BS 3338-15-1965 Methods for the sampling and analysis of tin and tin alloys - Method for the determination of copper and lead in white metal bearing alloys (electrodeposition metho.pdf

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 alloysBS3338-15:1965 This British Standard, having been approved by the Non-ferrousMetals Industry Standards Com

2、mittee and endorsed by the Chairman of theEngineering Divisional Council, was published undertheauthority of the GeneralCouncil on 18March1965 BSI 12-1999 The following BSI references relate to the work on this standard: Committee references NFE/27, NFE/27/1 Draft for comment D63/4040 ISBN 0 580 031

3、57 8 Co-operating organizations The Non-ferrous Metals Industry Standards Committee, under whose supervision this British Standard was prepared, consists of representatives from the following Government departments and scientific and industrial organizations: The Government departments and scientifi

4、c 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 British Standard: Aluminium Federation Institution of Mining and Metallurgy Association of Bronze and Brass Founder

5、s Institution of Production Engineers Association of Consulting Engineers Institution of Structural Engineers British Bronze and Brass Ingot Manufacturers Lead Development Association Association Light Metal Founders Association British Electrical and Allied Manufacturers London Metal Exchange* Asso

6、ciation* Magnesium Industry Council British Lead Manufacturers Association Ministry of Aviation British Non-ferrous Metals Federation Ministry of Defence, Army Department* British Non-ferrous Metals Research Ministry of Defence, Naval Department* Association* Ministry of Transport Copper Development

7、 Association National Brassfoundry Association Crown Agents for Oversea Governments and Non-ferrous Metal Stockists Administrations Post Office* Electric Cable Makers Federation Royal Institute of British Architects High Commission of India Society of British Aerospace Companies Ltd. High Conductivi

8、ty Copper Association Society of Motor Manufacturers and Traders Institute of British Foundrymen Ltd.* Institute of Metals Tin Research Institute* Institution of Mechanical Engineers Zinc Development Association (Automobile Division) Individual manufacturer British Railways Board London Transport Bo

9、ard British Tin Box Manufacturers Federation Solder Makers Association Cable Makers Association Tinplate Conference (1925) Electronic Engineering Association Tin Producers Association Gas Council White Metal Bearing Manufacturers Institution of Gas Engineers Individual firms Amendments issued since

10、publication Amd. No. Date CommentsBS3338-15:1965 BSI 12-1999 i Contents Page Co-operating organizations Inside front cover Foreword ii Introduction 1 Apparatus 1 Solutions required 1 Sampling 1 Procedure 1BS3338-15:1965 ii BSI 12-1999 Foreword This standard makes reference to the following British S

11、tandards: 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 alloy

12、s 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-fer

13、rous 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

14、of 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

15、ingot 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

16、 of 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 Bri

17、tish Standard methods will be found suitable for the grades of metals covered by BS3252, “Ingot tin”, BS219, “Soft solders” and BS3332, “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 u

18、sually 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 app

19、ear to be lengthy, it should be realized that they are put forward as “referee” methods to be used in cases of dispute.BS3338-15:1965 BSI 12-1999 iii A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correc

20、t 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 to iv, pages 1 and 2, an inside back cover and a back cover. This standard has been updated (see copyrig

21、ht date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.iv blankBS3338-15:1965 BSI 12-1999 1 Introduction a) Principle. Copper and lead are determined by electrolytic deposition from a nitric acid solution after removal of tin and an

22、timony as their volatile bromides. b) Range. From0.1 per cent to6 per cent copper. From0.1 per cent to5 per cent lead. c) Reproducibility. With 1 to 6 per cent copper or1 to5 per cent lead present 0.1 per cent. With 0.1 to 1 per cent copper or lead present 10 per cent of copper or lead present. Appa

23、ratus 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) Platinum-gauze electrodes of stationar

24、y type and of conventional size (about1dm 2surface area); the diameter and height of the cathode should be about1# in (44.5mm) and the diameter and height of the anode should be about1! in (32mm). c) Electrodeposition apparatus fitted with stirrer and capable of providing a direct current of3amps. S

25、olutions required All reagents shall be of the highest purity obtainable and distilled water 1)shall be used throughout. Solutions shall be freshly prepared and, where necessary, filtered. Bromine-acid mixture. To45ml of hydrochloric acid (sp. gr. 1.161.18) and45ml of hydrobromic acid (sp. gr. 1.461

26、.49) add carefully10ml of bromine. Nitric acid (50 per cent v/v). Dilute50ml of nitric acid (sp. gr. 1.42) to100ml. Sulphamic acid (5 per cent w/v). Dissolve5g of sulphamic acid in water and dilute to100ml. Sulphuric acid (50 per cent v/v). To400ml of water add cautiously500ml of sulphuric acid (sp.

27、 gr. 1.84) mix, cool and dilute to1litre. Sampling Recommended methods of obtaining a suitable sample for the analytical procedure given below are described in BS3338-14, “Sampling of white metal bearing alloy ingots”. Procedure Weigh 5g of sample (Note 1) and transfer toa400ml tall form beaker. Add

28、40ml of bromine-acid mixture (Note1) and evaporate to dryness. Add a further5ml of bromine-acid mixture and evaporate again. Dissolve the residue in30ml of nitric acid (50per cent) and boil until entirely freed from bromine. If lead is not to be determined, add4ml of sulphuric acid (50per cent), coo

29、l to room temperature, filter off and discard the precipitate formed. Insert a pair of weighed platinum-gauze electrodes, previously dried at105 C and cooled in a desiccator, and place as close to the bottom of the beaker as possible. Dilute the electrolyte with water until it covers the gauze of th

30、e electrodes. Add5ml of sulphamic acid (5per cent) and cover with a pair of split cover-glasses. Electrolyze for10minutes at a current of0.5amp and for a further50 minutes at3amps with stirring. Wash down the split cover-glasses, the rim of the beaker and electrode stems, then continue to electrolyz

31、e for a further10minutes. Lower the electrolyte beaker, replace it with another containing sufficient water to cover the electrodes and, with the stirrer still running, allow to wash for15seconds. Discard the washings and repeat this step. Replace the second beaker of water with a beaker of ethanol

32、(95per cent v/v) and allow to wash for15seconds. 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 and re-weigh. The increase in weight is due to copper. Dry the anode at150 C for half an hour,

33、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 of0.86 to convert this weight to lead. Calculate the percentage of copper and lead present. NOTEFor alloys containing between3 and5 per cent lead usea1g sample

34、and add20ml of the bromine-acid mixture. 1) Water demineralized by ion exchange may be used if it is of equivalent quality.2 blankBS3338-15:1965 BSI 12-1999 British Standards The following are available on application: YEARBOOK Including subject index and numerical list of British Standards15s. SECT

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