1、BRITISH STANDARD BS3907-3: 1966 Method for The determination of copper in magnesium and magnesium alloys (Photometric method) Methods for the analysis of magnesium and magnesium alloysBS3907-3:1966 This BritishStandard, having been approved by the Non-ferrous Metals Industry Standards Committee and
2、endorsed by theChairman of theEngineeringDivisional Council,was published undertheauthority of the General Council on 17March1966 BSI12-1999 The following BSI references relate to the work on this standard: Committee references NFE/23 andNFE/23/4 Draft for comment D65/1419 ISBN 0 580 04401 7 Co-oper
3、ating 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 department and scientific and industri
4、al 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 BritishStandard: Aluminium Federation Institution of Mining and Metallurgy Association of Bronze and Brass Founders Institution o
5、f 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 Manufacturers Magne
6、sium 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 Stockists* Association* P
7、ost Office Copper Development Association Royal Institute of British Architects Crown Agents for Overseas Governments and Society of British Aerospace Companies Ltd. Administrations Society of Motor Manufacturers and Electric Cable Makers Confederation Traders Ltd.* High Conductivity Copper Associat
8、ion Tin Research Institute Institute of British Foundrymen Zinc Development Association Institute of Metals Individual manufacturer Institution of Mechanical Engineers (Automobile Division) Institute of Sheet Metal Engineering Individual analysts Ministry of Aviation Ministry of Technology, Laborato
9、ry of the Government Chemist Amendments issued since publication Amd. No. Date CommentsBS3907-3:1966 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 Calculation 2 Notes 2BS3907-
10、3:1966 ii BSI 12-1999 Foreword This standard makes reference to the following BritishStandard: BS1499, Sampling non-ferrous metals. This method for the photometric determination of copper in magnesium and magnesium alloys is the third of a series which will form a complete BritishStandard under the
11、collective title “Methods for the analysis of magnesium and magnesium alloys” each being published as a separate part. Other methods in the series are as follows: Part1: Aluminium in magnesium alloys (gravimetric method); Part2: Iron in magnesium and magnesium alloys (photometric 1:10-phenanthroline
12、 method); Part4: Manganese in magnesium and magnesium alloys (photometric periodate method); Part5: Manganese in magnesium and magnesium alloys (photometric periodate method) (low contents). The preparation of this series of methods has been authorized by the Non-ferrous Metals Industry Standards Co
13、mmittee as part of a general programme for the standardization of methods for the sampling and analysis of non-ferrous metals. 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 appreciated that they are prim
14、arily intended as “referee” methods to be used in cases of dispute. This method is substantially the same as the corresponding method approved by ISO/TC79 which will be published as ISO R . . . . . . 1) . A British Standard does not purport to include all the necessary provisions of a contract. User
15、s 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, pages1 and2 and a back cover. This standard
16、 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. 1) In course of preparation.BS3907-3:1966 BSI 12-1999 1 Introduction a) Principle. The sample is dissolved in hydrochloric acid. Citric acid is ad
17、ded followed by acetaldehyde and oxalyldihydrazide. The optical density is measured at about540nm. b) Range. The method is suitable for copper contents between0.002 and0.4per cent. c) Reproducibility. Experiments have been carried out independently by a number of analysts using this method. The degr
18、ee of reproducibility that can be expected is shown by the following analysis of the results obtained: d) Application. The method has not been tested on alloys containing zirconium, rare earths or thorium. Apparatus a) Class A volumetric glassware complying with the appropriate BritishStandards shal
19、l be used throughout. b) Any instrument suitable for measuring the optical density of the solution at a wavelength of540nm may be used with2 or4cm cells. Alternatively when a filter photometer of the balanced two-cell type is used, the following conditions have been found suitable: Mercury vapour la
20、mp. Ilford605 or equivalent filter. 2 or4cm cells. Solutions required All reagents shall be of the highest purity obtainable, and either distilled or demineralized water shall be used throughout. Solutions shall be freshly prepared and where necessary filtered. Standard copper (1mlN 1mg of copper).
