( Reaffirmed 1999 )

Indian Standard
METHODS OF TEST FOR
DETERMINATI0.N OF WATER SOLUBLE
CHLORIDES IN CONCRETE ADMIXTURES
Cement and Concrete Sectional Committee, BDC 2

Chairman Representing
-DR H. C. VISVESVARAYA Cement Research Institute of India, New Delhi

Ir’ Members
DR A. S. BHADURI National Test House, Calcutta
SHRI E. K. RAMACHANDRAN

Central Building Research Institute ( CSIR ),

Roorkee
DR S. S. REHSI ( Alternate )
DIRECTOR CenEelhiRoad Research Institute ( CSIR.), New

DR R. K. GHOSH (Alternate)
DIRECTOR ( CSMRS ) Central Water & Power Commission, New Delhi
DEPUTY DIRECTOR ( CSMRS )
( Alternate )
SHRI K. H. GANQWAL Hyderabad Asbestos Cement Products Ltd,
Hvderabad
SRRI K. C. GHOSAL Alokuhyog Services Ltd, -New Delhi
SHRI A. K. BISWAS ( Alternate)
DR R. K. GHOSH Indian Roads Congress, New Delhi
DR R. R. HATTIAN~ADI Associated Cement -Companies Ltd. Bombav
SHXI P. J. JAQUS (Alternate)
JOINT DIRECTOR, STANDARDS Research, Designs & Standards Organization,
(B&S) Lucknow
DEPUTY DIRECTOR,
STANDARDS ( B & S ) CAlternate )
SHRI S. B. JOSEI ~ ’ S. B. Joshi & Co Ltd, Bombay
SHRI M. T. KANSE Directorate General of Supplies & Dispbsals
SHRI S. L. KATHURIA Roads -Wing, Ministry of Transport & Shipping
SHRI S. R. KULKARNI M. N. Dastur &‘Co (Private) Ltd, Calcutta
-. SHRI M. A. MEHTA Concrete Association of India, Bombay
SHRI 0. MUTHACREN Central Public Works Department
SUYERINTENDING ENGINEER
2ND CIRCLE ( Alternate )
SHRI ERACH A. NADIRSHAH Institution of Engineers ( India ) , Calcutta

( Continued on page 2 )

INDIAN
@ Coprright
STANDARDS
1973
INSTITUTION
This publication is protected under the Indian Copyright Jet (XIV of 1957 ) and
I’
reproduction in whole or in part by any means except with wrrtten permission of
the publisher shall be deemed to be an infringement of copyright under the said Act.
 16:69!2sP973
( Continuedfrompage 1 )

Members Representing
SHRI 5(. K. NAMBIAR ’ In personal capacity ( ‘ Ramanalaya ’ II First Crescent
Park Road, Gandhinagar, Adyar, Madras )
Bma NAREEE PRASAD Engineer-in-Chief’s Branch, Army Headquarters
CoL J. M. TOLANI ( Alternate)
PROF G. S. RAMASWAMY Stru;cta~eeEngineering Research Centre ( CSIR ),

DR N. S. BHAL ( Alternate)
DR A. V. R. RAO National Buildings Organization, New Delhi
SRRI K. S. SRINIVASAN (Alternate)
SHRI G. S. M. RAO Geological Survey of India, Nagpur
SHRI T. N. S. RAO Gammon India Ltd, Bombay
SHRI S.R. PINREIRO ( Alternate )
SECRETARY Central Board of Irrigation & Power, New Delhi
SHRI R. P. SHARMA Irrigation & Power Research Institute, hmritsar
SHRI MOHINDER SIN~H ( Alternate )
SHBI G. B. SINGH Hindustan Housing Factory Ltd, New Delhi
SERI C. L. KASLIWAL (Alternate)
SERI J. S. SINQHOTA Beas Designs Organization, Nangal Township
SH~I T. C. GARQ ( Alternate)
SHRI R. K. SINHA Indian Bureau of Mines, Nagpur
SHRI K. ALSUBRAMANIAM India Cements Ltd, Madras
SHRI P. S. RAMACHANDRAN
( Alternate )
SHRI L. SWAROOP Dalmia Cement ( Bharat ) Ltd, New Delhi
SHRI A. V. RAMANA (Alternate)
SHRI D. AJ~THA SIMHA, Director General, IS1 ( Ex-o$cio Member )
d’ Director ( Civ Engg )

