is used extensively
in the food industry to separate grease, fats, and waxy materials. Under such
conditions, these materials have a tendency to float so that they can be skimmed
off and removed. In citrus processing plants OAF is used to help separate sus-
pended pulp and waxes from screened waste water and to aid in sludge settling
after aerobic treatment. As mentioned in Chapter 21, waxes washed from fresh
market culls produce a waxy sediment in waste streams, which can be separated
by OAF. The skimmed residue then can be added to citrus pulp entering the
feedmill. It is estimated that 10 to 20% of the effluent waste loading can be
removed by using OAF.

Flocculation

Another method used to reduce waste effluent loading is flocculation of heavier


dissolved or suspended material in the waste streams. A flocculating agent is
introduced into the water, and it complexes, aggregates, or precipitates with
heavier components of the water, which then proceed to settle out. The settled
sludge can be removed by centrifugation and added to feedmill material. Lab-
oratory tests have shown that lime addition followed by centrifugation can re-
move up to 21 % of the effluent loading, and the use of lime and alum can reduce
the loading by as much as 43 % (Kimball 1981). In another study, lime and
polyelectrolyte floc used with DAF reduced the loading by 10 to 20% (Ratcliff
1974). Lime addition (4.4 Ib/1O,OOO gal of water) to clarifiers after aerobic
treatment can aid in sludge settlement as well.
WASTES FROM CITRUS PLANTS 357

Irrigation

In many areas where citrus is grown, irrigation is used extensively in agriculture


as a means of watering various crops. Citrus waste streams are being used as a
source of irrigation water in many such areas, especially in California. The San
Joaquin Valley's alkaline soils are ideally suited for the generally acidic citrus
waste streams. Even in the sandy soils of Florida, citrus effluents have been
shown to be effective water sources for citrus groves (Wood 1973). The sandy
Florida soils act like sieves that filter particulate matter from the water. It has
been reported that Florida soils can receive up to 500 lb BOD / acre day (Wheeler
1977).
Basic effluents have a tendency to "tie up" or bind the soil, forming a mat
that decreases soil permeability; so caustic cleanup solutions should be neu-
tralized or mixed with other acidic effluents before land deposition. Unaerated
ponding or pooling of citrus waste streams causes anaerobic off odors to de-
velop, which may be undesirable in less rural areas. Care should be taken in
depositing onto cropland those effluents from special processing that contain
high sodium levels from alkaline solutions. Additional sodium in the soil can
leech into the water table and can increase the salt level in water extracted from
wells. If necessary, pH control systems can be used to control the acidity of the
water used in irrigation.
Generally, little quality control is needed for such water, which is an advan-
tage of the method although local regulatory agencies may require monitoring
of sodium, nitrate, and BOD loading of water deposited on soils. Another ad-
vantage is that the water is being used for something useful rather than just
going down the drain. A common practice is to mix citrus effluents with well
water in order to dilute acidity and other contaminants before deposition on the
soil. This is usually done by the user of the irrigation water rather than the
processing plant.

Municipal Disposal

Processing plants that exist in less-rural areas often use municipal sewage treat-
ment plants as a means of waste water disposal. This usually requires some
quality control monitoring, as disposal fees usually are based on the loading of
the effluent and the volume. Outside laboratory analyses often are used in order
to ensure the impartiality of the analysis results. In larger communities, citrus
effluents make minor contributions to overall waste streams; but in smaller com-
munities, citrus effluents run the risk of becoming political footballs, whether
or not that is warranted. Careful records should be kept regardless of actual
requirements.
358 CITRUS JUICE BY-PRODUCTS

Sample collection for such monitoring can be done in several ways. The
easiest and least accurate method is to take periodic grab samples. Waste water
composition varies dramatically throughout processing, and such grab samples
are not likely to be representative of the total stream. Periodic autosamplers are
costly and, again, may not accurately represent the waste streams. The most
accurate sampling system is a bleed line attached to the main waste stream,
which empties into a composite tank. This continuous sampling gives the clos-
est representation of the total stream. When sampling is to be done, the tank
contents are thoroughly mixed, a sample is taken, and the tank is drained so
that it can collect another composition of the waste stream.
Daily sampling usually is sufficient. Daily samples can be blended into weekly
composites, which in tum can be blended into monthly composites according
to the volumes of the waste water per time period. For example, if the daily
volumes were 50,142 gallons, 64,321 gallons, 36,478 gallons, 84,168 gallons,
and 47,171 gallons, you could make a weekly composite by adding 50.1 mlof
sample one, 64.3 ml of sample two, 36.5 ml of sample three, 84.2 ml of sample
four, and 47.2 ml of sample five, to get 282.3 ml of total weekly composite.
Samples should be well mixed before blending in order to contribute a repre-
sentative amount of settleable solids to the composite. Also, all waste water
samples should be refrigerated to avoid changes in composition before analysis.
The common tests performed on such samples can be found in the following
sections.

Aerobic Treatment

There are many types of microorganisms, each growing under a certain range
of conditions. In waste water treatment, aerobic microbes-those that require
oxygen to grow-are known to consume most organic wastes without the pro-
duction of off odors. Those organic wastes that can be thus consumed are called
biodegradable. Anaerobic microbes-those that do not require oxygen to grow
or require that oxygen be absent-produce waste products associated with rotten
odors, which are environmentally undesirable. For this reason, aerated lagoons
are used to induce aerobic growth in treating most organic wastes.
Microbial growth is very sensitive to certain conditions, one of them being
the acidity or pH. Aerobes grow best at neutral pH levels, but citrus effluents
generally have pH values of around 3 to 4, which means that pH control systems
may be required prior to aerobic treatment. Most municipal effluents are basic
and are partially neutralized by citrus waste streams. Shock loadings of low pH
or high pH values from caustic cleanups can seriously upset aerobic activity.
Also, waste streams that are left standing without aeration for long periods of
time, especially during warm weather, may undergo anaerobic growth that can
significantly reduce the pH. After the pH has been adjusted, the waste stream
WASTES FROM CITRUS PLANTS 359

should be treated promptly; otherwise, the acid neutralization can be totally


reversed in a matter of hours.
Another important parameter to monitor during aerobic treatment is the dis-
solved oxygen (DO). In order for aerobes to function, a DO level of 1 to 2 ppm
must exist in the solution. The DO is usually measured by using an oxygen
meter equipped with an oxygen electrode. Oxygen meters can be calibrated in
ambient air according to the air pressure or altitude and the maximum solubility
in moisture-saturated air. First, the electrode is wrapped in a damp cloth or
inserted into a BOD bottle with a few drops of water. Care should be taken not
to let anything touch the membrane of the electrode, and about 10 minutes
should be allowed for temperature equilibration. The reading to which the meter
should be adjusted can be calculated by using either the atmospheric pressure
or the altitude, in the following equations:

O2 (ppm) = (0.001316)P /(0.0666 + 0.00216T) (22-1)

or:
02(ppm) = (0.9916 - 3.049 x 1O- 5A)/(0.066 + 0.00216T) (22-2)

where T is the temperature in degrees centigrade, A is the altitude in feet, and


P is the atmospheric pressure in mm Hg. These equations are sufficiently ac-
curate for most needs. For a little more accuracy, the following more complex
equations can be used:

02(ppm) = (0.001316)P/(6.02 x 1O- 6 (T + 156.8) - 0.07955) (22-3)

or:
1.136 x 10 14e-(A+1764110)2j9.616XIO 'O
02(ppm) - -----------=---- (22-4 )
6.025 x 1O- 6 (T + 156.8)2 - 0.07955
These equations are good from around O°C to 45°C, 502 mm Hg to 775 mm
Hg, and from - 540 feet to 11,273 feet above sea level. Once the oxygen meter
is calibrated, it can be used for several tests before recalibration is needed,
depending on the care of the electrode. The manufacturer's instructions should
be followed in the operation and care of the oxygen meter and the electrode.
When the DO levels in the aeration lagoon are too low, the aeration equipment
should be adjusted accordingly. The higher the loading, the higher the rate of
oxygen consumption will be. If insufficient aeration is performed, the water
will generate anaerobic growth, off odors, and low pH levels, and aerobic ac-
tivity will cease.
It also is important to monitor the d-limonene level in aerobic treatment. This
substance, obtained primarily from oil processing wastes, is toxic to most mi-
360 CITRUS JUICE BY -PRODUCTS

crobes and may affect aerobic activity (Murdock and Allen 1960; McNary,
Wolford, and Patton 1951). Water entering the aeration lagoon should have an
oil level of 0.005 % v Iv or less as measured by the Scott method (see Chapter
6). Oil strippers can be used on high-oil streams, or these oil-laden streams can
be isolated and treated separately. If the water content of high-oil streams is not
too high, they can be added to the press liquor in the feedmill and processed
into molasses, and then added back to the dried peel.
Determination of the biological oxygen demand (BOD) is the most common
way to find the loading or the necessary aerobic treatment for waste streams.
This is done by growing certain microbes in waste water samples and measuring
the rate of decrease of the DO, which usually takes 5 days. The seed bacteria
used in the test can be obtained from the aeration lagoon itself. The seed water
should be stored at 20°C for 24 to 36 hours, and 3.0 ml of the clear undisturbed
top layer should be used to seed the samples. The water used in the dilution of
the sample should be distilled from alkaline permanganate solution in order to
eliminate all organic residues. The use of water deionized by ion exchange is
not recommended because interfering organic residues may be contained therein.
The dilution water needs to be saturated with oxygen. This can be done by
filling one-gallon jugs three-quarters full with the distilled water and incubating
them at 20°C for at least 24 hours while sealed. The air in the head space above
the water will saturate the water. BOD nutrient buffer pillows can be purchased,
which can be added to a certain volume of dilution water to ensure proper pH
values and nutrients for microbial growth. The following procedure can be used.

Five-Day BOD

Equipment and Supplies

• Calibrated oxygen meter and electrode.


• Five 300 ml BOD bottles with screw caps and room to insert the oxygen
electrode. (The bottles should be made of glass.)
• 1, 2, 3, 4, and 5 ml pipettes with pipette bulb or the equivalent.
• Incubator (20 ± 1°C).
• 15 ml seed water from aeration lagoon.
• Dilution water free from extraneous organics, buffered and supplied with
nutrients using commercial BOD nutrient buffer pillows, and saturated with
oxygen (see text above).
• Stoppers for each BOD bottle.

Procedure

1. Using the O2 meter, measure the DO of the sample, and record it.
2. Using the pipette bulb, pipette 1,2,3,4, and 5 ml of stirred sample each
into corresponding 300 ml BOD bottles.
WASTES FROM CITRUS PLANTS 361

3. Add 3 ml of seed water to each bottle, and fill the bottles to just below
the lip with the dilution water. When pouring water, decant it along the
sides of the bottle to avoid the formation of air bubbles. Stopper each
bottle, being careful not to entrap air bubbles, and invert the bottles sev-
eral times to mix the contents.
4. Remove the stoppers, and fill the bottles to the top so that no head space
will remain when they are capped. Incubate the samples (20 ± 1 DC) for
5 days in the dark.
5. After 5 days, remove the cap of each bottle, and insert the oxygen elec-
trode and measure the DO. of each. The oxygen meter should have been
previously calibrated, as described above in the text. When DO. readings
are made, some stirring may be required, but excess stirring will cause
atmospheric oxygen to dissolve in the solution and distort the results.
6. Plot the DO. readings versus milliliters of sample taken. At least three
points should be on a straight line. Discard any extraneous points. Deter-
mine the DO. consumed per milliliter of sample (the slope of the plot) and
the dissolved oxygen level at "0" sample, or where the line crosses the
DO. axis. This should be between 8 and 9 ppm DO., depending on the
elevation of the laboratory. The Bo.D can be calculated from:

Bo.D = ( DO. larger - DO.smaller ) 300 - DO.; + Do. s (22-5)


Vsmaller - Vlarger

where DO.; is the DO. where the line intersects the DO. axis, and DO., is
the DO. measured in the pure sample. The 300 refers to the Bo.D bottle
volume. The oxygen consumed is found by selecting two points used in
the plot in Fig. 22-1 and subtracting the DO. of the larger DO. (Do.larger)
from the DO. of the smaller DO. (Do.smaller) and dividing by the volume
of the smaller DO. (Vsmaller) minus the volume of the larger DO. (Vlarger)'
For example, if we obtained DO. readings as shown in Fig. 22-1 and mea-
sured a DO. value of 1 ppm in the original sample, we would obtain the
following by using Equation 22-5:

7.5 ppm - 2.3 ppm)


Bo.D = ( 300 - 9.2 ppm + 1 ppm = 512 ppm
4 ml - 1 ml
Some problems in Bo.D analysis can result from insufficient seed bacteria
and/or excessive loading. The volumes of the samples used can be increased
for lighter waste loads and decreased for heavier loading. Also, the original
sample can be diluted and a factor applied to the final result. The pounds Bo.D
can be calculated by using:

P _ (Bo.D ) (453.6 g) (8.322 lb) ( 1 lb ) ( al)


BOD - ppm lb gal water 453.6 X 106 IJ-g g
(22-6)
362 CITRUS JUICE BY -PRODUCTS

-
6

E
Q. 5
.s
0 4
C

1
0
0 2 3 4 5
mls of sample
Fig_ 22-1. Plot of DO (ppm) of incubated BOD wastewater samples versus milliliters of sample
used in the sample BOD problem.

or:

(22-7)

For example:

(512ppmBOD) (8.322 x 10- 6 ) (50,000 gal) = 213 lb BOD

Even though BOD values give the amount of oxygen needed to aerobically
treat waste water, the analysis is time-consuming, requiring 5 days for comple-
tion. A more rapid method that can be used to estimate the BOD is the chemical
oxygen demand (COD). The COD can be measured in about 3 hours and pro-
vides for a good estimate of the BOD. Generally, BOD values range from 60
to 65 % of the COD values. In the COD determination, the organic material is
oxidized by the acid-catalyzed oxidizing agent potassium dichromate. After in-
cubation, the unreacted dichromate is titrated with a solution of ferrous am-
monium sulfate, which produces a greenish color. The endpoint is determined
by using a ferro in indicator, which reacts with excess ferrous ion to form a red
complex. The appearance of this red complex marks the end of the titration.
WASTES FROM CITRUS PLANTS 363

The chemical reactions involved in the titration are as follows:

CrlO~- + 14H+ + 6Fe1 + -> 6Fe3+ + 2C~+ + 7H 1 0 (22-8)


dichromate sulfuric ferrous chromic
(orange) acid ammonium ion
sulfate (green)

Fe2+ + (PhhFe3+ -> (PhhFe2+ + Fe3+ (22-9)


ferrous ferroin (red)
ammonium (colorless)
sulfate

COD kits are commercially available and are recommended. These kits in-
volve less chemical handling and are faster and safer to use than the method
below. In the absence of such kits, the following procedure can be used.

COD Test

Equipment and Supplies

• Three 100 ml volumetric flasks.


• 5 ml pipette.
• 10 ml pipette.
• 20 ml pipette.
• Three 200 ml + boiling flasks with water-cooled condensers attached for
refluxing each flask.
• Heat source to boil samples.
• Distilled water.
• 90 ml of 97.2 % sulfuric acid.
• 50 ml buret and magnetic stirrer.
• K1Cr207 solution. (Heat crystalline K2CrZ07 at 108°C for 2 hours to re-
move hydrated water. Cool it in a desiccator, and dissolve 12.259 g in
distilled water in a I-liter volumetric flask filled to the mark with distilled
water.)
• Ferrous ammonium sulfate solution (Dissolve about 39 g of Fe(NH 4hS04
. 6H zO in about 100 ml of distilled water. Add 20 ml of the concentrated
sulfuric acid and cool. Dilute the solution to 1 liter. The solution is stan-
dardized in the procedure.)
• Ferroin indicator. (Dissolve 1.591 g of 1, lO-phenanthroline monohydrate
together with 0.695 g of FeS04 . 7H20 in distilled water, and dilute the
solution to 100 ml.)
• One flask for the first blank.
• 50 ml graduated cylinder.
364 CITRUS JUICE BY-PRODUCTS

Procedure

1. Pipette 5 ml of the stirred waste water sample into a 100 ml volumetric


flask, and fill it to the mark with distilled water. More than one sample
can be run at one time by using the same two blanks (see below) in the
procedure.
2. Pipette 5 ml from each volumetric flask containing a diluted sample into
a boiling flask fitted with a condenser for refluxing. Add about 15 ml of
distilled water to each boiling flask. Make a blank solution by adding 20
ml of distilled water to a separate boiling flask to constitute the first blank.
3. Pipette 10 ml of the dichromate solution into each flask as well as into an
empty container to serve as a second blank. Fill the second blank up to
about 100 ml. This blank will be used to standardize the FAS solution.
4. Add about 30 ml of the sulfuric acid to each flask, including the blanks,
using a graduated cylinder. Be careful not to get any of the acid on your
skin or clothing. If you do, wash the area with water for 15 minutes.
5. Heat the flasks to boiling, and reflux them for 2 hours.
6. Cool the flasks to room temperature, and titrate each solution with the
ferrous ammonium sulfate solution. The solution will begin to tum green
with the production of the chromic ion, and then it will tum blue. At this
point 3 drops of the ferroin indicator should be added. Just before the
endpoint the solution will tum gray, and then the final development of a
red color will indicate the endpoint.
7. The normality of the ferrous ammonium sulfate solution is determined by
titrating the second blank, and is calculated as follows:

N FAS = (10 ml dichrm) (0.25N dichrm)/(ml FAS titrd) (22-10)

8. The COD is calculated as follows:

COD = (NFAs ) (8000) (ml FASlstblank - ml FASsample) (22-11)


(0.5 ml of sample)

For example:

N FAS = (10 ml)(0.25N)/(25.00 ml FAS2ndblank) = O.l00N

COD = (0. lOON FAS) (8000) (28.30 mllstblank - 24.32 mlsample)


(0.5 ml of sample)
= 6368 ppm

9. Using the COD to estimate the BOD, you can multiply by 65% or 0.65
to get 4139 ppm BOD in the example.
WASTES FROM CITRUS PLANTS 365

The amount of settleable solids is another important parameter in aerobic


treatment. Once the aerobic microbes have incorporated soluble material into
their bodies, they become more dense than the solution and can be settled out
and be removed from it. The level of settleable solids in the water stream prior
to aerobic treatment can affect the efficiency of the microbial digestion, as well
as the settleable solids loading in the clarifying ponds or tanks. Clarifiers should
be designed for about 2 hours of retention time with 5 to 10% settleable solids
in the sludge slurry being removed, depending on the type of pump used. This
sludge can be dewatered by using centrifuges or filters, and added to the feed-
mill; it is higher in nitrogen and vitamin B than citrus pulp and thus adds to the
nutritional value of the feed. DAF and/or lime addition sometimes is used to
aid in the separation of the sludge in the clarifier. Some of the sludge may be
recirculated back into the aeration lagoon or chamber to stabilize the micobial
activity.
Aerobic flora and fauna have the ability to adjust to a wide variety of con-
ditions as long as changes are slow enough to permit adaptation. If citrus ef-
fluents are the major wastes being treated, it may be possible to generate mi-
crobes that are pH- and oil-tolerant, which could reduce the need for some of
the pretreatment. Gradually reducing pretreatment operations may make it pos-
sible eventually to eliminate them all together.

Anaerobic Treatment

Primary anaerobic treatment of citrus processing effluents is not a common prac-


tice, one reason for this being the toxic effect of the peel oils on anaerobic
bacteria. The big advantage of anaerobic primary treatment is the recovery of
methane gas, a microbial by-product, which can be used as a fuel for boilers
and peel dryers. Assuming that the waste streams can be sufficiently stripped
of d-limonene, an anaerobic digester can reduce the BOD by 90%, producing
gas that is 60 to 70% methane, and can generate about 6000 Btu's per pound
of COD removed. Less sludge is produced in anaerobic treatment compared to
aerobic treatment, with about 0.02 to 0.10 pounds sludge produced per pound
of BOD removed.
Activated charcoal or sand often is used in the reactor as a site for bacterial
growth in fluidized-bed sealed reactors. As in aerobic treatment, some of the
sludge can be recycled back into the reaction chamber in order to maintain
reactivity. Precautions must be taken in anaerobic primary treatment to keep
the gases and odors that are generated from escaping into the atmosphere, as
they can cause environmental problems. Also, some of the anaerobes produce
volatile acids that can lower the pH and thus inhibit anaerobic activity. Buff-
ering agents can be used to modify the pH (such as bicarbonate). As with aero-
bic methods, gradual changes in effluents can allow anaerobic flora and fauna
366 CITRUS JUICE BY-PRODUCTS

to adapt to low-pH and high-peel-oil conditions that can reduce the need for
pretreatment.
Anaerobic treatment also is used as a secondary treatment in aerobic methods
to remove those contaminates that aerobic treatment could not remove, espe-
cially volatile organics. Carbon granules sometimes are added to help absorb
volatile organics as well as to provide a site for anaerobic growth. Sludge pro-
duced in this secondary treatment generally needs to be disposed of in a remote
site in order to prevent off odors from lowering the quality of feed coming from
the feedmill. However, as mentioned above, less sludge is produced with an-
aerobic treatment than with aerobic treatment. After secondary anaerobic treat-
ment, a tertiary chemical oxidation may be employed, using chlorine gas to
remove remaining organics and nitrogenous compounds. A final carbon filter,
used to remove residual chlorine gas and volatile organics, generally will pro-
duce potable water that usually is of a higher quality than that used by the plant
from other sources.

Reverse Osmosis

The process of high pressure filtration (about 800 psi) through semipermeable
membranes has been investigated in the treatment of citrus effluents (Kimball
1982). This method, using both cellulose acetate membranes and non-cellulose
acetate membranes, can reduce COD levels by about 75 %. The filtered per-
meate can undergo further processing or may be recycled as belt sprays or in
other suitable applications. About 10% of the original volume of the untreated
waste water will emerge as a concentrate with the Brix increased about fourfold
(-0.5°Brix untreated to -2.0oBrix treated), which can be added to press li-
quor and can be concentrated to molasses and added back to the feed in the
feedmill. About half of the peel oil can be removed from the waste stream as
well, by using reverse osmosis. This method requires frequent cleaning and
durable membranes.

HAZARDOUS WASTES

Hazardous wastes may be defined as substances that can ignite, corrode, react
in a dangerous manner, or be toxic. Citrus juice plants utilize materials such as
cleaning agents, lubricants, fuels, refrigerants, boiler treatment chemicals, pro-
cessing chemicals, compressed gases, and laboratory chemicals that fall into
this category. Whenever these chemicals are spilled, contaminated, or decom-
pose, they become waste material that must be properly disposed of by using
licensed disposal services. Empty containers that contained hazardous material
also must be disposed of in proper fashion, according to local laws. Empty
WASTES FROM CITRUS PLANTS 367

caustic containers can be triple-rinsed to render them safe in most areas. Empty
closed-head oil or solvent drums that contained flammable material should never
be opened with a torch. Most chemical suppliers will pick up used drums or
partially used drums that contained hazardous materials for recycle. Empty con-
tainers (generally over 5 gallons) should never by simply discarded, with no
regard for proper and legal disposal requirements. Care should be taken in the
disposal of hazardous chemicals from laboratories. Direct disposal of such
chemicals down the drain, so that they end up in municipal treatment plants,
may cause a hazardous condition. Used compressed gas cylinders should be
promptly returned to the vendor and not allowed to accumulate. When food
containers are used for nonfood purposes, they should be labeled as such and
not used to contain food material again.

QUESTIONS

1. What are some of the sources of air pollution in citrus processing plants?
2. What is the "total sulfur oxides" maximum level permitted by EPA in
ambient air during a 24-hour period?
3. Why should inert solid wastes be removed from plant sites?
4. How can DAF aid in the treatment of aqueous citrus plant effluents?
5. How many pounds of BOD/acre day can Florida's sandy soils receive,
according to text?
6. What is the advantage of aerobic treatment?
7. What are the quality control parameters of aerobic treatment?
8. What DO levels must be maintained in aerobic treatment?
9. What maximum peel oil content is permissible for successful aerobic
treatment?
10. What is the advantage of COD measurements over BOD measurements?

PROBLEMS

1. Suppose that daily samples of waste water were collected for 5 days, as listed below,
corresponding to the given daily meter readings for gallons of effluent. How would
you make 200 ml of a weekly composite that would represent the week's effluent?
Monday: 61,452 gallons
Tuesday: 85,967 gallons
Wednesday: 31,002 gallons
Thursday: 46,972 gallons
Friday: 55,012 gallons
2. In air calibration of an oxygen meter, what would you set the meter to if you were
at an altitude of about 1600 feet at a temperature of 28°C?
368 CITRUS JUICE BY-PRODUCTS

3. Suppose you obtained the following data in a BOD analysis. What would be the BOD
(ppm)?

DO
Initial sample 1. 6
After incubation using:
I ml of sample 6.5
2 ml of sample 4.0
3 ml of sample 1.6
4 ml of sample 0.0
5 ml of sample 0.0

4. Suppose we obtained the following data in COD a analysis. What would be the COD
(ppm) and the estimated BOD (ppm)?
29.27 ml FAS titrated in 2nd blank
25.60 ml FAS titrated in 1st blank
24.78 ml FAS titrated in sample
5. How many estimated pounds of BOD are there in 156,472 gallons of waste water
with a COD value of 4367 ppm?

REFERENCES

Kimball, D. A. 1981. Unpublished data. California Citrus Producers, Inc., Lindsay, Calif.
Kimball, D. A. 1982. Unpublished data. California Citrus Producers, Inc., Lindsay, Calif.
McNary, R. R., Wolford, R. W., and Patton, V. D. 1951. Experimental treatment of citrus waste
water, Food Tech., 8, 319-323.
Murdock, D. I. and Allen, W. E. 1960. Germicidal effect of orange peel oil and d-limonene in
water and orange juice, Food Tech., 14, 441-445.
Perry, R. H. and Green, D. 1984. Perry's Chemical Engineer's Handbook, 6th edition. McGraw-
Hill Book Company, New York, 26.11.
Ratcliff, M. W. 1974. Unpublished research. Citrus World, Lake Wales, Fla.
Wheeler, R. W. 1977. Unpublished communication. FMC, Riverside, Calif.
Wood, C. 1973. Recycling citrus waste water, Sunshine State Agr., September-October, 6-7.
Chapter 23

Quality Control Statistics

Quality control of any product inherently involves the use of statistical methods.
Statistical mathematics is used to evaluate parameters that cannot be determined
absolutely. For example, it would be impossible to determine the precise di-
acetyl level in chilled juice being processed and packaged continuously from
fresh extracted fruit, as the juice composition is constantly undergoing change.
However, statistical or spot checking could give a good indication of what the
quality would be. Although the field of statistics is broad, only a few techniques
that may be of use to quality control personnel in citrus processing plants are
discussed here.

SIGNIFICANT FIGURES

Errors in regard to significant figures often occur in the citrus industry. Often
labels are encountered with Brix readings to two decimal places, or acid levels
are reported to one decimal place. The subject of significant figures is one of
the first studied in science classes, as the number of significant figures repre-
sents a way to show the accuracy of a measurement. For example, if we report
the milliliters titrated as 23, do we mean exactly 23 ml or 23 ± 0.5 ml? Ac-
cording to the rules of significant figures, the latter is true. If exactly 23 ml is
intended, we should write 23.0 or 23.00, depending on the accuracy of the
measurement. The reading of a standard buret generally is ±0.02 ml, which
means that all buret readings should be expressed to the hundredths decimal
place. Using the proper number of significant figures should not replace the
need to express error ranges. If we were to report the milliliters titrated as
23.234, we would be implying that we could make the measurement accurate
to the thousandths decimal place, which would be false. On the other hand, if
we were to report the milliliters titrated as 23.4, we would not be reporting the
accuracy of the measurement as close by as we could. A 23.4 ml reading really
means 23.4 ± 0.05 ml, whereas 23.40 means exactly 23.40 ml or 23.40 ±
0.005.

371

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
372 CITRUS JUICE MANAGEMENT

The number of significant figures in a measurement or in raw data is deter-


mined by the assigned accuracy of the measurement. When the data are pro-
cessed, however, there are nine rules that can be used to determine the number
of significant figures in an answer after calculations have been made. Significant
figures are basically those figures that add accuracy or quantify a number; fig-
ures that are not significant are generally place holders and do not define the
quantity or accuracy of the number directly. The nine rules of significant figures
are as follows:

1. All nonzero figures are significant. For example, 123.45 = five significant
figures.
2. All zeros between nonzero figures are significant. For example, 3,076,002
= eight significant figures.
3. All zeros to the left of the first nonzero figure are not significant. For
example, 0.013 = two significant figures.
4. All zeros to the right of the last nonzero figure and to the right of the
decimal point are significant. For example, 3.2300 = five significant fig-
ures.
5. All zeros to the right of the last nonzero figure and to the left of the
decimal point mayor may not be significant. If the decimal point appears
(expressed decimal), then the zeros are significant. For example, 3700 =
two, three, or four significant figures, but 3700. = four significant fig-
ures.
6. Use scientific notation, when in doubt, to clarify the proper number of
significant figures in rule 5. For example, 3700 can be expressed as 3.700
X 103 , 3.70 X 103 , or 3.7 X 103 to indicate the exact number of intended
significant figures.
7. Some numbers have unlimited significant figures. For example, 5 people
means exactly 5 people because it generally is impossible to have a partial
person. In other words 5 people is the same as 5.0000000000000000000
people. Also, 60 seconds in one hour means the same as 60.00000000
seconds in one hour because exactly 60 seconds are in one hour. Absolute
or exact numbers have an unlimited number of significant figures.
8. When one is adding or subtracting numbers, the answer can be expressed
only to the number of significant figures that are completely known. To
begin with, one can insert any necessary zeros needed in the calculation
and then must round off to the nearest fully known figure. For example,
if we add or subtract the following:
25.3? 3455.346
+3.45 -321.1 ??
28.75 3134.246
or 28.8? 3134.2??
QUALITY CONTROL STATISTICS 373

The last figure(s) in the answer are not known for certain. Rounding off
to the nearest known figures would give 28.8 and 3134.2 for the answers
expressed to the correct number of significant figures. The least accurate
data determine the number of significant figures in the answer.
9. When one is multiplying or dividing, the total number of significant fig-
ures in the answer can be no more than the least number of significant
figures in the numbers multiplied or divided. For example, if we multi-
plied 34.56789 by 0.023, we would get an answer of 0.80. This is so
because even though the first number has seven significant figures, the
number with the least significant figures has only two. Thus, the answer
can have only two significant figures. In dividing 6.234 by 3.45633567,
we would get 1.804 because the least number of significant figures in the
data is four.

