IS:3535-1986 ( Rdtiid 1993) ( Reaffirmed 2004 )

Indian Standard
METHODS OF SAMPLING HYDRAULIC CEMENTS

( First Revision )
Third Reprint DECEMBER 1998

UDC 666.942.31:62&l

13

@ BUREAU
MANAK

Co&right 1986
INDIAN STANDARDS

OF

BHAVAN, 9 BAHADUR SHAH ZAFAR MARC NEW DELHI 110002

CP 4

August 1986

IS : 3535 - 1986

Indian Standard
METHODS OF SAMPLING HYDRAULIC CEMENTS

( First Revision )
Building Materials and Components Sampling BDC 31 Sectional Committee,

Chairman DR MOHAN RAI Members

Representing Central Building Roorkee Research Institute ( CSIR ),

SHRI S. K. Goswa~rr ( Aflcrnnte to Dr Mohan Rai ) National Test House, Calcutta SHRI S. K. BANEHJEE Central Road Research Institute ( CSIR ), New DI: P. R.~Y ClTAT_T~llUU Delhi Central Public Works Department, New Delhi SHRI P. S. GOPINATI~ SU~~VEYOR OF WOWI<S ( NZ ) ( Alfernntc ) Development Commissioner, Small Scale Industries, San1 S. C. KUYA-R New Delhi SHRI K. V. K. RAJU ( Alternate ) Indian Statistical Institute, Calcutta SRRl M. V. ~AKSHYANASAMY Struc;;;jayineering Research Centre ( CSIR ), DR A. G. MADH.~VA R-40 SI%HID. S. RAMACHANT)I~A MUI~THY ( Akrmolc ) S~rtr J. P. MAIKHURI

Export Inspection Council of India Commerce ), New Delhi

( Ministry

of

SHRI P. P. QAXENA ( Afkrnofc ) Railway Boaid ( Ministry of Railways ), New Delhi S~uu S. M. MITTAL DEPUTY DIRECTOR RES~AI~~H ( B & S )-I ( Alternate ) National Council for Cement and Building Materiala, DI: A. K. MULLICK New Delhi SHRI K. H. BABU ( Alternate*) Forest Research Institute and Colleges, Dehra Dun SHRI S. 5. RAJPUT National Buildings Organization, New Delhi S~nr K. S. SRINIVASAN SHRI T. R. BH.4TlA ( Alfemuta ) ( Conlincud on pose 2 ) @ Cqm&r 1986

BUREAU OF INDtAF.! STANDARDS This publication is protected under the Indian Co&ight Act ( XIV of 1957 ) and reproduction in whole or in part by any means except with written permission of the publirhy aball be deemed to be an infringement of copyright uader the said Act.

IS : 3535 - 1986
( Confirrucdfrom page 1 Members SHRI G. VEX~ATEEXLU

)
Rcprcsrntiq

?tlinistry of Shipping and Transport ( Roads Wing ), New Delhi SHRI PRAF~XL~ KUNAR ( dlfcrnafr ) Director General, ISI ( Ex-oJicio A/rmbrr ) SHRr G. W. DATEY, Director ( Statistics )
SHRI .\. K. T.~LWAR

Joint Director

( Statistics ), IS1

Panel
Memdcrs

on Sampling

of Hydraulic

Cements,

BDC 31/P-4
New Delhi and Building ( CSIR ), New

SHRI P. S. GOPIXATH

DR A. K. MELLICK

SHRI K. H. BABU ( AIfcntatc ) SHRI Y. R. PHULL

Central Public \Vorks Department, National Council for Cement Materials, New Delhi CentrDaclhFoad Research Cement Corporation Institute

