BS 3338-8-1961 Methods for the sampling and analysis of tin and tin alloys - Method for the determination of bismuth in ingot tin tin-lead solders and white metal bearing alloys (p.pdf

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1、BRITISH STANDARD BS3338-8: 1961 Method for The determination of bismuth in ingot tin, tin-lead solders and white metal bearing alloys (Photometric method) Methods for the sampling and analysis of tin and tin alloysBS3338-8:1961 This BritishStandard, having been approved by the Non-ferrous Metals Ind

2、ustry Standards Committee and endorsed by theChairman of theEngineeringDivisional Council,was published under the authority of the General Council on 29April1961 BSI12-1999 The following BSI references relate to the work on this standard: Committee references NFE/27,NFE/27/1 Draft for commentAA(NFE)

3、1388 ISBN 0 580 03087 3 Co-operating 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: The Government departm

4、ents 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 BritishStandard: Admiralty* Institution of Mining and Metallurgy Aluminium Development Associatio

5、n 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 Bronze and Brass Ingot Manu

6、facturers London Metal 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*

7、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 Traders Ltd.* Administrations Tin Research Institute* High Commission of In

8、dia War Office* High Conductivity 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, The British Com

9、mission Transport Commission 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 CommentsB

10、S3338-8:1961 BSI 12-1999 i Contents Page Co-operating organizations Inside front cover Foreword ii Introduction 1 Apparatus 1 Solutions required 1 Sampling 1 Procedure 1 Calibration 1BS3338-8:1961 ii BSI 12-1999 Foreword This standard makes reference to the following BritishStandard: BS3338-1, Sampl

11、ing of ingot tin. BS3338-12, Sampling of solders. BS3338-14, Sampling of white metal bearing alloys 1) . This method for the determination of bismuth in ingot tin, tin-lead solders and white metal bearing alloys is the eighth of a series of methods which will form a complete BritishStandard under th

12、e 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-ferrous Metals Industry Standards Committee as part of a general programme for the standardizatio

13、n 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 antimony in ingot tin; Part 4: Determination of copper in ingot tin and tin-lead solders; P

14、art 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 9: Determination of arsenic in ingot tin, tin-lead solders and white metal bearing alloys; Part 10: Determination of iron in

15、ingot tin, tin-lead solders and white metal bearing alloys; Part 11: Determination of tin in solders; Part 12: Sampling of 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 bear

16、ing alloy ingots”. In the methods for determining impurities, sample weights 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 aliquo

17、ts should be adjusted accordingly. The methods have been found to give reliable 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 calibrat

18、ion graphs an attempt has been made to define concentrations, but because 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 Brit

19、ish 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, pagesi andii, page1 and a back cover. This standard has been updat

20、ed (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. 1) In course of preparation.BS3338-8:1961 BSI 12-1999 1 Introduction a) Principle. Bismuth is determined photometrically with thiourea after removal of tin and a

21、ntimony as bromides in the presence of perchloric acid. b) Range. Up to0.07percent bismuth (Note1). c) Reproducibility. 10percent of bismuth present. Apparatus a) Any volumetric glassware used shall be of ClassA accuracy as defined in the appropriate BritishStandards, or where no BritishStandard exi

22、sts, 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 of465m may be used. c) 1cm or4cm cells (Note2). d) Alternatively, if a filter photometer of the b

23、alanced 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 Ilford602 or equivalent filters. Solutions required All reagents shall be of the highest purity obtainable and distilled water s

24、hall be used throughout. Solutions shall be freshly prepared and, where necessary filtered. Standard bismuthA (1ml N 1.0mg of bismuth). Dissolve0.250g of bismuth in10ml nitric acid (sp.gr.1.42) and dilute to250ml in a graduated flask. Standard bismuthB (1ml N 0.1mg of bismuth). Dilute25ml of the abo

25、ve solution to250ml in a graduated flask. Bromine-hydrobromic acid. Add10ml of bromine to90ml of hydrobromic acid(48percentv/v). Thiourea (8percentw/v). Dissolve8g of thiourea in100ml of water. Sampling Recommended methods of obtaining a suitable sample for the analytical procedure given below arede

26、scribed in BS3338, Part 1, “Sampling of ingot tin”; Part12, “Sampling of solders”; and Part14,“Sampling of white metal bearing alloys”. Procedure Dissolve2.00g of sample in20ml of bromine-hydrobromic acid in a150ml beaker and add5ml of perchloric acid (sp.gr.1.54). Evaporate to fuming, and if the so

27、lution is cloudy add a further quantity of hydrobromic acid. Repeat until the solution is clear, indicating complete removal of tin and antimony (Note3). Cool, dilute and transfer to a50ml graduated flask, add from a pipette25ml of thiourea solution(8percent) and dilute to the mark. Measure the opti

28、cal density of the solution at20 1 C using the conditions specified 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 an

29、d calculate the percentage bismuth in the sample by reference to the appropriate calibration graph. Calibration Transfer to150-ml beakers the following amounts of standard bismuth solution(1ml N 0.1mg Bi.): for the4cm cell0.5,1.0,2.0,3.0ml for the1cm cell5.0,8.0,10.0,14.0ml. Add5ml of perchloric aci

30、d (sp.gr.1.54) and heat to fuming. Cool, dilute, transfer to50ml graduated flasks and continue 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 bismuth in the various aliquots, after

31、 deduction of the blank reading. NOTE 1Bismuth content up to0.12percent may be determined if a sample weight of1g is taken. NOTE 2A4cm cell should be used for bismuth contents in the range0.0010.015percent, and a1cm cell for bismuth contents up to0.07percent. NOTE 3In the presence of more than10perc

32、ent of lead the bulk of the lead is removed as follows: Cool, dilute with20ml of water, add5ml of hydrochloric acid(50percentv/v) and cool in ice-water. Filter the lead chloride on a sintered glass filter (Porosity4) and wash with a little cold hydrochloric acid(10percentv/v). Evaporate the filtrate

33、 to fumes of perchloric acid, cool, dilute and transfer to a50ml graduated flask. Continue as in the procedure.BS3338-8: 1961 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing BritishStandards. It presents the UK vi

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