Secretary
SHRI Y. R. TENEJA
Deputy Director ( Civ Engg ), IS1

Cement Subcommittee, BDC 2 : 1

Convener

DR R. R. HATTIANQADI Associated Cement Companies Ltd, Bombay

c
Members

SHRI V. B. DESAI Hindustan Construction Co Ltd, Bombay

D~E;;~~C&MDD ) Central Water & Power Commission
DIRECTOR
( C&MDD ) ( Alternate)
DR R. K. GHOSH Cent;ralhyoad Research Institute (CSIR ), New

SHRI P. GON Hindustan Steel Ltd, Ranchi

SHRI P. J. JACXJS Associated Cement Companies Ltd, Bombay

( Continued on page 8 )
 IS : ma- 1973

Indian Standard
MET-HODS OF TEST FOR
DETERMINATION OF WATER SOLUBLE
CHLORIDES IN CONCRETE ADMIXTURES

0. FOREWORD
h
0.1 This Indian Standard was adopted by the Indian Standards,
““I Institution on 23 March 1973, after the draft finalized by the Cement
and Concrete Sectional Committee had been approved by the Civil
Engineering Division Council.

0.2 Various types of concrete admixtures are being used in this country,
such as accelerators, retarders, water-proofers and air entraining agents.
Some of these admixtures are likely to contain water soluble chlorides
which are likely to cause corrosion of reinforcement in the reinforced
concrete. In fact the use of such chlorides containing admixtures has
been prohibited by IS : 456-1964*. However, the option of using such
admixtures is left to the engineer-in-charge who has to use his discretion
on the basis of relevant data in respect of the admixtures. As informa-
tion on the percentage of water soluble chlorides in the admixtures is of
vital imnortance
I
it is considered necessarv to bring out a standard dealing
with the methods of test for determination of water soluble chlorid:
content in concrete admixtures.
0.3 In reporting the result of a test or analysis made in accordance with
this standard, if the final value, observed or calculated, is to be rounded
off, it shall be done in accordance with IS :2-1960t.

c
-,’ 1. SCOPE
1.1 This standard specifies the following methods of test for determina-
tion of water soluble chlorides in concrete admixtures:

a) Volumetric method,
b) Gravimetric method, and
c) Turbidimetric method.

*Code of practice for plain and reinforced concrete ( second revision ).

TRules for rounding off numerical values ( revised ) .

3
s IS:69251973

2. SELECTION OF METHOD

2.0 One of the three methods may be used appropriately depending on

the concentration of the chlorides in the admixtures as per the declaration
of the manufacturer.
2.1 The volumetric method may be used when the chloride concentra-
tion is nearly 1 percent or above.

2.2 The gravimetric method may be used when the chloride concen-
tration is more than 2’5 percent.

2.3 The turbidimetric method may be used when the concentration of

chloride is as low as 2 ppm and above.

2.4 Where a choice is open between volumetric and gravimetric methods

volumetric method is preferable as it is quicker and less laborious.
Turbidimetric method may be adopted when the chloride concentration
is very low.

3. VOLUMETRIC METHOD

3.1 Reagents

3.1.0 Qgality of Reagents-Unless otherwise specified, pure chemicals

and distilled water (see IS: 1070-1960*) shall be employed in the tests.
NOTE - ‘ Pure chemicals ’ shall mean chemicals that do not contain impurities
which affect the results of analysis.

3.1.1 .Nitric Acid - 1 : 2.5 - 6 N.

3.1.2 Sodium or Potassium Chloride Solution ( Standard) -- 0.1 N.

3.1.3 Potassium Chromate Indicator Solution

3.1.4 Silver Nitrate Solution - 0’ 1 N.

3.1.4.1 Preparation -Weigh about 8.5 g of silver nitrate, dissolve in

distilled water and make up to 500 ml in a volumetric flask. +.

3.1.4.2 Standardization- Standardize the solution against 0.1 N

sodium chloride or potassium chloride solution using potassium chromate
solution as indicator. Adjust the normality exactly to 0.1.

3.1.5 Mrobenzene

3.1.6 Ferric Alum Indicator Solution

3.1.7 Ammonium Thiocyanate Solution -00’1 N.

*Specification for water, distilled quality ( revised ) .

