《BS-ISO-11438-2-1993.pdf》由会员分享，可在线阅读，更多相关《BS-ISO-11438-2-1993.pdf（12页珍藏版）》请在三一文库上搜索。
1、BRITISH STANDARD BS ISO 11438-2:1993 Implementation of ISO 11438-2:1993 Ferronickel Determination of trace-element content by electrothermal atomic absorption spectrometric method Part 2: Determination of lead content UDC 669.245:543.422.064:546.815 Licensed Copy: sheffieldun sheffieldun, na, Mon No
2、v 27 07:21:52 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 11438-2:1993 This British Standard, having been prepared under the direction of the Non-ferrous Metals Standards Policy Committee, was published under the authority of the Standards Board and comes into effect on 15 May 1994 BSI 02-2000
3、 The following BSI references relate to the work on this standard: Committee reference NFM/10 Draft for comment 92/42087 DC ISBN 0 580 23352 9 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Non-ferrous Metals Standards Policy Committee
4、(NFM/-) to Technical Committee NFM/10, upon which the following bodies were represented: Association of Bronze and Brass Founders British Non-ferrous Metals Federation British Stainless Steel Association British Steel Industry Department of Trade and Industry (Laboratory of the Government Chemist) E
5、ngineering Equipment and Materials Users Association Institute of British Foundrymen London Metal Exchange Ministry of Defence Nickel Development Institute Non-ferrous Metal Stockists Steel Casting Research and Trade Association Coopted members Amendments issued since publication Amd. No.DateComment
6、s Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:21:52 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 11438-2:1993 BSI 02-2000i Contents Page Committees responsibleInside front cover National forewordii Forewordiii Text of ISO 11438-21 Licensed Copy: sheffieldun sheffieldun, na, Mon No
7、v 27 07:21:52 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 11438-2:1993 ii BSI 02-2000 National foreword This British Standard reproduces verbatim ISO 11438-2:1993 and implements it as the UK national standard. This British Standard is published under the direction of the Non-ferrous Metals Sta
8、ndards Policy Committee whose Technical Committee NFM 10 has the responsibility to: aid enquirers to understand the text; present to the responsible international committee any enquiries on interpretation, or proposals for change, and keep UK interests informed: monitor related international and Eur
9、opean developments and promulgate them in the UK. NOTEInternational and European Standards as well as overseas standards, are available from Customer Services, Publications, BSI, Linford Wood, Milton Keynes, MK14 6LE. A British Standard does not purport to include all the necessary provisions of a c
10、ontract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the ISO title page, pages ii
11、 to iv, pages 1 and 2 and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:21:52 GMT+00:00 2006, Uncontrolled
12、Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:21:52 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11438-2:1993(E) ii BSI 02-2000 Contents Page Forewordiii 1Scope1 2Normative references1 3Principle1 4Reagents1 5Apparatus1 6Sampling and sample preparation1 7Procedure1 7.1Pre
13、paration of the test solution1 7.2Blank test1 7.3Determination by the standard additions method1 7.3.1Atomic absorption measurements1 7.3.2Semi-quantitative estimation of the lead content1 7.3.3Quantitative determination of the lead content1 7.3.4Plotting of standard additions1 7.4Number of determin
14、ations1 8Expression of results2 8.1Calculation2 8.1.1Semi-quantitative estimation of the lead content2 8.1.2Quantitative determination of the lead content2 8.1.3Calculation of the lead content2 8.2Precision2 8.2.1Laboratory tests2 8.2.2Statistical analysis2 9Test report2 Table 1 Nominal composition
15、of test samples2 Table 2 Results of statistical analysis2 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:21:52 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11438-2:1993(E) BSI 02-2000iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of natio
16、nal 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 committee has been established has the right to be represented on that committee. Internati
17、onal 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 electrotechnical standardization. Draft International Standards adopted by the technical committ
18、ees 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. International Standard ISO 11438-2 was prepared by Technical Committee ISO/TC 155, Nickel and nickel alloys, Sub-Committee SC 3, Analys
