《ISO-16962-2005.pdf》由会员分享，可在线阅读，更多相关《ISO-16962-2005.pdf（38页珍藏版）》请在三一文库上搜索。
1、 Reference number ISO 16962:2005(E) ISO 2005 INTERNATIONAL STANDARD ISO 16962 First edition 2005-10-01 Surface chemical analysis Analysis of zinc- and/or aluminium-based metallic coatings by glow-discharge optical- emission spectrometry Analyse chimique des surfaces Analyse des revtements mtalliques
2、 base de zinc et/ou daluminium par spectromtrie dmission optique dcharge luminescente Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Qatar Petroleum/5943408001 Not for Resale, 04/12/2007 00:22:18 MDTNo reproduction or networking permitted wit
3、hout license from IHS -,-,- ISO 16962:2005(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer perf
4、orming the editing. In downloading this file, parties accept therein the responsibility of not infringing Adobes licensing policy. The ISO Central Secretariat accepts no liability in this area. Adobe is a trademark of Adobe Systems Incorporated. Details of the software products used to create this P
5、DF file can be found in the General Info relative to the file; the PDF-creation parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central
6、Secretariat at the address given below. ISO 2005 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 th
7、e 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 2005 All rights reserved Copyright International Organizati
8、on for Standardization Provided by IHS under license with ISO Licensee=Qatar Petroleum/5943408001 Not for Resale, 04/12/2007 00:22:18 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 16962:2005(E) ISO 2005 All rights reserved iii Contents Page Foreword iv 1 Scope . 1 2 N
9、ormative references. 1 3 Principle. 1 4 Apparatus 2 4.1 Glow discharge optical emission spectrometer 2 4.2 Minimum performance requirements . 2 5 Sampling 4 6 Procedure 4 6.1 Selection of spectral lines . 4 6.2 Optimizing the glow discharge spectrometer system settings . 5 6.3 Calibration . 8 6.4 Va
10、lidation of the calibration. 11 6.5 Verification and drift correction 12 6.6 Analysis of test samples 13 7 Expression of results . 13 7.1 Quantitative depth profile 13 7.2 Determination of total coating mass per unit area 13 7.3 Determination of average mass fractions 14 8 Precision 14 9 Test report
11、 . 15 Annex A (normative) Calculation of calibration constants and quantitative evaluation of depth profiles. 16 Annex B (informative) Suggested spectral lines for determination of given elements 24 Annex C (informative) Determination of coating mass per unit area 25 Annex D (informative) Additional
12、 information on interlaboratory tests . 29 Bibliography. 32 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Qatar Petroleum/5943408001 Not for Resale, 04/12/2007 00:22:18 MDTNo reproduction or networking permitted without license from IHS -,-,
13、- ISO 16962:2005(E) iv ISO 2005 All rights reserved Foreword ISO (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. Ea
14、ch 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 Internatio
15、nal 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. The main task of technical committees is to prepare International Standards. Draft International Standar
16、ds 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 vote. Attention is drawn to the possibility that some of the elements of this document may be the subject
17、of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 16962 was prepared by Technical Committee ISO/TC 201, Surface chemical analysis, Subcommittee SC 8, Glow discharge spectroscopy. It is based on the results from project SMT-CT96-2080, funded by the
18、 EC Industrial and Materials Technologies Programme. The project was initiated by ECISS/TC 20. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Qatar Petroleum/5943408001 Not for Resale, 04/12/2007 00:22:18 MDTNo reproduction or networking perm
19、itted without license from IHS -,-,- INTERNATIONAL STANDARD ISO 16962:2005(E) ISO 2005 All rights reserved 1 Surface chemical analysis Analysis of zinc- and/or aluminium-based metallic coatings by glow-discharge optical-emission spectrometry 1 Scope This International Standard specifies a glow disch
20、arge optical emission spectrometric 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
21、 is applicable to zinc contents 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 10 mass %; lead contents between 0,0
22、05 mass % and 2 mass %; antimony contents between 0,005 mass % and 2 mass %. 2 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
23、enced document (including any amendments) applies. ISO 14707, Surface chemical analysis Glow discharge optical emission spectrometry (GD-OES) Introduction to use ISO 14284, Steel and iron Sampling and preparation of samples for the determination of chemical composition ISO 17925, Zinc and/or alumini
24、um based coatings on steel Determination of coating mass per unit area and chemical composition Gravimetry, inductively coupled plasma atomic emission spectrometry and flame atomic absorption spectrometry 3 Principle The analytical method described here involves the following processes: a) Cathodic
25、sputtering of the surface coating in a direct current or radio frequency glow discharge device. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Qatar Petroleum/5943408001 Not for Resale, 04/12/2007 00:22:18 MDTNo reproduction or networking per
26、mitted without license from IHS -,-,- ISO 16962:2005(E) 2 ISO 2005 All rights reserved b) Excitation of the analyte atoms in the plasma formed in the glow discharge device. c) Spectrometric measurement of the intensities of characteristic emission spectral lines of the analyte atoms as a function of
27、 sputtering time (depth profile). d) Conversion of the depth profile 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 meas
28、ured sputtering rate. 4 Apparatus 4.1 Glow discharge optical emission spectrometer Required instrumentation includes an optical emission spectrometer system consisting of a Grimm type 1 or similar glow discharge source (direct current or radio frequency powered) and a simultaneous optical spectromet
