BS 3907-10-1969 Methods for the analysis of magnesium and magnesium alloys - Determination of manganese in magnesium alloys containing zirconium rare earths thorium and or silver (.pdf

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1、BRITISH STANDARD BS3907-10: 1969 Method for The determination of manganese in magnesium alloys containing zirconium, rare earths, thorium and/or silver (Photometric method) Methods for the analysis of magnesium and magnesium alloysBS3907-10:1969 This British Standard, having been approved by the Non

2、-ferrous Metals Industry Standards Committee, was published under the authority ofthe Executive Board on 18March1969 BSI12-1999 The following BSI references relate to the work on this standard: Committee references NFE/23 andNFE/23/4 Draft for comment67/32424 ISBN 580 04399 1 Co-operating organizati

3、ons 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: Aluminium Federation Institution of Mining and Metallurgy Associatio

4、n 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 Association Association London Metal Exchange Briti

5、sh 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 Association British Non-ferrous Metals Federati

6、on High Non-ferrous Metal Stockists* Conductivity Copper Group Post Office British Non-ferrous Metals Research Royal Institute of British Architects Association* Society of British Aerospace Companies Ltd. Copper Development Association Society of Motor Manufacturers and Traders Crown Agents for Ove

7、rsea Governments and Ltd.* Administrations Tin Research Institute Electric Cable Makers Confederation Zinc Development Association Institute of British Foundrymen Individual manufacturer Institute of Metals Institution of Mechanical Engineers (Automobile Division) The Government department and scien

8、tific 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 British Standard: Institute of Sheet Metal Engineering Individual analysts Ministry of Technology Ministry of T

9、echnology Laboratory of the Government Chemist Amendments issued since publication Amd. No. Date CommentsBS3907-10:1969 BSI 12-1999 i Contents Page Co-operating organizations Inside front cover Foreword ii 1 Introduction 1 2 Apparatus 1 3 Solutions required 1 4 Sampling 1 5 Procedure 1 6 Calibration

10、 2 7 Calculation 2BS3907-10:1969 ii BSI 12-1999 Foreword This standard makes reference to the following British Standards: BS1499, Sampling non-ferrous metals. BS3978, Water for laboratory use. This method for the photometric determination of manganese in magnesium alloys containing zirconium, rare

11、earths, thorium and/or silver is the tenth of a series which will form a complete British Standard 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 (gravimetri

12、c method); Part2: Iron (photometric 1.10 phenanthroline method); Part3: Copper (photometric method); Part4: Manganese (photometric periodate method); Part5: Manganese (photometric periodate method) (low contents); Part6: Zirconium (photometric method); Part7: Nickel (photometric method); Part8: Tota

13、l rare earths (gravimetric method) 1) ; Part9: Zinc (ion-exchange volumetric EDTA method); Part11: Silicon (photometric method) 1) . The preparation of this series of methods has been authorized by the Non-Ferrous Metals Industry Standards Committee as part of a general programme for the standardiza

14、tion 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 “referee” methods to be used in cases of

15、 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. Users of British Standards are responsible for their correct appli

16、cation. 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 aback cover. This standard has been updated (see copyright date) and may have had amendme

17、nts incorporated. This will be indicated in the amendment table on the inside front cover. 1) In course of preparation.BS3907-10:1969 BSI 12-1999 1 1 Introduction 1.1 Principle. The sample is dissolved in sulphuric acid and oxidized with nitric acid. The manganous ions are oxidized to permanganic ac

18、id with potassium periodate. The optical density is measured at about545nm. 1.2 Range. The method is suitable for manganese contents less than0.2%. 1.3 Reproducibility. Experiments have been carried out independently by a number of analysts using this method. The degree of reproducibility that can b

19、e expected is shown by the following analysis of the results obtained: 2 Apparatus 2.1 Class A volumetric glassware complying with the appropriate British Standards shall be used throughout. 2.2 Any instrument suitable for measuring the optical density of the solution at a wavelength of545nm may be

20、used with a2 or4cm cell. Alternatively when a filter photometer of the balanced two-cell type is used the following conditions have been found suitable: Mercury vapour 1 amp. Ilford605 filter with H503 heat filter or equivalent filters. 2 or4cm cell. 3 Solutions required All reagents shall be of the

