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IS : 247 - 1987
(Reaffirmed 2010)

Indian Standard
SPECIFICATION FOR
SODIUM SULPHITE, ANHYDROUS

(Fourth Revision)
Second Reprint JULY 2007
(Including Amendment No. 1)
UDC 661.833.522

Copyright 1987
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

Gr 5

November 1987

AMENDMENT NO. 1 NOVEMBER 2004

TO
IS 247 : 1987 SPECIFICATION FOR SODIUM
SULPHITE, ANHYDROUS
( Fourth Revision )

( Page 6, clause A-2 ) Substitute the following for the existing clause:
A-2

DETERMINATION OF SODIUM SULPHITE

A-2.0 Outline of the Method This method is used to determine the purity of
sodium sulphite in the presence of sodium bisulphite. This is done in two stages.
In the first stage, sodium bisulphite is determined by titration with sodium
hydoxide using phenolphthalein as indicator. In this titration, sodium bisulphite
is converted into sodium sulphite.
This is then titrated with standard
hydrochloric acid using methyl orange as indicator. The difference of the two
readings gives a measure of sulphite. The above chemical reactions are given by
the following equation:
NaHSO3 + NaOH = Na2SO3 + H2O
Na 2 SO 3 + HCl = NaHSO3 + NaCl
A-2.1 Reagent
A-2.1.1 Standard Sodium Hydroxide Solution 0.1 N.
A-2.1.2 Phenolphthalein Indicator
A-2.1.3 Standard Hydrochloric Acid Solution 0.1 N.
A-2.1.4 Methyl Orange Indicator
A-2.2 Procedure Weigh accurately about 0.55 g of the material and dissolve
it in about 50 ml of water. First titrate with standard sodium hydroxide solution
using phenolphthalein as indicator. Then titrate with standard hydrochloric acid
using methyl orange as indicator.

Amend No. 1 to IS 247 : 1987

A-2.3 Calculation
a) Sodium bisulphite (NaHSO3)
content, percent by mass

where
V1 = volume in ml of standard sodium hydroxide solution used in first
titration,
N1 = normality of standard sodium hydroxide solution, and
M = mass in g of the material taken for the test.
b) Sodium sulphite and bisulphite
(Na2SO3 and NaHSO3) content,
percent by mass

where
V2 = volume in ml of standard hydrochloric acid solution used in
second titration,
N2 = normality of standard hydrochloric acid solution, and
M = mass in g of the material taken for the test.
c) Sodium sulphite (Na2SO3)
content, percent by mass = b - a
( CHD 1 )

IS : 247 - 1987

Indian Standard
SPECIFICATION FOR
SODIUM SULPHITE, ANHYDROUS

(Fourth Revision)
Inorganic Chemicals ( Misc ) Sectional Committee, CDC 3
Chairman
DR M. S. VAIDYA

Representing
Dharamsi Morarji Chemical Co Ltd, Bombay

Members
SHRI R. S. V Y A S ( Alternate to

Dr M. S. Vaidya )
DR A. N. BHAT

DR B. S. M O U L I K ( Alternate )
D R R . M . BHATNAGAR
S H R I R. C. BHATTACHARYA

Hindustan Lever Ltd, Bombay

Projects & Development India Ltd, Sindri
Directorate General of Technical Development,
New Delhi

S H R I K U L T A R S I N G H ( Alternate )
S H R I S. N. BHATTACHARYA
Tata Chemicals
S H R I S. G A N A P A T H Y ( Alternate )
S H R I J. C. BOSE
Indian Oxygen

S H R I A. K. D A S ( Alternate )

CONTROLLER GENERAL
S H R I V . K. J A I N ( Alternate )
S H R I S. D A S
S H R I Y U D H I S T H I R ( Alternate )
D R A. V . D E O
S H R I C. H. P A G E ( Alternate )
DR S. GHOSH
DR S. H. IQBAL
SHRI V. B. KHANNA

Ltd, Bombay
Ltd, Culcutta

Indian Bureau of Mines, Dhanbad

Geological Survey of India, Calcutta
Associated Cement Companies Ltd, Bombay
In personal capacity ( 17-A, 'F' Block, Saket, Malviya
Nagar Extension, New Delhi )
National Chemical Laboratory ( CSIR ), Pune
Directorate General of Supplies & Disposals,
New Delhi

S H R I N. K. K A V S H A L ( Alternate )
SHRI N. J. KIKANI
Sarabhai M.
S H R I H. H. K A V A R A N A ( Alternate )
Development
SHRI P. R. M A L H A N

Chemicals, Vadodara

Commissioner, Small Scale Industries,

New Delhi

S H R I R. M U K H O P A D H Y A Y ( Alternate )

( Continued on page 2 )
Copyright 1987
BUREAU OF INDIAN STANDARDS
This publication is protected under the Indian Copyright Act ( X I V of 1957 ) and
reproduction in whole or in part by any means except with written permission of the
publisher shall be deemed to be an infringement of copyright under the said Act.

