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IS 4031-3 (1988): Methods of physical tests for hydrauliccement, Part 3: Determination of soundness [CED 2: Cementand Concrete]

Gr2

IS : 4031 ( Part 3) - 1988(Reaffirmed 2005)

Indian Standard

METHODS OF.PHYSICAL TESTS FOR HYDRAULIC CEMENT

PART 3 DETERMINATION OF SOUNDNESS

( First Revision)

Fifth Reprint JUNE 2006( IncludingAmendmentNo. I )

UDC 666.94: 620.17

© Copyright 1988

BUR E A U OF IN D I A N S TAN DAR D SMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

October 1988

AMENDMENT NO. 1 MARCH 1993TO

IS 4031 ( Part 3) : 1988 METHODS OF PHYSICALTESTS FOR HYDRAULIC CEMENT

PART 3 DETERMINATION OF SOUNDNESS

( First Revision)

( Page 2, clause 5.1.4 ) - Substitute the following for the existing clause:

'5.1.4 Water Bath - Water bath with means of heating, capable of containingimmersed Le-Chatelier moulds with specimens and of raising their temperaturefrom 27 ±ZOC to boiling in 27 ±3 minutes.' .

(CEDZ)Printed at Prabhat'Offset Press, New Delhi-2

IS I 4031 (Part 3 ) - 1988

Indian Standard

METHODS OFPHYSICAL TESTS FOR HYDRAlJLIC CEMENT

PART 3 DETERMINATION OF SOUNDNESS

( First Revision)

o. FOREWORD

0.1 This Indian Standard (Part 3) ( FirstRevision) was adopted by the Bureau of IndianStandards on 24 February 1988, after the draftfinalized by the Cement and Concrete SectionalCommittee had been approved by the CivilEngineering Division Council.

0.2 Standard methods of testing cement areessential adjunct to the cement specifications.This standard in different parts lays down theprocedure for the tests to evaluate physical pro­perties of different types of hydraulic cements.The procedure for conducting chemical testsof hydraulic cement is covered in IS : 4032­1985*.

0.3 Originally all the tests to evaluate thephysical properties of hY,draulic c~l?en!s werecovered in one standard but for facilitating theuse of this standard and future revisions it hasbeen decided to print the different tests asdifferent parts of the standard and, accordinglythis revised standard has been brought out inthirteen parts. This will also facilitate updating

*Method of chemical analysis of -hydraulic cement(first rllluion ).

1. SCOPE

1.1 This standard (Part 3) covers the proce­dures for determining the soundness of cement.

2. SAMPLING AND SELECTION OF TESTSPECIMEN

2.1 The samples of the cement shall be taken inaccordance with the requirements of IS : 3535­1986* and the relevant standard specificationfor the type of cement being tested. ·The repre­sentative sample of the cement selected as aboveshall be thoroughly mixed before testing.

s, TEMPERATURE AND HUMIDITY

3.1 The temperature of the moulding room, drymaterials and water shall be maintained at 27

*Methods of sampling hydraulic cements (first revUion).

1

of individual tests. Further, since publicationof the original standard in 1968, a number ofstandards covering, the requirements ofdifferentequipment used for testing of cement, a briefdescription of. which was also covered in thestandard, had been published. In this revision,therefore, reference is given to different instru­ment specifications deleting the description ofthe instruments, as it has been recognized thatreproducible and repeatable test results can beobtained only with standard testing equipmentcapable ofgiving desired level of accuracy. Thispart covers determination of soundness byLe-Chatelier method and autoclave test.

0.4 For the purpose of deciding whether aparticular requirement of this standard iscomplied with, the final value, observed orcalculated, expressing the result of a test oranalysis, shall be rounded off in accordance withIS: 2-1960*. The number of significant placesretained in the rounded off value should be thesame as that of the specified value in thisstandard.

*Rules for rounding off numerical values (""u,d).

