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1、BRITISH STANDARD BS EN 10318:2005 Determination of thickness and chemical composition of zinc- and aluminium-based metallic coatings Routine method The European Standard EN 10318:2005 has the status of a British Standard ICS 17.040.20; 25.220.40 ? Licensed Copy: sheffieldun sheffieldun, na, Thu Oct
2、26 04:39:25 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN 10318:2005 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 24 June 2005 BSI 24 June 2005 ISBN 0 580 46158 0 National foreword This British Standard is the official English language
3、version of EN 10318:2005. The UK participation in its preparation was entrusted to Technical Committee ISE/18, Sampling and analysis of Iron and Steel, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references
4、 The British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Stan
5、dards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the
6、 responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside fro
7、nt cover, the EN title page, pages 2 to 23 and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Thu Oct 26 04:39:25 GMT+00:00 2006, Unco
8、ntrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 10318 May 2005 ICS 17.040.20; 25.220.40 English version Determination of thickness and chemical composition of zinc- and aluminium-based metallic coatings - Routine method Dtermination de lpaisseur et de la composition chimi
9、que des revtements en zinc et en alliage daluminium - Mthode de routine Bestimmung der Dicke und der chemischen Zusammensetzung metallischer berzge auf Basis von Zink und Aluminium - Standard-Verfahren This European Standard was approved by CEN on 21 March 2005. CEN members are bound to comply with
10、the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat
11、 or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official ve
12、rsions. CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Swi
13、tzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2005 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. N
14、o. EN 10318:2005: E Licensed Copy: sheffieldun sheffieldun, na, Thu Oct 26 04:39:25 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 10318:2005 (E) 2 Contents Page Foreword 3 1Scope.4 2Normative references .4 3Principle.4 4Apparatus4 4.1Glow discharge optical emission spectrometer.4 4.2Data acquisition
15、 5 5Sampling5 6Procedure6 6.1Selection of spectral lines6 6.2Optimising the glow discharge spectrometer settings6 6.3Calibration.8 7Verification of the analytical accuracy 10 8Expression of results10 8.1Method of calculation .10 8.2Precision11 9Test report.17 Annex A (normative) Calculation of calib
16、ration constants and quantitative evaluation of depth profiles.18 Bibliography.23 Licensed Copy: sheffieldun sheffieldun, na, Thu Oct 26 04:39:25 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 10318:2005 (E) 3 Foreword This European Standard (EN 10318:2005) has been prepared by Technical Committee EC
17、ISS/TC 20 “Methods of chemical analysis of ferrous products”, the secretariat of which is held by SIS. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by November 2005, and conflicting national stand
18、ards shall be withdrawn at the latest by November 2005. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germa
19、ny, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: sheffieldun sheffieldun, na, Thu Oct 26 04:39:25 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN
20、10318:2005 (E) 4 1 Scope This European Standard specifies a glow discharge optical emission spectrometric method for the determination of the thickness and chemical composition of metallic surface coatings consisting of zinc and aluminium based alloys. The alloying elements considered are aluminium,
21、 nickel, silicon and lead. This method is applicable to zinc contents between 40 % (m/m) and 100 % (m/m); aluminium contents between 0,01 % (m/m) and 60 % (m/m); nickel contents between 0,01 % (m/m) and 15 % (m/m); silicon contents between 0,01 % (m/m) and 3 % (m/m); lead contents between 0,005 % (m
22、/m) and 0,1 % (m/m). 2 Normative references Not applicable. 3 Principle The analytical method described here involves the following processes: a) Cathodic sputtering of the surface coating in a direct current glow discharge device; b) Optical excitation of the analyte atoms in the plasma formed in t
23、he glow discharge device; c) Spectrometric measurement of characteristic emission spectral lines of the analyte atoms as a function of sputtering time (depth profile); and d) Conversion of the depth profile in units of intensity versus time to mass fraction versus depth by means of calibration funct
24、ions (quantification). Calibration of the system is achieved by measurements on calibration samples of known chemical composition and measured sputtering rate. 4 Apparatus 4.1 Glow discharge optical emission spectrometer 4.1.1 General An optical emission spectrometer equipped with a Grimm type (1) o
25、r similar direct current glow discharge source and a simultaneous optical spectrometer, incorporating suitable spectral lines for the analyte elements (see Table 1 for recommended lines) shall be used. The inner diameter of the hollow anode of the glow discharge shall be in the range 2 mm to 8 mm. A
26、 cooling device for thin samples, such as a metal block with circulating cooling liquid, is also recommended, but not strictly necessary for implementation of the method. It is desirable for the instrument to conform to the performance specifications given in 4.1.2 and 4.1.3, to be evaluated in 6.2.
