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IS 253 (1985): edible common salt [FAD 8: Food Additives]

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IS : 253 - 1985

Indian Standard
SPECIFICATION FOR
EDIBLE COMMON SALT
(

Third Revision)

Acids, Alkalis and Halides Sectional

Committee,

CDC 56

Refiresen t ing

Chairman
PROF M. M. TAQUI KHA~V

Central
Salt
and Marine Chemicals
Institute ( CSIR ), Bhavnagar

Research

Members
DR G. D. BHAT ( Alt#matc to
Prof M. M. Taqui Khan )
SHRI B. K. ANAND
SHRI R. C. JAIN ( Alternate )

Punjab National
Chandigarh

Fertilizers

and

Chemicals

Ltd,

National Test House, Calcutta

SHAI T. K. DUTTA ( Alternate )
Directorate
General of Technical
Development,
SHRI R. C. BRATTACIEARYA
New Delhi
Bengal
Chemicals
and
Pharmaceuticals
Ltd,
SHRI R. N. DAS
Calcutta
SHRI P. N. HALDAR ( Aknatc
j
Atul Products Ltd, Atul
SHRI M. V. DESAI

DR J. M. TUREL ( Alfernatd )
Kothari Industrial Corporation Ltd, Madras
SHRI B. L. GUPTA
E. I. D-Parry ( India ) Ltd, Madras
DR H. V. R. IEN~AR
DR V. C. NAIR ( Ahernatc)
Saurashtra Chemicals, Porbandar
SHRI N. V. KAMBLE
SHRI L. K. MALAVIYA ( Alternate )
Directorate General of Supplies and Disposals, New
SRRI V. B. KHANNA
Delhi
SHRI N. K. KANSAL ( Akernaie )
Indian Paper Mills Association, Calcutta
SHRI MANIIZOHANSINGH
SHRI N. K. GUPTA ( Ak?rnate )
Indian Dyestuff lndustries Ltd, Bombay
DR B. S. NACAR
SHRI N. R. FADNIS ( Alternate)
Ministrv of Defence ( DGI )
Da V. N. Nraain
SHRI K. B. DUTTA ( Alternate )

Deepak Nitrite Ltd, Vadodara

Dn ANIL PANDIT
SHRI J. T. VORA ( Alternate )
SHRI M. L. BEAMBANI

( Continued on jag8 2
@ Copyright 1985
INDIAN

STANDARDS

INSTITUTION

This publication is protected under the Indian Copyright Act ( XIV

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 : 253 - 1985
( Continurdfrom page 1 )
ReprcJcnting

Members

Gujarat State Fertilizers Co Ltd, Vadodara

SRRI M. D. PATEL
SHRI R.N. CHOKSHI( Alternate)
Shriram Foods & Fertiliser Industries, New Delhi
SBEI G. C. D~JTTA ROY
SRRI S. K. NANDA ( Alternate )
Gujarat Alkalis & Chemicals Ltd, Vadodara
SJIRI N. K. SACHAR
SHRI J. B. SHARXA ( Alternate )
SRRI V. S. SAXENA
Ballarpur Industries Ltd, New Delhi
SRRI J. S. TALWAR ( Alternate )
.Indian
Soap & Toiletries
Makers Association,
DR N. SEN
Bombay
Tata Chemicals Ltd, Bombay
DR N. N. &KARMA
SHRI K. H. PAREKR ( Alternate )
SHRI S. K. SUBBAROYAN
Hindustan Lever Ltd, Bombay
DR A. N. BHAT ( Alternate )
SERIP.
SUBRAMANIAN
Salt Commissioner, Jaipur
SHRI B. REVANNA ( Alternate )
Dharamsi Morarji Chemical Co Ltd, Bombay
DR M. S. VAIDYA
Standard Alkali ( Chemicals Division ), Bombay
DR A. S. VA~EWANATHAN
SHRI T. P. VENKATRAMAN ( Alternate )
Hindustan Organic Chemicals Ltd, Rasayani
SHRI H. K. VENKATARAMAIAH
Projects and Development India Ltd, Sindri
DR K. M. VE~MA
Director General, ISK ( &xx-o@cioMembur )
SHRI SATISH CHANDER,
Director ( Chem )
Secretary
SERI M. BAKSHI GUPTA
Deputy Director ( Chem ), IS1

Common

Salts

& Marine

Chemicals

Subcommittee,

CDC 56 : 4

Conuener
Tata Chemicals Ltd, Bombay
DR N. N. SHARMA
SHRI K. H. PAREKI~ ( Alternate to
Dr N. N. Sharma )
The Mettur Chemical & Industrial Corporation
SHRI T. N. BALAKRISHNAN
Ltd, Mettur Dam
Central Committee for Food Standards, Directorate
SIXRI D. S. CHADKA
General of Health Services, New Delhi
SXT DEBI MUEHERJEE ( Alternate )
Atul Products Ltd, Atul
SEIRI M V. DESAI
DR J. M. TU~ZEL ( Alternate )
Central Institute of Fisheries Technology, Cochin
DR K. GWARUMAR
Saurashtra Chemicals, Porbandar
SHRI N. V. KAMBLE
Srrnr L. K. MALAVIYA ( Alternate )
Directorate
General
of Technical
Development,
SHRI J. S. M~TIIAXU
New Delhi
SHXI R. C. BHRTTACHARYA ( Alternate )
( Continued on page 28 )

Indian Standard
SPECIFICATION FOR
EDIBLE COMMON SALT

( Third Revision)
0.

FdREWORD

0.1 This Indian

Standard
( Third Revision ) was adopted by the Indian
Standards
Institution
on 29 August
1985, after the draft finalized by
the Acids Alkalis and Halides Sectional Committee
had been approved
by the Chemical
Division Council.
0.2 A series of Indian
Standards
have been published
to cover the
requirements
of common
salt for various uses.
In the second revision,
IS : 1845-1961 and IS : 2035-1961?, had been amalgamated
with this
standard
because of their similar uses. The other standards
on common
salts published
so far are as follow:
IS : 593-1978 Specification
( second revision )

for

salt

for

hide-curing

IS : 594-1981

Specification

for common

salt

IS : 797-1982 Specification
( second revision )

for common

salt for

IS : 920-1,970 Specification
consumption
IS : 7224-1973 Specification

for common

salt cattle

for

( wet salting

fish-curing

( second

revision )

for iodized

0.3 In this revision, new requirement

methods
of test has been specified
evaporated
) dairy and salt ( vacuum

chemical
licks

industries
for animal

salt

of anicaking
additives
with their
for edible common salt ( vacuum
evaporated
).

0.4 For the purpose of deciding

whether
a particular
requirement
of
this standard
is complied
with, the final value, observed or calculated,
expressing the results 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 values shall be the same as that of the specified values
in this standard.
__-.
*Specification for common salt for butter and cheese industry.
jSpecification for free-flowing table salt.
SRules for rounding off numerical values ( rcoised).