± 2°C. The-relative humidity of the laboratoryshall be 65 ± 5 percent.

3.2 The moist closet or moist room shall bemaintained at 27 ± 2°C and at a relative humi­dity of not less than 90 percent.

4. GENERAL

4.1 Soundness of cement may be determined bytwo methods, namely Le-Chatelier method andautoclave method as described in 5 and 6.

5. LE-CHATELIER METHOD

5.1 Apparatus

5.1.1 The apparatus for conducting the Le­Chatelier test shall conform to IS : 5514-1969*.

*Specification for apparatus used in Le-Chatelier test.

IS a4031 ( Part 3 ) • 1988

TABLE 1 PERMISSIBLE VABlATIONSON WEIGHTS

5.1.3 Weights - The permissible variations onweights in use in weighing the cement shall beas prescribed in Table 1.

5.1.4 Water Bath - Water bath capable ofcontaining immersed Le-Chatelier moulds withspecimens and of raising their temperature from27 ± 2°C to boiling in 27 ± 3 minutes.

5.2 Procedure

NOTE 1 - The sensibility reciprocal is generallydefined as the change in load required to change theposition of rest of the indicating element or elements ofa non-automatic indicating scale a definite amount atany load,

NOTE 2 - Self-indicating balance with equivalentaccuracy may also be used.

being performed. Cover the mould with anotherpiece of lightly oiled glass sheet, place a smallweight on this covering glass sheet and immedia­tely submerge the whole assembly in water at atemperature of 27 ± 2°C and keep there for24 hours.

6. AUTOCLAVE METHOD

5.2.2 Measure the distance separating theindicator points to the nearest O'5 mm. Sub­merge the mould again in water at the tempera­ture prescribed above. Bring the water toboiling, with the mould kept submerged, in 25to 30 minutes, and keep it boiling, for threehours. Remove the mould from the water, allowit to cool and measure the distance between theindicator points. The difference between thesetwo measurements indicates the expansion ofthe cement.

5.3 CalculatioD - Calculate the mean of twovalues to the nearest 0'5 mm to represent theexpansion of cement.

5.4 Retest - In the event of cement failing tomeet the test for soundness, a retest may bemade after aeration.· For this purpose, spreadout the cement in a layer of 75mm thicknessand store it for 7 days in an atmosphere main­tained at 27 ± 2°C and relative humidity of 50to 80 percent. Retest this cement as describedin 5.2.

'6.1 Apparatus

6.1.1 Balance - Same as 5.1.2.

6.1.2 Weights - Same as 5.1.3.

6.1.3 Graduated Glass Cylinders - Graduatedglass cylinders of 150 ml capacity shall be used,The permissible variation on these cylindersshall be plus or minus one millilitre. The maingraduation lines of the cylinders shall be incircles and shall be numbered. The least gradua­tions shall extend at least one-seventh of theway around, and intermediate graduations shallextend at least one-fifth of the way around thecylinder. The graduation lines may be omittedfor the lowest 5 mI.

PBRMISSIBLEVARIATION ONWEIGHTS INUSB. PLUS OR

MINUSg

(2)

0'350'300'250~20

0'150'100'050'040'030'02

0'01

g

(1)

50630025020010050201052

1

WEIGHT

5.1.2 Balance ---'- The balance shall conform tothe following requirements:

On balance in use, the permissible variationat a load of I 000 g shall be plus or minus 1'0 g.The permissible variation on new balanceshall be one-half of this value. The sensibilityreciprocal shall be not greater than twicethe permissible variation.

