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IS 4202 (1967): Method for determination of chloride

content of textile materials [TXD 5: Chemical Methods of
Test]

“!ान $ एक न' भारत का +नम-ण”

Satyanarayan Gangaram Pitroda
“Invent a New India Using Knowledge”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह”

है”
ह
Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
 IS : 4202 -1967
( Reaffirmed 1999 )

Indian Standard
METHOD FOR DETERMINATION OF
CHLORIDE CONTENT OF TEXTILE MATERIALS

(Second Reprint AUGUST 1991)

UDC 677’01 : 543 : 546’131-2

%’ :

@ Copyright 1967

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

Gr 3 September 1967
 IS : 4202 - 1967

Indian Standard
METHOD FOR DETERMINATION OF
CH L@RIDE CONTENT OF TEXTILE MATERIALS

Textile Chemistry Sectional Committee, TDC 5

Representing
Ahmedabad Textile Industry’s Research Association,
Ahmcdabad

SIlKI K. 1). ~!All.4l~lJRJI Textile Auxiliaries Manufacturers’ Association,

Bombay
])I: s. .\I. ~:l’I.RAIII-T The Cotton Technological Research Laboratory
(ICAR), Bombay
SIlRl F;. s. hlUJANc. ORice of the Textile Commissioner, Bombay
SIII~I 15. 1%. <:II~\KKAvEI~TI Superintendence Company of India ( Privale )
Limited, Calcutta
Srrar R. C. n~ccrrx ( Alternnfe)
SIIRI R. c:. DASCUPTA National Test House, Calcutta
IhRIXTOR 01’ 1 ~hNDI.OOMS Government of Madras
SIIRI Ii. IIAW~MIXTIIY ( Alternate )
1h A. s. 1)ITI Indian Jute Industries’ Research Association,
Calcutta
~11111S. E;. hTT,, Ahmodabad Manufacturing & Calico Printing Co
Ltd, Alimedabad
STIRI GIJNVANT MAN(:ALI)AS Ahmedabad Millowners’ Association, Ahmedabad
I)lC V. P. KUIXAKNI All Jndia Handlodm Board, Bombay
Slmr I,. <;. ~~AKHIJANI Indian Rope Manufacturers’ Association, Calcutta
SIIRI A. K. GII~SE ( Alternafe )
SllllI S..IL RrelrTA The Bombay Textile Research Association, Bombay
SllltI s. S. MDIIT.4 ICI ( India ) Private Ltd, Calcutta
Srrlcl V. j, C’~rs~l,unv (Allen&e )
1)R s. 11. h~IIATl<E The Bangalore Woollen, Cotton & Silk Mills Co
Ltd, Bangalore.; and the Huckingham & Carnatic
Company LimIted, Madras
SIIRI s. hf. .IlISTKY Association of Merchants & Manufacturers of Textile
Stores & Machinery, India, Bombay
1)1X(!. .v. K. hiI:KTHY Ministry of Defence ( DGI )
SIrIt c:. I.. (;l:p.rA (.Urna&)
SlII<l I’. s. .~.\I)K.4KNI Ministry of Defence ( DGI )
1)~ \‘. IN. NI(:AM Ministry of Defcnce ( R & D )
Sllltl N. 1). !h4ND.\RI (.&V?&)
Ih XI. \.. N~>IKAK The Millowners’ Association, Bombay
1)K I). \‘. I’nKlhlr The Bombay Textile Research Association, Bombay
?iIIKI (;OKDII~\NII~IISI~~~. PATEL Shri Dinesh Mills Ltd, Baroda
( Continued on puxe 2 )

ISUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002
IS:4202-1967
(Continuedfrompa:e 1)

