SIST EN 13454-2:2004+A1:2007

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 13454-2:2003+A1:2007SIST EN 13454-2:2004+A1:2007en,fr,de91.100.50Veziva. Tesnilni materialiBinders. Sealing materials91.100.10Cement. Mavec. Apno. MaltaCement. Gypsum. Lime. MortarICS:SLOVENSKI
STANDARDSIST EN 13454-2:2004+A1:200701-december-2007







EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 13454-2:2003+A1
July 2007 ICS 91.100.10; 91.100.50 Supersedes EN 13454-2:2003 English Version
Binders, composite binders and factory made mixtures for floor screeds based on calcium sulfate - Part 2: Test methods
Liants, liants composites et mélanges fabriqués en usine à base de sulfate de calcium pour chapes de sol - Partie 2: Méthodes d'essai
Calciumsulfat-Binder, Calciumsulfat-Compositbinder und Calciumsulfat-Werkmörtel für Estriche - Teil 2: Prüfverfahren This European Standard was approved by CEN on 1 September 2003 and includes Amendment 1 approved by CEN on 22 June 2007.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN 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 translation under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
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B-1050 Brussels © 2007 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 13454-2:2003+A1:2007: E



EN 13454-2:2003+A1:2007 (E) 2 Contents Page Foreword.3 1 Scope.4 2 Normative references.4 3 Test conditions and sampling.4 3.1 General requirements for testing.4 3.1.1 Water.4 3.1.2 Apparatus.4 3.2 Sampling for binders (CAB, CAC).5 3.3 Sampling for factory made mixtures (CA).5 4 Test methods for binders (CAB ; CAC).5 4.1 Content of calcium sulfate.5 4.1.1 Principle.5 4.1.2 Apparatus.5 4.1.3 Reagents.6 4.1.4 Procedure.6 4.2 Determination of pH.7 4.3 Determination of setting time.7 4.3.1 Principle.7 4.3.2 Apparatus.7 4.3.3 Standard consistence test.7 4.3.4 Procedure.7 4.3.5 Setting time test.8 4.4 Determination of strengths.9 4.4.1 Apparatus.9 4.4.2 Procedure.11 4.4.3 Water demand for flow table value.12 4.4.4 Preparation of test specimens.12 4.4.5 Testing the specimens.13 4.5 Determination of shrinkage and swelling.14 4.5.1 Principle.14 4.5.2 Apparatus.15 4.5.3 Preparation and storage of the specimens.16 4.5.4 Measuring of the specimens.16 5 Test method for factory made mixtures (CA).17 5.1 Determination of pH value.17 5.2 Working time.17 5.2.1 Flowing mixture.17 5.2.2 Stiff mixture.18 5.3 Determination of strength.18 5.3.1 Composition of the test sample.18 5.3.2 Flexural and compressive strength.18 5.4 Determination of shrinkage and swelling.18 6 Test report.18 Bibliography.20



EN 13454-2:2003+A1:2007 (E) 3 Foreword This document (EN 13454-2:2003+A1:2007) has been prepared by Technical Committee CEN/TC 241 “Gypsum and gypsum based products”, the secretariat of which is held by AFNOR. This document shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by January 2008 and conflicting national standards shall be withdrawn at the latest by January 2008. This document includes Amendment 1 approved by CEN on 2007-06-22. This document supersedes EN 13454-2:2003. The start and finish of text introduced or altered by amendment is indicated in the text by tags ! ". !deleted text" The European Standard EN 13454 for binders, composite binders and factory made mixtures for floor screeds based on calcium sulfate consists of two parts:
Part 1: Definitions and requirements
Part 2: Test methods The 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 where the principal active component is calcium sulfate. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.