 IS : 6925; X973

3.1.7.1 Prejaration-Weigh about 8’5 g of ammonium thiocyanate

and dissolve it in 1 litre of water in a volumetric flask. Shake well, and
standardize by titrating against 0’1 N silver nitrate solution using ferric
alum solution as indicator. Adjust the normality exactly to O-1.
3.2 Procedure

3.2.1 Weigh accurately sufficient quantity of the admixture such that

about 0.1 g of chloride is present in the sample. Add enough hot water
SO as to make a volume of 150 ml, stir until dissolution is complete.
If there is insoluble matter, filter and wash with water. Make up the
clear solution thus obtained to a volume of 250 ml with water, shake
h well.

Y 3.2.2 Pipette 50 ml of the solution into a 250-ml conical flask contain-

ing 5 ml of 6 _N nitric acid. Add 10 to 15 ml of 0’1 N silver nitrate
solution from the burette. Then add 2 to 3 ml of nitrobenzene and 1 ml
ferric alum indicator and shake vigorously to coagulate the precipi-
tate. Titrate the excess silver nitrate with 0.1 N ammonium thiocyanate
until a permanent faint reddish brown colouration appears. Repeat the
titration with another 50 ml portion.
3.2.3 From the volume of silver nitrate ( AgNOs ) solution added sub-
tract the volume of thiocyanate solution required. Take the average of
the two determinations. Calculate the percentage .of chloride (Cl) in the
sample:

1 ml 0.1 N AgNOs = 0.003 546 g, Ci

4. GRAVIMETRIC METHOD

4.1 Reagents
4.1.1 Concentrated Nitric Acid

4.1.2 Dilute Nitric Acid - 1 : 50.

4.1.3 Silver Nitrate jblution - approximately 0’1 N ( see 3.1.4 ).

4.1.4 Dilute Hydrochloric Acid - 1 : 100.

4.2 Procedure

4.2.1 Weigh out accurately sufficient quantity of the admixture such that
about 0.05 g of chloride is present in the sample. Add enough hot water
s’o as to make a volume of 150 ml, stir until the dissolution is complete.
Filter and wash with water if, there is insoluble matter. Add 1 to 2 ml
of concentrated nitric acid. Then add the silver nitrate solution slowly
and with constant stirring until the precipitation is complete. Add a
slight excess ( 5 to 10 ml ) of the silver nitrate solution. -Heat the sus-
pension nearly to boiling, while stirring constantly and maintain it at

5
IS:6925;1973

this temperature until the precip2tate coagulate3 and the snpernatant

liquid is clear. Set aside the beaker in the dark .for one hour and filter
through a previously weighed sintered glass or porcelain crucible. Trans-
fer the last traces of silver chloride adhering to the beaker with a
policeman. Wash the precipitate in the crucible with 1 : 50 nitric acid
added in small portions until 3 to 5 ml of the washings collected in a test
tube give no turbidity with 1 or .2 drops of dilute hydrochloric acid. Dry
the crucible and contents in an air-oven at 130 to 150°C for one hour.
Allow to cool in a desiccator and weigh. Repeat the process of drying
and cooling until constant weight is attained.

4.2.2 Calculate the percentage -of chloride in the sample:

0’1 g AgCl - 0.024737 Ci

5. TURBIDIMETRIC METHOD

5.1 Apparatus
5.1.1 Turbidimeter

5.2 Reagents
5.2.1 Dilute Ntric Acid - 1 : 3.
5.2.2 Silver Ntrate Solution - See 4.1.3.

5.2.3 Standard Sodium Chloride Solution

5.2.3.1 Preparation - Weigh accurately 0’164 9 g of sodium chloride
( previously dried at 105 to 110°C for 2 h ) and dissolve in 1 000 ml of
distilled water in a volumetric flask. This solution contains 100 ppm
chloride, that is, 100 mg/l.

