BS 1728-8-1957 Methods for the analysis of aluminium and aluminium alloys - Determination of iron (absorptiometric 1 10-phenanthroline method)《铝与铝合金的分析方法 第8部分 铁的测定(1 10菲咯啉吸收测量法)》.pdf

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1、BRITISH STANDARD BS 1728-8: 1957 Method for The determination of iron in aluminium and aluminium alloys (Absorptiometric 1:10-phenanthroline method) Methods for the analysis of aluminium and aluminium alloysBS1728-8:1957 This British Standard, having been approved by the Non-ferrousMetals Industry S

2、tandards Committee and endorsed by the Chairman of theEngineering Divisional Council, was published undertheauthority of the GeneralCouncil on 12 September 1957 BSI 12-1999 The following BSI references relate to the work on this standard: Committee reference NFE/-/3 Draft for comment CW(NFE) 8553 IS

3、BN 0 580 01529 7 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: Admiralty* Aluminium Develo

4、pment Association* Aluminium Industry Council* Association of Bronze and Brass Founders Association of Consulting Engineers, Incorporated Association of Non-ferrous Metal Stockists Brass and Copper Tube Association Brass Wire Association British Bronze and Brass Ingot Manufacturers Association Briti

5、sh Electrical and Allied Manufacturers Association British Non-ferrous Metals Research Association* Cable Makers Association Cold Rolled Brass and Copper Association Copper Development Association Crown Agents for Oversea Governments and Administrations General Post Office High Commission of India H

6、igh Conductivity Copper Association Institute of British Foundrymen Institute of Metals Institution of Mechanical Engineers (Automobile Division) Institution of Mining and Metallurgy Institution of Structural Engineers Lead Sheet and Pipe Manufacturers Federation Light Metal Founders Association* Lo

7、ndon Metal Exchange Manufactured Copper Association Ministry of Supply* National Brassfoundry Association Nickel Silver Association Royal Institute of British Architects Society of British Aircraft Constructors Society of Motor Manufacturers and Traders Ltd. Tin Research Institute Zinc Development A

8、ssociation Individual manufacturers 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 sub-committee entrusted with the preparation of this British Standard: ALAR (Association

9、 of Light Alloy Refiners) Department of the Government Chemist Individual analysts Amendments issued since publication Amd. No. Date CommentsBS1728-8:1957 BSI 12-1999 i Contents Page Co-operating organizations Inside front cover Foreword ii Introduction 1 Special apparatus 1 Solutions required 1 Sam

10、pling 1 Procedure 1BS1728-8:1957 ii BSI 12-1999 Foreword This standard makes reference to the following British Standard: BS 1499, Sampling non-ferrous metals. This method for the determination of iron is the eighth of a series of methods for the analysis of aluminium and aluminium alloys, and is in

11、tended for use with alloys containing smaller percentages of iron as an alternative to the volumetric method given in Part6. This series will form a complete British Standard, each method being published as a separate part. Other methods in the series are as follows: Part 1: Copper; Part 2: Magnesiu

12、m; Part 3: Zinc (mercuric potassium thiocyanate method); Part 4: Zinc (polarographic method); Part 5: Copper (absorptiometric method); Part 6: Iron (volumetric titanous chloride method); Part 7: Zinc (zinc oxide method); Part 9: Manganese (volumetric arsenite/nitrite method); Part 10: Manganese (abs

13、orptiometric method). The preparation of this series of methods has been authorized by the Non-ferrous metals Industry Standards Committee as part of a general programme of the standardization of methods for the analysis of non-ferrous metals. These methods have been found to give reliable and repro

14、ducible results, and while in some instances the methods may appear to be lengthy, it should be realized that they are put forward as “referee” 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 Standard

15、s 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, an inside back cover and a back cover. This stan

16、dard 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.BS1728-8:1957 BSI 12-1999 1 Introduction a) Principle. The alloy is treated with sodium hydroxide solution, acidified with hydrochloric acid, a

17、nd undissolved copper is filtered off. After diluting to volume, an aliquot is taken and the ferrous 1:10-phenanthroline colour is developed by addition of a mixed reagent containing reducing agent, buffer and 1:10-phenanthroline. The light absorption of the orange-red solution is measured at about5

18、10m4. b) Range. The method is suitable for iron contents between0.05and0.6per cent. c) Reproducibility. Experiments have been carried out by a number of independent analysts using the method recommended in this standard. The degree of reproducibility that can be expected is shown by the following an

