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1、BRITISH STANDARD BS ISO 11438-7:1993 Implementation of ISO 11438-7:1993 Ferronickel Determination of trace-element content by electrothermal atomic absorption spectrometric method Part 7: Determination of silver content UDC 669.245:543.422.064:546.57 Licensed Copy: sheffieldun sheffieldun, na, Mon N
2、ov 27 07:22:17 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 11438-7:1993 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 02-200
3、0 The following BSI references relate to the work on this standard: Committee reference NFM/10 Draft for comment 92/42092 DC ISBN 0 580 23357 X 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)
5、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.DateCommen
6、ts Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:22:17 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 11438-7:1993 BSI 02-2000i Contents Page Committees responsibleInside front cover National forewordii Forewordiii Text of ISO 11438-71 Licensed Copy: sheffieldun sheffieldun, na, Mon N
7、ov 27 07:22:17 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 11438-7:1993 ii BSI 02-2000 National foreword This British Standard reproduces verbatim ISO 11438-7:1993 and implements it as the UK national standard. This British Standard is published under the direction of the Non-ferrous Metals St
8、andards 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 Eu
9、ropean 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
10、 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, pages
11、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 07:22:17 GMT+00:00 2006, Uncontrolle
12、d Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:22:17 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11438-7:1993(E) ii BSI 02-2000 Contents Page Forewordiii 1Scope1 2Normative references1 3Principle1 4Reagents1 5Apparatus1 6Sampling and sample preparation1 7Procedure1 7.1P
13、reparation 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 silver content1 7.3.3Quantitative determination of the silver content1 7.3.4Plotting of standard additions1 7.4Number of de
14、terminations1 8Expression of results2 8.1Calculation2 8.1.1Semi-quantitative estimation of the silver content2 8.1.2Quantitative determination of the silver content2 8.1.3Calculation of the silver content2 8.2Precision2 8.2.1Laboratory tests2 8.2.2Statistical analysis2 9Test report2 Table 1 Nominal
15、composition of test samples2 Table 2 Results of statistical analysis2 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:22:17 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11438-7:1993(E) BSI 02-2000iii Foreword ISO (the International Organization for Standardization) is a worldwide federat
16、ion 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 committe
17、e. 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 techn
18、ical 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 11438-7 was prepared by Technical Committee ISO/TC 155, Nickel and nickel alloys, Sub-Committee
19、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: Determination of lead
20、 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: sheffieldun sheffieldun,
21、na, Mon Nov 27 07:22:17 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv blank Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:22:17 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11438-7:1993(E) BSI 02-20001 1 Scope This part of ISO 11438 specifies an electrothermal atomic absorption spectro
22、metric method for the determination of silver in the range of 1,0 g/t to 6,0 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 1143
23、8-1. 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 agreements based on this
24、 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 repeatability and re
25、producibility 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 a
26、cid. Measurement of the absorption of the resonance line energy from the spectrum of silver in the test solution at a wavelength of 328,1 nm by an atomic absorption spectrometer fitted with a graphite furnace electrothermal atomizer. Calibration by the standard additions method described in ISO 1143
27、8-1. 4 Reagents In addition to the reagents listed in ISO 11438-1, the following special reagents are required. 4.1 Silver, standard reference solution (1 000 mg/l). Weigh, to the nearest 0,001 g, 1,000 g of silver metal of 99,9 % (m/m) minimum purity. Transfer to a 250 ml beaker and dissolve in a m
28、ixture of 10 ml of nitric 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 S
29、ilver, standard solution (10,0 mg/l). Pipette 10,0 ml of the silver 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
30、 of use. 4.3 Silver, working standard solution (1,0 mg/l). Pipette 10,0 ml of the silver 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 pre
31、pared. 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 to 7.2 of ISO 11438-1
32、: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 328,1 nm and proceed with checking the electrothermal atomizer as directed in 7.3.1 of ISO 11438-1:1993. 7.3.2 Semi-quantitative esti
33、mation of the silver content Proceed as directed in 7.3.2 of ISO 11438-1:1993. 7.3.3 Quantitative determination of the silver 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 applic
34、able 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 07:22:17 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11438-7:1993(E) 2 BSI 02-2000 8 Expression of results 8.1 Calculation
35、8.1.1 Semi-quantitative estimation of the silver content Proceed as directed in 8.1.1 of ISO 11438-1:1993. 8.1.2 Quantitative determination of the silver content Proceed as directed in 8.1.2 of ISO 11438-1:1993. 8.1.3 Calculation of the silver content Calculate the silver content wAg of the test sam
36、ple, in grams per tonne, using the formula 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
37、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 was rejected as a Cochran outlier for sample 1. 9 Test report Refer to clause 10 of ISO 11
38、438-1:1993. Table 1 Nominal composition of test samples Table 2 Results of statistical analysis where Agis the silver 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; wAg FAg 10m -= F
39、is the dilution factor of 2,5. Sample Content, g/tContent, % (m/m) PbSbSnTeTIAgInBiAsSeCdGaGeZnNiFe 11110,50,510,5 0,1 30,50,521225Remainder 264102162153144525Remainder Sample12 Mean wAg, g/t0,925,91 Within-laboratory standard deviation0,050,4 Between-laboratory standard deviation0,10,9 Repeatabilit
40、y0,151,1 Reproducibility0,42,7 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:22:17 GMT+00:00 2006, Uncontrolled Copy, (c) BSI blank Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:22:17 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 11438-7:1993 BSI 389 Chiswick High Road Lo
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