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( Reaffirmed 1999 )
METHODS OF SAMPLING HYDRAULIC CEMENTS
( First Revision )
Third Reprint DECEMBER 1998
BHAVAN, 9 BAHADUR SHAH ZAFAR MARC NEW DELHI 110002
IS : 3535 . New Delhi SHRI P. ~AKSHYANASAMY Struc. S. RAMACHANT)I~A MUI~THY ( Akrmolc ) S~rtr J. P. C.1986 Indian Standard METHODS OF SAMPLING HYDRAULIC CEMENTS ( First Revision ) Building Materials and Components Sampling BDC 31 Sectional Committee. New Delhi S~uu S. Small Scale Industries. K.jayineering Research Centre ( CSIR ).. BANEHJEE Central Road Research Institute ( CSIR ). RAJPUT National Buildings Organization. MADH. BABU ( Alternate*) Forest Research Institute and Colleges. Calcutta SHRI S. MITTAL DEPUTY DIRECTOR RES~AI~~H ( B & S )-I ( Alternate ) National Council for Cement and Building Materiala. R. V. San1 S. K. BH.! 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. SRINIVASAN SHRI T. R. Chairman DR MOHAN RAI Members Representing Central Building Roorkee Research Institute ( CSIR ). K. S. K. DI: A. G.~VA R-40 SI%HID. . MAIKHURI Export Inspection Council of India Commerce ). RAJU ( Alternate ) Indian Statistical Institute. Goswa~rr ( Aflcrnnte to Dr Mohan Rai ) National Test House. M. GOPINATI~ SU~~VEYOR OF WOWI<S ( NZ ) ( Alfernntc ) Development Commissioner. 5. S.4TlA ( Alfemuta ) ( Conlincud on pose 2 ) @ Cqm&r 1986 BUREAU OF INDtAF. QAXENA ( Afkrnofc ) Railway Boaid ( Ministry of Railways ). New DI: P. New Delhi S~nr K.. DR A. Dehra Dun SHRI S. P. V. KUYA-R New Delhi SHRI K. New Delhi ( Ministry of SHRI P. MULLICK New Delhi SHRI K. Calcutta SRRl M. SHRI S. H.~Y ClTAT_T~llUU Delhi Central Public Works Department.
W. SHARXA Central Public \Vorks Department. BABU ( AIfcntatc ) SHRI Y. New Delhi CentrDaclhFoad Research Cement Corporation Institute of India Ltd. National Council for Cement Materials. S.\. BDC 31/‘P-4 New Delhi and Building ( CSIR ). GOPIXATH DR A. MELLICK SHRI K. New Delhi . ISI ( Ex-oJicio A/rmbrr ) SHRr G. New SHRI P. S. New Delhi SHRI PRAF~XL~ KUNAR ( dlfcrnafr ) Director General.IS : 3535 . VEX~ATEEXLU ) Rcprcsrntiq ?tlinistry of Shipping and Transport ( Roads Wing ). K. H. PHULL SHRI C. DATEY.~LWAR Joint Director ( Statistics ). IS1 Panel Memdcrs on Sampling of Hydraulic Cements. K. Director ( Statistics ) SHRI . T. R.1986 ( Confirrucdfrom page 1 Members SHRI G.
In order to provide a better quality assurance to the consumer. It is being various modifications necessary in the light of experience use could be incorporated. The quantity of material required for the laboratory sample has.3 This standard was first issued in 1966.IS :3535-1986 Indian Standard METHODS OF SAMPLING HYDRAULIC CEMENTS ( First Revision) 0. 0. therefore. include the provisions for both process and lot inspection. been increased so that sufficient material is available for carrying out various tests on laboratory samples and the composite sample. X2.4 In this revised version. Keeping in view the practical difficulties in some cases in taking the requisite quantity of material in a single operation of the sampling equipment. 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. 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. 0. In order to obtain . 0. BDC 2.2 With the considerable increase in production and consumption of cement which is of vital importance to the building industry. provision for taking the material in two or three operations has been included. revised so that gained in its 0. The sampling procedures recommended in the standard.1This FOREWORD Indian Standard ( First Revision ) was adopted by the Indian Standards Institution on 2‘4 January 1986. an upper limit to the quantity of material in a lot has been provided. 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. after the draft finalized by the Building Materials and Components Sampling Sectional Committee had been approved by the Civil Engineering Division Council.1 Proper quality control during process ofmanufacture would also substantially reduce quality fluctuations of the material.
