SIST EN 13454-2:2004

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Binders, composite binders and factory made mixtures for floor screeds based on calcium sulfate - Part 2: Test methodsVeziva, sestavljena veziva in industrijsko pripravljene mešanice za estrihe na osnovi kalcijevega sulfata – 2. del: Preskusne metodeLiants, liants composites et mélanges fabriqués en usine a base de sulfate de calcium pour chapes de sol - Partie 2: Méthodes d'essaiCalciumsulfat-Binder, Calciumsulfat-Compositbinder und Calciumsulfat-Werkmörtel für Estriche - Teil 2: PrüfverfahrenTa slovenski standard je istoveten z:EN 13454-2:2003SIST EN 13454-2:2004en91.100.50Veziva. Tesnilni materialiBinders. Sealing materials91.100.10Cement. Mavec. Apno. MaltaCement. Gypsum. Lime. MortarICS:SLOVENSKI
STANDARDSIST EN 13454-2:200401-april-2004







EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13454-2December 2003ICS 91.100.10; 91.100.50English versionBinders, composite binders and factory made mixtures for floorscreeds based on calcium sulfate - Part 2: Test methodsLiants, liants composites et mélanges fabriqués en usine àbase de sulfate de calcium pour chapes de sol - Partie 2:Méthodes d'essaiCalciumsulfat-Binder, Calciumsulfat-Compositbinder undCalciumsulfat-Werkmörtel für Estriche - Teil 2:PrüfverfahrenThis European Standard was approved by CEN on 1 September 2003.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and UnitedKingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2003 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 13454-2:2003 E



EN 13454-2:2003 (E)2ContentsPageForeword.31Scope.42Normative references.43Test conditions and sampling.43.1General requirements for testing.43.1.1Water.43.1.2Apparatus.43.2Sampling for binders (CAB, CAC).53.3Sampling for factory made mixtures (CA).54Test methods for binders (CAB ; CAC).54.1Content of calcium sulfate.54.1.1Principle.54.1.2Apparatus.54.1.3Reagents.64.1.4Procedure.64.2Determination of pH.74.3Determination of setting time.74.3.1Principle.74.3.2Apparatus.74.3.3Standard consistence test.74.3.4Procedure.74.3.5Setting time test.84.4Determination of strengths.94.4.1Apparatus.94.4.2Procedure.114.4.3Water demand for flow table value.124.4.4Preparation of test specimens.124.4.5Testing the specimens.134.5Determination of shrinkage and swelling.144.5.1Principle.144.5.2Apparatus.154.5.3Preparation and storage of the specimens.164.5.4Measuring of the specimens.165Test method for factory made mixtures (CA).175.1Determination of pH value.175.2Working time.175.2.1Flowing mixture.175.2.2Stiff mixture.185.3Determination of strength.185.3.1Composition of the test sample.185.3.2Flexural and compressive strength.185.4Determination of shrinkage and swelling.186Test report.18Bibliography.20



EN 13454-2:2003 (E)3ForewordThis document (EN 13454-2:2003) has been prepared by Technical Committee CEN/TC 241 “Gypsum and gypsumbased products”, the secretariat of which is held by AFNOR.This European Standard shall be given the status of a national standard, either by publication of an identical text orby endorsement, at the latest by June 2004, and conflicting national standards shall be withdrawn at the latest byJune 2004.No existing European Standard is superseded.The European Standard EN 13454 for binders, composite binders and factory made mixtures for floor screedsbased on calcium sulfate consists of two parts:Part 1: Definitions and requirementsPart 2: Test methodsThe requirements in prEN 13454-1 are based on the results of tests according to EN 13454-2 on binders,composite binders and factory made mixtures for floor screeds based on calcium sulfate.This European Standard describes test methods for binders, composite binders and factory made mixtures wherethe principal active component is calcium sulfate.According to the CEN/CENELEC Internal Regulations, the national standards organizations of the followingcountries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal,Slovakia, Spain, Sweden, Switzerland and the United Kingdom.



