BS 3338-3-1961 Methods for the sampling and analysis of tin and tin alloys - Method for the determination of antimony in ingot tin (photometric method)《锡及锡合金取样及分析方法 第3部分 锡锭中锑含量测定方法.pdf

1、BRITISH STANDARD BS3338-3: 1961 Incorporating Amendment Nos.1 and2 Method for The determination of antimony in ingot tin (Photometric method) Methods for the sampling and analysis of tin and tin alloysBS3338-3:1961 This BritishStandard, having been approved by the Non-ferrous Metals Industry Standar

2、ds Committee and endorsed by the Chairman oftheEngineering Divisional Council, was published under theauthority of the General Council on 29 April1961 BSI12-1999 The following BSI references relate to the work on this standard: Committee references NFE/27, NFE/27/1 Draft for comment A(NFE)9200 ISBN

3、0 580 03037 7 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: Admiralty* Institution of Mining

4、 and Metallurgy Aluminium 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

5、 Association British Bronze 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 B

6、ritish Non-ferrous Metals 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 Traders Ltd.* Administratio

7、ns Tin Research Institute* 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 scie

8、ntific 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: British Railways, The British Transport London Transport Executive, The British Commission Tr

9、ansport 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 of issue Comments

10、August1961 4666 October1962 Indicated by a sideline in the marginBS3338-3:1961 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 2BS3338-3:1961 ii BSI 12-1999 Foreword This standard

11、 makes reference to the following BritishStandards: BS410, Test sieves. BS1400, Copper alloy ingots and castings. BS3338-1, Sampling of ingot tin. This method for the determination of antimony in ingot tin is the third of a series of methods which will form a complete BritishStandard under the colle

12、ctive 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 standardization of me

13、thods for the sampling and analysis of non-ferrous metals. Other methods in the series are as follows: Part1: Sampling of ingot tin; Part2: Determination of tin in ingot tin; Part4: Determination of copper in ingot tin and tin-lead solders; Part5: Determination of lead in ingot tin and tin-antimony

14、solders; Part6: Determination of copper in high purity ingot tin; Part7: Determination of silver in solders; Part8: Determination of bismuth in ingot tin, tin-lead solders and white metal bearing alloys; Part9: Determination of arsenic in ingot tin, tin-lead solders and white metal bearing alloys; P

15、art10: Determination of iron in ingot tin, tin-lead solders and white metal bearing alloys; Part11: Determination of tin in solders; Part12: Sampling of solders. The complete BritishStandard methods will be found suitable for the grades of metals covered by BS3252, “Ingot tin”, BS219, “Soft solders”

16、, 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 usually found in commercial tin ingots, solders and white metal bearing alloy ingots. For amounts of impurity outside this

17、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 appear to be lengthy, it should be realized that they are put forward as “referee” methods to be used in cases of dispute. In

18、 the preparation of the calibration 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 provisi

19、ons 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, pagesi andii, pages1 and2 and a ba

20、ck 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.BS3338-3:1961 BSI 12-1999 1 Introduction a) Principle. Antimony is determined photometrically with rhodamine B. b) Range. Up

21、 to0.25per cent antimony. c) Reproducibility. 10per cent of antimony present. Apparatus a) Any volumetric glassware used shall be of Class A accuracy as defined in the appropriate BritishStandards, or where no BritishStandard exists, as described in the National Physical Laboratory Publication “Volu

22、metric Tests on Volumetric Glassware”. b) Any instrument suitable for measuring the optical density of the solution at a wavelength of550m4 may be used. c) 1cm or2cm cells (Note1). d) Alternatively, if a filter photometer of the balanced two cell type is used, the filter combination should conform a

23、s closely as possible to the above wavelength. The following have been found suitable: Tungsten lamp Ilford605,604 (Note2) 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 prepare

24、d and, where necessary, filtered. Standard antimony (1mlN 1.2mg of antimony). Dissolve0.12g of pure antimony by heating with5ml of sulphuric acid (sp. gr.1.84) and allow to cool, and dilute with15ml of water. Cool, and add50ml of hydrochloric acid (sp. gr.1.161.18). Transfer to a100ml graduated flas

