BS ISO 19668-2017 Surface chemical analysis X-ray photoelectron spectroscopy Estimating and reporting detection limits for elements in homogeneous materials《表面化学分析 X射线光电子能谱学 同质材料中元.pdf

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1、Surface chemical analysis X-ray photoelectron spectroscopy Estimating and reporting detection limits for elements in homogeneous materialsBS ISO 19668:2017BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06 ISO 2017Surface chemical analysis X-ray photoelectron spectrosc

2、opy Estimating and reporting detection limits for elements in homogeneous materialsAnalyse chimique des surfaces Spectroscopie de photolectrons par rayons X Estimation et production de rapports sur les limites de dtection des lments contenus dans les matriaux homognesINTERNATIONAL STANDARDISO19668Fi

3、rst edition2017-08Reference numberISO 19668:2017(E)National forewordThis British Standard is the UK implementation of ISO 19668:2017.The UK participation in its preparation was entrusted to Technical Committee CII/60, Surface chemical analysis.A list of organizations represented on this committee ca

4、n be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2017 Published by BSI Standards Limited 2017ISBN 978 0 580 92393 7ICS 71.040.40Compl

5、iance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 September 2017.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS ISO 19668:2017 IS

6、O 2017Surface chemical analysis X-ray photoelectron spectroscopy Estimating and reporting detection limits for elements in homogeneous materialsAnalyse chimique des surfaces Spectroscopie de photolectrons par rayons X Estimation et production de rapports sur les limites de dtection des lments conten

7、us dans les matriaux homognesINTERNATIONAL STANDARDISO19668First edition2017-08Reference numberISO 19668:2017(E)BS ISO 19668:2017ISO 19668:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of

8、this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including 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

9、 the country of the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 19668:2017ISO 19668:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in Swi

10、tzerlandAll 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 photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be r

11、equested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgISO 19668:2017(E)Foreword ivIntroduction v1 Scope .

12、12 Normative references 13 Terms and definitions . 14 Symbols and abbreviated terms . 15 Calculating and reporting detection limits from XPS data . 35.1 General . 35.2 Required data . 55.3 XPS measurements 55.3.1 General 55.3.2 Composition of the sample . 55.3.3 Spectra for detection limit calculati

13、on 65.4 Calculation of background noise . 75.4.1 General 75.4.2 Standard deviation of intensity from counts . 75.4.3 Standard deviation of intensity from background fit . 85.5 Calculation of the elemental detection limit 95.5.1 Calculation of the minimal detectable summed intensity 95.5.2 Calculatio

14、n of the XPS detection limit . 95.6 Reporting the elemental detection limit 10Annex A (informative) Uncertainties associated with XPS detection limits .11Annex B (informative) Definition of XPS detection limits .15Annex C (informative) Examples 16Annex D (informative) Detection limit conversions 22B

15、ibliography .24 ISO 2017 All rights reserved iiiContents PageBS ISO 19668:2017ISO 19668:2017(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carrie

16、d 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 take part in the work. IS

17、O 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 particular the different

18、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 this document may b

19、e 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 www .iso .org/ paten

20、ts).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 voluntary nature of standards, the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about

21、ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www .iso .org/ iso/ foreword .html.This document was prepared by Technical Committee ISO/TC 201, Surface chemical analysis, Subcommittee SC 7, Electron spectroscopies.iv IS

22、O 2017 All rights reservedBS ISO 19668:2017ISO 19668:2017(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committ

23、ees. 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 take part in the work. ISO collaborates closely with the Int

24、ernational 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 particular the different approval criteria needed for the di

25、fferent 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 this document may be the subject of patent rights. ISO

26、 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 www .iso .org/ patents).Any trade name used in this doc

27、ument is information given for the convenience of users and does not constitute an endorsement.For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the World Trade O

28、rganization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www .iso .org/ iso/ foreword .html.This document was prepared by Technical Committee ISO/TC 201, Surface chemical analysis, Subcommittee SC 7, Electron spectroscopies.iv ISO 2017 All rights reserved ISO 1966

29、8:2017(E)IntroductionX-ray photoelectron spectroscopy (XPS) is a technique widely employed to measure the chemical composition of material surfaces. In many applications, it is used to either confirm or deny the presence of an elemental species at a surface. In either case, it is important to unders

30、tand the minimal concentration of the element that can be detected by XPS under the measurement conditions either to provide an assessment of confidence in a result or to understand how the measurement conditions should be changed to achieve the required detection limit.This document provides a stra