IS : 247 - 1987
( Continued from page 1 )
Members

Representing

D R ANIL PANDIT
Deepak Nitrite Ltd, Vadodara
S H R I C. S. N A G A R ( Alternate )
DR P. G. PRADHAN
Golden Chemicals Pvt Ltd, Bombay
S H R I T. S. K A L A H A S T Y ( Alternate )
S H R I A. K. R A O
Shriram Foods & Fertiliser Industries,
S H R I A. K. M E H R A ( Alternate )
D R S. B. R A Y
Ministry of Defence ( DGI )

S H R I P. D A S ( Alternate )
S H R I B. K. SACHAR
S H R I A. D . G U P T A ( Alternate )

Ministry o f Defence ( R & D )

S H R I C. R. SANTHANAKRISHNAN

Travancore Chemical & Mfg Co Ltd, Mettur Dam

S H R I K. V . M A N I ( Alternate )
S H R I C. P. SHARDA
Shri R a m Institute
S H R I L. B. SRIVASTAVA ( Alternate )
D R V . S . SUBRAMANIAN
Regional Research
D R M O H D Z A F A R J A M I L ( Alternate )
SHRI N. C. THAKKAR
Indian Chemical
S H R I S. C. T H A K U R

New Delhi

for Industrial Research, Delhi

Laboratory ( CSIR ), Hyderabad

Manufacturers'
Association,
Calcutta
Indian Oil Corporation Ltd ( Refineries & Pipelines
Division ), New Delhi

S H R I M U S A F I R SINGH ( Alternate )
S H R I SATISA C H A N D E R ,
Director

Director ( Chem )

General, BIS ( Ex-officio Member )

Secretary
S H R I M . BAKSHI G U P T A

Deputy Director ( Chem ), ISI

Auxiliary Chemicals Subcommittee, C D C 3 : 1 8

Convener
S H R I J . C . BOSE

Indian Oxygen Ltd, Calcutta

Members
S H R I S. BALASUBRAMANIAN
Tamil Nadu Chemical Products Ltd, Madras
S H R I K. SUBRAMANIAN ( Alternate )
D R R . M . BHATNAGAR
Projects & Development India Ltd, Sindri
S H R I A. T. BRAHMBHATT
Kalali Chemicals Ltd, Vadodara
S H R I P. M. S A R A I Y A ( Alternate )
Travancore-Cochin Chemicals Ltd, Udyogamandal
S H R I P. C. G O P I N A T H
S H R I C. N . G. N A I R ( Alternate )
S H R I A. R. J A T A N I A
All India Cast Iron Powder Mfgrs Association,

Ahmadabad
Nitrite Ltd, Vadodara

Deepak
D R ANIL PANDIT
S H R I C. S. N A G A R ( Alternate )
DR P. G. PRADHAN
Golden
S H R I T. S. K A L A H A S T Y ( Alternate )

Chemicals Pvt Ltd, Bombay

( Continued on page 17 )

IS : 247 - 1987

Indian Standard
SPECIFICATION FOR
SODIUM SULPHITE, ANHYDROUS

(Fourth Revision)
0.

FOREWORD

0.1 This Indian Standard ( Fourth Revision ) was adopted by the

Bureau of Indian Standards on 28 May 1987, after the draft finalized by
the Inorganic Chemicals ( Misc ) Sectional Committee had been approved
by the Chemical Division Council.
0.2 Sodium sulphite, anhydrous, is used in water treatment, as a
photographic developer, in paper industry, textile bleaching ( antichlor )
and as a dietary supplement.
0.3 The standard was first issued as a tentative standard in 1950 and
subsequently revised in 1957, 1964 and 1972.
0.4 This standard has been revised again deleting the photographic grade,
as a separate Indian Standard is being formulated by Photographic
Materials Sectional Committee of BIS. A new spectrophotometry method
has been prescribed as an alternate method for determination of iron.
0.5 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*. The number of significant places retained in
the rounded off value should be the same as that of the specified value
in this standard.
1. SCOPE
1.1 This standard prescribes the requirements and the methods of
sampling and test for sodium sulphite, anhydrous.
*Rules for rounding off numerical values ( revised ).

