BS 3338-18-1966 Methods for the sampling and analysis of tin and tin alloys - Method for the determination of aluminium in solders and white metal bearing alloys (photometric metho.pdf

1、BRITISH STANDARD BS 3338-18: 1966 Method for The determination of aluminium in solders and white metal bearing alloys (Photometric method) Methods for the sampling and analysis of tin and tin alloysBS3338-18:1966 This British Standard, having been approved by the Non-ferrousMetals Industry Standards

2、 Committee and endorsed by the Chairman oftheEngineering Divisional Council, was published under theauthority of the GeneralCouncil on 28July1966 BSI 12-1999 The following BSI references relate to the work on this standard: Committee references NFE/27, NFE/27/1 Draft for comment D65/3166 ISBN 0 580

3、03187 X 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 scient

4、ific 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 Bronze and Brass Foun

5、ders Institution of Production Engineers Association of Consulting Engineers Institution of Structural Engineers Board of Trade Lead Development Association British Bronze and Brass Ingot Manufacturers Light Metal Founders Association Association London Metal Exchange* British Electrical and Allied

6、Manufacturers Magnesium Industry Council Association* Ministry of Defence, Army Department* British Lead Manufacturers Association Ministry of Defence, Navy Department* British Non-ferrous Metals Federation National Brassfoundry Association British Non-ferrous Metals Research Non-ferrous Metal Stock

7、ists Association* Post Office* Copper Development Association Royal Institute of British Architects Crown Agents for Oversea Governments and Society of British Aerospace Companies Ltd. Administrations Society of Motor Manufacturers and Traders Electric Cable Makers Confederation Ltd.* High Conductiv

8、ity Copper Association Tin Research Institute* Institute of British Foundrymen Zinc Development Association Institute of Metals Individual manufacturer Institution of Mechanical Engineers (Automobile Division) British Railways Board London Transport Board British Tin Box Manufacturers Federation Sol

9、der 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 publication Amd. No. Date CommentsBS3338-18:1966

10、 BSI 11-1999 i Contents Page Co-operating organizations Inside front cover Foreword ii Introduction 1 Apparatus 1 Solutions required 1 Sampling 1 Procedure 1 Calibration 2 Notes 2BS3338-18:1966 ii BSI 11-1999 Foreword This standard makes reference to the following British Standards: BS 219, Soft sol

11、ders. BS 3252, Ingot tin. BS 3332, White metal bearing alloy ingots. BS 3338, Methods for the sampling and analysis of tin and tin alloys Part12: Sampling of solders Part 14: Sampling of white metal bearing alloy ingots. This method for the determination of aluminium in solders and white metal beari

12、ng alloys is the eighteenth 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 methods has been authorized by th

13、e 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 of tin in ingot tin; Part 3: Deter

14、mination 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 solders; Part 8: Determination of bi

15、smuth in ingot tin, tin-lead solders and white metal bearing alloys; Part 9: Determination of arsenic in 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: Determination of tin in solders; Part 12: Sampl

16、ing 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 16: Determination of tin in white metal bearing alloys; Part 17: Determin

17、ation of cadmium in solders and white metal bearing alloys; Part 19: Determination of zinc 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

18、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 range, sample weights or al

19、iquots 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.BS3338-18:1966 BSI 11-1999 iii

20、 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 This document comprises

21、 a front cover, an inside front cover, pagesi toiv, 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.iv blankBS3338-18:1966 BSI 11-1999 1 Introduction a)

22、 Principle. Aluminium is determined photometrically with chrome-azurol S after removal of interfering elements. b) Range. Up to0.05 percent aluminium. c) Reproducibility. 10percent of aluminium present. Apparatus a) All volumetric glassware used shall be of Class A accuracy as defined in the appropr

23、iate British Standards, or where no British Standard exists, as described in the National Physical Laboratory Publication “Volumetric Tests on Volumetric Glassware”. b) Any instrument suitable for measuring the optical density of the solution at a wavelength of550m may be used together with1cm cells