27、6. 4.1.2 Minimum repeatability Perform 10 measurements of the emission intensity on a homogeneous bulk sample with a content of the analyte exceeding 1 % (m/m). Allow the discharge at least 60 s stabilisation time (often referred to as preburn) before each intensity measurement. Each measurement sha
28、ll be located on a newly prepared surface of the sample. Calculate the standard deviation of the 10 measurements. The standard deviation should not exceed 2 % of the mean intensity of the analyte. If this is the case, repeat the test two more times. If the high standard deviation is Licensed Copy: s
29、heffieldun sheffieldun, na, Thu Oct 26 04:39:25 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 10318:2005 (E) 5 repeatable, there is probably some malfunction in the instrument or the sample used is not homogeneous. Before proceeding, the cause of the problem should be investigated and rectified. 4.1
30、.3 Limit of detection Detection limits 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-based alloys considered here. For the purposes of this document, the de
31、tection limit for each analyte will be acceptable if it is equal to or less than one third of the lowest concentration to be determined in the intended applications. The detection limit is determined using the method explained below. a). Select a bulk sample to be used as a blank. The sample composi
32、tion should be similar to the coatings to be analyzed in terms of the elemental composition of the matrix. Further, it shall be known to contain less than 0,1 mg kg-1 of the analyte. b). Perform ten replicate burns on the blank. For each burn, acquire the emission intensity at the analytical wavelen
33、gth for 10 s. These are the background emission intensity measurements. The glow discharge conditions used should be the same as those that will be used in the analysis of the coated samples. For each measurement, the blank should be preburned at these conditions for a sufficient length of time to a
34、chieve stable signals prior to the quantification of the emission intensity. An unsputtered area of the surface of the blank for each individual burn shall be used. c). Compute the detection limit using the following equation: m S DL = 3 where DL is the detection limit; S is the standard deviation o
35、f the ten background intensity measurements performed 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 greater than one third of the lowest concentration to be determined in
36、 the intended applications, then the test should be repeated. If the second value calculated is also greater than one third of the lowest concentration to be determined in the intended applications, then there may be an instrument malfunction. In such a case, the problem should be investigated prior
37、 to analyzing unknown samples. 4.2 Data acquisition Since the principle of 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 intensities. A system with capability for
38、data acquisition speed of at least 500 measurements/second per spectral channel is recommended, but for the applications within the scope of this standard a speed of 2 measurements/second per spectral channel may be acceptable. 5 Sampling Carry out sampling in accordance with the recommendations of
39、the manufacturer of the coated material. In general, the edges of a coated strip should be avoided. The size of the test samples should be suitable for the glow discharge source used. Typically, round or rectangular samples with a width of 20 mm to 100 mm are suitable. Licensed Copy: sheffieldun she
40、ffieldun, na, Thu Oct 26 04:39:25 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 10318:2005 (E) 6 6 Procedure 6.1 Selection of spectral lines For each analyte to be determined there exists a number of spectral lines which can be used. Suitable lines shall be selected on the basis of several factors i
41、ncluding the spectral range of the spectrometer used, analyte concentration range, sensitivity of the spectral lines and spectral interference from other elements present in the samples. In this type of application, where most of the analytes of interest are major elements in the samples, special at
42、tention shall be paid to the occurrence of self-absorption of certain highly sensitive spectral lines. Self- absorption may cause severe non-linearity of calibration curves at high analyte concentration levels, and such lines should therefore be avoided for the determination of majors. In Table 1, s
43、ome suggestions concerning suitable spectral lines are given. Table 1 Suggested spectral lines for determination of given elements ElementWavelength (nm) Estimated useful concentration range % (m/m) Comments Zn 330,26 0,001 to 100 Zn 334,50 0,001 to 100 Zn 481,053 0,001 to 100 Al 172,50 0,1 to 100 A
44、l 396,15 0,001 to 100 a Self-absorption Ni 231,603 0,01 to 100 Ni 341,78 0,001 to 100 a Weak self-absorption Ni 349,30 0,005 to 100 a Weak self-absorption Pb 202,20 0,001 to 10 Pb 405,87 0,01 to 100 Si 212,41 No data available Si 251,61 No data available Si 288,16 0,001 to 20 Fe 249,318 0,01 to 100
45、Fe 259,94 0,01 to 100 Fe 271,44 0,1 to 100 Fe 371,94 0,005 to 100 a Weak self-absorption Fe 379,50 0,01 to 100 Cu 296,12 0,01 to 100 Cu 327,40 0,001 to 5 a Strong self-absorption a Use of non-linear calibration curve recommended. 6.2 Optimising the glow discharge spectrometer settings 6.2.1 General
46、Follow the manufacturers instructions for preparing the instrument for use. In particular, check that the entrance slit to the spectrometer is correctly adjusted, following the procedure given by the instrument manufacturer. This Licensed Copy: sheffieldun sheffieldun, na, Thu Oct 26 04:39:25 GMT+00
47、:00 2006, Uncontrolled Copy, (c) BSI EN 10318:2005 (E) 7 ensures that the emission intensities are measured on the peaks of the spectral lines for optimal signal to background ratio. For further information, see e.g. ISO 14707. The source parameters shall be chosen to achieve three aims: adequate sp
48、uttering of the sample, to reduce the analysis time without over-heating the coatings; good crater shape, for good depth resolution; and constant excitation conditions in calibration and analysis, for optimum accuracy. There are often tradeoffs among the three specified aims. Modern DC glow discharg
49、e spectrometers usually have provisions for complete control/measurement of the electrical parameters (current, voltage, power), allowing any two of these parameters to be locked to constant values by varying the pressure (active pressure regulation). Older spectrometers often lack an active pressure regulation system, but the pressure can still be adjusted manually to maintain nearly constant current and voltage during calibration measurements. 6.2.2 Constant applied current and