of India Ltd, New Delhi

IS :3535-1986

Indian Standard
METHODS OF SAMPLING HYDRAULIC CEMENTS

( First Revision)
0. 0.1This FOREWORD

Indian Standard ( First Revision ) was adopted by the Indian Standards Institution on 24 January 1986, after the draft finalized by the Building Materials and Components Sampling Sectional Committee had been approved by the Civil Engineering Division Council. 0.2 With the considerable increase in production and consumption of cement which is of vital importance to the building industry, it is imperative that due consideration is given to sampling procedures which will help in the proper and objective evaluation of the various characteristics of cement. X2.1 Proper quality control during process ofmanufacture would also substantially reduce quality fluctuations of the material. The sampling procedures recommended in the standard, therefore, include the provisions for both process and lot inspection. 0.3 This standard was first issued in 1966. It is being various modifications necessary in the light of experience use could be incorporated. revised so that gained in its

0.4 In this revised version, inspection levels for routine control have been incorporated for those characteristics that have been included in various cement specifications from time to time by Cement and Concrete Sectional Committee, BDC 2. In order to provide a better quality assurance to the consumer, an upper limit to the quantity of material in a lot has been provided. The frequency of testing/inspection in process inspection for various characteristics has been modified so as to bring it in line with current practices in the cement industry. Keeping in view the practical difficulties in some cases in taking the requisite quantity of material in a single operation of the sampling equipment, provision for taking the material in two or three operations has been included. The quantity of material required for the laboratory sample has, been increased so that sufficient material is available for carrying out various tests on laboratory samples and the composite sample. In order to obtain

IS t 353s - *966*. the increased quantity of laboratory sample, the weight of increment particularly for included. 0.5 This standard covers the methods only. The methods for sampling of be covered in separate standards. _ .z. 0.6 In reporting the results of a test or or calculated, is to be rounded off, IS : 2-1960*. the provision for increasing smaller sub-lots, has been

for sampling of hydraulic cements concrete and cement products will analysis, if the final value, observed it shall be done in accordance with

1. SCOPE 1.1 This standard prescribes the methods for sampling and the criteria for conformity of hydraulic cements from bags, bulk storage ( silos ), Broad outlines with regard to. the ships hold, wagons and conveyors. controls to be exercised during the manufacturing process have also been indicated. 2. TERMINOLOGY 2.0 For the purpose apply. of this standard, the following definitions shall

2.1 Hydraulic Cement - Finely ground material which on addition of requisite quantity of water is capable of hardening both under water and in air by the chemical interaction of its constituents with water, and is also capable of binding together appropriate materials. 2.2 Lot -: The quantity and offered for inspection of cement from the same manufacturing at one time, not exceeding 2 000 tonnes. unit

2.3 Sub-Lot - The quantity a lot is divided for the purpose 2.4 Increment ing implement. The quantity

of cement in each of the parts into which of sampling. of cement taken at a time by the samplthat is, the increments by for

as collected from a sub-lot, 2.5 Gross Sample - Sample quantity of cement obtained by aggregating together all the from the same sub-lot. 2.6 Laboratory Sample reducing the gross sample laboratory testing.
*Rules for romding off numerical

The* quantity by following

of cement obtained a specified procedure

values

( revisvd

).

1s : 3535 - 19SS of cement obtained by mixing 2.7 Composite Sample - The quantity together equal quantities of cement from each of the laboratory samples representing the sub-lots into which the lot has been divided. 3. GENERAL RULES test samples, the

storing and handling 3.1 In drawing, preparing, following precautions and directions shall be observed: a) The sampling instrument shail be clean

and dry when used.

b) Precautions shall be taken to protect the sample, the material being sampled, the sampling implement and the containers for samples from adventitious contamination. c) The sample containers shall be of such a size that they are almost completely filled by the sample. d) The sample containers shall he sealed air-tight after filling and marked with full particulars of the material and the date of sampling. e) Samples shall be stored in such a manner that the temperature of the material does not vary unduly from the normal temperature. f) The place of sampling shall be clean and dry and free from draught. 3.2 The interval of drawing the increments shall be, as far as possible, uniform in terms of mass throughout the whole quantity of the lot. However, if the rate of handling quantity is uniform, the interval of drawing the increments may be based on time unit in place of quantity unit. 4. PROCEKS LNSPECTION

