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BRITISH STANDARD BS EN196-3:1995

Methods of testing cement —

Part 3: Determination of setting time and soundness

The European Standard EN 196-3:1994 has the status of aBritish Standard

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BS EN 196-3:1995

This British Standard, having been prepared under the direction of the Technical Committee B/516, was published under the authority of the Standards Board and comes into effect on15 March 1995

© BSI 01-1999

The following BSI references relate to the work on this standard:Committee reference B/516 Special announcement inBSI News December 1992

ISBN 0 580 21519 9

Cooperating organizations

The European Committee for Standardization (CEN), under whose supervision this European Standard was prepared, comprises the national standards organizations of the following countries:

Austria Oesterreichisches NormungsinstitutBelgium Institut belge de normalisationDenmark Dansk StandardFinland Suomen Standardisoimisliito, r.y.France Association française de normalisationGermany Deutsches Institut für Normung e.V.Greece Hellenic Organization for StandardizationIceland Technological Institute of IcelandIreland National Standards Authority of IrelandItaly Ente Nazionale Italiano di UnificazioneLuxembourg Inspection du Travail et des MinesNetherlands Nederlands Normalisatie-instituutNorway Norges StandardiseringsforbundPortugal Instituto Portuguès da QualidadeSpain Asociación Española de Normalización y CertificaciónSweden Standardiseringskommissionen i SverigeSwitzerland Association suisse de normalisationUnited Kingdom British Standards Institution

Amendments issued since publication

Amd. No. Date Comments

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BS EN 196-3:1995

© BSI 01-1999 i

Contents

PageCooperating organizations Inside front coverNational foreword ii

Foreword 2Text of EN 196-3 3

National annex NA (informative) Determination ofstandard consistence Inside back coverNational annex NB (informative) Committees responsible Inside back coverNational annex NC (informative) Cross-references Inside back cover

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BS EN 196-3:1995

ii © BSI 01-1999

National foreword

This British Standard has been prepared under the direction of Technical Committee B/516, Cement and lime. It is the English language versionof EN 196-3:1994 Methods of testing cement — Part 3: Determination of setting time and soundness published by the European Committee for Standardization (CEN). EN 196-3 was drawn up by CEN Technical Committee 51, Cement and building limes, as Part 3 of a series on testing cement which was originally accepted by CEN on 15 November 1985 and made available on 12 May 1987. The UK gave a negative vote at the final voting stage and, under the CEN Rules then in force, was not obliged to implement this Part. A second formal vote was taken in November 1992 when the UK again gave a negative vote but, under the CEN Rules now in force, is obliged to implement this Part. This British Standard supersedes BS 4550-3.5:1978, BS 4550-3.6:1978 and BS 4550-3.7:1978 which are withdrawn.The methods described in this standard retain the use of the familiar Vicat and le Chatelier apparatus. The UK negative votes on this Part were due to the fact that the draft European Standard contained certain errors, some of which remain in the 1994 text, e.g. the minimum laboratory relative humidity in 4.1 should be 50 % to accord with EN 196-1. Furthermore, the requirement in 7.1.3 for a minimum relative humidity of 98 % is inappropriate as values at this level can neither be measured nor controlled with any precision. The lengths of the standard consistence plunger and of the setting time needles are not critical where the Vicat apparatus is calibrated in advance of the test (see 5.2.3 and 6.2). However, for convenience in use, they should be of the same length within ± 1 mm. Hence, in the typical illustrations shown in Figure 1, the needle lengths in (d) and (e) should be shown to the upper shoulder of the cone.The Vicat mould is specified in 5.1 to be of hard rubber but “moulds of metal may be used provided that .... they can be shown to give the same test results”. Such data are available in the UK enabling metal moulds to be used.In the test for standard consistence, 5.2.3 requires repeat tests “with pastes containing different water contents until one is found to produce a distance between plunger and base-plate of (6 ± 1) mm”. The UK procedure for meeting this requirement is given in national annex NA.BS 4550-3.7:1978 included a soundness test for supersulfated cement, based on immersion in cold water, which does not appear in EN 196-3. This procedure is being retained in an appendix to BS 4248:1974.A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application.

Compliance with a British Standard does not of itself confer immunity from legal obligations.

Summary of pagesThis document comprises a front cover, an inside front cover, pages i and ii, the EN title page, pages 2 to 8, an inside back cover and a back cover.This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.