EN 13454-2:2003 (E)41 ScopeThis European Standard describes the test methods for binders and composite binders for floor screeds based oncalcium sulfate specified in prEN 13454-1.This European Standard describes the test methods for factory made mixtures for floor screeds based on calciumsulfate specified in EN 13813.This European Standard describes reference test methods. If other than these methods and conditions are used, itis necessary to show that they give results equivalent to those given by the reference methods. In the event of adispute, only the reference test method is used.2 Normative referencesThis European Standard incorporates by dated or undated reference, provisions from other publications. Thesenormative references are cited at the appropriate places in the text and the publications are listed hereafter. Fordated references, subsequent amendments to or revisions of any of these publications apply to this EuropeanStandard only when incorporated in it by amendment or revision. For undated references the latest edition of thepublication referred to applies (including amendments).EN 196-1:1994, Methods of testing cement – Part 1 : Determination of strength.EN 196-3:1994, Methods of testing cement – Part3 : Determination of setting time and soundness.EN 196-7:1989, Methods of testing cement – Part 7: Methods of taking and preparing samples of cement.EN 459-2:2001, Building lime – Part 2 : Test methods.EN 13813, Screed material and floor screeds - Screed material - Properties and requirements.EN 13892-1, Methods of test for screed materials - Part 1: Sampling, making and curing specimens for test.3 Test conditions and sampling3.1 General requirements for testing3.1.1 WaterThe water used for testing and chemical analyses shall be distilled or deionised.Unless otherwise specified, the water temperature shall be the same as the air temperature in the laboratory.3.1.2 ApparatusThe apparatus used for gauging and the moulds used for preparing the test specimens, shall be free from leaksand shall be manufactured from a water proof material which is non reactive to calcium sulfate (e.g. glass, brass,stainless steel, hardened steel, hard rubber and plastics etc.).Since the characteristics of calcium sulfate are strongly influenced by the presence of particles of calcium sulfatedihydrate which can influence the setting time, all equipment used in the tests shall be kept in a perfect state ofcleanliness.



EN 13454-2:2003 (E)53.2 Sampling for binders (CAB, CAC)Sampling for binders shall be carried out in accordance with EN 196-7 and EN 459-2.3.3 Sampling for factory made mixtures (CA)Sampling for factory made mixtures shall be carried out in accordance with EN 13892-1.The composition ofsamples shall always be representative of the average composition of the material, the possibility of segregationbeing taken into consideration. The test report shall state whether the samples taken are spot samples orcomposite samples (See 3.6 and 3.7 of EN 196-7:1989).Samples which are likely to change in air shall be placed in airtight containers, such as cans, immediately after theyhave been taken.Wherever possible tests shall be carried out on specimens prepared immediately after obtaining the sample, ifnecessary on site. Specimens shall be prepared during working time but not later than 2 h after gauging. Thisperiod shall also be observed when fresh samples are supplied to a testing centre, and may be appropriatelydecreased or increased for samples containing accelerators or retarders.If transportation of fresh samples cannot be avoided, they shall be supplied immediately for testing, accompaniedby a certificate stating which tests are to be carried out, and protected from changes, such as loss of water, entry ofwater etc., as may occur during transportation. Specimens shall be prepared immediately on receipt of the sample,after the sample has been mixed again manually.Specimens shall be prepared within the working time after gauging. For this reason, they shall as a rule (e.g. whenprepared in situ) be stored under vibration-free conditions and protected from climatic effects (e.g. frigobox etc.) forat least 24 h before they are conveyed in the moulds for testing. If special requirements in respect of thepreparation and storage of the particular sample are specified for the tests envisaged these shall be observed.4 Test methods for binders (CAB ; CAC)4.1 Content of calcium sulfate4.1.1 PrincipleThe calcium sulfate is decomposed by digestion with hydrochloric acid solution. Insoluble impurities are removedby filtration. The sulfate in the filtrate is determined gravimetrically as barium sulfate.4.1.2 Apparatusa) Sieve 0,1 mm mesh.b) 600 ml and 800 ml beakers.c) Rapid filtration funnels.d) Muffle furnace.e) Ignition crucible, porosity 4.f) Filter paper capable of retaining particles greater than 2,5 µm.g) Porous porcelain or silica crucible.



