BS ISO 11438-5-1994 Ferronickel - Determination of trace-element content by electrothermal atomic absorption spectrometric method - Determination of tellurium content《镍铁合金 采用电热原子吸收.pdf

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1、BRITISH STANDARD BS ISO 11438-5:1993 Implementation of ISO11438-5:1993 Ferronickel Determination of trace-element content by electrothermal atomic absorption spectrometric method Part 5: Determination of tellurium content UDC 669.245:543.422.064:546.24BSISO11438-5:1993 This BritishStandard, having b

2、een prepared under the directionof the Non-ferrous Metals Standards Policy Committee, was published underthe authority of the Standards Board and comes into effect on 15May1994 BSI 02-2000 The following BSI references relate to the work on this standard: Committee reference NFM/10 Draft for comment9

3、2/42090 DC ISBN 0 580 23355 3 Committees responsible for this BritishStandard The preparation of this BritishStandard was entrusted by the Non-ferrous Metals Standards Policy Committee (NFM/-) to Technical Committee NFM/10, upon which the following bodies were represented: Association of Bronze and

4、Brass Founders British Non-ferrous Metals Federation British Stainless Steel Association British Steel Industry Department of Trade and Industry (Laboratory of the Government Chemist) Engineering Equipment and Materials Users Association Institute of British Foundrymen London Metal Exchange Ministry

5、 of Defence Nickel Development Institute Non-ferrous Metal Stockists Steel Casting Research and Trade Association Coopted members Amendments issued since publication Amd. No. Date CommentsBSISO11438-5:1993 BSI 02-2000 i Contents Page Committees responsible Inside front cover National foreword ii For

6、eword iii Text of ISO11438-5 1BSISO11438-5:1993 ii BSI 02-2000 National foreword This BritishStandard reproduces verbatim ISO11438-5:1993 and implements it as the UK national standard. This BritishStandard is published under the direction of the Non-ferrous Metals Standards Policy Committee whose Te

7、chnical 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 European developments and promulgat

8、e them in the UK. NOTEInternational and European Standards, as well as overseas standards, are available from Customer Services, Publications, BSI, Linford Wood, Milton Keynes, MK146LE. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standa

9、rds 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, pagesi andii, theISO title page, pagesii to iv, pages1 and 2 and a back cove

10、r. 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.ISO11438-5:1993(E) ii BSI 02-2000 Contents Page Foreword iii 1 Scope 1 2 Normative references 1 3 Principle 1 4 Reagents 1 5 Appara

11、tus 1 6 Sampling and sample preparation 1 7 Procedure 1 7.1 Preparation of the test solution 1 7.2 Blank test 1 7.3 Determination by the standard additions method 1 7.3.1 Atomic absorption measurements 1 7.3.2 Semi-quantitative estimation of the tellurium content 1 7.3.3 Quantitative determination o

12、f the tellurium content 1 7.3.4 Plotting of standard additions 1 7.4 Number of determinations 1 8 Expression of results 2 8.1 Calculation 2 8.1.1 Semi-quantitative estimation of the tellurium content 2 8.1.2 Quantitative determination of the tellurium content 2 8.1.3 Calculation of the tellurium con

13、tent 2 8.2 Precision 2 8.2.1 Laboratory tests 2 8.2.2 Statistical analysis 2 9 Test report 2 Table 1 Nominal composition of test samples 2 Table 2 Results of statistical analysis 2ISO11438-5:1993(E) BSI 02-2000 iii Foreword ISO (the International Organization for Standardization) is a worldwide fede

14、ration 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 represented on that commi

15、ttee. 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 adopted by the te

16、chnical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least75% of the member bodies casting a vote. International Standard ISO11438-5 was prepared by Technical Committee ISO/TC155, Nickel and nickel alloys, Sub-Committee S

17、C3, Analysis of nickel and ferronickel. ISO11438 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 co

18、ntent; 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.iv blankISO11438-5:1993(E) BSI 02-2000 1 1 S

19、cope This part of ISO11438 specifies an electrothermal atomic absorption spectrometric method for the determination of tellurium in the range of0,3g/t to2,0g/t in ferronickel, according to the principle of standard additions. The general requirements concerning the apparatus, sampling, dissolution o

20、f the test sample, procedure, calculation and test report are given in ISO11438-1. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this part of ISO11438. At the time of publication, the editions indicated were valid. A

21、ll standards are subject to revision, and parties to agreements based on this part of ISO11438 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. IS

22、O5725:1986, Precision of test methods Determination of repeatability and reproducibility for a standard test method by inter-laboratory tests. ISO11438-1:1993, Ferronickel Determination of trace-element content by electrothermal atomic absorption spectrometric method Part1: General requirements and