4.1 The object of inspecting cement by the purchaser is to ensure its conformity to the specification requirements whereas inspection done by the manufacturer during production is to ensure uniformity and reduce quality fluctuations 10 minimum. For process control, the manufacturer shall take representative samples of the product at regular intervals to control the quality fluctuations. The inspection levels given in Table 1 are recommended for routine control over the manufacturing process. 4.2 Methods
of Drawing Samples

4.2.1 Clinker - Every hour, a sample shall be drawn from each kiln immediately after it comes out of the cooling chamber. All the hourly samples drawn during a day shall bemixed together and shall constitute the composite sample for the day. After taking out a sufficient quantity of clinker from this composite sample for chemical analysis, the remaining clinker in the composite sample shall be mixed together and pulverized with a proper proportion of gypsum or both or the additives and tested *for all other characteristics of the specification. 5

TABLE

P RECOMMENDED ROUTINE

INSPECTION CONTROL

LEVELS

FOR

( Clnrrrc 4.1 ) Sr, No. CHARACTERISTICS/ TESTS RWQI-I:?~CY 0~ INSPE~'I.ION/TIZ~TS *_-_----_-_---_-~ ____----_---_ Cemt nt Clinker;Pozzolana Cement Grinding Packing (3) ) One composite sample every day for clinker and every weelr for pozzolana One composite sample every day (clinker taken hourljl ) do (4) One composite sample every week * (5) One composite sample every week

(1) i)

(2) Chemical composition ( complete analysis

ii)

Fineness

sample One every alternate hour and one composite sample every da) a) One sample every hour comb) One posite sample every day do

One composite sample every day

iii)

Setting time

do -

iv)

Soundnes

do

v) vi)

Compressive

strength

do do

do do

One composite sample every day do do

vii).

Degree of whiteness ( for white Portland cement only ) Heat of hydration ( for low-heat Portland cement only ) Drying shrinkage Portland-pozzolana ment only ) ( for ce-

do

One composite every sample week do

One Composite sample every week do

viii)

ix)

x) xi) xii)

Transverse strength ( for Portland and Portland blast furnace cement only ) Air content ( for masonry cement only ) retention Water masonry cement ( for only )

do

do

do do do

do do do

Hydrophobicity ( for hydrophobic Portland cement only+ )

NOTE - For physical requirements laboratory ball mill by adding clinker relevant specification, shall be tested.

under co1 -3, cement samples prepared in the with different suitable additives as per the

IS : 3535 - 1986 4.2.2 Cement Grinding - Every hour, a sample shall be drawn from the For fineness, a sample taken grinding mill and tested for setting time. every alternate hour shall be tested. The remaining portions of the hourly samples shall be mixed together to give the composite sample for the day. Similarly, a composite sample for a week shall be prepared. The frequency of testing for various characteristics shall be according to co1 4 of Table I.
4.2.3 Cement Packing - One composite sample every day from the packing machine shall be tested for fineness, setting time, soundness, compressive strength and degree of whiteness. The remaining portions of the daily samples, shall be mlxed together to give the composite sample for the week which shall be tested for other characteristics of the specilication. 4.2.4 For effective process control, the use of statistical quality control techniques is recommended and helpful guidance may be obtained in this respect from IS : 397 ( Part 1 )-1972*, IS : 397 ( Part 2 )-1975t and IS : 397 ( Part 3 )-1~80:. 4.2.4.1 The inspection data or the results of tests done at the place of manufacturer may be made available along with the materials supplied to enable the purchaser to judge the acceptability of the lot. 4.2.5 When such information cannot be made available or when the purchaser so desires, the procedure laid down in 5 shall be followed for judging conformity of the lot of hydraulic cements to the requirements of the relevant material specifications. 5. LOT

INSPECTION
shall be selected and ejtamined for each lot separately their conformity to the requirements of the relevant