5.2.1 Place the lightly oiled mould on a lightlyoiled glass sheet and fill it with cement pasteformed by gauging cement with 0'78 times thewater required to give. a paste of standardconsistency [see IS : 4031 (Part 4 )-1988*]. Thepaste shall be gauged in the manner and underthe conditions prescribed in IS : 4031 (Part4 )­1988*, taking care to keep the edges of themould gently together while this operation is

6.1.4 Moulds - Moulds of 25 X 25 mm sizeand 282 mm internal length and other accessoriesconforming to IS : 10086-1982*.

6.1.5 Autoclave - The autoclave shall consistof a high pressure steam boiler equipped withsuitable safety device. The capacity of heatingunit shall· be such that with maximum load(water plus specimens) the pressure of thesaturated steam in the autoclave may be raised

-Methods of physical tests for hydrualic cement: Part4 Determination of consistency of standard cement paste(fir' rellision ).

·Specification for moulds for use in tests of cement andconcrete.

2

to a gauge pressure of 2'1 MPa or to an absolutepressure of about 2'2 MPa, in I to Ii hourfrom the time the heat is turned on. Theautomatic pressure control shall be capable ofmaintaining the pressure at 2'1 ± 0'1 MPacorresponding to a temperature of 215'7 ±1'7°C, The autoclave shall be designed to permitthe pressure to drop from 2'1 MPa to less than0'07 MPa in one hour after the heat supply hasbeen shut off, It shall be equipped with a ventvalve for allowing the escape of air during theearly part ofthe heating period and for releasingany steam pressure remaining at the end of theone-hour cooling period, The pressure gaugeshall have a nominal dial diameter of 115 mmand shall be graduated from 0 to 4'1 MPa withscale division of not more than 0'04 MPa. Theerror in the gauge shall not exceed plus or minus0'02 MPa at the operating pressure of2'1 MPa.

6.1.6 Length Comparator - Changes in length oft~e test specimen shall be measured by anapparatus conforming to IS: 9459-1980·,

6.2 Preparation ofTest Specimens

6.2.1 Preparation ofMould.f - The moulds shallbe thinly covered with mineral oil. After thisoperation, the stainless steel or non-corrodingmetal reference inserts with knurl heads shallbe set to obtain an effective gauge length of250 mm, care being taken to keep them cleanand free from oil.

6.2.2 Mixing Cement Paste- The standard batchof cement paste shall consist of 500 g of cement,mixed with sufficient water to give a paste ofstandard consistency, .

6.2.3 Moulding Specimens - Immediately follo­wing the completion of mixing, the testspecimens shall be moulded in one or two layers,each layer being compacted with the thumb orforefinger by pressing the paste into the corners,around the reference inserts, and along thesurfaces of the moulds until a homogeneousspecimen is obtained. After the top layer hasbeen compacted, the paste shall be cut off flushwith the top of the mould and the surfacesmoothed with a few strokes of the trowel.:During the operations of mixing and moulding,the hand shall be protected by rubber gloves,

6.2.4 Storage ofTest Specimen - After the mouldhas been filled, it shall be immediately placedin a moist closet or a moist room. Specimensshall remain in the moulds in the moist roomfor at least 24 h. If removed from the mouldsbefore 24 h, they shall be kept in the moistcloset or moist room until tested.

·Specification for apparatus for use in measurementof length change of hardened cement paste, mortar andconcrete.

3

IS : 4031 ( Part 3J • 1988

6.3 Procedure

6.3.1 At 24 ± t h after moulding, the speci­mens shall be removed from the moist atmos­phere, measured for length, and placed in theautoclave at room temperature in a rackso thatthe four sides of each specimen shall be exposedto saturated steam. The autoclave shall containenough water to maintain an atmosphere ofsaturated steam vapour during the entireperiod oftest. Ordinarily; 7 to 10 percent of thevolume of the autoclave shall be occupied bywater.

