IS : 323-1959

Indian Standard

( Reaffirmed 2005 )

SPECIFICATION FOR RECTIFIED SPIRIT

(

Revised)

Ninth Reprint DECEMBER 1989

( Incorporating

Amendments

No. 1 and 2 )

UDC 621722

0 Copyright 1978
BUREAU
MANAK

Gr 8

OF
BHAVAN,

INDIAN

STANDARDS

9 BAHADUR
SHAH
NEW DELHI 110002

ZAFAR

MARG

May 1960

Is:323-I959

Indian Standard
SPECIFICATION

FOR RECTIFIED
(

SPIRIT . ,

Revised )

Alcohol and Allied Products

Sectional

Committee,

CDC 2

Chairman
All India Distillers Association, New Delhi

Saar G. GUNDUBA~
Members

N&ion81 Carbon Company ( India ) Ltd. Celcutt8

Da H. C. BIJAWAT
DB C. J. DADACHANJI ( Alter~te )
Directonrte General of Supplies & Dispourlr
SHIU K. K. C~ATTEWEIE
( Ministry of Works, Housing & Supply )
SHBI K. L. BANXBJEE ( Alternate )
Governmentof Utter Predeah
Sanr W. R. DAMLE
Snsr R. K. GUPT~ ( AIternate )
Directorate of Medical & Health Services, GovernDn N. GHATAK
ment of Uttar lmdesll
All India Distillers Associntion, New Delhi
SARI G. S. GUPTA
The Mysore Sugar Co Ltd. Bangalore
SHRI 0. NARASIMHA IYEN~AR
SHRI K. LAKPAPPA ( Alternate)
12/X3,Gweltoli. Kanpul
DR B. K. JHA
Diiectorate General, Ordnance Factories (llinistry
Dn G. S. KASBEKAR
of Dsfence ), Calcutta
SHRI GAJENDRA SINC+H( Alternate )
Council of Scientific & Industrial Research
DE M. L. KHANNA
Central Revenues Control Laborrvtory ( Ministry
SH~I P. S. KRISHNAN
of Finance j
SHRI R. PICHAI ( Alternate )
Indian
Chemical >lanufactureFs
Assochation.
SHRI MANM~~AN
ce1outts
SHRI DEVRAJKAPUB ( Afternate )
The Alkali & Chemical Corporation ( India ) Ltd
SBR~ J. ~IATRUR
The Hindustan Sugar Mills- Ltd, Golagoksr8nnst.h
Saar M. A. RAN~ASAXI
Indian Chemical Manufacturers
Associstion,
D8 K. A. N. RAO
Cnlcutt8
DR S. ROHATOI ( Alteruate )

( Continued pn page 2

BUREAU
MANAK

OF
BHAVAN,

INDIAN

STANDARDS

9 BAHADUR
SHAH
NEW DELHI 110002

ZAFAR

MARa

IS:323-1959
( coarifudfiml

poll? 1)

Membere
DB R. 8. J. RAW
SEEI G. D. SAmrNA
SHBI rd. L. scE&orr
SHBI L. R. STJD
SHlrl S. L. VBNIKIT~WA~AN

Government Central Distillery, N&k Road

Sanya Diitillery, Sardunagsr
The Similk Limited, Sirpur-Ktsgh8znsgcrr
Directorate of Technical Development (Minirtry
of Defencu )
Development Wing, Ministry of Commerce k

&XIX R. A. WILLIAMS

C8mW & Co Ltd. Assnsol

hlaustry

SHB;:~ K. E$Y ( AIternate )

VEBIKAN Director, ISI
DB
.
( Ex-oficio 1
DP SAD~OFAT.( Alternate )
Deputy Dire&or ( Chem ). BIS
Secretaries
Assistant Director ( Chem ). BlS
Extra Assistant Director ( Ohem ), BIS

Snrr D. Du 0-1
DB G. M. 8~x1~1

Panel for Alcohol,

CDC 2 : PI

Convener
SEBI M. A. RANQASAMI

The Hindu&m

Sugar Mille Ltd, Golagokarnnath

Members
Sanr W. R. DAMLE
Da B. K. JHA

Government of Uttar Prade&

12/53,Gaaltoli, Kanpur

IS:323-1999

Indian Standard
SPECIFICATION

FOR RECTIFIED

SPIRIT

(Revised)
0.

FOREWORD

0.1 This revised Indian Standard was adopted by the Indian Standards
Institution on 6 July 1959, after the draft finalized by the Alcohol and
Allied Products Sectional Committee had been approved by the Chemical Division Council.
0.2 Indian Standard Specification for Rectified Spirit ( IS : 323-1952)
was first published in 1952. In that standard, the minimum ethanol
content of rectified spirit had been left to the option of the purchaser
and the vendor subject to a minimum of 9127 percent by volume ( 60
OP ). Since the publication of that standard, the alcohol industry has
iprogressed considerably and the industry stated that they are in a
tion to sup ly 66OP e&it.
In accordance
with the decision o pthe
Sectional 8 ommittee responsible for the preparation of this standard, a
survey was conducted to ascertain the views of the various distilleries in
On the basis of
India and the Excise Departments of various States.
information collected through this survey and from other sources, the
Sectional Committee decided to revise this standard, especially with
regard to ethanol conttri$, acidity, residue on evaporation and to prescribe potassium ferro-cyanide method as an alternate method for the
determination
of copper.
0.3 The computation of strength of aqueous solutions containing ethanol
is at present made in the country from specific gravity figures at 156C
d or 60F ) and the strength is expressed in terms of proof spirit. The
. *Sectional Committee responsible for the preparation of this standardg
however, felt that it would be advisable to abolish the proof spirit
method of expressing strength of alcoholic solutions and to introduce,
in its place, the method of stating the percentage of alcohol by volume,
The
using the centesimal alcoholometer and the Gay-Lussacs
tables.
compilation of alcoholometric
tables based on Gay-Lussacs tables with
necessary modifications to suit Indian conditions is under consideration
Till these tables are finally adopted by
of the Sectional Committee.
the Government
and the industry, it was considered necessary to eontinue prescribing, in this revised standard, the specific gravity figures
and strength of alcoholic solutions at 15*6C.
3

.lS:323-1959
0.4This standard requires rckrcnce to the following Indian Standard
Specifications:
*IS : 264-1950
*IS : 265-1950
*IS:266-1950

NITRICACID

HYDROCHLORIC
ACID
SULPHURICACID
*IS : 321-1952 ETHYL ALCOHOL(ABSOLUTE ALCD~OL)
*IS: 1070-1957 DISTILLED WATER

0.4.1 Wherever
a reference
to any Indian
Standard
mentioned
under 0.4 or otherwise appears in this specification,
it shall be taken as
a reference to the latest version of the standard.
0.5 This standard
is one of a series of Indian
Standard
Specifications
on materials
containing
ethanol ( CHsCHsOH ). The other specifications published
so far in the series are:
*IS: 321-1952 ETHYL ALCOHOL (ABSOLUTEALCOHOL)

IS:322-1952 POWER ALCOHOL

IS:324-1959 ORDINARY DENATURED SPIRIT(Revised)
*IS: 1049-1957 ALCOHOL, PERFUMERY GRADE
0.6Metric

system has been adopted

in India and all quantities
and
dimensions
in this standard
have been given in this system.
Non-metric
values to which the alcohol industry has been accustomed
are also given
in brackets, wherever
necessary,,for
the sake of smooth changeover
by
December
1966.

