1、BRITISH STANDARD BS3630-16: 1976 Methods for The sampling and analysis of zinc and zinc alloys Part16: Nickel in zinc alloys (photometric method) UDC 669.55:543.4:546.74BS3630-16:1976 This BritishStandard, having been approved by the Non-ferrous Metals Industry Standards Committee, was published und
2、er the authority ofthe Executive Board on 31March1976 BSI12-1999 The following BSI references relate to the work on this standard: Committee reference NFE/8 and NFE/8/4 Draft for comment74/40467 DC ISBN 0 580 08885 5 Co-operating organizations The Non-ferrous Metals Industry Standards Committee, und
3、er whose supervision this BritishStandard was prepared, consists of representatives from the following Government departments and scientific and industrial organizations: Aluminium Federation Association of Bronze and Brass Founders British Electrical and Allied Manufacturers Association British Lea
4、d Manufacturers Association British Non-ferrous Metals Federation* British Non-Ferrous Metals Technology Centre* British Steel Industry* Copper Development Association Department of Trade Electric Cable Makers Confederation Institute of British Foundrymen Institution of Mechanical Engineers Institut
5、ion of Mining and Metallurgy Institution of Production Engineers Institution of Structural Engineers Lead Development Association Light Metal Founders Association London Metal Exchange* Magnesium Industry Council Ministry of Defence* National Brassfoundry Association Non-ferrous Metal Stockists Post
6、 Office* Royal Institute of British Architects Society of Motor Manufacturers and Traders Ltd.* Tin Research Institute Zinc Development Association* Individual manufacturer The organizations marked with an asterisk in the above list, together with the following, were directly represented on the comm
7、ittees entrusted with the preparation of this BritishStandard: British Steel Industry Wire Section Department of Industry Laboratory of the Government Chemist Imperial Smelting Corporation Institute of Sheet Metal Engineering The Metals Society Zinc Alloy Die Castors Association Individual analysts
8、Amendments issued since publication Amd. No. Date of issue CommentsBS3630-16:1976 BSI 12-1999 i Contents Page Co-operating organizations 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 2 Publications referred to
9、Inside back coverBS3630-16:1976 ii BSI 12-1999 Foreword This method for the determination of nickel in ingot zinc and zinc alloys is the sixteenth of a series of methods which will form a complete BritishStandard under the collective title “Methods for the sampling and analysis of zinc and zinc allo
10、ys”, 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 the standardisation of methods for the sampling and analysis of non-ferrous metals. Other metho
11、ds in the series are as follows: Part1: Sampling of ingot zinc and zinc alloy ingots; Part2: Determination of tin in ingot zinc and zinc alloys (photometricmethod); Part3: Determination of magnesium in zinc alloys (gravimetric method); Part4: Sampling of ingot zinc, zinc alloy ingots and zinc alloy
12、die castings for spectrographic analysis; Part5: Determination of iron in ingot zinc and zinc alloys (photometricmethod); Part6: Determination of aluminium in zinc alloys (volumetric method); Part7: Determination of lead in zinc (grades Zn3 and Zn4) (polarographicmethod); Part8: Determination of lea
13、d and cadmium in zinc (grades Zn1 and Zn2) and zinc alloys (polarographic method); Part9: Determination of copper in ingot zinc and zinc Alloy A (photometricmethod); Part10: Determination of thallium in ingot zinc and zinc alloys (photometricmethod); Part11: Determination of indium in ingot zinc and
14、 zinc alloys (polarographic method); Part12: Determination of arsenic in ingot zinc and zinc alloys (photometricmethod); Part13: Determination of copper in zinc alloys (Alloy B) (electrolyticmethod); Part14: Determination of cadmium in zinc (grades Zn3 and Zn4) (polarographic method); Part15: Determ
15、ination of magnesium in zinc alloys (atomic absorption method). The complete BritishStandard methods will be found suitable for the grades of metals covered by BS3436 “Ingot zinc” and BS1004 “Zinc alloys for die casting and zinc alloy die castings”. In the methods for determining impurities, sample
16、weights and aliquots have been chosen to cover the range of impurity content usually found in commercial zinc ingots and zinc 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 reproduc
17、ible 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. NOTEThe titles of the BritishStandards referred to in this standard are listed on the inside back cover.BS3630-16:1976 BSI 12-
18、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 obligations. Summary of pages This document c
19、omprises a front cover, an inside front cover, pagesi to iv, pages1and 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 front cover.iv blankBS3630-16:197
20、6 BSI 12-1999 1 1 Introduction 1.1 Principle. The sample is dissolved in hydrochloric acid. The dimethylglyoxime complex of the nickel is formed in ammoniacal citrate solution and the complex is extracted into chloroform. Nickel is re-extracted into dilute hydrochloric acid solution and after oxidat
21、ion with bromine water the solution is made ammoniacal and dimethylglyoxime is added. The determination is completed photometrically. 1.2 Range. From0.0005 to0.0075% nickel (Note7.1). 1.3 Reproducibility. Experiments have been carried out independently by a number of analysts using the method recomm
22、ended in this standard. The degree of reproducibility that can be expected is shown by the following analysis of the results obtained: 2 Apparatus 2.1 Any volumetric glassware used shall be of ClassA accuracy as defined in the appropriate BritishStandard. 2.2 Any instrument suitable for measuring th
