BS 1728-15-1966 Methods for the analysis of aluminium and aluminium alloys - Determination of nickel (photometric method)《铝与铝合金的分析方法 第15部分 镍的测定(光度测量法)》.pdf

1、BRITISH STANDARD BS1728-15: 1966 Method for Thedetermination of nickel in aluminium and aluminium alloys (Photometric method) Methods for the analysis of aluminium and aluminium alloysBS1728-15:1966 This BritishStandard, having been approved by the Non-ferrous Metals Industry Standards Committee and

2、 endorsed by the Chairman of theEngineering Divisional Council, was published under theauthority of the General Council on 31May1966 BSI12-1999 The following BSI references relate to the work on this standard: Committee reference NFE/-/3 Draft for comment D65/8564 ISBN 0 580 01599 8 Co-operating org

3、anizations 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: Aluminium Federation* Association of Bronze and Brass Founders

4、 Association of Consulting Engineers Board of Trade British Bronze and Brass Ingot Manufacturers Association British Electrical and Allied Manufacturers Association British Lead Manufacturers Association British Non-ferrous Metals Federation British Non-ferrous Metals Research Association* Copper De

5、velopment Association Crown Agents for Oversea Governments and Administrations Electric Cable Makers Confederation High Conductivity Copper Association Institute of British Foundrymen Institute of Metals Institution of Mechanical Engineers (Automobile Division) Institution of Mining and Metallurgy I

6、nstitution of Production Engineers Institution of Structural Engineers Lead Development Association Light Metal Founders Association* London Metal Exchange Magnesium Industry Council Ministry of Defence, Army Department* Ministry of Defence, Navy Department* National Brassfoundry Association Non-fer

7、rous Metal Stockists Post Office Royal Institute of British Architects Society of British Aerospace Companies Ltd. Society of Motor Manufacturers and Traders Ltd. Tin Research Institute Zinc Development Association Individual manufacturers The Government departments and scientific and industrial org

8、anizations marked with an asterisk in the above list, together with the following, were directly represented on the sub-committee entrusted with the preparation of this BritishStandard: Association of Light Alloy Refiners and Smelters Ltd. Ministry of Technology Laboratory of the Government Chemist

9、Individual analysts Amendments issued since publication Amd. No. Date CommentsBS1728-15:1966 BSI 12-1999 i Contents Page Co-operating organizations Inside front cover Foreword ii Introduction 1 Apparatus 1 Solutions required 1 Sampling 2 Procedure 2 Calibration 2 Calculation 2 Notes 2BS1728-15:1966

10、ii BSI 12-1999 Foreword This standard makes reference to the following BritishStandards: BS1470-77, Wrought aluminium and aluminium alloys. BS1499, Sampling non-ferrous metals. This method for the determination of nickel is the fifteenth of a series which will form a complete BritishStandard under t

11、he collective title “Methods for the analysis of aluminium and aluminium alloys”, each being published as a separate part. Other methods in the series are as follows: Part1: Copper; Part2: Magnesium; Part3: Zinc (mercuric potassium thiocyanate method); Part4: Zinc (polarographic method); Part5: Copp

12、er (absorptiometric method); Part6: Iron (volumetric: titanous chloride method); Part7: Zinc (zinc oxide method); Part8: Iron (absorptiometric1:10 phenanthroline method); Part9: Manganese (volumetric arsenite/nitrite method); Part10: Manganese (absorptiometric method); Part11: Silicon (perchloric ac

13、id method); Part12: Silicon (absorptiometric molybdenum blue method); Part13: Titanium (absorptiometric chromotropic acid method); Part14: Nickel (gravimetric method). The preparation of this series of methods has been authorized by the Non-ferrous Metals Industry Standards Committee as part of a ge

14、neral 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 primarily intended as “refe

15、ree” methods to be used in cases of dispute. 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 obligatio

16、ns. Summary of pages This document comprises a front cover, an inside front cover, pagesi andii, 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.BS1728-

17、15:1966 BSI 12-1999 1 Introduction a) Principle. The alloy is dissolved in sodium hydroxide solution and the insoluble material containing the nickel dissolved in acid. The dimethylglyoxime complex is formed in ammoniacal citrate solution at a pH of8.6 and the complex is extracted with chloroform. T

18、he nickel complex is then extracted from the chloroform with dilute hydrochloric acid and, after addition of bromine water, the solution is made ammoniacal and dimethylglyoxime added. The optical density of this solution is then measured at about445m. b) Range. The method is recommended for nickel c

19、ontents between0.01 and0.3percent. c) Reproducibility. Experiments have been carried out independently by a number of analysts using this method. The degree of reproducibility that can be expected is shown by the following results obtained: Apparatus a) Class A volumetric glassware complying with th

20、e relevant BritishStandards shall be used throughout. b) Any instrument suitable for measuring the optical density of the solution at a wavelength of445m may be used together with2cm cells. Alternatively, if a filter photometer with two balanced photo-cells is used, the following conditions have bee

21、n found suitable: Mercury vapour lamp; Ilford601 or equivalent filter; 2cm cells. c) pH meter. Solutions required All reagents shall be of the highest purity obtainable and distilled 1)water shall be used throughout. Standard nickel (1.0mlN 0.02mg of nickel). Dissolve13.460g of ammonium nickel sulph

