BS 3907-5-1966 Methods for the analysis of magnesium and magnesium alloys - Determination of manganese in magnesium and magnesium alloys (photometric-periodate method) (low content.pdf

1、BRITISH STANDARD BS3907-5: 1966 Method for The determination of manganese in magnesium and magnesium alloys (Photometric periodate method) (Low contents) Methods for the analysis of magnesium and magnesium alloysBS3907-5:1966 This BritishStandard, having been approved by the Non-ferrous Metals Indus

2、try Standards Committee and endorsed by the Chairman oftheEngineering Divisional Council, was published undertheauthority of the GeneralCouncil on 17March1966 BSI12-1999 The following BSI references relate to the work on this standard: Committee references NFE/23 and NFE/23/4 Draft for comment D65/1

3、421 ISBN 0 580 04421 1 Co-operating 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: Aluminium Federation In

4、stitution of Mining and Metallurgy Association of Bronze and Brass Founders Institution of 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 Associ

5、ation Association London Metal Exchange British Electrical and Allied Manufacturers Magnesium Industry Council* Association Ministry of Defence, Army Department* British Lead Manufacturers Association Ministry of Defence, Navy Department British Non-ferrous Metals Federation National Brassfoundry As

6、sociation British Non-ferrous Metals Research Non-ferrous Metal Stockists* Association* Post 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 Manufacturer

7、s and Electric Cable Makers Confederation TradersLtd.* High Conductivity Copper Association Tin Research Institute Institute of British Foundrymen Zinc Development Association Institute of Metals Individual manufacturer Institution of Mechanical Engineers (Automobile Division) The Government departm

8、ent and scientific and industrial 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: Institute of Sheet Metal Engineering Individual analysts Ministry of Aviation Min

9、istry of Technology, Laboratory of the Government Chemist Amendments issued since publication Amd. No. Date CommentsBS3907-5:1966 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

10、 Calculation 2BS3907-5:1966 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 manganese (low contents) in magnesium and magnesium alloys is the fifth of a series which will for

11、m a complete BritishStandard under the 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

12、alloys (photometric 1 : 10-phenanthroline method); Part3: Copper in magnesium and magnesium alloys (photometric method); Part4: Manganese in magnesium and magnesium alloys (photometric periodate method). The preparation of this series of methods has been authorized by the Non-ferrous Metals Industry

13、 Standards Committee 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

14、they are primarily 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 co

15、ntract. 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 andii, pages1 and 2, an inside back co

16、ver 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. 1) In course of preparation.BS3907-5:1966 BSI 12-1999 1 Introduction a) Principle. The sample is dissolved in s

17、ulphuric acid and oxidized with ammonium persulphate. The manganous ions are oxidized to permanganic acid with potassium periodate in the presence of phosphoric acid. The optical density is measured at about525nm. b) Range. The method is suitable for manganese contents less than0.01per cent. c) Repr

18、oducibility. 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 analysis of the results obtained: d) Application. The method is not suitable for alloys containing zirconium, rare eart

19、hs or thorium. Apparatus a) Class A volumetric glassware complying with the appropriate BritishStandards shall be used throughout. b) Any instrument suitable for measuring the optical density of the solution at a wave-length of525nm may be used with4cm cells. Alternatively when a filter photometer o

20、f the balanced two-cell type is used the following conditions have been found suitable: Mercury vapour lamp. Ilford604 with H503 or equivalent filters. 4cm cells. Solutions required All reagents shall be of the highest purity obtainable and either distilled or demineralized water shall be used throu

21、ghout. Solutions shall be freshly prepared and where necessary filtered. Standard manganese (1mlN 1mg of manganese). Dissolve2.877g of very pure potassium permanganate in about200ml of water and add40ml of sulphuric acid(25per cent). Reduce by adding a few crystals of sodium sulphite or by adding hy

22、drogen peroxide(100vol). Boil to eliminate excess SO 2or H 2 O 2 , cool, transfer to a1litre volumetric flask, dilute to the mark and mix. Alternatively: Weigh1.000g of high purity manganese(99.9per cent min. purity), transfer to a600ml tall form beaker, add80ml of water and40ml of sulphuric acid(25

23、per cent). When dissolved, boil the solution for about5 minutes, cool, transfer to a1litre volumetric flask, dilute to the mark and mix. Standard manganese (1mlN 0.02mg of manganese). Transfer20.0ml of standard manganese solution (1mlN 1mg of manganese) to a1litre volumetric flask, dilute to the mar

24、k and mix. Sodium nitrite (2per cent w/v). Dissolve2g of sodium nitrite in water, dilute to100ml and mix. Sulphuric acid (25per cent v/v). To40ml of water add cautiously25ml of sulphuric acid (sp. gr.1.84), mix, cool, dilute to100ml and mix. Sampling Recommended methods of obtaining a suitable sampl

25、e for the analytical procedure given below are described in BS1499, “Sampling non-ferrous metals”. Procedure a) Sample solution. Weigh2 0.01g of sample, transfer to a250ml beaker, add20ml of water, then add in small portions30ml of sulphuric acid(25per cent). Transfer the solution to a250ml conical

26、flask rinsing the beaker with10ml of water. Add0.05g of ammonium persulphate and boil for45minutes. b) Blank test. Carry out simultaneously a blank determination as follows: Transfer20ml of sulphuric acid(25per cent) to a platinum dish and evaporate to dryness. Take up the residue in a little warm w

27、ater, transfer the solution to a250ml conical flask, rinsing the dish with water, then dilute to about25ml. Add10ml of sulphuric acid(25per cent)0.05g of ammonium persulphate and boil for45minutes. c) Colour development. To the sample solution and the blank test solution add1ml of phosphoric acid (s

28、p. gr.1.75) and0.05g of potassium periodate, and boil for5minutes. Add0.5g of potassium periodate and allow to stand at about98 C for3040minutes. Cool, transfer to a50ml volumetric flask, dilute to the mark and mix. Manganese content Standard deviation per cent 0.005 per cent 0.0002BS3907-5:1966 2 B

29、SI 12-1999 Measure the optical density using the conditions specified under “Apparatus” adjusting the apparatus to0 optical density with water ( Ec ). Then destroy the permanganic acid by adding2drops of sodium nitrite solution (2per cent) to the solution in the cell and repeat the optical density m

30、easurement ( Ed ). In order to obtain the value for the optical density due to manganese, calculate for each dilution the differences ( Ec Ed )( Bc Bd ), where Bcand Bdare the optical densities corresponding to the blank test coloured and decolorized. Calibration To each of a series of six250ml beak

31、ers transfer0 (compensating solution),1.0,2.0,5.0,8.0,10.0ml of standard manganese solution (1mlN 0.02mg of manganese). Dilute to about50ml, then add10ml of sulphuric acid (25per cent) and0.05g of ammonium persulphate. Boil for45minutes. Continue from Procedure subsection c “Colour development”. Pre

32、pare a calibration graph by plotting the optical density against the equivalent percentage of manganese. Calculation where A = weight (mg) of manganese found in the sample solution, W = weight (g) of sample taken. Manganese per cent A W - 100 1000 - =BS3907-5:1966 BSI 12-1999 BritishStandards The fo

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