1、BRITISH STANDARD BS3907-1: 1965 Method for The determination of aluminium in magnesium alloys (Gravimetric method) Methods for the analysis of magnesium and magnesium alloysBS3907-1:1965 This BritishStandard, having been approved by the Non-ferrous Metals Industry Standards Committee and endorsed by
2、 the Chairman of theEngineering Divisional Council, was published under theauthority of the General Council on 9 July1965 BSI 12-1999 The following BSI references relate to the work on this standard: Committee references NFE/23 and NFE/23/4 Draft for comment D63/11002 ISBN 0 580 04381 9 Co-operating
3、 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 Mining and Metallurgy
4、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 Association London Metal Exch
5、ange British Electrical and Allied Manufacturers Magnesium Industry Council Association Ministry of Aviation British Lead Manufacturers Association Ministry of Defence, Army Department* British Non-ferrous Metals Federation Ministry of Defence, Navy Department British Non-ferrous Metals Research Nat
6、ional Brassfoundry Association Association* Non-ferrous Metal Stockists Copper Development Association Post Office Crown Agents for Oversea Governments and Royal Institute of British Architects Administrations Society of British Aerospace Companies Ltd. Electric Cable Makers Confederation Society of
7、 Motor Manufacturers and High Conductivity Copper Association TradersLtd.* Institute of British Foundrymen Tin Research Institute Institute of Metals Zinc Development Association Institution of Mechanical Engineers Individual manufacturers (Automobile Division) The Government departments and scienti
8、fic 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 Technology Laboratory of th
9、e Government Chemist Amendments issued since publication Amd. No. Date CommentsBS3907-1:1965 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 Calculation 2BS3907-1:1965 ii BSI 12-1999 Foreword
10、 This standard makes reference to the following BritishStandard: BS1499, Sampling non-ferrous metals. This method for the gravimetric determination of aluminium in magnesium alloys is the first of a series which will form a complete BritishStandard under the collective title “Methods for the analysi
11、s of magnesium and magnesium alloys” each being published as a separate part. Other methods in the series are as follows: Part2: Iron-photometric method; 1) Part3: Copper-photometric method; 1) Part4: Manganese-photometric-periodate method; 1) Part5: Manganese-photometric-periodate method (low conte
12、nts). 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 standardization of methods for the sampling and analysis of non-ferrous metals. The methods have been found to give reliable and reprod
13、ucible 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 dispute. This method is substantially the same as the corresponding method approved by ISO/TC79 which will be published as
14、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 application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This documen
15、t 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 incorporated. This will be indicated in the amendment table on the inside front cover. 1) In course of preparation.BS3907-1:19
16、65 BSI 12-1999 1 Introduction a) Principle. The sample is dissolved in hydrochloric acid and aluminium is precipitated as benzoate in an acetic acid medium containing hydroxyammonium chloride. The precipitate is dissolved and the aluminium reprecipitated by8-hydroxyquinoline in an acetic acid buffer
17、 medium. The precipitate is filtered, washed, dried and weighed. b) Range. The method is suitable for aluminium contents between1.5and12.0 per cent. c) Reproducibility. Experiments have been carried out independently by a number of analysts using this method. The degree of reproducibility that can b
18、e 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 Class A volumetric glassware complying with the appropriate BritishStandards shall be used throughout. Solutions require
19、d All reagents shall be of the highest purity obtainable and either distilled or demineralized water shall be used throughout. Solutions shall be freshly prepared and where necessary filtered. Acetic acid (approximately1.7N). Dilute100ml of glacial acetic acid to1 litre and mix. Ammonia (25 per cent
20、 v/v). Dilute25ml of ammonia solution(sp.gr.0.880.91) to100ml and mix. Ammonium acetate (60 per cent w/v). Dissolve600g of ammonium acetate in water, dilute to1 litre and mix. Ammonium benzoate (10 per cent w/v). Dissolve100g of ammonium benzoate in tepid water, add0.001g of thymol and after cooling
21、 dilute to1 litre and mix. Ammonium benzoate wash. Dilute100ml of ammonium benzoate solution(10 per cent w/v) with900ml of water, add20ml of glacial acetic acid and mix. Complexing solution. Dissolve in a little water50g of hydroxyammonium chloride,50g of ammonium chloride and50ml of glacial acetic
22、acid, then dilute to1 litre and mix. Hydrochloric acid (25 per cent v/v). Dilute25ml of hydrochloric acid(sp.gr.1.161.18) to100ml and mix. 8-hydroxyquinoline (2 per cent w/v). Dissolve20g of8-hydroxyquinoline in80ml of glacial acetic acid and dilute to1 litre with water. Keep in a dark glass bottle.