29、er as described in ISO 14707, incorporating suitable spectral lines for the analyte elements (see Annex B for suggested lines). The inner diameter of the hollow anode of the glow discharge source shall be in the range 2 mm to 8 mm. A cooling device for thin samples, such as a metal block with circul
30、ating cooling liquid, is also recommended, but not strictly necessary for implementation of the method. Since the determination is based on continuous sputtering of the surface coating, the spectrometer shall be equipped with a digital readout system for time-resolved measurement of the emission int
31、ensities. A system capable of a data acquisition speed of at least 500 measurements/second per spectral channel is recommended, but for the applications within the scope of this International Standard a speed of 2 measurements/second per spectral channel may be acceptable. 4.2 Minimum performance re
32、quirements 4.2.1 General It is desirable for the instrument to conform to the performance specifications given in 4.2.2 and 4.2.3, and evaluated in 6.2.7. NOTE Setting up for analysis commonly requires an iterative approach to the adjustment of the various experimental parameters. 4.2.2 Minimum repe
33、atability The following test shall be performed in order to check that the instrument is functioning properly in terms of repeatability. Perform 10 emission intensity measurements on a homogeneous bulk sample with an analyte content exceeding 1 mass %. The glow discharge conditions shall be those se
34、lected for the actual analysis. These measurements shall be performed using a discharge stabilization time (often referred to as “preburn”) of at least 60 s and a data acquisition time in the range 5 s to 20 s. Each measurement shall be located on a newly prepared surface of the sample. Calculate th
35、e relative standard deviation of the 10 measurements. The relative standard deviation shall conform to any requirements and/or specifications relevant to the intended use. NOTE Typical relative standard deviations determined in this way are 2 % or less. Copyright International Organization for Stand
36、ardization Provided by IHS under license with ISO Licensee=Qatar Petroleum/5943408001 Not for Resale, 04/12/2007 00:22:18 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 16962:2005(E) ISO 2005 All rights reserved 3 4.2.3 Detection limit 4.2.3.1 General Detection limits
37、are instrument-dependent and matrix-dependent. Consequently, the detection limit for a given analyte cannot be uniquely determined for every available instrument or for the full range of Zn/Al-based alloys considered here. For the purposes of this International Standard, the detection limit for each
38、 analyte will be acceptable if it is equal to or less than one-fifth of the lowest mass fraction expected in the coating or one- fifth of the lower end of the range of mass fractions quoted in Clause 1 of this International Standard, whichever is greater. 4.2.3.2 SNR method The first method is often
39、 called the SNR (signal-to-noise ratio) method. In order to determine the detection limit for a given analyte, the following steps shall be performed: 1) Select a bulk sample to be used as a blank. The composition of the sample shall be similar to that of the coatings to be analysed in terms of the
40、elemental composition of the matrix. Further, it shall be known to contain less than 0,1 g/g of the analyte. 2) Perform ten replicate burns on the blank. For each burn, acquire the emission intensity at the analytical wavelength for 10 s. These are the background emission intensity measurements. The
41、 glow discharge conditions used shall be the same as those that will be used in the analysis of the coated samples. For each measurement, the blank shall be preburned at these conditions for a sufficient length of time to achieve stable signals prior to the quantification of the emission intensity.
42、Use an unsputtered area of the surface of the blank for each individual burn. 3) Compute the detection limit, expressed as a mass fraction, using the following equation: 3 DL S m = (1) where DL is the detection limit; S is the standard deviation of the ten background intensity measurements performed
43、 in step 2; m is the analytical sensitivity derived from the instrument calibration, expressed as the ratio of intensity to mass fraction. If the detection limit calculated is unacceptable, repeat the test. If the second value calculated is also unacceptable, then the cause shall be investigated and
44、 corrected prior to analysing samples. 4.2.3.3 SBR-RSDB method The second method, which does not require a blank, is often called the SBR-RSDB (signal-to-background ratio relative standard deviation of the background) method. The method is performed as follows: 1) Select a bulk sample that has a mat
45、rix composition that is similar to that of the coatings to be analysed, and for which the mass fraction of the analyte is greater than 0,1 % and known. If an analytical transition that is prone to self-absorption (see 6.1) is to be used, then the mass fraction of the analyte shall not exceed 1 %. 2)
46、 Perform three replicate burns on the chosen sample. For each burn, integrate the emission intensity at the analytical wavelength for 10 s. The glow discharge conditions used shall be similar to those that will be used in the analysis of the coated samples. For each measurement, the sample shall be
47、preburned at these conditions for a sufficient length of time to achieve stable signals prior to the quantification of the Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Qatar Petroleum/5943408001 Not for Resale, 04/12/2007 00:22:18 MDTNo rep
48、roduction or networking permitted without license from IHS -,-,- ISO 16962:2005(E) 4 ISO 2005 All rights reserved emission intensity. Use an unsputtered area of the surface of the sample for each individual burn. Average the three replicate emission intensities. 3) Select a peak-free region of the emission spectrum within 0,2 nm of the analytical peak. Perform ten replicate burns on the chosen sample. For each burn, integrate the intensity at the peak-free region for 10 s. These are the measurements of the backgro