BS-6783-13-1992 ISO-11400-1992.pdf
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1、BRITISH STANDARD BS 6783-13: 1992 ISO 11400: 1992 Sampling and analysis of nickel, ferronickel and nickel alloys Part 13: Method for the determination of phosphorus in nickel, ferronickel and nickel alloys by phosphovanadomolybdate molecular absorption spectrometry Licensed Copy: sheffieldun sheffie
2、ldun, na, Wed Dec 06 15:08:11 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6783-13:1992 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 December
3、 1992 BSI 10-1999 The following BSI references relate to the work on this standard: Committee reference NFM/10 Draft for comment 91/39171 DC ISBN 0 580 21416 8 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Non-ferrous Metals Standards
4、Policy Committee (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 Steel Industry Department of Trade and Industry (Laboratory of the Government Chemist) Engineering Equipment
5、 and Materials Users Association Institute of British Foundrymen London Metal Exchange Ministry of Defence Nickel Development Institute Non-ferrous Metal Stockists Stainless Steel Fabricators Association of Great Britain Steel Casting Research and Trade Association Coopted members Amendments issued
6、since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 15:08:11 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6783-13:1992 BSI 10-1999i Contents Page Committees responsibleInside front cover National forewordii 1Scope1 2Normative references1 3Principle1 4Reagen
7、ts1 5Apparatus2 6Sampling and sample preparation2 7Procedure2 8Expression of results3 9Test report4 Table 1 Mass of sample to be taken2 Table 2 Nominal composition of test samples4 Table 3 Results of statistical analysis4 List of referencesInside back cover Licensed Copy: sheffieldun sheffieldun, na
8、, Wed Dec 06 15:08:11 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6783-13:1992 ii BSI 10-1999 National foreword This Part of BS 6783 has been prepared under the direction of the Non-ferrous Metals Standards Policy Committee. It is identical with ISO 11400:1992 Nickel, ferronickel and nickel alloys
9、 Determination of phosphorus content Phosphovanadomolybdate molecular absorption spectrometric method published by the International Organization for Standardization (ISO). At present this British Standard consists of 13 Parts all concerned with analysis of nickel, ferronickel and nickel alloys. Fur
10、ther International Standards are in preparation on sampling and analysis of nickel, ferronickel and nickel alloys and, when available, these will be published as further Parts of this British Standard. The Technical Committee has reviewed the provisions of ISO 648, to which normative reference is ma
11、de in the text, and has decided that they are acceptable for use in conjunction with this standard. ISO 648 is related to BS 1583:1986 Specification for one-mark pipettes. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are respon
12、sible 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 (Identical) ISO 5725:1986BS
13、5497 Precision of test methods Part 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 to 4, an inside back cov
14、er 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 15:08:11 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 67
15、83-13:1992 BSI 10-19991 1 Scope This International Standard specifies a molecular absorption spectrometric method for the determination of the phosphorus content in nickel, ferronickel and nickel base alloys in the range of 0,000 5 % (m/m) to 0,05 % (m/m). Arsenic, chromium, hafnium, niobium, silico
16、n, tantalum, titanium and tungsten interfere, but the interferences can be avoided by complexation or volatilisation (for Cr). The lowest phosphorus content 0,000 5 % (m/m) can only be reached in samples with low contents of the interfering elements. 2 Normative references The following standards co
17、ntain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investi
18、gate 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 648:1977, Laboratory glassware One-mark pipettes. ISO 1042:1983, Laboratory glassware One-mark volumetric flasks. ISO
19、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 a mixture of nitric and hydrochloric acids. Fuming with perchloric acid in a PFA or PTFE beaker and removal of ch
20、romium as volatile chromylchloride. Complexation of silicon and the refractory elements with fluoride ions. Conversion of phosphorus to phosphovanadomolybdic acid in a perchloric and nitric acid solution. Extraction of phosphovanadomolybdic acid into 4-methyl-2-pentanone with citric acid present to
21、complex arsenic. 4 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. Verify by blank tests (7.6) that the relevant reagents are free from phosphorus. Lots giving high blank values are unsuit
22、able and should not be used. The blank value should be below 0,000 5 % (m/m), calculated for 1 g of sample. 4.1 Nitric acid, 20 = 1,41 g/ml, diluted 1 + 4. 4.2 Hydrofluoric acid, 40 % (m/m), 20 = 1,14 g/ml. WARNING Hydrofluoric acid is extremely irritating and corrosive to skin and mucous membranes,
23、 producing severe skin burns which are slow to heal. In the case of contact with skin, wash well with water and seek medical advice. 4.3 Citric acid, solution. Dissolve 500 g of citric acid monohydrate (H8C6O7.H2O) in water, dilute to 1 000 ml and mix. 4.4 4-methyl-2-pentanone (methyl isobutyl keton
24、e). 4.5 Hexaammonium heptamolybdate, solution. Dissolve 15 g of hexaammonium heptamolybdate tetrahydrate (NH4)6Mo7O24.4H2O in water and dilute to 100 ml. Prepare a fresh solution each day. If high and unstable blank values appear, there might be a problem with the salt used. In such a case, switch t
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