Most data reported in routine quality control measurements should be ex-


pressed to the proper number of significant figures. The most common param-
eter in citrus processing is the Brix measurement, whose standard error range
is ±0.1 °Brix. Thus Brix readings should be reported rounded off to the nearest
tenth of a °Brix; but because acid and temperature corrections often are deter-
mined to the hundredths decimal place, many processors report their Brix values
to the hundredths decimal place as well. This is incorrect according to the rules
of significant figures; such reporting implies deceptive accuracy in measure-
ment. Generally reports of oil levels give significant figures to the thousandths
of a percent, which is generally correct because all the data used have at least
two significant figures, and oil levels usually are expressed in two significant
figures (0.011 %, 0.025 %, etc.). However, oil levels below 0.010% usually
are expressed as one significant figure (0.009 %, 0.003 %, etc.), a practice that
technically violates the rules of significant figures. However, it is convenient
in the industry to use a standard decimal place and this practice has overridden
the rules of significant figures. The same condition applies to pulp levels. The
rules of significant figures dictate that a centrifuge tube can be read to ±0.2 ml
in measurements ranging from 0.2 ml to 9.0 ml; so the number of significant
figures can be one or two. The number of milliliters of pulp in the centrifuge
tube determines the number of significant figures in the final pulp level. Most
pulp levels are expressed as two significant figures (9.4 %, 8.1 %, etc.), but
pulp levels of 10% or more generally are expressed with three significant figures
00.4%,11.6%, etc.), a convention that is technically incorrect. Again, the
need of the industry to have a consistent number of decimal places has overrid-
den the rules of significant figures. Computers and calculators always disregard
rules of significant figures, and their use in the industry has led to the need to
use standard decimal places in reporting data.
374 CITRUS JUICE MANAGEMENT

ERROR ANALYSIS

The expression of error is an inherent part of any precise science. All measure-
ments contain error, regardless of the effort or care exercised to avoid or min-
imize such. Error can be reported in many ways, including the following four
ways in which the error range can be expressed.

Actual Range

The simplest expression is the actual error range (AR). For example, if we have
three acid determinations of 3.41 %, 3.48 %, and 3.49 %, we can say the range
is between 3.41 and 3.49. This type of error analysis does not take into consid-
eration the fact that two of the three data points are close together with the third
somewhat distant from the others. It is useful for bracketing data within groups
of absolute occurrence, however. Mathematically it can be expressed as:

AR = Xmax - X min

Average Deviation

The average deviation, (AD) is calculated by averaging the deviation from either
the average value or the median value. (The median value is the value exactly
midway between the two extremes.) In the acid example above, the median
value would be 3.45 % and the average 3.46 %. In calculating the average de-
viation, the average difference from the median is the preferred method, rather
than the difference from the average value. In our example this would be:

(13.45 - 3.411 + 13.45 - 3.481 + 13.45 - 3.491 )/3 = 0.04%

Mathematically this could be expressed as follows:

(23-1 )

with Xm representing the median and Xi the ith component of n components.


The average deviation is easily used for small samples. However, the absolute
values are hard to use in mathematical analysis and can be seriously affected by
extreme variations.

Root Mean Square Deviation

The square root of the average of the squared deviations from the mean is called
the root mean square deviation (RMSD). It can be calculated by using the fol-
QUALITY CONTROL STATISTICS 375

lowing expression:

(23-2)

This is similar to the average deviation except that one does not need to deal
with absolute values. However, the RMSD has an inherent bias and so is not
commonly used.

Standard Deviation

The standard deviation (SD) is the most commonly used means of determining
the error range of data. It is similar to the RMSD except that it eliminates the
inherent bias by multiplying the RMSD by the factor .In / (n - l). The SD can
be expressed as:

(23-3 )

For example, in our acid example, the SD would be:

~( (3.41 - 3.46/ + (3.48 - 3.46/ + (3.49 - 3.46)2)/(3 - 1) = 0.04

The above equation requires calculation of the data mean (Xm). A more con-
venient form of the equation, which does not require the calculation of the
mean, is:

In the % acid example, this would become:

~[3(35.92) - (10.38/]/3(2) = 0.05

You will notice that the above answer is given to only one significant figure.
This is done because the % acid data is reported to the hundredths place; the
error range is reported likewise. Otherwise, if the error range were reported to
the proper number of significant figures (four here), it would appear to be more
accurate than the original data, which is not the case. Also, more accurate re-
sults are obtained if one does not round off the summations or any intermediate
answer until the final error range. If this practice had been followed, we would
have obtained a standard deviation of 0.04 instead of 0.05, using 35.9186 for
the first summation instead of 35.92. The former (0.04) is the more accurate
376 CITRUS JUICE MANAGEMENT

standard deviation, as seen in the use of Equation 23-3 with the sample data.
The calculation of standard deviations is a built-in feature of many calculators
and computers.

CONTROL CHARTS

Control charts have been used to monitor on-line quality throughout the food
industry. A control chart consists of upper and lower allowable limits, depicted
on graph paper as shown in Fig. 23-1. The actual levels of the target parameter
are plotted in relation to these limits to determine not only if the product is
within specifications, but if undesirable trends are developing.
The median value and limits of control charts are determined mathematically
by statisticians. Often, however, in the food industry, the upper and/or lower
limits are determined by specification or quality thresholds and limits. For ex-
ample, the maximum level of diacetyl acceptable in citrus juices is determined
by the taste threshold and not by the probability of finding a diacetyllevel more
than 95 % away from the mean value. This absolute nature of quality in food
processing requires changes in the interpretation of quality control charts.

Runs

A run on a control chart is a consecutive series of plots that are on the same
side of the median value. Runs found above the median value are called' 'runs
up" and those below the median value "runs down." Long runs that consist
of many consecutive points are indicative of a trend, and such trends may result
in the product drifting out of specifications if not corrected. The use of control
charts enables quality control personnel to detect such trends early enough to

Upper Limit

Lower Limit

TIME---...
Fig. 23-1. A typical control chart, including the median and upper and lower control limits.
QUALITY CONTROL STATISTICS 377

correct them before the product is seriously damaged or contaminated. The


statistical determination of excessive runs or runs that cannot be described to
random occurrence is very simple. The following table shows the total number
of data points and the corresponding maximum number of points in a consec-
utive run (up or down) that can be considered random or acceptable statistically
at the 0.05 probability level:

Total data points Maximum points in a run


10 5
20 7
30 8
40 9
50 10

For example, if we made 30 measurements of % pulp from line or freshly


extracted juice, we could have up to 8 pulp levels above (or below) the generally
accepted median of 10.0% pulp consecutively before we could attribute the run
to a nonrandom effect in processing. In this case, the main adjustable processing
parameter in pulp levels is the finisher pressure. If more than 8 pulp levels are
above 10% pulp, then the finisher pressure is too high and should be decreased
to avoid a drift of pulp levels perhaps out of specification. If more than 8 pulp
levels are below the 10% median, then the finisher pressure should be increased
to avoid loss of juice yield with expelled unwashed pulp. Some quality control
engineers use 7 as a standard maximum length of runs before corrective action
is taken, regardless of the number of total data points.

Applications

Quality control charts have been used in the monitoring of the diacetyl levels
in single-strength juice products and pulp levels during juice extraction, and
some attempt has been made to apply the use of control charts to fruit grading.
In the production of single-strength juices, if the diacetyl values constitute a
run up, spoilage is setting in, and the temperatures and/or retention times in the
pasteurizers need to be increased. If the diacetyl values form a run down, too
much heat may have been applied, and perhaps the pasteurizer temperature and/
or retention time should be reduced. The example of % pulp monitoring given
above is another illustration of the application of control charts to citrus pro-
cessing. One can monitor fruit graders by taking counts of broken and rotten
fruit leaving the grading table and plotting the results on a control chart. The
upper limits of fruit grading have been established by the USDA-1O% for
broken fruit and 2 % for rotten fruit leaving the grading table. The establishment
of a median value will permit the detection of runs up, which would require the
use of more graders or grading activity, or runs down, which would allow the
378 CITRUS JUICE MANAGEMENT

use of fewer graders or less grading activity. Control charts can be used for
packaging equipment, sample monitoring, and many other applications in con-
tinuous processing.

ANALYSIS OF VARIANCE

It may be of interest to the quality control manager or technician to know whether


or not something is significantly different from something else; and many tech-
niques can be used to determine whether or not a statistically significant change
has occured. One method, where a large number of samples (> 30) exists, is
to convert the data to a standard normal frequency distribution and apply sta-
tistical methods to determine whether the data are significantly different from
each other or a set parameter. Such large samplings of a single lot are not
common in industrial practice, however, and other restrictions on the method
generally prohibit use of the technique on a commercial basis. A Student's t-test
is used in a similar manner for small samples ( < 30) and may be of more value
than the former method to commercial citrus plants. A chi-square test deter-
mines the significant variance in standard deviations, and an F-test determines
the significant difference between two variances. However, an analysis of
variance (A NOV A) is ideally suited for most industrial quality control deter-
minations of the significance of the difference among data and can be used as
a general method.
ANOV A uses an F-distribution where a significant variance is said to occur
if the test statistic (F value) falls beyond the 95 % critical value. In other words,
if the data exist beyond 95 % of the frequency distribution, a significant differ-
ence can be assumed. If such is the case, it is said that the variance is significant
at the 0.05 level. For example, suppose that three technicians are performing
Brix measurements, and you notice that there seems to be a difference in their
readings but are not sure if there is a difference and why that difference is
occurring. In order to find out, you can ask all three technicians to analyze each
of 10 samples of orange juice concentrate. The answers that you are given
probably will show some differences. Are these differences due to the lab tech-
nician or perhaps the samples of concentrate? Are these differences significant?
You can find out by using an analysis of variance. Such an analysis tests what
is called the null hypothesis, or the hypothesis that no difference exists. The
limits of the null hypothesis are expressed in terms of probability limits or lev-
els. If there is a certain probability that the differences can lie outside a certain
range, then the difference is statistically significant. As mentioned above, a
common probability of 5% or 0.05 is used as the critical value to determine the
acceptance or rejection of the null hypothesis.
We can illustrate the use of an analysis of variance through an example.
QUALITY CONTROL STATISTICS 379

Suppose that three technicians measure the Brix on three samples of concentrate
as shown in the table:

Tech A Tech B Tech C


Sample 1 61.2 61.4 60.8
Sample 2 61.3 61.0 60.9
Sample 3 60.9 61.2 60.9

Using a one-way analysis of variance, we will try to determine if there is a


significant difference between the results from each technician, or if one tech-
nician significantly varies from another. First, we can simplify our calculations;
by subtracting 60.0 from each of the numbers, we get:

Tech A Tech B Tech C


Sample 1 1.2 1.4 0.8
Sample 2 1.3 1.0 0.9
Sample 3 0.9 1.2 0.9

Then the following procedure can be used:

1. Sum each column, square the sum, add the squares, and divide by the
number of items in each column. For example:
2 2 2
(1.2 + 1.3 + 0.9) + (1.4 + 1.0 + 1.2) + (0.8 + 0.9 + 0.9)
3
= 10.43

2. Square each number, and add the results. For example:


2 2 2 2 2 2
(1.2) + (1.3) + (0.9) + (1.4) + (1.0) + (1.2)
+ (0.8)2 + (0.9)2 + (0.9) = 10.60

3. Sum all the items, square the sum, and divide by the total number of
items. For example:

(1.2 + 1.3 + 0.9 + 1.4 + 1.0 + 1.2 + 0.8 + 0.9 + 0.9/


10.24
9

4. Subtract the results in (3) from the results in (1). For example:

(1) - (3) = 10.43 - 10.24 = 0.19


380 CITRUS JUICE MANAGEMENT

5. Subract the results in (3) from (2). For example:

(2) - (3) = 10.60 - 10.24 = 0.36

6. Subtract the results in (4) from those in (5). For example:

(5) - (4) = 0.36 - 0.19 = 0.17

With this information we can construct an analysis of variance table. The


sum of squares for the columns is found from step 4 above. The sum of squares
for the columns is found from step 4 above. The sum of squares for the residual
error is found from step 6 above. The degrees of freedom (df) for the columns
is found by taking the number of columns (c) and subtracting I, or c - 1. The
degrees of freedom for the residual error is found from c (r - 1), where r is
the number of rows or Brix tests per technician. The mean square is found by
dividing the sum of the squares by the degrees of freedom. The variance ratio
then can be found by dividing the mean square of the columns by the mean
square of the residual error. For example:

Source Sum of squares df Mean square Variance ratio


columns 0.19 2 0.10 3.33
residual 0.17 6 0.03

The variance ratio can be compared to Table 23-1, where VI equals the de-
grees of freedom for the columns, and V2 equals the degrees of freedom of the
residual. At the 0.05 probability level, the variance ratio must exceed 5.14 in
order for a significant difference to occur between the lab technicians. Because

Table 23-1. F-distribution that can be used in the analysis of


variance to test the null hypothesis at the p = 0.05 level
(Duncan 1974).
V2 VI = I 2 3 4 5 6 7 8 9 10
161 200 216 225 230 234 237 239 241 242
2 18.5 19.0 19.2 19.2 19.3 19.3 19.4 19.4 19.4 19.4
3 10.1 9.55 9.28 9.12 9.01 8.94 8.89 8.85 8.81 8.79
4 7.71 6.94 6.59 6.39 6.26 6.16 6.09 6.04 6.00 5.96
5 6.61 5.79 5.41 5.19 5.05 4.95 4.88 4.82 4.77 4.47
6 5.99 5.14 4.76 4.53 4.39 4.28 4.21 4.15 4.10 4.06
7 5.59 4.47 4.35 4.12 3.97 3.87 3.79 3.73 3.68 3.64
8 5.32 4.46 4.07 3.84 3.69 3.58 3.50 3.44 3.39 3.35
9 5.12 4.26 3.86 3.63 3.48 3.37 3.29 3.23 3.18 3.14
10 4.96 4.10 3.71 3.48 3.33 3.22 3.14 3.07 3.02 2.98
QUALITY CONTROL STATISTICS 381

3.33 is less than 5.14, we fail to reject the null hypothesis, which means there
is no significant difference between the lab technicians' from a statistical point
of view. That is not to say that the lab technicians are performing the Brix
measurements with sufficient accuracy; it only means that statistically they are
all performing equally at the 5 % level.
We can expand the analysis of variance to include the determination of
whether or not there is a significant difference between the concentrate samples
as well as between the lab technicians. This is called a two-way ANOVA. We
use a similar example to illustrate how this is done. Suppose that four lab tech-
nicians each analyze three samples of orange concentrate for Brix, as shown
below:

Tech A Tech B Tech C Tech D


Sample 1 60.0 60.1 59.9 59.9
Sample 2 60.1 60.1 60.1 60.0
Sample 3 60.1 60.2 60.1 60.0

First, subtract 60.0 from each of the measurements in order to simplify the
calculations:

Tech A Tech B Tech C Tech D


Sample 1 o 0.1 -0.1 -0.1
Sample 2 0.1 0.1 0.1 o
Sample 3 0.1 0.2 0.1 o

The following procedure can be used:

1. Sum each column, square the sums, add the results, and divide by the
number of cases in each column. For example:

((0.2/ + (0.4)2 + (0.1)2 + (-0.1)2)/3 = 0.073

2. Sum each row, square the sums, add the results, and divide by the number
of cases in each row. For example:

( ( - O. 1 )2 + (0.3 / + (0.4) 2) /4 = 0.065

3. Square each number, and add the squares. For example:


2 2 2 2 2 2
0+(0.1) +(-0.1) +(-0.1) +(0.1) +(0.1) +(0.1) +0
+ (0.1)2 + (0.2)2 + (0.1)2 + 0 = 0.120
382 CITRUS JUICE MANAGEMENT

4. Sum all the cases, square the sum, and divide by the number of cases.
For example:

(0 + 0.1 - 0.1 - 0.1 + 0.1 + 0.1 + 0.1 + 0 + 0.1 + 0.2 + 0.1


+ 0)2/ 12 = 0.030
5. Subtract the results in (4) from those in (1). For example:

(1) - (4) = 0.073 - 0.030 = 0.043

6. Subtract the results in (4) from those in (2). For example:

(2) - (4) = 0.065 - 0.030 = 0.035

7. Subtract the results in (4) from those in (3). For example:

(3) - (4) = 0.120 - 0.030 = 0.090

8. Subtract the results in (5) and (6) from (7). For example:

(7) - (5) - (6) = 0.090 - 0.043 - 0.035 = 0.012

With this information we can construct an analysis of variance table. The


sum of squares for the columns is found from step 5 above. The sum of squares
for the rows is found from step 6 above. The sum of squares for the residual
error is found from step 8 above. The degrees of freedom for the columns is
found from c - 1. The degrees of freedom for the rows is found from r - 1.
The degrees of freedom for the residual error is found from (r - 1) (c - 1).
The mean square is found by dividing the sum of the squares by the degrees of
freedom. The variance ratio then can be found for both the rows and the col-
umns by dividing the mean square of the columns and rows by the mean square
of the residual error. For example:

Source Sum of squares df Mean square Variance ratio


columns 0.043 3 0.014 7.00
rows 0.035 2 0.018 9.00
residual 0.012 6 0.002

The variance ratios can be compared to Table 23-1, where VI equals the
degrees of freedom for the columns or rows, and V2 equals the degree of free-
dom of the residual. At the 0.05 probability level the variance ratio must exceed
4.76 for the columns and 5.14 for the rows in order for a significant difference
QUALITY CONTROL STATISTICS 383

to occur between the lab technicians or the samples of concentrate. As both


ratios are more than 4.76 or 5.14, there is a significant difference between the
lab technicians and the samples of concentrate from a statistical point of view.
As you may see, this difference is not obvious by inspection.

REGRESSION

Regression analysis involves the fitting of data to mathematical relationships,


which then can be used for a variety of quality control functions, including the
prediction of results. If, for example, a relationship can be found between the
pulp levels before and after freshly extracted juice has passed through a seven-
effect TASTE evaporator, then this relationship can be used to predict the pulp
level change under similar conditions. Another common use of regression anal-
ysis is the conversion of data into a form that can easily be placed into a pro-
grammable device such as a calculator, computer, bar code system, or auto-
mated processing controls. This was done with sucrose Brix/density tables and
Brix corrections that have been used extensively in this text.
Regression analysis simply means fitting a line or a curve to data points plot-
ted on a graph. This can be done by simply drawing a line or a curve by eye or
by seeking a somewhat simple mathematical relationship that may be made
somewhat obvious by the data; however, a statistical procedure exists that en-
ables the calculation of such relationships as well as an objective means of
determining the validity of such relationships. This method is called the method
of least squares.

Least Squares Analysis

Least squares analysis involves the use of differential calculus in determining


the equation that best fits a set of data. However, once the relationships have
been established, computers can be easily programmed to handle the bulk of
the calculations. The simplest example is determining the best equation for a
straight line that fits the data, of y = a + bx. Here b is the slope of the line,
and a is the y-intercept. In order to find the best values of a and b that will fit
the data, we must sum the squares of the differences between the actual y values
and the predicted or yp values:
yp = a + bx (23-4 )

2:(y - yp)2 = 2:(y - a - bX)2 = D (23-5 )

The best a and b values are those obtained when this sum of the squares is at a
minimum. In order to find the minimum point on this equation, we can try to
find the point where the slope is zero. This we can do by partially differentiating
384 CITRUS JUICE MANAGEMENT

Equation 23-5 with respect to each coefficient, and setting the result equal to
zero:

aD/aa = L; 2(y - a - bx)( -I} = 0 (23-6)


aD / ab = L; 2 (y - a - bx) ( -x) = 0 (23-7)

Rearranging the above equations gives:

an+bL;x=L;y (23-8 )
a L; x + b L; x 2 = L;xy (23-9)

This gives two equations that can be used to find the two unknowns a and b,
where n is the number of (x, y) data pairs used in the analysis. Using Equations
23-8 and 23-9 to solve for a and b, we obtain the following:

L; x 2 L; Y - L; x L; xy
(23-1O)
Y
a=
n L; x 2 - (L; x

n L;xy - (L;x L;y)


b = 2 (23-11 )
nL; x 2 - (L; x)
each of which is an independent equation. The equation for a can be simplified
by first calculating b and then using the following dependent equation:

a = Yavg - bXavg (23-12 )

Thus, using these two equations, we can calculate the best values for the con-
stants a and b by performing the above summations, using the sample data
points x and y and the number of data pairs n.
For example, suppose we were interested in finding a linear equation that
would best describe the change of pulp level in freshly extracted orange juice
before and after evapomtion to 65°Brix. We first obtain the following data:

Sample % Pulp before evap. (x) % Pulp after evap. (y)


16.5 10.6
2 15.9 8.8
3 16.9 10.5
4 17.4 11.4
5 18.6 11.7
QUALITY CONTROL STATISTICS 385

U sing Equations 23-10 and 23-11, we obtain the following parameters and the
resulting best a and b values:

:6 x = 85.3 a = -6.21
:6 y = 53.0
:6 x 2 = 1459.4 b = 0.985
:6 xy = 908.3
We can make a statistical prediction of pulp levels before and after evaporation
using the resulting equation:

% pulPafter = 0.985 (% pulPbefore) - 6.21 (23-13 )

Using this equation we can calculate predicted values and compare them to the
actual values:

Measured % pulp after evap. Calculated % pulp after evap.


10.6 10.0
8.8 9.5
10.5 10.4
11.4 10.9
11.7 12.1

This is a simple way to check the accuracy of the linear least squares best fit
of the data; however, the "goodness" of fit can be calculated mathematically
with more objective results by using the correlation coefficient, R2. The closer
the correlation coefficient is to 1.00, the better the data fit the regression equa-
tion. If the R2 equals exactly 1.00, the curve fits the data exactly, and exact
predictions can be made. For a linear equation, the R2 value can be calculated
from:

(23-14 )

In the above example, the R2 value becomes 0.892 or 89.2% of the y values
( % pulp after evaporation here) that can be accounted for using this least squares
equation.
It is important to keep in mind that "noisy" variations will give a lower
correlation coefficient than smooth or stretched deviations from the regression
386 CITRUS JUICE MANAGEMENT

line. Actual and calculated values should be checked to verify the correlation.
Also, the regression equation usually is valid only within the range of the data.
The linear least squares equation determined above may not fit the data as
closely as one would like. Because the above results represent the best linear
fit to the data, the only way to obtain a better fit is to use another equation-a
nonlinear equation. By using the principles illustrated above and substitution,
the method of least squares can be applied to a wide variety of equations. Also,
the least squares analysis can be programmed into computers for easy use. The
reader is referred to Kolb (1984), who provided not only the equations needed
to fit data to up to 19 different equations but also computer programs in a variety
of program languages, which can be used to determine regression relationships
automatically.

QUESTIONS

1. Give five areas where statistical methods can be applied to citrus quality
control in routine processing.
2. What is the purpose of using significant figures?
3. What is the difference between significant figures and the determination
of error ranges?
4. How are the control limits (upper and lower) usually determined in the
food industry?
5. How many points can constitute a run down in 32 measurements before
the process can be considered statistically influenced by some factor?
6. In what situation can an analysis of variance be useful in citrus quality
control?
7. Explain the null hypothesis.
8. Explain regression analysis.
9. What is the difference between regression analysis and least squares anal-
ysis?
10. How can the use of statistical analyses be greatly simplified in routine
use in citrus quality control?

PROBLEMS

1. How many significant figures does each of the following numbers have?
2,345.34
3000.1
2500
0.00230
6 dogs
QUALITY CONTROL STATISTICS 387

2. Express the answer to the following mathematical problems to the correct number of
significant figures:

23.460 1,234.5 0.002340 0.004 -;- 25,500.0 =


+ 6.0 - 523.000201 x 66.345

3. What is the variance ratio (VR) for a one-way ANDV A analysis between lab tech-
nicians using the data below, and does it prove the null hypothesis?

Measurement Tech A Tech B Tech C


61.2 61.4 60.5
2 61.3 62.0 60.6
3 60.9 61.4 60.4

4. What is the variance ratio for both rows (refractometers) and columns (lab techni-
cians) for the following data, and is there a significant variance between lab techni-
cians and/or refractometers?

Refractometer Tech A Tech B Tech C TechD


59.8 60.0 60.1 59.9
2 60.1 60.2 60.2 59.9
3 60.4 60.3 60.3 60.3

5. It may be useful to have an equation that predicts the acid correction to the Brix base
on the % acid. Determine the linear least squares constants and correlation coefficient
using the following data. Compare the calculated Brix corrections with the actual
Brix calculations.

% Acid Brix correction


0.50 0.10
1.00 0.20
1.50 0.30
2.05 0.40
2.55 0.50

REFERENCES

Duncan, A. J. 1974. Quality Control and Industrial Statistics, 4th edition. Richard D. Irwin, Inc.,
Homewood, Ill., 659-662.
Kolb, W. M. 1984. Curve Fitting for Programmable Calculators. 3rd edition, Syntec Inc., Bowie,
Md.
Chapter 24

Quality Control Management

Quality control involves more than just laboratories and test tubes; a good qual-
ity control department requires administration and management. Managerial
policies and procedures vary widely from plant to plant, but the success of any
system is dependent on basic principles. Like any other employee, quality con-
trol personnel must understand the basic policies and objectives of the company.
Also, quality control departments are run by people who report to non-quality
control adminstrators.
Like all employees, quality control personnel should be shown courtesy and
respect. They should be given concrete goals and responsibilities as well as the
resources and latitude needed to achieve those goals. Quality control personnel
must be leaders, with the courage to speak up when something is going wrong.
They must be competent, and their competency must be recognized. They need
sufficient resources to perform their jobs, such as adequate laboratory space and
equipment.
The quality control laboratory is a major focus of outside visitors, who often
judge a company by the professional appearance of the quality control labora-
tory. The plant's "IQ" is often evalulated by the laboratory's veneer.
Good employees should have a vision of where they are going and why they
are there. Just as they are required to support management in decisions regard-
ing the operation of the plant, management should stand behind quality control
personnel in their quest to protect the quality of the company's products. More-
over, quality control procedures should be part of some type of plan that ulti-
mately will benefit the company. Such a plan must be managed; it should be
efficient, personally rewarding, and profitable.

OTHER DEPARTMENTS
As complex and intricate as a quality control department may seem, it com-
prises only a portion of the overall manufacture of citrus products; and books
could be written about the other areas as well. The quality control department

388

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
QUALITY CONTROL MANAGEMENT 389

must interact with all of these other areas and act as a focal point for many of
the plant's decisions. It also acts as a helm that steers the course of many plant
activities.
One of the first things that should be done in setting up a quality control
department is to establish a realistic set of specifications, for both inbound and
outbound products. Quality control personnel can and should help to define
these specifications. The specifications should at least contain legal require-
ments as defined by the federal standards of identity, good manufacturing prac-
tice, and, if USDA grades are used, the requirements of the desired USDA
grade. Quality control then should be given the authority to reject products that
do not meet these specifications or sanitary conditions. A specification that is
not enforced is a specification that really does not exist.
It is important to keep the quality control department separate from the pro-
duction department because production often will have a tendency to cut comers
with respect to quality in order to get the product made and out on time. Quality
control, on the other hand, should be considerate of production's schedules,
and should not unduly delay or hamper their activities any longer than is nec-
essary to ensure quality products and sanitation.
Although company organizations may vary, the relationships between their
departments may have similarities. A general example of the communication
flow between departments is shown in Fig. 24-1. One should remember that
communication is a two-way street, and much follow-up communication is not
shown in the figure. The figure does show that quality control acts as a traffic
light that determines whether a product may proceed, or whether it must stop
and be rerouted.
In addition to routing quality control activities, the quality control department
may be called upon to become involved in other, non-quality control activities,
involving other departments. One such activity is the analysis of fruit samples
for maturity and juice yields, as mentioned in Chapter 5. The office generally
receives this information so that the owners of the fruit can be credited propor-
tionally. The sales department may ask quality control personnel to assist in
preparing and sending product samples to customers or potential customers.
Similarly, purchasing may ask quality control to analyze inbound product sam-
ples received from suppliers or potential suppliers. Quality control may be called
upon to work with research and development regarding new products, specifi-
cations, or complex problems. Quality control may and should be asked to assist
customers and suppliers in regard to quality problems and/or specifications.

