Oil of Lemongrass - Specification: Indian Standard

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IS 327 : 1991

(Reaffirmed
( Reaffirmed 1996)
2002 )
Edition 3.1
(1998-12)

Indian Standard
OIL OF LEMONGRASS — SPECIFICATION
( Second Revision )
(Incorporating Amendment No. 1)

UDC 665.524.26

© BIS 2002

BUREAU OF INDIAN STANDARDS


MANAK BHAVAN , 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

Price Group 2
Natural and Synthetic Perfumery Materials Sectional Committee, PCD 18

FOREWORD
This Indian Standard (Second Revision) was adopted by the Bureau of Indian Standards, after the
draft finalized by the Natural and Synthetic Perfumery Materials Sectional Committee had been
approved by the Petroleum, Coal and Related Products Division Council.
This standard was originally published in 1952 and first revised in 1961. The Sectional Committee
responsible for its preparation felt that the standard should be revised with a view to bring it in line
with trade practices prevalent in perfumery industry and also to align the quality level of material
currently being manufactured and sold in the country.
In the earlier revision, determination of citral content using freshly prepared 30 percent m/v solution
of sodium bisulphite was prescribed. In this revision hydroxylamine method is being included as an
alternative method for determination of citral content. Gas Layer Chromatographic method for
determination of neral and geranial content is being included for guidance only under Annex B.
In India, oil of lemongrass is produced in the South-Western State of Kerala by the distillation of
lemongrass ( Cymbopogon flexuosus Stapf fam. Gramineae ). This essential oil produced largely in
India since ages has come to be known as the East Indian Oil of Lemongrass and has found favour in
the world market particularly because of its uniformly high citral content and the solubility
in 70 percent alcohol of most of the oil produced in the country. This solubility in alcohol is regarded
as synonymous with freshness and freedom from adulterants; though investigations have disclosed
that some specimens of freshly distilled oil are also found to be insoluble in alcohol, if there is
adventitious mixture, even in small proportions, with a similar but botanically different
white-stemmed grass, locally known as ‘wella poolu’ found in the fields. The white-stemmed grass
now identified as Cymbopogon flexuosus Stapf Var. albescens has, however, been almost rooted out of
the lemongrass fields by intensive efforts of the State Departments of Agriculture and Forests. The
solubility of all specimens of the oil is known to be reduced on storage.
The oil produced in other countries, most notably West Indies, is insoluble in 70 percent alcohol. The
lower solubility of the ‘West Indian’ oil, particularly noticeable after storage of the freshly distilled oil,
is due to the presence, in the foreruns, of myrcene, an olefinic terpene, which on exposure to air and
light readily polymerizes. This difference in the quality of the oil is attributed to the different plant
species, Cymbopogon citratus Stapf. (fam. Gramineae) from which the ‘West Indian’ oil is derived.
This edition 3.1 incorporates Amendment No. 1 (December 1998). Side bar indicates modification of
the text as the result of incorporation of the amendment.
For the purpose of deciding whether a particular requirement of this standard is complied with, the
final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in
accordance with IS 2 : 1960 ‘Rules for rounding off numerical values ( revised )’. The number of
significant places retained in the rounded off value should be the same as that of the specified values
in this standard.
IS 327 : 1991

