BS 3338-10-1961 Methods for the sampling and analysis of tin and tin alloys - Method for the determination of iron in ingot tin tin-lead solders and white metal bearing alloys (pho.pdf

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1、BRITISH STANDARD BS 3338-10: 1961 Method for The determination of iron in ingot tin, tin-lead solders and white metal bearing alloys (Photometric method) Methods for the sampling and analysis of tin and tin alloysBS3338-10:1961 This British Standard, having been approved by the Non-ferrous Metals In

2、dustry Standards Committee and endorsed by the Chairman oftheEngineering Divisional Council, was published undertheauthority of the GeneralCouncil on 19 June 1961 BSI 12-1999 The following BSI references relate to the work on this standard: Committee references NFE/27, NFE/27/1 Draft for comment AA(

3、NFE) 1390 ISBN0 580 03107 1 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: Admiralty* Institution of Mining and Metallurgy Aluminium Development Asso

5、ciation Institution of Structural Engineers Aluminium 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

6、 Manufacturers London Metal Exchange* Association 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 Off

7、ice* Association* Royal Institute of British Architects Cable Makers Association* Society of British Aircraft Constructors Copper Development Association Society of Motor Manufacturers and Traders Crown Agents for Oversea Governments and Limited* Administrations Tin Research Institute* High Commissi

8、on of India War Office* High Conductivity Copper Association Zinc Development Association Institute of British Foundrymen Individual manufacturers Institute of Metals Institution of Mechanical Engineers (Automobile Division) British Railways, The British Transport London Transport Executive, The Bri

9、tish Commission Transport Commission British Tin Box Manufacturers Federation Solder Makers Association Electronic Engineering Association Tinplate Conference (1925) Gas Council Tin Producers Association Institution of Gas Engineers Individual firms Amendments issued since publication Amd. No. Date

10、CommentsBS3338-10:1961 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 Calibration 1BS3338-10:1961 ii BSI 12-1999 Foreword This standard makes reference to the following British Standards: BS

11、 3338-1, Sampling of ingot tin Part 12: Sampling of solders Part14:Sampling of white metal bearing alloys. This method for the determination of iron in ingot tin, tin-lead solders and white metal bearing alloys, is the tenth of a series of methods which will form a complete British Standard under th

12、e 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 the Non-ferrous Metals Industry Standards Committee as part of a general programme for the standardizatio

13、n 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: Determination of antimony in ingot tin; Part 4: Determination of copper in ingot tin and tin-lead solders; P

14、art 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 bismuth in ingot tin, tin-lead solders and white metal bearing alloys; Part 9: Determination of arsenic i

15、n ingot tin, tin-lead solders and white metal bearing alloys; Part 11: Determination of tin in solders; Part 12: Sampling of solders. 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 meta

16、l 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

17、aliquots 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. In the preparation of the c

18、alibration graphs an attempt has been made to define concentrations, but because these are linked with the particular instrument used for determining optical density they should be used only as a guide. A British Standard does not purport to include all the necessary provisions of a contract. Users

19、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 and ii, pages1 and 2 and a back cover. This standar

20、d 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.BS3338-10:1961 BSI 12-1999 1 Introduction a) Principle. Iron is determined photometrically with o-phenanthroline. b) Range. Up to 0.03 per cent ir

21、on (Note 1). c) Reproducibility. 10 per cent of iron 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 described in the National Physical Laboratory Publication “Volumetric Tests o

22、n Volumetric Glassware”. b) Any instrument suitable for measuring the optical density of the solution at a wavelength of510m4 may be used. c) 1 cm or 4 cm cells (Note2). d) Alternatively, if a filter photometer of the balanced two cell type is used, the filter combination should conform as closely a

23、s possible to the above wavelength. The following have been found suitable: Tungsten lamp Ilford 604 or equivalent filters. 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

24、, filtered. Standard iron solution A (1 ml N 1.0mg of iron). Dissolve 0.100g of pure iron wire in10ml of aqua regia and dilute to100ml in a graduated flask. Standard iron solution B (1 ml N 0.05 mg of iron). Dilute12.5ml of solution A to250ml in a graduated flask. Standard iron solution C (1 ml N 0.