PERSONNEL

The hiring of quality control personnel is generally left to the discretion of the
quality control manager. Job requirements and criteria usually are a function of
390 CITRUS JUICE MANAGEMENT

OUTBOUND INBOUND

mechanical?

yes

Fig. 24-1. Example of communication flow and interdepartmental relationships involving the
quality control department.

supply and demand in the local job market, but job descriptions for every po-
sition in the quality control department should be written and communicated to
personnel already on board as well as to potential employees. A new employee
should receive a complete orientation, including a written and an oral expla-
nation of the company and departmental policies, rules, and procedures. The
new employee should be given a comprehensive plant tour and be assigned an
on-the-job trainer. Every quality control department should have a manual out-
lining procedures and other information related to the quality control activities
QUALITY CONTROL MANAGEMENT 391

that are specific to the particular plant, and a copy of the manual should be
made available to both the new employee and older employees for reference.
The orientation should include instruction in the use of safety gear and safety
procedures (see below in this chapter). Also it should include a description of
the chain of command and the relationship that should exist between other su-
pervisors and members of management. As with any position, the one-boss rule
should be invoked so that communication up and down the chain of command
can go through one person in order to avoid confusion and conflicting direc-
tives. If more than one person is allowed to give quality control personnel di-
rectives, conflicts and confusion may arise.
Although training could begin right away, and even though the employee
may have existing experience and skills for the job, serious training should not
begin for several days in order to give the employee time to adapt to the new
environment. A new employee's success is determined to a significant degree
by how well he or she is allowed to adapt in the first week of employment.
Once the employee can perform the tasks contained in the job description at a
level that is satisfactory to the quality control manager, the initial training can
be considered complete. In addition to this initial training, all laboratory tech-
nicians should undergo continuous training, which may coincide with perfor-
mance evaluations. Cross training among employees of different job descrip-
tions protects quality control activities during times of sickness, layoff, leaves
of absence, vacations, and job changes.
Each employee should be evaluated by his or her supervisor at least once a
year, and should be rated on job performance as well as on how well he or she
has performed generally. A good employee may have poor technical ability,
and a good technician may find it difficult to arrive at work on time. Annual
evaluations provide a good opportunity to solicit employee input about the gen-
eral activities of the department and the company. This can be done during the
evaluation interview orally or by means of a written questionnaire. Many prob-
lems will not emerge without some degree of probing, and unless they do
emerge, they cannot be solved. Written exams on laboratory procedures and
tests as well as departmental and company policies stimulate thought and pro-
vide an excellent forum for instruction and review. Performance tests, where
all technicians analyze the same sample, can demonstrate the consistency of
analyses between lab technicians and ensure standardization in laboratory re-
sults. If possible, a program of incentives should be instigated to encourage
employees to improve and to excel, including such rewards as days off, longer
vacations, or cash awards. Morale is always high and work well done when an
employee feels that he or she is growing professionally and working toward a
goal. Evaluations also provide an important opportunity for the employee to
account for his or her performance. It is important for every employee to receive
appreciation and recognition for work well done.
392 CITRUS JUICE MANAGEMENT

One of the biggest problems in any corporate setting is communication. Both


written and oral communication should be used as much as possible in quality
control operations. Instructions and information should be written down, illus-
trated, demonstrated, and confirmed. Log books can be used for communication
from one shift to another. Each employee, including the quality control man-
ager, should be responsible for checking the log book at the beginning of each
shift. Employees should all feel free to communicate frankly with the quality
control manager at all times. An open door policy is important in any mana-
gerial setting.
From time to time it may be necessary to discipline errant employees. This
job is difficult when rules and guidelines are obscure, or disciplinary procedures
are not clearly defined. These procedures should be spelled out clearly in the
company policy manual and followed precisely in order to avoid favoritism.
Generally an oral warning is followed by a written warning, and records of all
warnings are kept in the employee's confidental file, including the date, time,
and nature of the warning, and the action taken. If undesirable conduct contin-
ues after a written warning, termination of the employee should be considered,
depending on the company policy. If multiple warnings are given without de-
finitive actions, the legal implication is that the company accepts the undesirable
behavior, and that can lead to legal entanglements. Failure of management to
follow company policies weakens the validity of the company policies and sug-
gests their nonexistence even though they are written down. Mistakes made in
the distant past should be generally forgiven and not brought up during disci-
plinary action. Some behavior may justify an employee's immediate dismissal,
such as insubordination, intentional product contamination, or threatening an-
other employee or another's safety. Any such problems that quality control
personnel observe should be reported immediately for the good of the company.
Problems originating in or pertaining to other departments should be reported
through the proper chain of command.
When it becomes necessary to layoff or dimiss an employee, the employee
should be so notified at least two weeks in advance. (An exception to this rule
is if an employee is immediately dismissed for serious misconduct.) Most peo-
ple need a two-week period to arrange their affairs in order to minimize the
impact of the layoff. The reason for the layoff should be discussed honestly and
clearly, as should such matters as how the final check will be handled, including
vacation pay and so forth, as well as the turning in of safety gear, keys, or other
equipment checked out to the employee. If the person has performed well, or
if there are plans to rehire him or her this information should be communicated,
as well as an estimated time or date of rehire. If the separation is due to mis-
conduct or poor workmanship, this too should be frankly explained.
People sometimes become involved with problems that they are unable to
solve by themselves, such as alcoholism or drug use; and it is the employer
who often wields the greatest influence in changing the lives of employees with
QUALITY CONTROL MANAGEMENT 393

such problems. A frank termination may be the last chance for such a person
to be jolted into getting the needed help. Employers must be sure that such
terminations are for the violation of company policies and not just the result of
someone's personal opinion about what ought to be done. It is advisable for the
employer and the employee to get professional advice in questionable situa-
tions.

EQUIPMENT MANAGEMENT

Citrus quality control departments utilize equipment that is specialized in com-


parison to equipment used elsewhere in the plant; so plant maintenance person-
nel are generally unacquainted with laboratory instruments. Minor repairs,
cleaning, and calibrations usually can be done by lab personnel according to
instructions from the manufacturer. Improper use can damage laboratory in-
struments, necessitating expensive repair; therefore, only trained technicians
should use laboratory equipment. Another source of equipment damage is in-
sects and rodents, as electronic equipment provides a warm comfortable habitat
for such pests. Pests may eat wire insulation, short-circuit the electronics, or
wedge themselves into areas that affect the mechanical operation of the instru-
ment. All owner's manuals should be kept on file for easy access, as well as
serve as a record of maintenance so that trends can be detected. Users should
be careful not to spill liquids on electronic instruments.
Like most other laboratories, citrus quality control labs utilize a wide selec-
tion of glassware, induding volumetric glassware. Delivered or measured vol-
umes are indicated by the markings of the glassware and are accurate for most
purposes. Volumetric markings on beakers and Erlenmeyer flasks are generally
accurate to about 5 %; volumetric flasks, burets, and pipettes are generally ac-
curate to within about 0.5 %, depending on the volume measured. If greater
accuracy is desired, volumetric glassware can be calibrated. One performs a
calibration by delivering or measuring a precise volume of water using the vol-
umetric glassware and weighing the water at a given temperature. The weights
obtained with analytical balances are more accurate than the measured volumes
obtained by using volumetric glassware, so the weight of water is used as a
standard and is converted to volume using standard density tables for water at
various temperatures (Weast 1968). This converted volume can be recorded as
a precise volumetric measurement for the particular piece of glassware used.
For example, if we delivered 24.941 grams of distilled water at 20.2°C using
a 25 ml pipette, we would divide the weight by the density (0.998162 g/ml)
(Weast 1968) to get 24.987 ml. The pipette then can be given a number or other
identifier so that when it is used 24.987 ml can be used as the volume instead
of the approximate 25 ml. One should be careful to read the meniscus properly
when using volumetric glassware, as shown in Fig. 3-7.
394 CITRUS JUICE MANAGEMENT

SAFETY

Safety training and accident avoidance should be integral parts of any industrial
operation. Mechanical, electrical, and fire safety should be emphasized in areas
where quality control personnel work. Shelf chemicals should be restrained in
case of an earthquake. Guards for belts and chains on equipment used by quality
control personnel in performing fruit maturity tests and yield tests should be in
place, and machinery should be locked out during cleaning. Employees should
not place their hands in machinery unless absolutely necessary, and even then
should do so only when the machine is locked out. Screw conveyers should
always be covered, to guard against the accidental insertion of a leg or an arm.
Employees should wear goggles and gloves when cleaning with caustic so-
lutions, and bump hats, hair nets, beard guards, and so on, should be used, not
only to avoid product contamination but to prevent hair from getting caught in
machinery. Likewise, loose clothing should not be worn around moving ma-
chinery. Proper hand rails and climbing equipment must be installed for sani-
tation inspections, the taking of samples, or the performance of other necessary
tasks. Quality control personnel should not climb onto tankers, rail cars, or
other moving vehicles until the vehicle has come to a complete stop, and the
driver is out of the cab. Finally, quality control personnel should avoid using
tools or equipment not included in their job description. Even if the lab tech-
nician is proficient in the use of such items, it could lead to unsafe and even
unsanitary conditions.

HAZARDOUS MATERIAL HANDLING

The Occupational Safety and Health Administration of the U.S. government


(OSHA) issued a Hazard Communication Regulation (part 1910.1200) effective
May 25, 1986 that has become known as the "Employee Right to Know Law. "
This law was designed to require employers to inform employees of the various
hazards of their work place. Most of the law is directed to manufacturers and
importers of hazardous chemicals, and food processors are largely exempt from
those provisions. Under this law, "hazardous chemical" is defined as "any
chemical which is a physical hazard or health hazard." Health hazards are said
to include "carcinogens, toxic or highly toxic agents, reproductive toxins, ir-
ritants, corrosives, sensitizers, hepatotoxins, nephrotoxins, neurotoxins, agents
which act on the hematopoietic system, and agents which damage the lungs,
skin, eyes, or mucous membranes." The term "chemical" is defined as "any
element, chemical compound or mixture of elements and/or compounds." To
a chemist, this is simply everything. "Physical hazard" is defined as a "chem-
ical for which there is scientifically valid evidence that it is a combustible liquid,
a compressed gas, explosive, flammable, an organic peroxide, an oxidizer, py-
QUALITY CONTROL MANAGEMENT 395

rophoric, unstable (reactive) or water-reactive." According to the strict defi-


nitions of these tenns, everything can be considered a hazard including water
and air (drowning, slippery ice, steam bums, cold air in freezers, etc.) In at
least partial recognition of the ambiguity of the definitions, appendix B of the
law states that the "hazard evaluation is a process which relies heavily on the
professional judgment of the evaluator." In other words, this hazard commu-
nication regulation must be defined by those to whom it applies, based on pro-
fessional interpretation, with the ultimate authority being the OSHA inspector
and/or the judicial branch of government.
Citrus juice plants utilize various cleaning agents, lubricants, fuels, refriger-
ants, boiler treatment chemicals, compressed gases, and laboratory chemicals
that professional judgment would dictate fall under this regulation. Food prod-
ucts are exempt from this law. Because it is concerned with "chemicals," a
large portion of the responsibility for dealing with this law falls on the quality
control department. Those persons trained in the use and care of chemicals,
such as laboratory technicians, are best equipped to monitor the use of chemi-
cals in the plant and to assist in emergencies. In order to comply with the law,
a written hazard communication program must exist, which includes training,
a hazardous material list including the location of each material, an outline of
the program including who is in charge of each portion, and material safety data
sheets on the hazardous materials used in the plant.
There should be a written explanation of how employees and outside con-
tractors will be notified regarding hazardous materials in each work area. This
information must be available to all employees, their designated representa-
tives, and OSHA. Even though chemical manufacturers are responsible for
proper warning labels, the employer must ensure that all such hazards are prop-
erly identified by using signs, process sheets, batch tickets, or other written
materials.
Chemical manufacturers and suppliers are required to supply their customers
with material safety data sheets (MSDSs) on the chemicals they sell. These
MSDS's are to be made available to all employees who use or work near the
hazardous material. An MSDS outlines the hazards and the emergency actions
necessary in handling a material. Even though there is no fixed fonnat for the
MSDS, the following infonnation must be included:

1. Identity of the material-chemical and common names.


2. Identity of components present at 1 % or greater concentrations (or, for
carcinogens, 0.1 % or greater).
3. Physical and chemical hazards (vapor pressure, flash point, etc.).
4. Health hazards.
5. Exposure limits where available.
6. Whether the material is a carcinogen.
396 CITRUS JUICE MANAGEMENT

7. Known safety precautions.


8. Emergency and first aid procedures.
9. The date of preparation of the MSDS or the last change.
10. Name, address, and phone number of the supplier or the manufacturer.

The written hazard communication program must include a list of the haz-
ardous materials in the plant and their location with an MSDS for each material.
Training should include methods to detect the release of the hazardous sub-
stance, information on physical and health hazards, and ways that employees
can protect themselves, especially in an emergency. It is a good idea to include
an outline of the training session in the written hazard communication program,
along with the date held and a list of employees who attended. For more details
on the Hazardous Communication Regulation, the reader is refered to the law
itself or to an appropriate consultant.

QUESTIONS

1. What is one of the first things that should be done in setting up a quality
control department?
2. Should production oversee quality control, or should quality control over-
see production?
3. What are some of the non-quality control activities that quality control
personnel may become involved with regarding other departments within
the company?
4. What is one of the biggest problems in any company?
5. Is it always true that an employee's personal problems are not the business
of the company? Why or Why not?

REFERENCES
Weast, R. C. 1968. Handbook of Chemistry and Physics, The Chemical Rubber Company, Cleve-
land, Ohio, F4.
Chapter 25

Inventory Management

The management of product inventories is primarily the function of the office


staff. However, some aspects of the inventory clearly cross over into the realm
of the quality control department, including inbound and outbound product sam-
pling, fill weights, blending, label preparation, tank volume measurements, and
the management of laboratory equipment and supplies. The management of
rejected or defective products in inventory is often under the quality control
department's direction.

SAMPLING

The sampling of bulk lots (drums, tankers, etc.) has been discussed in previous
chapters and is fairly straightforward. However, in continuous operations in the
manufacture of retail or consumer products, various sampling techniques must
be used because the product usually is not standardized or mixed to complete
uniformity. Questions arise about how many samples to take and analyze in
order to ensure representative sampling and how many defective samples can
be allowed. Numerous mathematical and statistical methods can be used to jus-
tify a wide variety of sampling plans. However, the simplest and easiest meth-
ods to consider can be copied from those sampling plans used by the Food and
Drug Administration (FDA) (CFR Title 21 145.3) and the U.S. Department of
Agriculture (USDA) (CFR Title 7 52.1-52.83), which are illustrated in Tables
25-1 and 25-2. These tables give the number of samples needed per total num-
ber of containers per lot and the number of permissible rejects. The USDA
sampling plan is based on container type or volume, and the FDA sampling
plan is based on the net weight. Because the FDA is looking for contamination
that would violate the standards of identity and/or health violations, its sampling
plan is more extensive than the USDA plan, which is looking for general grade
or quality characteristics. The continuous sampling performed by the USDA is
an involved procedure in which fewer samples are taken than the number listed
in Tables 25-1 and 25-2. Another sampling plan in the federal code is the one

397

D. Kimball, Citrus Processing


© Van Nostrand Reinhold, New York, NY 1991
398 CITRUS JUICE MANAGEMENT

Table 25-1. FDA sampling plan for canned fruits


(CFR Title 21 145.3).
Lot Size (containe rs) Needed Samples Acceptable Rejects
nt. wt. 1 kg
::5
0-4,800 13 2
4,801-24,000 21 3
24,001-48,000 29 4
48,001-84,000 48 6
84,001-144,000 84 9
144,001-240,000 126 13
over 240,000 200 19

1 kg < nt. wt. < 4.5 kg


0-2,400 13 2
2,401-15,000 21 3
15,001-24,000 29 4
24,001-42,000 48 6
42,001-72,000 84 9
72,001-120,000 126 13
over 120,000 200 19

over 4.5 kg nt. wt.


0-600 13 2
601-2,000 21 3
2,001-7,200 29 4
7,201-15,000 48 6
15,001-24,000 84 9
24,001-42,000 126 13
over 42,000 200 19

used to determine compliance with labeling regulations (CFR Title 21


101.9(e)(2)). It consists of taking 12 samples each from 12 different random
cases that represent one lot and making a composite from the 12 samples. This
composite then is checked for nutrient levels and compared to what is declared
on the label, as discussed in Chapter 11.
In addition to samples taken for analysis, it is a prudent industrial practice to
take extra samples (three minimum) as so-called retain samples. These retain
samples should be kept in a sealed container in cold storage and can be valuable
when complaints or problems arise. If a customer claims that a particular lot is
defective, the retain samples can be used to check the customer's claims. If the
retain samples do not show the same defects, it is likely that the defects arose
during shipment or customer storage. Retain samples also are handy when sea-
sonal products are needed in a special research project, or when a customer or
potential customer requests samples of a particular type of product. Retain sam-
ples may have a shelf life of a few weeks to a year, depending on the type of
product. Edible discarded samples can be given to local charities or employees.
INVENTORY MANAGEMENT 399

Table 25-2. USDA sampling plan in determining grade standards


(CFR Title 7 52.1-52.83'.
Lot Size (containers) Needed Samples Acceptable Rejects
0-3,000 3 0
3,001-12,000 6 I
12,001-39,000 13 2
39,001-84,000 21 3
84,001-145,000 29 4
145,001-228,000 38 5
228,00 1-336,000 48 6
336,001-480,000 60 7
Container Size (canned fruits) Portion of Lot Size Above*
303 x 406 (16 oz) and less Use lot sizes given above.
> 303 x 406 to No.3 cylinder (46 oz) Use same # of samples with! lot size
above.
> No.3 cylinder to #12 can (I gal) Use same # of samples with ~ lot size
above.
> #12 can Use ±above lot size for 6 lb equivalent.
For Fluid Comminuted or Homogeneous
Fruit Products Portion of Lot Size Above*
I lb or less fruit juice Use 1.5 times the lot sizes in the chart
above.
lIb to 3.75 lb (60 oz) Use 2.0 times the lot sizes in the chart
above.
3.75 lb to 10 Ib Use 2.0 times the lot sizes in the chart
above.
over 10 lb Convert to 6-lb equivalents and use chart
as is.
'For example, for 100,000 303 cans take 29 samples and accept 4 rejects. For 100,000 No.3 cylinder cans take
38 samples (or the same as 200,000 in the chart above) and accept 5 rejects. For 100,000 #12 cans take 60
samples (or the same as 400,000 in the chart above). For 10,000 60-lb pails, take 29 samples and accept 4 rejects
(60 X IO,OOOj61b = 100,000 equivalent containers for 100,000 container equivalents in chart above).

FILL WEIGHT

Fill weights are important for some citrus products, and general methods for
their determination are regulated by the federal government, The "general
method for fill of containers" can be found in the Code of Federal Regulations
Title 21 130, 12(b), which describes how the percent fill of a container is to be
determined. The lid is cut out and the distance from the double seam to the
level of food (or juice) is measured. The food is removed, and the container is
cleaned, dried, and weighed. The container then is filled with water to 1'6 inch
from the double seam and weighed, and the net weight ofthe water is recorded.
Then the water, at the same temperature, is removed down to the previously
measured level of the food (or juice), and the net weight of remaining water is
400 CITRUS JUICE MANAGEMENT

determined. The latter water weight is divided by the former water weight and
multiplied by 100% to give the percent fill of the container. For grapefruit juice
and lemon juice, the standards of identity require a 90% fill of the container.
Even though there are no other" fill of container" requirements in the standards
of identity for other citrus juice products, generally a 90% fill is a standard
procedure in the food industry.

LABELS

Labels come in a wide variety of shapes, sizes, and colors. The nutritional
aspect of labeling has already been discussed, in Chapter 11. Retail or consumer
commodity labels generally are fixed or quite inflexible from lot to lot and must
comply with the Fair Packaging and Labeling Act (Public Law 89-755 89th
Congress, S. 985 November 3, 1966) as well as the regulations for the enforce-
ment of the Federal Food, Drug, and Cosmetic Act and the Fair Packaging and
Labeling Act (CFR Title 21 10 1.1-10 1.105). A new addition to the law is the
country of origin regulation, which states that 75 % ofthe imported juice (citrus
and/or noncitrus) must be declared by country of origin on all labels for both
retail and nonretail products. The standards of identity also have labeling re-
quirements, as do the USDA grades for retail products. In addition to govern-
mental requirements, industrial organizations have established guidelines for
labeling, such as those of the National Food Processors Association (1977).
Lawyers and graphic artists are asked to design labels, which then are used to
manufacture large inventories of labels and/or labeled containers. The quality
control department should monitor the general quality of labels and containers
as a part of sample analysis. Lot or day codes imprinted on retail containers
also should be inspected, as well as the fill levels and the container seal quality.
Nonretail or nonconsumer commodities (generally bulk) sold to other com-
mercial entities still fall under the labeling requirements of the standards of
identity. Each lot of bulk juice (drums, pails, tankers, etc.) should be clearly
marked as the product described in the standards of identity. Often a product
will meet the criteria for several standards of identity, and the seller can choose
the one he or she prefers to use to identify the product. (See Chapter 19 for
brief descriptions of the standards of identity.) Included with the product name
should be the name and address of the manufacturer, the lot number, the date
of manufacture, the net weight, and the Brix. Perhaps the Brix/acid ratio, tare,
and gross weights would be appropriate as well. If any other ingredients have
been added, such as preservatives or sugar, or any material that may affect the
standards of identity, those ingredients also should be declared on the label.
Defective product should be marked with a highly visible tag, such as a red tag,
indicating the nature of the defect and the lot number. This facilitates proper
handling of the defective product. Tanker or barge lots generally have the above-
listed information on the bill of lading.
INVENTORY MANAGEMENT 401

Drum labels generally are preprinted or preprogrammed into a computer with


a fixed or unchanging label format with spaces for variable information. Later
the variable information, such as lot number, weights, Brix, and so on, is writ-
ten in by hand as the product is packaged. This infonnation often is determined
by the quality control personnel because they are the ones who determine some
of the parameters, such as the Brix and net weights. Also, the quality control
department usually is more aware of other labeling requirements and can be
more effective than production in label monitoring.

AUTOMATIC IDENTIFICATION METHODS

Automatic identification methods are the state-of-the-art methods used in com-


mercial and retail outlets across the country to identify products by machine.
The most common method employs bar codes. Other related methods include
optical character recognition, voice data entry, machine vision, radio frequency
data communication magnetic strips, and smart cards (Knill 1988), which are
tailor-made for different applications. Bar codes are used with most retail prod-
ucts and have found their way into the bulk citrus industry as well. On April 3,
1973 the Uniform Product Code Council, Inc. established the Uniform Product
Code (UPC), a bar code system designed for use with retail products (UPC
Council, Inc.). International interest in the UPC system led to the adoption of
the European Article Numbering system (EAN) in December of 1976, which
expanded the UPC capabilities. Now, nearly all products in supermarkets have
a UPC identifying bar code. The code consists of 10 digits divided into one or
two numbers. Slot scanners, which consist of two orthogonal scanners, are used
so that any orientation of the bar code will be scanned by one or the other
scanner as the product is moved across the slots. The scanners read the 5-or
lO-digit code and automatically associate it with a preprogrammed price and
product type in the cash register.
For in-house industrial use, the UPC code can be used to count empty con-
tainers, labels, or individual product containers. However, unlike the case of
the retail outlet, it is easier to count bulk quantities industrially, such as cases,
pallets, or drums, rather than individual cans or bottles. The bar codes used on
these bulk containers need not utilize the UPC system. Also, information such
as lot number, Brix, Brix/acid ratio, and net weights is of greater concern to
members of industry than to the consumer, who assumes these parameters to
be constant; and it might be helpful if this infonnation were encoded into bar
code symbologies for industrial purposes.
Citrus bulk processors are beginning to realize the great benefits of automatic
identification techniques. One such system involves the use of a preprogrammed
thermal printer that prints labels impervious to the wet environment of industrial
processing and storage. Such printers allow for computerized entry of variable
data on a lot-by-Iot basis, which can be converted instantly to bar code sym-
402 CITRUS JUICE MANAGEMENT

bologies. Labels can be customized on-site to fit the needs of any manufacturer.
Portable scanners can be used to scan the bar codes of bulk inventories and can
be programmed to process the data into any form or format. The portable scan-
ner then can be attached to a printer or a computer, and the finished manifest,
blend sheet, or inventory listing can be printed in the desired format with no
human error in counting or writing. This information also can go directly into
a central processing unit to automatically adjust product inventories, again with-
out human involvement. Examples of UPC/EAN symbology as well as an au-
tomatic identification drum label are shown in Fig. 25-1. Figure 25-2 shows a

UPC Symbol

1380 10121
CALIFORNIA CITRUS
PRODUCERS, INC.
P.O. 80x C
Lindsay , CA 93247 USA
UALENCIA
Concentrated Orange Juice

SAMPLE 1211
For Manufactur i ng

8PIX RAT ~T WT
162.eIL7.sl563 I

Dilute with 5 . 3
Pa.-ts Water

Fig. 25-1. Example of UPC lEAN bar code symbology and an industrial bar code label used
commercially for 52-gallon drums.
INVENTORY MANAGEMENT 403

CALIFORMIA CIYRU8
IPRODUCERS. INC.
P.O. Box C
525 E. Lindmore Ave.
Lindsay. CA 93247
(209) 562-5169

customer ______~S~u~n~n~y~O~r~a~n~g~e~C~o~millP~a~n~yL-__ ORDER NO. 6603 ROW NO. 8.N

LOT NUMBER NUMBER OF DRUMS BRIX B/A RATIO DRUM NET WEIGHT
VB1758 4 59.8 12.5 560
VA1758 18 59.9 12.6 559
VB1698 1 59.5 12.6 562
VB1728 20 59.9 12.9 559
VC1728 20 60.0 12.9 558
VB1738 21 59.8 12.5 560
TOTAL DRUMS= 84
Fig. 25-2. Example of shipping manifest printed from data transmitted directly from a bar code
label scanner. Counting, sorting. and manifest formatting can be programmed into the portable bar
code scanning unit.

drum manifest printed from a scanning of drum bar code labels that was pro-
cessed and transmitted directly to a small inexpensive printer.

TANK MEASUREMENT
Another important area that quality control personnel often get involved with is
the determination of the volume of product in bulk tanks. Fluid levels are mea-
sured from a fixed standard point, or they are measured using various types of
level meters. Level meters designed for water measurements according to den-
sity usually are not adequate for juices or concentrates because their densities
are quite different from that of water. Once the level is determined , equations
can be used to calculate the volume of fluid in the tank. Net weights then can
be determined too , if needed. Most processing tanks have the shape illustrated
in Fig. 25-3, with a dome top, cylindrical center, and slant bottom . As the
product fills from the bottom, each of the sections is filled , with a varying
relationship existing between the product level and the volume of the tank .
The slant bottom portion is divided into two sections, the first half and the
second half, as shown in Fig. 25-4, where the shaded area represents the prod-
uct or fluid in the tank. As the product fills the first half of the slant bottom,
the top surface area of the product may be represented as a segment of a circle,
404 CITRUS JUICE MANAGEMENT

DOME TOP

CYLINDRICAL
CENTER

Fig. 25-3. Typical shape of bulk tanks used in citrus processing, with three main sections.

-------p
~a ~
hO

SIDE VIEW
Fig. 25-4. Isometric views of the slant bottom portion of bulk tanks and dimensions used to derive
volume equations.
INVENTORY MANAGEMENT 405

described mathematically by:

(25-1)

with the variables as depicted in Fig. 25-4. Looking at the side view and using
a trigonometric relationship we get:

(r - y) / h = tan () = 2r / ho (25-2)

which leads to:

y = r(1 - 2h/ho) (25-3 )

With inches used as the unit of measurement, the volume of the slant bottom
during filling of the first half becomes:

(25-4 )

Substituting Equation 25-1 and 25-3 into Equation 25-4 gives the volume of the
first half of the slant bottom as a function of only one variable, the measured
vertical height h, as follows:

Vb = -hr
2
(7r- + 2 (2h
- - 1 ) -J(l - h/ho)h/ho - sin- I ( 1 - -2h)) (25-5)
~ 2 ~ ~

The volume is found in gallons.


Once the first half has been filled, the second half of the slant bottom will
have a surface area expressed as follows:

(25-6)

which is similar to Equation 25-1 except for a negative sign. Using the same
treatment as before, we obtain the following relationship for the volume of
product in the slant bottom as the product fills the second half of the slant
bottom:

Vb = :~~ (~ + 2 (~: - 1) .J(1 - h / ho) h / ho + sin - I (~: - 1 )) (25-7)

which is similar to Equation 25-5 except for the signs of the last terms.
Once the total bottom section is filled, the total volume can be calculated
406 CITRUS JUICE MANAGEMENT

simply by using the following:

(25-8)

The cylindrical section uses a volume equation similar to Equation 25-8:

(25-9)

By adding the filled volume of the slant bottom section to Vc ' the relationship
between the product level and the volume while the level is within the cylin-
drical section becomes:

(25-10)

When the cylindrical and slant bottom portions are full, the dome top begins
to fill, as shown in Fig. 25-5. The volume of a segment of a sphere can be
expressed as:

Vsegsphere = 7rvo(3R - vo)/693 (25-11 )

using the dimensions in Fig. 25-5. The radius of the sphere must be determined
by measuring the curve of the dome, transposing it to paper, and graphically
measuring the radius. Equation 25-11 represents the total volume of the dome
portion of the tank. The product volume in the dome is determined by subtract-

.......1 - - - - - - 2r -------1.~1

~
v
+

Fig. 25-5. Dimensions useful in detennining the volume of the dome top in citrus bulk tanks.
The radius R must be detennined graphically or by measurement.
INVENTORY MANAGEMENT 407

ing the volume of the spherical segment of space remaining above the product
from Equation 25-11. After simplification we obtain the following:

Vd = 1I"(v6(R - vo/3) - (vo - v/(R -(vo - v)/3}/231 (25-12)

With the cylindrical portion filled, the term h in Equation 25-10 can be ex-
pressed as the fixed constant d for the length of the cylindrical portion of the
tank, and the total volume of the tank with product in the dome top can be
expressed as follows:

V = -1I"r2 ( d + -ho) + - 11" ( Vo2 (Rv- o- ) - (vo - v) 2 ( R


'231 2 231 3

(25-13 )

The total height from the bottom of the tank to the product level in the dome
top is:

H,=ho+d+v (25-14 )

To illustrate the use of these equations, we will take an imaginary tank and
calculate the volume of fluid at different levels. Suppose the tank has a diameter
of 12 feet (r = 72 inches), a slant bottom of 12 inches vertically, a cylindrical
length of 15 feet (180 inches), a dome top with height of 3 feet, and a spherical
radius of 64 feet (78 inches) . We measure the total height H from the very
bottom of the tank and determine the volume of product in the tank by using
the various equations shown above. Table 25-3 summarizes the data and the
results. With the hatch set at 6 inches above the cylindrical portion of the tank,
the maximum v value is 6 inches. Paddle or propeller agitators in product tanks

Table 25-3. Calculated volumes of product from


fluid level measurements.
Measurement # H (total vertical level) Equation # Gallons
3" 25-5 21
2 8" 25-7 200
3 112" 25-10 7,473
4 195" 25-13 13,284
5 198" 25-13 13,444
Tank dimensions-a radius of 72", a vertical slant bottom of 12", a cylindrical length
of 180", a dome top height of 36", and a dome spherical radius of 78". The hatch is
6" above the cylindrical section and sets the maximum filling level of the tank.
408 CITRUS JUICE MANAGEMENT

displace a portion of the product, and their volume can be subtracted from the
product volume. However, this displaced volume generally is not significant.
If a tank has a spherical bottom, the volume with the juice level in this spher-
ical segment again can be described as in Equation 25-11, but with Vo now
representing the actual fluid level. This form of Equation 25-11 then can be
used in place of the equations used for the slant bottom portion in the above
procedures.
Using the above-derived equations every time a volume determination is
needed is awkward and time-consuming. The best way to use such equations is
to generate a table consisting of a level measurement and the corresponding
volume. Such charts or tables can be used quickly and effectively, not only by
quality control but by production personnel as well. Programmable calculators
or computers are ideally suited for such table generation. A flow chart that can
be used to program computers to generate a volume table is illustrated in Fig.
25-6.
A problem commonly found with some computer languages, such as RPG,
is the inability to perform the sin -I function. In such cases, a Taylor series
expansion (shown below) out to six terms gives sufficient accuracy in most
cases:

x3 9x 5 180x 7 10080x 9 833490x II


sin- I x =x +- +- + -- + + + ... (25-15)
3! 5! 7! 9! 11!