0.7 For the purpose

of deciding
whether
a particular
requirement
of
is complied with, the final value,observcd
or calculated,
qJr@SilJg
the result of a test or analysis, shall be rounded off in accordance with *IS: 2-1949 Rules for Rounding
Off Numerical
Values.
The number
of significant
places retained
in the rounded
off value
should be the same as that of the specified value in this standard.
this standard

0.8 This stdndard is intended

chiefly to cover the technical
provisions
.r&+ting
to the material,
and it does not include all the necessary provisions of a contract.
1. SCOPE
1.1 This standard
prescribes
the requirements
and the methods
of
sampling and test for the material
known as rectified spirit.
The
mterjal
js used as a reagent and solvent in the chemical
and pharmaceutical industries,
and for production
of potable alcoholic
beverages.
*Since revilsd.
4

IS:323-1959
2. TERMINCBL.OGY
2.0 For the purpose of &is standard, the following definitions shall
apply.
2.1 Ethyl ticoh
4 Absolute Alcohol ) - Mat&al obtained from spirit
by removing the water present, as much as possible, by suitable treatment. It shall not contain more than 0.5 percent of water by
volume.
2.2 Overproof Spirit ( OP ) - Mixture of ethanol ( C,H,OH ) and water,
containing a greater percentage of ethanol tjlan is contained in proof
spirit. If an overproof strength is added to 100, the sum represents
the volumes of spirit at proof strength which 100 volumes of spirit of
that particular overproof strength would yield when diluted with water.
For example, 100 volumes of 60 OP spirit would yield 160 volumes of
proof spirit.
23 Proof Spirit - Mixture of ethanol (C,H,OH ) and water, which
shall, at a temperature of 10*6C ( pr SlF ), weigh exactly +#thItpahrts 0:
an equal volume of distilled water at the same temperature.
density of O-919 76 at 15.6C ( or 60F ) and contains 49.28 percent by
weight of alcohol or 57.10 percent of alcohol by volume at 156C (or
60F ) .
2.4 Spirit -Mixture

of ethanol

( C,H,OH ) and water.

3. GRAPES
3.1 There shall be two grades of the material, namely Grade 1 and
Grade 2. In addition to the above two grades, additional requirements
(see 5.3 ) to Grkde 1 have been prescribed to cater to the needs of the
acetone industry.
3.1.1 The material conforming to Grade 1 shall be suitable for use
as a reagent, for pharmaceutical
and medicinal purposes and for the
production of alcoholic beverages; Grade 2 is intended for the materjal
for other industrial purposes.
4. SdhdLING
4.1 Representative
samples of the material
ed in Appendix A.

shall be drawn as prtscrib.

5. REQUIREMENTS

shall be a cIear, colo,urless, homo5.1 Description - The material

geneous liquid free from. suspended matter and consisting essentially of
ethanol ( CHsCHsOH.) admixed with water.
5

5.2 The material

Table I.

shall also comply with the requirements

TABLE I

prescribed

in

REQUIREMENTS FOR RECTIFIED SPIRIT

MBPBOD

or

TE:~T ( Rnp TO
APPEWDIX )
(3)

(2)

(1)
9

Specific gravity at 16*V/

16*WC t or 60/60B ).

ii)

Ethenol aontent:
a) Percent by volume
at WBC (or 60F ),

Max

Min

b) 2~

over-proof,

iii)

Miscibility with water

iv)

Alkalinity

v)

Acidity ( a8 CH,COOH 1,
percent
by
weight,

Max
vi)

Residue on evaporation,
percent
by
weight,

Ma
vii)

Aldehyde
CH,CHO

content
( as
), g per 100 ml,

Max
viii)

Eeter

content

ClWQCC,H~ 1.
100 ml, Max

xi)

xii)
xiii)

per

Lead ( aa Pb ), g per 100

ml, MUX
Methyl alcohol content

Fuse1 oil content

Furfural content

O-817 1

94.68

94.66 1

66

66

Miscible

Miscible

Nil

Nil

0902

Or01

0.005

001

WOO6

0.10

( as

ix)
x)

0-817 1

0902
00004

0900 1

To satisfy the
requirement
of the test

do
do

M
N

5.3 Additional Requirements for Rectified Spirit, Grade 1, for Acetone

Manafacture - In addition to the re uirements given in 5.1 and for
Grade 1 in Table I, excepting speci Bc gravity and ethanol content,
recti(ied spirit *for acetone manufacture
shall also comply with the
requirements given in Table II.
6

Is:323-1959
TABLE -II ADDITIONAL REQUIREMENTS FOR RECTIFIED SPIRIT,
GRADE 1, FOR ACETONE NUNUPACTURE

( ClotcJr 6.3 )
SL
No.

CHUACTEIXIWO

ii)

METHD 01
TB~T ( k ~CFTC
APPB~DIX )
(4)

(3)

(3)

(1)

i)

RE~UllIEMSUT

Specific gravity at 16~f3/UV60C( or

60D/600F ). Max
Ethsnol aontent:
a) Percent by volume at 15WC
( or 60F ), Min
b) Degrees overproof, Mln

iii)

Total sulphur and oompoundr

eulphur
((LB 8 ), percent
weight, Max

of
by

iv)

Sulphur dioxide ( aa SO* ), pemaemt,

by weight, Max

0818 0

Kg

0.001

I?

ooooo5

6. TESTS
6.1 Tests shall be carried out as prescribed in appropriate
specified in co1 5 of Table I and co1 4 of Tabie II.

appendices

6.2 Qoality of Reagents - Unless specified otherwise, pure chemicals

( see Note ) and distilled water ( see IS : 1070-1957 ) shall be employed
in tests.
Pure chemiceh ehsll mean cbemiaU)e which do not contain impuriNOTEties that effect the reeults of snalysin.

7. PACKING AND MARKING

I-

7.1 Packing
9.1.1 The material shall be packed in such containers as are agreed
to between the purchaser and the vendor, subject to the provisions of
law in force for the time being.
7.1.2 All containers,
in which the material is packed, shall be dry,
free from substances soluble in rectified spirit and leak-free..

clean,

7.1.3 Necessary safeguards against the risk arising from the storage
and handling of large volume of flammable liquids shall be provided,
and all due precautions shall be taken at all times to prevent accident
by fire or explosion.
lScared revhioo in 197;.

rs:323-1959
7.1.4 Except when they are opened for the purpose of cleaning and
rendering them free from alcohol vapour, all containers
shall be kept
securely closed unless they have been thoroughly cleaned and free from
alcohol vapour.
7.2 Marking - All containers in which the material is stored or transported shall be marked as prescribed by law in force for the time
being.
7.21
Mark.

The containers

may also be marked with the IS1 Certification

NOTE- The use of the Standard Mark is governed by the provisiona of the
&mu of Indim Standards Act, 1986 and thcilulcs and Regulations mado them.
w.
The Standard Mark on products covered by an Indian Standard conveys
tiw assurance that they have bean produced to comply with the requirements of that
u8ndrrd undor a well defined system of inspection, testing and quality control

APPENDIX
( Clause 4.2 )
SAMPLING

A-l.GENERAL

OF RECTIFIED

REQUIREMENTS

OF SAMPLING

A-l.% In drawing, preparing, storing and handling

ing precautions and directions shall be observed.

A-l.1Samples shall be taken in a protected

air, dust or soot.
A-l.2

The sampling

instrument

&ll

SPIRIT

be &an

samples,

the follow-

place not exposed to damp

and dry.

A-L.3 To draw a re,presentative sample, the contents of each container

selected for sampling shall be mixed as .&horoughly as possible by suitable means.
A-l.4 Precautions shall be taknn ,ti *pr&nct &e samPlea, the material
being sampled, the sampling instxmnc~t and &e containers for ran$les
from adventitious contamination_
A-l.5 The samples
glass containers.

sh&l ,be placed

in &tabXe

clean* &F and

air-t#ht

IS : 323 - 1959
A-l.6 The sample
least

10 percent

containers
shall be of such a size that an ullage
is left after pouring in the sample.

of at

A-l.7 Each sample container

shall be sealed air-tight
with a stopper
after filling and marked
with full details
of sampling,
the date of
sampling
and the year of manufacture
of the maternal.
A-1.8 Samples shall be stored.in a cool and dry place.
A-2. SAMPLING
INSTRUMENTS
A-2.0 The following forms of sampling
instruments
may be used:
a) Sampling
bottle or can for taking samples from various depths
in large tanks, and
b) Sampling
tube.
consists
of a weighted
bottle
or
A-2.1 Sampling Bottle or Can -It
metal container,
with removable
stopper or top, to which is attached
a
to a suitable
light chain ( see Fig. I ). The bottle or can is fastened
pole.
For taking a sample, it is lowered
in the tank to the required
depth, and the stopper or top is removed by means of the chain for filling the container.

