EN 196-2-2013 en Method of testing cement - Part 2 Chemical analysis of cement《测试水泥的方法 第2部分 水泥的化学分析》.pdf

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1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 196-2:2013Method of testing cementPart 2: Chemical analysis of cementBS EN 196-2:2013 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN

2、196-2:2013. Itsupersedes BS EN 196-2:2005 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee B/516/12, Sampling and testing.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport t

3、o include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2013. Published by BSI StandardsLimited 2013ISBN 978 0 580 78941 0ICS 91.100.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This

4、 British Standard was published under the authority of theStandards Policy and Strategy Committee on 30 June 2013.Amendments issued since publicationDate Text affectedBS EN 196-2:2013EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 196-2 June 2013 ICS 91.100.10 Supersedes EN 196-2:2005English Ve

5、rsion Method of testing cement - Part 2: Chemical analysis of cement Mthodes dessais des ciments - Partie 2: Analyse chimique des ciments Prfverfarhen fr Zement - Teil 2: Chemische Analyse von Zement This European Standard was approved by CEN on 5 April 2013. CEN members are bound to comply with the

6、 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-CENELEC Management

7、 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-CENELEC Management Centre has the same status a

8、s the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Ne

9、therlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2013 CEN All rights of ex

10、ploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 196-2:2013: EBS EN 196-2:2013EN 196-2:2013 (E) 2 Contents Page Foreword . 3 1 Scope 4 2 Normative references . 4 3 General requirements for testing 4 3.1 Number of tests 4 3.2 Repeatability and reproduci

11、bility 5 3.3 Expression of masses, volumes, factors and results . 5 4 Analysis by wet chemistry . 5 4.1 General . 5 4.2 Reagents . 6 4.3 Apparatus . 18 4.4 Analysis procedure 22 4.5 Determination of major elements 28 5 Chemical analysis by X-ray fluorescence . 49 5.1 Reagents and reference materials

12、 . 49 5.2 Apparatus . 50 5.3 Flux . 51 5.4 Determination of loss on ignition and the change in mass on fusion of the cement 53 5.5 Factoring test results and correcting total analyses for presence of sulfides and halides 54 5.6 Preparation of fused beads and pressed pellets 56 5.7 Calibration and va

13、lidation 59 5.8 Calculation and expression of results 68 5.9 Performance criteria (repeatability, accuracy and reproducibility limits) . 69 Annex A (informative) Examples of fluxes . 70 Annex B (informative) Sources of certified reference materials . 71 Annex C (informative) Examples of calibration

14、standards and monitor beads and pellets . 72 Bibliography 73 BS EN 196-2:2013EN 196-2:2013 (E) 3 Foreword This document (EN 196-2:2013) has been prepared by Technical Committee CEN/TC 51 “Cement and building limes”, the secretariat of which is held by NBN. This European Standard shall be given the s

15、tatus of a national standard, either by publication of an identical text or by endorsement, at the latest by December 2013, and conflicting national standards shall be withdrawn at the latest by December 2013. Attention is drawn to the possibility that some of the elements of this document may be th

16、e subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 196-2:2005. This edition adds, to the previous version EN 196-2:2005, provisions for the use of X-ray fluorescence (XRF) analysis as an alternative

17、method. In relation to correctly calibrating the method, specified procedures, reference materials and performance criteria are included in order to attain and maintain suitable accuracy and precision for equivalence. The method has not been validated for use yet as a reference procedure for conform

18、ity or dispute purposes. This European Standard on the methods of testing cement is comprised of the following parts: Part 1: Determination of strength Part 2: Chemical analysis of cement Part 3: Determination of setting times and soundness Part 5: Pozzolanicity test for pozzolanic cement Part 6: De

19、termination of fineness Part 7: Methods of taking and preparing samples of cement Part 8: Heat of hydration Solution method Part 9: Heat of hydration Semi-adiabatic method Part 10: Determination of the water-soluble chromium (VI) content of cement NOTE Another document, CEN/TR 196-4 Methods of testi

20、ng cement Part 4: Quantitative determination of constituents, has been published as a CEN Technical Report. According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cr

21、oatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

22、 the United Kingdom. BS EN 196-2:2013EN 196-2:2013 (E) 4 1 Scope This European Standard specifies the methods for the chemical analysis of cement. This document describes the reference methods and, in certain cases, an alternative method which can be considered to be equivalent. In the case of a dis

23、pute, only the reference methods are used. An alternative performance-based method using X-ray fluorescence (XRF) is described for SiO2, Al2O3, Fe2O3, CaO, MgO, SO3, K2O, Na2O, TiO2, P2O5, Mn2O3,SrO, Cl and Br. When correctly calibrated according to the specified procedures and reference materials,

24、it provides a method equivalent to the reference methods but has not been validated for use yet as a reference procedure for conformity and dispute purposes. It can be applied to other relevant elements when adequate calibrations have been established. This method is based on beads of fused sample a

25、nd analytical validation using certified reference materials, together with performance criteria. A method based on pressed pellets of un-fused sample can be considered as equivalent, providing that the analytical performance satisfies the same criteria. Any other methods may be used provided they a

26、re calibrated, either against the reference methods or against internationally accepted reference materials, in order to demonstrate their equivalence. This document describes methods which apply principally to cements, but which can also be applied to their constituent materials. They can also be a

27、pplied to other materials, the standards for which call up these methods. Standard specifications state which methods are to be used. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated

28、references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 196-7, Methods of testing cement Part 7: Methods of taking and preparing samples of cement ISO 385, Laboratory glassware Burettes ISO 835, Laborato

29、ry glassware Graduated pipettes ISO Guide 30, Terms and definitions used in connection with reference materials ISO Guide 31, Reference materials Contents of certificates and labels 3 General requirements for testing 3.1 Number of tests Analysis of a cement may require the determination of a number