Indian Standard
OIL OF LEMONGRASS — SPECIFICATION
( Second Revision )
1 SCOPE 4 SAMPLING
This standard prescribes the requirements and Representative samples of the material, shall be
the methods of test for the material commercially drawn as prescribed in IS 326 (Part 1) : 1984.
known as the oil of lemongrass or the East
Indian Oil of lemongrass. The material is largely 5 REQUIREMENTS
used in the extraction of citral, the chief 5.1 Description
constituent of the oil and the starting material
Oil of lemongrass shall be obtained by water or
for the manufacture of important ionones. It is
steam distillation of the freshly cut and partially
also employed in the preparation of lemon-like
dried grass botanically known as Cymbopogon
perfumes, germicides, etc.
flexuosus, Stapf fam. Gramineae.
2 REFERENCES 5.1.1 Oil of lemongrass shall be a clear liquid,
The following Indian Standards are necessary free from sediment, suspended matter, separated
adjuncts to this standard: water and added adulterants.
IS No. Title 5.1.2 The oil shall be examined for its colour,
326 Methods of sampling and test clarity, separated water, by notes and sediment,
for natural and synthetic as prescribed under IS 326 (Part 2) : 1980.
perfumery materials: 5.2 Solubility
(Part 1) : 1984 Sampling ( second revision ) Oil of lemongrass shall be soluble in 3 volumes of
(Part 2) : 1980 Preliminary examination of ethyl alcohol (70 percent by volume), occasionally
perfumery materials and with slight turbidity, when tested as prescribed
samples ( second revision ) in IS 326 (Part 6) : 1986.
(Part 3) : 1980 Relative density ( second 5.3 Oil of lemongrass shall also comply with the
revision ) requirements given in Table 1.
(Part 4) : 1980 Determination of optical
Table 1 Requirement for Oil of Lemongrass
rotation ( second revision )
(Part 5) : 1986 Determination of refractive Sl Characteristic Requirement Method of Test,
index ( second revision ) No. Ref to IS No.
(Part 6) : 1986 Determination of solubility in (1) (2) (3) (4)
ethanol ( second revision ) i) Colour and Dark yellow to IS 326
(Part 11) : 1986 Determination of carbonyl appearance light (Part 2) : 1980
brown-red
value and content of carbonyl mobile liquid
compounds ( second revision )
ii) Odour Lemon-like IS 2284 : 1988
1070 : 1977 Water for general laboratory
use ( second revision ) iii) Relative density*, 0.886 to 0.896 IS 326
27º/27ºC (Part 3) : 1980
2284 : 1988 Method for olfactory
iv) Optical rotation – 3º to + 1º IS 326
assessment of natural and (Part 4) : 1980
synthetic perfumery materials
v) Refractive index†, 1.479 9 to IS 326
( first revision ) 27ºC 1.485 9 (Part 5) : 1986
6597 : 1988 Glossary of terms relating to vi) Citral content, 75 Annex A
natural and synthetic percent by
perfumery materials ( first volume, Min
revision )
*The correction factor for relative density for each degree
3 TERMINOLOGY Celsius change in temperature is 0.000 62.
†The correction factor for refractive index for each degree
For the purpose of this standard, the definitions Celsius change in temperature is 0.000 44.
of terms given in IS 6597 : 1988 shall apply.

1
IS 327 : 1991

6 PACKING AND MARKING d) Batch number.


6.1 Packing 6.2.1 The containers may also be marked with
The material shall be supplied in air-tight the Standard Mark.
containers preferably glass, tin lined or 7 SAMPLING
aluminium; or as agreed to between the Representative samples of the material, shall be
purchaser and the supplier. drawn as prescribed in IS 326 (Part 1) : 1984.
6.1.1 The material shall be protected from light
8 TESTS
and stored in cool and dry place.
8.1 Tests shall be carried out as prescribed under
6.2 Marking 5.1, 5.2 and the appropriate references specified
The material shall be marked with the following in col 4 of Table 1.
information: 8.2 Quality of Reagents
a) Name of the material,
Unless specified otherwise, pure chemicals and
b) Indication of the source of manufacture, distilled water ( see IS 1070 : 1977 ) shall be
c) Net mass of the material and percentage of employed in tests.
total citral content, and NOTE — ‘Pure chemicals’ shall mean chemicals that do
not contain impurities which affect the results of analysis.

ANNEX A
[ Table 1, Sl No. (vi) ]
DETERMINATION OF CITRAL CONTENT
A-0 GENERAL complete reaction of the carbonyl compound with
A-0.1 Two methods, namely, hydroxylamine the bisulphite solution. After allowing the cassia
method and sodium bisulphite methods are being flask to stand undisturbed in boiling water for
prescribed for determining citral content of oil of 10 minutes to permit the unreacted material to
lemongrass. Any one of these may be adopted for rise to the surface, add sufficient volume of
determining citral content or as may be agreed to sodium bisulphite solution to raise the residual
between the purchaser and the supplier. The material into the neck of the flask. Gently tap
procedure for hydroxylamine method as given the flask and rotate it rapidly between the plams
under IS 326 (Part 11) : 1986 may be followed. of the hands to raise droplets of materials
Sodium bisulphite method has been prescribed adhering to the sides of the flask into the neck.
under this Annex. After cooling the flask to room temperature,
NOTE — It is of utmost importance always to record the
measure the volume of the residual material.
method used when reporting an analytical result.
A-1 REAGENTS
A small amount of the bisulphite addition
A-1.1 Sodium Bisulphite Solution compound often precipitates out of solution,
Freshly prepared, 35 percent ( m/v ). sometimes at the surface when the material and
aqueous layers meet, thus rendering exact
A-2 PROCEDURE
reading difficult. If so, add a few drops of water
A-2.1 Introduce 75 ml of the sodium bisulphite in such a way that the water runs down along
solution measured from a graduated cylinder, the inside of the neck of the flask so that it may
into a cassia flask (Fig. 1) Pipette exactly 10 ml remain temporarily on top of the bisulphite
of the material into the flask and shake solution and give a sharp separation of the
thoroughly. Immerse the flask in a boiling material and aqueous layers.
water-bath and shake repeatedly, until the solid
addition compound goes completely into solution. NOTE — If the material contains heavy metals, these
Make a further addition of 25 ml of the should be removed before the determination by shaking
bisulphite solution and again shake the flask the material thoroughly with a small amount (about 1
percent) of powdered tartaric acid and filtering, a sharper
repeatedly for one-half to one hour to ensure separation of the residual material will then result.