EN 13454-2:2003 (E)64.1.3 Reagentsa) Hydrochloric acid solution :2 N ;b) Ammonia solution :(50 % by volume)c) Barium chloride :(3 % by mass solution in water)d) Methyl orange or other suitable indicator.4.1.4 ProcedureGrind the dried sample until it passes completely through a sieve with a mesh of 0,1 mm. Weigh accurately about0,5 g into a 600 ml beaker, add 25 ml of hot distilled water.Mix the sample and water with a glass rod until all the lumps are dispersed. Add 25 ml of 2 N HCl. Bring to the boiland maintain this for 10 min. Add 150 ml of hot water and allow to boil for 15 min. Remove the beaker from theheat and filter through the filter paper into an 800 ml beaker. Wash out the beaker and filter paper using hot distilledor deionised water until the filtrate is free of chloride.Make up to approximately 350 ml using distilled water. Add a few drops of indicator and neutralise with ammoniasolution. Add 20 ml 2 N HCl. Bring to the boil again and add 50 ml of hot barium chloride solution stirring vigorouslyduring the addition. Bring to the boil and allow to settle just below boiling for at least 30 min.Filter by one of the following methods :a) Filtration using filter crucibles.Ignite a clean ignition crucible, porosity 4, or a porous porcelain filter crucible at (800 ± 25) °C for 10 min.Cool in a desiccator to room temperature and weigh.Decant the clear liquid through the crucible using a slight suction. Wash the precipitate 3 times by decantation withhot water, transfer to the crucible and wash 6 times with small quantities of hot water. The last wash should bechloride free. Dry the crucible and contents and ignite at (800 ± 25) °C for 10 min.b) Filtration using filter paper.Use filter paper as described. Decant the clear liquid through the filter paper. Wash the precipitate 3 times bydecantation with hot water, transfer to the filter paper and wash with small quantities of hot water until the wash ischloride free.After filtration and washing fold the paper around the precipitate and place it in a weighed porcelain or silicacrucible, previously ignited at (800 ± 25) °C and cooled in a desiccator. Heat gently to char the paper and expel thevolatile matter. Do not allow the paper to burst into flames. Raise the temperature slowly to burn off the carbon withfree access of air.Finally ignite for 10 min at (800 ± 25) °C. Cool in a desiccator and weigh. Calculate the CaSO4 content as apercentage from the equation :[CaSO4] = W2 x 58,33 / W1(1)whereW1 is the mass of sample, in grams ;W2 is the mass of precipitate, in grams.



EN 13454-2:2003 (E)74.2 Determination of pHDisperse 1 part by mass of the pulverised sample in 10 parts by mass of deionized or distilled water. Stir it for 5 minand then measure the pH by a pH-meter or pH-paper to the nearest ± 0,5 pH.4.3 Determination of setting time4.3.1 PrincipleDetermine setting time using the method given in EN 196-3, "binder" being substituted, where "cement" ismentioned.The setting time is determined by observing the penetration of a needle into a binder paste of standard consistenceaccording to clause 5 of EN 196-3:1994 until it reaches a specified value.Binder paste of standard consistency has a specified resistance to penetration by a standard plunger. The waterrequired for such a paste is determined by trial penetrations of pastes with different water contents.4.3.2 Apparatusa) Mixer : As described in 4.4 of EN 196-1:1994.b) Vicat penetration apparatus : As described in 5.1 of EN 196-3:1994.4.3.3 Standard consistence testUse the Vicat apparatus as shown in Figure 1(a) and 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 trulyvertical 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 truncatedconical 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 largerthan the mould and at least 2,5 mm thick.NOTEMoulds of metal or plastics or of cylindrical form may be used provided that they are of the specified depth and thatthey can be shown to give the same test results as the specified hard rubber mould of truncated conical form.4.3.4 Procedure4.3.4.1 Mixing the binder pasteWeigh, to the nearest 1 g, 500 g of binder. Weigh a quantity of water, e.g. 125 g, in the mixer bowl or measure thewater from the graduated cylinder or burette into the mixer bowl. Possible admixture should already be diluted inwater.Add the binder carefully to the water in order to avoid loss of water or binder. The time of addition shall not be lessthan 5 s nor more than 10 s. Note the time of completion of the addition as zero time from which latermeasurements of time shall be made. Start the mixer immediately and run at low speed for 90 s.Stop the machine after 90 s for 15 s during which remove with a suitable scraper any paste adhering to the bowloutside the mixing zone and return it to the mix. Restart the machine and run at low speed for a further 90 s. Thetotal mixer running time shall be 3 min.NOTEAny other mixing method, whether by machine or hand, may be used provided that it can be shown to give thesame test results as the specified method.