FIG. 1 SAMPLINOBOTTLE OR CAN

IS:323-19s

A-22 Sampling Tobe - It is made of metal or thick glass and is 20 to

40 mm in diameter and 350 to 750 mm in length ( ;Fcc Fig. 2 ). The

upper and lower ends are conical and reach 6 to 12 mm diameter
at
the narrow ends._ Handling is facilitated by two rings at the upper end.
For taking a sample, the apparatus is first closedat the top with the
-_I is reached.
thumb or a stopper and lowered until the dc&rcd
It
is then opened for a short time to admit the mat&aYth and finally closed
and withdrawn.
A-2.2.1 For small containers,
altered suitably.

FIG. 2

the size of the sampling

!SAMPLING TUBB

10

tube

may be

IS:323-l959
A-3. SCALE OF SAMPLING
A-3.1 Lot - All containers of the same type in a single consignment
of one grade of the material drawn from a single batch of manufacture
shall constitute the lot. If a consignment is declared or known to consist of different batches of manufacture,
the batches shall be marked
separately, and the group of containers of the same type in each batch
shall constitute separate lots.
containers selected for ascertaining conA-3.2 Gross Sample -The
formity to the specification from any lot of the material shall constitute
the gross sample representing
the lot. The number n of containers
constituting the gross sample shall be in accordance with Table III.
TABLE III
8tZE

OT

SCALE OF SAMPLING

LOT

SIZE

OF

aaorr

sAblPI,Z

W)

(4
2to

16
1.

L?

do

3 .

66::12
::
over

110

1:

A-3.2.1 The containers shall be chosen at random from the lot. To

ensure the randomness of selection, use of random number tables is
recommended.
Where random number tables are not available, the
following procedure may be adopted.
A-3.2.2 Arrange the containers in the lot systematically and, starting
from any container, count them as 1, 2, 3,...... N. The gross sample
shall consist of every rth container counted, where
r=- N
n
where
N = total number of containers in the lot, and
n = number of containers to be selected.
In ease r comes out to be a fractional number, its value shall be t&n
to be equal to the integral part of it.
A-4, TEST SAMPLES AND REFEREE SAMPLE

A-4.1Preparrtion of Sets of Soeples for Etbraoi Content-For

the
determination of ethanol content, draw with an appropriate
sampling
11

IS : 323 - 1999
instrument
( see A-2 ), small portions of the material from different parts
selected
for sampling
of each container
in the gross
sample
To obtain
samples representative
(see A-3.2 ) and freshly opened.
of each container
selected
for sampling,
mix these portions
of the
Keep these samples from diffmaterial
drawn
from each container.
erent containers
in separate containers.
Draw three equal portions
of
the material
each about 75 ml, from each of these separate
containers
and transfer them into thoroughly
cleaned and dried glass bottles, thus
obtaining
three sets of test samples.
Seal the bottles air-tight.
Send
one set of test samples to the purchaser and one to thovendor.
Reserve
the third set of test samples, bearing the seals of the purchaser
and the
vendor, as refree sample, to be kept at a place agreed
to between
the
purchaser
and the vendor.

of Composite Sample for Determination of Chrrrctera composite

sample
of
istics Other Than Ethrnol Content -Prepare

A-4.2 Preparation

not more than one litre by mixing equal portion of material

from the
samples representative
of each container
in the gross sample and keep
it in a separate
container.
Divide this composite sample into three
test samples, and transfer them immediately
to thoroughly
cleaned Lnd
Seal the bottles air-tight.
dried bottles.
Label as sample for general
Send
tests and give all the particulars
of sampling
specified in A-1.7.
one test sample to the purchaser
and one to the vendor.
Reserve
the
third test sample, bearing the seal of the purchaser
and the vendor,
as
referee sample to be kept at a place agreed to between
the purchaser
and the vendor.

A-5. NUMBER OF TESTS

A-5.1 Tests for Ethanol

Content - Tests

ethanol
content
shall be carried
representing
the lot ( see A-4.1 ).

out

for the determination

of
individually
on the test samples

A-5.2 Other Tests-Tests

for the determination
of other characteristics
specified in Table I, items (iii) to (xiii) and Table II, items (iii) and (iv),
shall be carried out on the composite sample (see A-4.2 ).
A-6. CRITERION

FOR

ACCEPTANCE

A-6.1 The material

in any lot shall he accepted as conforming
to the
specification,
if the results of testing the corresponding
test samples
satisfy the requirements
of A-6.2 and A-6.3.
Otherwise,
the lot shall
be rejected.
A-6.2 When
tested
for requirements
other
than
ethanol
content
(see A-5.2),
the test results shall satisfy the requirements
given in
Table I, items (iii) to (xiii), and Table II, items (iii) and (iv).
12

IS:323-l959
A-6.3 From the results of testing
and range

shall

be calculated

ethanol
as follows:

content

( see A-5.1), the mean

Mean

(X) = sum of the test results divided by the number of test

results so added, and
Range (R) = difference
between
the maximum
and minimum
values of the test results.
The range (R) so obtained
shall be multiplied
by 0.6 ayd the expression
(F - 0*6R ) shall be calculated.
The following table is illustrative:
TEBT

&WJLTll

ldCAN

RANOE

CBITERION

FOR

Acclcrrraam
1, 2... . . *.*. . #.,

;;

( T-W6 R ) shall be not lerr than

04.68

percent

by

volume

ut

IS-WC or W OP? or in the

oamnof rectified rplrit Grade 1
for acetone manufacture,
not
leu
than 94%
percent
by
volume at 15~VC or MW OP.

APPENDIX

[ Table I, Item (i) and Table II, Item (i) ]

DETERMINATION OF SPECIFIC GRAVITY
El.

DEFINITION

El.1 For the purpose of this standard, the specific gravity of a material
shall mean the ratio of the weight of a given volume of the material
at
the specified temperature
to the weight of an equal volume of distilled
water at the same temperature.
B-2. METHOD
B-2.1 The specific gravity
may be determined
by means of a pyknometer or a specific gravity bottle, or a special hydrometer,
such as Sikcs
A and R hydrometers;
for accurate
work the method
using specific
gravity bottle ( see B-3 ) shall be adopted.
B-3. APPARATUS
B-3.1 For determination
of specific gravity,
two alternate
specific
In case
gravity bottles shown in Fig. 3A and Fig. 3B are prescribed.
of dispute,
the vacuum
jacketed
specific gravity bottle shown in Fig.
3A shall be used.
13

IS : 323- 1959

Fm. 3A VACUUM JACKETED

FIG. 3B REGNAULT?
SPECIFICGRAVITY BOTTLE
SPECIFICGRAVITYBOTTLE

B-4. PROCEDURE
B-4.1 Fill the specific

gravity bottle with the material

to over-flowing,
holding
the specific gravity
bottle on its side in such a manner as to
prevent the entrapment
of air bubbles.
Insert the stopper, immerse in
the water bath maintained
at 15.6 f 02C ( or 60-O it 0*4F) and
Remove the specific gravity bottle from the bath
hold for 30 minutes.
and clean and dry it thoroughly.
Allow it to come to room temperature
and weigh.
B-4.2 Calculation
Specific

gravity,

at 196/15*6C
14

( or 60/60F ) = $$

Is : 323 - 1959
where
A = weight, in g, of the specific
material at 196C ( or 60F );

bottle with the

B = weight, in g, of the specific gravity bottle; and

C = weight, in g, of the specific gravity bottle with water at
15.6C ( or 60F ) .

APPENDIX

gravity

[ Table I, Item (ii) and Table II, Item (ii) ]

DETERMINATION
C-l.