5.1 The samples

5.1.1 For obtaining reliable conclusions, it is recommended that as far as possible, cement be sampled when it is in motion; that is, from conveyors or during loading or unloading. 5.2

Sampling .from Conveyors

5.2.1 Sub-Lots - For the. p&pose of sampling, a lot while it is being discharged over a conveyor shall be divided into a number of sub-lots in accordance with Table 2.
*Method for statistical quality control during production: Part 1 Control charts for variables ( jirsf rewim ). *Method for statistical quality control during production: Part 2 Control charts for attributes and count of defects ( second reoisim ). $.Method for statistical quality control during production: Part 3 Special control charts.

5.2.1.1 A representative gross sample shall be drawn from each of the sub-lots and shall be kept separately. Thus, there will be as many gross samples as the number of sub-lots into which the lot has been divided.
TABLE 2 NUMBER OF SUB-LOTS INTO IS TO BE DIVIDED WHICH ) A LOT

( Cfuuses5.2.1,

5.3.1, 5.4.1, 5.5.2 and5.6.1

WEIQHTOFTTHELOT ( IN TONNES )

No.0~ &B-LOTS
2 3 4 5 6 7

up to
101 201 301

100
200 300 500

501 1 000 1 001 2 000

5.2.2 Gross Sample - The gross sample shall be collected by taking a number of increments at regular intervals such that one increment is taken for every 10 tonnes or part thereof from the material discharged. The increment shall preferably be taken from the full cross-section and The best possible way of thickness of the stream and in one operation. taking the increment is to collect the material in a receptacle which cuts across the entire stream at the time when the material is discharged from the conveyor. If it is not possible to take the increment at. the point of discharge, it may be taken from the moving belt by means of a scoop For this which can sweep across the whole cross-section of the material. purpose, if practicable, the conveyor may be stopped while the increment is taken. The weight of increment shall not be less than 2 kg. It shall be ensured that the quantity of sample so collected is sufficient for the tests as per 5.7. 5.2.3 As increments are taken from the sub-lot, they shal! be placed directly in moisture-proof, air-tight containers to avoid moisture absorpIf the increments are placed in cans, tion and aeration of the sample. the cans shall be completely filled and sealed immediately. Moistureproof multiple wall paper bags or plastic bags may be used, if they are strong enough to avoid breakage and if they can be sealed immediately after filling in such a manner as to eliminate excess air in the bag and avoid moisture absorption and aeration of the sample. The containers shall carry suitable identification marks so that they can be related back to the particular sub-lot from which the gross sample has been taken. 8

1s : 3535

- 1986

5.3 Sampling

from

Bulk Storage

( Silos )

5.3.1 Sllb~Lols - For the purpose of sampling, the quantity of cement in the bulk storage shall be divided into a number of sub-lots depending upon the weight of the lot, in accordance with Table 2. The division into sub-lots shall be indicated by placing suitable markers on top of the cement.

5.3.2 Grass Sample - The gross sample shall be taken from a sub-lot by taking increments at regular intervals when the cement is being charged into the bulk storage or is being discharged from the bulk storage. If there is more than one opening for charging or discharging, the increments shall be taken from each opening. The number of increments shall be such that one increment is obtained for every 10 tonnes of the cement or part thereof. Each increment shall weigh at least 2 kg. It shall be ensured that the quantity of sample so collected is sufficient for tests as per 5.7. 5.3.3 The increments taken manner described in 5.2.3. 5.4 Sampling
from Ships

from
Hold

the sub-lot

shall

be

stored

in

the

5.4.1 Sub-Lots - For the purpose of sampling, the quantity in the ships hold shall he divided into a number of sub-lots upon the weight.of the lot, in accordance with Table 2.

