BS 3338-6-1961 Methods for the sampling and analysis of tin and tin alloys - Method for the determination of copper in high purity ingot tin (photometric method)《锡及锡合金取样及分析方法 第6部分 .pdf

1、BRITISH STANDARD BS3338-6: 1961 Method for The determination of copper in high purity ingot tin (Photometric method) Methods for the sampling and analysis of tin and tin alloysBS3338-6:1961 This BritishStandard, having been approved by the Non-ferrous Metals Industry Standards Committee and endorsed

2、 by the Chairman of theEngineering Divisional Council, was published under theauthority of the General Council on 29 April1961 BSI 12-1999 The following BSI references relate to the work on this standard: Committee references NFE/27, NFE/27/1 Draft for comment A(NFE)9203 ISBN 0 580 03067 9 Co-operat

3、ing organizations The Non-ferrous Metals Industry Standards Committee, under whose supervision this BritishStandard was prepared, consists of representatives from the following Government departments and scientific and industrial organizations: Admiralty* Institution of Mining and Metallurgy Alumini

4、um Development Association Institution of Structural Engineers Aluminium Industry Council Lead Development Association Association of Bronze and Brass Founders Lead Sheet and Pipe Manufacturers Association of Consulting Engineers, Federation (Incorporated) Light Metal Founders Association British Br

5、onze and Brass Ingot London Metal Exchange* Manufacturers Association Magnesium Industry Council British Electrical and Allied Manufacturers Ministry of Aviation* Association* National Brassfoundry Association British Non-ferrous Metals Federation Non-ferrous Metal Stockists British Non-ferrous Meta

6、ls Research Post Office* Association* Royal Institute of British Architects Cable Makers Association* Society of British Aircraft Constructors Copper Development Association Society of Motor Manufacturers and Crown Agents for Oversea Governments and TradersLtd.* Administrations Tin Research Institut

7、e* High Commission of India War Office* High Conductivity Copper Association Zinc Development Association Institute of British Foundrymen Individual manufacturers Institute of Metals Institution of Mechanical Engineers (Automobile Division) The Government departments and scientific and industrial or

8、ganizations marked with an asterisk in the above list, together with the following, were directly represented on the committee entrusted with the preparation of this BritishStandard: British Railways, The British Transport London Transport Executive, The British Commission Transport Commission Briti

9、sh Tin Box Manufacturers Federation Solder Makers Association Electronic Engineering Association Tinplate Conference(1925) Gas Council Tin Producers Association Institution of Gas Engineers Individual firms Amendments issued since publication Amd. No. Date CommentsBS3338-6:1961 BSI 12-1999 i Content

10、s Page Co-operating organizations Inside front cover Foreword ii Introduction 1 Apparatus 1 Solutions required 1 Sampling 1 Procedure 1 Calibration 1BS3338-6:1961 ii BSI 12-1999 Foreword This standard makes reference to the following BritishStandard: BS3338-1, Sampling of ingot tin. This method for

11、the determination of copper in high purity ingot tin is the sixth of a series of methods which will form a complete BritishStandard 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

12、 of methods has been authorized by the Non-ferrous 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: Determinati

13、on of tin in ingot tin; Part 3: Determination 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 7: Determination of silver in solders; Part 8: Determination of bismuth in ingot tin, t

14、in-lead solders and white metal bearing alloys; Part 9: Determination of arsenic in ingot tin, tin-lead 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 of

15、 solders. The complete BritishStandard 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 r

16、ange of impurity content 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 s

17、ome instances they may appear to be lengthy, it should be realized that they are put forward as “referee” methods to be used in cases of dispute. In the preparation of the calibration graphs an attempt has been made to define concentrations, but because these are linked with the particular instrumen

18、t used for determining optical density they should be used only as a guide. A British Standard does not purport to include 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 confe

19、r immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pagesi andii, pages1 and2, 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

