1、BRITISH STANDARD BS3908-13: 1970 Method for The determination of antimony in lead and lead alloys (lowcontents) (photometric method)BS3908-13:1970 This British Standard, having been approved by the Non-ferrousMetals Industry Standards Committee, was published under the authority ofthe Executive Boar
2、d on 30 January1970 BSI11-1999 The following BSI references relate to the work on this standard: Committee references NFE/22, NFE/22/6 Draft for comment68/21413 ISBN 580 05656 2 Co-operating organizations The Non-ferrous Metals Industry Standards Committee, under whose supervision this British Stand
3、ard 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 Founders Institution of Production Engineers Association of Consulting Engin
4、eers Institution of Structural Engineers Board of Trade Lead Development Association* British Bronze and Brass Ingot Manufacturers Light Metal Founders Association Association London Metal Exchange British Lead Manufacturers Association* Magnesium Industry Council British Non-ferrous Metals Federati
5、on* Ministry of Defence, Army Department British Non-ferrous Metals Research Ministry of Defence, Navy Department* Association* National Brassfoundry Association Copper Development Association Non-ferrous Metal Stockists Crown Agents for Oversea Governments and Post Office* Administrations Royal Ins
6、titute of British Architects Electric Cable Makers Confederation* Society of Motor Manufacturers and Traders High Conductivity Copper Group Ltd. Institute of British Foundrymen Tin Research Institute Institute of Metals Zinc Development Association Institution of Mechanical Engineers Individual manu
7、facturers (Automobile Division) The Government department 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: Accumulator Makers Associa
8、tion Ministry of Defence British Battery Makers Society Solder Makers Association Chemical Industries Association United Kingdom Atomic Energy Authority London Transport Board Amendments issued since publication Amd. No. Date CommentsBS3908-13:1970 BSI 11-1999 i Contents Page Co-operating organizati
9、ons Inside front cover Foreword ii 1 Introduction 1 2 Apparatus 1 3 Solutions required 1 4 Sampling 1 5 Procedure 1 6 Calibration 2 7 Notes 2BS3908-13:1970 ii BSI 11-1999 Foreword This standard makes reference to the following British Standards: BS3908, Method for the sampling and analysis of lead a
10、nd lead alloys Part1:Sampling of ingot lead, lead alloy ingots, sheet, pipe and cable sheathing alloys. BS3978, Water for laboratory use. This method for the determination of small amounts of antimony in lead and lead alloys is the thirteenth of a series of methods which will form a complete British
11、 Standard under the collective title “Methods for the sampling and analysis of lead and lead alloys” each method being published as a separate part. 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
12、 the standardization of methods for the sampling and analysis of non-ferrous metals. Other methods in the series are as follows: Part1: Sampling of ingot lead, lead alloy ingots, sheet, pipe and cable sheathing alloys; Part2: Determination of arsenic in lead and lead alloys (photometricmethod); Part
13、3: Determination of bismuth in lead and lead alloys (photometricmethod); Part4: Determination of copper in lead and lead alloys (photometricmethod); Part5: Determination of nickel in lead and lead alloys (photometric method); Part6: Determination of tellurium in lead and lead alloys (photometricmeth
14、od) 1) ; Part7: Determination of silver in lead and lead alloys 1) ; Part8: Determination of cadmium in lead and lead alloys 1) ; Part9: Determination of sulphur in lead and lead alloys 1) ; Part10: Determination of antimony in lead and lead alloys (volumetricmethod); Part11: Determination of tin in
15、 lead and lead alloys (volumetric method); Part12: Determination of zinc in lead and lead alloys 1) ; Part14: Determination of tin in lead and lead alloys (low contents) (photometric-quercetin method) 1) ; Part15: Determination of iron in lead and lead alloys (photometricmethod) 1) . The complete Br
