BS 7317-4-1990 Methods for analysis of high purity copper cathode Cu-CATH-1 - Method for determination of antimony arsenic bismuth lead selenium tellurium and tin by electrothermal.pdf

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1、BRITISH STANDARD BS7317-4:1990Methods forAnalysis of high purity copper cathodeCu-CATH-1 Part 4: Method for determination of antimony, arsenic, bismuth, lead, selenium, tellurium and tin by electrothermal atomization atomic absorption spectrophotometryUDC 669.3.015.4:543.422.062546.19 + 546.23/.24 +

2、 546.81 + 546.86/.87BS7317-4:1990This BritishStandard, having been prepared under the directionof the Non-ferrous Metals Standards Policy Committee, was published underthe authority of theBoardofBSI and comesintoeffecton31July1990 BSI01-2000The following BSI references relate to the work on this sta

3、ndard:Committee reference NFM/34Draft for Development DD95-4ISBN 0 580 18463 3Committees responsible for this BritishStandardThe preparation of this BritishStandard was entrusted by the Non-ferrous Metals Standards Policy Committee (NFM/-) to Technical Committee NFM/34, upon which the following bodi

4、es were represented:British Bathroom CouncilBritish Cable Makers ConfederationBritish Gas plcBritish Malleable Tube Fittings AssociationBritish Non-ferrous Metals FederationBritish Valve and Actuator Manufacturers AssociationCopper Development AssociationLondon Metal ExchangeNon-ferrous Metal Stocki

5、stsSociety of British Aerospace Companies Ltd.Transmission and Distribution Association (BEAMA Ltd.)Coopted membersThe following bodies were also represented in the drafting of the standard, through sub-committees and panels:BNF Metals Technology CentreBritish Bronze and Brass Ingot Manufacturers As

6、sociationBureau of Analysed Samples Ltd.Copper Smelters and Refiners AssociationMinistry of DefenceAmendments issued since publicationAmd. No. Date of issue CommentsBS7317-4:1990 BSI 01-2000 iContentsPageCommittees responsible Inside front coverForeword ii1 Scope 12 Principle 13 Reagents 14 Apparatu

7、s 15 Procedure 26 Calculation and expression of results 37 Repeatability and reproducibility 48 Test report 4Table 1 Calibration solutions 2Table 2 Typical electrothermal atomization measurement conditions 3Table 3 Minimum sensitivity 3Table 4 Maximum mean differences for impurity elements 3Table 5

8、Repeatability of results 4Table 6 Reproducibility of results 5Publications referred to Inside back coverBS7317-4:1990ii BSI 01-2000ForewordBS7317 has been prepared under the direction of the Non-ferrous Metals Standards Policy Committee. It describes methods for the determination of impurity element

9、s in high purity copper cathode designated Cu-CATH-1, each method being published as a separate Part. The methods are based on those previously issued in the Draft for Development series DD95-1 to DD95-7. The information and experience gained from the practical application of DD95 have been taken in

10、to account in the methods in BS7317.This Part of BS7317 supersedes DD95-4:1986, which is withdrawn. It is one of a series of methods in BS7317, the others being as follows: Part1: Method for determination of cadmium, manganese and silver (screening procedure for chromium, cobalt, iron, nickel and zi

11、nc) by atomic absorption spectrophotometry; Part2: Method for determination of chromium, cobalt, iron, nickel and zinc by discrete volume nebulization atomic absorption spectrophotometry; Part3: Method for determination of antimony, arsenic, bismuth, selenium, tellurium and tin by hydride generation

12、 and atomic absorption spectrophotometry; Part5: Method for determination of sulphur by hydrogen sulphide evolution and spectrophotometry; Part6: Method for determination of phosphorus and silicon by spectrophotometry; Part7: Method for determination of lead by lanthanum hydroxide separation and ato

13、mic absorption spectrophotometry.The atomic absorption spectrophotometric procedures in Parts1 and2 are complementary. A sample solution concentration found to be satisfactory for nebulizers in standard atomic absorptiometers was20g/L. At this concentration the precision obtainable, using the method

14、 described in Part1, is only sufficient to allow the determination of cadmium, manganese and silver. Results would be obtained for chromium, cobalt, iron, nickel and zinc that would prove useful in detecting impurities grossly in excess of the requirements for chemical compositions specified in BS60