OF ETHANOL

CONTENT

PROCEDURE

C-I.1 Determine the specific gravity of the material at 15*6/15*6C ( or

60/60F ) according to the method prescribed in Appendix B and find
out the strength of alcohol by weight and by volume, and also its proof
strength from Table IV
TABLE IV RELATION BETWEEN SPECIFIC GRAVITY, PERCENTAGE
OF ALCOHOL BY WEIGHT AND BY VOLUME, RND
PROOF STRENGTH
Q~mxrIc OBA~ITY IN
AXE AT 16~8/1560c
( OR 60/600F)
0.82948

PIWXNTAGE
r-------h-------~
By Weight
8732

OF ALCOHOL
By Volume at.
15wc ( or 60F )
9126

DEGREES
DvERPBOOl

60

0.82752
6%
0825

88.07
88.82

91.83
92.40

::

0.82348
0.82141
0.81929

89.60
90.38
9116

92.97
93.64
94.11

63

0.817 12
0.814 90
0.812 66

9195
92.76
93.57

94.68
9525
95*83

66
::

081030

94.39

96.38

69

080740
90
@8Ob

95.23
9609

9696
97.52

z?

@802\eS
0.80020

96.96
97%

98.09
98.66

72
73

::

NcTE - The percentage of proof spirit may by obtained by adding 100 to the
number of degrees overproof.

15

18:323-1999

APPENDIX
D
[ Table I, Item (iii) ]
TEST FOR MISCIBILiTY

WITH WATER

D-l.PROCEDURE
,D-1.1 Mix 10 ml ofthe

material with 190 ml of water in a suitable glasr

vessel and allow to stand at a temperature within the range of 27 f2C
for one hour.
Compare the clarity of the mixture with that of an
equal volume of water.

D-1.1.1 3%~ material shall be taken to comply with the specified

requirement if rbere is no noticeable difference in clarity between the
mixture and water.

APPENDIX
E
[ Table I, Item (iv) and (v) ]
TEST FOR ALKALINITY AND DETERMINATION
OF ACIDITY
El.
El.1

REAGENTS
Standard Sodium Hydroxide Solution - 0.1 N.

E-1.2Phenolphthakin

in
Indicator - Dissolve 0.5 g of phenolphthalein
100 ml of rectified spirit and carefully add standard sodium hydroxide
rolution till the colour is rendered faintly pink.
E2.

PROCEDURE

E2.1 Place 100 ml of water and a few pieces of clean porus pot in a
SOO=ml conical flask of resistance glasr, and boil gently for 5 minutes to
eliminate carbon dioxide.
Cool slightly and add 100 ml of the material.
At the end of this period,
Boil gently for a further
riod of 5 minutes.
close the neck of the F ask with a stopper carrying a soda-lime guard
tube, and allow to cool.
When cool, remove the stopper, add 0.5 ml
of phenolphthalein
indicator and examine for alkalinity; if not alkaline,
titrate with standard sodium hydroxide solution using a micro-burette.
1 2.2 Determine
the specific gravity of the material at room temperatrr . ,using a specific gravity bottle or a pyknometer
or_ a suitable
hydrometer.
16

IS : 323 - 1999
E-3. CALCULATION AND REPORT
E-3.1 Report whether

the material

is alkaline

or acidic.

E-3.2 Calculate the acidity, if any, in terms of acetic acid and

as percentage by weight of the material taken for the test:
Acidity

(as CHsCOOH

), percent

by weight =

express

iVN

where

V = volume,

in ml, of standard sodium hydroxide solution

required for the titration;
N = normality of standard sodium hydroxide so{ution; and
S = specific gravity of the material at room temperature.

APPENDIX
[ Table I, Item
DETERMINATION

F
(vi) ]

OF RESIDUE ON EVAPORATION

F-l. PROCEDURE
F-l.1 Evaporate,

on a water bath, lOO.ml or more of the material to

-l~tinum,
silica or resistance glass dish.
dryness in a weighed, clean, dryp.___
Dry the residue for 30 minutes in an oven at a temperature of 100 f2C.
Cool in a desiccator and weigh.
F-2. CALCULATION
F-2.1 Calculate
Residue

as follows:
on evaporation,

percent

by weight

B-A

= vs

x 100

where

B = weight,

in g, of dish after evaporation,

drying
and
cooling;
A = weight, in g, of empty dish;
V = volume, in ml, of the material taken for the test; and
S = specific gravity of the material determined
at room temperature ( see E-2.2 ).
17

Is:323-1959

APPENDIX
G
[ Table I, Item (vii) ]
DETERMINATION
EL

OF ALDEHYDE

CONTENT

METHODS

El.1 For Low Aldehyde C-tent - A suitable colour reaction is avaiiable when the aldehyde
content (as CHsCHO ) is expected not to
exceed 0906 g per 100 ml of the material.
This is based on the
resinification
that takes place and the yellow colour that results on
trcotment
of acet-aldehyde
with sodium hydroxide.
The procedure
described under G-4.1 provides a satisfactory qualitative limit test, but
in case of dispute, the quantitative
procedure described under G4.3
shall be adopted in the qualitative procedure, acetals are also included
as aldehydes.
Gl.2 For Higher Aldckyde Content - For materials containing @OS to
05 percent of aldehydes,
only the quantitative
procedure described
under G-4.2 shall be adopted.
G3,

APPARATUS

G-2.1 Stoppered Flasks -two,

shape, size and colour.
6-3.

each of 250-ml capacity

and identical

REAGENTS

G-3.1 Sodium Hydroxide Solution - Dissolve

in water and dilute to W-ml with water.

20 g of sodium

G-3.3 St@k Solotion of Hydroxylaqine Hydrochloride of hydroxylamine

hydrochloride
in 100 ml of water.
6-33

in

Metapheayleaedlrmiae

hydroxide

Dissolve

20 g

Hydrocblorlde

rectified
spirit over solid
6-3.4 Aldehyde-Frea
Alcohol - Re-distil
caustic soda or caustic potash, add 2 to 3 g of metaphenylenediamine
hydrochloride per litre of rectified spirit, digest at ordinary temperature
for several days or under a reflux condenser on a steam bath for several
hours and distil slowly, rejecting the first 100 ml and the last 200 ml of
the distillate.
G-3.5 Standard

Sodixm Hydroxide

SAtion

- 01 N.

G3.6 Bromqsbaxel BIxe SohtIox - Dissolve 01 g of bromophenol blue

in 1.5 ml of standard sodium hydroxide solution and dilute with water
to 250 ml.
18

IS : 323 . 1959

~~%fneydro@mine
Reagent ( Neutral A!cohol Solotiop of .Hydroxy- D&lute 10 ml of the stock solution of hydroxylamme
hydro-

chloride with 100 ml of aldehyde-free

alcohol, add 2 ml of bromophenol
blue solution and then add standard sodium hydroxide solution till the
characteristic
dichroic yellowish green colour is obtained.
G-4. PROCEDURE
G-4.1 Qualitative

Test

G-4.1.1 Mix 10 ml of the material

solution and set aside for 5 minutes.

with 5 ml of sodium hydroxide

G-4.1.2 The limit prescribed for aldehyde content (0.006 g per 100
ml ) shall be taken as not having been exceeded if no yellow colour is
produced in 5 minutes.
G-4.2 Quantitative

Test

6-4.2.1
Take 50 ml of the material in a flask, add 25 ml of hydroxylamine reagent and 25 ml of distilled water. Allow to stand for 15
minutes. Meanwhile prepare a blank in a similar flask by using 25 ml of
hydroxylamine reagent and 75 ml of distilled water. Titrate this solution
with standard sodium hydroxide solution until the characteristic dichroic
yellowish green colour appears. Titrate the sample solution with standa>d
sodium hydroxide solution until the colour matches with that of the blank
solution.
G-4.2.2 Calculation
Aldehyde content ( as CHsCHO ),
=0-O 8(V---v)N
g per 100 ml
where
V = volume, in ml, of standard sodium hydroxide solution
required for the titration;
v = volume, in ml, of standard sodium hydroxide solution
requised, if any, in the b1an.k; and
N = normality

of standard

sodium hydroxide solution.

APPENDIX
[ Table I, Item

H
(viii)

DETERMINATION
OF ESTER CONTENT
( AS ETHYL ACETATE )
H-l.