IS : 253 - 1985
I. SCOPE
1.1 This standard prescribes the requirements and methods of sampling
and test for edible common sah, free-flowing table salt and common
salt for butter and cheese industry ( dairy salt ).
2. REQUIREMENTS
2.1 Common

Salt

2.1.1 Description - The material

pale pink or light grey in colour.

shall

be crystalline

solid, white

or

6-O
2.1.2 Moisture - The material shall contain not more than
percent by mass of moisture, on as-received basis, when tested according
to the method prescribed in A-2.
2.1.3 In order to reduce the tendency to cake, vacuum evaporated salt
may contain not more than 15 ppm of potassium ferrocyanide
or
sodium ferrocyanide expressed as KhFe ( CN )s. Compliance with this
limit shall be tested by the method described in A-3.
Common salt
produced by solar evaporation may not contain anticaking agent.
2.1.4 The material, dried in accordance
with the method prescribed
in A-2, shall also comply with the requirements given in Table 1, when
tested according to the methods prescribed in Appendix A.
2.2 Table

Salt

shall be white, crystahine solid

2.2.1 Description - The
material
coated suitably with free-flowing agents, such as light magnesium
carbonate, calcium carbonate, tricalcium phosphate and calcium silicate
and aluminium silicate so as to retard moisture absorption, caking and
to impart free-flowing property to the salt.
2.2.2 Particle Size - 99 percent by mass of the material shall pass
through l-00-mm IS Sieve ( see IS : 460 ) and not more than 10 percent
by mass of the material shall pass through 212-micron IS Sieve ( see
IS : 460*).
2.2.3 Moisture - The material shall contain not more than 0.5 percent
by mass of moisture, on as-received basis, when tested according to the
method prescribed in A-2.
2.2.4 The material, dried in accordance with the method prescribed
in A-2, shall also comply with the requirements
presrribed in Table 1,
when tested according to the methods prescribed in Appendix A.
*Specification for test sieves.
4

1s : 253 - 1985
TABLE

( Clauscs2.1.4,

REQUIREMENTS
2.2.4, 2.3.5,

A-11.3.1,

FOR

CHARACTERISTIC:

9
ii)

Water insoluble matter,

by mass, Maw
Chloride
percent

iii)

Acid insoluble
matter,
by mass, Max

iv)

Matter soluble in water,

than sodium chloride,
by mass, Max

v)
vi)
vii)

(5)

(6)

2.2

0.03

A-4

1.5

3.0

( as
Ca ),
water
percent by mass, Max

METHOD cm
TEST ( REF
TO CL No.
IN APPENDIX A )

(4)

97.0

other
percent

DAIRY

1.0
96.0

percent

A-14.3.1 andB-5.2

(3)
percent

content
( as NaCl),
by mass, Min

SALT

COMMON

TAl3I.E

COimON

(2)

(1)

EDIBLE

A-12.3.3,A-13.2.4.3,

99%

A-5

A-6
A-7

O-10

0.01

A-8

Magnesium
( as Mg ), water
soluble, percent by mass, &fax

010

0.01

A-8

Suh&te;k;s

0.50

0.30

A-9

Calcium
soluble,

SO& ), percent by

Alkalinity ( as Na, CO, ),

cent by mass, Max

per-

0.20

0.10

A-10

Lead
( as Pb ),
million, Max

per

2.0

2.0

A-11

Iron ( as Fe ), parts per million,

50.0

10.0

A-12

xi)

Arsenic
( as As ),
million, Max

parts

per

1.0

1-o

A-13

xii)

Copper ( as Cu ),
million, Max

parts

per

2.0

A-14

viii)
ix)
x)

parts

Max

2.3 Dairy Salt

2.3.1 Description - The material
and free from any visible impurities.

shall

be

crystalline

2.3.2 Particle Size - 99 percent by mass of the material

completely
through 850-micron
IS Sieve ( see IS : 460*).

white
shall

rolid
pass

2.3.3 Moisture - The material shall contain not more than 0.5 percent
by mass of moisture, on as-received
basis, wheh tested according
to the
method prescribed
in A-2.
-~
*Specification

for test sieves.

Is:253 -1985
2.3.4In order to reduce the tendency to cake, the material may
contain not more than 15 ppm of suitable anticaking additive such as
potassium or sodium ferrocyanide or ammonia ferric citrate. Compliance
with this limit shall be tested by the method described in A-3.
2.3.5 The material, dried in accordance with the method prescribed
in A-2, shall also comply with the requirements given in Table 1, when
tested according to the methods prescribed in Appendix A.
3. PACKING

AND MARKING

3.1 Packing
3.1.1 EdibIe common salt shall be supplied in bulk
agreed to between the purchaser and the supplier.

or packages

as

3.1.2 For the free-flowing table salt the size and material of construction of the- containers shall be subject to agreement between the purchaser and the supplier.
3.1.3 Common salt for butter and cheese industry ( Dairy salt ) shall be
packed in a moistureproof
packing, such as polyethylene or similar
suitable material, as agreed to between the purchaser and the supplier.
3.2 Marking
- The package shall be securely closed and marked with
the manufacturers name; mass of the material in the package; type of
the material; recognized trade-mark,
if any; batch number; and the
date of packing.
3.2.1
Mark.

The packages may aIso be marked

with

the ISI

Certification

NOTE - The use of the ISI Certification Mark is governed by the provisions of the
Indian Standards Institution ( Certification Marks ) Act and the Rules and Regulations made thereunder.
The IS1 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 IS1 and operated by the producer.
IS1
marked products are also continuously checked by IS1 for conformity to that
standard as a further safeguard.
Details of conditions under which a licence for the
use of the ISI Certification
Mark may be granted to manufacturers or processors,
mav be obtained from the Indian Standards Institution.

4. SAMPLING
4.1 Representative

samples of the material shall be drawn and their

criteria for conformity shall be determined in accordance
with the
methods prescribed in Appendix B.
6

IS : 253 - 1985

APPENDIX
A
QCZauses2.1.4, 2.2.4 and 2.3.5 )
ANALYSIS
A-l.

QUALITY

+? EDIBLE

COMMON

SALT

OF REAGENTS

A-l.1 Unless specified otherwise, pure chemicals

( see IS : 1070-1977 ) shall be used in tests.
NOTE - Pure chemicals shall mean
which affect the results of analysis.

A-2. DETERMINATION

chemicals

OF MOISTURE

that

and
do

distilled

water

not contain impurities

CONTENT

A-2.1 Procedure
A-2.1.1 Grind rapidly the sample material as received ( say 100 g ),
where relevant, as in the case of common salt, in an agate mortar
approximately to a size of 2.8 mm IS Sieve, but do not actually sieve.
The material which shall be in the form of powder shall be kept in an
air-tight container.
A-2.L2 Weigh accurately about 20 g qf the material in the weighing
bottle ( about 30 ml capacity ), preferably wide mouth squat type, preDry in an oven at 140 to 150C for at least
viously dried and weighed.
4 hours.
Cool in a desiccator and weigh.
Repeat drying, cooling and
weighing until constant mass is obtained.
A-2.2

Calculation
Moisture,

percent by mass = 100

Ml

WA!

