1、BRITISH STANDARD BS3338-20: 1970 Method for The determination of nickel in capping metal (Photometric method) Methods for the sampling and analysis of tin and tin alloysBS3338-20:1970 This BritishStandard, having been approved by the Non-ferrous Metals IndustryStandards Committee, was published unde
2、rthe authorityof the Executive Board on 30 October 1970 BSI 12-1999 The following BSI references relate to the work on this standard: Committee references NFE/27, NFE/27/1 Draft for comment68/21414 ISBN 580 06234 1 Co-operating organizations The Non-ferrous Metals Industry Standards Committee, under
3、 whose supervision this BritishStandard was prepared, consists of representatives from the following Government departments and scientific and industrial organizations: Aluminium Federation Institution of Mining and Metallurgy Association of Bronze and Brass Founders Institution of Production Engine
4、ers Association of Consulting Engineers Institution of Structural Engineers Board of Trade Lead Development Association British Bronze and Brass Ingot Light Metal Founders Association Manufacturers Association London Metal Enchange* British Lead Manufacturers Association Magnesium Industry Council B
5、ritish Non-ferrous Metals Federation Ministry of Defence, Army Department* British Non-ferrous Metals Federations Ministry of Defence, Navy Department* High Conductivity Copper Group National Brassfoundry Association British Non-ferrous Metals Research Non-ferrous Metal Stockists Association* Post O
6、ffice* Copper Development Association Royal Institute of British Architects Crown Agents for Oversea Governments and Society of Motor Manufacturers and Administrations TradersLtd.* Electric Cable Makers Confederation* Tin Research Institute Institution of British Foundrymen Zinc Development Associat
7、ion Institute of Metals Individual manufacturers Institution of Mechanical Engineers (Automobile Division) The Government departments and scientific and industrial organizations marked with an asterisk in the above list, together with the following, were directly represented on the committee entrust
8、ed with the preparation of this BritishStandard: British Electrical and Allied Manufacturers London Transport Executive Association National Coal Board British Railways Board Solder Makers Association British Tin Box Manufacturers Federation Tinplate Conference(1925) Electronic Engineering Associati
9、on Tin Producers Association Gas Council White Metal Bearing Manufacturers Institution of Gas Engineers Individual firms Amendments issued since publication Amd. No. Date CommentsBS3338-20:1970 BSI 12-1999 i Contents Page Co-operating organizations Inside front cover Foreword ii Introduction 1 Appar
10、atus 1 Solutions required 1 Sampling 1 Procedure 1 Calibration 2 Notes 2BS3338-20:1970 ii BSI 12-1999 Foreword This standard makes reference to the following BritishStandards: BS3338, Methods for the sampling and analysis of tin and tin alloys Part14: Sampling of white metal bearing alloy ingots. BS
11、3978, Water for laboratory use. This method for the photometric determination of nickel in capping metal is the twentieth of a series of methods which will form a complete BritishStandard under the collective title “Methods for the sampling and analysis of tin and tin alloys”, each method being publ
12、ished 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 metals. Other methods in the series are as fol
13、lows: 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 tinlead solders; Part 5: Determination of lead in ingot tin and tinantimony solders; Part 6: Determination of copper in hig
14、h purity ingot tin; Part 7: Determination of silver in solders; Part 8: Determination of bismuth in ingot tin, tinlead 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, tinlead solders
15、 and white 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 beari
16、ng alloys; Part 16: Determination of tin in white metal bearing alloys; Part 17: Determination of cadmium in solders and white metal bearing alloys; Part 18: Determination of aluminium in solders and white metal bearing alloys; Part 19: Determination of zinc in solders and white metal bearing alloys
17、. The complete BritishStandard methods will be found suitable for the grades of metals covered by BS3252, “Ingot tin”, BS219, “Soft solders” BS3332, “White metal bearing alloy ingots” and BS643 “White metal ingots for capping steel wire ropes”. In the methods for determining impurities, sample weigh
18、ts and aliquots have been chosen to cover the range of impurity content usually found in commercial tin ingots, solders, white metal bearing alloy ingots and capping metal. For amounts of impurity outside this range, sample weights or aliquots should be adjusted accordingly. The methods have been fo