EN 13454-2:2003 (E)84.3.4.2 Filling the mould and carrying out the testTransfer the paste after mixing immediately to the mould, which has previously been placed on a lightly greasedplan glass base plate, and fill it to excess without undue compaction or vibration. Remove the excess by a gentlesawing motion with a straight-edged implement in such a way as to leave the paste filling the mould and having asmooth upper surface.Adjust the Vicat apparatus with the plunger (Figure 1c) attached in advance of the test, by lowering the plunger torest on the baseplate to be used and adjusting the pointer to read zero on the scale. Raise the plunger to thestand-by position.Immediately after levelling the paste, transfer the mould and baseplate to the Vicat apparatus and position itcentrally under the plunger. Lower the plunger gently until it is in contact with the paste. Pause in that position forbetween 1 s and 2 s in order to avoid initial velocity or forced acceleration of the moving parts. Then release themoving parts quickly and allow the plunger to penetrate vertically into the centre of the paste. The release of theplunger shall occur 4 min after zero time. Read the scale when penetration has ceased or 30 s after the release ofthe plunger, whichever is the earlier.Record the scale reading, which indicates the distance between the bottom face of the plunger and the baseplate,together with the water content of the paste expressed as a percentage by mass of the binder. Clean the plungerimmediately after each penetration.Repeat the test with pastes containing different water contents until one is found to produce a distance betweenplunger and baseplate of (6 ± 3) mm. Record the water content of that paste to the nearest 0,5 % as the water forstandard consistency.4.3.5 Setting time test4.3.5.1 Determination of initial setting timeRemove the plunger and replace it by the needle (Figure 1 (d)) which shall be of steel and in the form of a rightcylinder 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 withthat of the needle.Adjust the Vicat apparatus with the needle (Figure 1d), attached in advance of the test, by lowering the needle torest on the baseplate 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 consistency and level it, in accordance with 4.3.4.1 and 4.3.4.2.Place the filled mould and baseplate in the room and, after a suitable time, transfer to the Vicat apparatus andposition under the needle. Lower the needle gently until it is in contact with the paste. Pause in that position forbetween 1 s and 2 s in order to avoid initial velocity or forced acceleration of the moving parts. Then release themoving parts quickly and allow the needle to penetrate vertically into the paste. Read the scale when penetrationhas 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 the baseplate, togetherwith the time from zero. Repeat the penetration test on the same specimen at conveniently spaced positions, notless than 10 mm from the rim of the mould or from each other, at conveniently spaced intervals of time, e.g. at10 min intervals. Between penetration tests keep the specimen in a room. Clean the Vicat needle immediately aftereach penetration.Record the time measured from zero at which the distance between the needle and the baseplate is (6 ± 3) mm asthe initial setting time of the binder to the nearest 5 min. The required accuracy may be assured by reducing thetime interval between penetration tests near the end point and observing that successive results do not fluctuateexcessively.



