1、BRITISHSTANDARD BS3338-9: 1965 Method for The determination of arsenic in ingot tin, solders and white metal bearing alloys (Photometric method) Methods for the sampling and analysis of tin and tin alloysBS3338-9:1965 This BritishStandard, having been approved by the Non-ferrous Metals Industry Stan
2、dards Committee and endorsed by the Chairman of theEngineering Divisional Council, was published under theauthority of the General Council on 18March1965 BSI12-1999 The following BSI references relate to the work on this standard: Committee references NFE/27, NFE/27/1 Draft for comment D63/4039 ISBN
3、 0 580 03097 0 Co-operating organizations The Non-ferrous Metals Industry Standards Committee, under whose supervision this BritishStandard was prepared, consists of representatives from the following Government departments and scientific and industrial organizations: The Government departments and
4、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 thisBritishStandard: Aluminium Federation Institution of Mining and Metallurgy Association of Bronze and Brass
5、Founders Institution of Production Engineers Association of Consulting Engineers Institution of Structural Engineers British Bronze and Brass Ingot Lead Development Association Manufacturers Association Light Metal Founders Association British Electrical and Allied Manufacturers London Metal Exchang
6、e* 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 Transport Copper Deve
7、lopment 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 Companies Ltd. High Con
8、ductivity Copper Association Society of Motor Manufacturers and Institute of British Foundrymen Traders Ltd.* Institute of Metals Tin Research Institute* Institution of Mechanical Engineers Zinc Development Association (Automobile Division) Individual manufacturer British Railways Board London Trans
9、port 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 Amendments issued
10、 since publication Amd. No. Date CommentsBS3338-9:1965 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 Calibration 2 Figure 1 Distillation apparatus 3BS3338-9:1965 ii BSI 12-1999 Foreword Thi
11、s standard makes reference to the following BritishStandards: BS219, Soft solders. BS572, Interchangeable conical ground glass joints. BS3252, Ingot tin. BS3332, White metal bearings alloy ingots. BS3338, Methods for the sampling and analysis of tin and tin alloys Part1:Sampling of ingot tin Part 12
12、: Sampling of solders Part 14: Sampling of white metal bearing alloy ingots. This method for the determination of arsenic in ingot tin, solders and white metal bearing alloys is the ninth of a series of methods which will form a complete BritishStandard under the collective title “Methods for the sa
13、mpling 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 standardization of methods for the sampling and anal
14、ysis 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; Part 5: Determination of lead in ingot
15、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 10: Determination of iron in ingot tin, tin-lead solders and white
16、metal bearing alloys; Part 11: Determination 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;
17、Part 16: Determination of tin in white metal bearing alloys; Part 17: Determination of cadmium in solders and white metal bearing alloys. The complete BritishStandard methods will be found suitable for the grades of metals covered by BS3252, “Ingot tin”, BS219, “Soft solders”, and BS3332, “White met
18、al 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
19、 aliquots should be adjusted accordingly.BS3338-9:1965 BSI 12-1999 iii 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 disput
20、e. 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 compris
21、es a front cover, an inside front cover, pagesi toiv, pages1to3 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 blankBS3338-9:1965 BSI 12-1999 1 Introduction a)
22、Principle. After separation by distillation of the trichloride, arsenic is determined photometrically as the reduced arsenomolybdate complex. b) Range. From0.01 to0.3percent arsenic. c) Reproducibility. 10per cent of arsenic present. Apparatus a) All volumetric glassware used shall be of ClassA accu
