1、BRITISH STANDARD BS3907-4: 1966 Method for The determination of manganese in magnesium and magnesium alloys (Photometric Periodate method) Methods for the analysis of magnesium and magnesium alloysBS3907-4:1966 This BritishStandard, having been approved by the Non-ferrous Metals Industry Standards C
2、ommittee and endorsed by the Chairman of theEngineering 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 andNFE/23/4 Draft for comment D65/1420 ISBN 0 580
3、04411 4 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 Institution of Mi
4、ning 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 Association Associati
5、on 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 Association Briti
6、sh 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 Manufacturers and Electric
7、Cable Makers Confederation Traders Ltd.* 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 department and scient
8、ific 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 Ministry of Techn
9、ology, Laboratory of the Government Chemist Amendments issued since publication Amd. No. Date CommentsBS3907-4:1966 BSI 12-1999 i Contents Page Co-operating organizations Inside front cover Foreword ii Introduction 1 Apparatus 1 Solutions required 1 Sampling 1 Procedure 2 Calibration 2 Calculation 3
10、BS3907-4:1966 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 in magnesium and magnesium alloys is the fourth of a series which will form a complete BritishStandard
11、 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: Part 1: Aluminium in magnesium alloys (gravimetric method); Part 2: Iron in magnesium and magnesium alloys (photometric 1:10-p
12、henanthroline method); Part 3: Copper in magnesium and magnesium alloys (photometric method); Part 5: Manganese in magnesium and magnesium alloys (photometric periodate method) (low contents). The preparation of this series of methods has been authorized by the Non-ferrous Metals Industry Standards
13、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 they are pr
14、imarily 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 ISOR . . . . . . 1) . A British Standard does not purport to include all the necessary provisions of a contract. Use
15、rs 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 to3 and a back cover. This standard
16、 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.BS3907-4:1966 BSI 12-1999 1 Introduction a) Principle. The sample is dissolved in sulphuric acid and oxidized with nit
17、ric acid. 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 content between0.01 and0.8percent. c) Reproducibility. Experiments have been carrie
18、d 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 earths or thorium. Apparatus a) Class A volum
19、etric 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 with2cm cells. Alternatively when a filter photometer of the balanced two-cell type is used the
20、following conditions have been found suitable: Mercury vapour lamp. Ilford604 with H503 or equivalent filters. 2cm cells. Solutions required All reagents shall be of the highest purity obtainable, and either distilled or demineralized water shall be used throughout. Solutions shall be freshly prepar
21、ed 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 (25percent). Reduce by adding a few crystals of sodium sulphite or by adding hydrogen peroxide (100vol). Boil to elimin
22、ate excess SO 2orH 2 O 2 , cool, transfer to a1litre volumetric flask, dilute to the mark and mix. Alternatively. Weigh1.000g of high purity manganese (99.9percent min purity), transfer to a600ml tall form beaker, add80ml of water and40ml of sulphuric acid (25percent). When dissolved boil the soluti
23、on for about5minutes, cool, transfer to a1litre volumetric flask, dilute to the mark and mix. Standard manganese (1mlN 0.05mg of manganese). Transfer50.0ml of standard manganese solution (1mlN 1mg of manganese) to a1litre volumetric flask, dilute to the mark and mix. Sodium nitrite (2percentw/v). Di
24、ssolve2g of sodium nitrite in water, dilute to100ml and mix. Sulphuric acid (25percentv/v). To400ml of water add cautiously250ml of sulphuric acid (sp.gr.1.84), mix, cool, dilute to1litre and mix. Sampling Recommended methods of obtaining a suitable sample for the analytical procedure given below ar