6.3.2 To permit air to escape from the auto­clave during the early portion of the heatingperiod, the vent valve shall be left open untilsteam begins to escape (see 6.4), The valve shallthen be closed and the temperature of the auto-

. clave shall be raised at such a rate as will bringthe gauge pressure of the steam to 2'1 MPa in Ito Ii h from the time the heat is turned on. The2'1 ± O'lMPa pressure shall be maintained for3 h. At the end of 3 hours period, the heatsupply shall be shut offand the autoclave cooledat a rate such that the pressure will be less than0'1 MPa at the end of the hour, and any pressureremaining shall be slow released by partiallyopening the vent valve until atmospheric pressureis attained. The autoclave shall then be openedand the test specimens immediately placed inwater, the temperature of which is above 90°C.The water surrounding the bars shall· then becooled at a uniform rate by adding cold watersolthat the temperature of the water shall belowered to 27 ± 2°C in 15 min. The water sur­rounding the specimens shall then be maintainedat 27 ± 2°C in 15 min when the specimens shallbe surface-dried and their lengths measuredagain,

6.4 Safety Precautions

6.4.1 The pressure gauge should have amaximum capacity of 4'2 MPa. This is impor­tant because with too small a capacity there isbut a little length of arc in which the gaugehand may indicate pressure above the specifiedmaximum working pressure, The operator mustbe sure that the gauge hand has not passed themaximum graduation on the scale.

6.4.2 It is well to leave the pressure gaugetested, but in any event thermometer shallalways be used together with the pressure gauge,so as to provide a means of detecting any failureof the pressure gauge to operate properly andalso to indicate any unusual conditions such asthat resulting from loss of water from the auto­clave during the test.

6.4.3 The automatic control shall be main­tained in proper working order at all times.

6.4.4 The safety valve shall be set so as torelieve the pressure at about 6 to 10 percent

IS : 4031 ( Part 3 ). 1988

above the maximum of2"1 MPa specified, thatis. at about 2'3 MPa. The safety valve shall betested at least twice a year, either with a gauge­testing device or by adjusting the automaticcontrols so as to allow the autoclave to reach apressure of about 2'3 MPa at which pressure thesafety valve shall either open or be adjusted toopen. The safety valve discharge shall be direc­ted away from the operator.

NOTE - Unexpected combinations of conditions mayreally occur. For example, in one case the automaticcontrol had failed, the safety valve had stuck, and thegauge hand, which at first glance appeared to be atabout zero, had really passed the maximum graduationand had come to stop on the wrong side of the pin. Thiscondition of the gauge was finally detected and thepressure, then of an unknown magnitude, was releasedbefore failure could occur in the apparatus.

6.4.5 Heavy leather work gloves shall be wornto prevent burning of the hands when removingthe top of the autoclave at the end of the test.The vent valve shall be directed away from theoperator. When removing the autoclave lid, thelid shall be so tilted that any steam escaping frombeneath the lid may be discharged away fromthe operator. Care shall be taken to avoid scal­ding by any liquid that may have been used inthe autoclave well.

6.4.6 It shall be remembered that for many

4

of the autoclave pressure gauges now in use, thereturn of the gauge hand to the initial rest orstarting point does not necessarily indicate zeropressure within the autoclave; there may thenstill remain an appreciable pressure.

6.4.7 A few drops of kerosene placed in thevent valve about once a week will aid in keepingthe needle clean and in good-working condition.

6.5 CalculatioDS - The difference in lengthsof the test specimen before and after autoclavingshall be calculated to the nearest 0'01 percent ofthe effective gauge length which is the lengthbetween the innermost points of the metal insertsused as reference points and shall be reportedas the autoclave expansion of the cement. Acontraction ( negative expansion) shall be indi­cated by prefixing a minus sign to the percentageexpansion reported.

6.6 Retests - In the event of cement failing tomeet the test for soundness, a retest may hemade after aeration. For this purpose, spreadout the sample in a layer of 75 mm thicknessand store it for 7 days in an atmosphere maintai­ned at 27 ± 2°C and relative humidity of 50to 80 percent. Retest this cement as describedin 6.2 and 6.3.

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This Indian Standard has been developed from Doc': No. BDC 2 (4139)

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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