23、e optical density of the solution at a wavelength of445nm may be used together with a2cm cell. Alternatively, if a filter photometer of the balanced two-cell type is used the following conditions have been found suitable: Mercury vapour lamp Ilford601 or equivalent filter 2cm cell. 3 Solutions requi
24、red All reagents shall be of the highest purity obtainable and distilled or demineralized water complying with the requirements of BS3978 shall be used throughout. Solutions shall be freshly prepared, and where necessary, filtered. Standard nickel (1mlN 0.005mg of nickel). Dissolve0.2500g of high pu
25、rity nickel in25ml of hydrochloric acid (sp.gr.1.161.18). Cool, add35ml of hydrochloric acid (sp.gr.1.161.18), transfer to a500ml volumetric flask, dilute to the mark and mix. Transfer10ml of this solution to a1litre volumetric flask, dilute to the mark and mix. Ammonia (2%v/v). Dilute20ml of ammoni
26、a solution (sp.gr.0.880.91) to1litre and mix. Bromine water (saturated). To100ml of water add5ml of bromine, shake and allow to stand until saturated. Citric acid (30%w/v). Dissolve300g of citric acid (H 8 C 6 O 7 .H 2 O) in water, dilute to1litre and mix. Dimethylglyoxime (1%w/v alcoholic). Dissolv
27、e10g of dimethylglyoxime in nearly1litre of warm industrial methylated spirit 1) . Cool, dilute to1litre with spirit and mix. Hydrochloric acid (5%v/v). Dilute50ml of hydrochloric acid (sp.gr.1.161.18) to1litre and mix. Hydroxylammonium chloride (10%w/v). Dissolve10g of hydroxylammonium chloride in
28、water, dilute to100ml and mix. Sulphurous acid. Pass sulphur dioxide gas into1litre of water until a saturated solution is obtained. Bromothymol blue (0.1%w/v). Dissolve0.1g of bromothymol blue in5ml of ethanol, dilute to100ml with water and mix. 4 Sampling Recommended methods of obtaining a suitabl
29、e sample for the analytical procedure given below are described in BS3630-1 “Sampling of ingot zinc and zinc alloy ingots”. 5 Procedure 5.1 Weigh5g of sample and transfer to a250ml conical beaker. Add25ml of hydrochloric acid (sp.gr.1.161.18) and when the reaction has subsided add several drops of h
30、ydrogen peroxide(100vol) to complete the solution. Boil for5 to10minutes with the beaker covered. Add5ml of sulphurous acid and boil for5minutes. Cool, transfer to a50ml volumetric flask, dilute to the mark and mix. Nickel content Reproducibility index 2s % 0.001 0.006 0.0003 0.0008 1) It should be
31、noted that the use of industrial methylated spirit is governed by the Methylated Spirits Regulations1952 (S.I.1952 No.2230).BS3630-16:1976 2 BSI 12-1999 5.2 Carry out simultaneously a blank determination on the reagents. Follow the same procedure but omitting the sample. 5.3 Transfer by means of a p
32、ipette10ml of the sample solution to a100ml separating funnel. 5.4 Add the following reagents mixing after each addition: 20ml of citric acid solution(30%). 10ml of hydroxylammonium chloride solution(10%). 10drops of bromothymol blue indicator. 5.5 Add from a burette ammonia solution (sp.gr.0.880.91
33、) with swirling until the indicator changes from yellow to blue and then add1ml in excess (Note7.2). Cool to room temperature. 5.6 Add2ml of dimethylglyoxime solution(1%alcoholic) and mix. 5.7 Add10ml of chloroform and shake for45seconds. Allow the layers to separate and transfer the lower chlorofor
34、m layer to a second separating funnel. Repeat the extraction with a further10ml of chloroform and combine the two chloroform layers in the second separating funnel. Discard the aqueous layer. 5.8 Add10ml of ammonia solution(2%) and shake for1minute. Transfer the lower chloroform layer to another sep
35、arating funnel and repeat the extraction with a further10ml of ammonia solution(2%). (Note7.3). Discard the ammonia washings. 5.9 Extract the chloroform solution twice with10ml of hydrochloric acid(5%) each time shaking for1minute. Combine the two acid extracts in a50ml volumetric flask. 5.10 Add2ml
36、 of bromine water (saturated), swirl and allow to stand for15minutes. 5.11 Add dropwise, with swirling, ammonia solution (sp.gr.0.880.91) until the solution is decolorized and add2ml in excess. Cool to below30 C. 5.12 Add2ml of dimethylglyoxime solution(1%alcoholic), dilute to the mark and mix. 5.13
37、 Allow the solution to stand for10minutes and then measure the optical density within the next45minutes using the conditions specified under2 “Apparatus”, and water as reference solution. 6 Calibration 6.1 To a series of separating funnels, transfer respectively 0,1,2,6,10 and15ml of standard nickel
38、 solution(1mlN 0.005mg of nickel). Dilute to15ml and mix. 6.2 Continue from5.4 of the procedure. 6.3 Measure the optical density using the conditions specified under2. Apparatus and prepare a calibration graph by plotting the optical density against the equivalent percentage of nickel. 7 Notes 7.1 T
39、he range can be extended by taking a suitable smaller aliquot for extraction. 7.2 The suitable range of pH is810. If considerable copper is present the blue colour may mask the indicator change. Under these circumstances a pH meter should be used. 7.3 Washing with ammonia solution is necessary to re
40、move copper which seriously affects the stability of the nickel-dimethylglyoxime complex.BS3630-16:1976 BSI 12-1999 Publications referred to This standard make reference to the following BritishStandards: BS3630, Methods for the sampling and analysis of zinc and zinc alloys. BS3630-1, Sampling of in
41、got zinc and zinc alloy ingots. BS3978, Water for laboratory use. BS3630-16: 1976 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 interna
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