Tankers

The amount of juice in stationary tanks is most easily measured by volume.


However, mobile tanks, such as tankers, usually measure the amount of product
by weight, using industrial truck scales. This net weight of juice can be con-
verted to juice volume easily by using the density conversion from Equation
2-9 or 2-11. For example, if we had a tanker that weighed 46,765 pounds and
contained orange concentrate at 60.2°Brix, we would get:

(46, 765lbconc) / (10. 737Ib/[email protected]) = 4355 gal

LAB EQUIPMENT AND SUPPLIES

The Internal Revenue Service and general company accounting procedures gen-
erally require an annual inventory of products and supplies. Even if no inven-
tory is required, a knowledge of equipment and supplies on hand will help the
quality control manager to utilize resources efficiently and will facilitate the
timely restocking of supplies. Inventories can be classified according to such
INVENTORY MANAGEMENT 409

VOLUMES IN SLANT-
BOTTOM TANKS
Tk Btm to Juice (Ht)
Ht of Slant Btm (ho)
Tank Radius (r)
Ht Cyl Portion (d)
Radius Dome Top (R)
Max Ht in Dome Top (Vm) EO 25-5
Vb or Vt

EO 25-7
Vb' or Vt

EO 25-10
Vc+Vb or Vt

yes EO 25-13
Vb or Vt

TANK OVERFILL!!!!

Fig. 25-6. Flow chart that can be used to generate a volume table for a bulk tank using the
equations in the chapter.
410 CITRUS JUICE MANAGEMENT

categories as beakers, pipettes, burets, hardware, chemicals, and so on. Indi-


vidual items on the inventory can be priced by using identification numbers
found in supplier catalogues. Commercial inventories usually are performed in
pairs, with one person counting and another recording the number of items and
the item identification. Personnel should be careful to isolate items being counted
so that they are not used or moved before the counting can be completed. A
copy of the previous year's inventory can be used as a guide.
Laboratory technicians must monitor the current inventory of supplies at all
times to avoid running out of needed items. The establishment of minimum
supply levels can help them to determine when an item needs to be reordered.
Delivery time should be a factor in determining the minimum allowable inven-
tory. Most items can be obtained in a week or less, but some items may take
much longer. Some equipment and supplies are indispensable in the operation
of a quality control laboratory, and backups should always be kept on hand for
them. This includes such items as refractometers, balances, and titrating equip-
ment. If a piece of equipment must be sent away for repair, the backup can be
used. Because ordered supplies may take some time to arrive, ordering records
should be kept; and these records can be used as an aid in annual inventories
as well as to ensure timely shipments. Upon the receipt of supplies, packing
slips should be promptly and thoroughly examined to ensure that the proper
item was received, as well as to ensure proper storage or distribution to those
persons who need the item(s).

QUESTIONS

1. Why is a sampling plan for consumer products important?


2. Why are the USDA and FDA sampling plans different?
3. Why are retain samples important?
4. How can bar codes on labels be of use?
5. Why would a plant purchase two refractometers?

PROBLEMS

1. If the FDA sampling plan was used to determine the number of samples needed for
50,000 half-gallon containers of orange juice from concentrate, how many samples
should be taken, and how many rejects would be allowed? If the half-gallon con-
tainers were produced at the rate of 100/ min., at what time intervals should samples
be taken using this plan?
2. Consider a bulk tank with a radius of 150 inches, a vertical slant bottom of 36 inches,
a dome top height of 24 inches, a cylindrical section 250 inches high, and a dome
spherical radius of 300 inches. The hatch is 8 inches above the top of the cylindrical
section. What is the maximum capacity of the tank?
INVENTORY MANAGEMENT 411

3. If the tank in problem 2 were filled to a height of 200 inches from the vety bottom
of the slant section, what would be the product volume?
4. If the tank in problem 2 were filled to a height of 30 inches from the bottom of the
slant section, what would be the product volume?
5. Suppose a tank had a spherical bottom with a depth of 18 inches and a spherical
radius of 120 inches and a product level of 13 inches. What volume of juice is in the
tank?

REFERENCES

Knill, B. 1988. New directions in automatic identification, Industry Week, 237(4), AI-A36.
National Food Processors Association Labeling Manual, August 1977.
UPC Council, Inc. 7051 Corporate Way, Suite 201, Dayton, Ohio 45459.
Appendix A

Acid Corrections to the BRIX

% Acid Correction % Acid Correction % Acid Correction


0.10 0.02 1.75 0.35 3.40 0.66
0.15 0.03 1.80 0.36 3.45 0.67
0.20 0.04 1.85 0.37 3.50 0.68
0.25 0.05 1.90 0.38 3.55 0.69
0.30 0.06 1.95 0.39 3.60 0.70
0.35 0.07 2.00 0.39 3.65 0.71
0.40 0.08 2.05 0.40 3.70 0.72
0.45 0.09 2.10 0.41 3.75 0.73
0.50 0.10 2.15 0.42 3.80 0.74
0.55 0.11 2.20 0.43 3.85 0.75
0.60 0.12 2.25 0.44 3.90 0.76
0.65 0.13 2.30 0.45 3.95 0.77
0.70 0.14 2.35 0.46 4.00 0.78
0.75 0.15 2.40 0.47 4.05 0.79
0.80 0.16 2.45 0.48 4.10 0.80
0.85 0.17 2.50 0.49 4.15 0.81
0.90 0.18 2.55 0.50 4.20 0.81
0.95 0.19 2.60 0.51 4.25 0.82
1.00 0.20 2.65 0.52 4.30 0.83
1.05 0.21 2.70 0.53 4.35 0.84
1.10 0.22 2.75 0.54 4.40 0.85
1.15 0.23 2.80 0.54 4.45 0.86
1.20 0.24 2.85 0.55 4.50 0.87
1.25 0.25 2.90 0.56 4.55 0.88
1.30 0.26 2.95 0.57 4.60 0.89
1.35 0.27 3.00 0.58 4.65 0.90
1.40 0.28 3.05 0.59 4.70 0.91
1.45 0.29 3.10 0.60 4.75 0.92
1.50 0.30 3.15 0.61 4.80 0.93
1.55 0.31 3.20 0.62 4.85 0.94
1.60 0.32 3.25 0.63 4.90 0.95
1.65 0.33 3.30 0.64 4.95 0.96
1.70 0.34 3.35 0.65 5.00 0.97

412
ACID CORRECTIONS TO THE BRIX 413

% Acid Correction % Acid Correction % Acid Correction


5.05 0.98 7.50 1.44 9.95 1.90
5.10 0.99 7.55 1.45 10.00 1.91
5.15 1.00 7.60 1.46 10.05 1.92
5.20 1.01 7.65 1.47 10.10 1.93
5.25 1.02 7.70 1.48 10.15 1.94
5.30 1.03 7.75 1.49 10.20 1.95
5.35 1.03 7.80 1.50 10.25 1.96
5.40 1.04 7.85 1.51 10.30 1.97
5.45 1.04 7.90 1.52 10.35 1.98
5.50 1.05 7.95 1.53 10.40 1.99
5.55 1.06 8.00 1.54 10.45 2.00
5.60 1.07 8.05 1.55 10.50 2.01
5.65 1.08 8.10 1.56 10.55 2.02
5.70 1.09 8.15 1.57 10.60 2.03
5.75 1.10 8.20 1.58 10.65 2.04
5.80 1.11 8.25 1.59 10.70 2.05
5.85 1.12 8.30 1.60 10.75 2.06
5.90 1.13 8.35 1.61 10.80 2.06
5.95 1.14 8.40 1.62 10.85 2.07
6.00 1.15 8.45 1.63 10.90 2.08
6.05 1.16 8.50 1.64 10.95 2.09
5.75 1.10 8.55 1.65 11.00 2.10
6.10 1.17 8.60 1.66 11.05 2.11
6.15 1.18 8.65 1.67 11.10 2.12
6.20 1.19 8.70 1.68 11.15 2.13
6.25 1.20 8.75 1.69 11.20 2.14
6.30 1.21 8.80 1.69 11.25 2.15
6.35 1.22 8.85 1.70 11.30 2.16
6.40 1.23 8.90 1.71 11.35 2.17
6.45 1.24 8.95 1.72 11.40 2.18
6.50 1.25 9.00 1.72 11.45 2.19
6.55 1.26 9.05 1.73 11.50 2.20
6.60 1.27 9.10 1.74 11.55 2.21
6.65 1.28 9.15 1.75 11.60 2.21
6.70 1.29 9.20 1.76 11.65 2.22
6.75 1.30 9.25 1.77 11.70 2.23
6.85 1.31 9.30 1.78 11.75 2.24
6.90 1.32 9.35 1.79 11.80 2.24
6.95 1.33 9.40 1.80 11.85 2.25
7.00 1.34 9.45 1.81 11.90 2.26
7.05 1.35 9.50 1.82 11.95 2.27
7.10 1.36 9.55 1.83 12.00 2.27
7.15 1.37 9.60 1.83 12.05 2.28
7.20 1.38 9.65 1.84 12.10 2.29
7.25 1.39 9.70 1.85 12.15 2.30
7.30 1.40 9.75 1.86 12.20 2.31
7.35 1.41 9.80 1.87 12.25 2.32
7.40 1.42 9.85 1.88 12.30 2.33
7.45 1.43 9.90 1.89 12.35 2.34
414 APPENDIX A

% Acid Correction % Acid Correction % Acid Correction


12.40 2.35 14.85 2.79 17.30 3.23
12.45 2.36 14.90 2.80 17.35 3.24
12.50 2.37 14.95 2.80 17.40 3.25
12.55 2.38 15.00 2.81 17.45 3.26
12.60 2.39 15.05 2.82 17.50 3.26
12.65 2.40 15.10 2.83 17.55 3.27
12.70 2.41 15.15 2.84 17.60 3.28
12.75 2.42 15.20 2.85 17.70 3.29
12.80 2.42 15.25 2.86 17.75 3.30
12.85 2.43 15.30 2.87 17.80 3.31
12.90 2.44 15.35 2.88 17.85 3.32
12.95 2.45 15.40 2.89 17.90 3.33
13.00 2.46 15.45 2.90 17.95 3.34
13.05 2.47 15.50 2.91 18.00 3.35
13.10 2.48 15.55 2.92 18.05 3.36
13.15 2.49 15.60 2.93 18.10 3.37
13.20 2.50 15.65 2.94 18.15 3.37
13.25 2.51 15.70 2.95 18.20 3.38
13.30 2.52 15.75 2.96 18.25 3.39
13.35 2.53 15.80 2.97 18.30 3.40
13.40 2.54 15.85 2.98 18.35 3.41
13.45 2.55 15.90 2.99 18.40 3.42
13.50 2.56 15.95 2.99 18.45 3.43
13.55 2.57 16.00 3.00 18.50 3.44
13.60 2.57 16.05 3.01 18.55 3.45
13.65 2.58 16.10 3.02 18.60 3.46
13.70 2.59 16.15 3.02 18.65 3.47
13.75 2.60 16.20 3.03 18.70 3.48
13.80 2.61 16.25 3.04 18.75 3.48
13.85 2.62 16.30 3.05 18.80 3.49
13.90 2.63 16.35 3.05 18.85 3.50
13.95 2.64 16.40 3.06 18.90 3.51
14.00 2.64 16.45 3.07 18.95 3.52
14.05 2.65 16.50 3.08 19.00 3.53
14.10 2.66 16.55 3.08 19.05 3.54
14.15 2.67 16.60 3.09 19.10 3.55
14.20 2.68 16.65 3.10 19.15 3.55
14.25 2.69 16.70 3.11 19.20 3.56
14.30 2.70 16.75 3.12 19.25 3.57
14.35 2.71 16.80 3.13 19.30 3.58
14.40 2.72 16.85 3.14 19.35 3.59
14.45 2.73 16.90 3.15 19.40 3.59
14.50 2.74 16.95 3.16 19.45 3.60
14.55 2.74 17.00 3.17 19.50 3.61
14.60 2.75 17.05 3.18 19.55 3.62
14.65 2.76 17.10 3.19 19.60 3.63
14.70 2.77 17.15 3.20 19.65 3.64
14.75 2.77 17.20 3.21 19.70 3.65
14.80 2.78 17.25 3.22 19.75 3.66
ACID CORRECTIONS TO THE BRIX 415

% Acid Correction % Acid Correction % Acid Correction


19.80 3.67 22.25 4.10 24.70 4.53
19.85 3.68 22.30 4.11 24.75 4.53
19.90 3.69 22.35 4.12 24.80 4.54
19.95 3.69 22.40 4.13 24.85 4.55
20.00 3.70 22.45 4.14 24.90 4.56
20.05 3.71 22.50 4.15 24.95 4.57
20.10 3.72 22.55 4.16 25.00 4.58
20.15 3.72 22.60 4.17 25.05 4.59
20.20 3.73 22.65 4.18 25.10 4.60
20.25 3.74 22.70 4.19 25.15 4.61
20.30 3.75 22.75 4.19 25.20 4.62
20.35 3.76 22.80 4.20 25.25 4.63
20.40 3.77 22.85 4.21 25.30 4.64
20.45 3.78 22.90 4.22 25.35 4.65
20.50 3.79 22.95 4.23 25.40 4.66
20.55 3.79 23.00 4.24 25.45 4.67
20.60 3.80 23.05 4.25 25.50 4.68
20.65 3.81 23.10 4.26 25.55 4.68
20.70 3.82 23.15 4.26 25.60 4.69
20.75 3.83 23.20 4.27 25.65 4.70
20.80 3.84 23.25 4.28 25.70 4.71
20.85 3.85 23.30 4.29 25.75 4.72
20.90 3.86 23.35 4.29 25.80 4.73
20.95 3.87 23.40 4.30 25.85 4.74
21.00 3.88 23.45 4.31 25.90 4.75
21.05 3.89 23.50 4.32 25.95 4.75
21. IO 3.90 23.55 4.33 26.00 4.76
21.15 3.90 23.60 4.34 26.05 4.77
21.20 3.91 23.65 4.35 26.10 4.78
21.25 3.92 23.70 4.36 26.15 4.78
21.30 3.93 23.75 4.37 26.20 4.79
21.35 3.94 23.80 4.38 26.25 4.80
21.40 3.95 23.85 4.39 26.30 4.81
21.45 3.96 23.90 4.40 26.35 4.82
21.50 3.97 23.95 4.40 26.40 4.83
21.55 3.98 24.00 4.41 26.45 4.84
21.60 3.99 24.05 4.42 26.50 4.85
21.65 4.00 24.10 4.43 26.55 4.85
21.70 4.01 24.15 4.43 26.60 4.86
21.75 4.01 24.20 4.44 26.65 4.87
21.80 4.02 24.25 4.45 26.70 4.88
21.85 4.03 24.30 4.46 26.75 4.89
21.90 4.04 24.35 4.47 26.80 4.90
21.95 4.04 24.40 4.48 26.85 4.91
22.00 4.05 24.45 4.49 26.90 4.92
22.05 4.06 24.50 4.50 26.95 4.93
22.10 4.07 24.55 4.50 27.00 4.94
22.15 4.08 24.60 4.51 27.05 4.95
22.20 4.09 24.65 4.52 27.10 4.96
416 APPENDIX A

% Acid Correction % Acid Correction % Acid Correction


-.
27.15 4.96 29.50 5.37 31.85 5.78
27.20 4.97 29.55 5.38 31.90 5.79
27.25 4.98 29.60 5.39 31.95 5.79
27.30 4.99 29.65 5.40 32.00 5.80
27.35 4.99 29.70 5.41 32.05 5.81
27.40 5.00 29.75 5.41 32.10 5.82
27.45 5.01 29.80 5.42 32.15 5.83
27.50 5.02 29.85 5.43 32.20 5.84
27.55 5.02 29.90 5.44 32.25 5.84
27.60 5.03 29.95 5.45 32.30 5.85
27.65 5.04 30.00 5.46 32.35 5.86
27.70 5.05 30.05 5.47 32.40 5.87
27.75 5.05 30.10 5.48 32.45 5.88
27.80 5.06 30.15 5.48 32.50 5.89
27.85 5.07 30.20 5.49 32.55 5.89
27.90 5.08 30.25 5.50 32.60 5.90
27.95 5.09 30.30 5.51 32.65 5.91
28.00 5.10 30.35 5.52 32.70 5.92
28.05 5.1I 30.40 5.53 32.75 5.93
28.10 5.12 30.45 5.54 32.80 5.94
28.15 5.13 30.50 5.55 32.85 5.94
28.20 5.14 30.55 5.56 32.90 5.95
28.25 5.15 30.60 5.57 32.95 5.96
28.30 5.16 30.65 5.58 33.00 5.97
28.35 5.17 30.70 5.59 33.05 5.98
28.40 5.18 30.75 5.59 33.10 5.99
28.45 5.19 30.80 5.60 33.15 5.99
28.50 5.20 30.85 5.61 33.20 6.00
28.55 5.21 30.90 5.62 33.25 6.01
28.60 5.22 30.95 5.63 33.30 6.02
28.65 5.23 31.00 5.64 33.35 6.03
28.70 5.24 31.05 5.64 33.40 6.04
28.75 5.24 31.10 5.65 33.45 6.04
28.80 5.25 31.15 5.66 33.50 6.05
28.85 5.26 31.20 5.67 33.55 6.06
28.90 5.27 31.25 5.68 33.60 6.07
28.95 5.27 31.30 5.69 33.65 6.08
29.00 5.28 31.35 5.69 33.70 6.09
29.05 5.29 31.40 5.70 33.75 6.09
29.10 5.30 31.45 5.71 33.80 6.10
29.15 5.30 31.50 5.72 33.85 6.11
29.20 5.31 31.55 5.73 33.90 6.12
29.25 5.32 31.60 5.74 33.95 6.13
29.30 5.33 31.65 5.74 34.00 6.14
29.35 5.34 31.70 5.75 34.05 6.14
29.40 5.35 31.75 5.76 34.10 6.15
29.45 5.36 31.80 5.77 34.15 6.16
ACID CORRECTIONS TO THE BRIX 417

% Acid Correction % Acid Correction % Acid Correction

34.20 6.17 34.40 6.20 34.60 6.24


34.25 6.18 34.45 6.21 34.65 6.24
34.30 6.19 34.50 6.22 34.70 6.25
34.35 6.19 34.55 6.23
Appendix B

GWBASIC and RPG Programs

C***************************************************************************************
C* RPG CALCULATIONS SUBROUTINE THAT CAN BE USED TO CALCULATE
C* THE LBS SOLIDS/GALLON FROM THE BRIX USING EQUATION 2-10
C***************************************************************************************
CSR SUBI BEGSR
CSR Z-ADDI COUNT 20 INITIALIZE
CSR Z-ADDl.OOOOOOO TAYLOR 157 VARIABLES
CSR BRIX ADD 330.872 FO 154
CSR Z-ADDl.OOOO Fl 158
CSR Z-ADD 1.0000 F2 154
CSR Z-ADDl.OOOO F3 154
CSR Fl MULTF Fl H CALCULATE
CSR F2 MULT 170435 F2 FACTORS
CSR Fl DIV F2 Fl H FOR
CSR Fl DIV F3 Fl H TAYLOR
CSR Fl MULT FO Fl H SERIES
CSR Z-ADDFI F4 158
CSR RET TAG
CSR SETOF 10 TAYLOR
CSR TAYLOR ADDF4 TAYLOR SERIES
CSR F4 MULT F3 F4 H SUMMATION
CSR F4 MULT Fl F4 H
CSR COUNT ADD 1 COUNT H
CSR F3 MULT COUNT F3 H
CSR F4 DIV F3 F4 H
CSR COUNT COMP20 10
CSR N10 GOTO RET
CSR SETOF 10
CSR TAYLOR MULT .0437691 TAYLOR H
CSR TAYLOR MULT BRIX SPG 43H FINAL SPG
CSR ENDSR VALUE

418
GWBASIC AND RPG PROGRAMS 419

10 'PROGRAM TO ADJUST BRIX USING WATER OR HIGHER BRIX CONe.


20 INPUT "Brix on hand" ;BI
30 INPUT "Desired Brix" ;B
40 INPUT "Volume on hand" ;VC
50 IF BI > B THEN GOTO 200
55 INPUT "Brix of high Brix concentrate" ;BH
60 INPUT "Can the volume vary (Y /N)" ;Q$
70 IF Q$="Y" THEN GOTO 300
80 BB=BI
90 GOSUB 400
100 SPGI=SPG
110 BB=BH
120 GOSUB 400
130 SPGH ~ SPG
140 BB=B
150 GOSUB 400
160 VH=VC*(SPG-SPGI) /(SPGH -SPGI)
170 VH=CINT(VH)
180 PRINT "Volume of high Brix needed = " ;VH; "gallons"
190 END
200 INPUT "Can the volume vary (Y /N)" ;Q$
210 IF Q$="Y" THEN GOTO 300
220 BB=BI
230 GOSUB 400
240 SPGI=SPG
250 BB=B
260 GOSUB 400
270 VW=VC*(SPGI-SPG)/SPGI
275 VW=CINT(VW)
280 PRINT "Volume of water needed = " ;VW; "gallons"
290 END
300 BB=BI
310 GOSUB 400
320 SPGI=SPG
330 BB=BH
340 GOSUB 400
350 SPGH~SPG
360 BB=B
370 GOSUB 400
380 V=VC*(SPGI-SPG)/(SPG-SPGH)
385 V =CINT(V)
390 PRINT "Vol. of water or hi-Brix conc. needed = " ;V; "gallons"
395 END
400 SPG= .0437691 *BB*EXP( BB+330.872) -2/170435!)
410 RETURN

10 'PROGRAM TO DETN CUTBACK JUICE NEEDED


20 INPUT "Brix of concentrate" ;BC
30 INPUT "Brix of single strength juice" ;BJ
420 APPENDIX B

40 INPUT "Desired final Brix" ;B


50 INPUT "Desired final Volume" ;V
60 BB=BC
70 GOSUB 200
80 SPGC=SPG
90 BB=BJ
100 GOSUB 200
110 SPGJ =SPG
120 BB=B
130 GOSUB 200
140 VJ=V*(SPGC-SPG)/(SPGC-SPGJ)
150 VJ=CINT(VJ)
160 VC=CINT(V-VJ)
170 PRINT "Volume of ";BC; "Brix conc. needed = ";VC; "gallons"
180 PRINT "Volume of ";BJ; "Brix juice needed = ";VJ; "gallons"
190 END
200 SPG= .0437691 *BB*EXP«BB +330.872) '2/ 170435!)
210 RETURN

10 'THIS PROGRAM DETN'S THE AVERAGE BRIX OF A BLEND


20 DIM B(80):
25 'MAXIMUM NUMBER OF BLEND COMPONENTS IS 80 IN THIS
PROGRAM. THE NUMBER CAN BE CHANGED IN STEPS 20-40.
30 DIM V(80)
40 DIM SPG(80)
50 N=N+ 1
60 PRINT "Brix of component ";N;
70 INPUT B(N)
75 IF B(N)=O THEN GOTO 130
80 PRINT "Volume of component ";N;
90 INPUT V (N)
95 SPG(N) = .0437691 *B(N)*EXP«B(N) +330.872 )'2/ 170435!)
100 Z=Z+V(N)*SPG(N)
110 V = V + V (N)
120 GOTO 50
130 N=N-l
135 PRINT" #"," BRIX", "VOL"
140 FOR 1=1 TO N
150 PRINT I,B(I),V(l)
160 NEXT
170 S=Z/V
180 BF=S*lO
190 B=BF
200 BF=S/( .0437691 *EXP( (B+330.872) '2/170435!»
210 IF ABS(BF-B)< .0001 THEN GOTO 230
220 GOTO 190
230 BF=CINT(BF*10)
240 BF=BF /10
250 PRINT "AVERAGE BRIX=";BF;TAB(21);"TOT VOL=";V
GWBASIC AND RPG PROGRAMS 421

10 'THIS PROGRAM DETN'S THE VOL NEEDED FOR ONE COMPONENT


20 'IN ADJUSTING A BLEND TO A SPECIFIC BRIX
30 DIM B(80)
40 DIM V(80)
50 DIM SPG(80)
60 INPUT "Final desired Brix";B
70 INPUT "Brix of component used to adjust Brix";BI
80 N=N+I
90 PRINT "Brix of component";N
100 INPUT B(N)
110 IF B(N) =0 THEN GOTO 200
120 PRINT "Volume of component";N;
130 INPUT YeN)
140 BB=B(N)
150 GOSUB 320
160 SPG(N)=SPG
170 Z=Z+V(N)*SPG(N)
180 V=V +V(N)
190 GOTO 80
200 N=N-I
210 BB=Bl
220 GOSUB 320
230SPG1=SPG
240 BB=B
250 GOSUB 320
260 VI=CINT«V*SPG-Z)/(SPGl-SPG))
270 PRINT" U"," BRIX", "VOL"
280 FOR 1=1 TO N
290 PRINT I,B(I),V(I)
300 NEXT
305 V=V+VI
310 PRINT "ADD VOLUME OF";Vl;"OF";BI;"BRIX COMPONENT"
311 PRINT "TO GET VOLUME OF";V;"OF";B;"BRIX PRODUCT"
315 END
320 SPG= ,0437691 *BB*EXP( (BB+330.872 )'2/ 170435!)
330 RETURN

10 'THIS PROGRAM CALCULATES THE UNCORRECTED BRIX NEEDED FROM THE EVAPORA-
TOR IN ORDER TO ACHIEVE A DESIRED GPL IN PROCESSING LEMON CONCENTRATE
20 INPUT "Uncorrected Brix of inbound lemon single strength juice"; UBJ
30 'IF REFRACT CORRECTS FOR TEMP, DISREGARD STEPS 40-60
40 INPUT "Temperature for Brix correction to lemon SSJ";T
50 BB=UBJ
60 GOSUB 340
70 INPUT "mls of NaOH titrated with SSJ";MLS
80 'IF NaOH NORMALITY IS ALWAYS 0.3125N THEN DISREGARD STEPS 90-110
90 INPUT "Normality of NaOH";N
100 IF N=O THEN N=.3125
110 MLS=MLS*N/.3125
422 APPENDIX B

120 INPUT "Weight of SSJ sample (lO.4g = IOmls)";W


130 ACID=MLS*2/W
140 AC=.014+ . 192*ACID-.00035*ACID'2
150 BJ =UBJ +AC+TC
160 INPUT "Desired GPL";GPL
170 INPUT "Temperature of concentrate for Brix correction";T
180 SPGJ = .0437691 *BJ*EXP( (BJ +330.872 )'2/ 170435!)
190 DENSITYJ = . 524484*EXP( (BJ +330.872) '2/ 170435!)
200 SPGC=GPL*SPGJ /( IO*ACID*DENSITYJ)
210 BF = IO*SPGC
220 B=BF
230 BF =SPGC /( .0437691 *EXP( (B+330.872 )'2/ 170435!)
240 IF ABS(B-BF» .0001 THEN GOTO 210
250 DENSITYC = . 524484*EXP( (BF+330.872) '2/ 170435!)
260 ACIDCON =GPL/( IO*DENSITYC)
270 ACCON= .014+ . I 92*ACIDCON -.00035*ACIDCON'2
280 BB=BF
290 GOSUB 340
300 EV APBRIX = CINT( (BF - ACCON - TC)* 10)
310 EV APBRIX = EV APBRIX / 10
320 PRINT' 'Uncorrected Brix for evaporator =" ;EV APBRIX
330 END
340 A=BB'2*( .0001425 -8.605E-06*T+7.138E,08*T'2)
350 AA=BB*( - .02009+ .001378*T-1.857E-05*T'2)
360 AAA=-.7788+.017*T+.0011*T'2
370 TC=A+AA+AAA

10 'THIS PROGRAM CALCULATES THE GPL OF LEMON CONCENTRATES


20 INPUT "Uncorrected Brix";UB
30 'IF REFRACT CORRECTS FOR TEMP, DISREGARD STEPS 40-80
40 INPUT "Temperature for Brix correction";T
50 A= UB'2*( .0001425 -8.605E-06*T+7.138E-08*T'2)
60 AA=UB*( -.02009+.001378*T-1.857E-05*T'2)
70 AAA= -.7788+.017*T+.0011*T'2
80 TC=A+AA+AAA
90 INPUT "mls NaOH titrated";MLS
100 'IF THE NORMALITY IS ALWAYS 0.3125N, THEN DISREGARD STEPS 110-130
110 INPUT "Normality of NaOH";N
120 IF N=O THEN N=.3125
130 MLS=MLS*N / .3125
140 INPUT "Weight of sample";W
150 ACID=MLS*2/W
160 AC=.014+.192*ACID-.00035*ACID'2
170 BRIX=UB+AC+TC
180 DENSITY = .524484*EXP«BRIX +330.872) '2/ 170435!)
190 GPL = CINT(ACID*DENSITY* 10)
200 PRINT "GPL =";GPL
210 INPUT "Desired GPL";DGPL
220 INPUT "Volume of high GPL concentrate";V
230 WATER=CINT(V*(GPL-DGPL)/GPL)
GWBASIC AND RPG PROGRAMS 423

