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IS 14959-1 (2001): Method of Test determination of watersoluble and acid soluble chlorides in mortar and concrete,Part 1: Fresh mortar and concrete [CED 2: Cement andConcrete]

REAFFIRMED 2011

IS 14959 (Part 1) : 2001

Indian StandardDETERMINATION OF WATER SOLUBLE AND

ACID SOLUBLE CHLORIDES IN MORTAR ANDCONCRETE — METHOD OF TEST

PART 1 FRESH MORTAR AND CONCRETE

ICS 91.100.10; 91.100.30

BIS 2001

BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

July 2001 Price Group 3

AMENDMENT NO. I SEPTEMBER 2007TO

IS 14959 (PART 1): 1001 DETERMINATION OF WATERSOLUBLE AND ACID SOLUBLE CHLORIDES IN

MORTAR AND CONCRETE - METHOD OF TEST

PART1 FRESH MORTAR ANDCONCRETE

(Page I, clause 4.1.6, line I) - Insert 'dried at 160·C and cooled in adesiccator' after 'silver nitrate'.

(Page I, clause 4.1.6, IMlline) - Insert 'and recordthe exact normality ofthe silver nitrate solution' at the end.

(Page I, clause 4.1.7,jirst/ine) - Substitute' 1.'2 g' for '1.7 g'.

(Page 2, clause 4.1.7, last line) - Insert 'or recordthe exact nonnalily' Itthe end.

(Page 2, clause 4.1.7)- Insertthe following noteat the end:

'NOTE - Sometimes it isdifficult 10 make cxacdy 0.02 N solution if the standud normalityof thesolution is less '.

(Page 2, clause 4.3.1.2, line 3) - Insert Cor more' after '2S ml' andsubstitute '0.02 N' ft» '0.2 Nt.

(Page 2, clause 4.3.2.2, line.2) - Delete the sentence 'Add S ml of 6 Nnitric acid.'

(Page 2, clause 4.3.2.1, line 3) - Substitute 'or more of 0.02 N' for 4 0 fstandard' . '

(Page 2, clause 4.4, lines 3 to 7) - Substitute in following for the existingformula:

hi· 0.709 (X-Y)

C oride, percent =m

where

X = volume of 0.02 N silvernitrateadded, in ml;Y=volume of 0.02 N ammonium thiocyanate consumed; andm = massof concrete sampletaken for test, in g.

(CEO 2)RepfOlraphy Unit,81S,NewDelhi,India

Cement and Concrete Sectional Committee, CED 2

FOREWORD

This Indian Standard (Part 1) was adopted by the Bureau of Indian Standards, after the draft finalized by theCement and Concrete Sectional Committee had been approved by the Civil Engineering Division Council.

Chlorides in the concrete could be drawn from different sources like aggregates, mix water, admixtures andcement and could lead to durability problems namely, corrosion of reinforcing steel in concrete if present insufficient quantity .. Chlorides could be present in different degrees of binding in the concrete matrix and couldbe determined as water soluble and as acid soluble chlorides. In some cases ofcorrosion ofcarbonated concrete,the combined chlorides (water soluble and acid soluble) will be let free in pore water and these chlorides arebannful to concrete. To minimize the chances ofdeterioration of concrete due to harmful chlorides, the level ofthese chlorides has been limited in various design codes. Therefore, this standard has been formulated to providenecessary guidance for determination of water soluble and acid soluble chlorides in concrete. This Part 1 of thestandard covers volumetric method of test for determination of chlorides in fresh mortar and concrete, andPart 2 of this standard covers the method of test for hardened mortar and concrete.

The composition of the committee responsible for the formulation of this standard is given in Annex A.

In reporting the results of a test or analysis made in accordance with this standard, if the final value, observedor calculated, is to be rounded off, it shall be done in accordance with IS 2 : 1960 'Rules for rounding offnumerical values (revised)'.

IS 14959 (Part 1) : 2001

Indian Standard

DETERMINATION OF WATER SOLUBLE ANDACID SOLUBLE CHLORIDES IN MORTAR AND

CONCRETE - METHOD OF TESTPART 1 FRESH MORTAR AND CONCRETE

IS No.1070 : 1992

1 SCOPE

This standard (Part 1) covers volumetric method oftest for determination ofwater soluble and acid solublechlorides in fresh mortar and concrete.