19、is of nickel and ferronickel. ISO 11438 consists of the following parts, under the general title Ferronickel Determination of trace-element content by electrothermal atomic absorption spectrometric method: Part 1: General requirements and sample dissolution; Part 2: Determination of lead content; Pa
20、rt 3: Determination of antimony content; Part 4: Determination of tin content; Part 5: Determination of tellurium content; Part 6: Determination of thallium content; Part 7: Determination of silver content; Part 8: Determination of indium content. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov
21、27 07:21:52 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv blank Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:21:52 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11438-2:1993(E) BSI 02-20001 1 Scope This part of ISO 11438 specifies an electrothermal atomic absorption spectrometric metho
22、d for the determination of lead in the range of 1,0 g/t to 5,0 g/t in ferronickel, according to the principle of standard additions. The general requirements concerning the apparatus, sampling, dissolution of the test sample, procedure, calculation and test report are given in ISO 11438-1. 2 Normati
23、ve references The following standards contain provisions which, through reference in this text, constitute provisions of this part of ISO 11438. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this part of ISO 1
24、1438 are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 5725:1986, Precision of test methods Determination of repeatability and reproducibility
25、for a standard test method by inter-laboratory tests. ISO 11438-1:1993, Ferronickel Determination of trace-element content by electrothermal atomic absorption spectrometric method Part 1: General requirements and sample dissolution. 3 Principle Dissolution of a test portion in nitric acid. Measureme
26、nt of the absorption of the resonance line energy from the spectrum of lead in the test solution at a wavelength of 283,3 nm by an atomic absorption spectrometer fitted with a graphite furnace electrothermal atomizer. Calibration by the standard additions method described in ISO 11438-1. 4 Reagents
27、In addition to the reagents listed in ISO 11438-1, the following special reagents are required. 4.1 Lead, standard reference solution (1 000 mg/l). Weigh, to the nearest 0,001 g, 1,000 g of lead metal of 99,9 % (m/m) minimum purity. Transfer to a 100 ml beaker and dissolve in a mixture of 10 ml of n
28、itric acid (20= 1,41 g/ml) and 20 ml of water. Heat until completely dissolved. Boil to expel nitrogen oxides. Cool the solution and transfer to a 1 000 ml one-mark volumetric flask. Add 10 ml of nitric acid (20= 1,41 g/ml), make up to the mark with water and mix thoroughly. 4.2 Lead, standard solut
29、ion (10,0 mg/l). Pipette 10,0 ml of the lead standard reference solution (4.1) into a 1 000 ml one-mark volumetric flask containing 50 ml of nitric acid (20= 1,41 g/ml) diluted 1 + 1. Make up to the mark with water and mix thoroughly. This solution shall be prepared on the day of use. 4.3 Lead, work
30、ing standard solution (1,0 mg/l). Pipette 10,0 ml of the lead standard solution (4.2) into a 100 ml one-mark volumetric flask containing 5 ml of nitric acid (20= 1,41 g/ml) diluted 1 + 1. Make up to the mark with water and mix thoroughly. This solution shall be freshly prepared. 5 Apparatus The appa
31、ratus required is specified in clause 5 of ISO 11438-1:1993. 6 Sampling and sample preparation Refer to clause 6 of ISO 11438-1:1993. 7 Procedure 7.1 Preparation of the test solution Proceed as directed in 7.1 of ISO 11438-1:1993. 7.2 Blank test Refer to 7.2 of ISO 11438-1:1993. 7.3 Determination by
32、 the standard additions method 7.3.1 Atomic absorption measurements Use the peak area integration absorbance measurement at a wavelength of 283,3 nm and proceed with checking the electrothermal atomizer as directed in 7.3.1 of ISO 11438-1:1993. 7.3.2 Semi-quantitative estimation of the lead content
33、Proceed as directed in 7.3.2 of ISO 11438-1:1993. 7.3.3 Quantitative determination of the lead content Proceed as directed in 7.3.3 of ISO 11438-1:1993. 7.3.4 Plotting of standard additions Proceed as directed in 7.3.4 of ISO 11438-1:1993. NOTE 1The procedure is applicable to the linear part of the
34、graphs. 7.4 Number of determinations Carry out the determination at least in duplicate. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:21:52 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11438-2:1993(E) 2 BSI 02-2000 8 Expression of results 8.1 Calculation 8.1.1 Semi-quantitative estimat
