1、BSI Standards PublicationBS ISO 19272:2015Low alloyed steel Determination of C, Si, Mn, P,S, Cr, Ni, Al, Ti and Cu - Glowdischarge optical emissionspectrometry (routine method)BS ISO 19272:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 19272:2015.The UK p
2、articipation in its preparation was entrusted to TechnicalCommittee ISE/102, Methods of Chemical Analysis for Iron and Steel.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a
3、contract. Users are responsible for its correctapplication. The British Standards Institution 2015. Published by BSI StandardsLimited 2015ISBN 978 0 580 66322 2ICS 77.140.20Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the a
4、uthority of theStandards Policy and Strategy Committee on 31 August 2015.Amendments issued since publicationDate Text affectedBS ISO 19272:2015 ISO 2015Low alloyed steel Determination of C, Si, Mn, P, S, Cr, Ni, Al, Ti and Cu - Glow discharge optical emission spectrometry (routine method)Aciers faib
5、lement allis Dtermination de C, Si, Mn, P, S, Cr, Ni, Al, Ti et Cu Spectromtrie dmission optique dcharge luminescente (mthode de routine)INTERNATIONAL STANDARDISO19272First edition2015-08-15Reference numberISO 19272:2015(E)BS ISO 19272:2015ISO 19272:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PR
6、OTECTED DOCUMENT ISO 2015, 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 posting on the internet or an intranet, without pr
7、ior 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 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 19
8、272:2015ISO 19272:2015(E)Foreword iv1 Scope . 12 Normative references 13 Principle 24 Apparatus . 24.1 Glow discharge optical emission spectrometer 24.1.1 General 24.1.2 Short term stability 24.1.3 Detection limit . 24.1.4 Data acquisition and processing system . 24.1.5 Others 25 Sampling 36 Procedu
9、re. 36.1 Sample preparation 36.2 Selection of spectral lines 36.3 Optimization of the instrument 46.3.1 General 46.3.2 Setting the discharge parameters of a direct current (DC) source . 46.3.3 Setting the discharge parameters of radiofrequency (RF) source 56.3.4 Optimization of the detection system
10、66.3.5 Pre-burning time and integration time 66.3.6 Validation of the instrumental parameters . 66.4 Calibration 66.5 Checking of the trueness of the method 76.6 Drift correction . 76.7 Analysis of the samples 77 Expression of results 77.1 Method of calculation 77.2 Precision . 78 Test report 11Anne
11、x A (informative) Detection limit.12Annex B (informative) Additional information on international interlaboratory test .14Annex C (informative) Graphical representation of precision data 22Bibliography .32 ISO 2015 All rights reserved iiiContents PageBS ISO 19272:2015ISO 19272:2015(E)ForewordISO (th
12、e 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 technical committ
13、ee 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 electrotechn
14、ical 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 was drafted i
15、n 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 patent rights.
16、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 not constitute a
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18、responsible for this document is ISO/TC 17, Steel, Subcommittee SC 1, Method of determination of chemical composition.iv ISO 2015 All rights reservedBS ISO 19272:2015INTERNATIONAL STANDARD ISO 19272:2015(E)Low alloyed steel Determination of C, Si, Mn, P, S, Cr, Ni, Al, Ti and Cu - Glow discharge opt
19、ical emission spectrometry (routine method)1 ScopeThis International Standard specifies a glow discharge optical emission spectrometric (GD-OES) method for determination of the mass fraction Carbon, Silicon, Manganese, Phosphorus, Sulfur, Chromium, Nickel, Aluminium, Titanium and Copper in low alloy
20、ed steels.The content ranges to which the method is applicable are shown in Table 1.Table 1 Content rangesElementContent rangesmass fraction%C 0,060 to 0,35Si 0,14 to 1,50Mn 0,090 to 0,70P 0,010to 0,070S 0,005 to 0,050Cr 0,008 to 0,65Ni 0,050 to 0,50Al 0,006 to 0,90Ti 0,014 to 0,13Cu 0,005 to 1,002
21、Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable to its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendment
22、s) applies.ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitionsISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a
23、standard measurement methodISO 5725-3, Accuracy (trueness and precision) of measurement methods and results Part 3: Intermediate measures of the precision of a standard measurement methodISO 14284, Steel and iron Sampling and preparation of samples for the determination of chemical compositionISO 14
24、707, Surface chemical analysis Glow discharge optical emission spectrometry (GD-OES) Introduction to use ISO 2015 All rights reserved 1BS ISO 19272:2015ISO 19272:2015(E)3 PrincipleThe method used involves the following steps:a) a sample with a flat and smooth surface is used as the cathode of a dire
25、ct current or radio frequency glow discharge device;b) cathodic sputtering of the sample surface, atomization of the sputtered atoms and ions from the sample surface; excitation of these atoms and ions in the plasma formed in the glow discharge device;c) spectrometric measurement of the intensity of
26、 the emitted light from the ions or the atoms of the elements to be determined and, optionally, the emitted light from iron at 371,994 nm or 271,441 nm or another appropriate wavelength (if internal standard is used);d) conversion of the measured signals to the contents through calibration curves es
27、tablished by measuring certified reference materials.4 Apparatus4.1 Glow discharge optical emission spectrometer4.1.1 GeneralAn optical emission spectrometer system consists of a Grimm type or similar glow discharge source (direct current or radio frequency powered) and a simultaneous optical spectr
28、ometer as described in ISO 14707, with suitable spectral lines for the elements to be determined. A sequential optical system may also be used alone or combined with simultaneous channels.A 2 mm to 8 mm range of the inner diameter of the anode of the glow discharge is recommended. A cooling device i
29、s also recommended, but not strictly required for implementation of the method. The anode-cathode gap is normally around 0,1 mm to 0,3 mm; otherwise, follow the instrument manufacturers instructions.4.1.2 Short term stabilityCarry out at least 10 measurements of the emission intensity of an element