25、k, and dilute to the mark. Standard antimony Solution A (1mlN 0.0024mg of antimony). Dilute2.0ml of the standard antimony solution(1mlN 1.2mg of antimony) with hydrochloric acid (sp. gr.1.161.18) to1litre in a graduated flask. Standard antimony Solution B (1mlN 0.0012mg of antimony). Dilute1.0ml of

26、the standard antimony solution(1mlN 1.2mg of antimony) with hydrochloric acid (sp. gr.1.161.18) to1litre in a graduated flask. Ceric sulphate. Add100ml of sulphuric acid(3percent v/v) to3.3g of ceric sulphate, warm to dissolve, and filter. Hydrochloric acid (10per cent v/v). Dilute100ml of hydrochlo

27、ric acid (sp. gr.1.161.18) to1litre. Hydroxyammonium chloride (1per cent w/v). Dissolve1g of hydroxyammonium chloride in100ml of water. Rhodamine B (0.02per cent w/v). Dissolve0.02g of rhodamine B in100ml of hydrochloric acid(10percent v/v). Sodium metabisulphite (1per cent w/v). Dissolve10g of sodi

28、um metabisulphite in water and dilute to1litre. Sampling Recommended methods of obtaining a suitable sample for the analytical procedure given below are described in BS3338-1, “Sampling of ingot tin”. Procedure To0.25 g of sample in a250ml beaker add10ml of sulphuric acid (sp. gr.1.84) heat to disso

29、lve, and allow to cool. Add30ml of water, then50ml of hydrochloric acid (sp. gr.1.161.18), warming on a hot plate if necessary, to dissolve any lead sulphate. Cool, transfer to a100ml graduated flask and dilute to the mark. Transfer by means of a pipette a10ml aliquot (Note3) into a separating funne

30、l, and add0.5ml of sodium metabisulphite solution(1per cent). Cool to below25 C and add3ml of the ceric sulphate solution, then0.5ml of hydroxyammonium chloride solution(1per cent). Allow to stand until the ceric sulphate is reduced then dilute to60ml. Add10.0ml of isopropyl ether, and shake for30 s

31、econds. Allow to separate and run off the aqueous layer. Wash twice with2ml portions of hydrochloric acid(10per cent) discarding the aqueous layer each time. Finally add2ml rhodamine B solution and shake for10 seconds. Allow to separate and discard the aqueous layer (Note4) together with a few drops

32、 of the ether layer. Dry the stem of the funnel with a roll of filter paper, and run off the isopropyl ether layer into a small stoppered bottle. Measure the optical density of the solution at20 1 C, using the conditions specified under “Apparatus”, and using isopropyl ether in the reference cell. C

33、arry 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 antimony in the sample by reference to the appropriate calibration graph.BS3338-3:1961 2 BSI 12-199

34、9 Calibration Transfer the following amounts of standard antimony solution (Note5) 1.0,2.0,3.0,4.0,5.0ml into separating funnels and adjust the volume of each to5ml with hydrochloric acid (sp. gr.1.161.18). Add5ml of water, and0.5ml of sodium metabisulphite solution(1percent) and continue as in the

35、procedure. Carry out simultaneously a blank determination, using the same quantity of reagents. Prepare calibration graphs by plotting optical density against weight of antimony in the various aliquots, after deduction of the blank reading. NOTE 1A2cm cell should be used for antimony contents in the

36、 range0.004 to0.024per cent and a1cm cell for antimony contents up to0.05per cent. NOTE 2For amounts of antimony greater than0.01mg it is preferable to use the Ilford604 filter. NOTE 3For antimony contents between0.05 and0.1per cent a5ml aliquot should be taken, and for those between0.1 and0.25per c

37、ent a2ml aliquot. These aliquots should be diluted to10ml with hydrochloric acid(50per cent). NOTE 4This solution should still be coloured red. If colourless a smaller aliquot of the original solution should be used. NOTE 5For the1cm cell use standard antimony SolutionA(1mlN 0.0024mg Sb) and for the

38、2cm cell use Solution B(1mlN 0.0012mg Sb).blankBS3338-3: 1961 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing BritishStandards. It presents the UK view on standards in Europe and at the international level. It is

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