16、itish Standard methods will be found suitable for the grades of metals covered by BS334 “Chemical lead”, BS335 “Regulus metal”, BS602 and BS1085 “Lead pipes for other than chemical purposes”, BS801 “Lead and lead alloy sheaths of electric cable”, BS1178 “Milled lead sheet and strip for building purp
17、oses” and BS3909 “Ingot lead for radiation shielding”. 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 realized that they are put forward as “referee” methods to be used in cases of dispute. 1) In course
18、of preparation.BS3908-13:1970 BSI 11-1999 iii 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 obligati
19、ons. Summary of pages This document comprises a front cover, an inside front cover, pagesi to iv, pages1and 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 inside front cover.iv bla
20、nkBS3908-13:1970 BSI 11-1999 1 1 Introduction 1.1 Principle. The sample is dissolved in a mixture of acetic acid and hydrogen peroxide, hydrochloric acid is added and the pentavalent antimony chloride extracted into isopropyl ether. Rhodamine “B” is added and the determination is completed photometr
21、ically. 1.2 Range. From0.002to0.05% antimony. 1.3 Reproducibility. Experiments have been carried 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. 2 Apparatus 2.1 Any volumetric
22、glassware used shall be of ClassA accuracy as defined in the appropriate British Standards, or where no British Standards exists, as described in the National Physical Laboratory Publication “Volumetric tests on volumetric glassware”. 2.2 Any instrument suitable for measuring the optical density of
23、the solution at a wavelength of550nm may be used together with a2 or4cm cell. Alternatively when a filter photometer of the balanced two photo cell type is used the following conditions have been found suitable: 3 Solutions required All reagents shall be of the highest purity obtainable and distille
24、d or demineralised water complying with BS3978 2)shall be used throughout. Solutions shall be freshly prepared and where necessary filtered. Standard antimony (1mlN 0.0025mg of antimony). Dissolve0.15g of high-purity antimony trioxide in hydrochloric acid (sp.gr.1.161.18). Cool, transfer to a1litre
25、volumetric flask, dilute to the mark with hydrochloric acid (sp.gr.1.161.18) and mix. Transfer20ml of this solution to a1litre volumetric flask, dilute to the mark with hydrochloric acid (sp.gr.1.161.18) and mix. Hydrobromic acid (12% v/v). Dilute120ml of hydrobromic acid (sp.gr.1.461.49) to1litre a
26、nd mix. Hydrochloric acid (70% v/v). Dilute700ml of hydrochloric acid (sp.gr.1.161.18) to1litre and mix. Hydrogen peroxide-acetic acid. To10ml of glacial acetic acid add20ml of water and15ml of hydrogen peroxide(100vol.) and mix. Rhodamine “B”(0.01% w/v). Dissolve0.1g of Rhodamine “B” in water, tran
27、sfer to a1litre volumetric flask containing47ml of hydrochloric acid (sp.gr.1.161.18), dilute to the mark and mix. 4 Sampling Recommended methods of obtaining a suitable sample for the analytical procedure given below are described in BS3908-1, “Sampling of ingot lead, lead alloy ingots, sheet, pipe
28、 and cable sheathing alloys.” 5 Procedure 5.1 For alloys not containing thallium 5.1.1 Weigh0.25g of sample, transfer to a50ml beaker and add1ml of hydrogen peroxide-acetic acid. 5.1.2 Add20ml of hydrochloric acid (sp.gr.1.161.18) and swirl until the lead chloride has dissolved. (Note7.1.) 5.1.3 Tra
29、nsfer to a100ml separating funnel. Rinse the beaker with a further15ml of hydrochloric acid (sp.gr.1.161.18) (Note7.2) and transfer the washings to the separating funnel. 5.1.4 Add25.0ml of di-isopropyl ether (Note7.3) and shake for30 seconds carefully releasing the pressure during this stage. Add15
30、ml of water (Note7.2), mix immediately and shake for a further30seconds. 5.1.5 Allow the layers to separate, discard the lower (aqueous) layer and wash the ether layer with15ml of hydrochloric acid(70%) (Note7.2) again shaking for30seconds. Allow the layers to separate and discard the lower (aqueous
31、) layer. Antimony content Standard deviation s % 0.005 0.01 % 0.0005 0.001 Either Tungsten lamp Ilford605 filter with Calorex H503 heat filter or equivalent filters 2or4cm cell or Mercury vapour lamp Ilford605 or Kodak74 filter with Calorex H503 heat filter or equivalent filters 2or4cm cell. 2) BS39