MI

where
Ml = initial mass in g of the material taken for the test, and
M2 = final mass in g of the material taken for test.
A-3. DETERMINATION

OF FEBROCYANIDE

A-3.0 General - This test is designed for 15 ppm of ferrocyanide

f expresSed as K4Fe ( CN )s 1, although this amount of ferrocyanide
Ammonium ferric
is unlikely to be used as an anticaking additive.
citrate is, however, used up to this level, though its use will probably
become less wide-spread; if present, its Iimit can be determined by the
method described in A-12, but the limit so determined will include iron
from other sources.
*S+cification far water for general laboratory use ( second revision ).
7

- 1985

IS:253
A-3.1

Reagents

A-3.1.1

Dilute Sulphuric Acid -

about 0*5N solution.

ferrous
A-3.1.2
Ferrous/Ferric Solution - Dissolve 20 g of ammonium
sulphate
( NH4 )$S04.FeS04.6HeO,
and 2.5 g of ammonium
ferric
sulphate ( NH4 )$S04,Fez(
SOd)a.24HzO,
in water to which 10 ml of the
dilute sulphuric
acid has been added.
Dilute to 100 ml with water,
filter and store in a dark bottle.
A-3.1.3
Phosphate Solution - Dissolve 70 g of potassium
dihydrogen
phosphate
in water,
add 50 ml of the dilute sulphuric acid and make
up to 1 000 ml with water.
A-3.1.4
Sodium Chloride and allow to cool.
A-3.1.5

Before

use,

ignite

at 500C

for

hours,

Standard Potassium Ferrocyanide Solutions

2.294 g of potassium
A-3.1.5.1
Ferrocyanide stock solution - Dissolve
ferrocyanide
trihydrate,
KdFe( CN )e. 3He0, in water, add 5 ml of dilute
potassium hydroxide
solution ( about O.lN ) and dilute to 1 000 ml with
freshly boiled and cooled water.
Store in the dark.
A-3.1.5.2
Ferrocyanide working solution - Take 25 ml of the ferroadd 5 ml of potassium
hydroxide
solution
cyanide
stock
solution,
( about 0*lN ) and dilute to 1 000 ml with freshly boiled and cooled
water.
1 ml = 0.05 mg KdFe(

CN )6

A-3.2 Procedure
- Dissolve 10 f 0.1 g of the sample in about 40 ml
of water in a Nessler cylinder graduated
at 100 ml.
Add 10 ml of the
dilute sulphuric acid and 5 ml of the ferrous/ferric
solution, mixing
well
after each addition.
Allow to stand for about 2 minutes, then add 35 ml
of the phosphate solution, mix, dilute to the 100 ml mark and mix again.
The colour
shall not be greater
than the 15 ppm KaFe ( CN )6
standard
which is prepared
similarly using 10 g of the sodium chloride
reagent
to which has been added
3 ml of the ferrocyanide
working
solution in place of the 10 g of sample.
A-4.

DETERMINATION

OF MATTER

INSOLUBLE

IN WATER

A-4.1 Preparation
of the Sample
for Chemical
Tests - Spread
80 to 100 g of the sample ( see A-2.1.1 ) in a petri dish and dry by the
method
given in A-2.1.2.
The dried material shall be called the dried
sample and shall be used in the tests where so indicated.

IS:253-1985

A-4.2 Procedure - Accurately weigh about 20 g of the dried sample,

dissolve it in 200 ml of water in a beaker and heat to boiling and cool.
Filter the solution through a weighed Gooch or sintered glass crucible
( G NO. 4 ) and wash the residue till it is free from soluble salts. Collect
the filtrate and washings in a one-litre graduated flask and dilute to
mark.
Preserve the solution so obtained for subsequent tests. Dry the
crucible along with the insoluble residue to constant mass.
A-4.3

Calculation

Matter

insoluble in water = 100 g

2

where

Ml = mass in g of the residue, and

Ms = mass in g of dried sample taken for the test.
A-4.3.1 Insoluble matter in water, percent by mass, is calculated
on
moisture-free basis. However, in the case of table salt, insoluble matter
in water, percent by mass, also includes the free-flowing agents added
to the salt.
A-4.3.2 For dairy salt, repeat the above procedure with 50 g instead
of 20 g as per A-4.2, if it is difficult to obtain a difference in mass of
6 mg.
A-5. DETRRMINATION

OF TOTAL

CHLORIDES

A-5.1 Reagents
A-5.1.1

Potassium

A-5.1.2

Standard

Chromate Indicator
Silver Jfitrate

Solution -

Solution -

5 percent.

0.1 N.

Procedure
- Transfer 10 ml of the solution reserved in A-4.2
into a conical flask and add 1 ml of potassium chromate indicator
Titrate against standard silver nitrate solution till the reddish
solution.
brown tinge persits after brisk shaking. Carry out a blank determination.
A-5.2

A-5.3

Calculation

A-5.3.1

For Common Salt

Total chloride ( as Cl ), percent

by mass ( on dry basis )

VN

= 354.6 M

where
V = volume in ml of standard silver nitrate solution used in
the titration with the material, corrected to blank;
9

IS : 253 - 1985
N = normality

of standard

silver nitrate solution; and

M = mass in g of the dried sample in 1 000 ml of the solution

taken

for the test.

A-5.3.1.1
Residual
chloride is the chloride
obtained
by deducting
the chloride
attributed
to the other
chlorides,
such as magnesium
chloride,
potassium
chloride
( see A-15 ) and calcium chloride as described in A-7 from the total chloride determined
in A-5.3.
Sodium chloride ( as NaCl
percent by mass
A-5.3.2

)
= Residual

chloride

( as Cl ) x 1.648

For Table Salt and Dairy Salt

Sodium

chloride

( as NaCl

), percent

by mass -

584.5

VN
M

where
V = volume
. titration
N = normality

of standard

silver nitrate

mass in g of the dried sample

taken for the test.

M=

A-6.

in ml of standard
silver
with the material, corr&ted

DETERMINATION

A-6.0

Carry

A-6.1

Re,agents

A-6.1.1

Dilute Hydrchloric Acid -

A-6.1.2

ConcentratedHydrochloric

solution;

in

the

and

in 1 000 ml of the solution

OF ACID INSOLUBLE

out this test for free-flowing

nitrate, used
to blank;

MATTER

table salt only.

1 : 1 ( V/U) and 1 : 20 ( v/v ).

Acid -

conforming

to IS : 265-1976*.

the residue
obtained
in A-4.2
into a
A-6.2 Procedure
- Transfer
beaker.
Alternatively,
transfer
the sintered
crucible
itself with the
residue
to 100 ml beaker,
and add 15 to 20 ml of water and 25 ml of
concentrated
hydrochloric
acid so that the sinter base is immersed in
the acid.
Heat to boiling for 10 to 15 minutes so that practically
all the
residue and drier have decomposed
with the acid.
Remove the sintered
crucible from the beaker ( if it is transferred
to the beaker ) and wash
Evaporate
the extract
and wash solution
the crucible
with water.
together
to dryness
and transfer
the solid residue with 25 ml of dilute
hydrochloric
acid ( 1 : 1 ).
*Specification for hydrochloric acid ( secondrevision).
10

IS:253-1985
*A-6.2.1 Filter on a filter paper ( Whatman No. 41 or equivalent ),
wash the precipitate first with warm dilute hydrochloric
acid ( 1 : 20 )
Dry the
and then with hot water until washings are free from chloride.
Heat strongly at red heat for one
residue and ignite in a silica crucible.
hour. Cool and weigh.
NOTE - If silicate drier is not used, acid insoluble residue will be very
accurate weighing.
In that case, repeat with 50 g of dried material.

