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1、BRITISH STANDARD BS 3338-15: 1965 Method for The determination of copper and lead in white metal bearing alloys (Electrodeposition method) Methods for the sampling and analysis of tin and alloys Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:36 GMT+00:00 2006, Uncontrolled Copy, (c) BS
2、I BS 3338-15:1965 This British Standard, having been approved by the Non-ferrous Metals Industry Standards Committee and endorsed by the Chairman of the Engineering Divisional Council, was published under the authority of the General Council on 18 March 1965 BSI 12-1999 The following BSI references
3、relate to the work on this standard: Committee references NFE/27, NFE/27/1 Draft for comment D63/4040 ISBN 0 580 03157 8 Co-operating organizations The Non-ferrous Metals Industry Standards Committee, under whose supervision this British Standard was prepared, consists of representatives from the fo
4、llowing Government departments and scientific and industrial organizations: The Government departments and scientific and industrial organizations marked with an asterisk in the above list, together with the following, were directly represented on the committee entrusted with the preparation of this
5、 British Standard: Aluminium FederationInstitution of Mining and Metallurgy Association of Bronze and Brass FoundersInstitution of Production Engineers Association of Consulting EngineersInstitution of Structural Engineers British Bronze and Brass Ingot Manufacturers Lead Development Association Ass
6、ociationLight Metal Founders Association British Electrical and Allied ManufacturersLondon Metal Exchange* Association*Magnesium Industry Council British Lead Manufacturers AssociationMinistry of Aviation British Non-ferrous Metals FederationMinistry of Defence, Army Department* British Non-ferrous
7、Metals ResearchMinistry of Defence, Naval Department* Association*Ministry of Transport Copper Development AssociationNational Brassfoundry Association Crown Agents for Oversea Governments andNon-ferrous Metal Stockists AdministrationsPost Office* Electric Cable Makers FederationRoyal Institute of B
8、ritish Architects High Commission of IndiaSociety of British Aerospace Companies Ltd. High Conductivity Copper AssociationSociety of Motor Manufacturers and Traders Institute of British FoundrymenLtd.* Institute of MetalsTin Research Institute* Institution of Mechanical EngineersZinc Development Ass
9、ociation (Automobile Division)Individual manufacturer British Railways BoardLondon Transport Board British Tin Box Manufacturers FederationSolder Makers Association Cable Makers AssociationTinplate Conference (1925) Electronic Engineering AssociationTin Producers Association Gas CouncilWhite Metal B
10、earing Manufacturers Institution of Gas EngineersIndividual firms Amendments issued since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-15:1965 BSI 12-1999i Contents Page Co-operating organizationsI
11、nside front cover Forewordii Introduction1 Apparatus1 Solutions required1 Sampling1 Procedure1 Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-15:1965 ii BSI 12-1999 Foreword This standard makes reference to the following British Sta
12、ndards: BS 219, Soft solders. BS 3252, Ingot tin. BS 3332, White metal bearing alloy ingots. BS 3338, Methods for the sampling and analysis of tin and tin alloys Part 14: Sampling of white metal bearing alloy ingots. This method for the determination of copper and lead in white metal bearing alloys
13、is the fifteenth of a series of methods which will form a complete British Standard under the collective title “Methods for the sampling and analysis of tin and tin alloys”, each method being published as a separate part. The preparation of this series of methods has been authorized by the Non-ferro
14、us Metals Industry Standards Committee as part of a general programme for the standardization of methods for the sampling and analysis of non-ferrous metals. Other methods in the series are as follows: Part 1: Sampling of ingot tin; Part 2: Determination of tin in ingot tin; Part 3: Determination of
15、 antimony in ingot tin; Part 4: Determination of copper in ingot tin and tin-lead solders; Part 5: Determination of lead in ingot tin and tin-antimony solders; Part 6: Determination of copper in high purity ingot tin; Part 7: Determination of silver in solders; Part 8: Determination of bismuth in in
16、got tin, tin-lead solders and white metal bearing alloys; Part 9: Determination of arsenic in ingot tin, solders and white metal bearing alloys; Part 10: Determination of iron in ingot tin, tin-lead solders and white metal bearing alloys; Part 11: Determination of tin in solders; Part 12: Sampling o
17、f solders; Part 13: Determination of antimony in solders and white metal bearing alloys; Part 14: Sampling of white metal bearing alloy ingots; Part 16: Determination of tin in white metal bearing alloys; Part 17: Determination of cadmium in solders and white metal bearing alloys. The complete Briti
18、sh Standard methods will be found suitable for the grades of metals covered by BS 3252, “Ingot tin”, BS 219, “Soft solders” and BS 3332, “White metal bearing alloy ingots”. In the methods for determining impurities, sample weights and aliquots have been chosen to cover the range of impurity content