Members Representing
SHRI I. L. PATEL Inspection Wing, Directorate General of Supplies t
Disposals ( Ministry of Works, Housing &
SUPPlY )
SHRI A. K. PRAMANICK ( dltcrnatc )
SHRI Y. G. PATHAK The Textile Processors’ Association ( India ), Bombay
SHRI G. R. PODAR Silk & Art Silk Mills’ Association Ltd, Bombay
SHRI I. G. PARIKH ( Alternate )
REPRNE~TATIVE . Directorate of Industries, Government of Punjab
REPRESENTATIVE Shri.Ram Institute for Industrial Research, Delhi
SHRI JAJ~NADAS K. SHAH The Raipur Manufacturing Co Ltd, Ahmedabad
SHRI R. C. SHAH The Ahmedabad Textile Industry’s Research
Association, Ahmedabad
SHRI S. J. SHAH Association of hIerchants & Manufacturers of Text&
Stores & Machinery, India, Bombay
SHRI G. V. SHIROLKAR The Delhi Cloth & General Mdls Co Ltd, Delhi
DR R. V. R. SUBRAMANIAN The Silk & Art Silk Mills’ Research Association,
Bombay
SHRI S.M. CHAKRABORTY, Director General, IS1 ( Ex-ojkio Member )
Direclor (Tzs)
Secrelniy
SIJRI G. S. L\IIILYANKAK
Deputy Director ( Tcx ), ISI

Undyed Textile Materials Subcommittee, TDC 5 :2

Conr~encr
SHRI K. c. SIIhII .\hmcdabad ‘l’cxtile Industry’s Reseal+3 Association,
Ahmcdabad

SIIRI (;.G. ~ULK~RSI ( .I&cr,,a/e

lo
Shri R. C:. Shah I
DR KLZLIAKI hl. D. B&vs.\rr l‘hr Silk S; Art Silk Rlills’ Kcscarch .\ss’cirinlion,
Uombay
Supcrintendcncc Company of India ( I’ri\,atc ) l.td,
Calcutta
SIlKI 1~. c. llaacllr ( .I//rlwrrle )
SIIRI R. J. CIIIKTE ‘I‘hc Khatau Alakanji Spinning & \\‘caving Co Ltd,
Bombay
SIIRI C. I,. G~PTA Xlinistry of Dcfcncc ( lX;l )
SINI 13. K. KEDIA l’he Raymond \t’oollcn ?rlills Limitrd, Ilcw~l)ay
sI<Rt K. R'rANIvANNAN Shri Ram Institute for Industrial Research, Delhi
DK V.N.NIC'.AM Ministry of Dcfcnce ( R ,& D )
SHRI N. D. BHANDARI (.~&wzale )
DE 1). V. PARIEH The Bombay Textile Rcscarch Association, Bombay
REPRESENTATIVE Directorate of Industries, Government of Punjab
SIIRI,JAMNAD.\SK. SIIAli Raipur Manufacturing Co Ltd, Ahmcdabad
 IS : 4202 - 1967

Indian Standard
METHOD FOR DETERMINATION OF
CHLORIDE CONTENT OF TEXTILE MATERIALS

0. FOREWORD
0.1 This Indian Standard was adopted by the Indian Standards Instit\ltion
on 31 July 1967, after the draft finalized by the Textile Chemistry Sectional
Committee had been approved by the Textile Division Council.
0.2 In textile industry, textile materials undergo various treatments iI\
course of which extraneous matter of various types, such as skin: or
finishing material, water-soluble salts ( chlorides and sulphates ) is gatl~c~(l
by or added to the textile materials. Such water-soluble SUlJStaIlCt’S, il‘
present, in more than certain quantities may have deleterious elfccts OII tile
fibrous material or on other materials with which they arc associarcrl ill
use and may, therefore. affect their performance in scrvicc. It is 11op~1
that this standard will IX useful for dctcrmining the chloride colltcllt in
aqueous extract of textile materials.
0.3 The.gravimetric and vc,lumctric methods for cstinlatini the cllloridc
content m textile materials arc prescrihcd in this standard. Tht: potelttio-
metric titration method lvhich is suitable for very small quantities of
chloride prcscnt in text&: materials is al$o Kivcn as third method.
0.4 In reporting the result of a test ma& in accordance with this standard,
if the final value, ol,sc%rvcd or calculated, is to 1~ roundrd off, it sllall 1~
dorir in acrordanct: with IS : 2-lOW*.