NOTE- The source of samples for test in accordancewith thisstandardmaybeeitherthestationary samplesobtainedfromprojectsitesor ready-mixed concreteplants.

1 REFERENCES

The Indian Standards listed below contain provisionswhich through reference in this text, constituteprovisions of this standard. At the time ofpublication,the editions indicated were valid. All standards aresubject to revision and parties to agreements based onthis standard are encouraged to investigate thepossibility of applying the most recent editions of thestandards indicated below:

TitleReagent grade water - Specifica-tion (third revision)

3025 Methods of sampling and test(Part 32) : 1988 (physical and chemical) for water

and wastewater: Part 32 Chloride(first revision)

3 SAMPLING

A sample offresh concrete or mortar shall be collectedwithin a period of two hours from the time ofadditionof water to the ingredients that is, cement, coarse andfine aggregates and admixtures, etc. However, everyeffort shall be made to collect the samples immediatelyafter mixing. Samples shall be obtained by takinguniformly distributed increments (preferably withoutstopping the mixing operations, provided samplingcan be safely carried out), and mixed thoroughly toform a combined bulk sample. The number ofincrements and size of bulk sample necessarilydepends on the quantity of the material, its variabilityand the accuracy required of the test results.

At least three approximately equal sample incrementstotalling 0.02 mJ shall be taken in a clean and dryreceptacle across the stream ofmortar or concrete. Thisreceptacle shall be constructed of non-absorbentmaterial, preferably of metal and shall be such that

the sample retained is not segregated. A flat surfacewithout retaining sides will not fulfill this purpose.Where three sample increments are taken they shallbe taken at about the time when one quarter, one halfand three quarters ofthe concrete have been dischargedfrom the mixer, and if more than three are taken theyshall be at correspondingly shorter, but of equalintervals.

4 METHOD OF TEST

4.1 Reagents

4.1.1 Quality ofReagent

Unless otherwise specified, pure chemicals ofanalytical reagent grade and distilled water (seeIS 1070) shall be used in the test.

4.1.1 Nitric Acid (HNOJ) Concentrated (SpecificGravity 1.42)

Prepare the solution, 6N (approximately), by diluting38 ml of concentrated nitric acid to 100 ml withdistilled water.

4.1.3 Ferric Alum [FeNH4 (S04)2 12 H20]

Dissolve 10 g of ferric alum in 100 ml of distilledwater and add 1 ml of nitric acid.

4.1.4 Potassium Chromate (K2 Cr04) , 5 PercentSolution

Dissolve 5 g of potassium chromate in 100 rnl ofdistilled water. NO

4.1.5 Nitrobenzene ( @l)24.1.6 Silver Nitrate (AgNO) Solution, 0.02 N

Weigh 1.7 g, of silver nitrate, dissolve in distilledwater and dilute to 500 ml in a volumetric flask.Standardize the silver nitrate solution against 0.02 Nsodium chloride solution using potassium chromatesolution as indicator (S percent m/v) in accordancewith the procedure given in IS 3025 (Part 32).

4.1.7 Ammonium Thiocyanate (NH. SCN) Solution,0.02N

Weigh 1.7 g of ammonium thiocyanate and dissolve

IS 14959 (Part I) : 2001

in one litre of distilled water in a volumetric flask.Shake well and standardize by titrating with 0.02 Nsilver nitrate solution using ferric alum solution as anindicator. Adjust the normality exactly to 0.02 N.

4.1.8 Sodium Chloride (NaCl), 0.02 N

Weigh 1.169 2 g of sodium chloride dried at105 ± 2°e, dissolve in distilled water and make up to1 000 ml in a volumetric flask.

4.2 Use of Filter Paper

In the methods prescribed in. this standard, relativenumbers of Whatman filter paper only have beenprescribed since these are commonly used. However,any other suitable brand offilter papers with equivalentporosity may be used.

4.3 Procedure

4.3.1 Warer Soluble Chloride

4.3.1.1 Weigh 1 000 ± 5 g of fresh mortar or concretesample in a 2 litre capacity beaker and add 500 ml ofdistilled water (chloride free). Stir the mixturevigorously for 15 minutes. After allowing the mixtureto stand for 10 to 15 minutes for settling, decant about200 ml of the supernatant solution into a clean dry250 ml capacity beaker. Immediately, filter thesolution through Whatman filter paper No. 1 andcollect the filtrate.

