BS-EN-196-5-1995.pdf
BRITISH STANDARD BS EN 196-5:1995 Methods of testing cement Part 5: Pozzolanicity test for pozzolanic cements The European Standard EN 196-5:1994 has the status of a British Standard Licensed Copy: sheffieldun sheffieldun, na, Tue Nov 07 09:42:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN 196-5:1995 This British Standard, having been prepared under the direction of Technical Committee B/516, was published under the authority of the Standards Board and comes into effect on 15 March 1995 © BSI 02-1999 The following BSI references relate to the work on this standard: Committee reference B/516 Special announcement in BSI News December 1992 ISBN 0 580 21525 3 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: AustriaOesterreichisches Normungsinstitut BelgiumInstitut belge de normalisation DenmarkDansk Standard FinlandSuomen Standardisoimisliito, r.y. FranceAssociation française de normalisation GermanyDeutsches Institut für Normung e.V. GreeceHellenic Organization for Standardization IcelandTechnological Institute of Iceland IrelandNational Standards Authority of Ireland ItalyEnte Nazionale Italiano di Unificazione LuxembourgInspection du Travail et des Mines NetherlandsNederlands Normalisatie-instituut NorwayNorges Standardiseringsforbund PortugalInstituto Portuguès da Qualidade SpainAsociación Española de Normalización y Certificación SwedenStandardiseringskommissionen i Sverige SwitzerlandAssociation suisse de normalisation United KingdomBritish Standards Institution Amendments issued since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Tue Nov 07 09:42:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN 196-5:1995 © BSI 02-1999i Contents Page Cooperating organizations Inside front cover National foreword ii Foreword 2 Text of EN 196-5 3 National annex NA (informative) Determination of endpointsInside back cover National annex NB (informative) Committees responsibleInside back cover National annex NC (informative) Cross-references Inside back cover Licensed Copy: sheffieldun sheffieldun, na, Tue Nov 07 09:42:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN 196-5:1995 ii © BSI 02-1999 National foreword This British Standard has been prepared under the direction of Technical Committee B/516, Cement and lime. It is the English language version of EN 196-5:1994 Methods of testing cement Part 5: Pozzolanicity test for pozzolanic cement published by the European Committee for Standardization (CEN). EN 196-5 was drawn up by CEN Technical Committee 51, Cement and building limes, as Part 5 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 clause 15 of BS 4550-2:1970 and this clause is now deleted. In this Part the reference procedure requires the endpoint of titrations to be determined visually. However, for the standardization of the EDTA solution and the determination of the calcium oxide concentration a more satisfactory photometric procedure using the same indicator exists in EN 196-2. In the UK this photometric endpoint determination, as indicated in National annex NA, is preferred as an alternative. 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 pages This document comprises a front cover, an inside front cover, pages i and ii, the EN title page, pages 2 to 6, 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. Licensed Copy: sheffieldun sheffieldun, na, Tue Nov 07 09:42:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM EN 196-5 December 1994 ICS 91.100.10Supersedes EN 196-5:1987 Descriptors: Cements, pozzolans, chemical tests, determination of content, calcium hydroxide, EDTA, chemical reagents, apparatus English version Methods of testing cement Part 5: Pozzolanicity test for pozzolanic cement Méthodes dessais des ciments Partie 5: Essai de pouzzolanicité des ciments pouzzolaniques Prüfverfahren für Zement Teil 5: Prüfung der Puzzolanität von Puzzolanzementen This European Standard was approved by CEN on 1994-12-12. 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 Central Secretariat 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 Central 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 and United Kingdom. CEN European Committee for Standardization Comité Européen de Normalisation Europäisches Komitee für Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels © 1994 Copyright reserved to CEN members Ref. No. EN 196-5:1994 E Licensed Copy: sheffieldun sheffieldun, na, Tue Nov 07 09:42:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 196-5:1994 © BSI 02-1999 2 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 the 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 196-5:1987. 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 Page Foreword 2 1Scope 3 2Normative references3 3General requirements for testing3 4Preparation of a cement sample3 5Principle3 6Reagents3 7Apparatus4 8Standardization of solutions4 9Procedure5 10Results6 Figure 1 Diagram for assessing pozzolanicity6 Licensed Copy: sheffieldun sheffieldun, na, Tue Nov 07 09:42:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 196-5:1994 © BSI 02-19993 1 Scope This European Standard describes the method of measuring the pozzolanicity of pozzolanic cements conforming to ENV 197-1. This standard does not apply to Portland pozzolana cements or to pozzolanas. This method constitutes the reference procedure. 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. EN 196-2, Methods of testing cement Part 2: Chemical analysis of cement. EN 196-7, Methods of testing cement Part 7: Methods of taking and preparing samples of cement. ENV 197-1, Cement Composition, specifications and conformity criteria Part 1: Common cements. ISO 385-1:1984, Laboratory glassware Burettes Part 1: General requirements. ISO 835-1:1981, Laboratory glassware Graduated pipettes Part 1: General requirements. ISO 3534:1977, Statistics Vocabulary and symbols. 