25、01 mg of iron). Dilute20ml of solution B to100ml in a graduated flask. Ammonium nitrate (1 per cent w/v). Dissolve5g of ammonium nitrate in250ml of water. Dilute to500ml and mix. Bromine-hydrobromic acid. Add 10 ml of bromine to90ml of hydrobromic acid (48 per cent v/v). Buffer. Dissolve 270 g of so

26、dium acetate in500ml of water, add240ml of acetic acid (glacial) and dilute to1litre. Hydroxyammonium chloride (10 per cent w/v). Dissolve 10 g of hydroxyammonium chloride in100ml of water. Nitric acid (50 per cent v/v). Dilute50ml of nitric acid (sp. gr. 1.42) to100ml. o-phenanthroline. (0.25 per c

27、ent w/v). Dissolve0.25g of o-phenanthroline in100ml of hot water and allow to cool. Sampling Recommended methods of obtaining a suitable sample for the analytical procedure given below are described in BS 3338-1, “Sampling of ingot tin”; Part12, “Sampling of solders”; and Part 14, “Sampling of white

28、 metal bearing alloys”, Procedure Dissolve 1.00 g of sample in 10ml of bromine-hydrobromic acid in a150ml beaker and evaporate to dryness. Add a further5ml of bromine-hydrobromic acid and evaporate again. To the residue add5ml of nitric acid (50per cent) and boil until free from bromine (Notes 3 and

29、 4). Add ammonia solution.(sp. gr.0.91) until neutral to litmus paper then acetic acid (glacial) until just acid. Add2ml of hydroxyammonium chloride solution(10per cent) and15ml of the buffer solution and heat to incipient boiling to ensure reduction of iron. Cool, transfer to a 50 ml graduated flas

30、k, add10ml of o-phenanthroline and dilute to the mark. Measure the optical density of the solution at20 1 C, using the conditions specified under “Apparatus,” and using water in the reference cell. Carry out simultaneously a blank determination on the reagents. Follow the same procedure without the

31、sample and use the same quantity of reagents. Deduct the blank reading and calculate the percentage iron in the sample by reference to the appropriate calibration graph. Calibration Transfer to 150-ml beakers the following amounts of standard iron solution: for the 4 cm cell 1.0, 2.0, 3.0, 4.0, 5.0

32、ml of Solution C (1 ml N 0.01 mg Fe) for the 1 cm cell 1.0, 2.0, 3.0, 4.0, 5.0 ml of Solution B (1 ml N 0.05 mg Fe). Add 2 ml of hydroxyammonium chloride solution(10per cent) and15ml of the buffer solution. Heat to reduce the iron, cool, transfer to50-ml graduated flasks and continue as in the proce

33、dure. Carry out simultaneously a blank, using the same quantities of reagents. Prepare calibration graphs by plotting optical, density against weight of iron in the various aliquots, after deduction of the blank reading.BS3338-10:1961 2 BSI 12-1999 NOTE 1Iron content in excess of0.03per cent may be

34、determined if a smaller sample weight is taken. NOTE 2A 1 cm cell should be used for iron content in the range0.0050.03per cent, and a4cm cell for iron content down to0.001per cent. NOTE 3In the presence of more than 1mg of copper and for amounts of more than0.4g of lead in the weight of sample take

35、n, add1ml of sulphuric acid and evaporate to fuming. Cool, add25ml of water and saturate with hydrogen sulphide. Filter and discard the precipitate. Boil the filtrate until free from hydrogen sulphide and evaporate to less than20ml. Neutralize with ammonia solution (sp. gr.0.91) and continue as in t

36、he procedure. NOTE 4In the presence of alloying amounts of zinc, dilute to50ml, add a solution of3mg of aluminium as chloride, neutralize with ammonia solution (sp. gr.0.91), and add sufficient excess to re-dissolve the zinc hydroxide. Heat to coagulate, filter through a small paper pulp pad and was

37、h with hot ammonium nitrate (1per cent). Re-dissolve the precipitate in5ml of warm nitric acid (50per cent), wash with hot water, and continue with the standard procedure.blankBS 3338-10: 1961 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national bod

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