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1、BRITISH STANDARD BS 3338-5: 1961 Method for The determination of lead in ingot tin and tin-antimony solders (photometric method) Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:38 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-5:1961 This British Standard, having been approved by th
2、e Non-ferrous Metals Industry Standards Committee and endorsed by the Chairman of the Engineering Divisional Council, was published under the authority of the General Council on 29 April 1961 BSI 11-1999 The following BSI references relate to the work on this standard: Committee references NFE/27, N
3、FE/27/1 Draft for comment A(NFE) 9202 ISBN 0 580 03057 1 Co-operating organizations 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 org
4、anizations: Admiralty*Institution of Mining and Metallurgy Aluminium Development AssociationInstitution of Structural Engineers Aluminium Industry CouncilLead Development Association Association of Bronze and Brass FoundersLead Sheet and Pipe Manufacturers Association of Consulting Engineers,Federat
5、ion (Incorporated)Light Metal Founders Association British Bronze and Brass Ingot ManufacturersLondon Metal Exchange* AssociationMagnesium Industry Council British Electrical and Allied ManufacturersMinistry of Aviation* Association*National Brassfoundry Association British Non-ferrous Metals Federa
6、tionNon-ferrous Metal Stockists British Non-ferrous Metals ResearchPost Office* Association*Royal Institute of British Architects Cable Makers Association*Society of British Aircraft Constructors Copper Development AssociationSociety of Motor Manufacturers and Traders Crown Agents for Oversea Govern
7、ments andLtd.* AdministrationsTin Research Institute* High Commission of IndiaWar Office* High Conductivity Copper AssociationZinc Development Association Institute of British FoundrymenIndividual manufacturers Institute of Metals Institution of Mechanical Engineers (Automobile Division) The Governm
8、ent departments 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 British Standard: British Railways, The British TransportLondon Transport Executive, T
9、he British CommissionTransport commission British Tin Box Manufacturers FederationSolder Makers Association Electronic Engineering AssociationTinplate Conference (1925) Gas CouncilTin Producers Association Institution of Gas EngineersIndividual firms Amendments issued since publication Amd. No.DateC
10、omments Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:38 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-5:1961 BSI 11-1999i Contents Page Co-operating organizationsInside front cover Forewordii Introduction1 Apparatus1 Solutions required1 Sampling1 Procedure1 Calibration2 Licensed
11、 Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:38 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-5:1961 ii BSI 11-1999 Foreword This standard makes reference to the following British Standard: BS 3338-1, Sampling of ingot tin. BS 3338-12, Sampling of solders. This method for the determinat
12、ion of lead in ingot tin and tin-antimony solders is the fifth of a series of methods which will form a complete British Standard under the collective title “Methods for the sampling and analysis of tin and tin alloys”, each method being published as a separate part. The preparation of this series o
13、f 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. Other methods in the series are as follows: Part 1: Sampling of ingot tin; Part 2: Determination
14、 of tin in ingot tin; Part 3: Determination of antimony in ingot tin; Part 4: Determination of copper in ingot tin and tin-lead solders; Part 6: Determination of copper in high purity ingot tin; Part 7: Determination of silver in solders; Part 8: Determination of bismuth in ingot tin, tin-lead solde
15、rs and white metal bearing alloys; Part 9: Determination of arsenic in ingot tin, tin-lead solders and white metal bearing alloys; Part 10: Determination of iron in ingot tin, tin-lead solders and white metal bearing alloys; Part 11: Determination of tin in solders; Part 12: Sampling of solders. The
16、 complete British Standard methods will be found suitable for the grades of metals covered by BS 3252, “Ingot tin”, BS 219, “Soft solders” and BS 3332,“White metal bearing alloy ingots”. In the methods for determining impurities, sample weights and aliquots have been chosen to cover the range of imp
17、urity content usually found in commercial tin ingots, solders and white metal bearing alloy ingots. For amounts of impurity outside this range, sample weights or aliquots should be adjusted accordingly. The methods have been found to give reliable and reproducible results, and, while in some instanc
18、es they may appear to be lengthy, it should be realized that they are put forward as “referee” methods to be used in cases of dispute. In the preparation of the calibration graphs an attempt has been made to define concentrations, but because these are linked with the particular instrument used for
19、determining optical density they should be used only as a guide. 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
20、from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, pages 1 and 2 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 in
21、side front cover. Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:38 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-5:1961 BSI 11-19991 Introduction a) Principle. Lead is determined photometrically with dithizone after removal of tin as bromide. b) Range. Up to 0.9 per cent lead. c)
22、 Reproducibility. 10 per cent of lead present. Apparatus a) Any volumetric glassware used shall be of Class A accuracy as defined in the appropriate British Standards, or where no British Standard exists, as described in the National Physical Laboratory Publication “Volumetric Tests on Volumetric Gl
23、assware”. b) Any instrument suitable for measuring the optical density of the solution at a wavelength of 510 m4 may be used. c) 4 cm or 1 cm cells (Note 1). d) Alternatively, if a filter photometer of the balanced two cell type is used, the filter combination should conform as closely as possible t
24、o the above wavelength. The following have been found suitable: Tungsten lamp Ilford 604 or equivalent filters. Solutions required All reagents shall be of the highest purity obtainable and distilled water shall be used throughout. Solutions shall be freshly prepared and, where necessary, filtered.