23、racy as defined in the appropriate BritishStandards, or where no BritishStandard 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 of830m4 may b
24、e used together with1cm cells. c) Alternatively, when a filter photometer of the balanced two cell type is used, the following conditions have been found suitable: Tungsten lamp Ilford207 or equivalent filters NOTEIlford608 filters may be used, but involve a reduction in sensitivity of about50per ce
25、nt. 1cm cell. 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. Standard arsenic (1mlN 0.1mg of arsenic). Dissolve0.132g of arsenious oxide in2ml of sodium hydr
26、oxide solution (5per cent w/v). Dilute to approximately50ml and add1ml of hydrochloric acid (sp. gr.1.161.18). Transfer to a1litre volumetric flask and dilute to the mark. Ammonium molybdate (1per cent w/v). Dissolve1g of ammonium molybdate (NH 4 ) 6 Mo 7 O 24 .4H 2 O in sulphuric acid (20per cent v
27、/v) and dilute to100ml with the sulphuric acid. Hydrazine sulphate. Dissolve0.15g of hydrazine sulphate in water and dilute to100ml. Ammonium molybdate-hydrazine sulphate. Dilute10ml of the ammonium molybdate solution to90ml, add1ml of the hydrazine sulphate solution and dilute to100ml. Sulphuric ac
28、id (50per cent v/v). To400ml of wateradd cautiously500ml of sulphuric acid (sp.gr.1.84). Mix, cool and dilute to1litre. Sampling Recommended methods of obtaining a suitable sample for the analytical procedure given below are described in BS3338, Part 1, “Sampling of ingot tin”, Part12, “Sampling of
29、solders” and Part14, “Sampling of white metal bearing alloy ingots”. Procedure Weigh2g of sample and transfer to a500ml flat-bottomed flask fitted with a joint of size24/29 (also known as B24) complying with the requirements of BS572, “Interchangeable conical ground glass joints”. Add20ml of sulphur
30、ic acid (sp. gr.1.84) andheat until the space inside the flask is free from fumes. Cool, add30ml of water,120ml of hydrochloric acid(sp. gr.1.161.18) and0.2g of hydrazine sulphate. Distil the solution in an all-glass apparatus (Figure 1) collecting the distillate in a250ml beaker cooled in running w
31、ater and containing50ml of water,5ml of nitric acid (sp. gr.1.42) and1ml of sulphuric acid (50per cent). Continue the distillation until the volume in the flask is reduced to8090ml and then remove the beaker containing the distillate and evaporate its contents until fumes of sulphur trioxide are evo
32、lved. Cool, transfer to a50ml volumetric flask and dilute to the mark. Transfer a suitable aliquot (Note1) to a100ml volumetric flask, add70ml of the ammonium molybdate-hydrazine sulphate solution, dilute to95ml and heat in a water bath for20minutes. Cool and dilute to the mark. Measure the optical
33、density using the conditions specified under “Apparatus”. 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 calculate the percentage of arsenic in the sample by reference to
34、 the appropriate calibration graph. 1) Water demineralized by ion exchange may be used if it is of equivalent quality.BS3338-9:1965 2 BSI 12-1999 Calibration Transfer0,0.5,1.0,2.0 and3.0ml aliquots of standard arsenic solution (1mlN 0.1mg ofarsenic)to a series of250ml beakers, add to each5ml ofwater
35、,1ml of hydrochloric acid (sp.gr.1.161.18),1ml of nitric acid (sp. gr.1.42) and0.5ml of sulphuric acid (50per cent). Evaporate to fuming, cool, add70ml of the ammonium molybdate-hydrazine sulphate solution and transfer to a100ml volumetric flask. Dilute to95ml and heat in a water bath at100 C for20m
36、inutes. Cool and dilute to the mark. Measure the optical density at830m4 and prepare a calibration graph by plotting optical densities against the weight of arsenic in the various aliquots, after deduction of the blank reading. NOTE 1For arsenic contents up to0.03per centtake25ml aliquots. For arsen
37、ic contents between0.03percent and0.08percent take10ml aliquots. For arsenic contents between0.08percent and0.15percent take5ml aliquots. For arsenic contents between0.15per cent and0.30percent take2.5ml aliquots.BS 3338-9:1965 BSI 12-1999 3 Figure 1 Distillation apparatusBS3338-9: 1965 BSI 389 Chis
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