bulk storage ( silos ).3 Sub-Lot . _ . is to be rounded off. if the final value.4 Increment ing implement.0 For the purpose apply. 2.6 In reporting the results of a test or or calculated. 0. 4 . Broad outlines with regard to.Sample quantity of cement obtained by aggregating together all the from the same sub-lot. the following definitions shall 2. the weight of increment particularly for included.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. the increased quantity of laboratory sample. The quantity of cement in each of the parts into which of sampling.The quantity a lot is divided for the purpose 2.1 This standard prescribes the methods for sampling and the criteria for conformity of hydraulic cements from bags.5 This standard covers the methods only.2 Lot -: The quantity and offered for inspection of cement from the same manufacturing at one time.z. The methods for sampling of be covered in separate standards. IS : 2-1960*. 2.1 Hydraulic Cement . of cement taken at a time by the samplthat is. SCOPE 1. not exceeding 2 000 tonnes. the provision for increasing smaller sub-lots.6 Laboratory Sample reducing the gross sample laboratory testing. and is also capable of binding together appropriate materials.5 Gross Sample . unit 2. 2.IS t 353s . TERMINOLOGY 2. of this standard. has been for sampling of hydraulic cements concrete and cement products will analysis. the ship’s hold. wagons and conveyors. *Rules for romding off numerical The* quantity by following of cement obtained a specified procedure values ( revisvd ). the increments by for as collected from a sub-lot. 0. 2.*966*. controls to be exercised during the manufacturing process have also been indicated. observed it shall be done in accordance with 1.
2 Methods of Drawing Samples 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. the storing and handling 3. uniform in terms of mass throughout the whole quantity of the lot.2. 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.2 The interval of drawing the increments shall be. 3. the manufacturer shall take representative samples of the product at regular intervals to control the quality fluctuations. the interval of drawing the increments may be based on time unit in place of quantity unit. if the rate of handling quantity is uniform. b) Precautions shall be taken to protect the sample. the material being sampled. following precautions and directions shall be observed: a) The sampling instrument shail be clean and dry when used. a sample shall be drawn from each kiln immediately after it comes out of the cooling chamber. After taking out a sufficient quantity of clinker from this composite sample for chemical analysis.1 In drawing. PROCEKS LNSPECTION 4.1 Clinker .19SS of cement obtained by mixing 2. the sampling implement and the containers for samples from adventitious contamination.1s : 3535 . All the hourly samples drawn during a day shall be’mixed together and shall constitute the composite sample for the day. 3. 4.The quantity together equal quantities of cement from each of the laboratory samples representing the sub-lots into which the lot has been divided.7 Composite Sample . as far as possible. preparing. d) The sample containers shall he sealed air-tight after filling and marked with full particulars of the material and the date of sampling. For process control. GENERAL RULES test samples. The inspection levels given in Table 1 are recommended for routine control over the manufacturing process. e) Samples shall be stored in such a manner that the temperature of the material does not vary unduly from the normal temperature. 4. 5 . c) The sample containers shall be of such a size that they are almost completely filled by the sample.Every hour. However. f) The place of sampling shall be clean and dry and free from draught.
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).1 ) Sr. 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. No.TABLE P RECOMMENDED ROUTINE INSPECTION CONTROL LEVELS FOR ( Clnrrrc 4. CHARACTERISTICS/ TESTS RWQI-I:?~CY 0~ INSPE~'I. under co1 -3. cement samples prepared in the with different suitable additives as per the 6 . shall be tested.ION/TIZ~TS *_-_----_-_---_-~ ____----_---_ Cemt nt ’ Clinker.
2 Sampling . it is recommended that as far as possible. *Method for statistical quality control during production: Part 1 Control charts for variables ( jirsf rewim ). 4. every alternate hour shall be tested.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. the use of statistical quality control techniques is recommended and helpful guidance may be obtained in this respect from IS : 397 ( Part 1 )-1972*.1986 4. 4.2. p&pose of sampling.3 Cement Packing .Every hour. 5.1 For obtaining reliable conclusions. IS : 397 ( Part 2 )-1975t and IS : 397 ( Part 3 )-1~80:. 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. Similarly. soundness. compressive strength and degree of whiteness. a sample taken grinding mill and tested for setting time. 5.from Conveyors 5.1 The samples for ascertaining specification.IS : 3535 . setting time.1.2.1 Sub-Lots . $. *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.For the. 7 .2 Cement Grinding .2.5 When such information cannot be made available or when the purchaser so desires. 4. The frequency of testing for various characteristics shall be according to co1 4 of Table I. that is. The remaining portions of the hourly samples shall be mixed together to give the composite sample for the day. cement be sampled when it is in motion.4. LOT INSPECTION shall be selected and ejtamined for each lot separately their conformity to the requirements of the relevant 5. a sample shall be drawn from the For fineness. 5. a composite sample for a week shall be prepared.One composite sample every day from the packing machine shall be tested for fineness. 4.2. shall be mlxed together to give the composite sample for the week which shall be tested for other characteristics of the specilication.2.4 For effective process control. from conveyors or during loading or unloading. a lot while it is being discharged over a conveyor shall be divided into a number of sub-lots in accordance with Table 2. The remaining portions of the daily samples.2.
