1、BS ISO29581-2:2010ICS 91.100.10NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDCement TestmethodsPart 2: Chemical analysis by X-rayfluorescenceThis British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 31 May2010. BSI 2
2、010ISBN 978 0 580 58959 1Amendments/corrigenda issued since publicationDate CommentsBS ISO 29581-2:2010National forewordThis British Standard is the UK implementation of ISO 29581-2:2010.The UK participation in its preparation was entrusted to TechnicalCommittee B/516/12, Sampling and testing.A list
3、 of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obl
4、igations.BS ISO 29581-2:2010Reference numberISO 29581-2:2010(E)ISO 2010INTERNATIONAL STANDARD ISO29581-2First edition2010-03-01Cement Test methods Part 2: Chemical analysis by X-ray fluorescence Ciments Mthodes dessais Partie 2: Analyse chimique par spectromtrie de fluorescence X BS ISO 29581-2:2010
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8、 given below. COPYRIGHT PROTECTED DOCUMENT ISO 2010 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at
9、 the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2010 All rights reservedBS ISO 29581-2:2010ISO 29581-2:2
10、010(E) ISO 2010 All rights reserved iiiContents Page Foreword iv Introduction.v 1 Scope1 2 Normative references2 3 Terms and definitions .2 4 General requirements for testing.3 5 Reagents and reference materials.4 6 Apparatus.5 7 Preparation of a test sample of cement 6 8 Flux .7 9 Determination of
11、loss on ignition and the change in mass on fusion of the cement 8 10 Factoring test results and correcting total analyses for presence of sulfides and halides 10 11 Preparation of fused beads and pressed pellets .12 12 Calibration and validation.14 13 Calculation and expression of results 23 14 Perf
12、ormance criteria (repeatability, accuracy and reproducibility limits) .24 Annex A (informative) Examples of fluxes .25 Annex B (informative) Sources of certified reference materials26 Annex C (informative) Examples of calibration standards and monitor beads and pellets27 Annex D (informative) Determ
13、ination of the sulfate content of samples containing sulfide species28 Bibliography30 BS ISO 29581-2:2010ISO 29581-2:2010(E) iv ISO 2010 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). Th
14、e work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-gov
15、ernmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
16、The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vo
17、te. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 29581-2 was prepared by Technical Committee ISO/TC 74, Cement and lime. ISO 29581 consists of
18、 the following parts, under the general title Cement Test methods: Part 1: Analysis by wet chemistry Part 2: Chemical analysis by X-ray fluorescence BS ISO 29581-2:2010ISO 29581-2:2010(E) ISO 2010 All rights reserved vIntroduction This part of ISO 29581 incorporates the following technical principle
19、s based on comments received by the Secretariat. a) It provides an analytical method based on X-ray fluorescence (XRF) for use as the alternative method for the analysis of cement. When correctly calibrated according to the specified procedures and reference materials, it provides a method of suitab
20、le precision for conformity and information purposes. b) It introduces a reference method for TiO2, P2O5, SrO and Br analysis. c) Traceability of the method relies upon reference materials and “pure” chemicals so that the ultimate traceability to basic international chemical standards relies upon cl
21、assical analytical methods that are outside of the scope of this part of ISO 29581. XRF and other instrumental methods, such as differential thermal analysis for determination of carbon dioxide, atomic absorption spectroscopy, etc., can be used as alternative methods, provided they are calibrated ag
22、ainst the reference methods, or against internationally accepted reference materials. BS ISO 29581-2:2010BS ISO 29581-2:2010INTERNATIONAL STANDARD ISO 29581-2:2010(E) ISO 2010 All rights reserved 1Cement Test methods Part 2: Chemical analysis by X-ray fluorescence 1 Scope This part of ISO 29581 desc
23、ribes a performance-based method for the chemical analysis of cement for SiO2, Al2O3, Fe2O3, CaO, MgO, SO3, K2O, Na2O, TiO2, P2O5, Mn2O3,SrO, Cl and Br using X-ray fluorescence (XRF). It can be applied to other relevant elements when adequate calibrations have been established. This part of ISO 2958
24、1 describes an alternative method for analyses of cement for conformity and information purposes, based on beads of fused sample and analytical validation using certified reference materials, together with performance criteria. A method based on pressed pellets of unfused sample can be considered as
25、 equivalent, providing that the analytical performance satisfies the same criteria. NOTE 1 The use of fused beads generally improves the accuracy of analysis for non-volatile elements, since it eliminates variability arising from differences in mineralogical forms or oxidation states. Pressed pellet
26、s generally improve the accuracy of analysis for volatile elements and can give adequate accuracy for the routine analysis of non-volatile elements. NOTE 2 The presence of sulfide in a sample also leads to restrictions on the scope of the analysis that can be undertaken using the XRF technique based
27、 upon fused beads. In particular, sulfate (SO3) cannot be determined directly from such a fused bead because of the contribution to the analysis from the unknown amount of sulfide. In addition, sulfide cannot be determined directly (or accurately, indirectly) because of the contribution of the unkno
28、wn amount of sulfate to the analysis and because of the possibility that some sulfide can be lost by volatilization during fusion. Consequently, the method of ISO 29581-1, included as Annex D to this part of ISO 29581, is the reference method for determining the sulfate content of samples containing
29、 sulfide species. Other methods can be used, provided they are calibrated, either against the reference method or against internationally accepted reference materials, in order to demonstrate their equivalence. In the case of dispute, unless otherwise agreed by all parties, only the reference method