low for

A-6.3 Calculation
Acid insoluble matter, percent by mass = 100

M2

where
Ml = mass in g of the residue, and
Me = mass in g of dried sample taken for the test.
A-7. EXPRESSING
OF MATTER SOLUBLE
THAN SODIUM CHLORIDE

IN WATER

OTHER

A-7.0 Carry out this expression of result for common salts only.
A-7.1 Express the soluble carbonate as calcium carbonate ( marine salt ),
or as sodium carbonate ( Rajasthan salt, in absence of calcium and
magnesium ). If there is excess of calcium over the calcium
carbonate,
combine all the calcium with the sulphate radical and express the result
as percentage
of calcium
sulphate.
If there is excess of the sulphate
over what is required for calcium, combine the excess with magnesium
and express the result as percentage
of magnesium
sulphate.
Calculate
the balance of magnesium
as magnesium
chloride and deduct
the chloAlso, deduct from
ride corresponding
to it from the chloride content.
the chloride content an amount of chloride
corresponding
to potassium
content and express it as percentage
of potassium
chloride.
Calculate
the residual chlorine as percentage
of sodium chloride.
A-7.2 In the above procedure,
if there is excess of sulphate
over the
calcium
and magnesium
sulphate, express it as sodium sulphate, and if
there is excess of calcium over the calcium sulphate express it as calcium
chloride.
This situation
does not arise commonly
in the analysis of
edible common salt.
A-7.3 In the absence of calcium and magnesium,
express
sodium carbonate
and sulphate as sodium sulphate.

carbonate

as

A-7.4 Calculate the matter soluble in water other than sodium chloride
by subtracting
from 100 the sum of sodium chloride content and matter
insoluble
in water.
Matter
soluble in water includes
the water of
hydration
retained at the temperature
drying.
11

IS:253

-1985

DETERMINATION
( WATER SOLUBLE

A-8.

OF
)

CALCIUM

AND

MAGNESIUM

A-8.1 Reagents
A-8.1.1 Standard Calcium Solution -

Weigh l-0 g of calcium carbonate

120C: and dissolve
it in the minimum
quantity
of dilute
acid.
Dilute the solution to one litre in a graduated
flask.
One
rniliilitre
of the
solution
is equivalent
to 0.400 8 mg of calcium
( as (:a j.
delied
a:
hydrochloric

A-8.1.2 Standard EDTA

Sol&on - Dissolve
3.72 g of
disodium
ethylene
diamine
tetra
acetate
dihydrate
in water and dilute in a graduated flask to one litre.
The solution shall be standardized
frequently
against standard
calcium solution following the procedure
given in A-8.2.

A-8.1.3 E&chrome Bhck T Indicator Solution - Dissolve

in 20 ml of rectified spirit conforming
to IS : 323-195V.
shall be prepared
fresh every week.
A-8.1.4

Dilute Sod&m Hydroxide Solution -

@1 g of the dye
This solution

Approximately

10 percent.

0.2 g of murexide
with
A-8.1.5 Mwcxide
Indicator Solution - Grind
10 g of sodium chloride until the mixture is homogeneous.
Thus 0.2 g
of the mixture
is suitable for 100 ~1 of the sample solution.
0.1 g of calcein
A-8.1.6 Calcein Indicator - Grind thorougly
of thymolphthalein
with 10 g of potassium
chIoride.

and PO6 g

A-8.1.7 Ammonium
Dissolve
67.5 g of

Chloride-Ammanivm
Hydroxide
Bu&
So&ion ammonium
chloride
in a mixture of 570 ml of ammonium
hydroxide
( RD. 0.90 ) and 250 ml of water.
Also dissolve
separately
a mixture
of 0*931 g of disodium
ethylene diamine tetra
acetate dihydrate
and 0.616 g of magnesium
sulphate
( MgS04.7H20
)
Mix the two solutions and dilute to one Iirre.
in about 50 m1 of water.
KOTE
Five millilitres of buffer solution added 10 50 ml of distilled water should
not consume
more than a drop of ISDT.4 solution to change to distinct blue with
c&chrome
black T indicator.

A-8.2

Procedure

A-8.2.1 Standardizatiuz

of EDTA Solution - Transfer

2.5 ml of standard
solution
into a conical flask, add 25 ml of water, 10 ml of
ammonium
chloride-ammonium
hydroxide
buffer solution,
5 drops
of
the eriochrome
black T indicator
solution and titrate against the standard
EDTA solution to a pure blue end point.
calcium

'Speci5carion

for

rectified

spirit

( rcoirrd).

12

IS : 253 - 1985
A-8.2.2 Titrate 25 ml of the buffer solution with EDTA solution using
Subtract the buffer correction
for 10 ml
eriochrome
black T indicator.
( usually it will be 0.1 ml ) from the reading obtained in A-8.2.1 and
note the final titre value.
Calculate the calcium equivalent
of 1 ml of
EDTA solution ( say il ),
A-8.2.3
For the determination
of calcium and magnesium in common
salt and dairy salt, use the solution preserved in A-4.2, but for table
salt, use the solution preserved in A-10.2.2.2
and proceed as given below.
A-8.3

Determination

of Calcium

and

Magnesium

A-8.3.1 Pipette out 10 ml of the solution preserved

in A-10.2.2.2
and
dilute to 100 ml with water and proceed for the determination
of calcium
and magnesium
as given in A-8.3.2 and A-8.3.3 and calculate
as given
in A-8.4.
A-8.3.2
Transfer
exactly 100 ml. of the solution
preserved
in A-4.2
into a 250-ml conical flask and 10 ml of ammonium
chloride-ammonium
hydroxide
buffer solution,
5 drops of eriochrome
black T indicator
solution
and titrate against
standard
EDTA
solution till wine red
Note the EDTA
colour
of the solution changes to pure blue end point.
solution used in the titration.
A-8.3.3
Transfer exactly 100 ml of the solution
preserved
in A-4.2
into 250-ml
conical
flask and 5 ml sodium hydroxide
solution and stir
Add 0.2 g murexide
( or 100 mg calcein
mixed
indicator ) and
well.
titrate
against
standard
EDTA
solution
till wine red colour
of the
solution
changes
to pure blue end point with murexide ( or green to
purple with mlxed calcein indicator ). Note the volume of the standard
EDTA solution used in the titration.
A-8.4

Calculation
Calcium ( as Ga ), percent
mass ( on dry basis )

by

Magnesium
( as Mg ), percent
mass ( on dry basis )

A V

=+
by

A ( Vl O.cO6 8 __

v2 )

where

A = calcium

equivalent
in
determined
in A-8.2.1,

mg

VI = volume

in ml of standard

V2 = volume
A-8.3.3

in ml of standard
( for Ca only ), and

EDTA

M = mass in g of the dried sample

13

of

1 ml

of EDTA

solution

EDTA

solution

used in A-8.3.2,

solution

used

in

taken for the test in A-4.2.