19、und 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.BS3338-20:1970 BSI 12-1999 iii A British Standard does not purport to include all the necessa
20、ry 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 to iv, pages1and
21、2 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 blankBS3338-20:1970 BSI 12-1999 1 Introduction a) Principle. Nickel is determined photometrically with dimethyl
22、glyoxime after removal of interfering elements. b) Range. From0.001% up to0.01% of nickel. c) Reproducibility. 10% of nickel present. d) Application. The method is applicable to tin and tin alloys containing up to0.25% of copper. Apparatus a) Any volumetric glassware used shall be of Class A accurac
23、y 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 wave length of445nm may be u
24、sed together with a4cm cell. Alternatively when a filter photometer of the balanced two-cell type is used the following conditions have been found suitable: Mercury vapour lamp. Ilford601 with Calorex H503, or equivalent filters. 4cm cell. Solutions required All reagents shall be of the highest puri
25、ty obtainable and distilled or demineralized water complying with BS3978 1)shall be used throughout. Solutions shall be freshly prepared and where necessary filtered. Standard nickel(1ml=0.5mg of nickel). Dissolve0.5g of nickel in40ml of nitric acid(sp.gr.1.42). Cool, transfer to a1litre volumetric
26、flask, dilute to the mark and mix. Standard nickel(1ml=0.025mg of nickel). Transfer25ml of standard nickel solution(1ml=0.5mg of nickel) to a500ml volumetric flask, dilute to the mark and mix. Ammonia(50% v/v). Dilute500ml of ammonia solution(sp.gr.0.91) to1litre and mix. Bromine-hydrobromic acid. T
27、o90ml of hydrobromic acid(sp.gr.1.461.49) add carefully10ml of bromine. Bromine water(saturated). To100ml of water add5ml of bromine, shake and allow to stand until saturated. Citric acid(40% w/v). Dissolve400g of citric acid(C 6 H 8 O 7 .H 2 O) in water, dilute to1litre and mix. Dimethylglyoxime (0
28、.1% w/v ammoniacal). Dissolve1g of dimethylglyoxime in ammonia solution(50%), dilute to1litre with the ammonia solution and mix. Nitric acid(40% v/v). Dilute400ml of nitric acid(sp.gr.1.42) to1litre and mix. Sampling Recommended methods of obtaining a suitable sample for the analytical procedure giv
29、en below are described in BS3338-14, “Sampling of white metal bearing alloy ingots”. Procedure Weigh1g of sample and transfer to a150ml beaker. Add20ml of the bromine-hydrobromic acid mixture and heat gently until solvent action ceases. Add10ml of hydrochloric acid(sp.gr.1.161.18), evaporate to dryn
30、ess, and bake until no more fumes are evolved. Add10ml of nitric acid(40%) boil to remove brown fumes and evaporate to dryness.(Note1.) Add5ml of nitric acid(40%),20ml of citric acid(40%) and15ml of water, and warm to dissolve the residue of lead nitrate. Add ammonia solution(50%) until a small perm
31、anent precipitate is formed. Note2.) Cool, add10ml of bromine water,(saturated) add20ml of dimethylglyoxime solution(0.1% ammoniacal) transfer to a100ml volumetric flask and dilute to the mark. Allow to stand for10minutes and measure the optical density against water within30minutes, using the condi
32、tions specified under “Apparatus”. Carry out simultaneously a blank determination on the reagents, following the same procedure without the sample and using the same quantities of reagents. Deduct the blank reading and calculate the percentage nickel in the sample by reference to the calibration gra
33、ph. 1) BS3978, “Water for laboratory use”.BS3338-20:1970 2 BSI 12-1999 Calibration Transfer0,1.0,2.0,3.0 and4.0ml aliquots of standard nickel solution(1ml=0.025mg of nickel) to a series of150ml beakers and add to each1.25g of lead nitrate. Add to each5ml of nitric acid(40%)20ml of citric acid(40%) a
34、nd15ml of water and warm to dissolve the lead nitrate. Continue from paragraph5 of the procedure. Measure the optical density using the conditions given under “Apparatus” and prepare a calibration graph by plotting the optical density against the weight of nickel in the various aliquots after deduct
35、ion of the blank reading. Notes NOTE 1If the nitric acid solution is cloudy, evaporate to dryness, add a further5ml of the bromine-hydrobromic acid mixture, and5ml of hydrochloric acid(sp.gr.1.161.18) and repeat the evaporation. Finally add10ml of nitric acid(40%) boil to remove brown fumes and evap
36、orate to dryness. NOTE 2The solution at this stage should still be acid.blankBS3338-20: 1970 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 Europe and at
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