30、having a content around the corresponding upper limit specified in this International Standard on an appropriate sample. Allow the discharge to stabilize for at least 50 s before each measurement. The data acquisition time should be in the range of 5 s to 30 s. Each measurement shall be carried out
31、on a newly polished surface of the sample. Calculate the corresponding standard deviation and mean. The relative standard deviation (RSD) should not exceed 5 % for contents less than 0,5 %, otherwise, the RSD should not exceed 3 %.4.1.3 Detection limitDetection limits may be determined by either the
32、 SNR method or SBR-CVB method (see A.1 and A.2).4.1.4 Data acquisition and processing systemThe data acquisition and processing system is conducted by a computer, equipped with software suitable for controlling the instrument parameters and running the test programs.4.1.5 OthersFor other basic requi
33、rements of the instrument, use ISO 14707.2 ISO 2015 All rights reservedBS ISO 19272:2015ISO 19272:2015(E)5 SamplingCarry out sampling in accordance with ISO 14284 or appropriate national standards for steel.6 Procedure6.1 Sample preparationSamples shall be homogeneous, flat and free of porosity. The
34、 surface of the sample shall be prepared by using suitable methods to ensure cleanliness and flatness. Surface preparation may be achieved by using abrasive-wheel or milling machine. All the reference materials and samples shall be prepared under the same conditions and their size should be suitable
35、 for the glow discharge source used.6.2 Selection of spectral linesFor each element to be determined, there are a number of spectral lines that can be used. Suitable lines shall be selected on the basis of several factors, including the spectral range of the spectrometer used, element concentration,
36、 sensitivity of the spectral lines and spectral interference from other elements present in the samples. Table 2 contains some suggestions concerning suitable spectral lines. With these lines, no obvious inter-element interferences are observed in low alloyed steels. Spectral lines other than those
37、listed may be used, if they have favourable characteristics, but special attention needs to be paid to the influence of co-existing elements and corrections might be required.Table 2 Suggested wavelengths for the analysis of low alloy steelsElementWavelengthnmFe371,994271,441C165,700156,143Si288,158
38、251,611Mn403,449257,610P177,497178,287S 180,731Cr 425,433Ni349,296341,477Al 396,152Ti337, 279365,350Cu219,228327, 396 ISO 2015 All rights reserved 3BS ISO 19272:2015ISO 19272:2015(E)6.3 Optimization of the instrument6.3.1 GeneralFollow the manufacturers instructions or other suitable documented proc
39、edures to start and set the GD-OES and let it stabilize. Check, or adjust if necessary, the entrance slit in accordance with the manufacturers instructions to ensure it is correctly positioned so that the intensity is measured at the peak of the spectral line in order to obtain the best signal to ba
40、ckground ratio (make reference to ISO 14707 for further information). Carry out at least three preliminary discharges on a generic sample before any measurement procedures.NOTE Analyte lines are centred by adjusting the entrance slit whilst carrying out discharges on a reference material. It is advi
41、sable to profile the instrument on a daily basis for a newly installed instrument during the first week of operation and then periodically over time. Profiling is carried out initially on all lines or at least on those included in each analytical program or by following the recommendations of the in
42、strument manufacturer.Follow manufacturers recommendation or other suitable documented procedures to select or adjust all instrumental parameters: evacuation time, argon purging time pumpdown cycles, glow discharge spectrometer opening mode startup time, flush time cleaning time, sputtering time, et
43、c.6.3.2 Setting the discharge parameters of a direct current (DC) sourceDC glow discharge spectrometers usually have three parameters (current, voltage and pressure) to be controlled. Any two of these three parameters may be fixed to constant values by varying the third one. The user may adopt the f
44、ollowing procedures, or any other mode recommended by the manufacturers.6.3.2.1 Constant applied voltage and currentThe controlled parameters are applied voltage and current. Set the power supply of the glow discharge source to constant voltage and constant current operation. Firstly, set the voltag
45、e and current to typical values recommended by the manufacturer or reliable values. If the recommended values are not available or not suitable for the task, following steps could be pursued to determine the optimum parameters.Set the high voltage of the detectors as described in 6.3.4.Step one: set
46、 an initial value or the value recommended by the manufacturer for current and voltage (initial discharge condition). For DC glow discharge, electrical current is normally in the range of 5 mA to 10 mA for a 2 mm to 2,5 mm anode, 15 mA to 45 mA for a 4 mm anode and 40 mA to 100 mA for a 7 mm to 8 mm
47、 anode. Voltage is usually in the range of 600 V to 1250 V. Determine the intensities corresponding to an appropriate sample under the initial discharge condition. Fix one parameter (current or voltage), and change the other one gradually. Measure the intensities at least seven times at each setting
48、. Do this at the entire parameter range allowed by the instrument.Step two: fix the parameter which changed in step one and gradually change the other parameter. Repeat the operation as described in step one.Step three: calculate the CVs of the measurements for each setting. Investigate the influenc
49、e of the discharge parameters on the intensities and CVs and fix the optimum instrumental condition.6.3.2.2 Constant applied current and pressureThe controlled parameters are applied current and pressure. Set the power supply of the glow discharge source to constant current and constant pressure operation. Firstly, set the current and pressure to typical values recommended by the manufacturer or values suitably documented. If the recommended values are not available or not suitable for the task, the following steps could