EN 13454-2:2003 (E)94.3.5.2 Determination of final setting timeInvert the filled mould used in 4.3.4 on its baseplate so that the tests for final set are made on the face of thespecimen originally in contact with the baseplate. Fit the needle with a ring attachment (Figure 1 (e)) to facilitateaccurate observation of small penetrations. Use the procedure described in 4.3.4. The intervals of time betweenpenetration tests may be increased to e.g. 30 min.Record, to the nearest 15 min, the time measured from zero at which the needle first penetrates only 0,5 mm intothe specimen as the final setting time of the binder. This time is that which the ring attachment first fails to mark thespecimen and may be accurately established by reducing the time interval between tests near the end point andobserving that successive test results do not fluctuate excessively.NOTEAutomatic setting time machines are commercially available and may be used provided that they can be shown togive the same test results as the specified apparatus and procedure.4.4 Determination of strengthsDetermine the flexural and the compressive strength in accordance with EN 196-1, "binder" being substituted,where "cement" is mentioned.4.4.1 Apparatusa) Mixer : As described in 4.4 of EN 196-1:1994.b) Moulds with base : As described in 4.5 of EN 196-1:1994 for material see 3.1.3.c) Vibrating table : As described in 5.1.2.2.1 of EN 459-2:2001.d) Flexural strength, testing machine : As described in 4.7, 4.8, 4.9 of EN 196-1:1994.e) Compressive strength, testing machine : As described in clause 9 of EN 196-1:1994.f) Flow table, mould, cam and tamper : As described in 5.5.2.1.2 of EN 459-2:2001



EN 13454-2:2003 (E)10Dimensions in millimetresa) Side view with mould in upright positionfor initial setting time determinationb) Front view with mould inverted for finalsetting time determinationc) plunger for standard consistencyd) needle for initial teste) needle and attachment for final testKey1hard rubber mould2platform for correcting weights3basis plate4test container5water6air vent (diameter 1,5 mm)NOTEThe specified dimensions should be observed. If the plunger, needle and needle with attachment are all adjusted tohave the same mass, e.g. (9 ± 0,5) g, one correcting weight is sufficient for each apparatus.Figure 1 — Vicat apparatus for determination of the standard consistency and setting time



EN 13454-2:2003 (E)114.4.2 Procedure4.4.2.1 Preparation of sampleBinder (including possible admixtures), sand, water and apparatus shall be at the laboratory temperature. Carry outweighing by means of a balance accurate to ± 1 g.The composition of the test sample is 675 g binder, 1 350 g standard sand according to 5.1 of EN 196-1:1994 andthe necessary amount of water. The amount of water shall be such that a flow diameter of (150 ± 5) mm accordingto 5.5.2.3.2 of EN 459-2:2001, is achieved, but shall not fall below a minimum amount of 225 ml. Possibleadmixture shall already be diluted in water.Mix each batch of sample in accordance with 6.3 of EN 196-1:1994 mechanically using the mixer. With the mixer inthe operating position :a) pour the water into the bowl and add the binder (possible admixtures shall already have been diluted in thewater) ;b) then start the mixer immediately at the low speed and, after 30 s, add the sand steadily during the next 30 s.When separate sand fractions are used, add the required quantities of each fraction in succession starting withthe coarsest. Switch the mixer to the higher speed and continue the mixing for an additional 30 s ;c) stop the mixer for 1 min 30 s. During the first 15 s, remove by means of rubber scraper all the paste adheringto the wall and bottom part of the bowl and place in the middle of the bowl ;d) continue the mixing at the higher speed for 60 s.The timing of the various mixing stages shall be adhered to within ± 1 s.4.4.2.2 Determination of flow diameter4.4.2.2.1 PrincipleThe flow diameter is determined by measuring the diameter of a pat of binder sample after it has been subjected tojolting in the manner described in 4.4.2.2.2.4.4.2.2.2 Flow diameterIf the flow table has not been used during the hour prior to the test, jolt the empty table several times. There shallbe neither fluid nor dirt between the bearing (6), and the boss (8) according to Figure 7 of EN 459-2:2001.In order to determine the flow diameter, place the mould in the centre of the clean, dry surface of the flow table. Fillit with two layers of the sample (prepared just before in accordance with 4.4.2.1). During this operation hold themould with the mounted hopper firmly onto the plate with one hand in such a way that its edge coincides with thecircle engraved on the plate. Spread each layer of the sample by tamping it lightly ten times with the tamper so thatthe mould is filled to its circumference.Strike off excess sample, clean the flow table and remove any water in the proximity of the mould. After 10 s to 15 shave elapsed, lift the mould slowly a
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