1、BSI Standards PublicationMicrobeam analysis Electron probe microanalysis Guidelines for the specification of certified reference materials(CRMs)BS ISO 14595:2014National forewordThis British Standard is the UK implementation of ISO 14595:2014.Attention is drawn to the fact that, during the developme
2、nt of thisInternational Standard, the UK committee voted against its approval as anInternational Standard.This was due to an ambiguity in the formatting of equations 4, 20 and A8.The expression of the term sigma subscript the mean value ( ) squared isshown as follows:The UK committee would expect th
3、is to be displayed as:2The UK participation in its preparation was entrusted to TechnicalCommittee CII/9, Microbeam analysis.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisions ofa
4、contract. Users are responsible for its correct application. The British Standards Institution 2014Published by BSI Standards Limited 2014ISBN 978 0 580 86899 3ICS 71.040.30; 71.040.99Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published
5、under the authority of theStandards Policy and Strategy Committee on 31 December 2014. Amendments issued since publicationAmd. No. Date Text affectedBRITISH STANDARDBS ISO 14595:2014wswsw2National forewordThis British Standard is the UK implementation of ISO 14595:2014.Attention is drawn to the fact
6、 that, during the development of thisInternational Standard, the UK committee voted against its approval as anInternational Standard.This was due to an ambiguity in the formatting of equations 4, 20 and A8.The expression of the term sigma subscript the mean value ( ) squared isshown as follows:The U
7、K committee would expect this to be displayed as:2The UK participation in its preparation was entrusted to TechnicalCommittee CII/9, Microbeam analysis.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all th
8、e necessary provisions ofa contract. Users are responsible for its correct application. The British Standards Institution 2014Published by BSI Standards Limited 2014ISBN 978 0 580 86899 3ICS 71.040.30; 71.040.99Compliance with a British Standard cannot confer immunity fromlegal obligations.This Brit
9、ish Standard was published under the authority of theStandards Policy and Strategy Committee on 31 December 2014. Amendments issued since publicationAmd. No. Date Text affectedBRITISH STANDARDBS ISO 14595:2014wswsw2National forewordThis British Standard is the UK implementation of ISO 14595:2014.Att
10、ention is drawn to the fact that, during the development of thisInternational Standard, the UK committee voted against its approval as anInternational Standard.This was due to an ambiguity in the formatting of equations 4, 20 and A8.The expression of the term sigma subscript the mean value ( ) squar
11、ed isshown as follows:The UK committee would expect this to be displayed as:2The UK participation in its preparation was entrusted to TechnicalCommittee CII/9, Microbeam analysis.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does no
12、t purport to include all the necessary provisions ofa contract. Users are responsible for its correct application. The British Standards Institution 2014Published by BSI Standards Limited 2014ISBN 978 0 580 86899 3ICS 71.040.30; 71.040.99Compliance with a British Standard cannot confer immunity from
13、legal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 December 2014. Amendments issued since publicationAmd. No. Date Text affectedBRITISH STANDARDBS ISO 14595:2014wswsw2This British Standard is the UK implementation of ISO 1459
14、5:2014.Attention is drawn to the fact that, during the development of thisInternational Standard, the UK committee voted against its approval as anInternational Standard.This was due to an ambiguity in the formatting of equations 4, 20 and A8.The expression of the term sigma subscript the mean value
15、 ( ) squared isshown as follows:The UK committee would expect this to be displayed as:The UK participation in its preparation was entrusted to TechnicalCommittee CII/9, Microbeam analysis.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publicatio
16、n does not purport to include all the necessary provisions ofa contract. Users are responsible for its correct application. The British Standards Institution 2014Published by BSI Standards Limited 2014ISBN 978 0 580 86899 3ICS 71.040.30; 71.040.99itish Standarlegal obligations.This British Standard
17、was published under the authority of theAmd. No. Date Text affected2Amendments/corrigenda issued since publicationNational forewordThis British Standard is the UK implementation of ISO 14595:2014.Attention is drawn to the fact that, during the development of thisInternational Standard, the UK commit
18、tee voted against its approval as anInternational Standard.This was due to an ambiguity in the formatting of equations 4, 20 and A8.The expression of the term sigma subscript the mean value ( ) squared isshown as follows:The UK committee would expect this to be displayed as:2The UK participation in
19、its preparation was entrusted to TechnicalCommittee CII/9, Microbeam analysis.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisions ofa contract. Users are responsible for its correct
20、 application. The British Standards Institution 2014Published by BSI Standards Limited 2014ISBN 978 0 580 86899 3ICS 71.040.30; 71.040.99Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and
21、Strategy Committee on 31 December 2014. Amendments issued since publicationAmd. No. Date Text affectedBRITISH STANDARDBS ISO 14595:2014wswsw22.This British Standard is the UK implementation of ISO 14595:2014. It supersedes BS ISO 14595:2003, which is withdrawn. ISO 2014Microbeam analysis Electron pr
22、obe microanalysis Guidelines for the specification of certified reference materials (CRMs)Analyse par microfaisceaux Microanalyse par sonde lectrons Lignes directrices pour les spcifications des matriaux de rfrence certifis (CRM)INTERNATIONAL STANDARDISO14595Second edition2014-10-15Reference numberI
23、SO 14595:2014(E)BS ISO 14595:2014ISO 14595:2014(E)ii ISO 2014 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2014All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including
24、photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 0
25、9 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 14595:2014ISO 14595:2014(E) ISO 2014 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Preparation of the research material . 24.1 Selection of material
26、. 24.2 Preliminary inspection of the material 25 Heterogeneity of material . 25.1 Sample preparation 25.2 Sample size . 25.3 Test conditions 35.4 Test procedure . 45.5 Statistical evaluation of data . 45.6 Criteria for certification. 86 Stability of the research material . 87 Determination of the ch
27、emical composition of CRMs 97.1 Classification of CRMs . 97.2 Determination of classification of CRMs . 97.3 Selection of analytical method 97.4 CRM material tested by EPMA only . 98 CRM specimen preparation, packaging, transportation, and storage 98.1 Preparation of CRM specimen . 98.2 Packaging .