IS:253-1985
A-9. DETERMINATION
A-9.1

Gravimetric

A-9.1.1

OF SULPHATE

Method

Reagents

A-9.1.1.1

Dilute Hydrochloric

A-9.1.1.2

Barium

Acid -

Approximately

Chloride Solution -

Approximately

4 N.
10 percent.

A-9.1.2 Procedure - Dissolve about 10 g of dried common salt ( or

aliquot
volume of the prepared solution of A-4.2 representing
10 g ) or
about 20 g of dried table or dairy salt ( A-4.1 ) in about 400 ml of
Collect the
water, filter and wash the residue free from soluble salts.
filtrate and washings.
Add one drop of methyl orange
and 10 ml of
dilute hydrochloric
acid or more till it is pink and then boil.
Add to
the boiling solution,
10 to 12 ml barium
chloride
solution
drop by
drop so that the addition
is in slight excess and continue boiling for
Allow to stand for 4 hours
4 minutes to obtain a granular precipitate.
and filter through
a weighed
sintered
glass crucible
( G No. 4 ) or
Wash the precipitate
till free from chloride and dry
Gooch
crucible.
to constant mass at 105 to 110C.
Alternatively
filter through Whatman
filter paper No. 42 and wash till it is free from chloride.
Ignite and
determine as barium sulphate.
A-9.1.3

Calculation

Sulphate

( as SO* ), percent

by mass -

41.13

n/i,
K

where
.Ml = mass in g of barium
Ma = mass in g of dried
solution
is taken
400 ml ).

A-9.2

Volumetric

A-9.2.1

sulphate,

and

sample taken for test in A-4.2

( if
for common salt, mass of salt in g in

Method

Reagents

A-9.2.1.1
of barium
one litre.

Standard Barium Chloride Solution - O-05 N. Dissolve 6.108 g

chloride dihydrate ( BaCls. 2HaO ) in water and make up to

A-9.2.1.2

Dilute hpdrochloric

acid -

Approximately

1 N.

A-9.2.1.3 Standard EDTA

solution - Weigh
3.72 g of disodium
ethylene diamine
tetra acetate
dihydrate
in water and dilute in a graduated flask to one litre.
The solution shall be standardized
frequently
14

IS : 253-

1985

against standard barium chloride solution ( A-9.2.1.1 ) and follow the

procedure given in A-8.3.
One ml of standard EDTA solution is equal
to 0601 374 g Ba or 0000 96 g of Sod.
A-9.2.1.4

Eriochrome

black T indicator solution -

A-9.2.1.5 Ammonium chloride-ammonium

as in A-8.1.7.
A-9.2.2

hydroxide

Same as in

A-8.1.3.

bu$er solution -

Same

Procedure

A-9.2.2.1
Pipette out 20 ml g of standard barium chloride solution
into a conical flask, add 2 drops of hydrochloric acid and IO ml of
ammonium chloride-ammonium
hydroxide buffer solution.
Dilute it
with water to about 50 ml, add five drops of eriochrome black T indicator solution and titrate against standard EDTA solution to pure blue
end point.
Note the titre value ( say A ).

A-9.2.2.2 Pipette out 100 ml of the solution preserved in A-4.2 and

add two drops of hydrochloric acid and heat to gentle boiling.
To the
hot solution, add with a pipette 20 ml standard barium chloride solution.
Boil gently for about 5 minutes and then cool to room temperature.
The solution will be neutral or slightly acid when tested with a litmus
paper filtration. Add 10 ml of ammonium chloride-ammonium hydroxide
buffer solution and five drops of eriochrome black T indicator solution.
Titrate
against standard EDTA solution to pure blue end point.
Note
the titre value ( say B ).
A-9.2.3 Calculation
Sulphate ( as SO4 ), percent
by mass ( on dry basis ) = 0.96

A+Vl-B
M

where
A = volume in ml of standard EDTA
solution used in
A-9.2.2.1,
VI = volume in ml of standard EDTA solution used in A-8.3.2
( total Ca + Mg ),
B = volume in ml of standard EDTA
solution used in the
titration in A-9.2.2.2, and
M = mass in g of the dried sample taken for the test in A-4.2.
A-10. DETERMINATION

OF ALKALINITY

A-10.1 Reagents
A-10.1.1 Standard Hydrochloric

Acid -

15

0.1 N.

IS : 253 - 1985
A-10.1.2 Methyl Orange Indicator -

Dissolve 0.1 g of methyl

orange

in

100 mI of water.
A-10.2

Procedure

A-10.2.1 Procedure for Common Salt - Pipette out 100 ml of the solution,
preserved in A-4.2 and titrate against standard hydrochloric
acid using
methyl orange as indicator.
A-10.2.2 Procedure for Table Salt and Dairy Salt - Transfer about 20 g
of the prepared sample, accuratly weighed, in a lOO-ml measuring flask
through a funnel.
Wash the funnel in the flask with carbon dioxide-free
Shake the flask well
distilled water and fill it to the mark with water.
till all the salt goes into solution ( undissolved magnesium carbonate will
remain in suspension ).
A-10.2.2.1
Shake it well and filter first 10 to 15 ml of the solution
through Whatman
filter paper No. 1 and discard the filtrate.
Then
filter the remaining solution and titrate 50 ml of the solution so obtained
against standard hydrochloric acid using methyl orange as indicator.
A-10.2.2.2
Preserve the remaining filtered solution for. the
nation of water soluble calcium and magnesium for table salt.
A-10.3

determi-

Calculation

Alkalinity

( as Na2COa ), percent by mass:

For common salt = 5.3 4

For table salt and dairy salt L- 106 $
where
V =

volume in ml of standard
titration, and

hydrochloric

acid used in the

M = mass in g of the prepared sample taken for the test.

A-11.
A-11.1

TEST

Apparatus

A-11.1.1
A-11.2

FOR LEAD

.hessler Cylinders -

50 ml capacity.

Reagents

A-l 1.2.1 Acetic Acid A-11.2.2

Approximately

Diltute Ammonium Hydroxide

16

33 percent ( u/v).
-

Approximately

4 N.
f

IS : 253 - 1985
A-11.2.3 Potassium Cyanide Solution - Dissolve 10 g of potassium cynide
in 90 ml of water, add 2 ml of hydrogen peroxide (20 volume strength),
allow to stand for 24 hours and make up to 100 ml with water.
A-11.2.4 Sodium Sutphidc Solution ( Na$S.9HzO ) in 100 ml of water.

Dissolve 10 g of sodium

sulphide

A-11.2.5 Standard Lead Solution - Dissolve O-160 g of lead nitrate in

5 ml of concentrated
nitric acid ( conforming to IS : 264-1976* ) and
dilute to 100 ml in a graduated flask. Again dilute 10 ml of the solution
to 1 000 ml. One millilitre of the solution finally obtained contains
0.01 mg of lead ( as Pb ).
- Dissolve 5 g of the dried sample ( SIGA-4.1 ) in
A-11.3 Procedure
water in a Nessler cylinder and add 5 ml of acetic acid.
Make the
mixture alkaline with dilute ammonium hydroxide and add 1 ml of
If turbid, filter. Add two drops of sodium
potassium cyanide solution.
sulphide solution and mix well. Carry out a control test in another
Nessler cylinder in exactly the same manner but using 1 ml of standard
Dilute the solution in both
lead solution in place of the dried sample.
Compare the colour produced in the two
the cylinders to 50 ml mark.
cylinders against a white background.
A-11.3.1 The material shall be taken to have not exceeded the limit
specified in Table 1 if the intensity of colour obtained with the material
is not greater than that obtained in the control test.
A-12. TEST
A-12.1

IRON

Apparatus

A-12.1.1
A-12.2

FOR

.h%.ssle~

Cylinders -

50 ml capacity.