30、of its chemical properties. For each determination, one or more tests shall be carried out in which the number of measurements to be taken shall be as specified in the relevant clause of this document. Where the analysis is one of a series subject to statistical control, the determination of each ch

31、emical property by a single test shall be the minimum required. Where the analysis is not part of a series subject to statistical control, the number of tests for determination of each chemical property shall be two (see also 3.3 and 5.8). In the case of a dispute, the number of tests for determinat

32、ion of each chemical property shall be two (see also 3.3). BS EN 196-2:2013EN 196-2:2013 (E) 5 3.2 Repeatability and reproducibility Repeatability: Precision under repeatability conditions where independent test results are obtained with the same method on identical test items (material) in the same

33、 laboratory by the same operator using the same equipment within short intervals of time. Reproducibility: Precision under reproducibility conditions where test results are obtained with the same method on identical test items (material) in different laboratories with different operators using diffe

34、rent equipment. Repeatability and reproducibility in this document are expressed as repeatability standard deviation(s) and reproducibility standard deviation(s) in e.g. absolute percent, grams, etc., according to the property tested. 3.3 Expression of masses, volumes, factors and results Express ma

35、sses in grams to the nearest 0,000 1 g and volumes from burettes in millilitres to the nearest 0,05 ml. Express the factors of solutions, given by the mean of three measurements, to three decimal places. Express the results, where a single test result has been obtained, as a percentage generally to

36、two decimal places. Express the results, where two test results have been obtained, as the mean of the results, as a percentage generally to two decimal places. If the two test results differ by more than twice the standard deviation of repeatability, repeat the test and take the mean of the two clo

37、sest test results. The results of all individual tests shall be recorded. 4 Analysis by wet chemistry 4.1 General 4.1.1 Ignitions Carry out ignitions as follows. Place the filter paper and its contents into a crucible which has been previously ignited and tared. Dry it, then incinerate slowly in an

38、oxidising atmosphere in order to avoid immediate flaming, while ensuring complete combustion. Ignite the crucible and its contents at the stated temperature then allow to cool to the laboratory temperature in a desiccator. Weigh the crucible and its contents. 4.1.2 Determination of constant mass Det

39、ermine constant mass by making successive 15 min ignitions followed each time by cooling and then weighing. Constant mass is reached when the difference between two successive weighings is less than 0,000 5 g. 4.1.3 Check for absence of chloride ions (silver nitrate test) After generally five to six

40、 washes of a precipitate, rinse the base of the filter stem with a few drops of water. Wash the filter paper and its contents with several millilitres of water and collect this in a test tube. Add several drops of silver nitrate solution (4.2.44). Check the absence of turbidity or precipitate in the

41、 solution. If present, continue washing while carrying out periodic checks until the silver nitrate test is negative. BS EN 196-2:2013EN 196-2:2013 (E) 6 4.1.4 Blank determinations Carry out a blank determination without a sample, where relevant, following the same procedure and using the same amoun

42、ts of reagents. Correct the results obtained for the analytical determination accordingly. 4.1.5 Preparation of a test sample of cement Before chemical analysis, treat the laboratory sample, taken in accordance with EN 196-7, as follows to obtain a homogeneous test sample. Take approximately 100 g o

43、f the laboratory sample by means of a sample divider or by quartering. Sieve this portion on a 150 m or 125 m sieve until the residue remains constant. Remove metallic iron from the material retained on the sieve by means of a magnet (see Note 1). Then grind the iron-free fraction of the retained ma

44、terial so that it completely passes the 150 m or 125 m sieve. Transfer the sample to a clean dry container with an airtight closure and shake vigorously to mix it thoroughly. Carry out all operations as quickly as possible to ensure that the test sample is exposed to ambient air only for the minimum

45、 time. NOTE 1 Where the analysis is one of a series subject to statistical control and the level of the metallic iron content has been shown to be insignificant in relation to the chemical properties to be determined then it is not necessary to remove metallic iron. NOTE 2 Where the sample is to be

46、used for XRF analysis and it contains quartz, it might be necessary to grind the sample to pass a 90 m sieve in order to obtain a satisfactory fusion (see 5.6). The time and temperature required to obtain a satisfactory fusion is affected by the fineness of the sample. NOTE 3 Where the sample is to

47、be used for XRF analysis using pressed pellets, accuracy can be improved by grinding the sample more finely. 4.2 Reagents 4.2.1 General Use only reagents of analytical quality. References to water mean distilled or de-ionised water having an electrical conductivity 0,5 mS/m. Unless otherwise stated,

48、 percent means percent by mass. Unless otherwise stated, the concentrated liquid reagents used in this document have the following densities () (in g/cm3at 20 C): hydrochloric acid 1,18 to 1,19 acetic acid 1,05 to 1,06 nitric acid 1,40 to 1,42 phosphoric acid 1,71 to 1,75 perchloric acid 1,60 to 1,6

49、7 ammonium hydroxide 0,88 to 0,91 The degree of dilution is always given as a volumetric sum, for example: dilute hydrochloric acid 1 + 2 means that 1 volume of concentrated hydrochloric acid is to be mixed with 2 volumes of water. 4.2.2 Concentrated hydrochloric acid (HCl) 4.2.3 Dilute hydrochloric acid (1 + 1) 4.2.4 Dilute hydrochloric acid (1 + 2) BS EN 196-2:2013EN 196-2:2013 (E) 7 4.2.5 Dilute hydrochloric acid (1 + 3) 4.2.6 Dilute hydrochloric acid (1 + 9) 4.2.7 Dilute hydrochloric acid (1 + 11) 4.2.8 Dilute hydrochloric acid (1 +