IS : 247 - 1987
2. GRADES
2.1 There shall be the following three grades of the material:
a) Technical,
b) Pure, and
c) Analytical reagent.
3. REQUIREMENTS
3.1 Description The material of all grades shall be in the form of
a white granular powder free from extraneous matter.
3.2 Solution in Water A freshly prepared aqueous solution of the
material containing 20 g of the powder in 100 ml of carbon dioxide-free
water shall be colourless and free from sediment other than a slight
flocculence.
3.3 The material shall also comply with the requirements given in Table 1,
when tested according to the methods prescribed in Appendix A.
Reference to the relevant clauses of Appendix A is given in col 6 of the
table.
TABLE 1 REQUIREMENTS FOR SODIUM SULPHITE, ANHYDROUS
SL

No.

CHARACTERISTIC

R E Q U I R E M E N T FOR G R A D E

Technical

(1)
i)
ii)
iii)
iv)
v)
vi)
vii)
viii)
ix)

(2)

(3)
Sodium sulphite ( Na 2 SO 3 )
92.0
content, percent by mass,
Min
Insoluble matter and metals

other than alkali

metals,
percent by mass, Max
Free alkali ( as Na 2 O ), per2.0
cent by mass, Max
Sodium
thiosulphate ( as
Na 2 S 2 O 3 ), percent by mass,
Max
Heavy metals ( as Pb ), per0.02
cent by mass, Max
0.02
Iron ( as Fe ), percent by mass,
Max
Arsenic ( as As 2 O 3 ), percent

by mass, Max
Chlorides ( as Cl ), percent by

mass, Max
Free acid

METHOD OF TEST
( R E F TO C L A U S E
No. IN APPEN-

Pure

Analytical
Reagent

(4)

(5)

(6)

95.0

98.0

A-2

DIX A )

0.02

A-3

0.1

A-4

To pass
test

0.05

A-5

0.002

0.001

A-6

0.001

A-7

0.001

0.000 5

A-8

0.02

A-9

To pass
test

A-10

IS : 247 - 1987
4. PACKING AND MARKING
4.1 The material of technical and pure grade shall be packed in suitable
air-tight containers, the maierial of analytical reagent grade shall preferably be packed in hard glass bottles closed with air-tight stoppers.
4.2 Each container shall be securely closed after filling and marked with
the name of the manufacturer; grade and mass of the material in the
container; recognized trade-mark, if any; and batch number or month
and year of manufacture.
4.2.1 T h e analytical data of the material for the corresponding
characteristics prescribed in Table 1 shall also be shown on the containers
of the analytical reagent grade of the material.
4.2.2 The product may also be marked with Standard Mark.

4.2.3 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 details of conditions under which the licence for the use of Standard Mark
may be granted to manufactures or producers may be obtained from the Bureau
of Indian Standards.
5. SAMPLING
5.1 The method of preparation of test sample and the criteria of
conformity shall be as prescribed in Appendix B.

APPENDIX
( Clause 3.3 )

METHODS OF TEST FOR SODIUM SULPHITE, ANHYDROUS

A-1. QUALITY OF REAGENTS
A-1.1 Unless specified otherwise, pure chemicals and distilled water ( see
IS : 1070-1977* ) shall be employed in test.
N O T E 'Pure chemicals' shall mean chemicals that do not contain impurities
which affect the results of the analysis.
*Specification for water for general laboratory use ( second revision ).

IS : 247 - 1987
A-2. DETERMINATION OF SODIUM SULPHITE
A-2.0 Outline of t h e M e t h o d A known excess of standard iodine
solution is added to the material. The excess iodine solution is back
titrated with thiosulphate solution. The iodine consumed in oxidizing
the sulphite to sulphate gives a measure of the sulphite.
A-2.1 Reagents
A-2.1.1 Standard Iodine Solution 0.1 N ( see IS : 2316-1968* ).
A-2.1.2 Starch Indicator Triturate 5 g of starch and 0.01 g of mercuric
iodide with 30 ml of water in a mortar. Pour the resulting paste into one
litre of boiling water, boil for three minutes, allow the solution to cool
and decant off the clear liquid.
A-2.1.3 Standard Sodium Thiosulphate Solution 0.1 N, freshly standardized
( see IS : 2316-1968* ).
A-2.2 Procedure Weigh accurately about 0.25 g of the material in
a tared weighing bottle and add it to exactly 50 ml of standard iodine
solution acidified with 2 ml of dilute hydrochloric acid. Allow to stand
for 5 minutes and titrate the excess of iodine with standard sodium
thiosulphate solution using starch solution as indicator, the end point of
the reaction being indicated by the disappearance of blue colour. Carry
out a blank titration without using the material.
A-2.3 Calculation
Sodium sulphite ( Na 2 SO 3 ) content,
percent by mass
=
where
V 1 = volume in ml of standard sodium thiosulphate solution
used in the blank titration,
V 2 = volume in ml of standard sodium thiosulphate solution
used with the material,
N = normality of standard sodium thiosulphate solution, and
M = mass in g of the material taken for the test.
A-3. DETERMINATION OF INSOLUBLE MATTER AND METALS
OTHER THAN ALKALI METALS
A-3.0 Outline of t h e M e t h o d Insoluble matter and metals, other
than alkali metals, are determined by mixing the material with water,
adding to the solution, ammonium oxalate, ammonium phosphate and
ammonium hydroxide, and weighing the residue obtained on the filter.
*Methods of preparation of standard solutions for colorimetric and volumetric
analysis ( first revision ).

