1、BRITISH STANDARD BS3907-2: 1966 Method for The determination of iron in magnesium and magnesium alloys (photometric 1:10-phenanthroline method)BS3907-2:1966 This BritishStandard, having been approved by the Non-ferrous Metals Industry Standards Committee and endorsed by the Chairman of theEngineerin
2、g Divisional Council, was published under theauthority of the General Council on 17 March1966 BSI11-1999 The following BSI references relate to the work on this standard: Committee references NFE/23 andNFE/23/4 Draft for comment D65/1418 ISBN 0 580 04391 6 Co-operating organizations The Non-ferrous
3、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 Mining and Metallurgy Association of Bronze and Brass
4、 Founders Institution of Production Engineers Association of Consulting Engineers Institution of Structural Engineers Board of Trade Lead Development Association British Bronze and Brass Ingot Light Metal Founders Association Manufacturers Association London Metal Exchange British Electrical and All
5、ied 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 Research Non-ferrous Metal St
6、ockists* 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 Traders Electric Cable Makers Confederation Ltd.* High Condu
7、ctivity 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 scientific and industrial organizations marked with an as
8、terisk 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 Technology, Laboratory of the Government Chemist Amendme
9、nts issued since publication Amd. No. Date CommentsBS3907-2:1966 BSI 11-1999 i Contents Page Co-operating organizations Inside front cover Foreword ii Introduction 1 Apparatus 1 Solutions required 1 Sampling 1 Procedure 1 Calibration 2 Calculation 2BS3907-2:1966 ii BSI 11-1999 Foreword This standard
10、 makes reference to the following BritishStandard: BS1499, Sampling non-ferrous metals. This method for the photometric determination of iron in magnesium and magnesium alloys is the second of a series which will form a complete British Standard under the collective title “Methods for the analysis o
11、f 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); Part3: Copper in magnesium and magnesium alloys (photometric method); Part4: Manganese in magnesium and magnesium alloys (
12、photometric periodate method); Part5: 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 Committee as part of a general programme for the standardization
13、 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 dis
14、pute. 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 applicati
15、on. 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 updated (see copyright date) and may have had amendments
16、 incorporated. This will be indicated in the amendment table on the inside front cover. 1) In course of preparation.BS3907-2:1966 BSI 11-1999 1 Introduction a) Principle. The sample is dissolved in hydrochloric acid and any undissolved residue is filtered off. Hydroxyammonium chloride solution is ad
17、ded and the ferrous1:10-phenanthroline colour is developed in the presence of a buffer solution. The optical density of the orange-red solution is measured at about510nm. b) Range. The method is suitable for iron contents between0.0020.05percent. c) Reproducibility. Experiments have been carried out
18、 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 more than4percent of zinc and has not been tested in the presence
19、of zirconium. Apparatus a) Class A volumetric glassware complying with the appropriate British Standards shall be used throughout. It should be carefully washed with warm hydrochloric acid, thoroughly rinsed with water, and finally with distilled water. b) Any instrument suitable for measuring the o
20、ptical density of the solution at a wavelength of510nm may be used with1 or2cm cells. Alternatively when a filter photometer of the balanced two-cell type is used, the following conditions have been found suitable: Tungsten lamp. Ilford603 or equivalent filter. 1 or2cm cells. Solutions required All
21、reagents shall be of the highest purity obtainable, and either distilled or mineralized water shall be used throughout. Solutions shall be freshly prepared and where necessary filtered. Standard iron (1mlN 0.2mg of iron). Dissolve1.4045g of ammonium ferrous sulphate (NH 4 ) 2Fe(SO 4 ) 2 .6H 2 O) in
22、a little water and add20ml of hydrochloric acid(50percent). Transfer to a1litre volumetric flask, dilute to the mark and mix. Alternatively: Weigh0.2860g of pure ferric oxide (Fe 2 O 3 ) previously calcined at600 C and transfer to a100ml beaker, add30ml of hydrochloric acid(50percent) cover with a w
23、atch glass and heat. Cool, transfer to a1litre volumetric flask, dilute to the mark and mix. Standard iron (1mlN 0.01mg of iron). Transfer50.0ml of standard iron solution(1mlN 0.2mg of iron) to a1litre volumetric flask, dilute to the mark and mix. This solution should be freshly prepared. Buffer. Di
24、ssolve272g of sodium acetate (CH 3COONa.3H 2 O) in about500ml of water, add240ml of glacial acetic acid, filter if necessary then dilute to1litre and mix. Hydrochloric acid (50percentv/v). Dilute500ml of hydrochloric acid (sp.gr.1.16 to1.18) to1litre and mix. Hydroxyammonium chloride (1percentw/v).
25、Dissolve10g of hydroxyammonium chloride in water, dilute to1litre and mix. 1:10-phenanthroline (1percentw/v). Dissolve10g of1:10-phenanthroline hydrochloride (C 12 H 8 N 2 .HCl.H 2 O) in water, warm slightly to complete solution, cool, dilute to1litre and mix. Alternatively: Dissolve10g of1:10-phena
26、nthroline (C 12 H 8 N 2 .H 2 O) in ethanol, dilute to1litre with ethanol and mix. Sampling Recommended methods of obtaining a suitable sample for the analytical procedure given below are described in BS1499, “Sampling non-ferrous metals”. Procedure Adjust the weight of sample and quantity of hydroch
27、loric acid(50percent) to be added as follows: Transfer the appropriate weight of sample to a150ml beaker, add10ml of water, then gradually add the specified quantity of hydrochloric acid(50percent), cover the beaker and heat until solvent action ceases. Iron content Standard deviation percent 0.002
28、0.01 0.05 percent 0.0003 0.0006 0.0012 Iron content Weight of sample Hydrochloric acid (50percent) over up to and including percent 0.002 0.01 percent 0.01 0.05 g 1 0.001 0.5 0.001 ml 15 7.5BS3907-2:1966 2 BSI 11-1999 Carry out simultaneously a blank determination following the same procedure and us
29、ing the same amounts of reagents as with the sample. Filter through a medium texture filter paper, and wash the beaker and the residue5 or6times with warm water. Using a water bath, evaporate the solution to a syrupy consistency (about8ml for a1g sample and4ml for a0.5g sample). Add10ml of water, tr
30、ansfer to a100ml volumetric flask, wash the beaker and add the washings to the same volumetric flask. Dilute to about50ml and allow to cool. Add4ml of hydroxyammonium chloride solution(1percent),15ml of the buffer solution and the appropriate quantity of1:10-phenanthroline solution(1percent) given i
31、n the table below: Dilute to the mark and mix. After15minutes measure the optical density using the conditions specified under “Apparatus”. Calibration Into each of a series of fifteen100ml volumetric flaskstransfer:0,2.0,4.0,6.0,8.0,10.0,12.0,14.0, 16.0, 18.0,20.0,22.0,24.0,26.0,28.0ml of standard
32、iron solution(1ml=0.01mg of iron). Dilute to about50ml and continue from Paragraph5 of the procedure. Measure the optical density using the conditions specified under “Apparatus” and prepare a calibration graph by plotting the optical density against the equivalent percentage of iron. Calculation Ir
33、on percent= Material 1:10-phenanthroline solution Pure magnesium Magnesium alloys ml 2 Zinc content less than2percent Zinc content between 24percent 6 12 Where A = weight(mg) of iron found in the sample solution, W = weight(g) of sample taken. A W - 100 1000 - blankBS3907-2: 1966 BSI 389 Chiswick Hi
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