1. SCOPE

1.1 This standard prescribes the methods for determination of water-

soluble chloride in textile materials and the procedure for extracting the
textile materials with lvatcr.

2. PRINCIPLE

2.1 The aqueous extract of textile material is prepared, the chlor:c:e

content is determined, either gravimetrically or volumetrically and expresscri
as the percentage of the weight of the conditioned material.
+Ru!es for rounding off numerical values ( n&d),

3
IS : 4202 - 1967

3. SAMPLING
3.1 Sampling for Fibre and Yarn
3.1.1 Lot ( Fibre or Tarn ) - The quantity of fibre or yarn from the same
source shall constitute a lot.. If the lot contains more than 200 kg of fibre
or yarn, it shall be divided in sub-lots each weighing 200 kg or less.
3.1.2 From a sub-lot 15 increments each approximately weighing 10 m
shall be taken from different parts so that a representative sample %
obtained. All the increments thus collected shall be thoroughly mixed.
This shall constitute the test sample.
‘3.2 Sampling for Fabrics
3.2.1 Lot ( Fabric ) -The quantity of fabrics manufactured under
relatively uniform conditions shall constitute a lot.
3.2.2 The number of pieces to be selected from a lot shall be as given
below. The pieces thus selected shall constitute the gross sample:
Ldt Ske SamfileSQe
up to 100 3
101 ,) 300
301 500 4
501 &d above 7
3.2.3 From each p,iece in the gross sample about 25 g of fabric shall be
taken out from at least two different parts. The parts shall then be cut
into further smaller pieces and thoroughly mixed. The pieces thus
collected shall constitute the test sample.

4. TEST SPECIMENS
4.1 From thotestsample, draw at least two test specimens each weighing
about 10 g. Cut the test specimens into small pieces. If the sample
under analysis is lo&e fibre, take about 5 g of the test specimen.

,5. CONDITIONING OF TEST SPECIMENS

5.1 Prior to test, the test specimens shall be conditioned for 24 hours to
moisture equilibrium in a standard atmosphere at 65 & 2 percent relative
humidity and 27” & 2°C temperature ( see also IS : 196-1966* ).

6. APPARATUS
6.1 Flat-Bottom Flask -‘of a suitable capacity with a glass stopper.
6.2 Water-Cooled Condensers
6.3 Sintered-Glass Crucible - porosity 4.
*Atmosphericconditionsfor testing ( revised).

4
 IS : 4202 - 1967

6.4 Titration Vessel and Reference Half-Cell - With suitable @H

meter as used with glass electrode balanced to read in millivolts, or
galvdnometer and tapping key. A convenient arrangement is shown in
Fig. 1. The half-cell is filled with a suspension made by dissolving 14 g
of sodium oxalate and 10 g of potassium nitrate in one litre of distilled
water, adding with constant stirring, 100 ml of O-1 N silver nitrate
solution.
NOTE - The stock of suspension should he kept in dark glass bottle.
-

SILVER
ELECTRODE

REFERENCE
HALF-CELL

GROUND-GLASS
JOINT

\ / / DRAIN COCK

FIG. 1 TITRATION VESSEL AND REFERENCE HALF-CELL

7. QUALITY OF REAGENTS
7.1 Unless specified otherwise pure chemicals shall be employed in tests and
distilled water ( see IS : 1070-1960* ) shall be used where the use of water
as-reagent is intended.
NOTE - ‘ Pure chemicals ’ shall mean chemicals that do not contain impurities which
affect the test results.

*Specification for water, distilled quality ( revised ).

5
IS : 4202 - 1967

8. PREPARATION OF AQWOUS EXTRACT

8.1 Condition the test specimens to moisture equilibrium in the standard

atmosphere and weigh accurately each test specimen.

