1、BS ISO 16962:2017Surface chemical analysis Analysis of zinc- and/oraluminium-based metalliccoatings by glow-dischargeoptical-emission spectrometryBSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS ISO 16962:2017 BRITISH STANDARDNational forewordThis British Standard
2、is the UK implementation of ISO 16962:2017. The UK participation in its preparation was entrusted to Technical Committee CII/60, Surface chemical analysis.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include al
3、l 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 86888 7 ICS 71.040.40Compliance with a British Standard cannot confer immunity from legal obligations.This British
4、 Standard was published under the authority of the Standards Policy and Strategy Committee on 31 March 2017.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 16962:2017 ISO 2017Surface chemical analysis Analysis of zinc- and/or aluminium-based metallic coatings by glow
5、-discharge optical-emission spectrometryAnalyse chimique des surfaces Analyse des revtements mtalliques base de zinc et/ou daluminium par spectromtrie dmission optique dcharge luminescenteINTERNATIONAL STANDARDISO16962Second edition2017-02Reference numberISO 16962:2017(E)BS ISO 16962:2017ISO 16962:2
6、017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in SwitzerlandAll 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 p
7、osting 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 officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41
8、 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 16962:2017ISO 16962:2017(E)Foreword vIntroduction vi1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 15 Apparatus . 25.1 Glow-discharge optical-emission spectrometer 25.1.1 General 25.1.2 Selection of spectral lines . 25.1.3 Sel
9、ection of glow-discharge source type . 26 Adjusting the glow-discharge spectrometer system settings 36.1 General . 36.2 Setting the parameters of a DC source . 46.2.1 Constant applied current and voltage . 46.2.2 Constant applied current and pressure . 56.2.3 Constant voltage and pressure 56.3 Setti
10、ng the discharge parameters of an RF source . 66.3.1 General 66.3.2 Constant applied power and pressure 66.3.3 Constant applied power and DC bias voltage 66.3.4 Constant effective power and effective RF voltage . 76.4 Minimum performance requirements 76.4.1 General 76.4.2 Minimum repeatability . 76.
11、4.3 Detection limit . 87 Sampling 98 Calibration 98.1 General . 98.2 Calibration samples . 108.2.1 General. 108.2.2 Brass calibration samples . 108.2.3 Zn-Al alloy samples .108.2.4 Low alloy iron or steel samples 108.2.5 Stainless steel samples 108.2.6 Nickel alloy samples .108.2.7 Aluminium-silicon
12、 alloy samples . 108.2.8 Aluminium-magnesium alloy samples.108.2.9 High-purity copper and zinc samples .118.3 Validation samples and optional RMs for calibration 118.3.1 General. 118.3.2 Zinc-nickel electrolytically coated RM .118.3.3 Zinc-iron electrolytically coated RM 118.3.4 Zinc-aluminium hot d
13、ip coated RM 118.3.5 Zinc-iron hot dip coated and annealed RM .118.4 Determination of the sputtering rate of calibration and validation specimens .118.5 Emission intensity measurements of calibration specimens 138.6 Calculation of calibration equations 138.7 Validation using reference materials 138.
14、7.1 General. 138.7.2 Checking analytical accuracy using bulk reference materials .13 ISO 2017 All rights reserved iiiContents PageBS ISO 16962:2017ISO 16962:2017(E)8.7.3 Checking analytical accuracy using surface layer reference materials 148.8 Verification and drift correction . 149 Analysis of tes
15、t specimens .159.1 Adjusting discharge parameters . 159.2 Setting of measuring time and data acquisition rate 159.3 Quantifying depth profiles of test specimens 1510 Expression of results .1510.1 Expression of quantitative depth profile . 1510.2 Determination of total coating mass per unit area (coa
16、ting aeric mass) 1710.2.1 General method 1710.2.2 Method for special applications . 1710.3 Determination of average mass fractions . 1711 Precision 1712 Test report 18Annex A (normative) Calculation of calibration constants and quantitative evaluation of depth profiles 19Annex B (informative) Sugges
17、tions concerning suitable spectral lines 31Annex C (informative) Determination of coating mass per unit area (coating areic mass) .32Annex D (informative) Additional information on international cooperative tests 38Bibliography .40iv ISO 2017 All rights reservedBS ISO 16962:2017ISO 16962:2017(E)Fore
18、wordISO (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 committees. Each member body interested in a subject for which a techni
19、cal 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 International Electrotechnical Commission (IEC) on all matters of e
20、lectrotechnical 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 different types of ISO documents should be noted. This document wa
21、s 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 shall not be held responsible for identifying any or all such p
22、atent 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 document is information given for the convenience of users and does
23、 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 Organization (WTO) principles in the Technical Barriers to Trade
24、(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 8, Glow discharge spectroscopy.This second edition cancels and replaces the first edition (ISO 16962:2005), which has been technica
25、lly revised. ISO 2017 All rights reserved vBS ISO 16962:2017ISO 16962:2017(E)IntroductionThis document is a revision of ISO 16962. Developments in both GD-OES instrumentation and the types of zinc- and/or aluminium-based metallic coatings currently produced have rendered ISO 16962 partly obsolete, a
26、nd this revision is intended to bring it up to date.vi ISO 2017 All rights reservedBS ISO 16962:2017Surface chemical analysis Analysis of zinc- and/or aluminium-based metallic coatings by glow-discharge optical-emission spectrometry1 ScopeThis document specifies a glow-discharge optical-emission spe
27、ctrometric method for the determination of the thickness, mass per unit area and chemical composition of metallic surface coatings consisting of zinc- and/or aluminium-based materials. The alloying elements considered are nickel, iron, silicon, lead and antimony.This method is applicable to zinc con
28、tents between 0,01 mass % and 100 mass %; aluminium contents between 0,01 mass % and 100 mass %; nickel contents between 0,01 mass % and 20 mass %; iron contents between 0,01 mass % and 20 mass %; silicon contents between 0,01 mass % and 15 mass %; magnesium contents between 0,01 mass% and 20 mass%;