21、Dissolve1.000g of high purity copper in10ml of nitric acid(50per cent) to which20ml of water has been added. Cover with a watchglass and, when dissolved, evaporate on a water bath until crystallization commences. Take up with water, transfer to a1litre volumetric flask, dilute to the mark and mix. A
22、lternatively: Dissolve3.928g of copper sulphate (CuSO 4 .5H 2 O) in water, transfer to a1litre volumetric flask, dilute to the mark and mix. Standard copper (1mlN 0.05mg of copper). Transfer50.0ml of standard copper solution(1mlN 1mg of copper) to a1litre volumetric flask, dilute to the mark and mix
23、. Standard copper (1mlN 0.005mg of copper). Transfer50.0ml of standard copper solution(1mlN 0.05mg of copper) to a500ml volumetric flask, dilute to the mark and mix. This solution should be freshly prepared. Standard copper (1mlN 0.0025mg of copper). Transfer50.0ml of standard copper solution(1mlN 0
24、.05mg of copper) to a1litre volumetric flask, dilute to the mark and mix. This solution should be freshly prepared. Acetaldehyde (50per cent v/v). Transfer500ml of acetaldehyde to a1litre volumetric flask and cool to approximately5 C. Slowly add cooled distilled water (at approximately5 C) and make
25、up to the mark, ensuring that the temperature does not exceed15 C. Store in a refrigerator. Citric acid (50per cent w/v). Dissolve500g of citric acid (C 6 H 8 O 7 .H 2 O) in water, dilute to1litre and mix. Nitric acid (50per cent v/v). Dilute50ml of nitric acid (sp.gr.1.42) to100ml and mix. Oxalyldi
26、hydrazide (0.25per cent w/v). Dissolve2.5g of oxalyldihydrazide in water, dilute to1litre and mix. Filter if necessary. Sampling Recommended methods of obtaining a suitable sample for the analytical procedure given below are described in BS1499, “Sampling non-ferrous metals”. Procedure Adjust the we
27、ight of sample and degree of dilution of the main solution as follows: Transfer the appropriate weight of sample to a250ml tall form beaker add20ml of water, then gradually add20ml of hydrochloric acid (sp.gr,1.16 to1.18). Cover the beaker and heat until solvent action ceases. Copper content Standar
28、d deviation per cent 0.002 0.03 0.3 per cent 0.0005 0.0009 0.0049 Copper content Weight of sample Volume of main solution Size of aliquot to be taken over up to and including per cent 0.002 0.02 0.08 0.2 per cent 0.02 0.08 0.2 0.4 g 2 0.001 1 0.001 1 0.001 1 0.001 ml 100 200 500 500 ml 10.0 10.0 10.
29、0 5.0+5.0 of water g of copper 440 1040 840 2040BS3907-3:1966 2 BSI 12-1999 Carry out simultaneously a blank determination following the same procedure and using the same amounts of reagents as with the sample. Add dropwise1ml of hydrogen peroxide(100vol), heat to boiling and evaporate until a pasty
30、 mass is obtained. Take up with about50ml of hot water, heat until solvent action ceases and allow to cool. Filter through a medium texture filter paper 2)collecting the filtrate in a volumetric flask of the size indicated in the table, rinsing the beaker and adding the washings to the main solution
31、. Cool, dilute to the mark and mix. Transfer the appropriate aliquot to a50ml volumetric flask, and add4ml of citric acid solution(50percent) to a2g sample or2ml of citric acid solution(50percent) for a1g sample. Mix, then add10ml of acetaldehyde solution(50percent). Add, by means of a pipette orbur
32、ette, sufficient ammonia solution (sp.gr.0.880.91) with stirring to bring the pH of the solution to approximately9.0(8.9 to9.2) (Note1). Cool to about20 C, then add10ml of oxalyldihydrazide solution(0.25percent). Dilute to the mark and mix. After45minutes, measure the optical density using the condi
33、tions specified under “Apparatus”. Calibration Transfer20ml of hydrochloric acid (sp.gr.1.161.18) to a250ml beaker add1ml of hydrogen peroxide(100vol) and evaporate the liquid almost completely. Add50ml of water, heat to boiling and continue boiling for about5minutes. Cool and transfer to a200ml vol
34、umetric flask, rinsing the beaker and adding the washings to the flask. Dilute to the mark and mix. Transfer10ml aliquots of this solution to each of a series of nine50ml volumetric flasks, then to six of these add: 0,2.0,4.0,6.0,8.0,10.0ml of standard copper solution(1mlN 0.0025mg of copper) and to
35、 the remaining three add: 6.0,8.0,10.0ml of standard copper solution(1mlN 0.005mg of copper). Add2ml of citric acid solution(50percent) and continue from paragraph7 of the procedure. Measure the optical density using the conditions specified under “Apparatus” and prepare a calibration graph by plott
36、ing the optical density against the equivalent percentage of copper. Calculation Notes 1. A preliminary test should be carried out to determine the quantity of ammonia solution to be added to the appropriate aliquot and this test solution should then be discarded. The amount of ammonia solution adde
37、d is of the order of4 to6ml. 2) Whatman No.40 is suitable. Where A = weight(mg) of copper corresponding to the aliquot taken, R = the ratio of the volume of the main solution to the volume of the aliquot taken, W = weight(g) of sample taken. Copper per cent AR W - 1001000 - =blankBS3907-3: 1966 BSI
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