19、alysis of the results obtained: Special apparatus a) A suitable instrument for measuring the light absorption of the solution at a wavelength of about510m4. b) Any volumetric glassware used shall be of Class A accuracy as defined in the appropriate British Standards or, where no British Standard exi

20、sts, as described in the National Physical Laboratory publication, “Volumetric tests on volumetric glassware”. Solutions required All reagents used in making these solutions shall be of recognized analytical quality and distilled water shall be used throughout. Hydrochloric acid (sp. gr.1.16). Sampl

21、ing Recommended methods for obtaining a suitable sample for the analytical procedure given below are described in BS1499, “Sampling non-ferrous metals”. Procedure Treat0.1g of sample (0.5g for iron less than0.1per cent) in a200-ml beaker with10ml ofthe sodium hydroxide solution. Carry out simultaneo

22、usly a blank determination following the same procedure and using the same amounts of reagents as in the sample. When the attack is complete, wash down and boil gently for23minutes. For high silicon alloys (silicon greater than4per cent) stand the beaker on the edge of the hotplate for20minutes at a

23、 temperature just below boiling point, to oxidize the silicon, before boiling (see Note1). Wash down, dilute to approximately25ml, add15ml of hydrochloric acid, mix and boil gently for10minutes. Cool, filter through an open-textured filter paper (Whatman No.4 is suitable) into a200-mlgraduated flask

24、, wash with water, dilute to volume and mix well. Alloy Iron found (mean) Standard deviation per cent Pure aluminium 0.051 0.004 5 Special alloy 0.494 0.013 0 LM.6 to BS 1490 0.299 0.010 2 LM.10 to BS 1490 0.175 0.007 8 LM.5 to BS 1490 0.402 0.009 0 LM.4 to BS 1490 0.557 0.011 6 Mixed reagent Hydrox

25、yammonium chloride (hydroxylamine hydrochloride) (1 per cent w/v aqueous). 1:10-Phenanthroline monohydrate (0.15 per cent w/v aqueous). Warm to dissolve. Acetate buffer. Dissolve 272 g of sodium acetate (CH 3 COONa.3H 2 O) in 500 ml of water, filter, add240ml of acetic acid (glacial) and dilute to 1

26、 litre. Prepare the mixed reagent by mixing the above three solutions in the proportions 1:1:3. Sodium hydroxide (20 per cent w/v aqueous). Standard iron. Dissolve a weighed quantity of high purity iron of known iron content in 20 ml of sulphuric acid(1:3), the quantity weight being such as will giv

27、e 0.2000 g of iron. Cool and dilute to 1 litre. Dilute this solution 20-fold to give a solution of which 1 ml N 0.01 mg iron.BS1728-8:1957 2 BSI 12-1999 Pipette a25-mlaliquot (see Note2) into a100-mlgraduated flask, add25ml of mixed reagent, dilute to100ml and mix well. Treat a similar aliquot of th

28、e blank solution in the same way. Measure the light absorption on a suitable instrument (e.g.Spekker absorptiometer using the tungsten filament lamp and Ilford603 and Chance ON13 or ON20filters with4-cmcells). Calibration of instrument. Calibrate the instrument as follows: transfer accurately measur

29、ed aliquots of standard iron solution (1 mlN 0.01mg iron) up to15ml into a series of100-mlgraduated flasks. Dilute, add25ml of mixed reagent, dilute to volume, and measure the light absorptions as described for the samples. Carry out a blank determination on25ml of the mixed reagent diluted to100ml

30、and subtract the light absorption from the standards. A plot of light absorption against the nominal iron contents gives a straight line. NOTE 1Certain unmodified silicon alloys may require a longer period of heating for complete oxidation of silicon. NOTE 2For pure metal (less than0.1per cent Fe) w

31、here0.5g sample is used pipette50ml.BS1728-8:1957 BSI 12-1999 British Standards The following are available on application: YEARBOOK Including subject index and numerical list of British Standards SECTIONAL LISTS. Gratis Acoustics Aircraft materials and components Building materials and components C

32、hemical engineering Chemicals, fats, oils, scientific apparatus, etc. Cinematography and photography Coal, coke and colliery requisites Codes of Practice Consumer goods Documentation, including Universal Decimal Classification Drawing practice Electrical engineering Farming, dairying and allied inte

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34、rous metals Packaging and containers Paints, varnishes, paint materials and colours for paints Personal safety equipment Petroleum industry Plastics Printing, paper and stationery Road engineering Rubber Shipbuilding Textiles and clothing WeldingBS 1728-8: 1957 BSI 389 Chiswick High Road London W4 4

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