29、 lead contents between 0,005 mass % and 2 mass %, antimony contents between 0,005 mass % and 2 mass %.NOTE Due to environmental and health risks, lead and antimony are avoided nowadays, but this document is also applicable to older products including these elements.2 Normative referencesThe followin
30、g documents are referred to in the text in such a way that some or all of their content 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 14284,
31、 Steel and iron Sampling and preparation of samples for the determination of chemical compositionISO 17925, Zinc and/or aluminium based coatings on steel Determination of coating mass per unit area and chemical composition Gravimetry, inductively coupled plasma atomic emission spectrometry and flame
32、 atomic absorption spectrometry3 Terms and definitionsNo terms and definitions are listed in this document.ISO and IEC maintain terminological databases for use in standardization at the following addresses: IEC Electropedia: available at h t t p :/ www .electropedia .org/ ISO Online browsing platfo
33、rm: available at h t t p :/ www .iso .org/ obp4 PrincipleThe analytical method described here involves the following processes:a) preparation of the sample to be analysed, generally in the form of a flat plate or disc of dimensions appropriate to the instrument or analytical requirement (round or re
34、ctangular samples with a width of more than 5 mm, generally 20 mm to 100 mm, are suitable);b) cathodic sputtering of the surface coating in a direct current or radio frequency glow-discharge device;INTERNATIONAL STANDARD ISO 16962:2017(E) ISO 2017 All rights reserved 1BS ISO 16962:2017ISO 16962:2017
35、(E)c) excitation of the analyte atoms in the plasma formed in the glow-discharge device;d) spectrometric measurement of the intensities of characteristic emission spectral lines of the analyte atoms and ions as a function of sputtering time (qualitative depth profile);e) conversion of the depth prof
36、ile in units of intensity versus time to mass fraction versus depth by means of calibration functions (quantification). Calibration of the system is achieved by measurements on calibration samples of known chemical composition and measured sputtering rate.5 Apparatus5.1 Glow-discharge optical-emissi
37、on spectrometer5.1.1 GeneralThe required instrumentation includes an optical-emission spectrometer system consisting of a Grimm type1or similar glow-discharge source (direct current or radio frequency powered) and a simultaneous optical spectrometer as described in ISO 14707, capable of providing su
38、itable spectral lines for the analyte elements. It is also common to combine this with a sequential spectrometer (monochromator), allowing the addition of an extra spectral channel to a depth profile measurement. An array-type detector, such as a charge coupled device (CCD) or a charge injection dev
39、ice (CID) can also be used for simultaneous detection to cover a wide spectral range of the analytical lines.The inner diameter of the hollow anode of the glow-discharge source should be in the range 2 mm to 8 mm. A cooling device for thin specimens, such as a metal block with circulating cooling li
40、quid, is also recommended, but not strictly necessary for implementation of the method.Since the principle of determination is based on continuous sputtering of the surface layer, the spectrometer shall be equipped with a digital readout system for time-resolved measurement of the emission intensiti
41、es. A system capable of a data acquisition speed of at least 300 measurements/second per spectral channel is recommended, but for a large number of applications speeds of 50 measurements/second per spectral channel are acceptable. In practice, it has been established that 10 to 100 measurements/seco
42、nd per spectral channel are suitable.5.1.2 Selection of spectral linesFor each analyte to be determined, there exist a number of spectral lines which can be used. Suitable lines shall be selected on the basis of several factors, including the spectral range of the spectrometer used, the analyte mass
43、 fraction range, the sensitivity of the spectral lines and any spectral interference from other elements present in the test specimens. For applications where several of the analytes of interest are major elements in the specimens, special attention shall be paid to the occurrence of self-absorption
44、 of certain highly sensitive spectral lines (so-called “resonance lines”). Self-absorption causes non-linear calibration curves at high analyte mass fraction levels, and strongly self-absorbed lines should therefore be avoided for the determination of major elements. Suggestions concerning suitable
45、spectral lines are given in Annex B. Spectral lines other than those listed may be used, so long as they have favourable characteristics.5.1.3 Selection of glow-discharge source type5.1.3.1 Anode sizeMost GD-OES instruments on the market are delivered with options to use various anode diameters, 2 m
46、m, 4 mm and 8 mm being the most common. Some older instruments have one anode only, usually 8 mm, while the most commonly used anode in modern instruments is 4 mm. A larger anode requires larger specimens and higher power during analysis; therefore, the specimen is heated to a greater extent. On the
47、 other hand, a larger anode gives rise to a plasma of larger volume that emits more light, resulting in lower detection limits (i.e. higher analytical sensitivity). Furthermore, a larger anode helps 2 ISO 2017 All rights reservedBS ISO 16962:2017ISO 16962:2017(E)to mask inhomogeneity within a surfac
48、e layer. This may or may not be an advantage, depending on the application. In a large number of applications, the 4 mm anode is a good compromise. However, in surface analysis applications, it is rather common to encounter problems of overheating of the specimens due to surface layers of poor heat
49、conductivity and/or very thin specimens, for example. In such cases, a smaller anode (typically 2 or 2,5 mm) is preferable, even if there is some loss of analytical sensitivity.5.1.3.2 Type of power supplyThe glow-discharge source can be either a type powered by a direct current (DC) power supply or a radio frequency (RF) type. The most important difference is that the RF type can sputter both conductive and non-conductive specimens; hence, this is the only type that can be used for polymer coatings and insulating oxide layers,