3 General requirements for testing 3.1 Expression of masses, volumes and factors Express masses in grams to the nearest 0,0001 g and volumes from the burette in millilitres to the nearest 0,05 ml. Express the factors of solutions, given by the mean of three determinations, to three places of decimals. 3.2 Number of tests The number of tests shall be two (see also 3.3). 3.3 Expression of results Express the results of the determinations in millimoles per litre to the nearest 0,1 mmol/l. Give the final result as the mean of two determinations to one place of decimals. If the difference between two determinations is more than twice the standard deviation for repeatability, repeat the test and take the mean of the two closest values. 3.4 Repeatability and reproducibility The standard deviation of repeatability gives the closeness of agreement between successive results obtained with the same method on identical material tested under the same conditions (same operator, same apparatus, same laboratory and short intervals of time1). The standard deviation of reproducibility gives the closeness of agreement between individual results obtained with the same method on identical material but tested under different conditions (different operators, different apparatus, different laboratory and/or different time1). The standard deviations of repeatability and reproducibility are expressed in millimoles per litre. 4 Preparation of a cement sample Take a sample by the method described in EN 196-7. Treat this laboratory sample as described in EN 196-2. 5 Principle The pozzolanicity is assessed by comparing the quantity of calcium hydroxide present in the aqueous solution in contact with the hydrated cement, after a fixed period of time, with the quantity of calcium hydroxide capable of saturating a solution of the same alkalinity. The test is considered positive if the concentration of calcium hydroxide in the solution is lower than the saturation concentration. Experiment has shown that a mixture of 20 g of cement and 100 ml of water at 40 °C achieves equilibrium after a period of 8 days or 15 days2). To evaluate the results it is therefore necessary to know the solubility at 40 °C of calcium hydroxide in a solution of which the alkalinity varies from 35 to about 100 mmol OH per litre. 6 Reagents Use only reagents of recognized analytical quality and freshly boiled water, distilled or of equivalent purity, during the analysis. 6.1 Concentrated hydrochloric acid (HCl), approximately 12 mol/l (? = 1,18 g/cm3 to 1,19 g/cm3). 1) Definitions taken from ISO 3534. 2) 8 days are sufficient if the test is positive at this stage (see 10.2). Licensed Copy: sheffieldun sheffieldun, na, Tue Nov 07 09:42:19 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 196-5:1994 4 © BSI 02-1999 6.2 Dilute hydrochloric acid: about 0,1 mol/l. Using the 50 ml precision burette (7.8), add 8,5 ml of concentrated hydrochloric acid (6.1) to a 1 litre volumetric flask (7.10) containing about 500 ml of water. Then make up the volume with water. 6.3 Dilute hydrochloric acid (1 + 2): add 250 ml of concentrated hydrochloric acid to 500 ml water. 6.4 Methyl orange (dimethylaminoazobenzene p-sodium sulfonate). 6.5 Methyl orange indicator: dissolve 0,02 g of methyl orange in water and make up to 1 000 ml. 6.6 Sodium hydroxide (NaOH). 6.7 Sodium hydroxide solution: dissolve 100 g of sodium hydroxide in water and make up to 1 000 ml. 6.8 Calcium carbonate (CaCO3): dried at 110 °C. 6.9 Potassium chloride (KCl): dried at 110 °C. 6.10 Murexide (ammonium purpurate). 6.11 Murexide indicator: grind and mix 1 g of murexide with 100 g of dry potassium chloride. 6.12 EDTA (disodium dihydrate salt of ethylenediaminetetra-acetic acid). 6.13 EDTA solution about 0,025 mol/l : dissolve 9,306 g of EDTA in water and make up to 1 000 ml. 6.14 Sodium carbonate (Na2CO3): dried at 260 °C. 7 Apparatus 7.1 500 ml cylindrical polyethylene container of about 70 mm diameter with a pressure seal-plug locked by a screw plug. 7.2 Wide stem funnel 7.3 Porcelain Buchner funnel of 60 mm inner diameter. 7.4 Filter paper with low porosity (mean pore diameter of about 2 4m). 7.5 250 ml vacuum flask. 7.6 250 ml and 400 ml beakers. 7.7 50 ml and 100 ml precision pipettes (class A of ISO 835-1:1981). 7.8 50 ml precision burette (class A of ISO 385-1: 1984). 7.9 Uniform temperature enclosure controlled thermostatically at (40 ± 0,5) °C. 7.10 500 ml and 1 000 ml volumetric flasks. 7.11 250 ml conical flask. 8 Standardization of solutions 8.1 Standardization of the EDTA solution Weigh approximately 1 g of calcium carbonate (6.8) to the nearest 0,0001 g and introduce into the 250 ml beaker (7.6). Add approximately 100 ml of water and, very carefully, 50 ml of dilute hydrochloric acid (6.3) keeping the beaker covered with a watch glass. Stir with a glass rod and ensure that dissolution is complete. Then transfer the solution into the 500 ml volumetric flask (7.10), wash the beaker and watch glass carefully with water, adding the washings to the solution and make up the volume with water. Pipette 50 ml of the solution into the 400 ml beaker (7.6), dilute with approximately 150 ml of water and add the quantity of sodium hydroxide solution (6.7) necessary to achieve pH 13 (check the pH by means of a pH meter or by indicator papers). Add approximately 50 mg of murexide indicator (6.11) and titrate by means of the burette (7.8) against the EDTA solution (6.13) until there is a steady colour change from purple to violet. From the volume of EDTA solution used, calculate the factor f1 of the EDTA solution by the formula: where 8.2 Standardization of the 0,1 m