4.3.1.2 Pipette )0 ml of filtrate in a 250 ml capacityconical flask. Add 5 ml of 6 N nitric acid. Add aknown volume (X), preferably 25 ml of 0.2 N silvernitrate solution. Add 1 ml ferric alum and 5 ml ofnitrobenzene. Shake vigorously to coagulate the·precipitate. Titrate the excess silver nitrate with0.02 N ammonium thiocyanate solution until apermanent faint reddish brown colour appears. Note

2

down the volume (Y) ofammonium thiocyanate used.

4.3.2 Acid Soluble Chloride

4.3.2.1 Weigh about 1 000 ± 5 g of the fresh mortaror concrete sample in a 2 litre capacity beaker andadd 50 ml of 6 N nitric acid and 450 ml of distilledwater (chloride free) after stirring for few minutes.Stir the mixture vigorously for 15 minutes, Afterallowing the mixture to stand for 10 to IS minutes forsettling, decant about 200 ml of the supernatantsolution into a clean dry 250 ml capacity beaker .

. Immediately, filter the solution through Whatmanfilter paper No. 1 and collect the filtrate.

4.3.2.2 Pipette SO ml of filtrate in a 250 ml capacityconical flask. Add 5 ml of6 N nitric acid. Add a knownvolume (X), preferably 25 ml ofstandard silver nitratesolution. Add 1 ml ferric alum and 5 ml ofnitrobenzene. Shake vigorously to coagulate theprecipitate. Titrate the excess silver nitrate with 0.02 Nammonium thiocyanate solution until a permanentfaint reddish brown colour appears. Note down thevolume (Y) of ammonium thiocyanate used.

4.4 Calculation

Calculate the percentage of chloride (acid soluble/water soluble)by massofmortar or concrete as follows:

Chloride, percent = 0.0007 1 (X - Y),

where

X volume of silver nitrate added, in ml; and

Y volume of 0.02 N ammonium thiocyanateconsumed.

NOTE-Interference of silverchloridepanicles (whicharegen-erated ill-situ) in titration by reacting with thiocyanate can beavoided by the addition of'nitrobenzene which forms a filmonsilverchlorideparticles.

IS 14959 (Part I) : 2001

ANNEXA

(Foreword)

COMMITTEE COMPOSITION

Cement and Concrete Sectional Committee, CED 2

Builder'sAssociation of India,Mumbai

NationalCouncilforCementand BuildingMaterials. Ballabgarh

Gammon IndiaLtd,MwnbaiHospitalServicesConsultancy Corporation (India)Ltd,NewDelhi

CentralBoardof Irrigationand Power,NewDelhi

TheIndianHumePipeCompanyLtd,Mumbai

Hyderabad Industries Ltd,Hyderabad

Structural Engineering ResearchCentre(CSIR),Chennai

CementCorporationof'IndiaLtd,NewDelhi

GrasimIndustries Ltd,Mumbai

IndianInstitute ofTechnology,KharagpurThe IndiaCementsLtd,Chennai

GannonDunkerley andCo Ltd,Mumbai

CentralWaterCommission, NewDelhi

CentralSoil andMaterialsResearchStation, NewDelhi

StructuralEngineering ResearchCentre(CSIR),GhaziabadA.P.Engineering Research Laboratories, Hyderabad

SardarSarovarNannadaNigamLtd,Gandhinagar

B.G.SbirkeConstruction TechnologyLtd,PuneMinistryof SurfaceTransport,Department of SurfaceTransport(RoadsWing),

NewDelhiHindustanPrefabLtd,NewDelhi

CentralPublicWorksDepartment, NewDelhi

DirectorateGeneralofSuppJiesand Disposals, NewDelhi

ChairmanPADMASHRI DRH.C. VJSVESVARAYA

'Chandrika' , at 1S" Cross63-64 EastParkRoad,Malleswaram, BangaloreS60003Representing

OCL IndiaLtd,NewDelhiGeologicalSurveyof India,Kolkata

Me,,,bers

DRS.C. AHLUWALIADR S.S. Ameta

SHRJD.K. RAI (Alternale)SHRJ V.BA1.ASUBRAMAJ\1A

SHRJ R.P.S~GH (Altemale)SHRJ G.R.BHAIUTKARSHRJ C.C.8HATTACHARYA

SHRJI.K.PM1>EY (Alternate)SHJu A.K.CHADHA

SHRJ J. R. SIL (Altemale)CHIEF EJ\Gll\cER (DEsIGN)