35、ion of the lead content Proceed as directed in 8.1.1 of ISO 11438-1:1993. 8.1.2 Quantitative determination of the lead content Proceed as directed in 8.1.2 of ISO 11438-1:1993. 8.1.3 Calculation of the lead content Calculate the lead content wPb of the test sample, in grams per tonne, using the form
36、ula 8.2 Precision 8.2.1 Laboratory tests Six laboratories in five countries participated in the testing of this procedure using two samples of nominal composition given in Table 1. Samples were analysed three times on different days. 8.2.2 Statistical analysis 8.2.2.1 Results from the interlaborator
37、y test programme were evaluated according to ISO 5725 as described in 8.2.2 of ISO 11438-1:1993. The results of this analysis are given in Table 2. 8.2.2.2 All the laboratories passed statistical tests. 9 Test report Refer to clause 10 of ISO 11438-1:1993. Table 1 Nominal composition of test samples
38、 Table 2 Results of statistical analysis where Pbis the lead concentration, in micrograms per litre, found in the “zero” test solution, in accordance with 8.1.2 of ISO 11438-1:1993; mis the mass, in grams, of the test portion; wPb FPb 10m - -= Fis the dilution factor of 2,5. Sample Content, g/tConte
39、nt, % (m/m) PbSbSnTeTIAgInBiAsSeCdGaGeZnNiFe 11110,50,510,5 0,130,50,521225Remainder 264102162153144525Remainder Sample12 Mean wPb, g/t1,475,45 Within-laboratory standard deviation0,40,3 Between-laboratory standard deviation0,21,3 Repeatability1,00,7 Reproducibility1,23,8 Licensed Copy: sheffieldun
40、sheffieldun, na, Mon Nov 27 07:21:52 GMT+00:00 2006, Uncontrolled Copy, (c) BSI blank Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:21:52 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 11438-2:1993 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the i
41、ndependent national body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions British Standards are updated by amendment or revision. Users of British Standards should make sure that
42、 they possess the latest amendments or editions. It is the constant aim of BSI to improve the quality of our products and services. We would be grateful if anyone finding an inaccuracy or ambiguity while using this British Standard would inform the Secretary of the technical committee responsible, t
43、he identity of which can be found on the inside front cover. Tel: 020 8996 9000. Fax: 020 8996 7400. BSI offers members an individual updating service called PLUS which ensures that subscribers automatically receive the latest editions of standards. Buying standards Orders for all BSI, international
44、 and foreign standards publications should be addressed to Customer Services. Tel: 020 8996 9001. Fax: 020 8996 7001. In response to orders for international standards, it is BSI policy to supply the BSI implementation of those that have been published as British Standards, unless otherwise requeste
45、d. Information on standards BSI provides a wide range of information on national, European and international standards through its Library and its Technical Help to Exporters Service. Various BSI electronic information services are also available which give details on all its products and services.
46、Contact the Information Centre. Tel: 020 8996 7111. Fax: 020 8996 7048. Subscribing members of BSI are kept up to date with standards developments and receive substantial discounts on the purchase price of standards. For details of these and other benefits contact Membership Administration. Tel: 020
47、 8996 7002. Fax: 020 8996 7001. Copyright Copyright subsists in all BSI publications. BSI also holds the copyright, in the UK, of the publications of the international standardization bodies. Except as permitted under the Copyright, Designs and Patents Act 1988 no extract may be reproduced, stored i
48、n a retrieval system or transmitted in any form or by any means electronic, photocopying, recording or otherwise without prior written permission from BSI. This does not preclude the free use, in the course of implementing the standard, of necessary details such as symbols, and size, type or grade d
49、esignations. If these details are to be used for any other purpose than implementation then the prior written permission of BSI must be obtained. If permission is granted, the terms may include royalty payments or a licensing agreement. Details and advice can be obtained from the Copyright Manager. Tel: 020 8996 7070. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:21:52 GMT+00:00 2006, Uncontrolled Copy, (c) BSI