240 PRINT "Water needed =";WATER


250 TOTAVOL=CINT(V +WATER)
260 PRINT "Total volume =";TOTALVOL

10 'THIS PROGRAM DETN'S THE AVERAGE B/A RATIO OF A BLEND


20 DIM B(80)
30 DIM R(80)
40 DIM V(80)
50 DIM SPG(80)
60N=N+I
70 PRINT "Brix of component ";N;
80 INPUT B(N)
90 IF B(N)=O THEN GO TO 190
100 PRINT "Ratio of component ";N;
110 INPUT R(N)
120 PRINT "Volume of component ";N;
130 INPUT V (N)
140 SPG(N)= .0437691 *B(N)*EXP( (B(N) +330.872) '2/170435!)
150 Z=Z+V(N)*SPG(N)
160 ZZ =ZZ + V(N)*SPG(N) /R(N)
170 V=V+V(N)
180 GOTO 60
190 N=N-I
200 PRINT" #"," BRIX", "RATIO", "VOL"
210 FOR 1=1 TO N
220 PRINT I,B(I),R(I), V(I)
230 NEXT
240 R=Z/ZZ
250 PRINT "AVERAGE RATIO = ";R;TAB(30);"TOT VOL=";V

10 'THIS PROGRAM DETN'S THE VOL NEEDED FOR ONE COMPONENT


20 'IN ADJUSTING A BLEND TO A SPECIFIC B / A RATIO
30 DIM B(80)
40 DIM R(80)
50 DIM V(80)
60 DIM SPG(80)
70 INPUT "Final desired Ratio";R
80 INPUT "Brix of component used to adjust ratio";BI
90 INPUT "Ratio of component used to adjust ratio";RI
100N=N+I
110 PRINT "Brix of component ";N;
120 INPUT B(N)
130 IF B(N)=O THEN GOTO 240
140 PRINT "Ratio of component ";N;
150 INPUT R(N)
160 PRINT "Volume of component ";N;
170 INPUT V (N)
180 BB=B(N)
190 GOSUB 370
200 SPG(N) = SPG
424 APPENDIX B

210 Z=Z+ V(N)*SPG(N)*( I /R -I /R(N))


220 V=V+V(N)
230 GOTO 100
240 N=N-I
250 BB=Bl
260 GOSUB 370
270 SPGI=SPG
280 VI =CINT(Z/(SPGl *( I /RI-I /R)))
290 PRINT" #" ," BRIX" , "RATIO", "VOL"
300 FOR 1=1 TO N
310 PRINT I,B(l),R(l),V(I)
320 NEXT
330 V=V+VI
340 PRINT "ADD VOLUME OF";VI;"OF";RI;"RATIO COMPONENT"
350 PRINT "TO GET VOLUME OF";V;"OF";R;"RATIO PRODUCT"
360 END
370 SPG= .0437691 *BB*EXP( (BB+330.872) '2/ 170435!)
380 RETURN

10 'THIS PROGRAM CALCULATES THE BRIX, ACID, AND RATIO FROM LABORATORY DATA
20 INPUT "Uncorrected Brix";UB
30 'IF AN AUTO TEMP CORRECTING REFRACT IS USED, DISREGARD STEPS 40-80
AND ANY REFERENCES TO "TC"
40 INPUT "Temperature for Brix correction";T
50 A=UB'2*( .0001425-8.605E-06*T+7 .138E-08*T'2)
60 AA=UB*( -.02oo9+.001378*T-1.857E-05*T'2)
70 AAA=-.7788+.017*T+.00II*T'2)
80 TC=A+AA+AAA
90 INPUT "mls of NaOH titrated";MLS
100 'IF THE NORMALITY OF THE NaOH IS ALWAYS 0.1562, DISREGARD STEPS 110-130
110 INPUT "Normality of NaOH";N
120 IF N =0 THEN N = .1562
130 MLS=MLS*N/.1562
140 INPUT "Weight of juice sample (1O.5g = 10 mls SSJ)";W
150 ACID=MLS/W
160 AC=.014+.192*ACID-.00035*ACID'2
169 'THE FOLLOWING FIXES THE CORRECT DECIMAL PLACES
170 BRIX=CINT((UB+AC+TC)*lO)
180 BRIX=BRIX/lO
190 ACID=CINT(ACID*100)
200 ACID=ACID/loo
210 RATIO = CINT((BRIX/ACID)* 10)
220 RATIO=RATIO/I0
230 PRINT BRIX; "Brix"
240 PRINT ACID;"% acid"
250 PRINT RATIO;"B/ A ratio"
260 INPUT "Desired Brix";DB
270 INPUT "Volume of high Brix juice"; V
280 SPGI= .0437691 *BRIX*EXP((BRIX +330.872) '2/ 170435!)
290 SPGF= .0437691 *DB*EXP( (DB+330.872)'2/ 170435!)
300 WATER=CINT(V*(SPGI-SPGF)/SPGF)
GWBASIC AND RPG PROGRAMS 425

310 PRINT "Water needed =";WATER


320 TOTALVOL =CINT(V + WATER)
330 PRINT "Total final volume =";TOTALVOL

10 'THIS PROGRAM CALCULATES THE AVERAGE BRIX AND RATIO OF A BLEND


20 DIM B(80)
30 DIM R(80)
40 DIM V(80)
50 DIM SPG(80)
60 N=N+I
70 PRINT "Brix of component ";N;
80 INPUT B(N)
90 IF B(N)=O THEN GOTO 190
100 PRINT "Ratio of component ";N;
110 INPUT R(N)
120 PRINT "Volume of component ";N;
130 INPUT V (N)
140 SPG(N) = .0437691 *B(N)*EXP( (B(N) +330.872) '2/ I 70435 ! )
150 Z=Z+V(N)*SPG(N)
160 ZZ = ZZ + V (N) *SPG(N) / R(N)
170 V=V+V(N)
180 GOTO 50
190 N=N-I
200 PRINT" #"," BRIX","RATlO","VOL"
210 FOR 1=1 TO N
220 PRINT I,B(I),R(I),V(I)
230 NEXT
240 SPG=Z/V
250 RATlO=CINT( IO*Z/ZZ)
260 RATlO=RATlO/1O
270 BF=SPG*IO
280 B=BF
290 BF=SPG /( .0437691 *EXP( (B+330.872) '2/ 170435!»
300 IF ABS(BF - B) < .0001 THEN GOTO 320
310 GOTO 280
320 BRIX=CINT(BF*IO)
330 BRIX=BRIX/IO
340 PRINT "AVG BRIX=";BRIX;SPC(3);"AVG RATlO=";RATIO;SPC(3);"TOT VOL=";V
350 INPUT "Desired Brix";DB
360 DSPG= .0437691 *DB*EXP( (DB+330.872) '2/ 170435!)
370 WATER=CINT(V*(SPG-DSPG)/DSPG)
380 PRINT WATER;" of water needed."
390 VT = CINT(W A TER + V)
400 PRINT "Total volume ="; VT
410 INPUT "Add more components (Y /N)";Q$
420 IF Q$ = "Y" THEN GOTO 60

10 'THIS PROGRAM CALCULATES FRUIT SAMPLE TEST RESULTS FOR ORANGES,


GRAPEFRUIT, AND TANGERINES
20 INPUT "net weight of fruit";WF
30 INPUT "net with of juice";WJ
426 APPENDIX B

40 INPUT "Uncorrected Brix";UB


50 'IF REFRACT CORRECTS FOR TEMP DISREGARD STEPS 60-100
60 INPUT "Temperature for Brix correction";T
70 A= UB'2*( .0001425 -8.60500IE-06*T+7.138E-08*T'2)
80 AA=UB*( -.02009+.001378*T-1.857E-05*T'2)
90 AAA= - .7788+ .017*T+.00ll *T'2
100 TC=A+AA+AAA
110 INPUT "mls NaOH titrated";MLS
120 'IF YOU ALWAYS USE A NORMALITY OF 0.1562 DISREGARD STEPS
130-150
130 INPUT "Normality of NaOH";N
140 IF N=O THEN N=.1562
150 MLS=MLS*Nj.1562
160 'IF 10 MLS OF JUICE ARE USED DISREGARD STEPS 170-200
170 INPUT "Weight of juice sample (10.5g = 10mls)";W
180 IF w=o THEN W=IO.5
190 ACID=CINT«MLS/W)*100)/100
200 AC= .014+ .192*ACID- .00035*ACID'2
210 BRIX=CINT«UB+AC+TC)*IO)/IO
220 RATIO = CINT«BRIX/ ACID)*IO)/IO
230 SOL = CINT( (20*WJ*.85*BRIX/WF)*IO) /10
240 DENSITY =4.37691 *EXP«BRIX +330.872) '2/ 170435!)
250 GAL=CINT( (2000*WJ*.85 /(WF*DENSITY»*IO) / 10
260 PEEL = CINT( 2000*(WF - WJ) /WF)
270 PRINT BRIX;" Brix",ACID;" % acid",RATIO;" B/ A ratio"
280 PRINT SOL;" Ibs sol/ton", GAL;" gal/ton" ,PEEL;" Ibs peel/ton"
290 INPUT "net weight of fruit in load";NW
300 TGAL=CINT(GAL*NW /2000)
310 TSOL=CINT(SOL*NW /2000)
320 TPEEL= CINT(PEEL*NW /2000)
330 PRINT TSOL;" Ibs solid",TGAL;" gallons",TPEEL;" Ibs peel"

10 'THIS PROGRAM CALCULATES LEMON OR LIME FRUIT SAMPLE TEST RESULTS


20 INPUT "net weight of fruit";WF
30 INPUT "net weight of juice";WJ
40 INPUT "Uncorrected Brix";UB
50 'IF REFRACT CORRECTS FOR TEMP DISREGARD STEPS 60-100
60 INPUT "Temperature for Brix correction";T
70 A= UB'2*( .0001425 -8.60500IE-06*T+ 7.138E-08*T'2)
80 AA=UB*( -.02009+.001378*T-1.857E-05*T'2)
90 AAA= -.7788+.017*T+.001l*T'2
100 TC=A+AA+AAA
110 INPUT "mls NaOH titrated";MLS
120 'IF YOU ALWAYS USE A NORMALITY OF 0.3125 DISREGARD STEPS 130-150
130 INPUT "Normality of NaOH";N
140 IF N=O THEN N=.3125
150 MLS=MLS*Nj.3125
160 'IF 10 MLS OF JUICE ARE USED DISREGARD STEPS 170-200
170 INPUT "Weight of juice sample (1O.5g = 10mls)";W
180 IF W=O THEN W=IO.5
190 ACID =CINT« MLS*2 /W)* 100) /100
GWBASIC AND RPG PROGRAMS 427

200 AC=.014+ . 192*ACID- .00035*ACID"2


210 BRIX=CINT«UB+AC+TC)*1O)/l0
220 DENSITY =4.37691 *EXP«BRIX+330.872) "2/170435!)
230 APT:CINT«20*WJ*ACID*.78/WF)*1O)/1O
240 GPT:CINT«2000*WJ*.78/(WF*DENSITY»*1O)/1O
250 PEEL=CINT(2000*(WF-WJ)/WF)
260 PRINT
270 PRINT BRIX;"Brix";SPC(3);ACID;"% acid";SPC(3);APT;"lbs
acid/ton";SPC(3);GPT; "gal/ton"
280 PRINT
290 PRINT TAB(20);PEEL;"lbs peel/ton"
295 PRINT
300 INPUT "net weight of load" ; NW
310 TAPT= CINT(APT*NW /2000)
320 TGPT= CINT(GPT*NW /2000)
330 TPEEL=CINT(PEEL*NW /2000)
340 PRINT
350 PRINT TAPT; "lbs acid";SPC(3);TGPT; "gallons";SPC(3);TPEEL; "lbs peel"
360 PRINT

10 'THIS PROGRAM DETN'S THE AVG OIL AND OIL ADJUSTMENT OF A BLEND
20 DIM B(80)
25 DIM 0(80)
30 DIM V(80)
35 DIM SPG(80)
50 N=N+l
60 PRINT "Brix of component ";N;
70 INPUT B(N)
75 IF B(N) =0 THEN GOTO 130
76 PRINT "% oil of component ";N;
77 INPUT O(N)
78 O(N)=CINT( looo*O(N»/I000
80 PRINT "Volume of component ";N;
90 INPUT YeN)
95 SPG(N)=.0437691 *B(N)*EXP( (B(N)+330.872 )"2/ 170435!)
100 Z=Z+V(N)*SPG(N)
105 ZZ=ZZ+ V(N) *SPG(N) *O(N)
110 V=V+V(N)
120 GOTO 50
130 N=N-l
135 PRINT" #"," BRIX"," OIL", "VOL"
140 FOR 1=1 TO N
150 PRINT I,B(I),O(I),V(I)
160 NEXT
170 S=Z/V
1750=CINT(l000*ZZ/Z)/1OOO
180 BF=S*1O
190 B=BF
200 BF=S!( .0437691 *EXP( (B+330.872) "2/170435!»
210 IF ABS(BF-B)< .0001 THEN GOTO 230
220 GOTO 190
428 APPENDIX B

230 BF=CINT(BF*IO)/IO
250 PRINT "AVG BRIX = ";BF;SPC(3);"AVG OIL = ";0;SPC(3);"TOT VOL=";V
255 INPUT "Do you want to add oil (Y /N)";Q$
256 IF Q$ = "N" THEN END
260 INPUT "Desired final oillevel";OF
261 INPUT "Is volume in drums (52-gallon)(Y /N)";Q$
265 IF Q$="Y" THEN DD=52 ELSE DD=I
2700A=CINT«OF-0)*36.19*S*V*DD)
280 PRINT "Oil needed = ";OA
290 INPUT "mls oil enhancer needed per specification";OE
295 0I=OF-OE/(V*S*36.19*DD)
300 IF OA> =OE THEN PRINT "mls oil enhancer needed = ";OA: END
310 INPUT "Can the total volume of the blend change (Y /N)";Q$
330 INPUT "Number of blend component you wish to exchange";NN
340 FOR J = I TO N
350 ZZZ = ZZZ + SPG(J)*V(J)*(OI -0(1))
360 NEXT
370 ZZZ=ZZZ-SPG(NN)*V(NN)*(OI-O(NN»
375 01 =CINT«OI + ZZZ/(SPG(NN)*V(NN»)*lOoo) / 1000
380 IF Q$="N" THEN PRINT "% oil needed in component";NN;" =";01
390 V I = CINT(ZZZ / (O(NN)*SPG(NN)*( 1 - 01 /O(NN))))
400 IF Q$="Y" THEN PRINT "Volume needed in component";NN;" = ";VI
410 ZZZ=O
420 GOTO 310

10 'THIS PROGRAM DETN'S THE AVG PULP AND PULP ADJUSTMENT OF A BLEND
20 DIM B(80)
25 DIM P(80)
30 DIM V(80)
35 DIM SPG(80)
50 N=N+l
60 PRINT "Brix of component ";N;
70 INPUT B(N)
75 IF B(N)=O THEN GOTO 130
76 PRINT" % pulp of component ";N;
77 INPUT peN)
7 8 peN) = CINT( 1000*0(N» / 1000
80 PRINT "Volume of component ";N;
90 INPUT YeN)
95 SPG(N)= .0437691 *B(N)*EXP«B(N) +330.872 (2/ 170435!)
100 Z2 = Z2 + V (N)*SPG(N)
105 ZI =Zl + V(N)*SPG(N)*P(N)
120 GOTO 50
130 N=N-I
135 PRINT " #"," BRIX"," PULP", "VOL"
140 FOR 1=1 TO N
150 PRINT I,B(I),P(I),V(I)
160 NEXT
170 PAVG=ZI/Z2
250 PRINT "AVG PULP=";PAVG;SPC(3);"TOT VOL=";V
310 INPUT "Can the total volume of the blend change (Y /N)";Q$
GWBASIC AND RPG PROGRAMS 429

330 INPUT "Number of blend component you wish to exchange";NN


340 FORJ=1 TO N
350 Z3=Z3 +SPG(J)*V(J)*(PAVG- P(J»
360 NEXT
370 Z3=Z3-SPG(NN)*V(NN)*(PAVG-P(NN))
375 PNN=CINT«PAVG+Z3 /(SPG(NN)*V(NN»)*I000)/ 1000
380 IF Q$= "N" THEN PRINT" % pulp needed in component";NN;" = ";PNN
390 VNN =CINT(Z3 / (P(NN)*SPG(NN)*( 1 - PA VG /P(NN))))
400 IF Q$= "Y" THEN PRINT "Volume needed in component";NN;" = ";VNN
410 Z3=O
420 GOTO 310

10 'THIS PROGRAM DETN'S THE AVERAGE LIMONIN AND LIMONIN ADJUSTMENT


OF A BLEND
20 DIM B(80)
25 DIM L(80)
30 DIM V(80)
35 DIM D(80)
50 N=N+l
60 PRINT "Brix of component ";N;
70 INPUT B(N)
75 IF B(N) =0 THEN GOTO 130
76 PRINT "limonin of component ";N;
77 INPUT L(N)
78 peN) =CINT( l000*O(N)) / 1000
80 PRINT "Volume of component ";N;
90 INPUT YeN)
95 D(N) =4.37691 *EXP«B(N) +330.872) A2/170435!)
100 Z2=Z2+V(N)*D(N)
105 ZI =21 + V(N)*D(N)*L(N)
120 GOTO 50
130 N=N-l
135 PRINT" #"," BRIX"," LIM ","VOL"
140 FOR 1= I TO N
150 PRINT I,B(I),LI),V(l)
160 NEXT
170 LAVG=21/22
250 PRINT "AVG LIMONIN=";LAVG;SPC(3);"TOT VOL=";V
310 INPUT "Can the total volume of the blend change (Y /N)";Q$
330 INPUT "Number of blend component you wish to exchange";NN
340 FOR J=1 TO N
350 Z3 =Z3+ D(J)*V(J)*(LA VG - L(J»
360 NEXT
370 Z3 =Z3 - D(NN)*V(NN)*(LAVG- L(NN))
375 LNN =CINT«LAVG+Z3 /(D(NN)*V(NN)))*1000)/ 1000
380 IF Q$="N" THEN PRINT "Iimonin needed in component";NN;" = ";LNN
390 VNN =CINT(Z3 / (L(NN)*D(NN)*(1- LAVG /L(NN))))
400 IF Q$= "Y" THEN PRINT "Volume needed in component";NN;" = ";VNN
410 Z3=0
420 GOTO 310
Appendix C

HP-41 C Programs

The following HP-41C or HP-41CV programs can best be used by assigning the pro-
grams to convenient keys using the ASN function. Then the program will activate when
the calculator is in the USER mode. The programs are designed for the calculator to be
alloted 53 storage registers using the SIZE function (SIZE 053). Included with each
program is a brief explanation of how to use the program. It is assumed that the user is
familer with the HP-41C program language. Most programs are self-explanatory. You
enter the data when prompted. Consult the text and relevant flow charts for program
logic and the objectives of the programs.

PROGRAM TO ADJUST BRIX USING WATER OR HIGHER BRIX


CONCENTRATE

This program will calculate the parameters needed to adjust a full tank of juice to the
proper Brix by adding either water or higher Brix concentrate. If no entry is made for
the needed Brix, the program defaults to 11.8 °Brix. If the prompt does not apply, enter
nothing.

1. LBL HILOBX 16. PROMPT 31. RCL 46


2. 11.8 17. STO 47 32.
3. BRIX NEEDED? 18. RCL 44 33. /
4. TONE 5 19. XEQ 02 34. RCL47
5. PROMPT 20. STO 44 35. X
6. ST044 21. RCL 45 36. ST044
7. HI BRIX? 22. XEQ 02 37. FIX 0
8. PROMPT 23. STO 45 38. LBL03
9. STO 45 24. RCL 46 39. GAL HI=
10. 0 25. XEQ 02 40. ARCL 44
11. LOW BRIX? 26. STO 46 41. TONE 5
12. PROMPT 27. RCL 44 42. TONE 7
13. STO 46 28. RCL46 43. TONE4
14. TOT GAL? 29. 44. TONE 6
15. LBL 01 30. RCL 45 45. PROMPT

430
HP-41 C PROGRAM 431

46. RCL 47 56. GTO 03 66. X'2


47. RCL 44 57. LBL 04 67. 170435
48. - 58. WATER= 68. I
49. STO 45 59. ARCL 45 69. E' x
50. RCL 46 60. PROMPT 70 .. 0437691
51. X=O? 61. GT003 71. X
52. GTO 04 62. LBL02 72. RCLOO
53. GAL LO= 63. STOOO 73. X
54. ARCL 45 64. 330.872 74. END
55. PROMPT 65. +

PROGRAM THAT CALCULATES THE BRIX. ACID. AND RATIO FROM


LAB DATA

This program will calculate the Brix, % acid, and B / A ratio from laboratory results. No
entry when you are prompted for the temperature causes the program to default to 20°C
or to apply no temperature correction to the Brix. If nothing is entered for the normality,
the default is 0.1562N. This can be changed in the program to 0.3125N if desired. If no
entry is made when you are prompted for the sample weight, a weight of 10.5 g (10 ml
of SSJ) will be assumed.

1. LBL BAR 25. RCL49 49. LBL 01


2. UNCOR BRIX? 26. 1.857 E-5 50. MLS NaOH?
3. TONE 5 27. X 51. PROMPT
4. PROMPT 28. RCL 48 52. STO 48
5. STO 44 29. 1.378 E-3 53 .. 1562
6. 0 30. X 54. NaOH NORMAL?
7. TEMP-DEG C? 31. 55. PROMPT
8. PROMPT 32. CHS 56. RCL48
9. X=O? 33. .02009 57. X
10. GTO 01 34. - 58 . . 1562
11. STO 48 35. RCL44 59. I
12. X'2 36. X 60. STO 48
13. STO 49 37. + 61. 10.5
14. 7.138 E-8 38. RCL 49 62. WT mc SAMP?
15. X 39 .. 0011 63. PROMPT
16. RCL 48 40. X 64. RCL 48
17. 8.605 E-6 41. RCL 48 65. I
18. X 42 .. 017 66. 1/X
19. 43. X 67. STO 45
20. 1.425 E-4 44. + 68. 11.7
21. + 45 .. 7788 69. X>Y?
22. RCL 44 46. 70. GTO 03
23. X'2 47. + 71. X< >?
24. X 48. ST + 44 72. X'2
432 APPENDIX C

73. 1.9537 E-4 87. X 101. % ACID=


74. X 88. .01267 102. ARCL45
75. RCL 45 89. + 103. PROMPT
76 .. 184836815 90. ST + 44 104. RCL44
77. X 91. LBL02 105. RCL45
78. 92. FIX 1 106. /
79 . . 085917569 93. BRIX= 107. STO 43
80. 94. ARCL44 108. FIX 1
81. CHS 95. TONE 6 109. RATIO=
82. ST + 44 96. TONE 7 110. ARCL 43
83. GT002 97. TONE 4 Ill. PROMPT
84. LBL03 98. TONE 5 112. GOT002
85. X< >Y? 99. PROMPT 113. END
86 . . 19 100. FIX 2

SET OF PROGRAMS THAT ALLOWS ONE TO ENTER. DELETE.


CORRECT. AND VIEW BLEND COMPONENTS AND CALCULATE THE
AVERAGE BRIX AND RATIO

Each program below should be assigned a USER key. The BLD G?D program sets the
volume mode of the blend. Gallons mode assumes all volumes are in gallons. Gal/drums
mode assumes that all volumes less than 52 represent the number of 52-gallon drums,
and all volumes 52 or over are gallons. For example, an entry of 45 would mean 45
drums of concentrate, whereas 58 would be taken as 58 gallons of concentrate. This
allows the blending from bulk tanks and drums simultaneously without conversion of
one quantity to the volume units of the other. Each component is numbered and appears
in the prompts and displays. In the view program, if you enter nothing when prompted
for the number of the blend component desired, the default is the first component. The
calculator then will automatically step through the entered blend components for com-
parison to a blend manifest. You can add, delete, correct, or view blend components at
any time by using the separate assigned USER keys. The blend calculation takes a few
minutes. The calculation program also will prompt for the desired Brix and will calculate
the water needed in the blend, as well as the resulting final volume of the blend.

Entering Blend 11. T (BLANK) 23. ARCL 51


Component Data 12. ASTO 51 24. ARCL 41
1. LBLBLD ENT 13. FX?02 25. PROMPT
2. FS?C 01 14. GTO 02 26. 1 E2
3. GT003 15. FIX 0 27. /
4. FS? 03 16. GAL/DRUMS? 28. +
5. GT004 17. LBL 01 29. RATIO?
6. CLRG 18. TONE 3 30. ARCL 51
7. LBL03 19. ARCL 51 31. ARCL 41
8. 20. ARCL41 32. PROMPT
9. ST + 41 21. PROMPT 33. 1 E5
10. LBL04 22. BRIX? 34. /
HP-41 C PROGRAM 433

35. + 16. GTO 02 6. TONE 3


36. FS?C 03 17. STO IND 42 7. PROMPT
37. RTN 18. 8. 1
38. STO IND 41 19. ST + 42 9. -
39. GTO 03 20. GTOOI 10. ST042
40. LBL 02 21. LBL02 11. LBL 01
41. FIX 0 22. 12. 1
42. GALLONS? 23. ST - 41 13. ST + 42
43. GTO 01 24. 0 14. RCL IND 42
44. END 25. STO IND 42 15. INT
26. STO 42 16. ST043
Sets Gallons or 27. SF 01 17. X=O?
Drum/Gallons Mode 28. GTO BLD VU 18. GTOO2
1. LBL BLD G?D 29. END 19. RCL IND 42
2. FS? 02 20. FRC
3. GTO 01 Correcting Blend 21. 1 E3
4. SF 02 Component Data 22. X
5. GALLONS MODE 1. LBL BLD COR 23. INT
6. TONE 9 2. ITEM NO? 24. 10
7. PROMPT 3. PROMPT 25. /
8. GTO BLD G?D 4. RCL 41 26. ST044
9. LBL 01 5. ST042 27. RCL IND 42
10. CF 02 6. x<>y 28. 1 E3
11. GAL/DRM MODE 7. STO 41 29. X
12. TONE 3 8. SF 03 30. FRC
13. PROMPT 9. XEQ BLD ENT 31. 1 E2
14. GTOBLDG?D 10. STO IND 41 32. X
15. END 11. RCL41 33. STO 45
T
12. ST043 34. -
Add or Delete Blend 13. RCL42 35. ASTO 46
T
Component Data 14. ST041 36. ,
1. LBL BLD ADD 15. RCL43 37. ASTO 47
2. 1 16. ST042 38. CLA
3. ST - 41 17. SF 01 39. FIX 0
4. SF 01 18. 40. ARCL 42
5. GTO BLD ENT 19. ST - 42 41. ARCL 46
6. LBL BLD DEL 20. GTOBLD VU 42. ARCL 43
7. ITEM NO? 21. END 43. ARCL 51
8. PROMPT 44. FIX 1
9. STO 42 Viewing Blend 45. ARCL 44
lO. STO 43 Components 46. ARCL 47
11. LBLOI 1. LBL BLD VU 47. ARCL 45
12. 2. FS?C 01 48. TONE 7
13. ST + 43 3. GTOOl 49. AVIEW
14. RCL IND 43 4. 1 50. PSE
15. X=O? 5. START NO? 51. GTOOI
434 APPENDIX C

52. LBL 02 39. 170435 85. -


53. NO MORE DATA 40. / 86. ABS
54. PROMPT 41. EA x 87 .. 1
55. GTO BLD VU 42 ..0437691 88. x> Y?
56. END 43. X 89. GT006
44. RCLoo 90. RCL49
Calculation of Avg Brix 45. X 91. STO 00
and Ratio 46. STO 45 92. GT005
1. LBL BLD CAL 47. RCL 43 93. LBL 06
2. 0 48. X 94. FIX 1
3. STO 42 49. ST + 46 95. RCL 49
4. ST044 50. RCL IND 42 96. FIXO
5. STO 46 51. 1 E3 97. CLA
6. STO 47 52. X 98. ARCL44
7. CF 01 53. FRC 99. ARCL 51
8. LBL 01 54. 1 E2 100. FIX 1
9. 1 55. X 101. ARCL49
10. ST + 42 56. RCL 43 102. ARCL 51
11. RCL41 57. / 103. FS?C 05
12. 1 58. l/X 104. GTO 07
13. - 59. RCL 45 105. RCL47
14. RCL42 60. X 106. l/X
15. X> Y? 61. ST + 47 107. RCL 44
16. GTO 04 62. GTO 01 108. X
17. RCL IND 42 63. LBL 04 109. RCL 48
18. INT 64. 0 110. X
19. FS? 02 65. STO 42 111. STO 47
20. GTO 03 66. RCL46 112. LBL 07
21. 52 67. RCL 44 113. ARCL47
22. X< >Y 68. / 114. BEEP
23. X< =Y? 69. STO 48 115. PROMPT
24. XEQ 02 70. LBL 05 116. 0
25. LBL 03 71. RCL 00 117. BRIX NEEDED?
26. STO 43 72. 330.872 118. PROMPT
27. ST + 44 73. + 119. X=O?
28. RCL IND 42 74. XA2 120. 60
29. FRC 75. 170435 121. STO 00
30. 1 E3 76. / 122. 330.872
31. X 77. EAx 123. +
32. INT 78 .. 0437691 124. XA2
33. 10 79. X 125. 170435
34. / 80. RCL48 126. /
35. STO 00 81. / 127. EAx
36. 330.872 82. l/X 128. .0437691
37. + 83. STO 49 129. X
38. XA2 84. RCL 00 130. RCL 00
HP-41 C PROGRAM 435

131. X 145. RCL45 159. FRC


132. STO 50 146. RCL44 160. 1 E2
133. RCL 48 147. + 161. X
134. - 148. ST045 162. X=O?
135. CHS 149. TOT GAL= 163. GTO 08
136. RCL 50 150. ARCL45 164. RCL43
137. / 151. PROMPT 165. X
138. RCL 44 152. SF 02 166. GTO 03
139. X 153. GTO 06 167. LBL08
140. STO 45 154. LBL 02 168. RCL43
141. WATER= 155. ST043 169. 52
142. FIX 0 156. RCL IND 42 170. X
143. ARCL 45 157. 1 E6 171. END
144. PROMPT 158. X

FRUIT SAMPLE CALCULATIONS

This program can be used to calculate fruit sample data for oranges, tangerines, grape-
fruit, or other citrus fruit except lemons and limes. The default temperature for the
temperature correction to the Brix is, again, 20 C or no temperature correction. The
D

default normality is 0.1562, and the default sample weight is 10.5 g (10 ml SSJ).