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EUROPEAN STANDARD

NORME EUROPÉENNE

EUROPÄISCHE NORM

EN 196-3

December 1994

ICS 91.100.10 Supersedes EN 196-3:1987

Descriptors: Cements, tests, determination, setting time, consistence, stability

English version

Methods of testing cement —Part 3: Determination of setting time and soundness

Méthodes d’essai des ciments —Partie 3: Détermination du temps de prise etde la stabilité

Prüfverfahren für Zement —Teil 3: Bestimmung der Erstarrungszeiten und der Raumbeständigkeit

This European Standard was approved by CEN on 1994-12-12. CEN membersare bound to comply with the CEN/CENELEC Internal Regulations whichstipulate the conditions for giving this European Standard the status of anational standard without any alteration.Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to anyCEN member.This European Standard exists in three official versions (English, French,German). A version in any other language made by translation under theresponsibility of a CEN member into its own language and notified to theCentral Secretariat has the same status as the official versions.CEN members are the national standards bodies of Austria, Belgium,Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy,Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland andUnited Kingdom.

CENEuropean Committee for Standardization

Comité Européen de NormalisationEuropäisches Komitee für Normung

Central Secretariat: rue de Stassart 36, B-1050 Brussels

© 1994 Copyright reserved to CEN membersRef. No. EN 196-3:1994 E

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EN 196-3:1994

2 © BSI 01-1999

Foreword

This European Standard was drawn up by Technical Committee CEN/TC 51, Cement and building limes, of which the secretariat is held by IBN.The European Standard on the methods of testing cement comprises the following Parts:EN 196-1, Methods of testing cement — Part 1: Determination of strength.EN 196-2, Methods of testing cement — Part 2: Chemical analysis of cement.EN 196-3, Methods of testing cement — Part 3: Determination of setting time and soundness.ENV 196-4, Methods of testing cement — Part 4: Quantitative determination of constituents.EN 196-5, Methods of testing cement — Part 5: Pozzolanicity test for pozzolanic cements.EN 196-6, Methods of testing cement — Part 6: Determination of fineness.EN 196-7, Methods of testing cement — Part 7: Methods of taking and preparing samples of cement.EN 196-21, Methods of testing cement — Part 21: Determination of chloride, carbon dioxide and alkali content of cement.This European Standard shall be given the status of a National Standard, either by publication of an identical text or by endorsement, at the latest by June 1995, and conflicting national standards shall be withdrawn at the latest by June 1995.This European standard supersedes EN 196-3:1987.According to the CEN/CENELEC Internal Regulations, the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland, United Kingdom.

Contents

PageForeword 21 Scope 32 Normative references 33 Test principles 34 General requirements for testing 35 Standard consistence test 36 Setting time test 67 Soundness test 7Figure 1 — Vicat apparatus fordetermining the standard consistenceand setting time of cement 4Figure 2 — Le Chatelier apparatus for the determination of soundness of cements 8

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EN 196-3:1994

© BSI 01-1999 3

1 ScopeThis European Standard describes the methods for determining setting time and soundness of cements.It is applicable to all cements covered by ENV 197-1.This standard describes the reference procedure; it allows the use of alternative procedures as indicated in notes provided that they do not affect the results significantly. In the event of a dispute, only the reference procedure described in this standard shall be used, excluding any alternatives.

2 Normative referencesThis European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references, the latest edition of the publication referred to applies.EN 196-1, Methods of testing cement — Part 1: Determination of strength.ENV 197-1, Cement — Composition, specifications and conformity criteria — Part 1: Common cements.

3 Test principlesThe setting time is determined by observing the penetration of a needle into cement paste of standard consistence until it reaches a specified value.The soundness is determined by observing the volume expansion of cement paste of standard consistence as indicated by the relative movement of two needles.Cement paste of standard consistence has a specified resistance to penetration by a standard plunger. The water required for such a paste is determined by trial penetrations of pastes with different water contents.

4 General requirements for testing4.1 Laboratory

The laboratory in which specimens are prepared and tested shall be maintained at a temperature of (20 ± 2) °C and a relative humidity of not less than 65 %.

4.2 Apparatus

4.2.1 Balance, capable of weighing to the nearest 1 g.

4.2.2 Graduated cylinder or burette, capable of measuring to the nearest 1 % of the volume measured.4.2.3 Mixer, conforming to EN 196-1.