19、usually found in commercial tin ingots, solders and white metal bearing alloy ingots. For amounts of impurity outside this range, sample weights or aliquots should be adjusted accordingly. The methods have been found to give reliable and reproducible results, and, while in some instances they may ap
20、pear to be lengthy, it should be realized that they are put forward as “referee” methods to be used in cases of dispute. Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-15:1965 BSI 12-1999iii A British Standard does not purport to in
21、clude all the necessary provisions of 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, pag
22、es i to iv, pages 1 and 2, 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 Nov 29 07:54:36 GMT
23、+00:00 2006, Uncontrolled Copy, (c) BSI iv blank Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-15:1965 BSI 12-19991 Introduction a) Principle. Copper and lead are determined by electrolytic deposition from a nitric acid solution af
24、ter removal of tin and antimony as their volatile bromides. b) Range. From 0.1 per cent to 6 per cent copper. From 0.1 per cent to 5 per cent lead. c) Reproducibility. With 1 to 6 per cent copper or 1 to 5 per cent lead present 0.1 per cent. With 0.1 to 1 per cent copper or lead present 10 per cent
25、of copper or lead present. Apparatus a) All volumetric glassware used shall be of Class A accuracy as defined in the appropriate British Standards, or where no British Standard exists, as described in the National Physical Laboratory Publication “Volumetric tests on volumetric glassware”. b) Platinu
26、m-gauze electrodes of stationary type and of conventional size (about 1 dm2 surface area); the diameter and height of the cathode should be about 1# in (44.5 mm) and the diameter and height of the anode should be about 1! in (32 mm). c) Electrodeposition apparatus fitted with stirrer and capable of
27、providing a direct current of 3 amps. Solutions required All reagents shall be of the highest purity obtainable and distilled water1) shall be used throughout. Solutions shall be freshly prepared and, where necessary, filtered. Bromine-acid mixture. To 45 ml of hydrochloric acid (sp. gr. 1.161.18) a
28、nd 45 ml of hydrobromic acid (sp. gr. 1.461.49) add carefully 10 ml of bromine. Nitric acid (50 per cent v/v). Dilute 50 ml of nitric acid (sp. gr. 1.42) to 100 ml. Sulphamic acid (5 per cent w/v). Dissolve 5 g of sulphamic acid in water and dilute to 100 ml. Sulphuric acid (50 per cent v/v). To 400
29、 ml of water add cautiously 500 ml of sulphuric acid (sp. gr. 1.84) mix, cool and dilute to 1 litre. Sampling Recommended methods of obtaining a suitable sample for the analytical procedure given below are described in BS 3338-14, “Sampling of white metal bearing alloy ingots”. Procedure Weigh 5 g o
30、f sample (Note 1) and transfer to a 400 ml tall form beaker. Add 40 ml of bromine-acid mixture (Note 1) and evaporate to dryness. Add a further 5 ml of bromine-acid mixture and evaporate again. Dissolve the residue in 30 ml of nitric acid (50 per cent) and boil until entirely freed from bromine. If
31、lead is not to be determined, add 4 ml of sulphuric acid (50 per cent), cool to room temperature, filter off and discard the precipitate formed. Insert a pair of weighed platinum-gauze electrodes, previously dried at 105 C and cooled in a desiccator, and place as close to the bottom of the beaker as
32、 possible. Dilute the electrolyte with water until it covers the gauze of the electrodes. Add 5 ml of sulphamic acid (5 per cent) and cover with a pair of split cover-glasses. Electrolyze for 10 minutes at a current of 0.5 amp and for a further 50 minutes at 3 amps with stirring. Wash down the split
33、 cover-glasses, the rim of the beaker and electrode stems, then continue to electrolyze for a further 10 minutes. Lower the electrolyte beaker, replace it with another containing sufficient water to cover the electrodes and, with the stirrer still running, allow to wash for 15 seconds. Discard the w
34、ashings and repeat this step. Replace the second beaker of water with a beaker of ethanol (95 per cent v/v) and allow to wash for 15 seconds. Switch off stirrer and current. Remove the electrodes and dry in a gentle stream of warm air. Allow the cathode to cool to room temperature in a desiccator an
35、d re-weigh. The increase in weight is due to copper. Dry the anode at 150 C for half an hour, cool to room temperature in a desiccator and re-weigh. The increase in weight of the anode is due to lead dioxide; use the empirical factor of 0.86 to convert this weight to lead. Calculate the percentage o
36、f copper and lead present. NOTEFor alloys containing between 3 and 5 per cent lead use a 1 g sample and add 20 ml of the bromine-acid mixture. 1) Water demineralized by ion exchange may be used if it is of equivalent quality. Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:36 GMT+00:00
37、2006, Uncontrolled Copy, (c) BSI 2 blank Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-15:1965 BSI 12-1999 British Standards The following are available on application: YEARBOOK Including subject index and numerical list of British
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41、oad engineering Rubber Shipbuilding Textiles and clothing Welding Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-15: 1965 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent national bod
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