1. LBL ORG FRT 24. X 47. RCL 48


2. WT OF FRUIT? 25. - 48 .. 017
3. TONE 9 26. 1.425 E-4 49. X
4. PROMPT 27. + 50. +
5. STO 42 28. RCL44 51. .7788
6. WT OF JUICE? 29. X'2 52. -
7. PROMPT 30. X 53. +
8. STO 50 31. RCL49 54. ST + 44
9. UNCOR. BRIX? 32. 1.857 E-5 55. LBL03
10. PROMPT 33. X 56. MLS NaOH?
11. ST044 34. RCL48 57. PROMPT
12. 0 35. 1.378 E-3 58. STO 48
13. TEMP-DEG C? 36. X 59. 10.5
14. PROMPT 37. - 60. WT SAMPLE?
15. X=O? 38. CHS 61. PROMPT
16. GT003 39 .. 02009 62. RCL48
17. STO 48 40. - 63. /
18. X'2 41. RCL44 64. l/X
19. STO 49 42. X 65. STO 45
20. 7.138 E-8 43. + 66 .. 19
21. X 44. RCL49 67. X
22. RCL48 45 .. 0011 68 . .01267
23. 8.605 E-6 46. X 69. +
436 APPENDIX C

70. ST + 44 94. X 118. RCL 42


71. LBL02 95. l/X 119. RCL 50
72. FIX 1 96. RCL 50 120.
73. BRIX= 97. X 121. RCL 42
74. ARCL44 98. RCL 42 122. /
75. TONE 6 99. / 123. 2 E3
76. TONE 6 100. 2000 124. X
77. TONE 7 101. X 125. FIX 0
78. TONE 9 102 .. 85 126. STO 48
79. PROMPT 103. X 127. PEEL/TN=
80. FIX 2 104. STO 46 128. ARCL 48
81. % ACID= 105. FIX 2 129. PROMPT
82. ARCL45 106. GAL/TN= 130. GT002
83. PROMPT 107. ARCL 46 131. LBLOI
84. RCL44 108. PROMPT 132. RCL44
85. RCL 45 109. XEQ 01 133. 330.872
86. / 110. RCL 44 134. +
87. STO 43 111. X 135. X'2
88. FIX 1 112. RCL 46 136. 170435
89. RATIO= 113. X 137. /
90. ARCL 43 114. STO 47 138. E'x
91. PROMPT 115. SOL/TN= 139 . . 043769
92. XEQ 01 116. ARCL 47 140. X
93. 100 117. PROMPT 141. END

CALCULATION OF AVERAGE OIL OR PULP

This program will calculate the average % oil or % pulp in a blend, as the two calcu-
lations are similar. The difference between oil and pulp is determined by the magnitude
of their values. The Brix of each component must be entered, as well as the % oil or
pulp. The volume prompt assumes that all units are the same (all drums or all gallons).
When all the components have been entered, enter nothing, press R/S, and the weighted
average % oil or pulp will appear.

1. LBL AVG O/P 13. PROMPT 25. PROMPT


2. 0 14. X=O? 26. DRMS/GALS?
3. STO 42 15. GTO 02 27. ARCL44
4. ST043 16. 1 28. PROMPT
5. ST044 17. X< >y 29. RCL 45
6. LBLOI 18. X=Y? 30. X
7. 1 19. GTO 04 31. ST + 42
8. ST + 44 20. XEQ 03 32. X
9. FIX 0 21. STO 45 33. ST + 43
10. BRIX? 22. LBL 04 34. GTO 01
11. ARCL 44 23. % OIL/PLP? 35. LBL 02
12. TONE 9 24. ARCL44 36. FIX 3
HP-41 C PROGRAM 437

37. RCL 43 46. ARCLOO 55. 170435


38. RCL 42 47. BEEP 56. /
39. / 48. PROMPT 57. E' x
40 .. 1 49. GTO AVG O/P 58 .. 0437691
41. X<=Y? 50. LBL 03 59. X
42. FIX 1 51. STO 00 60. RCL 00
43. X< >Y 52. 330.872 61. X
44. STO 00 53. + 62. END
45. WT AVG= 54. X'2

LEMON/LIME FRUIT SAMPLE CALCULATIONS

This program calculates the fruit sample information for lemons and limes. The default
for temperature is, again, 20°C; the default for the NaOH normality is 0.1562; and the
default for the sample weight is 10.5 g.

1. LBL LEM FRT 30. X 59 . . 1562


2. WT OF FRUIT? 31. RCL 49 60. NaOH NORMAL?
3. TONE 8 32. 1.857 E-5 61. PROMPT
4. PROMPT 33. X 62. RCL48
5. ST047 34. RCL 48 63. X
6. WT OF JUICE? 35. 1.378 E-3 64 .. 1562
7. PROMPT 36. X 65. /
8. STO 46 37. - 66. STO 48
9. UNCOR. BRIX? 38. CHS 67. 10.5
10. PROMPT 39 .. 02009 68. WT SAMPLE?
11. STO 44 40. - 69. PROMPT
12. 0 41. RCL 44 70. RCL48
13. TEMP-DEG C? 42. X 71. /
14. PROMPT 43. + 72. I/X
15. X=O? 44. RCL 49 73. ST045
16. GTO 01 45 .. 0011 74. 11.7
17. STO 48 46. X 75. X> Y?
18. X'2 47. RCL 48 76. GTO 03
19. STO 49 48 .. 017 77.X<>Y
20. 7.138 E-8 49. X 78. X'2
21. X 50. + 79. 1.9537 E-4
22. RCL 48 51. .7788 80. X
23. 8.605 E-6 52. - 81. RCL 45
24. X 53. + 82 . . 184836815
25. - 54. ST + 44 83. X
26. 1.425 E-4 55. LBLOI 84.-
27. + 56. MLS NaOH? 85 . . 085917569
28. RCL 44 57. PROMPT 86. -
29. X'2 58. STO 48 87. CHS
438 APPENDIX C

88. ST + 44 112. X 136. RCL 49


89. GT002 113. RCL47 137. /
90. LBL03 114. / 138. I/X
91. x<>y 115. 20 139. STO 48
92 . . 19 116. X 140. FIX 2
93. X 117. .78 141. GAL/TON=
94 . . 01267 118. X 142. ARCL 48
95. + 119. ST049 143. PROMPT
96. ST + 44 120. LBL 05 144. RCL 47
97. LBL02 121. FIX 2 145. RCL46
98. FIX 1 122. ACID/TN= 146.
99. BRIX= 123. ARCL 49 147. RCL47
100. ARCL 44 124. PROMPT 148. /
101. TONE 7 125. RCL 44 149. 2000
102. TONE 9 126. 330.872 150. X
103. TONE 6 127. + 151. FIX 0
104. TONE 7 128. X'2 152. STO 50
105. PROMPT 129. 170435 153. PEEL/TN =
106. FIX 2 130. / 154. ARCL 50
107. % ACID= 131. E'x 155. PROMPT
108. ARCL 45 132 .. 0437691 156. GT002
109. PROMPT 133. X 157. END
110. RCL45 134. RCL 45
111. RCL46 135. X

CALCULATION OF UNCORRECTED BRIX NEEDED DURING


EVAPORATION OF LEMON/LIME CONCENTRATES IN ORDER TO
ACHIEVE A DESIRED GPL

This program will calculate the uncorrected Brix needed by evaporator operators in order
to concentrate lemon or lime juices to a desired GPL level. The temperature, normality,
and sample weight defaults are as before-20°C, 0.1562N, and 10.5 g, respectively.
The default for the desired GPL is 400,GPL. If you want to subtract an acid correction
from the Brix observed by the evaporator operator, then enter the temperature of the
concentrate observed by the refractometer.

1. LBL LEM BRX 10. GTO 01 19. RCL 48


2. LEM SSJ BRX? 11. XEQ 10 20. X
3. TONE 6 12. LBL 01 21. .1562
4. PROMPT 13. MLS NaOH? 22. /
5. ST044 14. PROMPT 23. STO 48
6. 0 15. STO 48 24. 10.5
7. TEMP-DEG C? 16 .. 1562 25. WT SAMPLE?
8. PROMPT 17. NaOH NORMAL? 26. PROMPT
9. X=O? 18. PROMPT 27. RCL 48
HP-41C PROGRAM 439

28. / 74. / 120. RCL 46


29. I/X 75. I/X 121. .184836815
30. STO 45 76. RCL 42 122. X
31. 11.7 77. RCL 44 123. -
32. X> Y? 78. X 124. .085917569
33. GTO 03 79. X 125. -
34. X< >Y 80. STO 43 126. CHS
35. XA2 81. 10 127. GTO 04
36. 1.9537 E-4 82. X 128. LBL 08
37. X 83. STO 00 129.X<>Y
38. RCL 45 84. LBL 07 130 .. 19
39 .. 184836815 85. XEQ 05 131. X
40. X 86. RCL 43 132 .. 01267
41. - 87. / 133. +
42 .. 085917569 88. l/X 134. LBL 04
43. - 89. STO 50 135. ST - 50
44. CHS 90. RCL 00 136. 0
45. ST + 44 91. - 137. CONC TEMP?
46. GT002 92. ABS 138. PROMPT
47. LBL 03 93 .. 1 139. X=O?
48. X< >Y 94. X>Y? 140. GTO 09
49 .. 19 95. GTO 06 141. XEQ 10
50. X 96. RCL 50 142. LBL09
51. .01267 97. STO 00 143. FIX 1
52. + 98. GTO 07 144. ST - 50
53. ST + 44 99. LBL 06 145. EVAP BRIX=
54. LBL 02 100. RCL 50 146. ARCL 50
55. 400 101. STO 00 147. TONE 7
56. DESIRED GPL? 102. XEQ 05 148. TONE 9
57. PROMPT 103. 100 149. TONE 8
58. 10 104. X 150. TONE 9
59. / 105. 453.59237 151. PROMPT
60. STO 47 106. X 152. GTO LEM BRX
61. RCL 44 107. 3785.306 153. LBL 05
62. STO 00 108. / 154. RCL 00
63. XEQ 05 109. RCL47 155. 330.872
64. STO 42 110. / 156. +
65. 100 111. I/X 157. XA2
66. X 112. 11.7 158. 170435
67. 453.59237 113. X>Y? 159. /
68. X 114. GTO 08 160. EAx
69. 3785.306 115. X< >Y 161 .. 0437691
70. / 116. STO 46 162. X
71. RCL 45 117. XA2 163. RTN
72. X 118. 1.9537 E-4 164. LBL 10
73. RCL 47 119. X 165. STO 48
440 APPENDIX C

166. X~2 179. RCL 49 192. RCL49


167. STO 49 180. 1.857 E-3 193 . . 0011
168. 7.138 E-8 181. X 194. X
169. X 182. RCL 48 195. RCL 48
170. RCL 48 183. 1.378 E-3 196 . . 017
171. 8.605 E-6 184. X 197. X
172. X 185. - 198. +
173. - 186. CHS 199. .7788
174. 1.425 E-4 187 .. 02009 200.
175. + 188. - 201. +
176. RCL44 189. RCL 44 202. ST + 44
177. X'2 190. X 203. END
178. X 191. +

CALCULATION OF LEMON/LIME GPL

This program calculates the GPL from Brix and acid measurements. The temperature,
normality, sample weight, and desired GPL defaults are 20°C, 0.3125N, 10.5 g, and
400 GPL, respectively. Any volumes can be used, but you must use the same units
throughout the calculation. The program also calculates the water needed to adjust high
GPL concentrates or juices.

1. LBL LEM GPL 24. X 47. +


2. UNCOR. BRlX? 25. RCL 49 48. ST + 44
3. TONE 8 26. 1.857 E-3 49. LBLOI
4. PROMPT 27. X 50. MLS NaOH?
5. STO 44 28. RCL48 51. PROMPT
6.0 29. 1.378 E-3 52. STO 48
7. TEMP-DEG C? 30. X 53 . . 3125
8. PROMPT 31. 54. NaOH NORMAL?
9. X=O? 32. CHS 55. PROMPT
10. GTO 01 33 .. 02009 56. RCL48
11. STO 48 34. 57. X
12. X'2 35. RCL 44 58 . . 1562
13. STO 49 36. X 59. /
14. 7.138 E-8 37. + 60. STO 48
15. X 38. RCL49 61. 10.5
16. RCL 48 39 ..0011 62. WT SAMPLE?
17. 8.605 E-6 40. X 63. PROMPT
18. X 41. RCL 48 64. RCL 48
19. 42 . .017 65. /
20. 1.425 E-4 43. X 66. l/X
21. + 44. + 67. STO 45
22. RCL44 45. .7788 68. 11.7
23. X'2 46. 69. X>Y?
HP-41 C PROGRAM 441

70. GTO 02 88 .. 01267 106. /


71.X<>Y 89. + 107. RCL 45
72. X"2 90. ST + 44 108. X
73. 1.9537 E-4 91. LBL 03 109. 10
74. X 92. RCL 44 110. X
75. RCL 45 93. 330.872 111. FIX 0
76 .. 184836815 94. + 112. STO 42
77. X 95. X"2 113. LEM GPL=
78. - 96. 170435 114. ARCL 42
79 .. 085917569 97. / 115. TONE 6
80. - 98. E"x 116. TONE 4
81. CHS 99 ..0437691 117. TONE 3
82. ST + 44 100. X 118. TONE 6
83. GTO 03 101. 100 119. PROMPT
84. LBL 02 102. X 120. GTO LEM GPL
85. X< >Y 103. 453.59237 121. END
86 .. 19 104. X
87. X 105. 3785.306

CALCULATION OF WATER NEEDED TO DILUTE JUICE TO A DESIRED


BRIX

This program is convenient when dilution to a desired Brix is all that is wanted. The
default desired Brix is 11.8°Brix. Any units of volume can be used as long as they are
consistent.

1. LBL ORG DIL 18. PROMPT 35. PROMPT


2. HIGH BRIX? 19. STO 47 36. GTO ORG DIL
3. TONE 7 20. X 37. LBL 01
4. PROMPT 21. STO 44 38. STO 00
5. XEQ 01 22. WATER= 39. 330.872
6. STO 48 23. ARCL44 40. +
7. 11.8 24. TONE 6 41. X"2
8. NEEDED BRIX? 25. TONE4 42. 170435
9. PROMPT 26. TONE4 43. /
10. XEQ 01 27. TONE 6 44. E"x
11. STO 43 28. PROMPT 45 .. 0437691
12. RCL48 29. RCL 47 46. X
13. - 30. RCL 44 47. RCLoo
14. CHS 31. + 48. X
15. RCL43 32. STO 45 49. END
16. / 33. TOT VOL=
17. VOL HI BRIX? 34. ARCL 45
442 APPENDIX C

GENERATION OF VOLUME TABLE FOR BULK TANKS

This program will generate data to construct a volume table for a particular bulk tank.
After entering the needed tank dimensions (see text for greater details), you enter the
distances from the hatch to the juice level, and the equivalent volume of the tank will
appear. The hatch depth is the distance from the lower lip of the hatch to the edge of
the tank.

1. LBLTANKS 39. RCL 46 77.


2. TANK SIZE 40. RCL 45 78. X*O?
3. AVIEW 41. + 79. X< >Y
4. PSE 42. X> Y? 80. RCL 44
5. DIAMETER-IN? 43. GTO 02 81. X'2
6. TONE 2 44. RCL 50 82. PI
7. PROMPT 45. RCL 46 83. X
8. 2 46. - 84. STO 00
9. / 47. RCL 45 85. RCL 46
10. STO 44 48. - 86. X
11. SLOPE HT -IN? 49. RCL 48 87. 231
12. PROMPT 50. X 88. /
13. STO 45 51. RCL 47 89. +
14. CYLINDER HT? 52. X*O? 90. RCL 00
15. PROMPT 53. / 91. RCL45
16. STO 46 54. X*O? 92. X
17. HATCH HT-IN? 55. X< >Y 93. 2
18. PROMPT 56. RCL 44 94. /
19. ST047 57. - 95. 231
20. HATCH DEPTH? 58. CHS 96. /
21. PROMPT 59. ENTER 97. +
22. STO 48 60. ENTER 98. STO 00
23. JUICE LEVEL? 61. X 99. GTO 05
24. PROMPT 62. X 100. LBL 01
25. LBL07 63. RCL 44 101. 2
26. ST049 64. X'2 102. /
27. RCL45 65. RCL 44 103. RCL 50
28. RCL46 66. X 104. X>Y?
29. + 67. - 105. GTO 03
30. RCL47 68. CHS 106. -1
31. + 69. RCL 47 107. STO 51
32. - 70. X 108. GTO 04
33. CHS 71. PI 109. LBL 03
34. STO 50 72. X 110. 1
35. RCL 45 73. 693 111. STO 51
36. X>Y? 74. / 112. LBL 04
37. GTO 01 75. RCL 48 113. RCL 50
38. X< >Y 76. X*O? 114. RCL 45
HP-41C PROGRAM 443

115. / 141. X 167. /


116. STO 43 142. 2 168. RCL 50
117. 2 143. X 169. RCL 45
118. X 144. + 170. -
119. 1 145. PI 171. RCL 00
120. - 146. 2 172. X
121. CHS 147. / 173. +
122. RCL 51 148. + 174. 231
123. X 149. RCL 44 175. /
124. RAD 150. X'2 176. STO 00
125. ASIN 151. X 177. LBL 05
126. DEG 152. RCL 50 178. RCL 00
127. RCL 51 153. X 179 . . 5
128. X 154. 462 180. X< =Y?
129. CHS 155. / 181. GTO 06
130. 1 156. STO 00 182. 0
131. RCL43 157. GTO 05 183. STO 00
132. - 158. LBL02 184. LBL 06
133. RCL43 159. RCL44 185. FIX 0
134. X 160. X'2 186. GALS =
135. SQRT 161. PI 187. ARCLOO
136. RCL 43 162. X 188. TONE 9
137. 2 163. STO 00 189. PROMPT
138. X 164. RCL 45 190. GTO 07
139. 165. X 191. END
140. - 166. 2
Appendix 0

Answers to Select Questions and Problems

Chapter 2

Questions

3. No.
5. Temperature, acid level, lab technician or techniques, refractometer calibration,
wavelength or color of light source, sample concentration.

Problems

3. 0.76% acid 3.83% acid 24.76% acid 37.86% acid


EQI-2 0.16 0.74 4.55 6.78
EQI-3 0.16 0.75 4.55 6.75
TBL-l 0.15 0.75 4.53 not on table

4. 1l.5°Brix, 10.6 B/A ratio.


7. 92 gallons of 64.5°Brix concentrate.
9.659 gallons of 11.9°Brix cutback juice.

Chapter 3

Questions

2. The mitochondria of the juice cell.


7. Yes.

Problems

4. 4.82% acid
7. 60.6°Brix
10. 245 gallons of the 398 GPL concentrate, 3146 total gallons.

444
ANSWERS TO SELECT QUESTIONS AND PROBLEMS 445

Chapter 4

Questions

3. Taste is caused by electrical disturbances on the tongue, usually by ionic or polar


compounds or compounds most associated with electrical charge.

Problems

2. 12.7 using Equation 3-1.


3. IS drums.

Chapter 5

Questions

4. Because the smaller and irregular size of the lemon fruit causes more fruit to be
lost during conveyance, and the nonspherical shape results in less efficient juice
extraction.

Problems

3. Yes. 104.8% efficiency is within 100-110% efficiency.


5. 53.6 sol/ton, 67.5 gal/ton, 1314.7Ib peel/ton.

Chapter 6

Questions

1. Citrus oils and aromas and their components.


8. Because the bromine reacts preferentially with the d-limonene.
10. No. A volatile condenser should be used as shown in Fig. 6-1. Straight tube
condensers may not be capable of condensing the highly volatile alco-
hol / d-limonene mixture.
17. None.

Problems

4. 20,000 ml oil flavor enhancer.


7. Yes. It gives the 0.010% oil needed.
446 APPENDIX D

Chapter 7

Questions

2. Increased.
3. The yield would be low, also.
9. Pulp wash may be used in drinks or beverages, or in other food products.

Problems

4. 4.7% pulp.
5. 1.8% pulp.

Chapter 8

Questions

3. The deesterification of pectin by pectinase enzymes that form carboxyl groups,


which, in tum, precipitate with divalent cations, such as calcium, removing juice
cloud from single-strength juices or forming gels in concentrates.

Problems

5. 5.48 X 10- 6 equivalents/gsolublesolids - sec, compared to the method in the text


which gives 4.12 x 10- 5 equivalents/ml-min., which would be stable cloud.

Chapter 9

Questions

2. California orange juice is usually deeper in color than Florida orange juice be-
cause of California's drier climate.

Chapter 10

Questions

4. USDA: no standards. Florida: Grade A, 600 ppm naringin and 5.0 ppm limonin;
Grade B, 750 ppm naringin and 7.0 ppm limonin.
7. Test the juice for limonin, heat, and retest until the heating no longer increases
the limonin level.
ANSWERS TO SELECT QUESTIONS AND PROBLEMS 447

Problems

2. 20.3 ppm limonin.


3. 7.2 ppm limonin.
6. 435 ppm naringin.

Chapter 11

Questions

4. Advantages: It emphasizes nutritional value and looks professional. Disadvan-


tages: Because only a few of the mandatory nutrients are declared, it may give
the impression of a lack of nutrition; it takes space on the label; it requires mon-
itoring for compliance with the law.
6. Actually it is water because the definition of a nutrient in the first paragraphs of
the chapter states that nutrients are those components that engender growth. Car-
bohydrates is the answer sought here, however.
10. 120% vitamin C and 8% thiamin.

Problems

4. • 1 g protein and less than 2 % USRDA.


• 20 g carbohydrates.
• 120% USRDA vitamin C, which includes a 20% increase. (Again remember
that naturally occurring nutrients can occur at 80% of the declared value.)
• 8% USRDA thiamin which includes a 20% increase (for the same reason as
for vitamin C).
• 6% USRDA calcium. (Because this is added, it must be declared at the actual
level.)
5. Ascorbic acid = 48.5 mg/IOO ml; dehydroascorbic acid = 6.3 mg/IOO ml.
Because both have vitamin C potency, the total vitamin C level is the combined
54.8 mg/IOO ml. To find what would be declared on the label, multiply 54.8 by
1.77 (177 ml/serving versus 54.8 mg per 100 ml) and divide by 60 mg (the
USRDA value) to get 162% USRDA, or 160% USRDA rounded off according
to the labeling rules.

Chapter 12

Questions and Problems

4. Extractors.
5. 58 sec-I.
448 APPENDIX D

Chapter 13

Questions

3. The delayed bitterness and lighter color of the navel varieties.


5. Blood oranges have the best flavor, and mandarins have the best color.
7. Seedy and dark pigmented.

Chapter 14

Questions

4. Chewing tobacco in processing areas is prohibited according to Title 21 Code of


Federal Regulations section 110.10 paragraph (b)(6).
9. No, but the FDA can be notified, which may result in a special inspection and
subsequent action.
12. Quality of the products.

Chapter 15

Questions

9. This minimum plate count is unknown, perhaps in the tens of thousands or higher.
12. By a pure random correlation; or, it does not correlate.
14. Several months.

Problems

1. Too many to count (TMTC) or too numerous to count (TNTC) , as over 300
colonies appeared on the plate.
4. 3.2 ppm.

Chapter 16

Questions

2. Food, water, light, sex odor, and temperature.


4. Because the peel oils and acidity of the juice are toxic or unpalatable to most
insects.
6. Keep the plant clean, seal openings in the plant, keep doors closed, use air screens,
and fog the plant with appropriate insecticides.
ANSWERS TO SELECT QUESTIONS AND PROBLEMS 449

Chapter 17

Questions

2. Quality control personnel.


3. None.

Chapter 18

Questions

4. No black flakes are generally pennitted.


8. During storage.
13. Acid hydrogens tie up the water molecules in concentrates, forcing the potassium
and citrate to crystallize.

Problems

1. 2.35 - 2.27 meq/IOO ml = 0.08, less than the 0.10 that produces off flavors.
Therefore, the shelf life has not expired, but it is about to do so shortly.
3. Ksp (O°C) = 0.014 M2

Chapter 19

Questions

4. Water addition (adding water to pasteurized orange juice), carbohydrate addition


(adding sugars to FCOl), cover-up (adding colors), and blending of unauthorized
juices or juice products (adding grapefruit juice to orange juice).
6. Oxygen isotope analysis. Other methods are used because the oxygen isotope
analysis is very costly and complex.
9. The detennination of the isocitric acid, which can detect any type of dilution. As
there is no commercial source of isocitric acid, it cannot be added to obscure the
results.
14. Members of the industry themselves.

Problems

2. ml Titrated % Reducing Sugars Action

5.21 4.59 none


6.03 3.97 diluted with sucrose
3.12 7.67 diluted with fructose

4. No. Early-season juice is authentic and may contain this much acid.
450 APPENDIX 0

Chapter 20

Questions

2. "Nature's glue" holds membranes and tissues together.


9. Polyvalent cations.
11. The drain weight.
15. Juice drinks are cheaper to make, with a lower price to the consumer, and they
provide a market for low-quality bitter juices, pulp washes, or other cheap juice-
like products.
17. 30% protein, 10-15% hemicellulose, 5% pectin.

Problems

3. 688 pounds of citric acid, 13,134 gallons of water, 13,838 pounds of sugar, and
5797 gallons of juice.
5. 0 pounds of citric acid, 5,645 gallons of water, and 5,492 pounds of sugar.

Chapter 21

Questions

1. Protein, fiber, fat, and nitrogen-free extract.


6. To remove the slimy texture of the peel and aid in the expression of moisture
from the peel.
8. Peel oil.

Problems

1. 25.0.
5. 6.3% alcohol; no.

Chapter 22

Questions

3. So they will not provide harborages for rodents and insects.


6. It produces no off odors.
9. 0.005% v Iv.

Problems

2. 7.5 using Equation 22-2 or 22-4.


4. 1121 ppm COD and 728 ppm BOD.
ANSWERS TO SELECT QUESTIONS AND PROBLEMS 451

Chapter 23

Questions

3. Significant figures determine the number of decimal places that legitimately can
be used but do not indicate the actual error range. Error analysis does not indicate
the precision of measurement, only the range of error.
4. By specification.
9. Least squares analysis is a form of regression analysis that uses calculus to math-
ematically determine the best fit of a particular curve to particular data.

Problems

2. 29.5, 711.5, 0.1552, 0.0000002.


3. VR = 15.25. No, there is a significant difference.

Chapter 24

Questions

2. Neither should be done. Production and quality control should be completely


separate.
5. No. When an employee's personal problems affect his or her performance on the
job, they become the business of the company, and the company has a right to
act accordingly, especially to protect its products and other employees.

Chapter 25

Questions

3. To check customcr complaints, to provide samples for potential customers, and


for research purposes.
5. To continue quality control operations in the event of refractometer breakdown.

Problems

1. 84 samples and 9 acceptable rejects. One every 6 minutes.