4.3 Materials

4.3.1 Distilled or deionized water shall be used for making, storing and boiling specimens.NOTE Other water may be used provided that it can be shown to give the same test results.

4.3.2 Cement, water and apparatus used to make and test specimens shall be at a temperature of (20 ± 2) °C.

5 Standard consistence test5.1 Apparatus

Use the Vicat apparatus as shown in Figure 1(a) and Figure 1(b) with the plunger shown in Figure 1(c). The plunger [Figure 1(c)] shall be of non-corrodible metal in the form of a right cylinder of (50 ± 1) mm effective length and of (10,00 ± 0,05) mm diameter. The total mass of moving parts shall be (300 ± 1) g. Their movement shall be truly vertical and without appreciable friction, and their axis shall coincide with that of the plunger.The Vicat mould [see Figure 1(a)] to contain the paste under test shall be of hard rubber. It shall be of truncated conical form (40,0 ± 0,2) mm deep and shall have internal diameters at top and bottom of (70 ± 5) mm and (80 ± 5) mm respectively. It shall be adequately rigid and shall be provided with a plane glass base-plate larger than the mould and at least 2,5 mm thick.NOTE Moulds of metal or plastics or of cylindrical form may be used provided that they are of the specified depth and that they can be shown to give the same test results as the specified hard rubber mould of truncated conical form.

5.2 Procedure

5.2.1 Mixing the cement paste

Weigh, to the nearest 1 g, 500 g of cement. Weigh a quantity of water, e.g. 125 g, in the mixer bowl or measure the water from the graduated cylinder or burette and place it into the mixer bowl.Add the cement carefully to the water in order to avoid loss of water or cement. The time of addition shall be not less than 5 s nor more than 10 s. Note the time of completion of the addition as zero time from which later measurements of time shall be made. Start the mixer immediately and run at low speed for 90 s.

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EN 196-3:1994

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NOTE The specified dimensions have to be observed. If the plunger, needle and needle with attachment are all adjusted to have the same mass, e.g. (9 ± 0,5) g, one correcting weight is sufficient for each apparatus.

Figure 1 — Vicat apparatus for determining the standard consistenceand setting time of cement

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EN 196-3:1994

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Stop the machine after 90 s for 15 s during which remove with a suitable scraper any paste adhering to the bowl outside the mixing zone and return it to the mix. Restart the machine and run at low speed for a further 90 s. The total mixer running time shall be 3 min.NOTE Any other mixing method, whether by machine or hand, may be used provided that it can be shown to give the same test results as the specified method.

5.2.2 Filling the mould

Transfer the paste immediately to the mould, which has previously been placed on a lightly greased plane glass base-plate, and fill it to excess without undue compaction or vibration. Remove the excess by a gentle sawing motion with a straight-edged implement in such a way as to leave the paste filling the mould and having a smooth upper surface.

5.2.3 Penetration test

Calibrate the Vicat apparatus with the plunger [Figure 1(c)], attached in advance of the test, by lowering the plunger to rest on the base-plate to be used and adjusting the pointer to read zero on the scale. Raise the plunger to the stand-by position.

Immediately after levelling the paste, transfer the mould and base-plate to the Vicat apparatus and position it centrally under the plunger. Lower the plunger gently until it is in contact with the paste. Pause in that position for between 1 s and 2 s in order to avoid initial velocity or forced acceleration of the moving parts. Then release the moving parts quickly and allow the plunger to penetrate vertically into the centre of the paste. The release of the plunger shall occur 4 min after zero time. Read the scale when penetration has ceased or 30 s after the release of the plunger, whichever is the earlier.Record the scale reading, which indicates the distance between the bottom face of the plunger and the base-plate, together with the water content of the paste expressed as a percentage by mass of the cement. Clean the plunger immediately after each penetration.Repeat the test with pastes containing different water contents until one is found to produce a distance between plunger and base-plateof (6 ± 1) mm. Record the water content of that paste to the nearest 0,5 % as the water for standard consistence.

NOTE The specified dimensions have to observed. If the plunger, needle and needle with attachment are all adjusted to have the same mass, e.g. (9 ± 0,5) g, one correcting weight is sufficient for each apparatus.

