BS 3338-4-1961 Methods for the sampling and analysis of tin and tin alloys - Method for the determination of copper in ingot tin and tin-lead solders (photometric method)《锡及锡合金取样及分.pdf

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1、BRITISH STANDARD BS 3338-4: 1961 Method for The determination of copper in ingot tin and tin-lead solders (photometric method) Methods for the sampling and analysis of tin and tin alloysBS3338-4:1961 This British Standard, having been approved by the Non-ferrous Metals Industry Standards Committee a

2、nd endorsed by the Chairman oftheEngineering Divisional Council, was published under theauthority of the General Council on 29 April1961 BSI11-1999 The following BSI references relate to the work on this standard: Committee references NFE/27, NFE/27/1 Draft for comment A(NFE)9201 ISBN 0 580 03047 4

3、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 scientific and

4、 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 BritishStandard: Admiralty* Institution of Mining and Metallurgy Aluminium Development Association Institution of Struct

5、ural 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 Bronze and Brass Ingot Manufacturers London Metal

6、Exchange* 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 Metals Research Post Office* Association* Royal Inst

7、itute 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 Traders Ltd.* Administrations Tin Research Institute* High Commission of India War Office* High Co

8、nductivity Copper Association Zinc Development Association Institute of British Foundrymen Individual manufacturers Institute of Metals Institution of Mechanical Engineers (Automobile Division) British Railways, The British Transport London Transport Executive, Commission The British Transport Commi

9、ssion British 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 CommentsBS3338-4:1961 BSI 11-199

10、9 i Contents Page Co-operating organizations Inside front cover Foreword ii Introduction 1 Apparatus 1 Solutions required 1 Sampling 1 Procedure 1 Calibration 1BS3338-4:1961 ii BSI 11-1999 Foreword This standard makes reference to the following British Standard: BS 3338-1, Sampling of ingot tin. BS

11、3338-12, Sampling of solders. This method for the determination of copper in ingot tin and tin-lead solders is the fourth 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 pub

12、lished as a separate part. The preparation of this series 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 fo

13、llows: Part 1: Sampling of ingot tin; Part 2: Determination of tin in ingot tin; Part 3: Determination of antimony in ingot tin; 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;

14、Part 8: Determination of bismuth in ingot tin, tin-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: Deter

15、mination of tin in solders; Part 12: Sampling of solders. The complete British 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 weig

16、hts and aliquots have been chosen to cover the range 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 re

17、liable and reproducible results, and, while in some 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 becaus

18、e these are linked with the particular instrument 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

19、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, pagesi andii, pages1 and2, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had ame

20、ndments incorporated. This will be indicated in the amendment table on the inside front cover.BS3338-4:1961 BSI 11-1999 1 Introduction a) Principle. Copper is determined photometrically with hydrobromic acid/phosphoric acid mixture. b) Range. From0.01 to0.4 percent copper. c) Reproducibility. 10perc

21、ent of copper present. Apparatus a) Any 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) Any instrum

22、ent suitable for measuring the optical density of the solution at a wavelength of600m4 may be used. c) 1cm 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 wavelength. The fo

23、llowing have been found suitable: Tungsten lamp Ilford607 or equivalent filters. 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 Solution A (1ml

24、N 0.5mg of copper). Dissolve0.125g of pure copper in5ml of bromine-hydrobromic acid and dilute to250ml. Standard copper Solution B (1mlN 0.1mg of copper). Dilute50ml of the above solution to250ml. Bromine-hydrobromic acid. Add10ml of bromine to90ml of hydrobromic acid(48percentv/v). Hydrobromic acid

25、/phosphoric acid. Add1ml of bromine to1 litre of colourless hydrobromic acid(48percentv/v), and mix with1 litre of phosphoric acid (sp. gr.1.71). Store in a stoppered bottle. Sampling Recommended methods of obtaining a suitable sample for the analytical procedure given below are described in BS3338-

26、1, “Sampling of ingot tin” andPart12, “Sampling of solders.” Procedure Dissolve1.0g of sample in10ml of bromine-hydrobromic acid in a150ml beaker and evaporate to dryness. Cool, add25ml of hydrobromic acid/phosphoric acid mixture, transfer to a50ml graduated flask, and dilute to the mark with the hy

27、drobromic acid/phosphoric acid mixture (Note2). Measure the optical density of the solution at20 1 C using the conditions specified under “Apparatus” and using the hydrobromic acid/phosphoric acid mixture in the reference cell. Carry out simultaneously a blank determination on the reagents. Follow t

28、he 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 reference to the appropriate calibration graph. Calibration Transfer the following amounts of standard copper solution (Note3) 2.0,4.0,6.0,8.0ml t

29、o150ml beakers and evaporate to dryness. Cool, take up in50ml hydrobromic acid/phosphoric acid mixture and continue as in the procedure. Prepare calibration graphs by plotting optical density against weight of copper in the various aliquots. NOTE 1A4cm cell should be used for copper contents in the

30、range0.01 to0.1percent and a1cm cell for copper contents up to0.4percent. NOTE 2If any lead bromide remains undissolved, allow to settle and decant the supernatant liquid. NOTE 3For the1cm cell use standard copper SolutionA(1mlN 0.5mgCu) and for the4cm cell use SolutionB(1mlN 0.1mgCu).2 blankBS3338-

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