1、BRITISH STANDARD BS3338-11: 1961 Method for The determination of tin in solders (Nickel coil reduction method)BS3338-11:1961 This British Standard, having been approved by the Non-ferrous Metals Industry Standards Committee and endorsed by the Chairman oftheEngineering Divisional Council, was publis
2、hed undertheauthority of the GeneralCouncil on 17February1961 BSI12-1999 The following BSI references relate to the work on this standard: Committee references NFE/27, NFE/27/1 Draft for comment AA(NFE)1391 ISBN 0 580 03117 9 Co-operating organizations The Non-ferrous Metals Industry Standards Commi
3、ttee, under whose supervision this British Standard was prepared, consists of representatives from the following Government departments and scientific and industrial organizations: Admiralty* Institution of Mining and Metallurgy Aluminium Development Association Institution of Structural Engineers A
4、luminium 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 Manufacturers London Metal Exchange* Associa
5、tion 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* Association* Royal Institute of British
6、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 India War Office* High Conductivity Copper
7、 Association Zinc Development Association Institute of British Foundrymen Individual manufacturers Institute of Metals Institution of Mechanical Engineers (Automobile Division) The Government departments and scientific and industrial organizations marked with an asterisk in the above list, together
8、with the following, were directly represented on the committee entrusted with the preparation of this British Standard: British Railways, The British Transport Solder Makers Association Commission Tinplate Conference(1925) British Tin Box Manufacturers Federation Tin Producers Association Electronic
9、 Engineering Association White Metal Bearing Manufacturers Gas Council Individual manufacturers Institution of Gas Engineers London Transport Executive, The British Transport Commission Amendments issued since publication Amd. No. Date CommentsBS3338-11:1961 BSI 12-1999 i Contents Page Co-operating
10、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 2BS3338-11:1961 ii BSI 12-1999 Foreword This standard makes reference to the following BritishStandards: BS219, Soft solders. B
11、S3338, Methods for the sampling and analysis of tin and tin alloys Part12:Sampling of solders. This method for the determination of tin in solders, is the eleventh of a series of methods which will form a complete British Standard under the collective title “Methods for the sampling and analysis of
12、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 methods for the sampling and analysis of non-ferrous met
13、als. Other methods in the series are as follows: Part1: Sampling of ingot tin; Part2: Determination of tin in ingot tin; Part3: Determination of antimony in ingot tin; Part4: Determination of copper in ingot tin and tin-lead solders; Part5: Determination of lead in ingot tin and tin-antimony solders
14、; 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; Part10:
15、Determination of iron in ingot tin, tin-lead solders and white metal bearing alloys; Part12: Sampling of solders. 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”
16、. 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 of aliquots should be adju
17、sted 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. A British Standard does not purport to include all
18、 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 This document comprises a front cover, an inside front cover, pagesi andii
19、, pages1 and2 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.BS3338-11:1961 BSI 12-1999 1 Introduction a) Principle. Tin is determined volumetrically with potassiu
20、m iodate after reduction with nickel. b) Range. For tin contents exceeding1percent. c) Reproducibility. 0.1percent of tin present. Apparatus a) Any volumetric glassware used shall be of Class A accuracy as defined in the appropriate British Standards, or where no British Standard exists, as describe
21、d in the National Physical Laboratory Publication “Volumetric Tests on Volumetric Glassware”. b) A suitable form of apparatus is illustrated in Figure 1. The nickel coil should be etched before use by boiling in hydrochloric acid(50per cent v/v) containing20per cent of sodium chloride. Wash well in
22、cold water and leave immersed in cold water until required. Solutions required All reagents shall be of the highest purity obtainable and distilled water shall be used throughout. Solutions shall be freshly prepared and, where necessary filtered. Standard potassium iodate/iodide (1mlN 0.01g of tin).
23、 Dissolve6.05g of potassium iodate (previously dried at105110 C) in400ml of water containing1g of sodium hydroxide. Add30g of potassium iodide and dilute to1litre in a graduated flask. Standard potassium iodate/iodide (1mlN 2mg of tin). Dilute200ml of the above solution to1litre in a graduated flask
24、. Bromine-hydrochloric acid. Add20ml of bromine to2litres of hydrochloric acid (sp. gr.1.161.18). Hydrochloric acid (50per cent v/v). Dilute50ml of hydrochloric acid (sp. gr.1.161.18) to100ml. Sodium hydrogen carbonate. Saturated solution. Starch. Make a suspension of0.5g of starch in a10ml of water
25、. 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 BS3338-12, “Sampling of solders”. Procedure Weigh accurately triplicate portions of1.00g of sample a
26、nd transfer each to a500ml beaker. To each add100ml of bromine-hydrochloric acid and warm gently until dissolved, ensuring that bromine is always in excess, if necessary by the addition of a further25ml of bromine-hydrochloric acid. Add a few pieces of porous pot and boil to expel excess bromine (No
27、te1), then add100ml of water, and2g of iron powder. Heat gently until the reaction ceases. Filter through a small paper-pulp pad into a500ml flask, washing three times with hydrochloric acid(50per cent). Transfer the residue and the pad to the original beaker, and boil for5minutes with20ml of bromin
28、e-hydrochloric acid. Add2g of iron powder, and when the reaction ceases, filter through a small pad of paper-pulp into the first filtrate. Wash four times with hydrochloric acid(50per cent). Fill the reservoir of the Contat-Gckel trap with sodium hydrogen carbonate solution (saturated), introduce th
29、e nickel coil and Contat-Gckel assembly, close the flask and boil gently for30minutes. Cool slightly and close the outlet tube with a rubber cap. Cool in running water, remove the nickel coil and wash with water into the solution. Add5ml of starch solution, and titrate quickly, with a minimum of sti
30、rring, with standard potassium iodate/iodide solution(1mlN 0.01g of tin) (Note2) to a permanent blue colour. Standardization Weigh accurately triplicate portions of0.4g of pure tin foil, and transfer to500ml flasks. Add100ml of bromine-hydrochloric acid and heat gently until dissolved, ensuring that
31、 bromine is always in excess. Add a few pieces of porous pot and boil to expel the excess bromine (see Note1). Add50ml of hydrochloric acid (sp. gr.1.161.18),100ml of hot water, and2g of iron powder. Boil gently until the iron is dissolved. Introduce the nickel coil and Contat-Gckel assembly. Close
32、the flask and boil gently for30minutes. Cool in running water and titrate as described in the procedure. NOTE 1The solution should not be boiled longer than is necessary. The use of a boiling rod will facilitate rapid removal of bromine. NOTE 2For silver bearing solders, e.g.BS219, “Soft solders”,1S
33、 and5S, standard potassium iodate/iodide(1mlN 2mg of tin) should be used.BS3338-11:1961 2 BSI 12-1999 Figure 1 Assembly for reduction of tinblankBS3338-11: 1961 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing Brit
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