REAGENTS

H-l.1 Standard Potassinm Hydroxide Solutions - two, O-1 N and 05 N

H-l.2

Standard

Ssipbmic

Acid -

0.1 N.
19

IS : 323 - 1959
in
H-l.3 Phenolpbtb8leia
Indicrtor
- Dissolve 05 g of phenolphthalein
100 ml of rectified
spirit and carefully
add standard
potassium hydraxidc solution (0.1 N ) till the colour is rendered
faintly pink.
H-2.

PRO,CEDURE

H-2.1 Transfer
exactly 100 ml of the material
into a heat resistant flask
of about 200-ml capacity, add a few drops of phenolphthalein
indicator
and neutralize,
in the cold, the free acid, if present, with standard potaAdd two millilitres
of standard
ssium hydroxide
solution
(O-1 N).
potassium
hydroxide solution (@5 N ), attach the flask to a reflux condenser provided with a soda-lime
guard tube and reflux the contents on
Cool the contents,
pour into ana water bath for at least one hour.
other flask, wash the original flask with 100 ml of freshly distilled water,
add the washings to the original liquor and then titrate
with standard
sulphuric
acid adding a few drops more of phenolphthalein
indicator.
H-2.2 Carry out a blank,
ized material.
H-3.
H-3.1

using

100 ml ofwater

in place of Lhe neutral-

CALCULATION
Calculate

the percentage

of esters

(as ethyl acetate)

as follows:

Esters as ethyl acetate ( CHsCOOCsH,

),
g per 100 ml
= 0.088 ( V, -Ya ) N
where
V, = volume,
in ml, of standard
sulphuric
acid required in
the blank;
Vg 7 volume, in ml, of standard
sulphuric
acid required
with
the material;
and
l

N = normality

of standard

sulphuric

acid.

APPENDIX
J
[ Table I, Ifem (ix) ]
DETERMINATION
J-1.

OF COPPER

METHODS

J-l.1 Diethyl dithio carbamate

and potassium ferrocyanide
methods are
recommended.
The potassium ferrocyanide
method is easier to perform
and sufficiently
sensitive
and accurate
for routine
type of analysis.
20

lS:323-ml9
The diethyf dithio ea.&mate method ( see J-4.1.1 ) is more sensitive and
zhall serve az a referee method in Case of dispute or where zinc is present.
J-2. APPARATus
J-2,1 Nasler Tabea - flat bottom tubes of thin, colourless glass, about
25 mm in diameter and about 150 mm in length, graduated at SOml.
The depth, measured internally from the graduation mark to the
bottom, shall not vary by more than two millimetres in the tubes used
for the test..
J-3. REAGENTS
J-3.1 Dilute Salphuric Acid - approximately 10 percent (v/v).
J-3.2 Aqve Regia - A mixture of one volume of concentrated nitric
acid (-conforming to IS : 264-1950*)and three volumes of concentrated
hydrochloric acid ( conforming to IS : 26%195Oe).
J-3.3 Citric Acid
J-3.4 Dilotc Ammonium Hydroxide - approximately 10 percent ( v/v).
J-3.5 Standard Copper Solution - Dissolve 1.119 g of copper.sul hate
( CuSO,, 5H,O ) in water and dilute to one litre. Dilute 10 ml oF this
rolution to 100 ml. One millilitre of the diluted solution ( referred to
later as standard copper solution ) contains O-02845 mg of copper. The
diluted solution shall always be prepared immediately before use.
J-3.6 Sodium Dicthyl D/thio Cnrbamate Solution - Prepare 0.1 percent,
by weight, solution of sodium diethyl dithio carbamate [ ( C,H, )*
NCS.SNa] in water.
J-3.6.1 Sometimes the dicthyl dithio carbamatc available may be
incompletely soluble in water, in which case the insoluble material may
be removed by filtration through an ashless filter paper. . The reagent
is best prepared just before use, but can be stored for one or two weeks
in an amber-coloured bottle without appreciable deterioration.
J-3.7 Carbon Tetracbloride
J-3.8 Ammonium Chloride
J-3.9 Acetic Acid - approximately 5 percent by weight.
J-3.10 Potrsaiam Ferrocyaaide Solution - approximately
weight.
. _*Since revined.

21

4 percent by

IS : 323 - 1959
J-4. DIETHYL DITHIO CARBAMATE METHOD
of copper, an aqueous solution of sodium ( or
zinc ) diethyl dithio carbamate gives a golden brown colour in acid,
ammoniacal
or neutral
solutions.
The diethyl dithio carbamate
method has advantages over the ferrocyanidc method, which is in vogue
in some laboratories,
since it is more sensitive and is free from interference by iron and zinc. The method is suitable when the copper
content ranges from 0.01 to O-15 mg of copper in the quantity of the
material taken. With larger quantities of copper, the mixture of the
test solution and reagent rapidly becomes cloudy, and any observance
of this in the prescribed test is sufficient for condemning the sample as
containing excessive quantities of copper.
If a quantitative determination is required, the test should be repeated by using proportionately
smaller quantities of sample for test.

J-4.1 In the presence

J-4.1.1 Two variations of the method are available: (a) without

extraction, and (b) with extraction.
Ordinarily, it is not necessary to
resort to the procedure of extraction which shall be obligatory only
when a referee method is required in case of dispute between the
purchaser and the vendor.
J-4.2 Preparation of Test Solation - Transfer 20 m of the material
into a silica evaporating dish and add one millilitre of dilute sulphuric
acid.
Heat gently in the beginning and then evaporate almost to dryness on a water bath.
Ignite the residue over a smokeless flame to
eliminate the sulphuric acid. Cool, dissolve the residue in two millilitres of water, add three drops of aqua regia and evaporate to dryness
on a water bath.
Dissolve the residue in water, neutralize, if required,
with dilute ammonium hydroxide and make up the volume to 25 ml.
J-4.2.1 TO detect copper contamipation,
if any, in any of the
reagents, blank experiment shall be carried out using the same quantities of the reagents.
J-4.3 Procedure Without Extraction

J-4.3.1 Take in a 50-ml Nessler tube, 10 ml of the test solution prepared as described under J-4.2.
Add two grams of citric acid and 10
ml of dilute ammonium hydroxide.
Make up to 50 ml with water.
J-4.3.2 Prepare a series of control solutions, each containing in 50 ml,
two grams of citric acid and 10 ml of dilute ammonium hydro$ide together with increasing amount of copper, namely @I, 0.2, 0.4, O-6, @g
and 1.0 ml of standard copper solutiim ( see J-3.5).
J-4.3.3 The
turbidity.

test solutions

and

controls
22

should be free from any

IS:323-1959
J-4.3.4Cool all solutions to 20% and
diethyl
dithio carbamate
solution and
the control solutions.
Note the number
copper solution added in the control
possibic, the same intensity
of colour as
J-4.4

to each add two millilitres

of
match the test solution against
of millilitres
of the standard
solution
having,
as nearly
as
that of the test solution.

Procedme with Extraction

_J-4.4.1 Extract
immediately
the copper
organometallic
compound
produced
as described
under J-4.3.4 with four successive portions,
2.5
ml each, of carbon tetrachl-oride
and compare the colour of the solution
so obtained
in a calorimeter
with the extracts
of control
solutions
similarly
prepared.
J-4.4.2 Chloroform
it is almost insoluble
quickly.
J-4.5

may be used but carbon tc!rachloride

is better as
in water and forms clearer solutions which separate

Calculation

Copper ( as Cu ), g per 100 ml = 0900028 45 X 12.5 Y

where
V = volume, in mf, of the standard bpfx-r salurion in the control solution which gives the closer; match.

J-5. POTASSIUM FERROCYANIDE METHOD

20 mi of the material
in?0 a silica evaporatJ-5.1 Procedure - Tr2:dcr
ing dish and add one milli!itre
of dilute sulphuric
acid.
Meat gently
in the beginning
and then evaporate
almost to dry_lless on a water bath.
Ignite
the residue over a smokeless
flame to &m&ate
the sulphuric
acid.
Cool, dissolve the residue in two millilitres
of water, add three
drops of aqua regia and evaporate
to dryness on a water bath.
Dissolve
the residue in two millilitres
of dilute hydrochloric
acid and warm
Add 0.5 g of ammonium
chloride
gently till the residue is dissolved.
in all-glass
apparatus.
Add
and dilute to 15 ml with water distilled
dilute ammonium
hydroxide
till alkaline:
Roi! off excess of ammonia
and filter into a clean Nessler tube.
Cool and then render the solution
acidic with acetic acid ( 3 to 5 drops are usually sufficient ). Dilute to
40 ml.
Add O-5 ml of potassium ferrocyanide
solution,
stir and make
up the volume to 50 ml.
NOTE-If
the copper is more, a lesser amount, scry 10 ml, of the material
mtly be taken for the test.