IS : 247 - 1987
A-3.1 Reagents
A-3.1.1 Ammonium Oxalate Solution 4 percent.
A-3.1.2 Ammonium Phosphate Solution 10 percent.
A-3.1.3 Dilute Ammonium Hydroxide Solution 1 : 9 ( v/v ).
A-3.1.4 Dilute Ammonium Hydroxide Solution 1 : 39 ( v/v ).
A-3.2 Procedure Dissolve about 10 g of the material, accurately
weighed, in 75 ml of water. Add 5 ml of ammonium oxalate solution,
2 ml of ammonium phosphate solution, and 10 ml of dilute ammonium
hydroxide ( 1 : 9 ) . Allow to stand overnight. Filter off the precipitate
formed through an ashless filter paper and wash with dilute ammonium
hydroxide ( 1 : 39 ). Dry the residue, ignite at about 600C, cool in a
desiccator and weigh.
A-3.3 Calculation
Insoluble matter and metals other than alkali
metals, percent by mass =
where
M 1 = mass in g of the ignited residue, and
M 2 = mass in g of the material taken for the test.
A-4. DETERMINATION OF FREE ALKALI
A-4.0 O u t l i n e of t h e M e t h o d Sodium sulphite is oxidized to sodium
sulphate using hydrogen peroxide and the free alkali is then titrated
against standard acid.
A-4.1 Reagents
A-4.1.1 Hydrogen Peroxide Approximately 30 percent ( m/v ), neutral
to methyl red indicator.
A-4.1.2 Methyl Red Indicator Dissolve 0.03 g of water soluble methyl
red in water and dilute to 100 ml.
A-4.1.3 Standard Hydrochloric Acid 0.1 N.
A-4.2 Procedure Dissolve 5 g of the material, accurately weighed, in
50 ml of water and add 10 ml of hydrogen peroxide. Mix well, add a
drop of methyl red indicator and titrate with standard hydrochloric acid.
Run a blank without using the material.
7

IS : 247 - 1987
A-4.3 Calculation
Free alkali ( as Na 2 O ),
percent by mass
=
where
V 1 = volume in ml of standard hydrochloric acid used in the
test with the material,
V 2 = volume in ml of standard hydrochloric acid used in the
blank,
N = normality of standard hydrochloric acid, and
M = mass in g of the material taken for the test.
A-5. TEST FOR SODIUM THIOSULPHATE
A-5.1 For Pure Grade
A-5.1.0 Outline of the Method Thiosulphate gives with hydrochloric
acid a turbidity due to white precipitate of sulphur which is taken as a
test for thiosulphate.
A-5.1.1 Reagent
A-5.1.1.1 Concentrated hydrochloric acid See IS : 265-1976*.
A-5.1.2 Procedure Dissolve 1 g of the material in 15 ml of water.
Add to it 5 ml of concentrated hydrochloric acid. Allow to stand for 5
minutes.
A-5.1.3 T h e material shall be taken to have passed the test if no
turbidity is produced.
A-5.2 For Analytical Reagent Grade
A-5.2.0 Outline of the Method The opalescence produced by the
material with potassium bromide-mercurjc chloride reagent is compared
with that produced by the standard sodium thiosulphate solution.
A-5.2.1 Apparatus
A-5.2.1.1 Nessler cylinders 50 ml capacity.
A-5.2.2 Reagents
A-5.2.2.1 Potassium bromide-mercuric chloride reagent Dissolve 25 g
each of potassium bromide and mercuric chloride in 900 ml of water at
about 50C. Cool, dilute to one litre and allow to stand overnight. Filter,
if necessary, to obtain a perfectly clear solution.
*Specification for hydrochloric acid ( second revision ).

