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1、BRITISH STANDARD BS ISO 11438-5:1993 Implementation of ISO 11438-5:1993 Ferronickel Determination of trace-element content by electrothermal atomic absorption spectrometric method Part 5: Determination of tellurium content UDC 669.245:543.422.064:546.24 Licensed Copy: sheffieldun sheffieldun, na, Mo
2、n Nov 27 07:22:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 11438-5:1993 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-
3、2000 The following BSI references relate to the work on this standard: Committee reference NFM/10 Draft for comment 92/42090 DC ISBN 0 580 23355 3 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Non-ferrous Metals Standards Policy Commit
4、tee (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 Chemis
5、t) Engineering 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.DateCom
6、ments Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:22:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 11438-5:1993 BSI 02-2000i Contents Page Committees responsibleInside front cover National forewordii Forewordiii Text of ISO 11438-51 Licensed Copy: sheffieldun sheffieldun, na, Mo
7、n Nov 27 07:22:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 11438-5:1993 ii BSI 02-2000 National foreword This British Standard reproduces verbatim ISO 11438-5:1993 and implements it as the UK national standard. This British Standard is published under the direction of the Non-ferrous Metals
8、 Standards 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
9、 European 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 o
10、f a contract. 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, pag
11、es ii 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 07:22:09 GMT+00:00 2006, Uncontro
12、lled Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:22:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11438-5:1993(E) ii BSI 02-2000 Contents Page Forewordiii 1Scope1 2Normative references1 3Principle1 4Reagents1 5Apparatus1 6Sampling and sample preparation1 7Procedure1 7
13、.1Preparation 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 tellurium content1 7.3.3Quantitative determination of the tellurium content1 7.3.4Plotting of standard additions1 7.4Num
14、ber of determinations1 8Expression of results2 8.1Calculation2 8.1.1Semi-quantitative estimation of the tellurium content2 8.1.2Quantitative determination of the tellurium content2 8.1.3Calculation of the tellurium content2 8.2Precision2 8.2.1Laboratory tests2 8.2.2Statistical analysis2 9Test report
15、2 Table 1 Nominal composition of test samples2 Table 2 Results of statistical analysis2 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:22:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11438-5:1993(E) BSI 02-2000iii Foreword ISO (the International Organization for Standardization) is a
16、 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 committee has been established has the right to be represente
17、d 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 electrotechnical standardization. Draft International Standards ad
18、opted 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. International Standard ISO 11438-5 was prepared by Technical Committee ISO/TC 155, Nickel and nickel allo
19、ys, Sub-Committee SC 3, Analysis 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: Det
20、ermination of lead content; Part 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: sheffie
21、ldun sheffieldun, na, Mon Nov 27 07:22:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv blank Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:22:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11438-5:1993(E) BSI 02-20001 1 Scope This part of ISO 11438 specifies an electrothermal atomic
22、absorption spectrometric method for the determination of tellurium in the range of 0,3 g/t to 2,0 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
23、are given in ISO 11438-1. 2 Normative 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 agr
24、eements based on this part of ISO 11438 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
25、 repeatability and reproducibility 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 tes
26、t portion in nitric acid. Measurement of the absorption of the resonance line energy from the spectrum of tellurium in the test solution at a wavelength of 214,3 nm by an atomic absorption spectrometer fitted with a graphite furnace electrothermal atomizer. Calibration by the standard additions meth
27、od described in ISO 11438-1. 4 Reagents In addition to the reagents listed in ISO 11438-1, the following special reagents are required. 4.1 Tellurium, standard reference solution (1 000 mg/l). Weigh, to the nearest 0,001 g, 0,100 g of tellurium metal of 99,9 % (m/m) minimum purity. Transfer to a 100
28、 ml beaker and dissolve in 5 ml of nitric acid (20= 1,41 g/ml) diluted 1 + 1. Heat until completely dissolved. Boil to expel nitrogen oxides. Cool the solution and transfer to a 100 ml one-mark volumetric flask. Add 5 ml of nitric acid (20= 1,41 g/ml), make up to the mark with water and mix thorough
29、ly. 4.2 Tellurium, standard solution (10,0 mg/l). Pipette 10,0 ml of the tellurium 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 prep
30、ared on the day of use. 4.3 Tellurium, working standard solution (1,0 mg/l). Pipette 10,0 ml of the tellurium 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
31、 shall be freshly prepared. 5 Apparatus The apparatus 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
32、to 7.2 of ISO 11438-1:1993. 7.3 Determination by the standard additions method 7.3.1 Atomic absorption measurements Use the peak area integration absorbance measurement at a wavelength of 214,3 nm and proceed with checking the electrothermal atomizer as directed in 7.3.1 of ISO 11438-1:1993. 7.3.2 S
33、emi-quantitative estimation of the tellurium content Proceed as directed in 7.3.2 of ISO 11438-1:1993. 7.3.3 Quantitative determination of the tellurium 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. NO
34、TE 1The procedure is applicable to the linear part of the graphs. 7.4 Number of determinations Carry out the determination at least in duplicate. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:22:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11438-5:1993(E) 2 BSI 02-2000 8 Expression
35、of results 8.1 Calculation 8.1.1 Semi-quantitative estimation of the tellurium content Proceed as directed in 8.1.1 of ISO 11438-1:1993. 8.1.2 Quantitative determination of the tellurium content Proceed as directed in 8.1.2 of ISO 11438-1:1993. 8.1.3 Calculation of the tellurium content Calculate th
36、e tellurium content wTe of the test sample, in grams per tonne, using the formula 8.2 Precision 8.2.1 Laboratory tests Seven 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 di
37、fferent days. 8.2.2 Statistical analysis 8.2.2.1 Results from the interlaboratory 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 One laboratory gave no results for sample 1. All the laboratorie
38、s passed statistical tests. 9 Test report Refer to clause 10 of ISO 11438-1:1993. Table 1 Nominal composition of test samples Table 2 Results of statistical analysis where Teis the tellurium concentration, in micrograms per litre, found in the “zero” test solution, in accordance with 8.1.2 of ISO 11
39、438-1:1993; mis the mass, in grams, of the test portion; wTe FTe 10m - -= Fis the dilution factor of 2,5. Sample Content, g/tContent, % (m/m) PbSbSnTeTlAgInBiAsSeCdGaGeZnNiFe 11110,50,510,5 0,130,50,521225Remainder 264102162153144525Remainder Sample12 Mean wTe, g/t0,351,97 Within-laboratory standard
40、 deviation0,10,2 Between-laboratory standard deviation0,10,2 Repeatability0,20,6 Reproducibility0,40,7 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:22:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI blank Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:22:09 GMT+00:00 2006, Unco
41、ntrolled Copy, (c) BSI BS ISO 11438-5:1993 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent 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
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