J-5.1.1 Prepare a seriel of control solutions each containing in 50 ml,

0*5 g of ammonium
chloride,
3 to 5 drops of acetic acid, O-5 ml ofpotassium ferrocyanide
solution together with increasing
amount
of copper,
namely 2, 4, 6, 8 and 10 ml of the srandcvd copper solution ( see J-3.5).
23

IS:323-1959
J-5.1.2 Compare the test solution (see J-S.1 ) with control solutions
and note the number of millilitres of the ~fandurd copper solution added
in the control solution having, as nearly as possible, the same intensity
of colour as that of the test solution.
J-S.2 Calculation
Copper (asCu),gper
100m1=000002845
x SY
where
V = volume, in ml, of the standard copper solution in the control solution which gives the closest match.

APPENDIX
K
[ TabZe I, Item (x) ]
DETERMINATION

OF LEAD

K-9. METHOD
K-O.1 The dithizone method, although more accurate, is considered too
lengthy for adoption, and the determination of lead content by use of
sodium sulphide 1s satisfactory for the material.
K-l. APPARATUS
K-l.1 Nessler Tubes - same as described in J-2.1.
K-2. REAGENTS
K-2.1 Bromine Water - saturated
K-2.2 Concentrated
IS : 266-1950 *).

solution of bromine in water.

Sulpburic Acid ( Lead-Free ) - ( conforming

to

K-2.3 Silver Nitrate

K-2.4 Sodium Hydroxide Solution - 10 percent

K-2.5 Alcobol ( Lead-Free )-approximately
50 percent by volume.

by weight.

95 percent by volume and

K-2.5.1 Treat alcohol (95 percent by volume ) with bromine water

until a permanent reddish brown colour is obtained, and add sodium
hydroxide solution till the colour is discharged.
Add one gram of
*Since revid.

24

SS:S3-l9S9
silver nitrate, leave overnight 8nd dirtil. Reject the culier .fmcti8n of
the distiWe,
collect the nuddle fnction 8ep~ately 8nd store in bottl8a
of lead-free glass.
K-2.5.2 Dilut!: the strong
required, by adding water.

alcohol

to SO percent

by volume,

wh8n

K-2.6 hBBlOBiOm Acetate ~btion

( ba&%rcr ) -Dissolve
20 g of
ammonium acetate in water and dilute to 50 ml. This solution should
be practically colourless.
K-2.7 Strndud
Dilute Lerd sOlutio8 - Dissolve
in 100 ml of w8ter,
0159 8 g of lead of nitrate [ Pb(NOs);I which has been 5nely ground
previously
and dried at 100 &2C.
Clear any cloudiness with a few
drops of acetic acid and dilute to 1000 ml.
Further dilute 10 ml of
this solution to 100 ml.
gach millilitre of this dilute rolution contains
an equivalent of 0400 01 g of lead.
K-2.8 Wdiom Sulphide %htiOB - Dissolve 10 g of crystallized sodium
sulphide in 100 ml of water.
The solution should be colourless.
I
K-3. PROCEDURE
K-3.1 Prepu8tion
of Teut Solution - Transfer 100 ml of the material
into a silica basin and treat with bromine water until a permanent reddish brown colour is obtained.
Evaporate the solution to drynur on a
water bath and then ignite over a Bunsen flame to destroy organic
Dissolve the mineral residue in concentrated
sulphuric acid
matter.
( lead-free ) and heat continuously until copiour fumes of sulphufoxidcs
are given off. Cool, wash down the sides with a little water, and again
evaporate on a water bath and heat to fuming.
Transfer the resuiue
tb a small 2%ml beaker with the aid of a few millilitrer of water, treat
with anequal volume of lead-free alcohol ( 95 percent by volume ) and
allow to stand overnight
for completion
of the precipitation ofliad
Filter off the precipitate, and wash, four times with 8 few
sul hate.
mi Plilitres of lead-free alcohol ( 50 percent ). Dissolve the precipitate
of lead sulphatc by adding, each time, 10 ml of boiling ammonium
acetate solution in small quantities at a time on to the fil_ter paper containing the lead sulphate precipitate.
Collect the filtrate in a S&d,
graduated flask and make up to volume with water.
K-3.2 Take in a Xl-ml Nessler tube. 10 ml of the prepared test solution
prepared as described under KU.
Dilute to SO ml with water. Prepre
8 series of standard comparison rolutions in other Ncsslcr tubes, e8ch
containing in 50 ml, two millilitres of .ammo$um
acetate solution togethlr with increasing amount -of le8d, namely 1.5, 20,2S and 30 nd
of standard dilute lead solution.
The test solutions and sta8&r&
should be water-white.
To e&h of the compirison
tubes, add two

-2s

IS:323-l9$!J
dropm

ofsodium

sulphide solution, mix thoroughly and view the coiour. light reflected through the Nessier tubes from a glazed white
tile ia zn cd at an angle to the observer.

ation

K4.3
been
under
ml of

The specified limit of requirement ,+a11 be taken as not having

exceeded if the coiour produced m the tube with the material
test is not darker than that produced in the tube containing
29
the standard .diiute lead solution.

K-4. CALCULATION
K-4.1 If a quantitative
result for lead content is required, note the
volume of standard dilute lead solution added in the comparison
tube
having, as nearly as possible, the same shade as that obtained with the
material under test.
Lead (as Pb ), g per 100 ml = 040001 x SA
where
A = volume, in ml, of standard dilute lead solution
the tube which gives the closest match.

us:d in

K-4.2 The test should be repeated starting with proportionately

smaller
amounts of prepared test solution if the shade obtained is darker than
that Iproduced in the tube containing
3 ml of standard dilute lead
solution.

APPENDIX
L
[ Table I, Item (ki) ]
TEST FOR METHYL
Ll.

ALCOHOL

REAGENTS

L-1.1, Potassium Pemmaganate

Solution in Phosphoric Acid - Dissolve
3 g of potassium permanganate
in a mixture of I5 ml of phosphoric acid
containing 89 percent by weight of phosphoric acid ( HsPO, ) and 70 ml
ofwater, and add a sufficient quantity of water to produce 100 ml.
L-I.$ Oxalic Acid Solation in Sdpbaric Acid -Cautiously
add 6Oml
of concentrated
sulphuric
acid ( conforming
to .IS : 266-1950*) to an
equal ~oiume of water and cool.
To 100 ml of this cooled, dilute sulphuric acid, add 5 g of oxalic acid crystals.

L-1.3 Tbhgemclr 18drtbn,

De~~loarhad

rineirr600mlofw;rtaandcoeiinuricebeth.
lSinoordnd.

26

- Diive

one gram of fuchAdd2Ogofaodium

IQ:323
sulphite dissolved in 100 ml of water, cool in an ice bath and further
slowly and with constant stirring, 10 ml of concentrated
hydrochloric
( conforming
to IS : 265-1950* ). Dilute to 1000 ml.

-I%9
add,
acid

L-1.3.1 Decolourized
solution of magenta should be protected
from
If the resulting
solution is turbid,
it should be fiftered
and if
light.
brown in colour, should be shaken with sufficient animal
charcoal
(0.2
Occato @3 g ) to render it colourless,
and then filtered immediately.
sionally,
it is necessary
to add 2 to 3 ml of concentrated
hydrochloric
The
acid followed by shaking, to remove a little residual pink colour.
solution
resulting
from any of the foregoing modifications
should be
allowed to stand over-night
before use.
L-2.