24、. c) Alternatively, where a filter photometer of the balanced two-cell type is used, the following conditions have been found suitable: Tungsten lamp Ilford605 or equivalent filters 2cm cells Solutions required All reagents shall be of the highest purity obtainable and distilled 1)water shall be use

25、d throughout. Solutions shall be freshly prepared and; where necessary, filtered. Standard aluminium (1mlN 0.1mg of aluminium). Dissolve1.7589g of aluminium potassium sulphate Al 2 (SO 4 ) 3. K 2 SO 4 .24H 2 O in water, transfer toa1litre volumetric flask and dilute to the mark. Standard aluminium (

26、1mlN 0.005mg of aluminium). Transfer25ml of standard aluminium solution (1mlN 0.1mg of aluminium) to a500ml volumetric flask and dilute to the mark. Acetic acid (1.16percent v/v). Dilute11.6ml of glacial acetic acid to1litre. Ammonia (10percent v/v). Dilute10ml of ammonia solution (sp. gr. 0.91) to1

27、00ml. Ascorbic acid (5percent w/v). Dissolve5g of ascorbic acid in water and dilute to100ml. This solution should be prepared freshly each day. Bromine-acid mixture. To45ml of hydrochloric acid (sp. gr. 1.161.18) and45ml of hydrobromic acid (sp. gr. 1.46 to1.49) add carefully10ml of bromine. Bromine

28、-hydrochloric acid. To90ml of hydrochloric acid (sp. gr. 1.16 to1.18) add carefully10ml of bromine. Buffer. To850ml of sodium acetate solution(2.72percent) add150ml of acetic acid(1.16percent) and mix. Chrome-Azurol S (0.3percent w/v). Dissolve0.3g of chrome Azurol S in water and dilute to100ml. Thi

29、s solution should be prepared freshly each day. Hydrochloric acid (10percent v/v). Dilute10ml of hydrochloric acid (sp. gr. 1.16 to1.18) to100ml. Hydrogen sulphide-sulphuric acid. Pass hydrogen sulphide through sulphuric acid (2percent) for10minutes. Nitric acid (50percent v/v). Dilute50ml of nitric

30、 acid (sp. gr. 1.42) to100ml. Sodium acetate (2.72percent w/v). Dissolve27.2g of sodium acetate (CH 3 COONa. 3H 2 O) in water and dilute to1litre. Sodium hydroxide (5percent w/v). Dissolve5g of sodium hydroxide in water and dilute to100ml. Sulphuric acid (50percent v/v). To40ml of water add cautious

31、ly50ml of sulphuric acid (sp. gr. 1.84) mix, cool and dilute to100ml. Sulphuric acid (2percent v/v). To40ml of water add cautiously2ml of sulphuric acid (sp. gr. 1.84) mix, cool and dilute to100ml. Sampling Recommended methods of obtaining a suitable sample for the analytical procedure given below a

32、re described in BS3338, Part 12 “Sampling of solders”, and Part 14, “Sampling of white metal bearing alloy ingots”. Procedure Weigh1g of sample and transfer to a150ml beaker. Add10ml of the bromine-acid mixture and evaporate to dryness. Add a further5ml of the bromine-acid mixture and repeat the eva

33、poration to dryness (Note1). 1) Water demineralized by ion exchange may be used if it is of equivalent quality.BS3338-18:1966 2 BSI 11-1999 Dissolve the residue in5ml of nitric acid(50percent) cool, add2ml of sulphuric acid(50percent) and evaporate to fuming. Cool, dilute to20ml, simmer for5minutes

34、and allow the precipitate to settle for1hour. Filter through a sintered glass filter (porosity4) washing with small quantities of sulphuric acid (2percent). Pass hydrogen sulphide through the warm filtrate for15minutes. Filter off any precipitate and wash with small quantities of hydrogen sulphide-s