Reagents

A-12.2.1 Thioglycollic Acid thioglycollic acid by mass.

A-12.2.2

containing

not less than

Concentrated Ammonium Hydroxide -

Relative

97

percent

of

density 0.90.

Dissolve 2.81 g of ferrous ammonium

A-12.2.3
sulphate [ FeSO4. ( NH4 )~SOQ. 6HzO ] in water, add a few millilitres
of dilute sulphuric acid and dilute to 1 000 ml with water. *
Standard Iron Solution -

10 ml of the standard iron

A-12.2.4 Dilute Standard Iran Solution -Dilute
The solution should be
solution ( A-12.2.3 ) to 1 000 ml with water.
This solution contains O*OOO004 g of iron
prepared freshly as required.
per millilitre ( 1 ml = 0004 mg Fe ).
*Specification

for nitric acid ( second revision ).

,, 17

IS : 253 - 1985
A-12.3 Procedure
A-12.3.1 Procedurefor Dairy Salt - Dissolve exactly 2 g of the dried
sample in 10 ml of water and transfer to a Nessler cylinder.
Dilute to
20 ml with water and add 4 drops of thioglycollic acid followed by 1 ml
of concentrated ammonium hydroxide.
A-12.3.1.1
Carry out a control test is another Nessler cylinder
using 5 ml of dilute standard iron so!ution and the same quantities of
other reagents.
Dilute the solution in both the cylinders to 50 ml and
mix well.
A-12.3.2
prescribed
and add 4
ammonium
cylinder as

Procedurefor Table Salt - Pipette out 20 ml of the solution

in A-4.2 into a Nessler cylinder.
Dilute to 20 ml with water
drops of thioglycollic
acid followed by 1 ml concentrated
hydroxide.
Carry out a control test in another Nessler
given in A-12.3.1.1.

A-12.3.3 The requirement specified in Table 1 shall be taken as not

having been exceeded, if the intensity of colour produced with the
material is not greater than that obtained in the control test ( 10 ppm ).
A-13.

TEST

FOR ARSENIC

A-13.1 Method I ( Gutzeit Method ) - Weigh accurately

100 g of
the material and dissolve in 10 ml of water and carry out the test for
arsenic as prescribed
in IS : 2088-1983+ using 0.001 32 mg of arsenic
trioxide ( As203 ) for preparing the comparison stain.
A-13.2 Method II ( Silver
Absorptiometric
Method

Diethyl
)

Dithiocarbamate

Red Complex

A-13.2.Q Principle - Arsenic reacts with a soIution of silver diethyl

dithiocarbamate,
[ AgS.CS.N ( C&-H, )z ] in pyridine to form a soluble
red complex which has an absorption maximum at 540 nanometre
( nm ). The arsenic shall be in the trivalent state in the sample which
is secured by reducing the arsenate with potassium iodide and stannous
The arsenic is converted into arsine by the
chloride in acide media.
treatment of hydrochloric
acid and zinc and evolved
arsine is
Using any standard
absorbed in the reagent to form a red complex.
photoelectric absorptiometer, absorption measurement is done at 540 nm,
with coloured red complex solution against blank reagent solution
for total transmittance.
From the transmittance
or optical density
obtained with known arsenic content covering the range O-10 pg ( as
O-10 nm As ), standard calibration graph is prepared by plotting the
percent transmittance
or optical density or logarithm
of percent
*Method

for determination

of arsenic ( second

18

revision).

IS : 253 - 1985
transmittance ( log T ) against known concentration.
As it obeys Beers
Law, log T or the optical density are directly proportional to the
concentration
and only a few points are required to establish the graph
for the determination of arsenic under the experimental condition.
A-13.2.1 Apfiaratus - The
evolution
and
as shown in Fig. 1 shall consist of the following.

absorption
-

10 TO

apparatus

12*--

BALL
JOINT

1t

FIG. 1

APPARATUSFOR ARSENICDETERMINATION

A-13.2.1.1

Conical flask -

A-13.2.1.2

Connection tube -

100 ml for the evolution of arsine ( A ).

to trap hydrogen sulphide ( B ).
19

IS : 253 - 1985
A-13.2.1.3 Absorption tub C
A-13.2.1.4
Spring clip - to secure the joint connecting B to C. ( It
may be either ground cone-socket joint or ball joint with hooks. )
A-13.2.2

Spect?ophotometer or Photoelectric Absorptiometer

A-13.2.3

Reagents

A-13.2.3.1
dark place.

Potassium iodide -

150 g per Iitre

A-13.2.3.2

Stannous chloride solution

A-13.2.3.3

zinc shots -

solution.

Store

in a

arsenic-free.

A-13.2.3.4
Silver diethyl dithiocarbamate - 5 g/l solution in pyridine.
Dissolve 1 g of silver diethyl dithiocarbamate
( SDDC ) in pyridine
( relative density O-980 approx ) and dilute to 200 ml with pyridine.
Store in a well stoppered glass bottle protected from light.
This solution
is stable for 2 months ( see Note ).
Ifsuitable reagent is not available it may
NOTE
diethyl dithiocarbamate by the method given below:
a)

be prepared

from sodium

Purification of sodium diethyl dithiocarbamats - Dissolve

10 g sodium
diethy
dithiocarbamate
[ ( C&H, )s N.CSNa.3HsO
] in 35 ml of ethanol ( 95 percent
v/v ) and filter. Add to this solution with continual stirring, 100 ml of diethyl
ether.
Filter with suction, wash the precipitate with ether and dry in air.

b) Preparation of the reagent- Dissolve 225 g sodium diethyl dithiocarbamate in

Dissolve l-7 g of silver nitrate in 100 ml water.
Mix the two
100 ml water.
Keep the mixture at a temperature
solutions slowly with continuous agitation.
below 10C. Filter with the aid of suction pump and dry the product in
Preserve in a cool place protected from light.
vacuum at room temperature.
The,solution is unsatisfactory
using 5 ml of this solution.

if the optical density is less than O-03 pg of arsenic

A-13.2.4 Procedure
A-13.2.4.1
Transfer 10 ml of the standard arsenic solution containing
10 pg of arsenic and 10 ml of the concentrated hydrochIoric acid into
a loo-ml conical flask A and dilute it approximately
to 40 ml with
Add 2 ml of the potassium iodide solution ( A-13.2.3.1 ) and
water.
0.5 ml of the stannous chloride solution ( A-13.2.3.2 ). Mix and allow
to stand for 15 minutes.
Place some dry lead acetate paper in the
lower portion of the connection tube B and. glass wool ( or cotton )
Assemble the
moistened with lead acetate solution in its upper portion.
apparatus.
Transfer
5.0 ml of silver diethyl dithiocarbamate
solution
to the absorption tube.
After 15 minute standing period, introduce 5 g
of the zinc shots ( A-13.2.3.3 ) into the conical flask A and rapidly
replace the cone into the neck of the flask. Allow the reaction to
Disconnect the absorption tube C and tilt the
continue for 45 minutes.
20