EN 13454-2:2003+A1:2007 (E) 4 1 Scope This European Standard describes the test methods for binders and composite binders for floor screeds based on calcium sulfate specified in prEN 13454-1. This European Standard describes the test methods for factory made mixtures for floor screeds based on calcium sulfate specified in EN 13813. This European Standard describes reference test methods. If other than these methods and conditions are used, it is necessary to show that they give results equivalent to those given by the reference methods. In the event of a dispute, only the reference test method is used. 2 Normative references This 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 (including amendments). !EN 196-1:2005", Methods of testing cement – Part 1 : Determination of strength !EN 196-3:2005, Methods of testing cement - Part 3: Determination of setting times 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 sampling 3.1 General requirements for testing 3.1.1 Water The 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 Apparatus The apparatus used for gauging and the moulds used for preparing the test specimens, shall be free from leaks and 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 sulfate dihydrate which can influence the setting time, all equipment used in the tests shall be kept in a perfect state of cleanliness.



EN 13454-2:2003+A1:2007 (E) 5 3.2 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 of samples shall always be representative of the average composition of the material, the possibility of segregation being taken into consideration. The test report shall state whether the samples taken are spot samples or composite 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 they have been taken. Wherever possible tests shall be carried out on specimens prepared immediately after obtaining the sample, if necessary on site. Specimens shall be prepared during working time but not later than 2 h after gauging. This period shall also be observed when fresh samples are supplied to a testing centre, and may be appropriately decreased or increased for samples containing accelerators or retarders. If transportation of fresh samples cannot be avoided, they shall be supplied immediately for testing, accompanied by a certificate stating which tests are to be carried out, and protected from changes, such as loss of water, entry of water 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. when prepared in situ) be stored under vibration-free conditions and protected from climatic effects (e.g. frigobox etc.) for at least 24 h before they are conveyed in the moulds for testing. If special requirements in respect of the preparation 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 sulfate 4.1.1 Principle The calcium sulfate is decomposed by digestion with hydrochloric acid solution. Insoluble impurities are removed by filtration. The sulfate in the filtrate is determined gravimetrically as barium sulfate. 4.1.2 Apparatus a) 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+A1:2007 (E) 6 4.1.3 Reagents a) 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 Procedure Grind the dried sample until it passes completely through a sieve with a mesh of 0,1 mm. Weigh accurately about 0,5 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 boil and maintain this for 10 min. Add 150 ml of hot water and allow to boil for 15 min. Remove the beaker from the heat and filter through the filter paper into an 800 ml beaker. Wash out the beaker and filter paper using hot distilled or 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 ammonia solution. Add 20 ml 2 N HCl. Bring to the boil again and add 50 ml of hot barium chloride solution stirring vigorously during 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 with hot water, transfer to the crucible and wash 6 times with small quantities of hot water. The last wash should be chloride 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 by decantation with hot water, transfer to the filter paper and wash with small quantities of hot water until the wash is chloride free. After filtration and washing fold the paper around the precipitate and place it in a weighed porcelain or silica crucible, previously ignited at (800 ± 25) °C and cooled in a desiccator. Heat gently to char the paper and expel the volatile matter. Do not allow the paper to burst into flames. Raise the temperature slowly to burn off the carbon with free access of air. Finally ignite for 10 min at (800 ± 25) °C. Cool in a desiccator and weigh. Calculate the CaSO4 content as a percentage from the equation : [CaSO4] = W2 x 58,33 / W1 (1) where W1 is the mass of sample, in grams ; W2 is the mass of precipitate, in grams.



EN 13454-2:2003+A1:2007 (E) 7 4.2 Determination of pH Disperse 1 part by mass of the pulverised sample in 10 parts by mass of deionized or distilled water. Stir it for 5 min and then measure the pH by a pH-meter or pH-paper to the nearest ± 0,5 pH. 4.3 Determination of setting time 4.3.1 Principle Determine setting time using the method given in EN 196-3, "binder" being substituted, where "cement" is mentioned. The setting time is determined by observing the penetration of a needle into a binder paste of standard consistence according to clause 5 of !EN 196-3:2005" until it reaches a specified value. Binder paste of standard consistency 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. 4.3.2 Apparatus a) Mixer : As described in 4.4 of !EN 196-1:2005". b) Vicat penetration apparatus : As described in 5.1 of !EN 196-3:2005". 4.3.3 Standard consistence test Use 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 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. 4.3.4 Procedure 4.3.4.1 Mixing the binder paste Weigh, to the nearest 1 g, 500 g of binder. Weigh a quantity of water, e.g. 125 g, in the mixer bowl or measure the water from the graduated cylinder or burette into the mixer bowl. Possible admixture should already be diluted in water. Add the binder carefully to the water in order to avoid loss of water or binder. The time of addition shall not be 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. 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.