8.2 Put a test specimen in the flask and add sufficient amount of water to
it to make liquor in material ratio of 20 : 1 ( see Note ). Connect the flask
to the condenser and bring rapidly to the boil and continue to boil the
liquor *gently for 60 minutes. Disconnect and remove the flask whiIe the
liquor IS still boiling and close it immediately with the glass stopper fitted
with the stopcock. Rapidly cool the flask to room temperature ( 27°C ).
Do not remove or open the tap until ready for filtration.

NOTE - If the test specimen is wool in any form, felt or loose fibre masses of any
composition, the liquor to material ratio should be 50 : 1.

8.3 Similarly prepare separate extracts for each of the remaining test
specimens.

9. FIRST METHOD ( GRAVIMETRIC )

9.1 Reagents

9.1.1 &‘her J%tYde Solution - 0.1 N.

9.1.2 .;\i’tric .-kid

4 concentrated (sp gr 1.42 )

b) 0.5 percent ( ZO/? )

9.2 Procedure

9’.2.1 Take a suitable measured portion of extract ( see 8.2 ). Add .5 ml

of concentrated *nitric acid per 100 ml, boil for 5 minutes and leave it over-
night. Filter through a paper-pulp pad, wash with distilled water and
add a slight excess of O-1 N silver nitrate solution to the combined filtrate
and washings. Heat the solution, protected from direct light, in a water-
bath until the precipitate is coagulated and supernatant liquor is clear.
Verify completeness of precipitation by adding a drop of O-1 N silver nitrate
solution to the supernatant liquor. Allow it to cool overnight in the dark
and then filter through a tardd sintered-glass crucible. Wash the preci-
pitate with 0.0 percent nitric’acid until the washings give no opalescence
when tested with sodium chlotide solution. Dry the crucible first at 100°C
and finally to constant weight at 130’ to 150°C.

9.2.2 Carry out a blank determination.

6
 IS : 4202 - 1967

9.2.3 Calculate the chloride content of the test specimen by either of

the following formulae:
a) For materials in yarn and fabric form other than wool (w
Note 1 ):
+495x
- (A-B)
v -
b) For wool in any textile form and for felts and loose fibre masses
of any composition (see Note 2 ):
pJ237x(A--B)
V
where
P = percentage, by weight, of water-soluble chloride as
chloride ion;
A = weight, in g, of the precipitate obtained in the test
( see 9.2.1) ;
B = weight, in g, of the precipitate obtained in blank (see
9.2.2 ); and
V = volume, in ml, of the extract taken for the test (see
9.2.1).
So-m1- 100 ml of estract are equivalent to 5.0 g of conditioned
tcsl specimen.
NOTE 2 - 100 ml of extract are equivalent to 2.0 g of conditionrd
test specimen.

9.2.4 Kepeat the test with the extracts of the remaining test specimens.
9.2.5 Calculate the average of the values obtained as in 9.2.3 and 9.2.4.

lu. SECOND METHOD ( VOLUMETRIC)

10.1R-agents
10.1.1Standard Silver JYitrate Solution - O-1 NJ.
10.1.2Stundard Potassium Thiocyanute Solution - 0.1 NT.

10.1.3Ferric Alum Indichtor Solution -‘Dissolve IO0 g of ferric ammonium

sulphate in 250 ml of water. Heat the solution to boiling and add con-
centrated nitric acid ( sp gr 1.42 ) slowly until the red colour disappears.
NOTE-The amount of nitric acid used should be between 6 and 15 ml.

10.2Procedure
10.2.1Take a suitable measured portion of extract. Acidify it with
5 ml of nitric acid. Add 5 ml of 0.1 N siiver nitrate solution and 5 ml

7
IS : 4202- 1967

ferric alum indicator solution. Add sufficient amount of nitrobenzene

(see Note ). Titrate the excess of the silver nitrate against 0.1 N potassium
thiocyanate solution till the first appearance of faint pink colour.
KOTE - About 1 ml of nitrobenzene is required in every 0.05 g 01 chloride.