of cement depending

5.4.2 Gross Sample - When the depth of the cement to be sampled does not exceed 2 m, increments may be obtained by a slotted tube sampler as shown in Fig. 1. The slotted tube-sampler shall be between 15 to 18 m long and about 35 mm in outside diameter and shall consist of two polished brass telescopic tubes with registering slots which are opened or closed by rotation of the inner tube; the outer tube being provided with a sharp point to facilitate penetration. Where applicable, for depths of cement greater than 2 m, a sampling pipe activated by an air jet which is capable of removing cement from different depths may be used. The increments obtained by the slotted tube-sampler or sampling pipe shall be taken from well-distributed points and various depths of the cement in the sub-lot The number of increments shall be such that one increment is obtained for every 10 tonnes or part thereof from the cement. The increment shall weigh at least 2 kg. The material may be drawn in two or three operations. It shall be ensured that the quantity of sample so collected is sufficient for tests as per 5.7. 5.4.3 manner The increments taken described in 5.2.3.
from Wagons

from

the sub-lot

shall

be

stored

in

the

5.5 Sampling
5.5.1

received

This method in wagons.

shall apply when loose cement or cement in bulk is If thecement is supplied in bags, 5.6 shall apply. 9

IS : 3535 - 1986 5.5.2 Sub-Lots - For the purpose of sampling, the $uantity of cement in wagons shall be divided into a number of sub-lots depending upon the weight of the lot: in accordance with Table 2. The sub-lots shall consist of approximately equal number of wagons. 5.5.3 Gross Sample - The gross sample shall be taken from a sub-lot with the help of a slotted tube-sampler of the same design as shown in Fig. 1 but about 60 cm in length. The sampler shall be taken in the manner described in 5.4.2 from at least six evenly distributed points in each selected wagon.
~ll5-+--15O--+-115~+l5O---+ t-225

35-O

00

SLOTS IN BOTH THE TUBE5 X 2.24mm THICK BRASS TUBE

INNER TUBE.IS FRE TO ROTATE INSIDE

ENLARGED

VIEW

OF A SLOT

All dimewiona Fro. 1

in millimetm.

SLOTTEDTUBE-SAMPLER

FOR BULK CEMENT of less It for the

5.5.3.1 ,From each selected wagon approximately equal number increments shall be taken and weight of increment shall be not than 2 kg. The material may be drawn in two or three operations. shall be ensured that the quantity of sample so collected is sufficient teats as per 5.7. 5.5.4 mannez The increments taken described in 5.2.3. for the sub-lot shall be stored in

5.6 Sampling from Bags of cement 5&l SuQ.Lots - For the purpose of sampling, the quantity in the lot shall be divided into a number of sub-lots, depending upon the weight of the lot, in accordance with Table 2. The sub-lots shall consist of approximately equal number of bags. 5.6.2 Gross lot, at least 2 sampled. In to be selected representative sample from a subSample - FQr drawing percent of the bags subject to a minimum of five shall be case fractional numbers are obtained, the number of bags shall be taken to be equal to the next higher integer. 10

IS : 3535 - 1986
5.6.2.1 These bags shall be chosen at random from the sub-lot. To ensure the randomness of selection, a random number table as agreed to between the purchaser and the supplier shall be used ( see IS : 49051968* ). In case such a table as not available, the following procedure may be followed:

Starting from any bag at random, count the bags in the sub-lot in one order as 1, 2, 3, up to Y and so on. Every rth bag SO counted shall be removed, where r = N/n, .N being the number of bags in the sub-lot and n the number of bags to be selected. In case the value of Y comes out to be a fractional number, its .value shall be taken as equal to the integral part of it. 5.6.2.2 The sampling tube shown in Fig. 2 shall be inserted diagonally into the valve of the bag and the thumb placed over the airThe material may be drawn in two hole and then shall be withdrawn. or three operations. n 520 -1

All dimensions in millimetres.

Fro. 5.6.2.3 i,ncrements than 2 kg. is sufficient 5.6.3 manner

TUBE-SAMPLER FOR PACKAGED CEMENT VOLUME 300 cm3 AP~ROX

From each selected bag, approximately equal number of shall be taken and weight of each increment shall be not less It shall be ensured that the quantity of sample so collected for tests as per 5.7. from the sub-lot shall be stored in the

The increments taken described in 5.2.3.

