1、BRITISH STANDARD BS 3338-16: 1965 Method for The determination of tin in white metal bearing alloys (Nickel coil reduction method) Methods for the sampling and analysis of tin and tin alloysBS3338-16:1965 This British Standard, having been approved by the Non-ferrousMetals Industry Standards Committ
2、ee and endorsed by the Chairman of theEngineering Divisional Council, was published undertheauthority of the GeneralCouncil 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 D63/1212 ISBN 0 580 03167 5
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 an
4、d 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 Bronze and Brass Founders In
5、stitution 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 London Metal Exchange* Associat
6、ion* 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 Transport Copper Development Ass
7、ociation 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 Companies Ltd. High Conductivity C
8、opper 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 Board London Transport Board
9、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 Amendments issued since publ
10、ication Amd. No. Date CommentsBS3338-16:1965 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 Standardization 1 Figure 1 Assembly for reduction of tin 2BS3338-16:1965 ii BSI 12-1999 Foreword T
11、his standard makes 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 14: Sampling of white metal bearing alloy ingots. This method for the determ
12、ination of tin in white metal bearing alloys is the sixteenth 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 preparation of this series of
13、 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; Part 2: Determination
14、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: Determination of silver in so
15、lders; 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 alloys; Part 11: Determi
16、nation of tin in solders; Part 12: Sampling of solders; Part 13: Determination of antimony in solders and white metal bearing alloys; Part 14: Sampling of white metal bearing alloy ingots; Part 15: Determination of copper and lead in white metal bearing alloys; Part 17: Determination of cadmium in s
17、olders 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 aliquots h
18、ave 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 and reprodu
19、cible 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.BS3338-16:1965 BSI 12-1999 iii A British Standard does not purport to include all the necessary provisions of a contract. Use
20、rs 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 toiv, pages1and2 and a back cover. This standard
21、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 blankBS3338-16:1965 BSI 12-1999 1 Introduction a) Principle. Tin is determined volumetrically with potassium iodate after reduction with nickel.
22、b) Range. For tin contents from5 to90per cent. c) Reproducibility. 0.2per cent. Apparatus a) 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 Publication “
23、Volumetric tests on volumetric glassware”. b) A suitable form of apparatus is illustrated inFigure 1. The nickel coil should be etched before use by boiling in hydrochloric acid (50per centv/v) containing20per cent of sodium chloride. Wash well in cold water and leave immersed in cold water until re
24、quired. 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 iodate/iodide (1mlN 0.01g of tin). Dissolve6.05g of potassium iodate (previously dried at105
25、110 C) in400ml of water containing1g of sodium hydroxide. Add30g of potassium iodide, transfer to a1litre volumetric flask and dilute to the mark. Potassium iodate/iodide (1mlN 2mg of tin). Transfer200ml of potassium iodate/iodide solution(1mlN 0.01g of tin) to a1litre volumetric flask and dilute to
26、 the mark. Bromine-hydrochloric acid. To2litres of hydrochloric acid (sp.gr.1.161.18) add20ml of bromine. Hydrochloric acid (10per centv/v). Dilute10ml of hydrochloric acid (sp.gr.1.161.18) to100ml. Sodium hydrogen carbonate. Saturated solution. Starch (0.5per centw/v). Make a suspension of0.5g of s
27、tarch in10ml of water. Add to90ml of boiling water. Cool and dilute to100ml. Prepare freshly each day. Sampling Recommended methods of obtaining a suitable sample for the analytical procedure given below are described in BS3338-14, “Sampling of white metal bearing alloy ingots”. Procedure Weigh accu
28、rately0.5g of sample (Note1) and transfer to a500ml beaker. Add50ml of bromine-hydrochloric acid and warm gently until dissolved. Add50ml of water and4g of iron powder, reduced by hydrogen. Heat gently until the iron is dissolved, cool and add a further1g of iron powder. Filter immediately through a
29、 small paper-pulp pad into a500ml flask, washing three times with hydrochloric acid (10per cent). Transfer the residue and the pad to the original beaker and boil for5minutes with20ml of the bromine-hydrochloric acid. Add a further4g of the iron powder and allow to stand until the iron is nearly dis
30、solved. Cool and filter through a small paper-pulp pad into the first filtrate. Wash three times with hydrochloric acid (10per cent). Fill the reservoir of the Contat-Gckel trap with sodium hydrogen carbonate solution (saturated), introduce the nickel coil and Contat-Gckel assembly, close the flask
31、and boil gently for30minutes. Cool slightly and close the outlet tube with a rubber cap. Cool in running water to below20 C, remove the nickel coil and wash with freshly boiled and cooled water into the solution. Add5ml of starch solution(0.5per centw/v) and titrate quickly, with a minimum of stirri
32、ng, with standard potassium iodate/iodide solution (1mlN 0.01g of tin) (Note2) to a permanent blue colour. Standardization Weigh accurately0.4g of high purity tin foil and transfer to a500ml flask. Add50mg of antimony as the trichloride and50ml of the bromine-hydrochloric acid and heat gently to dis
33、solve. Continue from the second paragraph of “Procedure”. NOTE 1For alloys containing up to50per cent of tin use a1g sample. NOTE 2For tin contents less than10per cent, standard potassium iodate/iodide (1mlN 2mg of tin) should be used. 1) Water demineralized by ion exchange may be used if it is of e
34、quivalent quality.BS3338-16:1965 2 BSI 12-1999 Figure 1 Assembly for reduction of tinblankBS 3338-16: 1965 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
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