10.2.2 Calculate the chloride content of the test specimen by either of

the following formulae:
a) For materials in yarn and fabric form o&r than wooi (see
Note 1 ):

b) For wool in any textile form and for felts and loose fibre masses
of any composition ( see 1\Tote 2 ):
P _ LAB - CD ) x 3.55 x 5.
V
where
P = percentage, by weight, of Gater-soluble chloride as
chloride ion;
fI = volume, in ml, of silver nitrate solution;
B = normality of silver nitrate solution;
C = volume, in ml, of potassium thiocyanate, required for
back titration;
D = normality of potassium thiocyanate solution; and
V = volume, in ml, of extract taken for test.
NOTE 1- 100 ml of extract is equivalent to 5.0 g of conditioned
test specimen.
XOTE 2 - 100 ml of extract is cquivalcnt to 2.0 g of conditioned
test specimen.

10.2.3 Repeat the test with the extracts of the remaining test specimens.
10.2.4 Calculate the average of the results obtained as in 10.2.2
and 10.2.3.

11. THIRD METHOD ( POTENTIOMETRIC TITRATION )

11.1 Reagents
11.1.1 Silver Nitrate Sol&m - 0.01 S.
11.1.2 Nitric Acid - concentrated ( sp gr 142 ).
11.2 Procedure
11.2.1 Take a suitable measured portion of the extract ( see 8.2 ). Add
5 ml of concentrated nitric acid per 100 ml of extract and boil for five

8
 IS : 4202 - 1967

minutes. Cool rapidly to room temperature and transfer to the titration

vessel. Start the stirrer, connect the electrodes to the pil meter balanced
to read in millivolts and titrate with 0.01 N silver nitrate solution until the
galvanometer first indicates zero.
11.2.2 Carry out a blank determination.
NOTE -Before each test, it should be verified that all parts of the apparatus are
clean. The silver electrodes should be cleaned with very fine abrasive or a suitable
chemical method. Discard and replace the silver oxalate suspension at the first sign of
darkening, and to delay darkening half-cell should be shielded from light when not in
use. The suspension bottle should be shaken thoroughly before replenishing th.e half-
cell. Take particular care that clecrrolytes do not come into contact with the junction
between the silver wire electrodes and their leadr to the pH meter. Flush the electro-
lyte junction after each determination by easing the stopper at the bottom of the half-
cell to allow fresh extract suspension to flow into the junction.

11.2.3 Calculate the chloride content of the test specimen by either of

the following formulae:

a>For materials
Note 1 ):
in yarn and fabric form, other than wool (see

p=O*71 x (VI-V,)
V

b) For wocl in any textile form and for felts and loose fibre masses
of any composition ( see Note 2 ):
p= 1.77 x (G-v,)
V
where
P = percentage, by weight, of chloride content as chloride
ion;
VI = volume, in ml, of 0.01 N silver nitrate solution required
for test ( see 11.2.1 );
Vs = volume, in ml, of 0.01 N silver nitrate solution required
for blank ( see 11.2.2 ) ; and
V = volume, in ml, of extract taken for the test.
NOTE 1 - 100 ml of the extract are equivalent to 5.0 g of
conditioned test specimen.
No= 4 - 100 ml of the extract are equivalent to 2.0 g of
conditioned test specimen.

21.2.4 Repeat the test with the extracts of the remaining test specimens
and calculate the percentage of water-soluble chloride in each test
specimen.
11.2.5 Calculate the average of the values obtained as in 11.2.3
and 11.2.4.

9
IS : 4202- 1967

12. REPORT

12.1 Report the value obtained as in 9.2.5, 10.2.2 or 11.2.5 as the

percentage of water-soluble chloride as chloride ions in textile materials.
NOTE - If the percentage of the water-soluble chlorides is to be expressed as sodium
chloride, then multiply P by l-65.

12.2 Report also the method used (whether gravimetric, volumetric or

potentiometric titration ).

10
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