IS : 253 - 1985

absorber tube so that the reagent solution flows back and forth between
the absorber and bulb to dissolve any red complex and to thoroughly
mix the solution.
Transfer the solution to the photometric cell. Absorption measurement is done at 540 nm with 5 ml coloured red complex
solution in a cell of 1 cm thickness against blank reagent solution for
Volume and apical path of the comparison cell
total transmittance.
shall be same for both the measurements and may be adjusted to suit
the instrument.
Alternatively, record its optical density at 540 nm as
both are calibrated on the scale.
A-13.2.4.2 Transfer 10 g of the dried sample into the conical flask
With the absorbed
and carry out the procedure as described above.
solution, measure its percent transmittance or optical density at 540 nm
Since the colour is not
against total transmittance
for the reagent.
stable, measurement of optical density or percent transmittance
shall be
done immediately.
A-13.2.4.3 The material shall be taken to have not exceeded the
limit prescribed
in Table
1 if the percent transmittance is more than
the percent transmittance obtained for 10 ml of standard arsenic solution
( 10 pg ). If the optical density with the sample is less than the optical
density obtained with 10 ml of standard solution, it passes the limit test
of 1 ppm arsenic.
A-13.2.4.4
Plotting and determination of arsenic - If it is desired to
know the exact amount of arsenic, determine the percent transmittance
or optical density for another standard solution containing 5 pg of arsenic.
Since it obeys Beers Law, draw a graph plotting the logarithm of the
percent transmittance
( log T) or optical density determined for the
Straight line is obtained
standard solution against their arsenic content.
From
passing through the points obtained for 0, 5 and 10 pg of arsenic.
the graph, read the amounts of arsenic corresponding to the respective
percent transmittance
or optical density of the sample and blank
solution.
A-13.2.4.5

Calculation

Arsenic content in the sample in

microgram per gram ( ppm ) = 01 ( Ml -

M2 )

where

A-14.1

Ml -= mass in microgram

in the sample, and

M2 = mass in microgram

in the blank.

Apparatus

A-14.1.1

Kessler Cylinders -

50 ml capacity.

21

IS:253-1985
A-14.2 Reagents
A-14.2.1

&tric Acid Sojutiq

A-14.2.2

Ammonium Hydroxide - Relative

.*
So,dium Diethy
D<thiocarbam@e

A-1$.23

20 percent aqueous.

sodium diethyl dithiocarbamate

in 1.000
amber bottle and- protect from strong light,

density 0.90.
- Dissolve
1 g of
ml of water.
Keep in an

Solution

A-14.2.4 Standard Copper Solution - Dissolve O-392 g of copper sulphate

pentahydrate
( CuSO4. 5HsO ) in water.
Make up the volume with
water to 1 000 ml. When required for use, pipette 10 ml of the solution
into a 1 000 ml volumetric flask and, dihtte up to the mark with water.
One millilitre of this solution contains O*OOlmg of copper ( as Cu ).
A-14.3 Procedure - Dissolve 2 g of the dried material in 10 ml of
water in cylinder, add 5 ml of citric acid solution, 2 ml of ammonium
hydroxide and 10 ml of sodium, &ethyl dithiocarbamate solution. Dilute
to the mark and mix v,ell. In the other Nessler cylinder, carry out a
control test using 4 ml of st+andar,d copper solution proceeding exactly the
same way as with the sample.
A-14.3.1 The limit prescribed in Table 1 shall be taken as not having
been exceeded if the intensity of colour developed with the sample 1s
not greater than that obtained in the control test.
A-15. DET&RMI&$TION
q-15.1 Gravimetri?
I:
A-15.1.1 Reagents
4-15.1,J.l

1976*.

OF POTAS+IU~J

Method Using Tetraphenyl

Concentrated

hydrochlogic

acid -

Boron

Conforming

to IS : 265-

A-15.1.1.2 Sodium tetrathenyl boron solution - Dissolve 1 g of sodium

tetraphenyl
boron in 100 ml of sodium hydroxide sojution ( 0.01 N ).
Before use cool the solution in ice.
A-15.1.1.3
Wash solution - Recrystallize potassium tetraphenyl boron
from acetone and saturate water with the recrystallized
product.
The
solution shall be prepared fresh each day.
A-15.1.2 Procedure - Transfer 59 rn! of the solution preserved in A-4.2
into a lOO-ml conical flask and add 3 ml of concentrated
hydrochloric
acid.
Place the flask in an ice-bath for 5 to 10 minutes.
When the
solution has cooled, add 25 ml of sodium tetraphenyl boron solution
*Specification

for hydrochloric

acid ( second revision ).

22

IS: 253-1985
previously
cooled in ice.
Mix by gentle swirling and leave in the icethrough
a sintered
glass crucible
bath for 5 to IO minutes.
Filter
( G No. 4 ) or a Gooch crucible, wash the flask and the precipitate
with
three lo-ml portions of the wash solution and dry the crucible containing
Cool in a desiccator
and
the precipitate
for one hour at 110 to 120C.
weigh.
A-15.1.3

Calculation

Potassium ( as K ), percent
by mass ( on dry basis )

= 218.20%

where
Ml

mass in g of the precipitate,

M2 = mass in g of the prepared

1 000 ml.
A-15.1.3.1
by multiplying
A-15.2

and
sample

Potassium
( as KC1 ), percent
the value obtained in A-15.1.3

By Flame

taken

for

the

test

in

by mass, shall be obtained

by a factor 1.906.

Photometer

A-15.2.1

Simple Flame Photometer

A-15.2.2

Reagents

Equipped

with interference

filter.

A-15.2.2.1
Standard
pdtassium
solution - Weigh
exactly
1 g of
potassium
chloride,
dissolve in water and dilute to one litre with water
in measuring
flask.
This solution contains 0.1 g KC1 per 100 ml.
A-15.2.2.2
Calibration graph - Take 10, 20, 40, 60 and 80 ml of
standard
potassium
solution ( see A-15.2.2.1
) and dilute to 100 ml with
distilled water in different measuring
flasks.
Each flask now contains
0.01, O-02, 0.04, 0.06 and 0.08 g KC1 per 100 ml,
Use these dilute
solutions
to obtain
a corresponding
galvanometer
readicg
as given
in A-15.2.3
and plot the concentration
against galvanometer
reading
in a rectalgular
co-ordination
graph.
Draw a smooth
curve
over the
points which gives a calibration
graph in the range 001 to 0.1 percent
KCI.
approximately
10 g of the
A-15.2.2.3
Sample
solution - Dissolve
sample in minimum
quantity of water and dilute to 100 ml in measuring
flask with water.
A-15.2.3

Procedure

A-15.2.3.1
Use a flame photometer
equipped
optical selective device consisting of the reflectors,
and measuring instrument
consisting of photocell,
23

with atomizer,
burner;
lenses and diaphragms;
amplifier and sensitive

IS : 253 -

1985

galvanometer.
The galvanometer
scale ranges from 0 to 100
which
measures
the intensity
of the radiation
transmitted
element.