EN 13454-2:2003+A1:2007 (E) 8 4.3.4.2 Filling the mould and carrying out the test Transfer the paste after mixing immediately to the mould, which has previously been placed on a lightly greased plan 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. Adjust the Vicat apparatus with the plunger (Figure 1c) attached in advance of the test, by lowering the plunger to rest on the baseplate 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 baseplate 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 baseplate, together with the water content of the paste expressed as a percentage by mass of the binder. 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 baseplate of (6 ± 3) mm. Record the water content of that paste to the nearest 0,5 % as the water for standard consistency. 4.3.5 Setting time test 4.3.5.1 Determination of initial setting time 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. Adjust the Vicat apparatus with the needle (Figure 1d), attached in advance of the test, by lowering the needle to rest 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 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 the baseplate, 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. Clean the Vicat needle immediately after each penetration. Record the time measured from zero at which the distance between the needle and the baseplate is (6 ± 3) mm as the initial setting time of the binder 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.



EN 13454-2:2003+A1:2007 (E) 9 4.3.5.2 Determination of final setting time Invert the filled mould used in 4.3.4 on its baseplate so that the tests for final set are made on the face of the specimen originally in contact with the baseplate. Fit the needle with a ring attachment (Figure 1 (e)) to facilitate accurate observation of small penetrations. Use the procedure described in 4.3.4. The intervals of time between penetration 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 into the specimen as the final setting time of the binder. This time is that 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. 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. 4.4 Determination of strengths Determine the flexural and the compressive strength in accordance with EN 196-1, "binder" being substituted, where "cement" is mentioned. 4.4.1 Apparatus a) Mixer : As described in 4.4 of !EN 196-1:2005". b) Moulds with base : As described in 4.5 of !EN 196-1:2005" 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 196-1:2005". e) Compressive strength, testing machine : As described in clause 9 of !EN 196-1:2005". f) Flow table, mould, cam and tamper : As described in 5.5.2.1.2 of EN 459-2:2001



EN 13454-2:2003+A1:2007 (E) 10 Dimensions in millimetres
a) Side view with mould in upright position
for initial setting time determination b) Front view with mould inverted for final setting time determination
c) plunger for standard consistency d) needle for initial test e) needle and attachment for final test Key 1 hard rubber mould 2 platform for correcting weights
3 basis plate 4 test container
5 water 6 air vent (diameter 1,5 mm) NOTE The specified dimensions should 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 determination of the standard consistency and setting time



EN 13454-2:2003+A1:2007 (E) 11 4.4.2 Procedure 4.4.2.1 Preparation of sample Binder (including possible admixtures), sand, water and apparatus shall be at the laboratory temperature. Carry out weighing 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 196-1:2005" and the necessary amount of water. The amount of water shall be such that a flow diameter of (150 ± 5) mm according to 5.5.2.3.2 of EN 459-2:2001, is achieved, but shall not fall below a minimum amount of 225 ml. Possible admixture shall already be diluted in water. !For flowing mixtures for self levelling floor screeds the minimum flow diameter shall be 150 mm and the minimum amount of water shall be 225 ml. If the required flow diameter is not achieved the amount of water shall be increased." Mix each batch of sample in accordance with !6.2 of EN 196-1:2005" mechanically using the mixer. With the mixer in the operating position : a) pour the water into the bowl and add the binder (possible admixtures shall already have been diluted in the water) ; 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 with the 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 adhering to the wall and bottom part of the bowl and place in the middle of the bowl ; d) continue
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