32、78, “Water for laboratory use.”BS3908-13:1970 2 BSI 11-1999 5.1.6 Add50ml of Rhodamine “B” solution(0.01%) and shake for1minute. Discard the lower (aqueous) layer and filter the ether layer into a small beaker through a dry filter paper to remove droplets of water. 5.1.7 Measure the optical density
33、of the solution against isopropyl ether using the conditions specified under2, Apparatus (Note7.4). 5.1.8 Carry out simultaneously a blank determination on the reagents following the same procedure without the sample and using the same quantity of reagents. 5.1.9 Deduct the blank reading and calcula
34、te the percentage antimony in the sample by reference to the calibration graph. 5.2 For alloys containing thallium 5.2.1 Follow the procedure set out in5.1 which determines antimony plus thallium. 5.2.2 To correct for the thallium weigh0.25g of sample, transfer to a50ml beaker and add1ml of hydrogen
35、 peroxide-acetic acid. 5.2.3 Add30ml of hydrobromic acid(12%) and swirl. Filter off the lead bromide formed through a dry filter paper 3)collecting the filtrate in a100ml separating funnel. Rinse the beaker with a further20ml of hydrobromic acid(12%) (Note7.2) and transfer the washings to the separa
36、ting funnel (Note7.5). 5.2.4 Add25.0ml of di-isopropyl ether (Note7.3) and shake for30seconds. 5.2.5 Allow the layers to separate, discard the lower (aqueous) layer and wash the ether layer with15ml of hydrobromic acid(12%) (Note7.2) again shaking for30seconds. Allow the layers to separate and disca
37、rd the lower (aqueous) layer. 5.2.6 Add50ml of Rhodamine “B” solution(0.01%) and shake for1minute. Discard the lower (aqueous) layer and filter the ether layer into a small beaker through a dry filter paper to remove droplets of water. 5.2.7 Measure the optical density of the solution against isopro
38、pyl ether using the conditions specified under2, Apparatus (Note7.4). 5.2.8 Carry out simultaneously a blank determination on the reagents following the same procedure without the sample and using the same quantity of reagents. 5.2.9 Deduct the blank reading, then subtract this corrected optical den
39、sity reading (due to thallium) from the optical density reading (corrected for blank) obtained in5.2.1 (due to thallium plus antimony). Calculate the percentage antimony in the sample by reference to the calibration graph. 6 Calibration 6.1 Transfer0,1.0,2.0,3.0,4.0 and5.0ml of standard antimony sol
40、ution(1mlN 0.0025mg of antimony) to a series of50ml beakers. Add to each0.25g of pure lead then continue as in procedure5.1. 6.2 Measure the optical density using the conditions specified under2, Apparatus and prepare a calibration graph by plotting the optical density after deduction of the blank r
41、eading against the weight of antimony in the various aliquots (Note7.4). 7 Notes 7.1 For antimony contents greater than0.005% transfer this solution to a100ml volumetric flask, dilute to the mark with hydrochloric acid (sp.gr.1.161.18) and mix. Transfer a suitable aliquot to the separating funnel, d
42、ilute to35ml with hydrochloric acid (sp.gr.1.161.18) and continue from5.1.4 of the procedure. 7.2 It is essential to adhere closely to the specified volumes of acid and water in order to obtain virtually complete extraction or the antimony into the ether layer. 7.3 It is essential that the di-isopro
43、pyl ether used should be either unstabilized or re-distilled. 7.4 The Antimony-Rhodamine “B” complex in isopropyl ether is relatively stable, fading only by about1% in1hour, but care should be taken to avoid changes of concentration due to solvent evaporation. However, the coloured complex is readil
44、y bleached by ammonia vapour. 7.5 For antimony contents greater than0.005% transfer this solution to a100ml volumetric flask, dilute to the mark with hydrobromic acid(12%) and mix. Transfer to the separating funnel, an aliquot of the same size as that taken in Note7.1, dilute to50ml with hydrobromic
45、 acid(12%) and continue from5.2.4. of the procedure. 3) Whatman No.540 is suitable.blankBS3908-13: 1970 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 Eur
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