3. 55,692 gallons
Index

Acidless orange, 181, 188, 190 a-ketoglutaric, 35


Acids, 34-53 (see also Brix/acid Ratio) Maillard oxidation effects. 264
aconitic, 35 malic, 35
adaptation of aerobic microbes to, extremes, mitochondria source of, 34-36
365 oxalacetic, 35
adaptation of anaerobic microbes to, pH effect on potassium citrate crystalliza-
extremes, 366 tion.274
addition to drink bases, 333 pH effects on aerobic treatment of waste-
addition to juice drinks. 328-331 water. 358
barrier of. to insects in fruit. 246 production of, in molasses fermentation,
blending of. in lemon and lime juices. 47- 347
52 pyruvic, 34,35
carbonic. 44. 45 reduced, orange juices. 52, 53, 281
changes of. during maturation. 37. 38 removal during debittering. 157, 158
citric. 10. 17, 19.34.35,38-53.55. 165. soil effects from, during irrigation with
201,227.264,272-276.321,322, wastewater, 357
326-335.412-417 succinic. 35
citrus acid cycle, 34-38 USDA grade standards for, 47
computer applications, 49, 51 use of, in jelly or jam gelation, 315
correction of. in juice drinks. 331, 332 use of, in juice drinks, 322
correction of. to the Brix. 10. 17. 19.412- Adulteration, 279-298
417 (table) annatto, 288-290
drink base components. 326 ARTHUR FDA adulteration screening, 297
effect of, on microbes. 226 carbon isotope ratios in detection of, 287
effect on potassium citrate crystallization, coal tar dyes, 290, 291
272,275 color addition, 288
fumaric, 35 cover-up, 287
GPL (grams acid as citric acid per liter), Dutch standards, 292, 295
47-51 economic fraud, 283, 284
in juice drinks. 320 FD&C dyes. 290.291
in lemons, 47-51 food additives. 280
in limes, 47-51, 202 formol test, 288
in sample drink base formulation, 334 French AFNOR standards. 292, 294. 295
isocitric acid levels to detection adultera- German RSK standards. 292, 296, 297
tion, 291 grapefruit juice. in orange juice. 291

453
454 INDEX

Adulteration (Continued) Bacillus pumilus, 228


isocitric acid levels in detection of, 291 Bacillus subtilis, 228
matrix method, 293, 298 Bacteria (see Microbiology), 226-229
optical rotation to detect, in oils, 92 bacillus pumilus bacteria, 228
pattern recognition method, 295 bacillus subtilis bacteria, 228
reducing sugar test, 285-287 diacetyl determination, 232-234
refractive index to detect, in oils, 94 diacetyl production, 227
screening methods, 292-298 lactobacillus bacteria, 226, 227
sodium benzoate tracer used to detect, 291 leuconcostoc bacteria, 226-228
specific gravity to detect, in oils, 94, 95 d-limonene toxicity to aerobic, 360
standards of identity, 280 seed, in BOD determinations, 360
sugar addition, 285-287 Benzoates
tangerine juice in orange juices, 291 in citrus drinks, 326
turmeric, 288-290 use of, in molasses fermentation, 347
unauthorized juice addition, 291 use of, to detect pulpwash, 291
United States standards, 293 Berry juices, 2, 102, 292, 321, 323
water addition, 284, 285 Biological Oxygen Demand (BOD), 360-362
Air pollution, 354-355 maximum allowed, for irrigation use of
primary ambient air standards (table), 354 wastewater, 357
sulfur compounds, 354, 355 Birds, 244, 252, 253
volatile organic compounds (YOC), 354 detection of, 253
Alcohol (see also Fuel By-products) 344-347 Bitterness (see Limonin or naringin)
denaturing of, 349 Black flakes, 260
determination of, 348-351 effect on juice appearance, 127
distillation of, 347, 348 Blood oranges, 181, 187-190
in citrus oils, 74 juice color, 126
production from pressed liquor, 342 Brix, 7-31
specific gravity determination of, 349 acid correction to, 10, 17, 19,412-417
Aldehydes (table)
citral in lemon oil, 96 adjustment of, 21-28, 419, 420, 430,431
content in steam distilled oil, 87 analysis of variance, 379-383
dec anal in non-lemon oils, 96 blending of, 28-30, 420, 421, 423-427,
in citrus oils, 74, 95, 96 432-435
measurement of, in oils, 96, 97 computer applications, 24-27, 418-426,
Amino acids 430-435
detection of, using formol test, 265-267 determination of, 8-19
oxidation of, in citrus juices, 261-263 regression applications, 21-22, 383
Anaerobic treatment, 365, 366 significant figures of, 373
Analysis of variance, 378-383 soluble solids and, 2, 3
F-distribution, 380 temperature corrections to, 10, 11, 17, 18.
Annatto adulteration and detection, 288-290 31
Anthocyanins, 126, 188, 193, 194 USDA grades for, 20 (table)
Anticarcinogenic attributes of citrus juices, 2 Brix/acid ratio, 55-64
Antifeedant use of debittering wastes, 2 blending of, 55-59
Apple, 2, 102,261,291,292,321 changes of, during maturation, 59-61, 63
Aromas, 2, 73, 83,88 computer applications, 56-61, 423-425,
essence aromas, 88 431-435
flavor enhancer use, 73 flavor effects of, 55
wet dog aroma, 88 USDA grades for, 59, 62
Automatic identification methods, 401 Buret reading, 43
INDEX 455

Calcium, 166, 172,284 in nutritional labeling, 165


addition of, to juice drinks, 321, 322, 325 oxidation enhancement of, 264
adulteration detection using, levels, 284 potassium citrate crystallization enhance-
precipitation of, citrate in feedmill, 344 ment of, 272-276
use of, pectate to enhance fruit section production of, from lemons, 201
firmness, 318 removal of, during debittering, 53
Candy formation, 260 in reduced acid juices, 52
Carbonic acid, 44, 45 salts of, 19,34,35,38
Carotenoids, 126, 288 Citric acid cycle, 34-38, 171
in citrus oils, 74 Citron, 181
in juice drinks, 323 Citrus aurantifolia (Christm.) Swing. (Lime),
Iycopene, 193 181, 202, 203
Casein, use in juice drink cloud, 324 Citrus aurantium L. (Sour Orange), 181, 191
Centrifuge Citrus decumana L. (Pummelo), 181, 193
liquid wastes from, 355 Citrus deliciosa Tenore (Mediterranean
low pulp juice quality control, 107, 108 Tangerine), 181, 199
significant figures in, tube levels, 373 Citrus grandis (L.) Osbeck (Pummelo), 181,
use of, in clarification of juices, 2 193
in cold press oil production, 86, 87 Citrus latifolia Tan. (Large Fruited Lime),
in Davis test, 137-139 203,204
in depulping, 52, 107, 108 Citrus limetta Risso (Lemon-like), 201
in dewatering wastewater sludge, 365 Citrus limettoides Tan. (Sweet Lime), 203,
in molasses desludging, 344 204
in production of steam distilled oil, 87 Citrus limon (L.) Burm. f. (Lemon), 181, 20 I
in pulp level determinations, 102, 103 Citrus maxima (Burm.) (Pummelo), 181, 193
in pulp wash production, 115 Citrus nobilis Loureiro (King Tangerine), 181,
in oil production, 85 200
in reducing sugar determination, 286 Citrus paradisi Macfadyen (Grapefruit), 181,
in vitamin C determination, 170-171 192
viscosity effects from use of, 177 Citrus reticulafa Blanco (Common Tangerine),
Chemical Oxygen Demand (COD), 362-364 181, 195, 196
Chlorine Citrus sinensis (L.) Osbeck (Sweet Orange),
as a contaminant, 256, 335 181-185, 187, 189, 190
determination of, 239 Citrus sudachi Hort. Shirai (Tangerine
use of, as a sanitizer, 241 Hybrid), 20 I
to wash fruit, 238 Citrus unshiu Marc. (Satsuma Tangcrine), 181
in wastewater treatment, 366 Clevenger Method of Oil Analysis (see Oils).
Citral, 75, 96 74,75
determination of, (Scott Method), 96, 97 Cloud, 117-124
effect of, on juice flavor, 73 composition of, 117
on Scott oil determination, 75 deactivation of pectinase, 120
Citric acid, 17, 35 degree of gel, 123
Brix/acid ratio and, 55 gelation due to calcium pectates, 118, 119
correction of, to the Brix, 10, 17, 19,412- in juice drinks, 324, 326
417 (table) loss of, 118
determination of, 38-47 pectin in, 117
diacetyl from, 227 PEU measurement, 120-123
in drinks, 321, 322, 326-335 pulp levels and, 117
in lemons and limes, 47-51 Steven's cloud test, 120
in purees, 321 viscosity effects from, 123, 124
456 INDEX

Clouding agents, 324 for blending limonin levels, 156


casein used as, 324 for blending of oil levels and oil addition,
core wash used as, 115 84
pulp wash used as, 115 for Brix adjustments, 24
soy flour used as, 324 for Brix blending, 26, 27
Cockroaches, 245, 246 for cutback juice blending, 25
Color, 126-134 for fruit sample data calculation, 69
iJ-carotene use in juice drinks, 323 for GPL calculation, 51
annatto use to enhance, 288 for lemon/lime fruit sample calculations,
blood orange juice, 188 71
browning reactions, 271, 272 to adjust sugars and acids in juice drinks,
carotenoids, 126, 193,288 334
coal tar dyes used to enhance, 290 to calculate average pulp levels, III
color tube test, 127 to formulate a drink base, 333
colorimeters other than Hunter, 133 to measure tank volumes, 409
FD&C dyes used to enhance, 290, 291, GWBASIC programs, 419-429
323, 324 HP41-CV programs, 430-443
Hunter citrus colorimeter, 129 pulp level blending, 109, 110,428,429,
Hunter color scheme, 129 436,437
Hunter colorimeter procedure, 130, 132-134 RPG programs, 22, 408, 418
in juice drinks, 320, 321 standard deviation built-in function, 376
in sample drink base formulation, 334 use of, in ethanol determination, 349
Iycopene in grapefruit juices, 288 in HPLC analyses, 139
maillard oxidation effect on, 126 in quality control, 3
of dried juice sacs, 112 in regression analysis, 383, 386
off, due to slow thawing of juice sacs, 110 in tank measurements, 408
pink color of grapefruit, 193 Containers
tristimulus method, 128 fill weights of, 397, 399, 400
tristimulus X, Y, Z values versus pulp appearance in clear, 102
wavelength (table), 131 sampling of, 397-399
turmeric use to enhance, 288 Control charts, 376-378
USDA color grades (table), 130 applications, 377, 378
USDA color scores (table), 129 runs, 376, 377
USDA grade scoring, 127 Core wash, 115
use of, in adulteration, 284, 288 Cutback juice
in juice drinks, 322, 323, 326 blending of, 25, 28, 419, 420
vitamin C oxidation effects on, 168 replaced by essential oil addition, 73
Common mandarin, 195-197 Cyclotene, Maillard oxidation product, 262
Common orange, 181-186
Compensation point, 36, 37 D-limonene (see also Oils)
Computers, 3, 23, 70, 83, 109, 156, 329, by refractive index, 94
334,418-443 by specific gravity, 94
blending of limon in levels, 156, 429 content in citrus oils, 74
blending of oil levels, 83,427,428,436, effects of, on aerobic wastewater treatment,
437 360
CITQUIC software, 3 flavor of, 73
disregard for significant figures, 373 measurement of using Scott method, 76-79
flow chart explanation of symbols, 24, 25 measurement using Scott method, 75
flow charts optical rotation, 92
for acid blending (lemon and lime juices), taste threshold of, 79
49 toxicity of, to bacteria, 360
for B/A ratio blending, 59-61 Davis test for flavonoids, 137-139
INDEX 457

Deaeration of juice for Brix measurement, 9, concentrated juice addition to, 328
10, 12 core wash use in, 115
Debittering (see also Limonin) 2, 156-158, flavors in, 323, 324
280 flow chart to formulate a drink base,
adsorption resins use in, 157, 158 333
auxin sprays use in, 157 foaming agents in, 326
immobilized bacteria use in, 157 juices used in, 321, 322
insect antifeedant use of wastes from, 2 low pulp juices in, 107
neodiosmin use in, 157 nutrients in, 325
of core wash, 115 preservatives in, 325, 326
supercritical carbon dioxide use in, 157 sample base formulation, 334
Decolorization of grapefruit, 134 sugar addition to, 327-329, 333
Defoaming agents in juice drinks, 326 sugar correction in, 331, 332, 334
Density (see also Specific gravity), 21,94 sulfites in, 325
of juices, 7-9,13,14,31,40,47,48,50, sweeteners used in, 322
52, 68, 70, 148, 150, 154, 166, 324- texturizers in, 324
328,331,383,393,408 vitamin C addition to, 325
of pellets, 341 vitamin C as an antioxidant in, 326
of oils, 87, 94, 95 water addition to, 328-330
of water, 94, 95, 403 water quality used to make, 334, 335
optical, 94, 143 Drosophila fruit fly, 246, 247
radioactive, 178 light effects on, 248
tables of, 8 Dutch standards, 292, 295
temperature corrections to juice, 31
a-terpineol, 264
Deoiling of single strength juice, 83 Employee discipline, 392, 393
Diacetyl Employee evaluations, 391
determination of, 232-234 Employee training, 391
non-random effects of, levels, 377 Enzymes
statistical analysis of, 371 aconitase, in citrus acid cycle, 35
Dried juice sacs, 110-112 deactivation of pectinase, 83, 119, 120,
color of, 112 177,239,281
composition of, (table), 112 deactivation of pectinase in juice sac
Dried peel, 339-341 production, 110
dust from, 339 effect of. on pressed peel due to liming,
heat production from, 339, 340 342
moisture addition to, by oil recovery immobilized, used in debittering, 157
systems, 340 immunoassay limonin determination, 142-
moisture content of, 339, 340 144
moisture test, 340 lemon juice clarification using, 124
nutrients in, (table), 341 melanin formation via, 271
Drinks, 303, 320-335 oxidation via, 260
acid addition to, 327-331, 333 PEV measurement of, activity, 121-123
acid correction, 331, 332, 334 protein as, 164
acids used in, 322 Steven's cloud test, 120
anti foaming agents in, 326 thiamine as coenzyme, 171
base formulation, 320, 326-331, 333 use of, as drink preservative, 326
calcium addition to, 325 in first stage of pulp wash, 124
~-carotene, 323 in Florida not allowed, 124
clouding agents in, 324 in oil production, 85
colors in, 322, 323 in pectin extraction, 304, 305
computer applications, 333, 334 in production of cold pressed oil, 87
458 INDEX

Enzymes (Continued) of Florida citrus, I


use of, as drink preservative (Continued) of potassium citrate crystals, 272
in pulp wash production, 114, 115, 124 of pummelos, 194
in thiamin determinations, 172 off, due to slow thawing of juice sacs, 110
viscosity reduction applications of, 124, 177 oxygenated hydrocarbons contribution, 73
Equipment management, 393,408,410 quality control of, in citrus oils, 89
glassware calibration, 393 sanitation effects of, 213
insect and rodent damage to, 393 vitamin C oxidation effects on, 168
Error analysis, 374-376 Floating pulp, 110-113
actual range, 374 determination of, procedure, 112, 113
average deviation, 374 Florida Department of Citrus, 1
root mean square deviation, 374, 375 color determination approved by, 129- 134
standard deviation, 375 Foaming agents in juice drinks, 326
Essences, 73, 88, 89 Food and Drug Administration (FDA), 214-
allowed in standards of identity, 281, 282, 220
303 adulteration administration, 279-284, 293
flavor enhancer use, 73 adulteration detection, 297
juice drink component, 323 cleaners used in plant, 256
puree base component, 321 good manufacturing practice, 216, 255
imported product inspection form, 221
Fat, 163, 164, 166 inhouse inspections based on, 224
as part of TON, 338 insect contamination and, 244
as texturizer in drinks, 324 inspections, 214-220
in dried peel, 337,338,341 ion exchange resins approval by, 52
in pressed peel, 339 nutritional labeling, 162
in wet peel, 338 pattern recognition adulteration detection,
removal from wastewater using OAF, 356 295
solubility of {3-carotene, 323 sampling plan, 397, 398
FD&C dyes standards of identity, 280-283, 315
detection of, as adulterants, 290, 291 Food Chemicals Codex (FCC)
in sample drink base formulation, 334 oil specifications, 89
use of, in juice drinks, 323 oil specifications (table), 90, 91
Feeds (see Peel) pectin specifications, 305-311
Fill weights, 397, 399,400 Formol test
Flavor adu Iteration detection, 288
aldehyde contribution in oils, 95 for oxidation detection, 265, 266
bitterness (see Limonin and naringin) procedure, 266, 267
in pulp wash, 114 Freeze damaged fruit processed, 1
Brix/acid ratio effects on, 55 French AFNOR standards, 292, 294, 295
citrus oil contribution, 73 Fructose, 7, 8, 165, 285
d-limonene contribution, 73 adulteration detection of, 285-287
encapsulated flavors, 303 component of sucrose, 7, 8
extracts used in juice drinks, 326 nutritional labeling, 165
fold oils used to enhance, 88 oxidation of, 262
four-dimensional aspects of, 136 required, in Florida molasses, 344
furaneol pineapple-like, due to oxidation, slime molds metabolized from, 228
263 use of, in drinks, 322
furfural correlation with, 268 Fruit sample testing, 66-71, 389
in juice drinks, 320, 321, 323, 324 computer applications, 68, 69, 71,425-
in sample drink base formulation, 334 427, 435-438
Maillard oxidation in producing off, 261 for lemons and limes, 70,71
INDEX 459

safety during, 394 decolorization of, 134


statistical analysis of fruit quality, 377 FCC standards of, oils, 91
trouble shooting, 68-70 FD&C dyes used in, drinks, 323
Fruit sections, 303, 317-320 fill weights for, 400
analytical procedures, 318 Florida !imonin grade standards, 151
drain weight, 319 fruit section production, 317
filling, 318 furfural detection in, 268
fruit preparation, 317 HPLC determination of naringin in, 139,
peeling, 317 140
sectionizing, 317, 318 illegal use in orange juices, 291
standards of identity, 319 juice cocktail, 193
USDA grade standards, 319, 320 limonin in, juice, 140
Fuel byproducts (see also Molasses, Waste- moisture in, peel, 340
water) 337, 344-350 naringin bitterness, in, 137
alcohol dehydration, 348 oil characteristics, 86
alcohol determinations, 348-351 oil composition of, juice, 74
alcohol production, 349 oxidation of, juice, 263
as hazardous waste, 366 pulp in, juice, 104
distillation of alcohol, 347 USDA grade standards of pulp in, juice
methane gas from anaerobic treatment of (table), 105
wastewater, 365 USDA grade standards of, sections, 319,
reducing sugar test in fermentation of 320
molasses, 347 standards of identity of, juices, 282
sulfur content in, 355 USP standards of, oil, 91
Wick fermentor, 346 uv adsorption of, oils, 98
varieties of (see Varieties)
German RSK standards, 292, 296, 297 vitamin C in, juices, 168
Glassware calibration, 393 GWBASIC programs, 3
Glucose, 7, 8, 165,285 average Brix, 30,420,421
addit;on of, to pasteurized orange juice, 281 average Brix/acid ratio, 56, 423
adulteration detection of, 285-287 average Brix and Brix/acid ratio, 58, 425
component of sucrose, 7, 8 average limonin, 156, 429
fermentation of, 230 average oil, 83, 427, 428
nutritional labeling, 165 average pulp, 110, 428, 429
oxidation of, 262 Brix adjustment, 27, 419
required, in Florida molasses, 343 Brix and Brix/acid ratio from laboratory
use of, in drinks, 322 data, 58, 424, 425
Gluc()sides of limonin, 141, 143 Brix needed in concentrating lemon juice,
Good manufacturing practice (see Food and 49,421,422
Drug Administration), 214-216 cutback juice addition program, 25, 28,
GPL (grams acid as citric acid per liter), 47- 419,420
52 fruit samples (lemon), 70, 426, 427
computer applications, 49, 421-423, 438- fruit samples (non-lemon), 68, 425, 426
441 GPL calculation, 50, 422, 423
Grape, 2, 102,291,321,392 volume needed for I blend component for
Grapefruit (Citrus paradisi Macfadyen), 181, desired Brix, 31
191-195, 204-209, 263 volume needed for I blend component for
browning reactions in, 271 desired Brix/acid ratio, 31, 423, 424
color, 126
color scoring method, 134 Hazardous materials, 394-396
Davis test for naringin in, 137-139 Hazardous Wastes, 366, 367
460 INDEX

Hesperidin, 137, 258, 259 Jams, 303, 314-317


determination of, 137-140 acid effects on, 315
effect on juice appearance, 127 mineral effects on gelation of, 315
in juice cloud, 117, 324 orange marmalade formulation, 316
HP-4IC programs pectin effects on gelation of, 315
average Brix and Brix/acid ratio, 30, 58, Jellies, 303, 314, 316, 317
432-435 acid effects on, 315
average oil, 83, 436, 437 mineral effects on gelation of, 315
average pulp, 110, 436, 437 orange jelly formulation, 315
Brix adjustment, 27,430,431,441 pectin effects on gelation of, 315
Brix and Brix/acid ratio from laboratory USDA grades for, 316, 317
data, 58, 431, 432 Juice sacs (see also Pulp)
Brix needed in concentrating lemon juice, frozen 110
49,438-440 viscosity effects, 177
cutback juice addition program, 28 Juice yields, pulp level control and, 104
fruit samples (lemon), 70, 437, 438
Kumquats, 182
fruit samples (non-lemon), 68, 435
GPL calculation, 50,440,441 Labeling, 397, 398, 400-403
tank volumes, 442, 443 automatic identification methods, 401
Hunter citrus colorimeter, 128-130, 132-134 bar code samples, 402
Hydrometer nutritional, 160-172
acid corrections for, 10 sample manifest from bar code scanning,
Brix measurement using, 8-12 403
temperature corrections for, 9-11 universal product code (UPe), 401-403
Lactobacillus bacteria, 227
Imported product inspections, 220 colony recognition, 234
Insects, 244-251 in citric molasses, 344
air screens, 250, 251 Laying off employees, 392
antifeedant use of debittering wastes, 2 Least squares analysis (see Regression
cockroaches, 245, 246 analysis)
crickets, 245 Lemon (Citrus limon L. Bunn. f.), 19, 181,
Drosophila fruit fly, 246, 247 201-209,292
food and water, 245 acids in, juices, 40, 46, 47, 50, 165
in dried peel, 342 adulteration in, juices, 284
insecticides, 249, 250 aldehyde determination in, oils, 96, 97
light effects on, 248, 249 blending of, concentrates, 50, 51
Mediterranean fruit fly, 246 browning reactions in, juice processing,
Mexican fruit fly, 246 265, 271
Oriental fruit fly, 246 citral in, oils, 96
physical barriers, 250, 251 clouding agents used in, drinks, 324
solid wastes harborages for, 355 composition of, oils, 74, 75
temperature effects on, 247, 248 enzyme clarification in, juices, 124
Inspections, 213-224 enzyme deactivation in, juices, 120
FDA inspections, 214-220 gelation of, concentrates, 119, 120
imported product inspections, 220 GPL in, concentrates, 47,48, 50, 51, 421-
in-house inspections, 224 423, 438-441
USDA inspections, 220, 222-224 FCC specifications for, oils (table), 90
Inventory of lab equipment, 408, 410 fill weights for, 400
Isocitric acid use of, in adulteration detection, fruit sample testing of, 68, 70, 71
291 Mediterranean fruit fly repelled by, 247
INDEX 461

microbiological use of, serum agar in HPLC determination of, 144- I 50


plating, 236 in core wash, 115
oils of, 75, 87 hassaku juice, 194
optical rotation correction for, oils, 93 iyo tangor, 20 I
pectin from, peel, 304 pulp wash, 114
pectin jelly grade from, peel, 311 limonoate A-ring lactone precurser, 140
potassium citrate crystallization in, concen- methods of determination, 142-153
trates, 275 processing considerations, 153
processing, concentrates, 47-51 rate of, development, 141
refractive index correction for, oils, 94 removal of, using adsorption resins, 157
specific gravity correction for, oils, 95 solubility of, 141
standards of identity for, juices, 47, 282, structure of, 140
283 TLC determination of, 151-153
vitamin C in, juices, 168 Low pulp juices, 106-108
use of, juice in drink bases, 321-323 Lycopene, 126, 134, 193
USP specifications for, oils, 90
uv adsorption of in, oils, 98
Leuconostoc bacteria 227, 228 Magnesium
colony recognition, 234 as buffering agent in juice drinks, 322
in citric molasses, 344 in natural juices, 284
Lime (Citrus aurantifolia Swingle, Citrus Maillard oxidation, 261-271
latifola Tananka, and Citrus limettoides effect of, on juice color, 126
Tanaka), 19, 181,201-209 Malic acid
acids in, 40, 46J 47, 50, 165 effect of, on acid corrections to the Brix, 17
blending of, concentrates, 50, 5 I in citrus juice, 38, 40
clarification of, juices, 124 use of, in drinks, 322
composition of, oils, 74, 75 Management, 3, 388-396, 400
evaporative residue test for, oil, 97, 98 communication, 392
gelation of, concentrates, I 19, 120 employee discipline, 392, 393
in sample drink base formulation, 334 employee evaluations, 391
fruit sample testing, 68, 70, 71 equipment, 393, 408, 410
GPL in, concentrates, 47, 48,50,51,421- hazardous materials, 394, 395
423, 438-441 inventory, 397-410
vitamin C in, 167, 168 lay offs, 392
processing of, concentrates, 47 new employees, 390, 391
USP and FCC standards for, oil, 90 OSHA, 394, 395
uv adsorption of, oils, 98 personnel, 389-39 I
Lime (oxide of calcium) product samples, 389, 397
use of, in flocculation of wastewater, 356 relationship of quality control to other
in dried peel production, 87, 342 departments, 388-390
Limonin, 136, 140- 157 relationship of quality control to research
acids masking taste of, 142 and development, 389
bitter taste of, 136 safety, 394
blending of, levels, 154-156 sampling, 397
carbohydrate masking taste of, 142 specifications, 389
debittering, 156-158 Mandarin (see Tangerine)
E1A determination of, 142-144 Marmalade
Florida grade standards for, 150, 151 formulation, 316
glucosides of, 141, 143 from sour oranges, 190
heat required to develop, 141, 142 Material Data Safety Sheet (MSDS), 395, 396
462 INDEX

Matrix method of adulteration detection, 293, Moisture test


295, 298 dried juice sacs, 112
Mediterranean fruit fly, 246 of citrus peel, 339, 340
lemons are not a host for, 247 Molasses, 343, 344
Melanin, 271 alcohol production from, 344-350
Melanoidins,271 benzoate use in fermentation of, 347
Methane gas from anaerobic treatment of fermentation of, 345-347
wastewater, 337, 365 Florida requirements for, 343
Methyl orange indicator Scott method use of, foaming in, 344
76 from press liquor, 342
Mexican fruit fly, 246 nutrients in, (table), 343
Microbiology, 226-241 penicillin use in fermentation of, 347
acid effect on, 226 pH changes in, 344
aerobic treatment of wastewater, 358 reducing sugar test in fermentation of, 347
anaerobic effects in wastewater treatment, reverse osmosis wastewater concentrate
358 added to, 366
automated methods of determination, scale formation during evaporation of, 344
238 suspended matter in, 344, 345
Bacillus pumilus bacteria, 228 use in drying peel, 339
bacteria, 226-228 use in pellet production, 341
cleanup and water effects, 240, 241 viscosity changes in, 344
colony recognition, 234 viscosity reduction using pectinase, 347
cooling effects, 239, 240 waxes in, 344
d-limonene toxicity during aerobic waste- Mold, 222, 226, 229-232
water treatment, 360 colony recognition, 234
diacetyl determination, 232-234 fruit decay grade-out due to, 238
factors that affect, 226 growth in dried citrus peel, 341
fermentation, 229-231, 344-351 growth on jellies and jams, 314
fruit washing effects, 238, 239 plating for, 237
Lactobacillus bacteria, 226, 227 specifications for, 235
Leuconostoc bacteria, 226-228 Mouth-feel
microbes as a component of settleable solids pulp contributions to, 102, 110, 115
in wastewater, 365 texturizers to enhance, in drinks, 324
molds, 222, 226,229-232,234,235,237, viscosity and, 177
238,314,341
non-random effects of diacetyl determina-
tion,377 Naringin, 136-140
of citric molasses, 344 bitter taste of, 136
oil toxicity to, 345 Davis test for, 137-139
osmotic effects on, 229 Florida grades for, 140
pasteurization effects, 239 HPLC determination of, 139, 140
plating, 234-237 in juice cloud, 324
processing considerations, 238, 239 processing considerations, 153
relative sizes of yeasts and bacteria, 229 removal using adsorption resins, 157, 158
seed bacteria for BOD determination, 360 structure of, 137
yeasts, 226, 228-230, 232, 234-237, 240, use of, in adulteration detection, 291
326, 345-347 Navel orange (Citrus sinensis L. Osbeck),
Mineral levels in citrus juices (see individual 181,182,186,187
minerals) acid levels in, juice, 36, 37
in adulteration detection, 284 bitterness in, juice, 140-143, 153, 188
in nutritional labeling, 166, 167, 172 Brixl acid ratio versus heat during matura-
Mitochondria, 34-36, 117 tion of, 60
INDEX 463

potassium citrate in, juice, 273, 274 deoiling of single strength juice, 83, 88, 89
use of, juice in drinks, 321 effect on alcoholic fermentation of
Neodiosmin, 157 molasses, 345
Nomilin, precurser to limonin, 140 essence oils, 88
Nootkatone evaporative residue, 97, 98
from valencene in excessively heated FCC specifications for, 89-91
essence oils, 88 flavor enhancer use of, 73
unique component in grapefruit oil, 74 flavor source for juice drinks, 323
Nutrients, 162-172 folded oils, 88
calcium, 172,321,322,325 freshly extracted juice levels, 83
calories, 164 grapefruit oils, 86
carbohydrates, 165, 166 in citric molasses fermentation, 347
drink base components, 325, 326, 334 in sample drink base formulation, 334
fat, 166 insect barrier of, to fruit, 245
flavonoids, 172 juice oils, 88
labeling, 162-167 levels in press liquor, 342
labeling example, 163 moisture addition to peel from, recovery,
macronutrients, 164 340
micronutrients, 166, 167 non-food product use, 73
minerals, 166, 167, 172 optical rotation of, 89, 92, 93
pectin, 172 production of, 83-99
potassium, 166 refractive index of, 93, 94
protein, 164, 165 removal during debittering, 157
sample plan for determination of nutrional Scott method of determination of, 74-79
label compliance, 398 significant figures of, levels, 373
sodium, 166 specific gravity of, 94, 95
thiamine, 171, 172,334 standards of identity allowance, 281
vitamin C, I, 166-172, 188,202,325 steam distilled, 87
vitamins, 166, 167,334 storage of, 85
taste threshold of, 79
Occupational Safety and Health Administra- USDA grades of, in juices, 80, 83
tion (OSHA), 394, 395 USP specifications for, 89-91
Oils, 2, 73-99, 303 use of, in juice drink flavor emulsions, 326
a-pinene in, 74 in juice drinks, 323, 324
a-terpineol oxidative by-product, 264 uv absorption of, 98, 99
addition of, to juice products, 80-82 winterizing of, 85
air pollution from d-limonene burning in yield change of, with maturity of fruit, 86
feedmill, 354 Oriental fruit fly, 246
aldehyde determination in, 95-97 Oxidation, 97, 260-272
blending of, levels in juices, 79-83, 427, acid contributions to, 264
428, 436, 437 amino acid contribution to, 261
centrifuge use in production of, 86 cyclotene formation due to, 262
Clevenger method determination of, 74, 75 detection of, 265
cold pressed, production, 85-87 2,5-dimethyl-4-hydroxy-3(2H)-furanone
composition of, 74 formation due to, 264, 270
computer applications, 83, 84, 427, 428, N-ethylpyrrole-2-carboxaldehyde formation
436,437 due to, 264
d-limonene effects in aerobic wastewater l-ethyl-2-formylpyrrole formation due to,
treatment, 359, 365 261,270
d-limonene effects on aerobic wastewater formol test, 267
treatment, 360, 366 furaneol formation due to, 263
d-limonene in, 74 furfural, 267, 270
464 INDEX

