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1、BRITISH STANDARD BS 3338-13: 1965 Method for The determination of antimony in solders and white metal bearing alloys (Volumetric: potassium bromate method) Methods for the sampling and analysis of tin and tin alloys Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:34 GMT+00:00 2006, Unco
2、ntrolled Copy, (c) BSI BS 3338-13:1965 This British Standard, having been approved by the Non-ferrous Metals Industry Standards Committee and endorsed by the Chairman of the Engineering Divisional Council, was published under the authority of the General Council on 18 March 1965 BSI 12-1999 The foll
3、owing BSI references relate to the work on this standard: Committee references NFE/27, NFE/27/1 Draft for comment D63/1210 ISBN 0 580 03137 3 Co-operating organizations The Non-ferrous Metals Industry Standards Committee, under whose supervision this British Standard was prepared, consists of repres
4、entatives from the following Government departments and scientific and industrial organizations: The Government departments 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 th
5、e preparation of this British Standard: Aluminium FederationInstitution of Mining and Metallurgy Association of Bronze and Brass FoundersInstitution of Production Engineers Association of Consulting EngineersInstitution of Structural Engineers British Bronze and Brass Ingot ManufacturersLead Develop
6、ment Association AssociationLight Metal Founders Association British Electrical and Allied ManufacturersLondon Metal Exchange* Association*Magnesium Industry Council British Lead Manufacturers AssociationMinistry of Aviation British Non-ferrous Metals FederationMinistry of Defence, Army Department*
7、British Non-ferrous Metals ResearchMinistry of Defence, Naval Department* Association*Ministry of Transport Copper Development AssociationNational Brassfoundry Association Crown Agents for Oversea Governments andNon-ferrous Metal Stockists AdministrationsPost Office* Electric Cable Makers Federation
8、Royal Institute of British Architects High Commission of IndiaSociety of British Aerospace Companies Ltd. High Conductivity Copper AssociationSociety of Motor Manufacturers and Traders Institute of British FoundrymenLtd.* Institute of MetalsTin Research Institute* Institution of Mechanical Engineers
9、Zinc Development Association (Automobile Division)Individual manufacturer British Railways BoardLondon Transport Board British Tin Box Manufacturers FederationSolder Makers Association Cable Makers AssociationTinplate Conference (1925) Electronic Engineering AssociationTin Producers Association Gas
10、CouncilWhite Metal Bearing Manufacturers Institution of Gas EngineersIndividual firms Amendments issued since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:34 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-13:1965 BSI 12-1999i Contents Page Co-oper
11、ating organizationsInside front cover Forewordii Introduction1 Apparatus1 Solutions required1 Sampling1 Procedure1 Calculation1 Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:34 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-13:1965 ii BSI 12-1999 Foreword This standard makes refer
12、ence to the following British Standards: 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 12: Sampling of solders Part 14: Sampling of white metal bearing alloy ingots. This method for the d
13、etermination of antimony in solders and white metal bearing alloys is the thirteenth 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 prepar
14、ation 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 follows: Part 1: Sampling of ingot tin;
15、 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; Part 5: Determination of lead in ingot tin and tin-antimony solders; Part 6: Determination of copper in high purity ingot tin; Part 7: Determ
16、ination of silver in solders; Part 8: Determination of bismuth in 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 a
17、lloys; Part 11: Determination of tin in solders; Part 12: Sampling of solders; Part 14: Sampling of white metal bearing alloy ingots; Part 15: Determination of copper and lead in white metal bearing alloys; Part 16: Determination of tin in white metal bearing alloys; Part 17: Determination of cadmiu
18、m in solders and white metal bearing alloys. The complete British Standard methods will be found suitable for the grades of metals covered by BS 3252, “Ingot tin”, BS 219, “Soft solders”, and BS 3332, “White metal bearing alloy ingots”. In the methods for determining impurities, sample weights and a
19、liquots 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 reliable an
20、d 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. Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:34 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-
21、13:1965 BSI 12-1999iii 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 confer immunity from legal obligations. Summary of pages T
22、his 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 copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Lic
23、ensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:34 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv blank Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:34 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-13:1965 BSI 12-19991 Introduction a) Principle. Antimony is determined v
24、olumetrically with potassium bromate. b) Range. From 0.2 to 17 per cent antimony. c) Reproducibility. 0.05 per cent. Apparatus 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
25、 Physical Laboratory Publication “Volumetric tests on volumetric glassware”. Solutions required All reagents shall be of the highest purity obtainable and distilled water1) shall be used throughout. Solutions shall be freshly prepared and, where necessary, filtered. Potassium bromate (N/10). Dissolv
26、e 2.7836 g of potassium bromate (previously dried for one hour at 105110 C) in water. Transfer to a 1 litre volumetric flask and dilute to the mark. Potassium bromate (N/20). Transfer 500 ml of potassium bromate solution (N/10) to a 1 litre volumetric flask and dilute to the mark. Methyl orange (0.1
27、 per cent w/v). Dissolve 0.1 g of methyl orange in water and dilute to 100 ml. Sampling Recommended methods of obtaining a suitable sample for the analytical procedure given below are described in BS 3338-12, “Sampling of solders” and Part 14, “Sampling of white metal bearing alloy ingots”. Procedur
28、e Weigh 2 g of sample (Note 1) and transfer to a 500 ml conical beaker. Add 20 ml of sulphuric acid (sp. gr. 1.84) and 2 g to 3 g of potassium sulphate, and heat over an open flame to expel sulphur. Cool, add 10 ml of water, 75 ml of hydrochloric acid (sp. gr. 1.161.18) and 1 g of sodium sulphite. B
29、oil vigorously until the volume is reduced 60 5 ml, to ensure removal of arsenic. Dilute to 300 ml, heat to 8090 C, and if more than 0.3 per cent copper is present pass a rapid current of air through the solution for 5 minutes. Titrate the solution at a temperature of 8090 C with potassium bromate s
30、olution (N/20) (Note 1) using 3 drops of methyl orange as indicator preferably added near the end of the titration. The end point is indicated by the disappearance of the red colour of the methyl orange. Carry out simultaneously a blank determination on the reagents. Follow the same procedure withou
31、t the sample and use the same quantity of reagents. Deduct the blank reading and calculate the percentage antimony in the sample. Calculation 1 ml of potassium bromate (N/20) N 3.044 mg of antimony NOTE 1For solder 95A of BS 219 and white metal bearing alloys use a 1 g sample and titrate with potass
32、ium bromate solution (N/10). 1) Water demineralized by ion exchange may be used if it is of equivalent quality. whereA = volume (ml) of potassium bromate (N/20) used, W = weight (g) of sample taken. Antimony per cent A0.3044 W -= Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:34 GMT+00
33、:00 2006, Uncontrolled Copy, (c) BSI 2 blank Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:34 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-13:1965 BSI 12-1999 British Standards The following are available on application: YEARBOOK Including subject index and numerical list of Bri
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