22、ate (NH 4 ) 2 SO 4 NiSO 4 .6H 2 O in water and dilute to1litre. Transfer10ml of this solution to a1litre volumetric flask, dilute to the mark and mix. Bromine water (saturated). To100ml of water, add5ml of bromine, shake and allow to stand until saturated (preferably overnight). Citric acid (30perce

23、ntw/v). Dissolve300g of citric acid (C 6 H 8 O 7 H 2 O) in water, dilute to1litre and mix. Dimethylglyoxime (1percentw/v alcoholic). Dissolve10g of dimethylglyoxime in nearly1litre of warm ethanol. Cool, dilute to1litre with ethanol and mix. Hydrochloric acid (5percentv/v). Dilute50ml of hydrochlori

24、c acid (sp. gr.1.161.18) to1litre and mix. Hydrochloric-nitric acid. To100ml of water add75ml of hydrochloric acid (sp. gr.1.161.18), mix, add25ml of nitric acid (sp. gr.1.42) and mix. This reagent should be freshly prepared. Sodium hydroxide (20percentw/v). Dissolve200g of sodium hydroxide in water

25、, dilute to1litre and mix. Sodium hydroxide (0.2percentw/v). Dilute10ml of sodium hydroxide solution(20percent) to1litre. Sulphurous acid. Pass sulphur dioxide gas into1litre of water until a saturated solution is obtained. Thiourea (10percentw/v). Dissolve100g of thiourea in water and dilute to1lit

26、re. Nickel content Standard deviation percent 0.025 0.1 0.25 0.0015 0.003 0.006 1) Water demineralized by ion exchange may be used if it is of equivalent quality.BS1728-15:1966 2 BSI 12-1999 Sampling Recommended methods for obtaining a suitable sample for the analytical procedure given below are des

27、cribed in BS1499, “Sampling non-ferrous metals”. Procedure Adjust the weight of sample and quantities to be used as follows: Weigh the appropriate weight of sample and transfer to a400ml squat beaker. Add20ml of sodium hydroxide solution(20percent) (Note1). Simultaneously carry a blank determination

28、 through the procedure using the same quantities of reagents. When the reaction is complete, wash down the cover and side of the beaker, dilute to about150ml and boil for23minutes. Filter through a paper pulp pad and wash the filter six times with hot sodium hydroxide solution(0.2percent). Discard t

29、he filtrate. Extract the insoluble residue into the original beaker with three10ml portions of hot hydrochloric-nitric acid, wash well with hot water and evaporate to about15ml. (For nickel contents greater than0.05percent, dilute to25.0 or50.0ml (see table above) and take a10ml aliquot.) Add2ml of

30、sulphurous acid,10ml of citric acid(30percent) and10ml of thiourea solution(10percent). Then add ammonia solution (sp. gr.0.880.91) dropwise until the pH of the solution is8.6 0.1 (Note2). Then add2ml of dimethylglyoxime solution(1percent alcoholic). Extract in a100ml separating funnel with10ml of c

31、hloroform, shaking for30seconds, allow the layers to separate and transfer the lower organic layer to a second separating funnel. Repeat the extraction with5ml of chloroform, again shaking for30seconds. After separation of the layers, combine the two organic extracts and discard the aqueous layer. E

32、xtract the combined chloroform solutions twice with hydrochloric acid(5percent) each time using10ml and shaking for one minute. Combine the two acid extracts in a50ml volumetric flask. Add2ml of bromine water (saturated), allow to stand for15minutes then add ammonia solution (sp. gr.0.880.91) until

33、the solution is decolorized and add2ml excess. Cool to below30 C, add2ml of dimethylglyoxime solution(1percent alcoholic) and dilute to volume. Allow the solution to stand for10minutes then measure the optical density within the next30minutes using the conditions specified under “Apparatus”. Calibra

34、tion Into a series of150ml squat beakers transfer varying known amounts of standard nickel solution(1mlN 0.02mg of nickel) to cover the range00.12mg of nickel. Add to each2ml of sulphurous acid,10ml of citric acid solution(30percent) and10ml of thiourea solution(10percent). Then add ammonia solution

35、 (sp. gr.0.880.91) dropwise until the pH of the solution is8.6 0.1. Then add2ml of dimethylglyoxime solution(1percent alcoholic) and continue from Paragraph6 of the procedure. Deduct the blank on the reagents from the gross optical densities and prepare a calibration graph by plotting the net values

36、 against the nominal nickel contents of the solution. Calculation Convert the optical density reading for the test sample corrected for blank to percentage nickel by means of the calibration graph. Notes 1. For high silicon alloys (silicon over4percent) use40ml of sodium hydroxide solution(20percent

37、). 2. Where the copper content is less than1percent the pH is less critical and adjustment can be made by making the solution slightly ammoniacal and then adding a few drops in excess. Ni content (percent) Weight of sample(g) Dilute to(ml) 0.010.03 0.40 0.030.05 0.20 0.050.15 0.20 25.0 0.150.30 0.20

38、 50.0 Aliquot(ml) Use whole of sample solution 10.0 10.0blankBS1728-15: 1966 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 the internationa

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