Oxidation (Continued) Steven's cloud test, 120


furfural test, 267-269 structure of, 118
GLC procedure, 269, 270 Pectinase (see Pectin and Enzymes)
hydroxymethylcyclopentenone formation Peel, 337-342
due to, 264 air pollution from drying, 354
2-hydroxy-3-methyl-2-cyclo-pentene-l-one as solid waste, 355
formation due to, 270 dried, 339, 340
5-hydroxymethyl furfural formation due to, dust from drying, 339
270 extracts from, used in drinks, 303, 321
5-hydroxymethyl-2-furaldehyde formation fruit sample testing, 68-70, 425-427, 435-
due to, 264 437
in oils, 85, 97 fuels from, 2, 344-349
5-methyl-2-furaldehyde formation due to, 270 heat production from dried, 339, 340
5-methylfurfural formation due to, 262, 263 insects in dried, 342
oxygen effects, 264, 265 liming of, 342
prevention in juice drinks, 326 moisture content of dried, 339
temperature effects, 265 moisture test, 340
a-terpineol formation due to, 264, 270 molasses use in drying, 339
4-vinyl guaiacol formation due to, 263, nutrients in dried, (table), 341
264,270 pectin extraction from, 304
Oxygen (see Oxidation) pellets from, 341
biological, demand (BOD), 360-362 press liquor from, 342
chemical, demand (COD), 362-366 pressed, 338, 339
dissolved, 359-362 total digestible nutrients (TON) in, 338
isotope ratios of, in adulteration detection, unprocessed, 338
285 Pellets (see Peel), 341
PEV test (see Pectin and Enzymes) procedure,
Packaging, (see Labeling) 121-123
aseptic, 2, 239, 325 Phosphorus, 284
color and, 126 Photosynthesis, 35-37
pulp and, 102 Pinene
Pectin, 117-124,303-314 effect on Scott method, 75
arsenic in, 305 in lemon and lime oils, 74
ash, 305-307 Polarimeter, use of, in oil quality control, 89,
calcium pectate structure, 119 92,93
degree of esterification, 305, 307, 308 Potassium
esterification of, 118 buffering agents containing, in drinks,
FCC specifications for, 305 322
grade of, 118 crystallization of, citrate in concentrates,
heavy metals in, 305, 309, 310 106, 176,272-276
in jams and jellies, 314-316 natural levels of, in juices, 284
in juice cloud, 117-124, 324 nutritional labeling of, 166
jelly grade, 311-314 preservatives containing, in drinks, 326
nutrition of, 172 salts of, in juice, 38
pectinic acid, 304 Potassium citrate crystallization, 106, 176,
pectric acid, 304 272-276
peel liming effect on, 342 pH effects on, 275
PEV determination, 120-123 rate of, 275, 276
polymerization due to, 118 solubility of MPC crystals, 273, 274
production of, 303-305 Preservatives
protopectin, 304 use of, in fruit sections, 318
solvent content, 310, 311 in juice drinks, 292, 325, 326
INDEX 465

Preserves, 314, 315 quick fiber test, 104, 105


Press liquor, 342, 343 regression analysis of, 383-385
from pressed peel, 339 relationship of, to cloud, 117
nutrients of, (table), 343 removal of, during debittering, 153, 157
oil levels in, 342 removal of, prior to evaporation, 260
soluble solids in, 342 removal of, from wastewater using DAF,
steam distilled oils from, 87 356
use of, in alcohol production, 345-347 significant figures of, 373
wastes added to, 360, 366 sinking, or spindown, 102-110
waxes in, 344 standards of identity allowance, 281, 282,
Pressed peel, 338, 339 293
composition of, (table), 339 statistical non-random effect of, 377
used of, to make dried peel, 339 USDA grade standards for, (table), 105
Protein, 162, 164, 165 viscosity effects of, 123, 175, 177, 324
as natural emulsifiers in drinks, 324 Pulpwash, 2, 105, 110, 113-115
distillage from alcoholic fermentation used efficiency of, system, 113-115
as, supplement in feeds, 348 in dried sac production, 110
guarantee of, in citrus feeds, 337 in juice drinks, 292, 321
in citric molasses, 343 in sample drink base formulation, 334
juice cloud, 117, 324 juice yield relationship to, 113
nutritional labeling, 164-166 mineral levels in, 284
pressed peel, 339 quality control of, 114, 115
wet peel, 338 restriction of use of, in juice products, 114,
part of TDN, 338 115,291
Pulp, 102-124,303 (see also Peel) sodium benzoate tracer used in, 114, 115,
appearance of, 102 291,292
blending of, levels, 108-111,428,429, spindown pulp in, 115
436, 437 viscosity of, 177
Brix contribution of, 7 Pummelo (Citrus grandis (L) Osbeck, Citrus
computer applications, 109-111, 156, 428, maxima (Burm.) Merrill, Citrus
429, 436, 437 decumana L), 181, 191-195,200,
contribution of, to bitterness, 194 205-209
control chart application of, level Purees, 303, 320, 321
monitoring, 377 Pycnometer, in procedure to find specific
control of, levels, 104 gravity of oils, 95
core wash, 115
dried juice sac composition (table), 112
Quick fiber test, 104, 105
dried juice sacs, 110-112
effects of, in reduced acid juice production,
52 Reduced acid orange juices, 52,53,281
entrapment of, within monopotassium Reducing sugar test
citrate crystals, 273 in adulteration detection, 285-287
enzyme treatment of, 124 in alcoholic fermentations, 347
floating, 110-113 Refractometer, 13- I 9
frozen juice sacs, 110 acid corrections to, 17, 19,412-417
in drinks, 321, 324 Brix measurement using, 13-19
low, juices, 106-108 calibration of, 15-17
pectin in, 304 principles of, operation, 13-16
physical condition of fruit and, 105 refractive index using, IS, 16,90,91,93,
prediction of, levels, 106, 107 94
processing effects on, 105, 106 temperature corrections to, 17, 18
pulp wash, 113,284,288,291,292 used in oil quality control, 90, 91, 93, 94
466 INDEX

Regression analysis, 383-386 spoilage from entrapped pulp, 107


least squares analysis, 383-386 USDA inspection, 220, 224-224
of acid corrections to the Brix, 17 use of recycled water, 256
of juice density versus Brix, 21 Satsuma tangerine (Citrus unshui Marc.), 197,
of pulp levels before and after evaporation, 198
106, 107 Scott method of oil analysis, 74-79, 86, 87
of temperature corrections to the Brix, 17 Shaddocks (see also Pummelo), 191
Respiration, 34-38 Shear rate, 178
Reverse osmosis, 2 Sherbet, 321
in wastewater treatment, 366 Significant figures, 371-373, 375
Rheology of citrus juices, 175-178 in Brix levels, 14
Rodents, 244, 252, 253 in oil levels, 373
detection of, 253 in pulp levels, 373
solid wastes harborages for, 355 Sodium, 166, 284
RPG computer language benzoate salt as a adulteration tracer, 114,
subroutine to calculate SPG values from the 115, 291
Brix, 418 benzoate salt as a preservative, 318, 326
Taylor expansions of equations to facilitate, citric acid salts of, 38
22,408 in nutritional labeling, 163, 166
insects attracted less to, vapor lights, 248
polarimeter use of, vapor lamp, 92, 93
Safety, 394 refractometer use of, vapor lamp, 13
hazardous materials, 396 salts of, used as buffers for drinks, 322
Material Data Safety Sheet (MSDS), 395, sodium hydroxide solutions, 41-45
396 sodium methyl sulfate specifications for
OSHA, 394, 395 pectin, 305
Sampling, 397-399 soil effects of, when deposited on ground,
FDA, plan, 397,398 357
for nutritional label compliance, 398 Solid wastes (glass, metal, peel), 355
in-house, plan, 398 Soluble solids, 7-31, (see also Brix)
USDA, plan, 397,399 Sorbate, 326, 334
Sanitation, 3, 212-367 Sour orange (Citrus aurantium L.), 181, 190,
bird contamination, 252, 253 191
black flakes, 260 Specific gravity (see also Density)
caustics used in cleaning, 256 of alcohol, 349, 350
chemical contamination, 254-256 of oils, 94, 95
diacetyl determination, 115 of oxidation products, 262
FDA inspection, 215-220 scales or tables, 7, 8, 21
good manufacturing practice, 214, 215 Species of citrus, 181
hair protection, 254, 255 Citrus aurantifolia (Christm.) Swing.
hesperidin flakes, 258, 259 (Lime), 181,202,203
imported product inspection form, 221 Citrus aurantium L. (Sour Orange), 181,
insect contamination, 244 191
loose items near product containters, 254 Citrus decumana L. (Pummelo), 181,
oxidation, 260, 261 193
physical contamination, 254, 255 Citrus deliciosa Tenore (Mediterranean
processing contamination, 258 Tangerine), 181, 199
rodent contamination, 252 Citrus grandis (L.) Osbeck (Pummelo),
sanitizers, 256 181, 193
spoilage due to slow thawing of juice sacs, Citrus latifolia Tan. (Large Fruited Lime),
110 203, 204
INDEX 467

Citrus limetta Risso (Lemon-like), 201 tangerine juice addition and, 195, 281
Citrus limettoides Tan. (Sweet Lime), 203, varietal blending and, 291
204 vitamin C addition and, 188
Citrus limon (L.) Burm. f. (Lemon), 181, Statistics, 371-386
201 actual range, 374
Citrus maxima (Burm.) (Pummelo), 181, analysis of variance, 378-383
183 average deviation, 374
Citrus nobilis Loureiro (King Tangerine), control charts, 376, 377
181,200 error analysis, 374-376
Citrus paradisi Macfadyen (Grapefruit), F-distribution, 380
181, 192 least squares analysis, 383-386
Citrus reticulata Blanco (Common pulp level control applications, 104
Tangerine), 181, 195, 196 regression, 383-386
Citrus sinensis (L.) Osbeck (Sweet Orange), root mean square deviation. 374, 375
181-185, 187, 189, 190 runs, 376, 377
Citrus sudachi Hort. Shirai (Tangerine significant figures, 371-373
Hybrid), 201 standard deviation, 375
Citrus unshiu Marc. (Satsuma Tangerine), Steven's cloud test, 120
181 Sulfites
Specifications, 3, 234 as antioxidants, 272, 325, 326
black flake, 260 as preservative, 325, 326
Brix,28 in juice drinks. 325, 326
color, 130 Sucrose (see also Brix)
FCC, for oils, 89-91 adulteration detection of, 285
for pectin, 305 as Brix, 8
inbound and outbound, 389 as soluble solids. 7
microbial, 235 in nutritional labeling, 164-166
oil, 79 potassium citrate solubility in, solutions,
pulp, 107, 109 273
use of, to prevent adulteration, 297, 298 refractometer calibration using, solutions.
with control charts, 376 15
USP, for oils, 89-91 regression analysis of, tables, 21. 383
SPG (pounds soluble solids per gallon, see slime molds metabolized from. 228
Brix) structure of. 8
Standard deviation, 375, 376 viscosity contributions of, 177
Standards of identity, 280-284, 293. 389, 397 use of, density tables, 21. 47.154,383
antioxidants and. 272 in juice drinks. 322
calcium addition and, 172 solutions to increase limonin solubility,
cleaning agents and, 256 141
dried juice sacs and, 110 yeast fermentation of, 230, 231
food additives and, 256 Supercritical extraction, 2, 157
fruit sections, 319 Sweet orange (Citrus sinensis L. Osbeck).
grapefruit juices, 282 181, 182
imported juice, 220
jellies, 314, 315
labeling requirements, 400 Tangeretin, unique component in tangerine
lemon juices, 47, 282, 283, 400 oils, 74
oils and, 73, 281 Tangerines or mandarins, 181, 194-197
orange juices, 52, 53, 280-282 acid determination of, juice, 46
pulp and, 281 blending of, juice in orange juices, 126,
pulpwash and, 105, 114 281,291
468 INDEX

Tangerines or mandarins Continued) for jellies, 315-317


Brix USDA grades for, juice (table), 20 for oil, 79, 80, 83
carotenoids in, juice, 126 for pulp, 104, 105
color of, 126, 323 hesperidin flakes and, defects scoring, 259
common, 195-197 insect contamination and, defects scoring,
FCC standards for, oils, 91 244
fruit sample test, 68 labeling requirements, 400
fruit section production, 317 naringin standards, 140
hesperidin in, juice, 258 pH endpoint used by, in acid determina-
hybrids of, 194,200,201 tions,40
in sample drink base formulation, 334 sampling plan, 397, 399
King, 200 sanitation inspections, 220, 222-224
Mediterranean, 199 use of, grades in establishing specifications,
oil composition of, 74 389
potassium citrate crystallization in, 275 water addition to canned tangerine juice,
pulp USDA grades for, juice (table), 105 284
satsuma, 197, 198 United States Pharmacopeia (USP) standards
thiamine in, juice, 172 for oils, 89-91
use of, in drinks to enhance color, 323 Universal Product Code (UPC), 401-403
use of, in orange juices, 126, 291
USP standards for, oil, 91 Vacuoles of juice cell, 34-36, 117
uv absorption of oil, 98 Valencene in essence oils, 88
vitamin C in, 168 Valencia (Citrus sinensis L. Osbeck), 182
water addition to, juice, 284 acid changes in, juice during maturation,
Tank volume measurements, 397, 403-409 36,37
Tankers, 408 compensation point for, 36
Taxonomy of citrus (table), 181 hesperidin crystallization in, juice, 259
Thiamine, 171, 172 late season fruit, 186
in sample drink base formulation, 334 limonin levels in, 155
in nutritional labeling, 166, 167 Mediterranean tangerine in Spain, 199
in sample drink base formulation, 334 Pakistan, 186
Total Digestible Nutrients (TON), 338 potassium citrate crystallization in, concen-
Tristimulus color scheme, 128, 131 trate, 273, 274
Turmeric Varieties of citrus, 180-209
as colorant in drinks, 323 Agrio de Espana orange, 191
detection of, as adulterant, 288-290 Aoe tangerine, 198
Aoe wase tangerine, 198
Ultraviolet adsorption, in oil quality control, Apepu orange, 190, 191
90,91,98,99 Atwood navel orange, 187
United States Department of Agriculture Bahia navel orange, 187
(USDA) Bahianinha navel orange, 187
Atwater method for determining calories, Baia navel orange, 187
164 Baiana navel orange, 187
color grading, 126-134 Baianinha orange, 187
FDA inspections and, inspector, 216 Baianinha navel piracicaba orange, 187
flavor, 126 Bakrai tangerine, 196
fruit grading requirements, 238, 377 Balta orange, 183, 186
grades for acid, 47 Banpeiyu pummelo, 193, 194
for Brix, 19,20 Bearss lemon, 201, 202
for Brix/acid ratio, 59, 62 Bearss lime, 203, 204
for grapefruit sections, 319, 320 Bearss seedless lime, 203
INDEX 469

Beauty of Glen tangerine, 196 Dobashi Beni tangerine, 198


Beauty tangerine, 196, 197 Doblefina Amelioree orange, 188, 189
Bedmar orange, 185 Doblefina orange, 188, 189
Beledi orange, 183 Dolce orange, 190
Belladonna orange, 183, 185 Don Jao orange, 183
Belladonna Sanguigno orange, 189 Dorshapo lemon, 201
Bergamot hybrid orange, 190, 191 Dream navel orange, 186
Bema lemon, 201, 202 Duncan grapefruit, 192, 193
Bema orange, 185 Egami pummelo, 193
Bernia lemon, 202 Egyptian Shamouti orange, 185
Bernia orange, 185 Ellendale Beauty tangerine, 196
Biondo Commune orange, 183, 186 Ellendale tangerine, 196, 197
Biondo Riccio orange, 183 Emperor of Canton tangerine, 196
Bittersweet of Florida orange, 191 Emperor tangerine, 197
Bittersweet orange, 190, 191 Emperoro tangerine, 196
Blood Oval orange, 189 Entrefina orange, 188, 189
Blood Red Malta orange, 189 Eureka lemon, 201, 202
Blood Red orange, 189 Fallgo hybrid tangerine, 200, 201
Bombay-Decan orange, 184 Femminello Ovale lemon, 201, 202
Bonanza navel orange, 186, 187 Fewtrell tangerine, 196, 197
Bourouhaine navel orange, 187 Fewtrell's Early tangerine, 196
Cadena Fina orange, 183 Fino lemon, 202
Cadena sin Jueso orange, 183 Fisher navel orange, 187
Cadenera orange, 183 Flame grapefruit, 192
Calabrese orange, 183, 185, 186 Frost Owari tangerine, 198
Calabrese Ovale orange, 183 Frost Washington navel orange, 187
Calabrese Sanguigno orange, 189 Fukuhara orange, 183
Calderon orange, 185 Fukumoto navel orange, 187
California Mediterranean sweet orange, 184 Galgal hybrid lime, 203
Campeona tangerine, 196, 197 Garey's sweet orange, 184
Canamiel orange, 190 Gillette navel orange, 187
Canton lemon, 202 Glen navel orange, 186
Carvalhalorange, 183 Glen tangerine, 196
Castellana orange, 183 Grosse Sanguine, 189
Chamouti orange, 184 Gulgal hybrid lime, 203
Chini of South Indian orange, 184 Gunter hybrid orange, 190, 191
ChinoUo hybrid orange, 191 Hamlin orange, 183, 185, 186
Chironja orangelo, 194, 195 Hart Late orange, 185
Clan William orange, 183 Hart's Tardiff orange, 185
Clanor orange, 183 Hassaku Mikan tangelo, 195
Clementine tangerine, 196, 197, 199 Hassaku tangelo, 194, 195
Communa-Spain orange, 183 Hassaku Zubon tangelo, 195
Commune lemon, 202 Hayashi Unshiu tangerine, 198
Coorg orange (tangerine), 196 Henderson grapefruit, 192
Cravo tangerine, 196, 197 Hirado Buntan pummelo, 193
Dalmau navel orange, 187 Hirado pummelo, 193, 194
Damawi orange, 189 Hitmali orange, 183
Dancy tangerine, 196, 197 Homosasa orange, 183, 185
Darjeeling Orange (tangerine), 197 Imperial Grano de Oro orange, 190
Delta orange, 185 Imperial tangerine, 196, 197
Desi of Punjab tangerine, 196 in Algeria, 204
470 INDEX

Varieties of citrus (Continued) Jaffoui orange, 184


Imperial tangerine (Continued) Japanese Mikan tangerine, 198
in Argentina, 204 Joppa orange, 183
in Arizona, 205 Juuman tangerine, 198
in Australia, 205 K-early tangelo, 194, 195
in Brazil, 205 Kabusu orange, 191
in California, 205 Kabusudaidai orange, 191
in China, 205 Kao Pan pummel0, 193, 194
in Cuba, 205, 206 Kao Panne pummel0, 193
in Egypt, 206 Kao Phuang pummel0, 193, 194
in Florida, 206 Karystini lemon, 202
in Greece, 206 Kashi Orange of Assam (tangerine), 196
in India, 206 Katmali orange, 183
in Iran, 206 Key lime, 203
in Iraq, 206 Khalily White orange, 185
in Israel, 207 Khettmali orange, 183, 186
in Italy, 207 King tangerine, 197, 200
in Jamaica, 207 Kinnow tangerine, 196, 197
in Japan, 207 Kitchli hybrid orange, 191
in Java, 207 Koines-Greece orange, 183
in Lebanon, 207 Kumaon lemon (hybrid), 203
in Malaysia, 207 Kuno Unshiu tangerine, 198
in Mexico, 207 Lane's Late navel orange, 186, 187
in Morocco, 207, 208 Laranja Cravo tangerine, 196
in New Zealand, 208 Lee tangerine, 196, 197
in North Africa, 208 Leng navel orange, 186, 187
in Okinawa, 208 Lima orange, 190
in Philippines, 208 Lime lemon, 202
in Portugal, 208 Limetta lemon, 201
in Puerto Rico, 208 Limun Boussera hybrid lime, 203
in Reunion Island, 208 Lisbon lemon, 201, 202
in South Africa, 208 Liscio orange, 183
in Spain, 208 Lou Gim Gong, 185
in Sri Lanka, 208 Macetera orange, 183, 185, 186
in Syria, 208 Malta Blood orange, 189
in Taiwan, 208, 209 Maltaise blonde orange, 183, 185, 186
in Texas, 209 Maltaise orange, 183, 190
in Thailand, 209 Maltaise Oval orange, 184
in Tunisia, 209 Maltaise Ovale orange, 184, 186
in Turkey, 209 Maltaise Sanguine orange, 188, 189
Indian lime, 203,204 Malvaiso tangerine, 196, 197
Indian tangerine, 196 Mandalina tangerine, 196, 197
Ingles a orange, 189 Marrakech limonette, 203
Interdonato lemon, 201, 202 Marrs early orange, 184
Iseki Wase tangerine, 198 Marrs orange, 184, 186
Ishikawa tangerine, 198 Marsh grapefruit, 192, 193
Ishikawa Unshiu tangerine, 198 Marsh Seedless grapefruit, 192
Iyo Mikan tangor, 200 Mato Buntan pummelo, 193
Iyo tangor, 200 Mato pummelo, 193, 194
Jackson grapefruit, 192 Matsuyama Wase tangerine, 198
Jaffa orange, 184 Mawadri Beladi orange, 189
INDEX 471

Mawadri Beledi orange, 188 Okitsu Wase tangerine, 198


Mawadria Beledi orange, 189 Orlando tangelo, 197,200,201
Mediterranean limetta, 201 Orobanco tangelo, 195
Mediterranean Sweet lime, 203 Ortanique tangerine, 197
Mediterranean tangerine, 199 Osceola tangerine, 197
Melogold tangelo, 194, 195 Ova Ie orange, 183
Mesero lemon, 20 I, 202 Ovale Sangre orange, 189
Mexican lime, 203 Owari Satsuman tangerine, 198
Meyer lime, 203, 204 Owari tangerine, 198
Midknight orange, 185 Owari Unshiu tangerine, 198
Miho Wase tangerine, 198 Pai Yau pummelo, 193
Mikan tangerine, 198 Pai You pummelo, 193
Millsweet lemon, 201 Pakistan Valencia orange, 186
Minneola tangelo, 200, 201 Palestine Jaffa orange, 184
Miyagawa tangerine, 198 Palestine lime, 203, 204
Miyagawa Wase tangerine, 198 Pandan Bener pummelo, 193
Moanalua pummelo, 193 Pandan Wangi pummelo, 193
Monachello lemon, 201, 202 Paraguay orange, 190, 191
Morlotte orange, 189 Parson Brown orange, 184-186
Moro orange, 188, 189 Pedro Veyrat orange, 189
Moroccan limetta, 203 Pera Coroa orange, 184, 186
Mosambi orange, 184, 186 Pera Natal orange, 184, 186
Mosambique orange, 184 Pera orange, 184, 186
Moscatello lemon, 202 Pera Rio orange, 186
Murcott tangerine, 196, 197 Pero Rio orange, 184
Musami orange, 184 Persian lime, 203
Mutera orange, 188, 189 Petite Jaffa orange, 183
Myrtleleaf hybrid orange, 190, 191 Pineapple orange, 184, 186
Mytrleleaf orange, 191 Piracicaba orange, 186
Nagahashi tangerine, 198 Polyphoros lemon, 202
Nagpur tangerine, 197 Pond lime, 204
Nankan-4 tangerine, 198 Ponkan tangerine, 197
Natal of Brazil orange, 185 Poorman orange (tangelo), 195
Natsudaidai tangelo, 195 Poorman tangelo, 194, 195
Natsukan tangelo, 195 Pope orange, 185
Natsumikan tangelo, 195 Portugaise blonde orange, 183
Natusdaidai tangelo, 194 Portugaise orange, 189
Navel orange, 186 Precoce de Valence orange, 183
Navelate navel orange, 187 Precoce des Canaries orange, 183
Navelina navel orange, 187 Premier orange, 184, 186
Navelina orange, 186 Primitiori lemon, 202
Negra orange, 189 Queen orange, 184, 186
New Zealand grapefruit (tangelo), 195 Rangpur lemon, 202
Norris orange, 183 Rangur type tangerine, 196
Nostrale orange, 183 Ray Ruby grapefruit, 192
Nova tangerine, 196, 197 Real orange, 190, 191
Oberho1zer navel orange, 187 Red Blush grapefruit, 192, 194
Oberholzer orange, 186 Red Marsh grapefruit, 192
Oberholzer Palmer navel orange, 187 Red Seedless grapefruit, 192
Ogami pummelo, 193 Rio Grande navel orange, 187
Okitsu Unshiu tangerine, 198 Rio Grande orange, 186
472 INDEX

Varieties of citrus (Continued) Sue Linda tangor, 200


Rio Red grapefruit, 192, 194 Sugiyama Unshiu tangerine, 198
Riverside navel orange, 187 Suhoikan tangerine, 199
Robinson tangerine, 197 Sukkari orange, 190
Rojo Oval orange, 189 Summerfield navel orange, 186
Ruby blood orange, 189 Sunburst tangerine, 197
Ruby grapefruit, 192 Sweet orange, 184
Ruby orange, 188, 189 Tahiti lime, 203, 204
Ruby Red grapefruit, 192 Tahitian pummelo, 193, 194
Ruvittaru lemon, 202 Tajamur orange, 185
Sahesli lime, 204 Tankan tangerine, 197
Salus orange, 184 Tarocco dal Muso orange, 189
Salustiana orange, 184 Tarocco di Francofonte orange, 189
Sanbo hybrid orange, 190, 191 Tarocco orange, 188, 189
Sanguigno Semplice orange, 188, 189 Tarocco Ovale orange, 189
Sanguina Oval orange, 189 Temple tangor, 200
Sanguine Ovale orange, 189 Thompson grapefruit, 192, 194
Sanguinella Moscata orange, 188 Thomson Improved navel orange, 187
Sanguinella orange, 189 Thomson navel orange, 186, 187
Sanguinelli orange, 189 Thong Dee pummelo, 193, 194
Sanguinello Commune orange, 188, 189 Thorton, tangelo, 200, 201
Sanguinello Moscato orange, 188, 189 Tomango orange, 185, 188, 189
Sathgudi orange, 184-186 Triumph grapefruit, 192, 193
Satsuma tangerine, 198, 199 Tunisia lime, 204
Selecta orange, 184 Tunisian Sweet lime, 203
Seleta orange, 184, 186 Ugli tangelo, 200, 201
Seminole tangelo, 200, 201 Umatilla tangor, 200
Seto Unshiu tangerine, 198 Vadlapudi hybrid orange, 191
Sevillano orange, 190, 191 Vainiglia orange, 188, 190
Shamouti Maouardi orange, 189 Valence san Pepins orange, 183
Shamouti Masry orange, 185 Valencia Late orange, 185
Shamouti Mawadri orange, 188, 189 Valencia orange, 182, 185, 186
Shamouti orange, 184-186 Valencia temprana orange, 182
Siam pummelo, 193 Vaniglia orange, 190
Siamese Pink pummelo, 193 Vema lemon, 202
Siamese pummelo, 193 Vema orange, 185
Sicilian lemon, 202 Vernia lemon, 202
Sicily lemon, 202 Vernia orange, 185
Sikkim tangerine, 197 Vicieda orange, 185, 186
Siletta orange, 184 Viciedo orange, 185
Silverhill tangerine, 198 Vilafranca lemon, 202
Smooth Flat Seville tangelo, 195 Warrnurco tangerine, 197
Smoothe Seville tangelo, 195 Washington navel orange, 186, 187
Sour Seville orange, 191 Washington Sangre, 189
Spanish Sanguinelli orange, 188, 189 Washington Sanguine orange, 189
Speciale lemon, 202 West Indian lime, 202-204
Star Ruby grapefruit, 192, 194 Westin orange, 185, 186
Succari orange, 190 Wheeny grapefruit (tangelo), 195
Sucrena orange, 190 Wheeny tangelo, 194, 195
Sudachi hybrid tangor, 200, 201 White Marsh grapefruit, 192
INDEX 473

Wilking tangerine, 197 municipal disposal, 357, 358


Willow leaf, 197 reuse water, 356
Willow leaf tangerines, 199 reverse osmosis treatment of, 366
Yonezawa tangerine, 198 settleable solids in liquid, 365
Viscosity (see also Rheology) 175-178 solid, 353, 355
consumer considerations of, 177 volatile organic compounds (VOC), 354
determination of, 178 Wastewater, 355-366
equipment sizing applications of, 176 aerobic treatment of, 358, 359
in low pulp juices, 107 anaerobic treatment of, 365, 366
in pulp wash, 114, 115 biological oxygen demand (BOD), 360-362
low pulp juices, 108 chemical oxygen demand (COD), 362-364
processing considerations, 177 clarifiers, 365
shear rate, 178 dissolved air flotation (DAF), 356
texturizers in juice drinks, 324 dissolved oxygen determination, 359
use of enzymes to reduce, 124 filtration of, 355
Vitamin C, 1, 166-172, 167, 168, 188,202, flocculation of, 356
261, 283, 325, 326 irrigation use of, 357
addition to juice drinks, 325 methane gas production, 337, 365
as an antioxidant in juice drinks, 326 municipal disposal of, 357, 358
browning contributions of, 271 reuse water, 356
determination of, 169-171 reverse osmosis, 366
in limes, 202 settleable solids in, 365
in sample drink base formulation, 334 Waxes
oxidation of, 168 in citric molasses, 344, 345
oxidative off flavor development, 261 in oils, 74, 85-87
removal of, in debittering blood orange in wastewater, 355, 356
juice, 188 on fruit, 238, 344
use of, in adulteration, 283 Wet dog aroma, from excessively heated
essence aroma, 88
Wastes, 337, 353-367 Wet peel, 338 (see also Pressed peel)
aerobic treatment, 358, 359 Wick fermentor, 346
anaerobic treatment, 365, 366 Winterizing of oils, 85
biological oxygen demand (BOD), 306-326
chemical oxygen demand (COD), 362-364 Yeasts, 226, 228-230
dissovled air flotation (DAF), 356 colony recognition, 234
dissolved oxygen determination, 359 fermentation, 229-231, 344-350
flocculation, 356 growth in product lines, 240
gaseous, 353-355 in alcoholic fermentation of citric molasses,
hazardous, 353, 366, 367 344-350
irrigation use of, 357 osmotic effects on, 229
liquid, 353, 355 (see also Wastewater) species found in citrus juices (table), 231

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