PROCEDURE

L-2.1 Dilute 0.5 ml of the material

with water to 5 ml, and add 2.0 ml
Set aside for
of potassium
permanganate
solution in phosphoric
acid.
ten minutes
and then add 2.0 ml of oxalic acid solution in sulphuric
acid.
To the colourless solution,
add 5 ml of decolourized
solution
of
magenta
set aside at a temperature
between
15C and 30C. and
examine
after 30 minutes.
L-2.2 Compare the final change in colour against a blank produced
by
The material shall be
adding 5 ml of water to 5 ml of magenta solution.
taken as satisfying the requirement
of this test if no colour change is visible
between the two solutions.

APPENDIX
M
[ Table I, Item (xii) ]
TEST
M-l.

FOR

FUSEL

OIL

PROCEDURE

M-l.1 Allow 25 ml of the material

to evaporate
in a porcelain
dish,
protected from dust, until a little liquid is left over. Remove the dish away
from the water bath and allow the liquid left in the dish to evaporate
without applying
any external
heat till the surface of the dish is hardy
moist. Observe if foreign odour is perceptible.
M-l.2 Add one millilitre
to IS : 266-1950 *).

of concentrated

sulphuric

acid

( conforming

M-l.3 The material

shall be taken as satisfying the requirement
of this
test if no foreign
odour is perceptible
and no red or brown colour is
produced
on treatment
with concentrated
sulphuric
acid.
--_.___
__.. _.
*Since revised.

IS : 323 - 1959

APPENDIX

[ TabZe I, nItem (xiii) ]

TEST
N-l.

FOR

FURFURAL

METHOD

N-I.1 Unlike acetaldehyde or other higher aliphatic aldehydes, a solution of furfural in rectified spirit gives a characteristic
red colour with
aniline acetate which may be used both for the detection and the
quantitative calorimetric determination of furfural in spirits in the presence ofthe other aldehydes.
The rate of development
of the colour
is slow if the atmospheric temperature is below 15C, but at temperatures above 15C, the optimum time for reaching the colour is 5 to 10
When the quantity of furfural is
minutes after mixing the solutions.
small, the colour rapidly fades away after this interval, the fading being
The limit of sensitivity of the test is
more rapid in hotter months.
about 0000 2 percent or 2 parts per million of furfural.
N-I.2 Copper, when present in excessive quantities, interferes with the
test by giving a green colour which masks the red, so that when an
excessive amount of copper is suspected, the test is carried out on a
distilled sample.
N-2. REAGENTS
N-2.1 Aniline-pure,
re-distilled.
coloured yellow or reddish, re-distil
coloured bottle.

In case the material

is deeply
before use and stock in an amber-

N-2.2 Glacial Acetic Acid

Solution) - Dilute I.0 g of

furfural in 100 ml of furfural-free alcohol ( 50 percent by volume ) and
further dilute 5 ml of this solution to 100 ml with furfural-free
alcoho1
( 50 percent by volume ). The stock solution thus prepared contains
0.05 g of furfural per 100 ml.
N-2.3 Standard Furfural Solution (Stock

N-2.3.1 Stock solution should be prepared from freshly distilled furfural ( boiling point 161C).
Best results are obtained by using furfural
purified by distillation under reduced pressure ( boiling point 54 to 55C:
at 17 mm).
N-2.4 Standard Furfural Solotion, Dilute -.Dilute
two millilitres of the
stock solution to 100 ml with pure, furfural-free alcohol (50 percent by
volume).
One millilitre of this dilute solution contains 001 mg of
furfural.
28

lS:323-l959
N-2.4.1 The stronger solution of furfural ( stock solution ) may be
retained for use up to a year, but the dilute solution wiI1 not retain its
strength for more than a few days.

N-3. PROCEDURE
N-3.1 Take 5 ml of the material under test in a colourless glass cylinder.
Dilute with 5 ml of water and, after thorough mixing, .add 0.5 ml Of
aniline, preferably with a pipette, and 1.0 ml of glacial acetic acid, preGently agitate the mixture till it becomes
ferably from a burette.
homogeneous and then set it aside for a period of 5 minutes at a temperature above 15C.
N-3.1.1 A 2Eml graduated cylinder, with a spout, would be more
suitable than Nessler tubes if quantitative
determination
of the furfural content is reqW
N-3.2 In case furfural is present in the material, a red colour starts
developing
in the course of a few seconds and reaches its maximum
intensity in 5&o 10 minutes.
N-3.3 The test for furfural content
ifno r,ed colour, either permanent
prescrtbtd test.

shall be taken to have been satisfied

or transient, develops during the

APPENDIX
P
[ Table II, Item (iii).]

DETERMI[NATION OF TOTAL SULPHUR AND COMPOUNDS OF SULPHUR (as S)

P-l.

METHOD

P-1.1 A known quantity of the material is burnt in a lamp, the products

of combustion being drawn through sodium peroxide solution and the
resulting sulphate being determined by nephelometric
method.
P-2. ASSEMBLY
P-2.0 Tht following

OF. APPARATUS
apparatus

shall be assembled

as shown in Fig. 4.

It shall consist of two bottles A and B and

P-2.1 Air Purifyfag Twina tower .C, of the dimensions shown in Fig. 4, all packed with pumice;
The pumiccin A at&C still betsoaked with potassium hydroxide,solution, so thatlfta depth&
former is 2 or -3 cm, and in the. latter ust
suIRcitnt tooover thetiltt
tube. The pumict ln B shall be aoa c cd
29

iii
..

7
5CJ

c
II

Fro.4 ASSEMBLY OF

,,-

APPARATUS

IS:323-1959
with lead acetate solution to a depth of 2 or 3 cm. The inlet tubes in
A and B shall reach within a few millimetres of the bottom.
P-2.1.1 This arrangement
will remove acidic sulphur compounds
only and if the air contains such compounds as carbon bisulphide or
thiophene, the train should be preceded by a length of combustion tubing, packed with coarse copper oxide, and heated to dull redness.
In
that case, the bottle B should contain potassium hydroxide solution
instead of lead acetate solution.
P-2.2 Chimney and Absorption Train -The
air from the tower C shall
be introduced by the side-tube E to the foot of the chimney D, into
which the lamp F fits with a rubber stopper.
The products of combustian shall be drawn up the chimney D and thence into the first absorp-,
tion bottle G, which shall consist of a 500-ml wide-mouth bottle,
immersed in an ice bath.
The connection shall be sloped at L to
avoid the possibility of condensed water running down the hot chimney.
The ice bath condenses the water and also cools the gases before they
enter the sodium peroxide solution, thus avoiding undue decomposition
of the latter.
P-2.2.1 From the absorption bottle G, the gases shall pass through
the tower H, containing short pieces of glass rod. The train shall be
completed with the Drechsel wash-bottle K of about 2%ml
capacity.
The bottles G and K and the tower H shall each contain 25 ml of
The liquid from H can be drained by
sodium peroxide solution.
pinchcock M.

_ -

P-2.3 Lamp - The lamp F as shown in Fig. 5A shall consist of a flat

bottom flask of about 400 ml capacity.
The neck of the flask shall be
constricted at N to support the tube R in which shall be loosely fitted
an ordinary cylindrical cotton-wick.
The length of R shall be such that
when the lamp is in position, the top of R shall be about 4 cm above
the top of E ( see Fig. 5B ). During weighing, a test tube P should be
inverte-d over the wick as a sheath ( see Fig. 5A >.
P-2.4 Nessler Tubes - two tubes of thin white glass, about 25 mm in
diameter and about 150 mm in length, graduated at 50 ml. The depth,
m,easured internally from the graduated mark to the bottom, shall not
vary by more than 2 mm in the tubes used.
P-3. REAGENTS
Alcohol
P-3.1 Ethyl
IS : 321-1952*.

(Absolute

AJcoboJ ) - conforming

P-3.2 Potassium Hydroxide Solution - 50 percent ( w/v ).

*Since revised.
- --

__..3l

to

33

5A
FIG. 521 AND 5B

P-33

Leaia da&ate

.!LAW

20 percent

( w/v 3.

P-3.4 Sodimn Pm&de

S&tiQa - Dissolve
,pepoxide Gn %&I .X&lof%CX!c&M w&t=.
P4B:5 C?on~~tz&ed
.P&s Barb
xqtS&als.