21、 highest purity obtainable, and either distilled or demineralized water complying with BS3978 2)shall be used throughout. Solutions shall be freshly prepared and where necessary filtered. Standard manganese (1ml N 1mg of manganese). Dissolve2.877g of very pure potassium permanganate in about200ml of

22、 water and add40ml of sulphuric acid(25%). Reduce by adding a few crystals of sodium sulphite or by hydrogen peroxide(100vol). Boil to eliminate excess SO 2or H 2 O 2 , cool, transfer to a litre volumetric flask, dilute to the mark and mix. Alternatively: Weigh1.000g of high purity manganese (at lea

23、st99.9%Mn), transfer to a600ml tall form beaker, add80ml of water and40ml of sulphuric acid(25%). When dissolved boil the solution for about5 minutes, cool, transfer to a1litre volumetric flask, dilute to the mark and mix. Standard manganese (1ml N 0.1mg of manganese). Transfer100.0ml of standard ma

24、nganese solution(1ml N 1mg of manganese) toa1litre volumetric flask, dilute to the mark and mix. Standard manganese (1ml N 0.02mg of manganese). Transfer20.0ml of standard manganese solution(1mlN 1mg of manganese) to a1litre volumetric flask, dilute to the mark and mix. Fluoroboric acid (1%v/v). Dil

25、ute10ml of fluoroboric acid 3)to1litre. Sodium nitrite(2% w/v). Dissolve2g of sodium nitrite in water, dilute to100ml and mix. Sulphuric acid (25%v/v). To40ml of water add cautiously25ml of sulphuric acid (sp.gr.1.84), mix, cool, dilute to100ml and mix. 4 Sampling Recommended methods of obtaining a

26、suitable sample for the analytical procedure given below are described in BS1499, “Sampling nonferrous metals”. 5 Procedure 5.1 Weigh1 0.01g of sample, transfer to a250ml beaker, add10ml of water, then add in small portions25ml of sulphuric acid(25%). 5.2 Carry out simultaneously a blank determinati

27、on following the same procedure and using the same amounts of reagents as with the sample. 5.3 When the reaction appears to be complete add25ml of nitric acid (sp.gr.1.42) and5ml of fluoroboric acid(1%), and boil vigorously for2minutes. 5.4 Add0.5g of potassium periodate, boil for5minutes then allow

28、 to stand at about98 C for15minutes. Cool, transfer to a100ml volumetric flask, dilute to the mark and mix. Manganese content Standard deviation % 0.006 0.03 0.12 0.0006 0.0015 0.003 2) BS3978, “Water for laboratory use”. 3) This refers to the usual analytical reagent grade of42%w/w.BS3907-10:1969 2

29、 BSI 12-1999 5.5 Measure the optical density at about545nm, adjusting the apparatus to0 optical density with water (% E c ). Then destroy the permanganic acid by adding2 drops of sodium nitrite solution(2%) to the solution in the cell and repeat the optical density measurement (% E d ). In order to

30、obtain the value for the optical density due to manganese, calculate for each dilution the differences (% E c % E d )(% B c % B d ), where % B cand % B dare the optical densities corresponding to the blank test coloured and decolorized. 6 Calibration 6.1 For manganese contents up to0.01% 6.1.1 To ea

31、ch of a series of six250ml beakers transfer0 (compensating solution),1.0,2.0,5.0,8.0,10.0ml of standard manganese solution(1ml N 0.02mg of manganese). 6.1.2 Dilute to about50ml then add15ml of sulphuric acid(25%), and continue from5.3 of the procedure. 6.1.3 Prepare a calibration graph by plotting t

32、he optical density against the equivalent percentage of manganese. 6.2 For manganese contents between0.01% and0.2% 6.2.1 To each of a series of six250ml beakers transfer1.0,2.0,5.0,10.0,15.0,20.0ml of standard manganese solution(1ml N 0.1mg of manganese). 6.2.2 Dilute to about50ml then add15ml of su

33、lphuric acid(25%), and continue from5.3 of the procedure. 6.2.3 Prepare a calibration graph by plotting the optical density against the equivalent percentage of manganese. 7 Calculation where A =weight (mg) of manganese found in the sample solution, W =weight (g) of sample taken. Manganese per cent

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