23、sample dissolution. 3 Principle Dissolution of a test 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 of214,3nm by an atomic absorption spectrometer fitted with a graphite furnace electrothermal at

24、omizer. Calibration by the standard additions method described in ISO11438-1. 4 Reagents In addition to the reagents listed in ISO11438-1, the following special reagents are required. 4.1 Tellurium, standard reference solution(1000mg/l). Weigh, to the nearest0,001g,0,100g of tellurium metal of99,9%

25、(m/m) minimum purity. Transfer to a100ml beaker and dissolve in5ml of nitric acid ( 20 =1,41g/ml) diluted1+1. Heat until completely dissolved. Boil to expel nitrogen oxides. Cool the solution and transfer to a100ml one-mark volumetric flask. Add5ml of nitric acid ( 20 =1,41g/ml), make up to the mark

26、 with water and mix thoroughly. 4.2 Tellurium, standard solution(10,0mg/l). Pipette10,0ml of the tellurium standard reference solution(4.1) into a1000ml one-mark volumetric flask containing50ml of nitric acid ( 20 =1,41g/ml) diluted1+1. Make up to the mark with water and mix thoroughly. This solutio

27、n shall be prepared on the day of use. 4.3 Tellurium, working standard solution(1,0mg/l). Pipette10,0ml of the tellurium standard solution(4.2) into a100ml one-mark volumetric flask containing5ml of nitric acid ( 20 =1,41g/ml) diluted1+1. Make up to the mark with water and mix thoroughly. This solut

28、ion shall be freshly prepared. 5 Apparatus The apparatus required is specified in clause5 of ISO11438-1:1993. 6 Sampling and sample preparation Refer to clause6 of ISO11438-1:1993. 7 Procedure 7.1 Preparation of the test solution Proceed as directed in7.1 of ISO11438-1:1993. 7.2 Blank test Refer to7

29、.2 of ISO11438-1:1993. 7.3 Determination by the standard additions method 7.3.1 Atomic absorption measurements Use the peak area integration absorbance measurement at a wavelength of214,3nm and proceed with checking the electrothermal atomizer as directed in7.3.1 of ISO11438-1:1993. 7.3.2 Semi-quant

30、itative estimation of the tellurium content Proceed as directed in7.3.2 of ISO11438-1:1993. 7.3.3 Quantitative determination of the tellurium content Proceed as directed in7.3.3 of ISO11438-1:1993. 7.3.4 Plotting of standard additions Proceed as directed in7.3.4 of ISO11438-1:1993. NOTE 1The procedu

31、re is applicable to the linear part of the graphs. 7.4 Number of determinations Carry out the determination at least in duplicate.ISO11438-5:1993(E) 2 BSI 02-2000 8 Expression of results 8.1 Calculation 8.1.1 Semi-quantitative estimation of the tellurium content Proceed as directed in8.1.1 of ISO114

32、38-1:1993. 8.1.2 Quantitative determination of the tellurium content Proceed as directed in8.1.2 of ISO11438-1:1993. 8.1.3 Calculation of the tellurium content Calculate the tellurium content w Teof the test sample, in grams per tonne, using the formula 8.2 Precision 8.2.1 Laboratory tests Seven lab

33、oratories 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 interlaboratory test programme were evaluated according to ISO

34、5725 as described in8.2.2 of ISO11438-1:1993. The results of this analysis are given in Table 2. 8.2.2.2 One laboratory gave no results for sample1. All the laboratories passed statistical tests. 9 Test report Refer to clause10 of ISO11438-1:1993. Table 1 Nominal composition of test samples Table 2

35、Results of statistical analysis where Te is the tellurium concentration, in micrograms per litre, found in the “zero” test solution, in accordance with8.1.2 of ISO11438-1:1993; m is the mass, in grams, of the test portion; w Te F Te 10 m - = F is the dilution factor of2,5. Sample Content, g/t Conten

36、t, % (m/m) Pb Sb Sn Te Tl Ag In Bi As Se Cd Ga Ge Zn Ni Fe 1 1 1 1 0,5 0,5 1 0,5 0,1 3 0,5 0,5 2 1 2 25 Remainder 2 6 4 10 2 1 6 2 1 5 3 1 4 4 5 25 Remainder Sample 1 2 Mean w Te , g/t 0,35 1,97 Within-laboratory standard deviation 0,1 0,2 Between-laboratory standard deviation 0,1 0,2 Repeatability

37、0,2 0,6 Reproducibility 0,4 0,7blankBS ISO 11438-5:1993 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing BritishStandards. It presents the UK view on standards in Europe and at the international level. It is incorp

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