30、 in ISO 29581-1 can be used. This part of ISO 29581 describes methods that apply principally to cements, but which can also be applied to their constituent materials and to other materials, the standards for which call up these methods. International Standard specifications state which methods can b
31、e used. BS ISO 29581-2:2010ISO 29581-2:2010(E) 2 ISO 2010 All rights reserved2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the refer
32、enced document (including any amendments) applies. ISO Guide 30, Terms and definitions used in connection with reference materials ISO Guide 31, Reference materials Contents of certificates and labels ISO 29581-1, Cement Test methods Part 1: Analysis by wet chemistry EN 196-7, Methods of testing cem
33、ent Part 7: Methods of taking and preparing samples of cement EN 197-1, Cement Part 1: Composition, specifications and conformity criteria for common cements 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 beads glassy discs of fused sample f
34、or analysis by X-rays in the spectrometer 3.2 pellets compressed discs of finely ground sample for analysis by X-rays in the spectrometer 3.3 calibration beads or pellets beads or pellets used for establishing the calibration equation 3.4 analysis beads or pellets beads or pellets containing the sam
35、ple being analysed 3.5 accuracy closeness of agreement between a test result and the certified value for a reference material 3.6 repeatability closeness of agreement among independent test results obtained with the same method on identical test items in the same laboratory by the same operator usin
36、g the same equipment within short intervals of time 3.7 reproducibility closeness of agreement between independent test results obtained with the same method on identical test items in different laboratories with different operators using different equipment 3.8 expert laboratory laboratory capable
37、of consistently meeting the expert performance criteria set out in Clause 14 3.9 normal laboratory laboratory capable of consistently meeting the normal performance criteria set out in Clause 14 BS ISO 29581-2:2010ISO 29581-2:2010(E) ISO 2010 All rights reserved 34 General requirements for testing 4
38、.1 Number of tests Analysis of a cement can require the determination of a number of its chemical elements. For each determination, one or more tests shall be carried out in which the number of measurements taken shall be as specified in the relevant clause of this part of ISO 29581. Where the analy
39、sis is one of a series subject to statistical control, the determination of each chemical element by a single test shall be the minimum required. Where the analysis method (including preparation and measurement) is checked at least once a week, as in accordance with 12.5.1, a determination of each c
40、hemical element by a single test shall be the minimum required. In the other cases, the number of tests for the determination of each chemical element shall be two; see also Clause 13. 4.2 Accuracy and precision limits 4.2.1 Accuracy limit The accuracy performance criterion in this part of ISO 29581
41、 is measured as a limit on the closeness of agreement between a test result and an accepted reference value for a certified reference material. The limits for accuracy, expressed in percent absolute, are set out in Table 2; one set is appropriate to the performance it is expected that an “expert” la
42、boratory can achieve, whereas the other is appropriate for a “normal” laboratory. 4.2.2 Repeatability limit The repeatability performance criterion in this part of ISO 29581 is measured as a limit on the repeatability where independent test results are obtained with the same method on identical test
43、 items (material) in the same laboratory by the same operator using the same equipment within a short interval of time. The limits for repeatability, expressed in percent absolute, are set out in Table 1; one set is appropriate to the performance it is expected that an “expert” laboratory can achiev
44、e, whereas the other is appropriate to a “normal” laboratory. 4.2.3 Reproducibility limit The reproducibility performance criterion in this part of ISO 29581 is measured as a limit on the reproducibility where test results are obtained with the same method on identical test items (material) in diffe
45、rent laboratories with different operators using different equipment. The limits for reproducibility, expressed in percent absolute, are set out in Table 3; one set is appropriate to the performance it is expected that an “expert” laboratory can achieve, whereas the other is appropriate to a “normal
46、” laboratory. 4.2.4 Laboratory competence The laboratory shall demonstrate that it can achieve the required performance in accordance with 12.3.3 and 12.3.4. 4.3 Expression of mass Express mass in grams to the nearest 0,000 5. 4.4 Other methods Other methods may be used, provided they are calibrated
47、, either against the reference method or against internationally accepted reference materials, in order to demonstrate their equivalence. BS ISO 29581-2:2010ISO 29581-2:2010(E) 4 ISO 2010 All rights reserved5 Reagents and reference materials 5.1 Pure reagents Reagents shall be of analytical quality
48、and, wherever possible, pure oxides or carbonates, except for the calibration of such elements as sulfur, chlorine, bromine or phosphorus, which do not form stable oxides or carbonates, where some guarantee of stoichiometry is required. Reagents shall be free of (or corrected for) the presence of wa
49、ter (and, in the case of oxides, carbon dioxide) when weighed out for fusion. Also, the reagents shall be in a known oxidation state. The specified procedure ensures that the correct oxidation state is obtained. The reagents used to prepare the standard beads for cations shall be pure oxides or carbonates of at least 99,95 % purity (excluding moisture or CO2). Reagents shall be used in a known stoichiometry in terms of content. In order to achieve this, they can be treated before use as follows. a) Determine the loss on