IS : 247 - 1987
A-5.2.2.2 Standard sodium thiosulphate solution Dilute 50 ml of
exactly 0.1 N sodium thiosulphate ( Na 2 S 2 O 3 .5H 2 O ) solution ( see
A-2.1.3 ) to one litre.
A-5.2.3 Procedure Dissolve 10.0 g of the material in water and dilute
to exactly 100 ml. Slowly pipette out 0.5 ml of the solution into a Nessler
cylinder containing 10 ml of potassium bromide-mercuric chloride
reagent. In a second Nessler cylinder containing 10 ml of potassium
bromide-mercuric chloride reagent, add 0.2 ml of standard sodium
thiosulphate solution. Let both cylinders stand for 10 minutes without
agitation. Then carefully agitate to distribute the opalescence and
examine immediately ( see Note ).
N O T E If the solutions stand for more than 15 minutes, secondary reactions may
take place, vitiating results.

A-5.2.3.1 The limit prescribed in Table 1 shall be taken as not

having been exceeded if the opalescence produced with the material is
not greater than that in the control test.
A-6. TEST FOR HEAVY METALS
A-6.0 Outline of the Method The colour produced by heavy
metals with hydrogen sulphide is compared with that produced with
standard lead solution under identical conditions.
A-6.1 Apparatus
A-6.1.1 Nessler Cylinders 50 ml capacity.
A-6.2 Reagents
A-6.2.1 Concentrated Hydrochloric Acid See IS : 265-1976*.
A-6.2.2 Dilute Ammonium Hydroxide approximately 10 percent ( m/m ).
A-6.2.3 Hydrogen Peroxide approximately 6 percent ( m/v ).
A-6.2.4 Potassium Cyanide Solution Dissolve 10 g of potassium cyanide
in 90 ml of water, add 2 ml of hydrogen peroxide, allow to stand for 24
hours and make up the volume to 100 ml with water.
A-6.2.5 Acetic Acid approximately 33 percent by mass.
A-6.2.6 Concentrated Nitric Acid See IS : 264-1976.
*Specification for hydrochloric acid ( second revision ).
Specification for nitric acid ( second revision ).

IS : 247 - 1987
A-6.2.7 Standard Lead Solution Dissolve 1.60 g of lead nitrate in water,
add 1 ml of concentrated nitric acid and make up the volume to 1 000
ml. Pipette out 10 ml of this solution and dilute again to 1 000 ml with
water. One millilitre of this solution contains 0.01 mg of lead ( as Pb ).
A-6.2.8 Sodium Sulphide Solution approximately 10 percent ( m/v ),
freshly prepared.
A-6.3 Procedure Dissolve 0.5 g of the material of technical grade
and 5.0 g of the material of other grades, in 30 ml of hot water, add 20 ml
of concentrated hydrochloric acid and evaporate the contents nearly
to dryness on a water-bath add 15 ml of hot water and 3 ml of concentrated hydrochloric acid, again evaporate on a water-bath and then heat for
one hour at 1502C. Extract the residue with water, filter and make
up the filtrate to 25 ml. Take 5 ml of the filtrate in a Nessler cylinder.
Make it alkaline to litmus by gradual addition of dilute ammonium
hydroxide and then add 1 ml of potassium cyanide solution. Carry out
a control test in the other Nessler cylinder using 2 ml of standard lead
solution ( 1 ml for analytical reagent grade ) in place of the material
and the same quantities of other reagents. Add 1 ml of acetic acid to
both the solutions and make up the volume to 50 ml with water. Add 2
drops of sodium sulphide solution. Mix thoroughly and compare the
colours produced in the two cylinders.
A-6.3.1 T h e limit prescribed in Table 1 shall be taken as not having
been exceeded if the intensity of colour produced in the test with the
material is not greater than that produced in the control test.
A-7. TEST FOR IRON
A-7.0 T w o methods are prescribed, namely:
a) Colorimetric Method, and
b) Spectrophotometric Method.
A-7.1 C o l o r i m e t r i c M e t h o d
A-7.1.0
potassium
oxidation
solution.
A-7.1.1

Outline of the Method Ferric iron gives a red colour with

thiocyanate. T h e colour produced by the material after
is compared with the colour formed by a standard iron
Apparatus

A-7.1.1.1 Nessler cylinders 50 ml capacity.

