BS-6200-3.34.3-1990 ISO-9647-1989.pdf
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1、BRITISH STANDARD BS 6200-3.34.3: 1990 ISO 9647:1989 Sampling and analysis of iron, steel and other ferrous metals Part 3: Methods of analysis Section 3.34 Determination of vanadium Subsection 3.34.3 Steel and cast iron: flame atomic absorption spectrometric method Licensed Copy: sheffieldun sheffiel
2、dun, na, Wed Dec 06 15:04:49 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6200-3.34.3:1990 This British Standard, having been prepared under the direction of the Iron and Steel Standards Policy Committee, was published under the authority of the Board of BSI and comes into effect on 31 August 1990
3、BSI 10-1999 The following BSI references relate to the work on this standard: Committee reference ISM/18 Draft for comment 87/43479 DC ISBN 0 580 18430 7 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Iron and Steel Standards Policy Com
4、mittee (ISM/-) to Technical Committee ISM/18, upon which the following bodies were represented: BCIRA British Forging Industry Association British Steel Industry Department of Trade and Industry (Laboratory of the Government Chemist) Ferro Alloys and Metals Producers Association Ministry of Defence
5、Amendments issued since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 15:04:49 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6200-3.34.3:1990 BSI 10-1999i Contents Page Committees responsibleInside front cover National forewordii 1Scope1 2Normative reference
6、s1 3Principle1 4Reagents1 5Apparatus1 6Sampling2 7Procedure2 8Expression of results4 9Test report5 Annex A (informative) Additional information on the international co-operative tests6 Annex B (informative) Graphical representation of precision data7 Annex C (normative) Procedures for the determinat
7、ion of instrumental criteria8 Figure B.1 Logarithmic relationship between vanadium content % (m/m) and repeatability r or reproducibility R and Rw7 Table 13 Table 23 Table 35 Table A.16 Publication(s) referred toInside back cover Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 15:04:49 GMT+00
8、:00 2006, Uncontrolled Copy, (c) BSI BS 6200-3.34.3:1990 ii BSI 10-1999 National foreword This Subsection of BS 6200 has been prepared under the direction of the Iron and Steel Standards Policy Committee. It is identical with ISO 9647:1989 “Steel and iron Determination of vanadium content Flame atom
9、ic absorption spectrometric method”, published by the International Organization for Standardization (ISO). The Technical Committee has reviewed the provisions of ISO 377, ISO 385-1 and ISO 648, to which reference is made in the text, and has decided that they are acceptable for use in conjunction w
10、ith this standard. Related British Standards for ISO 377:1985, ISO 385-1:1984 and ISO 648:1977 are, respectively, BS 1837:1970 “Methods for the sampling of iron, steel, permanent magnet alloys and ferro-alloys”, BS 846:1985 “Specification for burettes” and BS 1583:1986 “Specification for one-mark pi
11、pettes”. Appropriate procedures from ISO 377 will be incorporated in BS 6200-2 “Methods of sampling and sample preparation”, which will be published in due course and which will supersede BS 1837. A British Standard does not purport to include all the necessary provisions of a contract. Users of Bri
12、tish Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Cross-references International StandardCorresponding British Standard ISO 1042:1983BS 1792:1982 Specification for one-mark volumetric flasks (Id
13、entical) BS 5497 Precision of test methods ISO 5725:1986Part 1:1987 Guide for the determination of repeatability and reproducibility for a standard test method by inter-laboratory tests (Identical) Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, pages 1
14、 to 10, an inside back cover 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, Wed Dec 06 15:04:49 GMT+00:00 2006, Uncont
15、rolled Copy, (c) BSI BS 6200-3.34.3:1990 BSI 10-19991 1 Scope This International Standard specifies a flame atomic absorption spectrometric method for the determination of vanadium in steel and iron. The method is applicable to vanadium contents between 0,005 % (m/m) and 1,0 % (m/m), provided that t
16、he tungsten content in the test portion is not higher than 10 mg and/or the titanium content is not higher than 5 mg. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publicat
17、ion, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards listed below. Members of IEC and ISO maintain registers of
18、 currently valid International Standards. ISO 377:1985, Wrought steel Selection and preparation of samples and test pieces. ISO 385-1:1984, Laboratory glassware Burettes Part 1: General requirements. ISO 648:1977, Laboratory glassware One-mark pipettes. ISO 1042:1983, Laboratory glassware One-mark v
19、olumetric flasks. ISO 5725:1986, Precision of test methods Determination of repeatability and reproducibility for a standard test method by inter-laboratory tests. 3 Principle Dissolution of a test portion in hydrochloric, nitric and perchloric acids. Addition of aluminium solution as spectrochemica
20、l buffer. Spraying the solution into a dinitrogen monoxide-acetylene flame. Spectrometric measurement of the atomic absorption of the 318,4 nm spectral line emitted by a vanadium hollow cathode lamp. 4 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical
21、grade and only distilled water or water of equivalent purity. 4.1 Pure iron, containing less than 0,000 5 % (m/m) of vanadium, or of low known vanadium content. 4.2 Hydrochloric acid, about 1,19 g/ml. 4.3 Nitric acid, about 1,40 g/ml. 4.4 Perchloric acid, about 1,67 g/ml. 4.5 Hydrochloric acid, abou
22、t 1,19 g/ml, diluted 1 + 50. 4.6 Aluminium, solution, 20 g/l. Dissolve 90 g of aluminium chloride hexahydrate (AlCl36H2O) in about 300 ml of water, add 5 ml of hydrochloric acid (4.2), dilute to 500 ml with water and mix. 4.7 Vanadium, standard solutions. 4.7.1 Stock solution, corresponding to 2 g o
23、f V per litre. 4.7.1.1 Preparation using vanadium metal Weigh, to the nearest 0,001 g, 1,000 g of high purity vanadium purity 99,9 % (m/m) and dissolve in 30 ml of aqua regia mix three volumes of hydrochloric acid (4.2) with one volume of nitric acid (4.3). Heat to evaporate to just before dryness a
24、nd add 20 ml of hydrochloric acid (4.2). Cool and transfer the solution quantitatively to a 500 ml one-mark volumetric flask, dilute to the mark with water and mix. 1 ml of this solution contains 2 mg of V. 4.7.1.2 Preparation using ammonium metavanadate Dry several grams of ammonium metavanadate (N
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