H#rochloric

Cl&&&

Sslntion-

cautiously

( con&rming

A&-

12 percent

i0 g of sodium
to IS : 265-1950* ).

(W/V) of barium chloride

.P-u
$&&&I
SnIpWe Sletion - Acidify 75 ml of sodium peroxide
hydrochloric acid, bring to the boil and then
sol&ion wit48 wtrated
Add 15.6 ml
.cool. Trans&zr t3se solution to a NO-ml ,volumetric ask.
cof&fX N standand s~lplmric acid and make up the volume to 500 ml
The volume of standard sulphuric acid to be added has been
mark.
caicuhsed from the following formula:
V = 0.625 PW

N
where
Y = volume,

in ml, of standard

P = percentage

of sulphur

W = weight, in g, of the material

N = normality

of standard

Since rev&d.

32

sulphuric

acid;

specified;
taken for the test; and

sulphuric

acid.-

EM. I!!RoQID~381&:
ml.1 Cle&ldng Qf w&k - Boil,.t&retick f6n an,Hm with sow&-n
ti removaloily. mtzr
and SJzo- (;w&ch mightz aontain suiRhun c4ngaunds ), than:hail!itt. for seven& minutes tit311 mcessivc
abaw
of
water until;&:rema_ins-alhas1and br$$$t+ aueeze outrtiwick,
msh it twicrr_iir.&lute
alcc&r& c&y at IO@ & 2% and inmt&ntie
R.
mdlslbp
F,
?-4.2 Tran+Z$$g
of the madldniidlaccur.a&yweighed
pouring a &t&z, &?mm the tuba&, replace t&e s&at11 and \~&g,lL.Attach
the wash&ot&z! 1 to a suc&m pump, l%#& PBe lamps. &atwa rapid
stream ofa$rt&mnugh the apeaJntus and q@iu%ly push t&e clamp into
position.
T~,ioaitial stream&air
should n%cn~
be too slow otherwise
the lamp will be extinguish&
Once the ttestis under way;, xeduce the
air stream a &&e bu: take-m
that it is, rapiid enough tzo,keep the lamp
burning,vigmusly.
When &I the Sam:+ has been buuz&!, which will
take about 24 hours, stop t&e flow of ai;a &rough the apparatus, remove
the lamp+ FepbtCC
the sheath and weigh. The differelachcez
between the.
two wdghings, W, is the weight of material consumed,
P-4.3 Transfer the contents of the vessels G, H and l&Z
to a beaker.
Ef
necessary, boil until the volume of the liquid is reduced to about 460
ml, then add 10 ml &concentrated
hydrochloric acid. Filter, ag,&
brirag to the boil. Co& the solution and make up thi volume to 500 ml
in a volumetric flask.
P-4.4 Pipette out 50 ml of the test, soIution ( see P-4.3 ) into a Nessler
tube and add 2 ml of barium chloride solution.
Carly out a control
test in another Nessler tube using 50 ml of standard sulphate solution
[if W is exactly equal to 250 g otherwiSe a proportionate lower or
higher volume ( ae P-3.7) ] and 2 ml of barium chloride solution.
Mix both the solutions well, stir and compare the turbid&y produced,
if any, after five minutes.
P-4.5 The ,matcrial shall be considered to have satisfied the require-
ment if the turbidity produced in the test with the material is not greater
than that produced in the control test.

APPENDIX
Q
[ Tnhlc 1I, Iiern (iv) ]
DETERMINATION
Q-l. APPARATUS
cl.,!, TQle apparatus
. .

OF SlJLPHUR

DIOXIDE

( SOs )

consists of the following parts assembled as shown

33

CARBON
DIOXIDE

CARBONATE

- 100

FIG. 6

HYDROGEN

ASSEMBLY

PEROXIDE

ml

SOLUTION

OF APPARATUS

FOR THE DETERMINATION

OF &JLPHUR

I)IOXlDE

IS:323-1959
Q-1.1.1 Boti& Aremove chlorine.

containing

dilute

Q-1.1.2 Round Bottom Flask C ml capacity.

Q-1.1.3 Rubber Stopper D -with

sodium

carbonate

of heat resistant

solution to

glass and of 750

8

three holes.

Q-1.1.4 Reflux Condenser F

Q-1.1.5 Delivery

Tube H

Q-1.1.6 Erlenmeyer

receiver.

Flask

J-

of 100 ml

Q-1.1.7 Peligot Tube L - containing

capacity,

4 ml of 3 percent

serving as a
( W/V) hydro-

gen peroxide.

Q-1.1.8 Rubber Stopper

Q-1.1.9

G - with one hole.

Dropping Funnel E

Q-2. REAGENTS
Q-2.1 Dilate Sodium Carbonate Solution-

approximately

1 N.

Q-2.2 Hydrogen Peroxide - 3 percent ( w/v ) prepared from 30 percent

( w/v ) hydrogen.,peroxide
by diluting it and neutralizing
with baryta
After allowing
to
solution using bromophenol
blue as indicator.
settle in cold for some time, filter any precipitate *formed; and then
determine its strength by titrating with standard potassium permanganate solution.
,&nally adjust the strength to 3 percent ( w/v).
Q-2.3 ConcenttiM!
1s :265-1950 l).
Q-2.4 Standard

Hydrochloric

Acid -

( conforming

to

Sodium Hydroxide Solution - 01 N.

0.1 g of bromophenol blue

Q-2.5 Bromophenol Blue Indicator -Grind
powder with 1.5 ml of standard s?%lium hydroxide solution and dilute
to 25 ml.
Q-2.6 Dilute

Hydrochloric

Acid - approximately

Q-2.7 Buiom Chloride Motioncrystals in 100 ml of water.

Dissolve

@5 N.

10 g of barium

chloride

Q-3. PROCEDURE
Q-3.1 Connect round bottom fiask C to reflux condenser F and glass
bottle A as shown in Fig. 6. Also insert dropping funnel E into round
*Since

mvimed.

35

Is:323-1959
bottom flask C through rubber stopper D. We dUwy
tube H to connect upper end of reflux condenser to E&nflask J, which is
followed by Peligot tube L. Extend the delivery t&e to the bottom of
Erlenmeyer flask .I to whichi 15. ml of hydmgen, paroxide have been
added.
Q-3.2 Pass carbon. d&xGdc. from the generasor- ttircgh
the apparatus
for some time to eq&all.aih
Stop flow ofr carbon; dioxide and then
add 200 ml of the,matt&lito_
the round bottom fi&&c thmugh dropping funnel E. F$K&CIG~addi thinough droppihg fun&E,
suIZicient water
to make the total v,olu_me:300iml and then ad& 2@ ml: oL concentrated
hydrochloric acid.
&lhwtdiamixture
to stand for a tiwminutes
until
fumes have s&ed.
J&d@& @he burner so that rapours do not rise
higher than one-tent& oE:&z liength of the wa&er j&ket.of the condenser
Adjust the. %w c& -bon
dioxide so
and then boil for %~GM&zx
that a slow but steadiy s&ream passes through the ronsnd bottom flask
during distillationl
Q-3.3 WasI%thp di&teq tube H and cmter& of PeIigot tube L into the
Erlenmeyer && J and titrate the solution, with standakd sodium hydroxide solution usi@ bromophenol blue as indicator.
Add 5 ml of dilute
hydrochloric acid and then 5 ml of barium chloride solution at room
temperature.,
Allow the precipitate to settle, filter through a sintered
glass cruciI& (G No. 4) or a C%ocb crucible, wash the precipitate
with boiliig water till it is free from chlorides and dry to constant
weight at 105 to 110C.
w.4

Carry out a blank on all, seagents.

Q-4. CALCULATION
Q-4.3

Sulphur dioxide ( SO,),

27.44 ( WI percent by weight = --vs

W, )

where
W, = weight, in g, of the precipitate
the material;

formed in the test with

W, = weight, in g, of the precipitate fbrmed in the blank;

V = volume, in ml, of the material taken for the test; and
S

= specific aravity
( see E2.2 ).

of the material at room temperature

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