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1、BRITISH STANDARD BS 3338-21: 1983 Methods for the sampling and analysis of tin and tin alloys Part 21: Determination of high cadmium content of soft solders UDC 669.654:543.24:546.48 Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:55 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-21
2、:1983 This British Standard, having been prepared under the direction of the Non-ferrous Metals Standards Committee, was published under the authority of the Board of BSI and comes into effect on 31 October 1983 BSI 12-1999 The following BSI references relate to the work on this standard: Committee
3、reference NFE/27 Draft for comment 82/76769 DC ISBN 0 580 134334 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Non-ferrous Metals Standards Committee (NFE/-) to Technical Committee NFE/27 upon which the following bodies were represente
4、d: Association of British Pewter Craftsmen British Steel Industry Electric Cable Makers Confederation Electronic Engineering Association Federation of Wire Rope Manufacturers of Great Britain International Tin Research Institute London Metal Exchange Metal Packaging Manufacturers Association Nationa
5、l Coal Board Solder Makers Association Coopted members The following bodies were also represented in the drafting of the standard, through subcommittees and panels: British Association for Brazing and Soldering BNF Metals Technology Centre British Telecom Ministry of Defence Telecommunication Engine
6、ering and Manufacturing Association (TEMA) Amendments issued since publication Amd. No.Date of issueComments Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:55 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-21:1983 BSI 12-1999i Contents Page Committees responsibleInside front cover
7、Forewordii 1Scope1 2Reagents1 3Apparatus1 4Sampling1 5Analysis procedure1 6Standardization of EDTA2 Publications referred toInside back cover Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:55 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-21:1983 ii BSI 12-1999 Foreword This Part o
8、f this British Standard has been prepared under the direction of the Non-ferrous Metals Standards Committee. It is an additional Part of a series describing methods for the sampling and analysis of tin and tin alloys. Other Parts of the series are as follows: Part 1: Sampling of ingot tin; Part 2: D
9、etermination of tin in ingot tin (aluminium reduction method); Part 3: Determination of antimony in ingot tin (photometric method); Part 4: Determination of copper in ingot tin and tin-lead solders (photometric method); Part 5: Determination of lead in ingot tin and tin-antimony solders (photometric
10、 method); Part 6: Determination of copper in high purity ingot tin (photometric method); Part 7: Determination of silver in solders (volumetric: ammonium thiocyanate method); Part 8: Determination of bismuth in ingot tin, tin-lead solders and white metal bearing alloys (photometric method); Part 9:
11、Determination of arsenic in ingot tin, solders and white metal bearing alloys (photometric method); Part 10: Determination of iron in ingot tin, tin-lead solders and white metal bearing alloys (photometric method); Part 11: Determination of tin in solders (nickel coil reduction method); Part 12: Sam
12、pling of solders; Part 13: Determination of antimony in solders and white metal bearing alloys (volumetric: potassium bromate method); Part 14: Sampling of white metal bearing alloy ingots; Part 15: Determination of copper and lead in white metal bearing alloys (electrodeposition method); Part 16: D
13、etermination of tin in white metal bearing alloys (nickel coil reduction method); Part 17: Determination of cadmium in solders and white metal bearing alloys (photometric method); Part 18: Determination of aluminium in solders and white metal bearing alloys (photometric method); Part 19: Determinati
14、on of zinc in solders and white metal bearing alloys (photometric method); Part 20: Determination of nickel in capping metal (photometric method). The complete series is judged suitable for the analysis of tin and tin-base alloys covered by BS 219, BS 3252, BS 3332 and BS 5140. In the methods for de
15、termining impurities, sample masses and aliquots have been chosen to cover the range of impurity content usually found in commercial tin ingots, solders and white metal bearing alloy ingots. While it is appreciated that other convenient and rapid methods are more than adequate for normal routine com
16、mercial requirements, all the methods described have been found to give reliable and reproducible results and are therefore intended primarily as referee procedures to be used in cases of dispute. Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:55 GMT+00:00 2006, Uncontrolled Copy, (c)
17、BSI BS 3338-21:1983 BSI 12-1999iii 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. Summar
18、y of pages This document comprises a front cover, an inside front cover, pages i to iv, pages 1 and 2, an inside back cover 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 fron
19、t cover. Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:55 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv blank Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:55 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-21:1983 BSI 12-19991 1 Scope This Part of this British Stand
20、ard describes a method for the determination of cadmium in tin base soft solder alloys containing 10 % to 30 % of cadmium and with reproducibility of 0.15 % of the cadmium present. NOTEThe titles of the publications referred to in this standard are listed on the inside back cover. 2 Reagents During
21、the analysis use only reagents of the highest purity obtainable, and of analytical reagent quality. Use water complying with BS 3978 throughout and solutions which are freshly prepared and, where necessary, filtered. 2.1 Ammonia solution. Dilute 50 mL of ammonia solution, approximately 0.88 g/mL, to