5.7 Reduction

Sample

5.7.1 Each gross sample shall be reduced separately. The material collected in the gross sample shall be thoroughly mixed, breaking the lumps and removing the foreign materials. It shall then be passed through 850-micron IS sieve. The foreign materials and hardened lumps that do not break on sieving or brushing, shall be discarded.
*Methods for random sampling.

11

IS : 3535 - 1986 5.7.2 Coning and Qtcartering - The material shall be scooped into a coneshaped pile. Care shall be taken to drop each scoopful exactly over the same spot as otherwise the central axis of the cone will be slackened. After the coneis formed, it shall be flattened by pressing the top of the cone with the smooth surface of the scoop. Then the cone is cut into quarters by two lines which intersect at right angles at the centre of the cone. The reduction isachieved by rejecting any two diagonally opposite quarters.

5.7.2.1 Sample splitter or riffle samplers of the appropriate tie used for reducing the gross sample mechanically.

size may

5.7.3 The reduction of the sample m the manner described in 5.7.2 shall be continued till 11 kg of the material required for the laboratory sample is obtained. 5.7.4 Equal quantities-of the material shall be taken from each of the laboratory samples representing the sub-lot into which the lot has been divided and mixed together to constitute a composite sample representing the lot as a whole. The weight of the composite sample shall be about 21 kg. and the composite sample shall be 5.7.5 The laboratory sample divided into three equal parts, one fir the purchaser, another for tLe The reicree supplier and the third to be used as a referee sample. sample shall be used in case of a dispute between the purchaser a&l the supplier. Each of these parts shall then be placed in a moisture-nrobf air-tight container to avoid moisture absorption and aeration ofFhe samples. They shall be labelled with full identification particulars such as suppliers name, the lot and the sub-lot number, the date of sampling, etc. 5.8 Number
5.8.1 The of Tests

laboratory

chemical and physical requirements samples shall be tested are: sulphur content as sulphuric anhydride,

for which and

individual

a) Total

b) Fineness. 5.8.2 A composite sample shall be tested for all the requirements.

5.9 Criteria

for Conformity

5.9.1 For those characteristics where a composite sample has tested for a lot, only one test result will be available and that result satisfy the requirements of the specification. 12

been shall

IS :3535 - 1986
5.9.2 When two laboratory samples have been analyzed individually from a lot for any characteristic, the lot shall be considered as conforming to the requirement -for that characteristic only if both of them pass. 5.9.3 When three or more laboratory samples have been analyzed individually from a lot for any characteristic, the following procedure shall be followed for judging the conformity to the requirements of that characteristic.

5.9.3.1 For
laboratory calculated

dilikrent samples, the as follows: (3 ) =

test results obtained by analyzing different average ( 2 ) and the range ( R ) shall be

Average Range

The sum of test results Number of test results and the

( R ) = The difference between the maximum minimum val.ues of the test results.

5,9.3.2 If the specification limit for the characteristic is given as a minimum, the value of the expression ( 2 - 0.5 R ) shall be calculated from the relevant test results. If the value SO obtained is greater than or equal to the minimum limit, the lot shall be declared as conforming to the requirement of that characteristic. 5.9.3.3 If the specification limit for the characteristic is given as a mauimum, the value of the expression ( Z + 0.5 R ) shall be calculated rrom the relevant test results. If the value SO obtained is less than or equal to the maximum limit, the lot shall be declared as conforming to the rkquirement of that characteristic. 5.9.3.4 If the characteristic has two-sided specification limits the value of the expression ( ;i: - 0.5 R) and ( ? + 0.5 R) shall be calculated from the relevant test results. If the values SO obtained lie between the two specification limits, the lot shall be declared as conforming to the requirement of that characteristic.

13

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