Figure 1 — Vicat apparatus for determining the standard consistenceand setting time of cement (concluded)

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EN 196-3:1994

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6 Setting time test6.1 Apparatus

6.1.1 Room or humidity cabinet

A room or a humidity cabinet of adequate size and maintained at (20 ± 1) °C and not less than 90 % relative humidity.NOTE Provided that it can be shown to give the same test results, a water-bath capable of maintaining filled moulds in water at (20 ± 1) °C may be used.

6.1.2 Vicat apparatus for initial set

Remove the plunger and replace it by the needle [Figure 1(d)] which shall be of steel and in the form of a right cylinder of effective length (50 ± 1) mm and diameter (1,13 ± 0,05) mm. The total mass of moving parts shall be (300 ± 1) g. Their movement shall be truly vertical and without appreciable friction, and their axis shall coincide with that of the needle.NOTE Automatic setting time machines are commercially available and may be used provided that they can be shown to give the same test results as the specified apparatus and procedure.

6.2 Determination of initial setting time

Calibrate the Vicat apparatus with the needle [Figure 1(d)], attached in advance of the test, by lowering the needle to rest on the base-plate to be used and adjusting the pointer to read zero on the scale. Raise the needle to the stand-by position.Fill a Vicat mould with paste of standard consistence and level it, in accordance with 5.2.1 and 5.2.2.Place the filled mould and base-plate in the room or humidity cabinet specified in 6.1.1 and, after a suitable time, transfer to the Vicat apparatus and position under the needle. Lower the needle gently until it is in contact with the paste. Pause in that position for between 1 s and 2 s in order to avoid initial velocity or forced acceleration of the moving parts. Then release the moving parts quickly and allow the needle to penetrate vertically into the paste. Read the scale when penetration has ceased, or 30 s after the release of the needle, whichever is the earlier.

Record the scale reading, which indicates the distance between the end of the needle and thebase-plate, together with the time from zero. Repeat the penetration test on the same specimen at conveniently spaced positions, not less than 10 mm from the rim of the mould or from each other, at conveniently spaced intervals of time, e.g. at 10 min intervals. Between penetration tests keep the specimen in a room or humidity cabinet as specified in 6.1.1. Clean the Vicat needle immediately after each penetration. Record the time measured from zero at which the distance between the needle and the base-plate is (4 ± 1) mm as the initial setting time of the cement to the nearest 5 min. The required accuracy may be assured by reducing the time interval between penetration tests near the end-point and observing that successive results do not fluctuate excessively.

6.3 Determination of final setting time

Invert the filled mould used in 6.2 on its base-plate so that the tests for final set are made on the face of the specimen originally in contact with thebase-plate. Fit the needle with a ring attachment [Figure 1(e)] to facilitate accurate observation of small penetrations. Use the procedure described in 6.2. The intervals of time between penetration tests may be increased to e.g. 30 min.Between penetration tests keep the specimen in a room or humidity cabinet as specified in 6.1.1. Clean the Vicat needle immediately after each penetration.Record, to the nearest 15 min, the time measured from zero at which the needle first penetrates only 0,5 mm into the specimen as the final setting time of the cement. This time is that at which the ring attachment first fails to mark the specimen and may be accurately established by reducing the time interval between tests near the end-point and observing that successive test results do not fluctuate excessively.

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EN 196-3:1994

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7 Soundness test7.1 Apparatus

7.1.1 Le Chatelier apparatus. The mould shall be of spring brass with indicator needles and shall have the dimensions shown in Figure 2(a). The resilience of the mould shall be such that the action of a mass of 300 g applied as shown in Figure 2(c) shall increase the distance between the indicator ends of the needles by (17,5 ± 2,5) mm without permanent deformation.A pair of plane glass base and cover plates shall be provided for each mould. Each plate shall be larger than the mould. The cover plate shall weigh at least 75 g; an additional small mass may be placed on a thin plate to satisfy this requirement.7.1.2 Water-bath, with means of heating, capable of containing immersed Le Chatelier specimens and of raising the temperature of the water from (20 ± 2) °C to boiling in (30 ± 5) min.7.1.3 Humidity cabinet, of adequate size and maintained at (20 ± 1) °C and not less than 98 % relative humidity.