22、 100 mL with water. 2.2 Bromine-hydrobromic acid solution. Carefully add 10 mL bromine to 90 mL of hydrobromic acid, 1.46 g/mL to 1.49 g/mL. 2.3 Buffer solution. Dissolve 54 g of ammonium chloride in 650 mL water and add 350 mL ammonia solution, approximately 0.88 g/mL. 2.4 Ethylenediamine tetra-ace
23、tic acid solution (EDTA) (0.05 mol/L). Dissolve 18.61 g of the disodium salt of EDTA in 1 L of water and standardize against cadmium as described in clause 6. 2.5 Eriochrome black T solution (EBT) (0.5 % m/V). Dissolve 0.5 g of EBT and 4.5 g of hydroxylamine hydrochloride in 90 mL of water containin
24、g 10 mL triethanolamine. 2.6 Nitric acid solution (approximately 7 mol/L). Dilute 50 mL of nitric acid solution, approximately 1.42 g/mL, to 100 mL with water. 2.7 Nitric acid solution (approximately 0.3 mol/L). Dilute 20 mL of nitric acid, approximately 1.42 g/mL, to 1 L with water. 2.8 Sulphuric a
25、cid solution (approximately 9 mol/L). Carefully add 50 mL of sulphuric acid, approximately 1.84 g/mL, to 55 mL of water, mixing and cooling if necessary. 2.9 Sulphuric acid solution (approximately 0.02 mol/L). Dilute 2 mL of sulphuric acid solution (2.8) to 1 L with water. 2.10 Hydrochloric acid (ap
26、proximately 2 mol/L). Dilute 180 mL of hydrochloric acid, approximately 1.18, to 1 L with water. 2.11 Hydrochloric acid (approximately 0.6 mol/L). Dilute 50 mL of hydrochloric acid, approximately 1.18, to 1 L with water. 3 Apparatus 3.1 All glassware used for volumetric measurement of solutions shal
27、l be of class A accuracy as described in BS 700-1, BS 846, BS 1583 and BS 1792. 3.2 A cation exchange column shall be constructed of glass tube 16 mm internal diameter and approximately 400 mm long, and fitted with a tap. It shall be filled to a depth of 350 mm with cation resin1) prepared in the fo
28、llowing manner. Stir approximately 50 g of the resin with the hydrochloric acid (2.10) and then allow it to settle. Decant the fine particles and fill the column to the required depth. Elute the column with 400 mL of distilled or demineralized water at the rate of 3 mL/min to 4 mL/min. 4 Sampling Th
29、e sample for analysis shall be taken by one of the suitable procedures described in BS 3338-12. 5 Analysis procedure 5.1 Weigh accurately 0.6 g of the sample and transfer to a 250 mL conical beaker. Add 20 mL of the bromine-hydrobromic acid solution (2.2) and evaporate to dryness, cool and add a fur
30、ther 10 mL of the bromine-hydrobromic acid solution and evaporate to dryness again. Cool, add 10 mL of the nitric acid solution (2.6) and 10 mL of water, and heat to dissolve the salts. Cool, add 2 mL of the sulphuric acid solution (2.8) evaporate to fumes and heat strongly. Cool, add 50 mL of water
31、, boil and allow to stand at room temperature for a minimum period of 1 h. 5.2 Filter, either through a sintered glass crucible of porosity No. 4 (see BS 1752), or through a suitable filter paper2) and wash with the sulphuric acid solution (2.9). 5.3 Pass the filtrate through the cation exchange col
32、umn and wash with 150 mL of water, discarding the effluent. Elute the cadmium by passing 700 mL of the hydrochloric acid (2.11) through the resin. When the first 50 mL of eluate has been collected, stop the flow for 15 min and then continue the elution at the rate of 3 mL/min to 4 mL/min. 1) Zeolit
33、225 SRC 14 is known to be suitable. 2) A Whatman No. 40 filter paper is known to be suitable. Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:55 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-21:1983 2 BSI 12-1999 5.4 Evaporate the total eluted solution to dryness, cool, add 10 mL o
34、f the nitric acid (2.7) and dilute to 100 mL with water. 5.5 Neutralize the solution with the ammonia solution (2.1) using methyl red as indicator. Add 10 mL of the buffer solution (2.3) and sufficient EBT solution (2.5) to produce a colour, titrate with EDTA solution (2.4) and note the volume (V1)
35、required to change the indicator colour from red to blue. 5.6 Calculate the value C of the cadmium content of the alloy, as a percentage, from the equation: 6 Standardization of EDTA 6.1 Weigh accurately (in quadruplicate) between 0.1 g and 0.15 g of pure cadmium metal into 250 mL beakers, dissolve
36、in 10 mL of nitric acid solution (2.6), evaporate to dryness and add 10 mL of nitric acid solution (2.7). 6.2 Cool, dilute to 100 mL with water, and then follow that part of the analysis procedure described in 5.5. 6.3 The mean value of the four titrations V2 (in mL) shall be taken as the standard v
37、alue. 6.4 Calculate the value of the factor F from the equation: where V1is the titration volume of the EDTA solution (in mL); Fis the factor obtained by the procedure described in clause 6; M1is the mass of sample (in g). C V1F M1 - -100= where M2is the mass of cadmium metal used (in g); V2is the m
38、ean value of the four titrations (in mL). F M2 V2 - -= Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:55 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-21:1983 BSI 12-1999 Publications referred to BS 219, Specification for soft solders. BS 700, Graduated pipettes. BS 700-1, Specifi
39、cation for general requirements. BS 846, Specification for burettes. BS 1583, One-mark pipettes. BS 1752, Laboratory sintered or fritted filters. BS 1792, Specification for one-mark volumetric flasks. BS 3252, Ingot tin. BS 3332, White metal bearing alloy ingots. BS 3338, Methods for the sampling an
40、d analysis of tin and tin alloys. BS 3338-12, Sampling of solders. BS 3978, Water for laboratory use. BS 5140, Pewter. Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:54:55 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3338-21: 1983 BSI 389 Chiswick High Road London W4 4AL BSI British Stan
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