23、 Nitric acid (75 per cent v/v). Dilute75ml of nitric acid(sp.gr.1.42) to100ml and mix. Tartaric acid (50 per cent w/v). Dissolve500g of tartaric acid in water, dilute to1 litre and mix. Tartaric acid hydrochloric acid. To50ml of hydrochloric acid(25 per cent v/v) add10ml of tartaric acid solution(50
24、 per cent w/v) and mix. Bromophenol blue (0.2 per cent w/v). Dissolve0.20g of bromophenol blue in100ml of ethanol(95percent) and mix. Neutral red (0.05 per cent w/v). Dissolve0.05g of neutral red in100ml of ethanol(95 per cent) and mix. Sampling Recommended methods of obtaining a suitable sample for
25、 the analytical procedure given below are described in BS1499, “Sampling non-ferrous metals”. Procedure Adjust the weight of sample and quantity of hydrochloric acid(sp.gr.1.161.18) to be added as follows: Transfer the appropriate weight of sample to a250ml beaker, add25ml of water then gradually ad
26、d the specified quantity of hydrochloric acid (sp.gr.1.161.18) and2ml of nitric acid(75percent), cover the beaker and heat until solvent action ceases. Carry out simultaneously a blank determination following the same procedure and using the same amounts of reagents as with the sample. Aluminium con
27、tent Standard deviation per cent per cent 10 6 2 0.05 0.05 0.03 Aluminium content Weight of sample Hydrochloric acid (sp.gr1.161.18) per cent g ml 1.5 to5 5to12 0.5 0.001 1 0.001 5 10BS3907-1:1965 2 BSI 12-1999 Filter the solution through a medium texture filter paper and wash the beaker and the res
28、idue5 or6 times with warm water adding the washings to the sample solution. Discard the residue. Boil the solution for1 to2 minutes. Cool, wash the watch glass and the sides of the beaker with a little water then dilute to about50ml. For a 1 g sample, transfer the solution to a250ml volumetric flask
29、, dilute to the mark, mix and transfer50.0ml of this solution to a250ml beaker. For a 0.5g sample, carry out the analysis on the whole of the solution. Add40ml of water,2 or3 drops of bromophenol blue indicator(0.2 per cent) and ammonia solution(25 per cent) until the solution becomes violet. Then a
30、dd20ml of the complexing solution and20ml of ammonium benzoate solution(10percent). Heat to boiling whilst stirring, continue boiling gently for5 minutes, then filter through a medium texture filter paper. Wash the beaker and the precipitate8 to10 times with boiling ammonium benzoate wash solution d
31、iscarding the filtrate. Dissolve the precipitate from the filter with small portions of boiling tartaric acid-hydrochloric acid solution. Wash the filter with warm water and collect the solution and washings in the original beaker. Transfer to a400ml beaker, add1g of sodium sulphite(Na 2 SO 3 .7H 2
32、O), a few drops of neutral red indicator(0.05 per cent) and carefully add ammonia solution (sp.gr.0.880.91) until the solution becomes yellow. Dilute to about200ml then heat to about70 C. Add acetic acid (approximately1.7N) until the solution becomes red, then, whilst stirring,40ml of8-hydroxyquinol
33、ine solution(2 per cent) and50ml ammonium acetate solution(60 per cent). Allow the precipitate to settle at about70 C for30minutes. Filter the precipitate through a tared sintered glass crucible (porosity315 microns) by applying weak suction, then wash thoroughly at least6times with hot water. Dry t
34、o constant weight in an oven at130 C, cool in a disiccator and weigh. Calculation where: A = weight (g) of the precipitate 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 the sample taken. Aluminium per cent A
35、 5.87 R W - =blankBS3907-1: 1965 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing BritishStandards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter
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