A-7.1.2 Reagents
A-7.1.2.1 Concentrated hydrochloric acid See IS : 265-1976*.
*Specification for hydrochloric acid ( second revision ).

10

IS : 247 - 1987
A-7.1.2.2 Ammonium persulphate or potassium persulphate
A-7.1.2.3 Butanolic potassium thiocyanate solution Dissolve 10 g of
potassium thiocyanate in 10 ml of water. Add sufficient n-butanol to
make up the volume to 100 ml and shake vigorously until the solution is
clear.
A-7.1.2.4 Standard iron solution Dissolve 0.702 g of ferrous ammonium
sulphate [ Fe ( N H 4 ) 2 , ( SO 4 ) 2 . 6H 2 O ] in 10 ml of dilute sulphuric acid
( 10 percent v/v ) and dilute with water to 1 000 ml. Pipette out 10 ml
of the solution and dilute with water to make up the volume to 100 ml.
One millilitre of this solution contains 0.01 mg of iron ( as Fe ).
A-7.1.3 Procedure Pipette out 5 ml of the solution prepared in A-6.3
in a Nessler cylinder. Add 1 ml of concentrated hydrochloric acid, about
30 mg of ammonium persulphate or potassium persulphate and 15 ml of
butanolic potassium thiocyanate solution. Shake vigorously for 30
seconds and allow the liquids to separate. Carry out a control test in
another Nessler cylinder using the following volumes of standard iron
solution in place of the material:
a) Two ml for technical grade, and
b) One ml for analytical reagent grade.
A-7.1.3.1 The limit prescribed in Table 1 shall be taken as not
having been exceeded if the intensity of any red colour produced in the
butanolic layer in the test with the material is not greater than that
produced in the control test.
A-7.2 S p e c t r o p h o t o m e t r i c M e t h o d
A-7.2.0 Outline of the Method Iron is reduced to ferrous state by
thioglycollic acid and then treated with excess of ammonium hydroxide.
The intensity of the resultant pink coloured complex is measured in a
spectrophotometer at 535 nm at pH 10.
A-7.2.1 Apparatus
A-7.2.1.1 Any suitable spectrophotometer.
A-7.2.2 Reagents
A-7.2.2.1 Dilute sulphuric acid 10 percent ( v/v ).
A-7.2.2.2 Standard iron solution - Weigh 0.702 g of ferrous ammonium
sulphate [ FeSO 4 ( N H 4 ) 2 SO 4 .6H 2 O ] and dissolve in 10 ml of dilute
sulphuric acid. Dilute with water to make up the volume to 1 000 ml.
Transfer 10 ml of this solution and again dilute with water to make up
the volume to 100 ml. One ml of this solution is equivalent to 0.01 mg
of iron ( as Fe ).
11

IS : 247 - 1987
A-7.2.2.3 Concentrated hydrochloric acid See IS : 265-1976*.
A-7.2.2.4 Dilute ammonium hydroxide approximately 6 N.
A-7.2.2.5 Thioglycollie acid AR 10 percent (v/v).
( SHCH2COOH )
A-7.3 Procedure Weigh about 10 g of the sample, dissolve in about
75 ml of water. Add 5 ml of concentrated hydrochloric acid and boil
for two minutes. Cool to 15C and add 10 ml of 10 percent thioglycollic
acid solution. Add dilute ammonium hydroxide solution drop by drop
till pale pink colour appears keeping the temperature of the solution
below 15C. Add one millilitre more of dilute ammonium hydroxide
solution to bring the pH to about 10. Dilute to 100 ml in a standard
volumetric flask. Read the intensity of the colour in a spectrophotometer
using 535 nm wavelength. Note down the reading. Run a blank on all
the reagents following the above procedure. Subtract this reading from
the reading obtained with the sample. Let this be A.
A-7.3.1 Prepare a series of standard iron solution by taking 2, 5, 7, 10,
15 and 20 of standard iron solution. Subject them to above procedure
and note down the readings. Plot a standard curve for readings obtained
against concentration of iron ( as Fe ).
A-7.4 Calculation
Iron ( as Fe ), percent by mass =
where
A = mg of Fe from the calibration curve, and
M = mass in g of prepared sample taken for test.
A-8. TEST FOR ARSENIC
A-8.0 O u t l i n e of t h e M e t h o d The stain produced by arsenic on a
mercuric bromide paper is compared with stains produced by standard
arsenic solution.
A-8.1 Reagent
A-8.1.1 Concentrated Sulphuric Acid See IS : 266-1977.
A-8.2 Procedure
A-8.2.1 Preparation of solution Dissolve in 50 ml of water 1.00 g of
the material of pure grade and 2.00 g of the material of analytical
reagent grade. Add 5 ml of concentrated sulphuric acid and evaporate
to about 15 ml.
*Specification for hydrochloric acid ( second revision ).
Specification for sulphuric acid ( second revision ).

