BS 1728-10-1957 Methods for the analysis of aluminium and aluminium alloys - Determination of manganese (absorptiometric method)《铝与铝合金的分析方法 第10部分 锰的测定(吸收测量法)》.pdf

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1、BRITISH STANDARD BS1728-10: 1957 Method for The determination of manganese in aluminium and aluminium alloys (Absorptiometric method) Methods for the analysis of aluminiumandaluminium alloysBS1728-10:1957 This BritishStandard, having been approved by the Non-ferrous Metals Industry Standards Committ

2、ee and endorsed by theChairman of the EngineeringDivisional Council, was published under theauthorityof the GeneralCouncil on 12September1957 BSI 12-1999 The following BSI references relate to the work on this standard: Committee referenceNFE/-/3 Draft for commentCW(NFE)8555 ISBN 0 580 01549 1 Co-op

3、erating 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 scientific and indu

4、strial 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 BritishStandard: Admiralty* High Conductivity Copper Association Aluminium Development Association* Institute of British

5、Foundrymen Aluminium Industry Council* Institute of Metals Association of Bronze and Brass Founders Institution of Mechanical Engineers Association of Consulting Engineers, (Automobile Division) Incorporated Institution of Mining and Metallurgy Association of Non-ferrous Metal Stockists Institution

6、of Structural Engineers Brass and Copper Tube Association Lead Sheet and Pipe Manufacturers Brass Wire Association Federation British Bronze and Brass Ingot Manufacturers Light Metal Founders Association* Association London Metal Exchange British Electrical and Allied Manufacturers Manufactured Copp

7、er Association Association Ministry of Supply* British Non-ferrous Metals Research National Brassfoundry Association Association* Nickel Silver Association Cable Makers Association Royal Institute of British Architects Cold Rolled Brass and Copper Association Society of British Aircraft Constructors

8、 Copper Development Association Society of Motor Manufacturers and Crown Agents for Oversea Governments and Traders Ltd. Administrations Tin Research Institute General Post Office Zinc Development Association High Commission of India Individual manufacturers ALAR (Association of Light Alloy Refiners

9、) Individual analysts Department of the Government Chemist Amendments issued since publication Amd. No. Date CommentsBS1728-10:1957 BSI 12-1999 i Contents Page Co-operating organizations Inside front cover Foreword ii Introduction 1 Special apparatus 1 Solutions required 1 Sampling 1 Procedure 1BS17

10、28-10:1957 ii BSI 12-1999 Foreword This standard makes reference to the following BritishStandard: BS1499, Sampling non-ferrous metals. This method for the determination of manganese is the tenth of a series of methods for the analysis of aluminium and aluminium alloys. It is intended mainly for use

11、 with alloys containing smaller percentages of manganese than those dealt with in the volumetric method given in Part9. This series will form a complete BritishStandard, each method being published as a separate part. Other methods in the series are as follows: Part 1: Copper; Part 2: Magnesium; Par

12、t 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 8: Iron (absorptiometric 1:10-phenanthroline method); Part 9: Manganese (volumet

13、ric arsenite nitrite 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 a

14、nd reproducible 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

15、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 has been upd

16、ated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.BS1728-10:1957 BSI 12-1999 1 Introduction a) Principle. The alloy is dissolved by means of sodium hydroxide solution followed by an acid mixture. The manganese

17、is oxidized to permanganate by boiling with potassium periodate. The light absorption of the solution is determined at about525m4. The permanganate is reduced by nitrite and the light absorption of the reduced solution is deducted. b) Range. The method is recommended for manganese contents between0.

18、01 and0.5percent, and is applicable to alloys containing up to1.0percent chromium. 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 ana

19、lysis of the results obtained: Special apparatus a) A suitable instrument for measuring the light absorption of the solution at a wavelength of about525m4. Suitable instruments and conditions are: i) A Spekker absorptiometer with tungsten lamp and Ilford604 filters, or mercury vapour lamp and Ilford

20、605 filters, heat absorbing filters and4-cm or2-cm cells according to the manganese content. ii) Unicam S.P.500 or S.P.600 spectrophotometer with4-cm to1-cm cells according to the manganese content, using a wavelength of525m4. b) Any volumetric glassware used shall be of ClassA accuracy as defined i

21、n the appropriate BritishStandards or, where no BritishStandard exists, 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 wat

22、er shall be used throughout. Sodium hydroxide (15percentw/v aqueous). Sampling Recommended methods for obtaining a suitable sample for the analytical procedure given below are described in BS1499, “Sampling non-ferrous metals”. Procedure Treat the sample in a250-ml beaker with25ml of the sodium hydr

23、oxide solution. Cover with a watchglass and, when the reaction slows down, boil gently for not more than5minutes. If any manganese dioxide forms this should be reduced by dropwise addition of the sodium nitrite solution, avoiding any unnecessary excess. Wash down the watchglass with not more than5ml

24、 of water. Cool slightly and add25ml of the acid mixture while shaking vigorously. Boil for at least3minutes to expel nitrous fumes, the watchglass being raised on a glass hook. Add3ml of the potassium periodate solution, remove and rinse the glass hook and cover with the watchglass again. Manganese

25、 found (mean) percent Standard deviation 0.0096 0.0013 0.064 0.0029 0.346 0.0101 0.492 0.0106 1.244 0.0371 Acid mixture Nitric acid (sp.gr.1.42) 325ml Phosphoric acid (sp.gr.1.75) 25ml Water 150ml Potassium periodate. Potassium periodate. Cautiously add25ml of sulphuric acid (sp.gr.1.84) to50ml of w

26、ater. Cool and dilute to100ml. Dissolve7.5g of potassium periodate in this solution. Standard manganese. A) Dissolve a weighed quantity of electrolytic manganese of known manganese content in5ml of nitric acid(1:1), the quantity weighed being such as will give0.2500g of manganese. Cool and dilute to

27、 one litre. 1ml N 0.25mg manganese. B) Dilute part of solutionA) so that1ml N 0.05mg manganese. Sodium nitrite (2percentw/v aqueous). Manganese content per cent Weight of sample g 0.01 to0.1 0.500 0.1 to0.5 0.250BS1728-10:1957 2 BSI 12-1999 Boil gently until the colour starts to develop and continue

28、 boiling for a further3minutes approximately; keep hot (e.g.on edge of hot-plate) but not boiling for a further35minutes, add about25ml of cold water (to prevent salts from crystallizing out during cooling) cool, transfer to a100-ml volumetric flask and dilute to volume. Measure the light absorption

29、 of the solution in the appropriate cell. Decolorize the liquid remaining in the flask (or the solution in the cell) by dropwise addition of sodium nitrite solution and mixing. Measure the light absorption of the decolorized solution under the same conditions and deduct the reading from that of the

30、coloured solution. Calibration of instrument. To establish calibration graphs, transfer suitable aliquots (not more than15ml) of the standard manganese solutionsB) orA) according to the manganese content of the sample into a series of250-ml beakers. Add25ml of the acid mixture and then25ml of the so

31、dium hydroxide solution. Add3ml of the periodate solution,etc., and continue as detailed in the procedure, but omit the addition of25ml of cold water.blankBS1728-10: 1957 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for prep

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