2. 5. 5. 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.1. the conveyor may be stopped while the increment is taken.5.2. air-tight containers to avoid moisture absorpIf the increments are placed in cans.1. If it is not possible to take the increment at. if practicable. 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. 8 . they shal! be placed directly in moisture-proof. Moistureproof multiple wall paper bags or plastic bags may be used. 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.2. the cans shall be completely filled and sealed immediately.1 WEIQHTOFTTHELOT ( IN TONNES ) No. tion 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.1 A representative gross sample shall be drawn from each of the sub-lots and shall be kept separately.3. purpose. Thus. The weight of increment shall not be less than 2 kg. TABLE 2 NUMBER OF SUB-LOTS INTO IS TO BE DIVIDED WHICH ) A LOT ( Cfuuses5.2 and5.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 point of discharge.5.2. 5. 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.4.1.2 Gross Sample .18.104.22.168 As increments are taken from the sub-lot. 5. It shall be ensured that the quantity of sample so collected is sufficient for the tests as per 5.0~ &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. there will be as many gross samples as the number of sub-lots into which the lot has been divided.
6 shall apply.7. increments may be obtained by a slotted tube sampler as shown in Fig. If there is more than one opening for charging or discharging. shall apply when loose cement or cement in bulk is If the’cement is supplied in bags.2.3. The material may be drawn in two or three operations. the outer tube being provided with a sharp point to facilitate penetration.1s : 3535 . Where applicable.When the depth of the cement to be sampled does not exceed 2 m.3 manner The increments taken described in 5. in accordance with Table 2. the quantity in the ship’s hold shall he divided into a number of sub-lots upon the weight. The number of increments shall be such that one increment is obtained for every 10 tonnes of the cement or part thereof. 9 . 5.5.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. in accordance with Table 2.1986 5.3. 5. 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.3.1 received This method in wagons.3. the increments shall be taken from each opening. 5. It shall be ensured that the quantity of sample so collected is sufficient for tests as per 5.3 The increments taken manner described in 5. from Wagons from the sub-lot shall be stored in the 5. The division into sub-lots shall be indicated by placing suitable markers on top of the cement.1 Sub-Lots .of the lot.2.5 Sampling 5. Each increment shall weigh at least 2 kg.1 Sllb~Lols . It shall be ensured that the quantity of sample so collected is sufficient for tests as per 5.4.3 Sampling from Bulk Storage ( Silos ) 5. The slotted tube-sampler shall be between 1’5 to 1’8 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.For the purpose of sampling. of cement depending 5.7.For the purpose of sampling.2 Grass Sample .3. a sampling pipe activated by an air jet which is capable of removing cement from different depths may be used. The increment ‘shall weigh at least 2 kg.4 Sampling from Ship’s from Hold the sub-lot shall be stored in the 5. 22.214.171.124 Gross Sample . 5. the quantity of cement in the bulk storage shall be divided into a number of sub-lots depending upon the weight of the lot. for depths of cement greater than 2 m. 5.
2. 5. SLOTTEDTUBE-SAMPLER FOR BULK CEMENT of less It for the 5.IS FRE TO ROTATE INSIDE ENLARGED VIEW OF A SLOT All dimewiona Fro. In to be selected representative sample from a subSample .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.2 from at least six evenly distributed points in each selected wagon.IS : 3535 . the number of bags shall be taken to be equal to the next higher integer.6. at least 2 sampled.3 Gross Sample .1 .FQr drawing percent of the bags subject to a minimum of five shall be case fractional numbers are obtained.3.4. for the sub-lot shall be stored in 5.4 mannez The increments taken described in 5. The material may be drawn in two or three operations.5. shall be ensured that the quantity of sample so collected is sufficient teats as per 5.5.5. ~ll5-+--15O--+-115~+l5O---+ t-225 35-O 00 SLOTS IN BOTH THE TUBE5 X 2.For the purpose of sampling.2 Sub-Lots .24mm THICK BRASS TUBE INNER TUBE. 10 . The sampler shall be taken in the manner described in 5. The sub-lots shall consist of approximately equal number of bags. The sub-lots shall consist of approximately equal number of wagons. 1 in millimetm.6 Sampling from Bags of cement 5&l SuQ.From each selected wagon approximately equal number increments shall be taken and weight of increment shall be not than 2 kg.2 Gross lot. 5.For the purpose of sampling.3. depending upon the weight of the lot. 5.Lots . 1 but about 60 cm in length.7.5. the quantity in the lot shall be divided into a number of sub-lots.1986 5. in accordance with Table 2. 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.
