1、BRITISH STANDARD BS 3338-13: 1965 Method for The determination of antimony in solders andwhite metal bearing alloys (Volumetric: potassium bromate method) Methods for the sampling and analysis of tin and tin alloysBS3338-13:1965 This British Standard, having been approved by the Non-ferrous Metals I
2、ndustry Standards Committee and endorsed by the Chairman of theEngineering Divisional Council, was published under theauthority of the General Council on 18March1965 BSI 12-1999 The following BSI references relate to the work on this standard: Committee references NFE/27, NFE/27/1 Draft for comment
3、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 representatives from the following Government departments and scientific and industrial organizations: The Government de
4、partments 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 British Standard: Aluminium Federation Institution of Mining and Metallurgy Association of B
5、ronze and Brass Founders Institution of Production Engineers Association of Consulting Engineers Institution of Structural Engineers British Bronze and Brass Ingot Manufacturers Lead Development Association Association Light Metal Founders Association British Electrical and Allied Manufacturers Lond
6、on Metal Exchange* Association* Magnesium Industry Council British Lead Manufacturers Association Ministry of Aviation British Non-ferrous Metals Federation Ministry of Defence, Army Department* British Non-ferrous Metals Research Ministry of Defence, Naval Department* Association* Ministry of Trans
7、port Copper Development Association National Brassfoundry Association Crown Agents for Oversea Governments and Non-ferrous Metal Stockists Administrations Post Office* Electric Cable Makers Federation Royal Institute of British Architects High Commission of India Society of British Aerospace Compani
8、es Ltd. High Conductivity Copper Association Society of Motor Manufacturers and Traders Institute of British Foundrymen Ltd.* Institute of Metals Tin Research Institute* Institution of Mechanical Engineers Zinc Development Association (Automobile Division) Individual manufacturer British Railways Bo
9、ard London Transport Board British Tin Box Manufacturers Federation Solder Makers Association Cable Makers Association Tinplate Conference(1925) Electronic Engineering Association Tin Producers Association Gas Council White Metal Bearing Manufacturers Institution of Gas Engineers Individual firms Am
10、endments issued since publication Amd. No. Date CommentsBS3338-13:1965 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 Calculation 1BS3338-13:1965 ii BSI 12-1999 Foreword This standard makes
11、reference 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
12、the determination 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 p
13、reparation 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
14、 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; Part 5: Determination of lead in ingot tin and tin-antimony solders; Part 6: Determination of copper in high purity ingot tin; Part 7: D
15、etermination 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 bear
16、ing alloys; 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 c
17、admium in solders and white metal bearing alloys. 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 weights and
18、 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 reliable
19、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.BS3338-13:1965 BSI 12-1999 iii A British Standard does not purport to include all the necessary provisions of a co
20、ntract. 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, pages i to iv, pages1and 2, an inside back co
21、ver 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.iv blankBS3338-13:1965 BSI 12-1999 1 Introduction a) Principle. Antimony is determined volumetrically with potas
22、sium bromate. b) Range. From0.2 to17percent antimony. c) Reproducibility. 0.05percent. 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 Physical Laboratory Publicati
23、on “Volumetric tests on volumetric glassware”. Solutions required All reagents shall be of the highest purity obtainable and distilled water 1)shall be used throughout. Solutions shall be freshly prepared and, where necessary, filtered. Potassium bromate (N/10). Dissolve2.7836g of potassium bromate
24、(previously dried for one hour at105110 C) in water. Transfer to a1litre volumetric flask and dilute to the mark. Potassium bromate (N/20). Transfer500ml of potassium bromate solution (N/10) to a1litre volumetric flask and dilute to the mark. Methyl orange (0.1percent w/v). Dissolve0.1g of methyl or
25、ange in water and dilute to100ml. Sampling Recommended methods of obtaining a suitable sample for the analytical procedure given below are described in BS3338-12, “Sampling of solders” and Part 14, “Sampling of white metal bearing alloy ingots”. Procedure Weigh2g of sample (Note1) and transfer to a5
26、00ml conical beaker. Add20ml of sulphuric acid (sp. gr.1.84) and2g to3g of potassium sulphate, and heat over an open flame to expel sulphur. Cool, add10ml of water,75ml of hydrochloric acid (sp. gr.1.161.18) and1g of sodium sulphite. Boil vigorously until the volume is reduced605ml, to ensure remova
27、l of arsenic. Dilute to300ml, heat to8090 C, and if more than0.3percent copper is present pass a rapid current of air through the solution for5minutes. Titrate the solution at a temperature of8090 C with potassium bromate solution(N/20) (Note1) using3 drops of methyl orange as indicator preferably a
28、dded 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 without the sample and use the same quantity of reagents. Deduct the blank reading and
29、 calculate the percentage antimony in the sample. Calculation 1 ml of potassium bromate (N/20)N 3.044 mg of antimony NOTE 1For solder95A of BS219 and white metal bearing alloys use a1g sample and titrate with potassium bromate solution(N/10). 1) Water demineralized by ion exchange may be used if it
30、is of equivalent quality. where A = volume (ml) of potassium bromate (N/20) used, W = weight (g) of sample taken. Antimony per cent A 0.3044 W - =2 blankBS3338-13:1965 BSI 12-1999 British Standards The following are available on application: YEARBOOK Including subject index and numerical list of Bri
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