25、Standard lead (1 ml N 0.10 mg of lead). Dissolve 40.0 mg of lead nitrate in nitric acid (5 per cent v/v), transfer to a 250 ml graduated flask, and dilute to the mark. Standard lead (1 ml N 0.01 mg of lead). Dilute 25 ml of the above solution to 250 ml in a graduated flask. Bromine-hydrobromic acid.
26、 Add 10 ml of bromine to 90 ml of hydrobromic acid (48 per cent v/v). Dithizone solution (0.006 per cent w/v). Dissolve 30 mg of dithizone in 25 ml of chloroform and extract twice in a large separating funnel with 100-ml portions of ammonia solution (2 per cent v/v). Discard the chloroform layer and
27、 wash the combined aqueous layers with about 20 ml of chloroform. Again discard the chloroform layer. Make the aqueous solution just acid by addition of hydrochloric acid (sp. gr. 1.161.18) and shake with 250 ml of chloroform. Separate the chloroform layer, add a further 250 ml of chloroform and sha
28、ke again. Separate and combine the two chloroform extracts. Wash with water and store in a dark bottle. Hydroxyammonium chloride (10 per cent w/v). Dissolve 10 g of hydroxyammonium chloride in 100 ml of water. Nitric acid (50 per cent v/v). Dilute 50 ml of nitric acid (sp. gr. 1.42) to 100 ml. Nitri
29、c acid (5 per cent v/v). Dilute 5 ml of nitric acid (sp. gr. 1.42) to 100 ml. Potassium cyanide (ammoniacal). Dissolve 5 g of potassium cyanide and 1 g of sodium sulphite in 400 ml of water and add 250 ml of ammonia solution (sp. gr. 0.91). Sodium tartrate (20 per cent w/v). Dissolve 20 g of sodium
30、tartrate in water and dilute to 100 ml. Thymol blue indicator. Warm 0.1 g of thymol blue with 4.3 ml of sodium hydroxide solution (0.2 per cent w/v) and 5 ml of alcohol until dissolved. Dilute with alcohol (20 per cent) to 250 ml. Sampling Recommended methods of obtaining a suitable sample for the a
31、nalytical procedure given below are described in BS 3338-1, “Sampling of ingot tin” and Part 12, “Sampling of solders”. Procedure Dissolve 0.25 g of sample in 10 ml of bromine-hydrobromic acid in a 150 ml beaker and evaporate to dryness. Add a further 5 ml of bromine-hydrobromic acid and evaporate a
32、gain. To the residue add 5 ml of nitric acid (50 per cent) and boil until free from bromine. Cool, transfer to a 100 ml graduated flask and dilute to the mark. Transfer by means of a pipette a 10 ml aliquot (Note 2) into a small beaker, add 1 ml of hydroxyammonium chloride solution (10 per cent) and
33、 heat just to boiling. Cool, add 2 ml of sodium tartrate solution (20 per cent) and one drop of thymol blue indicator, and neutralize with ammonia solution (sp. gr. 0.91) to the blue colour. Transfer to a 200 ml separating funnel, add 65 ml of potassium cyanide solution (ammoniacal) and 20.0 ml of d
34、ithizone solution (0.006 per cent), and shake for one minute. Insert a roll of filter paper1) in the stem of the funnel and run off the chloroform layer into a small stoppered bottle. Measure the optical density of the solution at 20 1 C using the conditions specified under “Apparatus”, and using ch
35、loroform in the reference cell. Carry out simultaneously a blank determination on the reagents. Follow the same procedure without the sample and use the same quantity of reagents. 1) Whatman No. 41 is suitable. Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:38 GMT+00:00 2006, Uncontrol
36、led Copy, (c) BSI BS 3338-5:1961 2 BSI 11-1999 Deduct the blank reading and calculate the percentage lead in the sample by reference to the appropriate calibration graph. Calibration Transfer to 50-ml beakers the following amounts of standard lead solution (1 ml N 0.01 mg Pb): for the 4 cm cell 0.5,
37、 1.0, 1.5, 2.0 ml for the 1 cm cell 2.0, 4.0, 6.0, 8.0 ml. Dilute to 10 ml, add 1 ml of hydroxyammonium chloride solution (10 per cent) and 2 ml sodium tartrate solution (20 per cent) and continue as in the procedure. Carry out simultaneously a blank, using the same quantities of reagents. Prepare c
38、alibration graphs by plotting optical density against weight of lead in the various aliquots, after deduction of the blank reading. NOTE 1A 4 cm cell should be used for lead contents up to 0.08 per cent and a 1 cm cell for lead contents up to 0.9 per cent. NOTE 2For lead contents between 0.3 and 0.6
39、 per cent a 5 ml aliquot should be taken, and for lead contents between 0.6 and 1.0 per cent a 2 ml aliquot. All aliquots should be diluted to 10 ml with water. Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:38 GMT+00:00 2006, Uncontrolled Copy, (c) BSI blank Licensed Copy: sheffieldun
40、 sheffieldun, na, Wed Nov 29 07:54:38 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-5: 1961 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Europe
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