3. the following procedure may be followed: Starting from any bag at random.2 The sampling tube shown in Fig.1 These bags shall be chosen at random from the sub-lot. 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. 5.N being the number of bags in the sub-lot and n the number of bags to be selected. .2.1986 5.2. count the bags in the sub-lot in one order as 1.3.IS : 3535 .7.6.1 Each gross sample shall be reduced separately. up to Y and so on.6.ncrements than 2 kg. The material collected in the gross sample shall be thoroughly mixed. Fro.6. 2.7 Reduction Sample 5. It shall then be passed through 850-micron IS sieve. 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* ).2. 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. from the sub-lot shall be stored in the The increments taken described in 5. of Gross 5. In case such a table as not available.value shall be taken as equal to the integral part of it. 5. breaking the lumps and removing the foreign materials. its . where r = N/n. n 520 -1 All dimensions in millimetres.3 manner 2 TUBE-SAMPLER FOR PACKAGED CEMENT VOLUME 300 cm3 AP~ROX From each selected bag. *Methods for random sampling. In case the value of ‘Y’ comes out to be a fractional number. is sufficient 5.3 i. 11 . The foreign materials and hardened lumps that do not break on sieving or brushing. or three operations.2.7.6. shall be discarded. Every rth bag SO counted shall be removed.
5 The laboratory sample divided into three equal parts. only one test result will be available and that result satisfy the requirements of the specification. 12 been shall . sample shall be used in case of a dispute between the purchaser a&l the supplier.7.8.1 For those characteristics where a composite sample has tested for a lot.8 Number 5.The material shall be scooped into a coneshaped pile.2.2 shall be continued till 11 kg of the material required for the laboratory sample is obtained.3 The reduction of the sample m the manner described in 5.IS : 3535 . another for tLe The reicree supplier and the third to be used as a referee sample.2 Coning and Qtcartering ‘. They shall be labelled with full identification particulars such as supplier’s name. The reduction is’achieved by rejecting any two diagonally opposite quarters. 5. The weight of the composite sample shall be about 21 kg. Then the cone is cut into quarters by two lines which intersect at right angles at the centre of the cone.8. Care shall be taken to drop each scoopful exactly over the same spot as otherwise the central axis of the cone will be slackened. the lot and the sub-lot number.7. the date of sampling.9 Criteria for Conformity 5. 5. etc.1 The of Tests laboratory chemical and physical requirements samples shall be tested are: sulphur content as sulphuric anhydride.1 Sample splitter or riffle samplers of the appropriate tie used for reducing the gross sample mechanically. 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. 5.7. 5.7. Each of these parts shall then be placed in a moisture-nrobf air-tight container to avoid moisture absorption and aeration ofFhe samples.9. After the coneis formed.1986 5. and the composite sample shall be 5.2 A composite sample shall be tested for all the requirements. it shall be flattened by pressing the top of the cone with the smooth surface of the scoop. one fir the purchaser. for which and individual a) Total b) Fineness. size may 5.7.
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.i: .2 When two laboratory samples have been analyzed individually from a lot for any characteristic.1986 5.3. If the value SO obtained is greater than or equal to the minimum limit.9.0.5 R ) shall be calculated rrom the relevant test results. the lot shall be declared as conforming to the requirement of that characteristic.3 When three or more laboratory samples have been analyzed individually from a lot for any characteristic.3. 5.5 R) shall be calculated from the relevant test results.2 If the specification limit for the characteristic is given as a minimum. 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.5 R ) shall be calculated from the relevant test results. the lot shall be considered ‘as conforming to the requirement -for that characteristic only if both of them pass.4 If the characteristic has two-sided specification limits the value of the expression ( . the value of the expression ( Z + 0.3 If the specification limit for the characteristic is given as a mauimum.3. the lot shall be declared as conforming to the requirement of that characteristic.5 R) and ( ? + 0.0. 5. the value of the expression ( 2 . If the values SO obtained lie between the two specification limits. 5. the following procedure shall be followed for judging the conformity to the requirements of that characteristic. 5. 13 .9.1 For laboratory calculated dilikrent samples.ues of the test results.9.3.9. 5.9.9.IS :3535 .
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