31、ightforward approach to calculating detection limits in X-ray photoelectron spectroscopy from experimental data in common analytical situations. It also provides informative annexes which allow the uncertainty in the calculated detection limit to be determined (see Annex A) and describe how the XPS

32、detection limit is defined (see Annex B). Example data and calculations are provided in Annex C. Annex D contains useful conversions and references which describe how detection limits may be estimated for an X-ray photoelectron spectrometer in the absence of any data except that from a reference mat

33、erial such as clean silver.These calculations are of critical importance because the technique is routinely used to measure the concentration of elements, which are present in low concentrations at a material surface, and knowledge of the limit of detection provides a statement of confidence when no

34、 element can be detected. Furthermore, if a particular detection limit is required, it permits the analyst to calculate the acquisition time required to achieve the specified limit of detection. ISO 2017 All rights reserved vBS ISO 19668:2017Surface chemical analysis X-ray photoelectron spectroscopy

35、 Estimating and reporting detection limits for elements in homogeneous materials1 ScopeThis document specifies a procedure by which elemental detection limits in X-ray photoelectron spectroscopy (XPS) can be estimated from data for a particular sample in common analytical situations and reported. Th

36、is document is applicable to homogeneous materials and is not applicable if the depth distribution of elements is inhomogeneous within the information depth of the technique.2 Normative referencesThe following documents are referred to in the text in such a way that some or all of their content cons

37、titutes requirements of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 18115-1, Surface chemical analysis Vocabulary Part 1: General terms and terms used in spectroscopy

38、ISO 18115-2, Surface chemical analysis Vocabulary Part 2: Terms used in scanning-probe microscopy3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 18115-1 and ISO 18115-2 and the following apply.ISO and IEC maintain terminological databases for use in s

39、tandardization at the following addresses: ISO Online browsing platform: available at h t t p :/ www .iso .org/ obp IEC Electropedia: available at h t t p :/ www .electropedia .org/ 3.1reference elementchemical element present in the sample for which a peak area and relative composition can be measu

40、red3.2specified elementchemical element for which the detection limit calculation is being undertaken4 Symbols and abbreviated termsAisummed intensity of the photoelectron line of element i, counts or cpsACcritical level of detection for a peak in summed intensity, counts or cpsADminimal detectable

41、summed intensity for a peak at the required level of confidenceAMRSF average matrix relative sensitivity factoramcoefficients of order m in a polynomial equationINTERNATIONAL STANDARD ISO 19668:2017(E) ISO 2017 All rights reserved 1BS ISO 19668:2017Surface chemical analysis X-ray photoelectron spect

42、roscopy Estimating and reporting detection limits for elements in homogeneous materials1 ScopeThis document specifies a procedure by which elemental detection limits in X-ray photoelectron spectroscopy (XPS) can be estimated from data for a particular sample in common analytical situations and repor

43、ted. This document is applicable to homogeneous materials and is not applicable if the depth distribution of elements is inhomogeneous within the information depth of the technique.2 Normative referencesThe following documents are referred to in the text in such a way that some or all of their conte

44、nt constitutes requirements of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 18115-1, Surface chemical analysis Vocabulary Part 1: General terms and terms used in spect

45、roscopyISO 18115-2, Surface chemical analysis Vocabulary Part 2: Terms used in scanning-probe microscopy3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 18115-1 and ISO 18115-2 and the following apply.ISO and IEC maintain terminological databases for u

46、se in standardization at the following addresses: ISO Online browsing platform: available at h t t p :/ www .iso .org/ obp IEC Electropedia: available at h t t p :/ www .electropedia .org/ 3.1reference elementchemical element present in the sample for which a peak area and relative composition can b

47、e measured3.2specified elementchemical element for which the detection limit calculation is being undertaken4 Symbols and abbreviated termsAisummed intensity of the photoelectron line of element i, counts or cpsACcritical level of detection for a peak in summed intensity, counts or cpsADminimal dete

48、ctable summed intensity for a peak at the required level of confidenceAMRSF average matrix relative sensitivity factoramcoefficients of order m in a polynomial equationINTERNATIONAL STANDARD ISO 19668:2017(E) ISO 2017 All rights reserved 1 ISO 19668:2017(E)at.% atomic percent concentration average e

49、mission angle of electrons relative to the surface normal of the sampleB(E) function of E describing background, counts or cpsBE binding energyb number of data points that define the background under a peakc number of data points from b that are used in a summed intensity measurementcps counts per secondd diameter of the atoms of the specified elementA(x)relative uncertainty of peak intensity, AxSrelative uncertainty of the detection limit, S(B)relative uncertainty of the standard