7.2 Procedure

Carry out the test simultaneously on two specimens from the same batch of cement paste.Prepare a cement paste of standard consistence. Place a lightly oiled Le Chatelier mould on the lightly oiled base-plate and fill it immediately without undue compaction or vibration using only the hands and a straight-edged implement, if desired, to level the top surface. During filling, prevent, the split in the mould from accidentally opening e.g. by gentle pressure with the fingers or by tying or by use of a suitable rubber band.Cover the mould with the lightly oiled cover plate, add the additional mass, if necessary, and then immediately place the complete apparatus in the humidity cabinet. Maintain it for (24 ± 0,5) h at (20 ± 1) °C and not less than 98 % relative humidity.NOTE 1 Provided that it can be shown to give the same test results, the mould may be placed, between its glass plates, with the additional mass, if necessary, in a water-bath and maintained under water for (24 ± 0,5) h at (20 ± 1) °C.

At the end of the (24 ± 0,5) h period measure the distance (A) between the indicator points to the nearest 0,5 mm. Then heat the mould gradually to boiling during (30 ± 5) min and maintain thewater-bath at boiling temperature for 3 h ± 5 min.NOTE 2 Where it can be shown that the expansion after a shorter boiling period is the same as that after 3 h, such a shorter period may be used.

At the end of the boiling period the distance (B) between the indicator points may be measured to the nearest 0,5 mm.Allow the mould to cool to (20 ± 2) °C. Measure the distance (C) between the indicator points to the nearest 0,5 mm.For each specimen, record the measurements A and C and calculate the difference C – A.Calculate the mean of the two values of C – A to the nearest 0,5 mm.

7.3 Interpretation

The main purpose of the soundness test is to assess the possible risk of late expansion due to hydration of uncombined calcium oxide and/or magnesium oxide. For this purpose report the mean difference C – A.NOTE Where it can be shown that the conditions of the test lead to no significant difference between measurements B and C, the difference B – A may be reported since this reduces the time needed for the test.

7.4 Retest

Should the fresh cement fail to comply with the specified soundness requirement it may be retested after storage. For this purpose, spread out the cement in a layer of 7 cm thickness and store it for 7 days in an atmosphere maintained at (20 ± 2) °C and not less than 65 % relative humidity. Then retest the cement according to 7.2.

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EN 196-3:1994

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Figure 2 — Le Chatelier apparatus for the determination of soundness of cements

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BS EN 196-3:1995

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National annex NA (informative)Determination of standard consistenceIn order to meet the requirement of 5.2.3 to find a paste which produces a distance between plunger and base-plate of (6 ± 1) mm, the following procedure should be adopted.Follow the procedure in 5.2 using a paste consisting of 500 g of the cement and a selected. quantity of water, e.g. 125 g. If this gives a distance from the base-plate of (6 ± 1) mm record the water content of this paste to the nearest 0.5 % as the water for standard consistence.If the first paste gives a distance from the base-plate outside the range (6 ± 1) mm, prepare another paste with a greater or smaller quantity of water as appropriate. If this gives a distance from the base-plate of (6 ± 1) mm record the water content of this second paste to the nearest 0.5 % as the water for standard consistence.If this second paste gives a distance from the base-plate outside the range of (6 ± 1) mm, prepare a third paste with a greater or smaller quantity of water as appropriate. If this gives a distance from the base-plate of (6 ± 1) mm record the water content of this third paste to the nearest 0.5 % as the water for standard consistence.If this third paste gives a distance from the base-plate outside the range of (6 ± 1) mm, interpolate, from the three readings already obtained (providing at least one lies at each end of the range of (6 ± 1) mm), the water content required for a distance from the base-plate of 6 mm and record this value to the nearest 0,5 % as the water for standard consistence.NOTE Any test in which the plunger fails to penetrate the paste, or penetrates the paste to rest on the base-plate, should be ignored.

National annex NB (informative)Committees responsibleThe United Kingdom participation in the preparation of this European Standard was entrusted by Technical Committee B/516 Cement and lime, to Subcommittee B/516/4, upon which the following bodies were represented:

British Cement AssociationBritish Civil Engineering Test Equipment Manufacturers’ AssociationBritish Ready Mixed Concrete AssociationCementitious Slag Makers’ AssociationDepartment of the Environment (Building Research Establishment)Electricity AssociationQuality Ash AssociationSociety of Chemical Industry

National annex NC (informative)Cross-referencesThe British Standards corresponding to the European Standards referred to in the text are identical in number and title with those given in clause 2.

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