5.3 Procedure
5.3.1 Calibration of the Turbidimeter -Take 5 ml of dilute nitric acid
in a loo-ml volumetric flask, add 5 ml of silver nitrate solution and
make up the volume with distilled water. Shake well and use the solu- L

tion as ‘ blank ’ for adjusting the ‘ z&o ’ of the galvanometer. Take

20 ml of the standard sodium chloride solution in a loo-ml volumetric
flask, add 5 ml of dilute nitric acid and 50 to 60 ml distilled water. Shake
well and add 5 ml of silver nitrate solution and make up the volume with
distilled water. Shake well and use this turbid solution to adjust the
galvanometer deflection to full ~scale.

5.3.1.1 Run in 1’0, 2’5, 5.0, 7’5, 10’0, 15’0, 17’5 and 20.0 ml standard
chloride solution from a burette into separate lOO-ml volumetric flasks.
Take the first flask, add 5 ml of dilute nitric acid and 50 to 60 ml distil-
led water. Shake well, add 5 ml of silver nitrate solution and make up

6-
 the volume with ~distilled water. Shake well and measure the turbidity
after checking the galvanometer c zero ’ again. Repeat the above proce-
dure with the remaining solutions.
5.3.1.2 Plot the galvanometer readings against chloride concentration
in ppm.
5.3.2 Determination of Chloride in the Test Sample-Weigh accurately
sufficient quantity of admixture such that $it contains about 0’01 g of chlo-
ride and boil with 100 to 150 ml distilled water. Filter and wash with hot
distilled water. Collect the filtrate and washings into a 500-ml volumetric
flask and make up the volume. Take 50 ml (see Note) of this solution
into a loo-ml ‘volumetric flask, add 5 ml dilute nitric acid and 5 ml
cI silver nitrate solution, and make up the volume with distilled water.
v Shake well and measure the turbidity after checking the galvanometer
‘ zero ‘. Read the chloride ion concentration in ppm from the calibra-
tion plot prepared earlier and then calculate the percentage of chloride
in the sample.
Weight of chloride in g x loo
Percentage chloride = ---
Werght of the sample taken
NOTE-Suitable dilutions may have to be carried out such that the galvanometer
reading falls within the range 2 to 15 ppm chloride whenever it is found necessary.
is :&!e - 1973

( Continued from page 2 )

1
Members Representiftg

JOINT DIRECTOR, RESEARCH Research, Designs & Standards Organization

(B&S) ( Ministry of Railways )
ASSISTANT DIRECTOR. RE-
SEARCH (B & S ) ( kter?ZUte )
SHRI S. V. MAHESHWARY Rohtas Industries Ltd, Dalmianag&
SXRI M. A. MEHTA Concrete Association of India, Bombay’
SRRI K. P. MOHIIZ~EN Central Warehousing Corporation, New Delhi
SHRI K. K. NAMBIAR In nersonal cavacitv ( ‘ Ramanalava ’ II First Crescem
* Park Road,. Gondhinogar, Ad&, Madras )
SARI E. K. RAMACHAN~RAN National Test House, Calcutta
DR A. V. R. RAO National Buildings Organization, New Delhi
SEICI G. T. BHIDE ( Alternate )
Snru
____~S. 1 A. REDDY Gammon India Ltd, Bombay
@RI R. P. SHARMA Irrigation & Power Research Institute, Amritsar
SHRI MOHINDER SINCE ( Alternate j
\
SHRI K. K. SOMANI Shree Digvijay Cement Co Ltd, Bombay
SHRI R. K. GATTANI ( Alternate )
SHRI K. A. SUBRAMANIAM Cement Manufacturers Association, Bombay
SUPERINTENDING ENGINEER Publkadyorks Department, Government of Tam3
( PLANNING & ~DESIQNS
CIRCLE )
E~ECUZI~E ENGINEER, BUILD-
rno CENTRE DIVISIONS( Alternate )
SHRI L. SWAROOP Dalmia Cement ( Bharat ) Ltd, New Delhi
SHRI A. V. RAMANA ( Alternate )
DR C. A. TANEJA Cent;iorkEilding Research Institute ( CSIR ),
DR R. K. DATTA ( Alternate )
COL J. M. TOLAN~ Engineer-in-Chief’s Branch, Army Headquarters
MAJ D. D. SRARMA (Alternate)
DR S. P. VARMA Directorate General of Technical Development
SHRI N. G.~BAAK (Alternate )
DE H. C. VISVESVARAYA Cement Research Institute of India, New Delhi
Da S. K. CHOPRA (Alternate)