20、the amendment table on the inside front cover.BS3338-6:1961 BSI 12-1999 1 Introduction a) Principle. Copper is determined photometrically with rubeanic acid. b) Range. Up to0.04 per cent copper. c) Reproducibility. 10 per cent of copper present. Apparatus a) Any volumetric glassware used shall be of

21、 Class A accuracy as defined in the appropriate BritishStandards, or where no BritishStandard exists, as described in the National Physical Laboratory Publication “Volumetric Tests on Volumetric Glassware”. b) Any instrument suitable for measuring the optical density of the solution at a wavelength

22、of650m4 may be used. c) 2cm or4cm cells (Note1). d) Alternatively, if a filter photometer of the balanced two cell type is used, the filter combination should conform as closely as possible to the above wave-length. The following have been found suitable: Tungsten lamp Ilford608 or equivalent filter

23、s. Solutions required All reagents shall be of the highest purity obtainable and distilled water shall be used throughout. Solutions shall be freshly prepared and, where necessary, filtered. Standard copper (1mlN 0.5mg of copper). Dissolve0.125g of pure copper in nitric acid (sp.gr.1.42) and dilute

24、to250ml in a graduated flask. Standard copper (1mlN 0.05mg of copper). Dilute25ml of the above solution to250ml in a graduated flask. Bromine-hydrobromic acid. Add10ml of bromine to90ml of hydrobromic acid(48 per cent v/v). Buffer. Dissolve400g of ammonium acetate in a mixture of400ml of glacial ace

25、tic acid and200ml of water. Gum arabic (gum acacia)(0.5 per cent w/v). Dissolve1.25g of gum arabic (gum acacia) crystals in hot water, filter and dilute to250ml. Nitric acid (50 per cent v/v). Dilute50ml of nitric acid (sp. gr.1.42) to100ml. Rubeanic acid (0.1 per cent w/v alcoholic). Dissolve0.1g o

26、f rubeanic acid in100ml of industrial methylated spirit (I.M.S.). 1) Sampling Recommended methods of obtaining a suitable sample for the analytical procedure given below are described in BS3338-1, “Sampling of ingot tin”. Procedure Dissolve1.00g of sample in10ml of bromine-hydrobromic acid in a150ml

27、 beaker and evaporate to dryness. Add a further5ml of bromine-hydrobromic acid and evaporate again. To the residue add5ml of nitric acid(50 per cent) and boil until free from bromine. Add ammonia solution (sp.gr.0.91) until neutral to litmus paper, then add acetic acid until just acid. Add2.5ml of t

28、he buffer solution and5ml of gum arabic solution(0.5 per cent). Transfer to a50ml graduated flask, and dilute to about45ml. Add1ml of rubeanic acid solution(0.1 per cent), dilute to the mark, and allow to stand for10minutes. Measure the optical density of the solution at20 1 C using the conditions s

29、pecified under “Apparatus” and using water in the reference cell. Carry out simultaneously a blank determination on the reagents. Follow the same procedure without the sample and use the same quantity of reagents. Deduct the blank reading and calculate the percentage copper in the sample by referenc

30、e to the appropriate calibration graph. Calibration Transfer to50-ml beakers the following amounts of standard copper solution (1mlN 0.05mg Cu): for the4cm cell,1.0,2.0,3.0,4.0ml for the2cm cell,2.0,4.0,6.0,8.0ml. Neutralize with ammonia solution (sp. gr.0.91), make just acid with acetic acid and co

31、ntinue as in the procedure. Carry out simultaneously a blank, using the same quantities of reagents. Prepare calibration graphs by plotting optical density against weight of copper in the various aliquots, after deduction of the blank reading. NOTE 1A2cm cell should be used for copper contents in th

32、e range0.01 to0.04 per cent and the4cm cell for copper contents below0.01 per cent. 1) It should be noted that the use of industrial methylated spirit is governed by the Methylated Spirits Regulations,1952 (S.I.1952, No.2230).2 blankBS3338-6:1961 BSI 12-1999 British Standards The following are avail

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