25、e described in BS1499, “Sampling non-ferrous metals”. Manganese content Standard deviation per cent 0.01 0.1 0.8 per cent 0.002 0.005 0.02BS3907-4:1966 2 BSI 12-1999 Procedure a) Sample solution. Adjust the weight of sample and quantities of acid to be used as follows: Transfer the appropriate weigh
26、t of sample to a250ml tall form beaker, add10ml of water, then in small portions, the appropriate quantity of sulphuric acid (25percent). When the reaction appears to be complete add the appropriate quantity of nitric acid (sp.gr.1.42) and2 or3 drops of hydrofluoric acid 2) . Boil the solution for a
27、 few minutes, and cool. For manganese contents over 0.01up to and including 0.2percent use the whole of the solution. For manganese contents over 0.2 up to and including 0.8 percent transfer the solution obtained to a100ml volumetric flask, cool, dilute to the mark and mix. Transfer20.0ml of this so
28、lution (corresponding to0.1g of sample) to a250ml beaker. Then add15ml of sulphuric acid (25percent) and25ml of nitric acid (sp.gr.1.42). b) Blank test. Carry out simultaneously a blank determination as follows: Transfer the quantities of reagents shown in the following table to a platinum dish. Eva
29、porate to dryness and take up the residue in a little warm water. Transfer the solution to a250ml beaker and dilute to about40ml. For manganese contents over 0.01 up to and including 0.2 percent, add20ml of sulphuric acid (25percent), and two or three drops of hydrofluoric acid 2) . For manganese co
30、ntents over 0.2 up to and including 0.8percent, add16ml of sulphuric acid(25percent),3ml of nitric acid (sp.gr.1.42), and a few drops of hydrofluoric acid. c) Colour development. To the sample solution and the blank test solution add the quantity of water necessary to obtain a volume of about60ml th
31、en5ml of phosphoric acid (sp.gr.1.75). Heat to boiling and add0.5g of potassium periodate. Boil for3minutes, then allow to stand at about98 C for15minutes. Cool, transfer to a100ml volumetric flask, dilute to the mark and mix. Measure the optical density using the conditions specified under “Apparat
32、us” adjusting the apparatus to0optical density with water ( Ec ). Then destroy the permanganic acid by adding2drops of sodium nitrite solution (2percent) to the solution in the cell and repeat the optical density measurement ( Ed ). In order to obtain the value for the optical density due to mangane
33、se, calculate for each dilution the differences( Ec Ed )( Bc Bd ), where Bcand Bdare the optical densities corresponding to the solution of the blank test coloured and decolorized. Calibration To each of a series of six250ml beakers transfer1.0,2.0,5.0,10.0,15.0,20.0ml of standard manganese solution
34、 (1mlN 0.05mg of manganese). Dilute to about40ml, then add15ml of sulphuric acid (25percent),25ml of nitric acid (sp.gr.1.42) and5ml of phosphoric acid (sp.gr.1.75). Manganese content Weight of sample Volume of sulphuric acid (25percent) Volume of nitric acid (sp.gr.1.42) over up to and including pe
35、rcent 0.01 0.05 0.2 percent 0.05 0.2 0.8 g 1 0.001 0.5 0.001 0.5 0.001 ml 25 20 10 ml 25 25 5 2) This refers to the usual analytical reagent grade of40percentw/w. Manganese content Volume of sulphuric acid (25percent) Volume of nitric acid (sp.gr.1.42) over up to and including per cent 0.01 0.05 0.2
36、 per cent 0.05 0.2 0.8 ml 5 ml 25 25 25BS3907-4:1966 BSI 12-1999 3 Transfer20ml of nitric acid (sp.gr.1.42) to a platinum dish and evaporate to dryness. Take up the residue in a little warm water, transfer to a seventh250ml beaker. Dilute to about40ml, then add15ml of sulphuric acid (25percent),5ml
37、of nitric acid (sp.gr.1.42) and5ml of phosphoric acid (sp.gr.1.75). For each beaker continue from procedure Subsection c “Colour development” paragraph2. Prepare a calibration graph by plotting the optical density against the equivalent percentage of manganese. Calculation Manganese percent= Where A
38、 = weight (mg) of manganese corresponding to the aliquot taken, R = the ratio of the volume of the main solution to the volume of the aliquot taken, W = weight (g) of sample taken. AR W - 100 1000 - BS3907-4: 1966 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the ind
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