28、98.3 Storage 108.4 Repolishing and recoating of CRMs 109 CRM certificate .109.1 Classification of CRM 109.2 Contents of the certificate 10Annex A (informative) Spreadsheet instructions for the statistical evaluation of heterogeneity data 11Annex B (normative) Suggested classification of CRMs for EPM
29、A 14Annex C (informative) Example of a certificate for EPMA CRMs .15Bibliography .16BS ISO 14595:2014ISO 14595:2014(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Stand
30、ards 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-governmental, in liaison with ISO, also ta
31、ke part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In pa
32、rticular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).Attention is drawn to the possibility that some of the elements of
33、 this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see
34、www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to
35、the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 202, Microbeam analysis, Subcommittee SC 2, Electron probe microanalysis.This second edition cancels and replaces the first edi
36、tion (ISO 14595:2003), which has been technically revised. It also incorporates Technical Correction ISO 14595:2003/Cor 1:2005.iv ISO 2014 All rights reservedBS ISO 14595:2014ISO 14595:2014(E)IntroductionFor electron probe microanalysis (EPMA), a comparative quantitative analytical method used throu
37、ghout the world, certified reference materials (CRMs) play a crucial role in the analytical accuracy.This International Standard has been developed to facilitate international exchange and compatibility of analysis data in EPMA.It gives guidance on evaluating and selecting reference materials (RMs),
38、 on evaluating the extent of heterogeneity and stability of RMs, and it gives recommendations for the determination of the chemical composition of RMs for production as EPMA-certified reference materials. ISO 2014 All rights reserved vBS ISO 14595:2014Microbeam analysis Electron probe microanalysis
39、Guidelines for the specification of certified reference materials (CRMs)1 ScopeThis International Standard gives recommendations for single-phase certified reference materials (CRMs) used in electron probe microanalysis (EPMA). It also provides guidance on the use of CRMs for the microanalysis of fl
40、at, polished specimens. It does not cover organic or biological materials.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated refer
41、ences, the latest edition of the referenced document (including any amendments) applies.ISO Guide 31:2000, Reference materials Contents of certificates and labels3 Terms and definitionsFor the purposes of document, the following terms and definitions apply.3.1heterogeneitymeasured variation in compo
42、sitions of elements measured from a group of specimensNote 1 to entry: The contributions to heterogeneity include the uncertainties in the measurements from specimen to specimen, from micrometre to micrometre within each specimen, and from the test procedure itself.3.2research materialmaterial that
43、appears to have the physical and chemical characteristics required of a CRM, but which is to be examined in detail, including the determination of chemical composition, stability, and micro-heterogeneity and macro-heterogeneity, before certification as a CRM3.3stabilityresistance of a specimen to ch
44、emical and physical change during long-term storage at normal temperature and pressure3.4stabilityresistance of the material to changes in chemical composition during electron bombardment, i.e. the resistance to change of the intensity of the relevant characteristic X-rays observed during the time t
45、he specimen is exposed to the electron beam3.5uncertaintyquantitative statement that provides a value for the expected deviation of a measurement from an estimate of the value of the specific measured quantityINTERNATIONAL STANDARD ISO 14595:2014(E) ISO 2014 All rights reserved 1BS ISO 14595:2014ISO
46、 14595:2014(E)4 Preparation of the research material4.1 Selection of materialThe research material used for the preparation of a CRM should exhibit little or no heterogeneity on a micrometre scale, should be free from unwanted inclusions, and should be sufficiently dense (such that voids, if present
47、, can be readily avoided during testing and analysis) and stable under prolonged electron bombardment.The mounted research material should be of sufficient size to provide several areas suitable for point beam analysis; each area should be approximately 20 m or more in diameter. At a minimum, the si
48、ze should be at least twice the area of X-ray emission.The quantity of research material should be adequate for the preparation of certified specimens.In the case of a synthetic RM, a detailed description of the preparation technique should be provided. In the case of minerals, the geographic origin
49、, the source, and the separation process should be specified.4.2 Preliminary inspection of the materialInitial inspection of a possible research material for a CRM should be made using a binocular optical microscope to evaluate the material for the presence of unwanted inclusions, voids, or other phases, and if these are found to be sufficiently abundant to interfere with EPMA of the major phase of interest, i.e. to prevent a clean samp