2
IS 327 : 1991

A-2.2 Calculation where


Calculate the citral content by the following v = volume in ml of residual material.
formula: NOTE — Citral content may be expressed as percent by
mass ( M ) if the relative density of the original material
Citral content, and of the carbonyl compound is known at the same
percent by volume = 10 (10 — v) temperature, using the formula:
Relative density of carbonyl compound
M = v × -----------------------------------------------------------------------------------------------------------
Relative density of material

FIG. 1 CASSIA FLASK

ANNEX B
( Clause 0.2 )
GAS CHROMATOGRAPHIC ANALYSIS FOR OIL OF LEMONGRASS
B-0 GENERAL B-0.2 Outline of the Method
B-0.1 The chromatographic conditions given here A sample of the material is dissolved in a
are for guidance only. suitable solvent (for example, cyclohexane and

3
IS 327 : 1991

petroleum ether) and is injected into the gas B-2 CALCULATION


chromatograph where it is carried by the carrier B-2.1 Area Measurements ( see Note 1 )
gas from one end of the column to the other.
During its movement the constituents of the Since normal peaks approximates a triangle, the
sample undergo distribution at different rates area is measured by multiplying the peak height
and ultimately get separated from one another. times the width of the half height. The normal
The separated constituents emerge from the end peak base is not taken since large deviations may
of the column one after another and are detected be observed due to tailing or adsorption. This
by suitable means whose response is related to technique is rapid, simple and fairly accurate
the amount of a specific component leaving the when peaks are symmetrical and of reasonable
column. width.
B-1 APPARATUS
B-1.1 Any gas chromatograph capable of being
operated under conditions suitable for resolving
the individual constituents into distinct peaks
may be used. The typical chromatogram for oil of
lemongrass using a chromatograph with the
following chromatographic conditions is shown in
Fig. 2.
Sample Oil of Lemongrass
Column AT — 1 000
Material Stainless steel
Length 5m
Orifice 0.32 cm
Stationary phase 10 percent by mass on FIG. 2 OIL OF LEMONGRASS
and solid support* chromosorb B-2.2 Area Normalization ( see Note 2 )
WHP 100-120 mesh By normalizing, it is meant calculating the
Carrier Gas Nitrogen percentage composition by measuring the area of
each and dividing the individual areas by total
Conditions area, for example:
Column temperature 190ºC Area of A
Percentage of A = ---------------------------- × 100
Injection port temperature 250ºC Total area
Detector NOTES
Type F.I.D 1 Other methods of area measurements, namely
triangulation, disc integrator and electronic digital
Temperature 250ºC integrator if fixed with GLC machine would be of great
advantage.
*The analysis may also be accomplished with columns 2 Internal standardization may be used if pure
containing : DEGS (Diethylene glycol succinate) and appropriate internal standard is available. This method is
FFAP (Free Fatty Acid Phase) in carbowax 20 M treated known as relative or indirect calibration.
with nitrophthalic acid.

4
Standard Mark
The use of the Standard Mark is governed by the provisions of the Bureau of Indian
Standards Act, 1986 and the Rules and Regulations made thereunder. The Standard Mark on
products covered by an Indian Standard conveys the assurance that they have been produced
to comply with the requirements of that standard under a well defined system of inspection,
testing and quality control which is devised and supervised by BIS and operated by the
producer. Standard marked products are also continuously checked by BIS for conformity to
that standard as a further safeguard. Details of conditions under which a licence for the use of
the Standard Mark may be granted to manufacturers or producers may be obtained from the
Bureau of Indian Standards.
Bureau of Indian Standards
BIS is a statutory institution established under the Bureau of Indian Standards Act, 1986 to promote
harmonious development of the activities of standardization, marking and quality certification of goods and
attending to connected matters in the country.

Copyright
BIS has the copyright of all its publications. No part of these publications may be reproduced in any form
without the prior permission in writing of BIS. This does not preclude the free use, in the course of
implementing the standard, of necessary details, such as symbols and sizes, type or grade designations.
Enquiries relating to copyright be addressed to the Director (Publications), BIS.

Review of Indian Standards


Amendments are issued to standards as the need arises on the basis of comments. Standards are also
reviewed periodically; a standard along with amendments is reaffirmed when such review indicates that no
changes are needed; if the review indicates that changes are needed, it is taken up for revision. Users of
Indian Standards should ascertain that they are in possession of the latest amendments or edition by
referring to the latest issue of ‘BIS Catalogue’ and ‘Standards : Monthly Additions’.
This Indian Standard has been developed from Doc : No. PCD 18 (953)

Amendments Issued Since Publication


Amend No. Date of Issue
Amd. No. 1 December 1998

BUREAU OF INDIAN STANDARDS


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