35、ulphuric acid, collecting the filtrate ina100ml beaker. Evaporate to fuming and continue fuming until freed from sulphuric acid. Dissolve the residue in4ml of hydrochloric acid (10percent) and add20ml of water. Add sodium hydroxide solution(5percent) until the pH is approximately2.5. This should req

36、uire about3 4ml. Transfer to a50ml volumetric flask and dilute to the mark. Transfer a suitable aliquot (Note2) to a50ml volumetric flask, add1ml of ascorbic acid solution(5percent), 0.5ml of chrome-Azurol S solution (0.3percent) dilute to20ml and add ammonia solution (10percent) until the colour ch

37、anges to yellow. (Note3). Add20ml of the buffer solution, dilute to the mark and allow to stand for5to10minutes. Measure the optical density of the solution at20 1 C using the conditions specified under “Apparatus”. Carry out simultaneously a blank determination on the reagents. Follow the same proc

38、edure without the sample and use the same quantities of reagents. Deduct the blank reading and calculate the percentage of aluminium in the sample by reference to the calibration graph. Calibration Transfer to a series of100ml beakers the following amounts of standard aluminium solution(1ml=0.005mg

39、of aluminium): 0, 1.0, 2.0, 3.0, and4.0ml Continue from Paragraph3 of the procedure. Prepare a calibration graph by plotting optical density against the weight of aluminium in the various aliquots after deduction of the blank reading. Notes NOTE 1In the presence of more than15percent of lead remove

40、the bulk of the lead as follows: Dissolve the sample in20ml of the bromine-hydrochloric acid, evaporate to about3ml, dilute with20ml of water and cool in ice. Filter off the lead chloride on to a sintered glass filter (porosity4) and wash with small quantities of ice cold hydrochloric acid (10percen

41、t). Evaporate the filtrate to about5ml, add10ml of the bromine-acid mixture and evaporate to dryness. Add a further5ml of the bromine-acid mixture and repeat the evaporation to dryness. Continue from paragraph2 of the procedure. NOTE 2The aliquot taken should contain not more than0.02mg of aluminium

42、. NOTE 3This colour change occurs at a pH of approximately6. For alloy BS3332-9 the colour changes to mauve and not to yellow.blankBS 3338-18: 1966 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing BritishStandards.

43、 It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions BritishStandards are updated by amendment or revision. Users of BritishStandards should make sure that they possess the latest amendments or editions. It is the constant aim

44、 of BSI to improve the quality of our products and services. We would be grateful if anyone finding an inaccuracy or ambiguity while using this BritishStandard would inform the Secretary of the technical committee responsible, the identity of which can be found on the inside front cover. Tel:0208996

45、9000. Fax:02089967400. BSI offers members an individual updating service called PLUS which ensures that subscribers automatically receive the latest editions of standards. Buying standards Orders for all BSI, international and foreign standards publications should be addressed to Customer Services.

46、Tel:02089969001. Fax:02089967001. In response to orders for international standards, it is BSI policy to supply the BSI implementation of those that have been published as BritishStandards, unless otherwise requested. Information on standards BSI provides a wide range of information on national, Eur

47、opean and international standards through its Library and its Technical Help to Exporters Service. Various BSI electronic information services are also available which give details on all its products and services. Contact the Information Centre. Tel:02089967111. Fax:02089967048. Subscribing members

48、 of BSI are kept up to date with standards developments and receive substantial discounts on the purchase price of standards. For details of these and other benefits contact Membership Administration. Tel:02089967002. Fax:02089967001. Copyright Copyright subsists in all BSI publications. BSI also ho

49、lds the copyright, in the UK, of the publications of the international standardization bodies. Except as permitted under the Copyright, Designs and Patents Act 1988 no extract may be reproduced, stored in a retrieval system or transmitted in any form or by any means electronic, photocopying, recording or otherwise without prior written permission from BSI. This does not preclude the free use, in the course of implementing the standard, of necessary details such as symbols, and size, type or grade designations. If the