divisions
by the

A-15.2.3.2
Insert the potassium filter corresponding
to wave-length
767 nm light burner
fed by illuminating
gas ( laboratory
gas ) and
adjust the specified air pressure between O-5 to 0.7 kg/cm2 and maintain
First spray water and adjust the pointer to zero in
the control
knob.
galvanometer
scale by zero adjustment
knob.
Then
spray the KC1
standard
solution
( A-15.2.2.1
) and adjust the deflection to maximum
( 100 ) by using sensitivity
control
knob.
Again spray water to see
pointer
comes to zero; then spray standard
solution to indicate 100.
Repeat till water reads zero and standard
solution read
100 with same
Now reading zero by water
adjustment
during
both the operations.
and with the same adjustment
100 by standard solution indicate that the
instrument
is ready for measurement.
A-15.2.3.3
Without altering the earlier adjustment
of the instrument
spray various
diluted solutions prepared
in A-15.2.3.2
and obtain
a
After washing
calibration
graph in the range 001 to 0-I percent KCI.
with water,
spray the sample solution
and obtain
the galvanometer
reading.
From
the graph, read out the corresponding
concentration
of
KC1 in the solution ( say A ).
A-15.2.4

Calculation
Potassium

chloride,

percent

= 100 -$-

where
A=
ilf =

concentration
mass of
solution.

of KC1 in the sample

dried

salts

taken

for

APPENDIX
( czause4.1 3
METHODS
B-l.

GENERAL

OF

SAMPLING

OF

REQUIREMENTS

B-1.0 In drawing,
storing,
preparing
following precautions
shall be observed.
B-l.1

Samples

shall not be taken

and

preparing

the

COMMON

sample

SALT

SAMPLING
handling

at a place exposed
24

and

EDIBLE
OF

solution,

test

samples,

to weather.

the

IS :253-1985
B-l.2 Precautions shall be taken to protect the samples, the sampling
instrument and the containers for samples from adventitious contamination.
B-I.3 To draw a representative sample, the contents of each container
selected for sampling shall be mixed thoroughly by suitable means.
B-l.4 The sample shall be placed
glass containers.

in suitable,

clean,

dry and

air-tight

B-l.5 Each sample container shall be sealed air-tight after filling and
marked with full details of sampling, the date of sampling and year of
manufacture.
B-2.

SCALE

OF SAMPLING

B-2.1 Lot of the same

constitute a
batches, the
containers in

All the packages in a single consignment of common salt

grade drawn from a single batch of manufacture
shall
lot. If the consignment is declared to consist of different
batches shall be marked separately and the group of
each batch shall constitute separate lots.

B-2.1.1 The number of packages ( n ) to be selected from the lot shall

depend upon the size of the lot ( N) and shall be in accordance
with
Table 2.
TABLE

NUMBER

OF PACKAGES
LOT

TO BE SELECTED

FOR

SAMPLING

No. OFPACKAGES

SIZE

TO BE SELECTED
11

N
50

51 >> 100
101 )) 150

4 to

4
5
7

151 )) 300
301andabove

10

NOTE - When the size of the lot is 3 or less, the number of packages to be selected
and the criterion for judgement conformity of the lot to the specification shall be as
agreed to between the purchaser and the supplier.

B-2.1.2 These packages shall be selected at random from the lot and
in order to ensure the randomness of selection, a random number table
( see IS : 4905-1968* ) may be used.
B-2.1.3 Samples shall be tested for each lot for ascertaining
of the material to the requirements of this specification.
*Methods

for random sampling.

25

conformity

is : 253 - 1985

B-3.1 Packages
B-3.1.1 From each of the packages selected according to B-2.1.2,
a
portion of the material about 200 g shall be drawn with the help of a
suitable sampling instrument.
B-3.1.2 Out of these portions equal quantities of the material shall be
taken and m,ixed. thoroughly to form :a composite sample of about 500 g.
The composite samples shall be divided into, three equal parts, namely,
one for the purchaser, one for the supplier and the third to be used as a
referee sample.
B-3.1.3 The remaining portion of the material
shall ,be divided into three equal parts, each
sample. One set of individual samples representing
shall be marked for the purchaser, another for the
to be used as a referee sample.

from each container

forming an individual
the container samples
supplier and the third

B-3.2 All the individual samples and the composite sample shall be
transferred to separate sample containers.
All the containers shall be
seaIed and Iabelled with full identification particular.
B-3.3 The referee test samples consisting of a composite sample and a
set ofindividual samples shall bear the seal of both the purchaser and
the supplier.
They shall be kept at a place agreed to between the
purchaser and the supplier, to be used in case af dispute between the
two.
B-4.

NUMBER

OF TESTS

B-4.1 For common salt, table salt and dairy salt, tests for the determination of moisture content, sodium chloride content and matter insoluble
in water shail be performed on each of the individual samples.
B-4.2 Test for the determination
of all other characteristics
given
Table 1 shall be performed on the composite sample ( SEIB-3.1.2 ).

in

B-5. CRITERIA FOR CONFORMITY

Samples - From the test results, the average
( X) and the range ( R) shall be computed for each of the characteristics
tested and on individual samples ( the range being defined as the
difference
between the maximum and minimum values of the test
results ). The appropriate expression as shown in co1 5 of Table 3 shall
be calculated for these characteristics.

B-5.1 For Individual

26

ISA!&-lb85
TABLE

CRITERIA

FOR

CONFORMITY

BASED ON

INbIVIDUAL
SAMPLE
( Clause B-5.1 )
SL CEARAGTERISTIC
No.

(1)

(2)

i)

Moisture content

ii)

Sodium chloride

AVER

AGE

TEST
RESULTS
1, 2, 3..., n

(5)

(4)

(3)

RZ

content

iii)

CRITERION FOR
CONFORYITY

RANQE

OF

@6 R, ) shall be

( zl

Rz

( %* - 0.6 R, ) shall be
greater than or equal
to 96 in case of common salt, 97 in case
of table salt and 99.6
in case of dairy salt

less than or equal to

60 in the case of
common salt and 0.5
in case of table salt
and dairy salt

( %s + 0.6 R, ) shall be
less than or equal to
1.0, 2.2 and WO3 in
case of common salt,
table salt, and dairy
salt

Percentage matter
insoluble in water

to have
B-5.2 For Composite Samples - The lot shall be considered
passed in respect of the characteristics
tested on the composite test sample,
if the test results
satisfy
the corresponding
requirements
given
in
Table 1.
B-5.3 The lot shall be considered
as conforming
to the specification
satisfies all the criteria given in B-5.1 and B-5.2.

27

if it

IS : 253 - 1985
( Continusdfro7n puge 2 )
Representing

Members

Shriram Fertilizers & Chemicals, Kota

DR S. K. SA~AR
SHRI RAJIV SINHA ( Alternate )
Central Salt and Marine
Chemicals
Research
DR J. R. SAN~EAVI
Institute ( CSIR ), Bhavnagar
DR M. J. MEH~A ( Alternate)
Salt Commissioner, Jaipur
SHRI P. SUBRAYANIAN
SHRI B. REVENNA ( Alternate j
Indian Salt Manufacturers Association, Bombay
SHRI G. P. THACKER
SHRI DHIRAJLAL G. SHAH ( Ahernate )
Standard Alkali ( Chemicals Division ), Bombay
SHRI T. P. VENKATRAMAN

28