12

IS : 247 - 1987
A-8.2.2 Carry out the test for arsenic as prescribed in IS : 2088-1983*
using 0 01 mg of arsenic trioxide (As 2 O 3 ) for preparing the standard
stain.
A-8.2.3 The limit prescribed in Table 1 shall be taken as not having
been exceeded if the length of the stain as well as intensity of its colour
produced in the test with material are not greater than those produced
in the control test.
A 9. TEST FOR CHLORIDES
A-9.0 Outline of t h e M e t h o d The opalescence or turbidity produced
by the material with silver nitrate is compared with that produced by
standard sodium chloride solution under identical conditions of test.
A-9.1 Apparatus
A-9.1.1 Nessler Cylinder 50 ml capacity.
A-9.2 Reagents
A-9.2.1 Hydrogen Peroxide 30 percent ( m/v ).
A-9.2.2 Concentrated Nitric Acid See IS : 264-1976.
A-9.2.3 Silver Nitrate Solution 2 percent.
A-9.2.4 Standard Chloride Solution Dissolve 0.164 7 g of sodium
chloride, previously dried at 105 5C, in water and make up the volume
to 1 000 ml. Pipette out 10 ml of this solution and dilute again to 100 ml.
One millilitre of this solution is equivalent to 0.01 mg of chloride
( as Cl ).
A-9.3 Procedure Dissolve 1.00 g of the material in 10 ml of water.
Make up the volume to 100 ml. Transfer 10 ml of the solution to a Nessler
cylinder, add 2 ml of hydrogen peroxide and allow to stand for 30
minutes. Add 2 ml of concentrated nitric acid and 1 ml of silver nitrate
solution. Carry out a control test using 2 ml of standard chloride solution
in place of the material. Compare the opalescence or turbidity produced
in the two tubes five minutes after the addition of silver nitrate solution.
A-9.3.1 The limit prescribed in Table 1 shall be taken as not having
been exceeded if the opalescence or turbidity produced in the test with
the material is not greater than that produced in the control test.
A-10. TEST FOR FREE ACID
A-10.0 Outline of t h e M e t h o d The development of pink colour on
adding phenolphthalein to a solution of the material is taken to indicate
absence of free acidity.
*Methods for determination of arsenic ( second revision ).
Specification for nitric acid ( second revision ).

13

IS : 247 - 1987
A-10.1 Reagent
A-10.1.1 Phenolphthalein Indicator Dissolve 0.1 g of phenolphthalein in
60 ml of rectified spirit ( see IS : 323-1959* ) and dilute with water to
100 ml.
A-10.2 Procedure Dissolve 1.00 g of the material in 15 ml of water
and add two drops of phenolphthalein indicator.
A-10.2.1 The material shall be taken to have passed the test if a pink
colour is produced on the addition of phenolphthalein.

APPENDIX
( Clause 5.1 )

SAMPLING A N D CRITERIA FOR CONFORMITY

B-1. GENERAL REQUIREMENTS FOR SAMPLING
B-1.0 In drawing, preparing, storing and handling test samples, the
following precautions shall be observed.
B-1.1 Samples shall not be taken at a place exposed to weather.
B-1.2 Precautions shall be taken to protect the samples, the material
being sampled, the sampling instrument and the containers for samples
from adventitious contamination.
B-1.3 To draw a representative sample, the contents of each container
selected for sampling shall be mixed thoroughly by suitable means.
B-1.4 The samples shall be placed in suitable, clean, dry and air-tight
opaque glass or plastic containers.
B-1.5 T h e sample containers shall be of such a size that they are almost
completely filled by the sample.
B-1.6 Each sample container shall be sealed air-tight after filling and
marked with full details of sampling, the date of sampling and the year
of manufacture.
B-1.7 Samples shall be stored in such a manner that the temperature
of the material does not vary unduly from the normal temperature.
B-2. SCALE OF SAMPLING
B-2.1 Lot All the containers in a single consignment of the material
drawn from a single batch of manufacture shall constitute a lot. If a
*Specification for rectified spirit ( revised ).