SlJPE1Ul\-ra"D~GEl'GR\m (8&S) (Allemale)CHJEF El'GIt\"EER (NAVGAM DAM)

SUPEmTE~DIl'G EI'GIl\"EER (QCC) (Allemale)CHlEf EI'G~"EER (REsEARCH)-cuM-DIRECTOR Irrigation andPowerResearch Institute, Amritsar

REsEARCH0mcER (CO"CRE'TE 1"EcHJ\OLQGV)(Allemale)SHRJ 1.P. 0EsAJ GujaratAmbujaCementsLtd,Ahmedabad

SHRJB.K.JAGEnA (Alternate)DIRECTOR

I>JREcroRJOIl\& DIRECTOR (Alten,a/e)

DIRECTOR

SHRI P.L.KAsHYAP(Allen,ale)DIRfllOR (CMDD) (N&W)

[)EPUll DIRECTOR(CMDD)(NW&S) (Allernate)SHRI K. H. GAl'GWAI.

SHRJ V. PATTABHJ (Alten,ale)GEI\CJW. MANAGER

SEl'IOR MASAGER (EI'GIl'EEfWl;G) (A/temate)OR ASHOK KUMAR GHOSHSHRJ S.~A11i

SHRJ R.ARU1\Al~ (Alternate)SHRJ C.JAYARAMAJ\

SHRI A. K. JAll\ (AI/en,ate)SHRIS.S.GoVAUYA

SHRJV. K. Goa (A/ten,ate)JOIP\,. DIRECTOR (STAl'OARDS) (B&S)(CB-n Research, Designs& StandardsOrganization (Ministryof Railways), Lucknow

JOIl'\T DIRECTOR (STASOARDS) (8&S) (CB-II)(Alternate)SHRJ D.K.~"Ul\OO NationalTestHouse,Kolkata

SHRJ B.R. MEEJ\A (Alten,ate)MfMBFR-SEcRETARY

DIRECTOR (CIVIL) (A/ten,a/e)SHRJP.R.C.NAIR

S~P.D.~~(Ahemak)

DR R.NARAYANANSHRI S. GoPALKJUSHl'Al'\ (A/temate)

DRC. IWKUMARDRK. MOHA~ (Alternate)

SHJU S.A. REDoISHJU J. SARUP

SHRJ P.K.JAIPURJAR (A/ternate)SlDErARY

(Continued on page 4)

3

IS 14959 (Part I) : 2001

(Continued from page 3)

Members

SHRIS.S.SF.EHRA

SHRI SAT""DER KUMAR (Alten,ate)SHRI S. S. SEEHRA

SHRI A.K.SHARMA (Altemale)BRI

(Continuedfrom page 4)

Members

JOI~'T DIRECTORSTA!\DARDS (B&S)lCB-lJOI1\TDIREcToR STAl\1>AJU)S(B&S)/CB-U (Altemate)

DR S. C. MAITIOR SUDHIR M1sHRASHRJ R NAR.AYA1\~

SHRI K. MA!\I (Alternate)SHRI A. 8. PHADKE

SHRJ D.M.SAvuR(Allenrate)SHRI RAM KUMAR

SHRI RAJEEvGOEl (Alternate)SHIt( V.V. GoVll\1>A RAo

SHRJ R. P.GOEl (Alternate)SHRl S.A.REool

DR N. K. NAYAK (Altenlate)SHRJSUDDliOOA!\ Roy

SHRIM. K~DU (AI/ernate)SHRJ S.C. SA\VMSEY

SHRI R.P.MEHRolM (Alternate)SHRJ S.S.SEEHRA

SHlU SATAl\1>ERKUMAR (Alternale)

PROf M. S.SHElTYSHRI S.N.S~GH

SHRJSUIm'OER MOHAI\' (Altenla/e)

SHRI P. S~IVASAI\'SHRI P.BA1\'DOPADHYAY (AI/en,a/e)

SUPERJl\TEl'Dlt'G E!\GIt\'EER(DESI

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This Indian Standard has been developed from Doc: No. CED 2 (5722).

Amendments Issued Since Publication

Amend No.

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