14

IS : 247 - 1987
consignment is declared to consist of different batches, the batches shall
be marked separately and the group of containers in each batch shall
constitute separate lots.
B-2.2 From each lot, five containers shall be selected ( B-2.2.1 ) for
drawing samples for test. In case the lot contains less than five
containers, each container shall be tested.
B-2.2.1 Arrange the containers in a lot in a systematic way and
starting from any container, count them as 1, 2, 3
and so on. Every
rth container thus counted shall be separated for drawing for test, where

NOTE In case the value of r comes out to be a fractional number, it shall be

taken as equal to the integral part of that value.

B-3. PREPARATION OF TEST SAMPLES

B-3.1 D r a w i n g of Samples Draw a representative sample from each
container selected.
B-3.1.1 Mix portions of the material drawn from the same container
to prepare the test sample representing the container. The quantity of
material to be darwn from each container shall be sufficient to conduct
all the tests given in 3.3 and shall be not less than 200 g.
B-3.1.2 The samples shall be stored in dry glass bottles or other
suitable containers, sealed air-tight and labelled with all the particulars
of sampling given in B-1.6.
B-3.1.3 Five test samples, representing the five containers selected as
in B-2.2, shall constitute a set of test samples.
B 4. NUMBER OF TESTS
B-4.1 For Technical Grade Tests for the determination of sodium
sulphite shall be conducted on each of the five test samples ( see B-3.1.3 ).
Tests for all other characteristics prescribed in 3 and Table 1 shall be
conducted on a composite test sample, prepared by mixing equal
quantities of material from each of the five test samples.
B-4.2 For Pure Grade Tests for the determination of sodium sulphite,
heavy metals and arsenic shall be conducted on each of the five test
samples ( see B-3.1.3 ). Tests for all other characteristics prescribed in
3 and Table 1 shall be conducted on the composite sample ( see B-4.1 ).
B-4.3 For Analytical Reagent Grade Tests for the determination of
sodium sulphite and free alkali shall be conducted on each of the five test
samples ( see B-3.1.3 ). Tests for all other characteristics prescribed in 3
and Table 1 shall be conducted on the composite sample ( B-4.1 ).
15

IS : 247 - 1987
B-5. CRITERIA FOR CONFORMITY
B-5.1 Teats Carried Out on Five T e s t S a m p l e s
B-5.1.1 Sodium Sulphite From the test results for sodium sulphite, the
mean ( ) and range ( R ) of test results shall be calculated ( range being
denned as the difference between the maximum and the minimum
values of test results ). The lot shall be considered to have passed if the
value of the expression ( 0'6 R ) is equal to or greater than the respective limit prescribed in Table 1.
B-5.1.2 Free Alkali From the test results for free alkali, the mean ( )
and range ( R ) of test results shall be calculated. The lot shall be considered to have passed if the value of the expression ( -f-0'6 R ) is equal
to or less than 0 1 .
B-5.1.3 Heavy Metals, Iron and Arsenic The lot shall be considered to
have passed for the characteristics tested ( see B-4.2 and B-4.3 ) if each
test sample passes the corresponding test prescribed.
B-5.2 T e s t Carried Out on C o m p o s i t e Test Sample The lot
shall be considered to have passed in respect of the characteristics tested
on the composite test sample ( see B-4.1 to B-4.4 ) if the composite test
sample satisfies the corresponding tests prescribed.
B-5.3 The lot shall be considered as conforming to the specification if it
satisfies all the criteria given in B-5.1 and B-5.2.

16

IS : 247 - 1987
( Continued from page 2 )
Members
S H R I R. R. R A Y

Representing
Waldies Ltd, Calcutta

S H R I S. K. BARAT ( Alternate )

DR H. C. S H A H

3 K Chemical Co, Thane

SHRIMATI K. H . S H A H ( Alternate )

S H R I S. R. SINGH

Development Commissioner, Small Scale Industries,

New Delhi

S H R I J . C. PASRIJA ( Alternate )

S H R I S. S. SINGHANIA

Forum of Small Scale Entreprenuers, Calcutta

S H R I B. L. KANODIA ( Alternate )

DR J. K. S I N H A
S H R I V. B. SONI

S H R I D . G H O S H ( Alternate )

DR M. S. V A I D Y A

Central Mining Research Station ( CSIR ), Dbanbad

Electrolytic Manganese Co ( Division of Union
Carbide India Ltd ), Thane

Dharamsi Morarji Chemical Co Ltd, Bombay

S H R I R . S. V Y A S ( Alternate )

17

M G I P F 2 0 9 Deptt. o f B I S / 2 0 0 7 9 - 7 - 2 0 0 7 1 0 0 B o o k s

BUREAU OF INDIAN STANDARDS

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