15、17 for Cu-CATH-1 and would give a guide to the levels to be determined by Part2.The discrete volume nebulization procedure in Part2 was developed to enable a higher equivalent sample solution concentration of100g/L to be used without nebulizer blockage. The method involves no chemical separation, wh

16、ich can give rise to contamination problems, and the extra sensitivity obtained enables the impurities to be determined to an adequate accuracy for the requirements for chemical composition specified in BS6017 for Cu-CATH-1.Parts1 and2 essentially cover the same impurities. Part4 covers the electrot

17、hermal atomization atomic absorption spectrophotometric method and is recommended where the facility is available. Parts1,2,3 and7 are included for use where the electrothermal atomization equipment is not available.A British Standard does not purport to include all the necessary provisions of a con

18、tract. 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 pagesThis document comprises a front cover, an inside front cover, pagesi andii, pages1 to6, an inside back cover an

19、d 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.BS7317-4:1990 BSI 01-2000 11 ScopeThis Part of BS7317 describes a method for the determination of the actual amounts of

20、 the impurity elements antimony, arsenic, bismuth, lead, selenium, tellurium and tin present in high purity copper cathode (designated Cu-CATH-1), by electrothermal atomization atomic absorption spectrophotometry. It is applicable to concentrations of the impurity elements not exceeding the followin

21、g limits. NOTEThe titles of the publications referred to in this Part of BS7317 are listed on the inside back cover.2 PrincipleTest solutions are prepared by dissolving the analysis sample in50%V/V nitric acid and diluting it to a standard volume. The impurity element is determined in aliquot portio

22、ns by atomic absorption spectrophotometry using electrothermal atomization techniques.3 Reagents3.1 GeneralDuring the analysis, use only reagents of recognized analytical quality or higher purity and only distilled water, deionized water, or water of equivalent purity that has no detectable levels o

23、f the particular elements to be determined.NOTEUnless otherwise stated, all solutions are aqueous solutions.3.2 Nitric acid, 1.42g/mL.3.3 Nitric acid, 1.42g/mL,50%V/V solution.3.4 Hydrofluoric acid, 1.13g/mL.3.5 Hydrochloric acid, 1.18g/mL.3.6 Hydrochloric acid, 1.18g/mL,50%V/V solution.3.7 Acetone3

24、.8 Copper1), a certified reference material of a minimum of99.999% copper, containing less than0.54g/g of each of the impurity elements.3.9 Copper solution containing approximately10.0g copper per100mL, prepared by the following method. Weigh10.0g of copper(3.8) into a500mL beaker. Wash the copper w

25、ith50mL of hydrochloric acid solution(3.6) and drain. Wash the copper with water, followed by acetone and dry using gentle heat. Add30mL of water,50mL of nitric acid(3.3) and allow the copper to dissolve, without heating. Cool. Transfer the solution to a100mL volumetric flask. Dilute to the mark and

26、 mix well.3.10 Primary calibration solutions, as given in3.10.1 to3.10.7. These are solutions containing1.0 0.0005g/L of the appropriate element.3.10.1 Antimony. Dissolve2.669g antimony potassium oxide tartrate K(SbO)C4H4O6 in water and dilute to1L with water.3.10.2 Arsenic. Dissolve4.165g sodium ar

27、senate (Na2HAsO4.7H2O) in water and dilute to1L with water.3.10.3 Bismuth. Dissolve1.000g bismuth in40mL of nitric acid solution(3.3) and dilute to1L with water.3.10.4 Lead. Dissolve1.000g lead in40mL of nitric acid solution(3.3) and dilute to1L with water.3.10.5 Selenium. Dissolve1.000g selenium in

28、40mL of nitric acid solution(3.3) and dilute to1L with water.3.10.6 Tellurium. Dissolve1.000g tellurium in40mL of nitric acid solution(3.3) and dilute to1L with water.3.10.7 Tin. Dissolve1.000g tin in40mL of nitric acid solution(3.3) and2mL of hydrofluoric acid(3.4) in a100mL plastics beaker. Dilute

29、 to about70mL, transfer to1L volumetric flask containing about500mL of water, dilute to the mark and mix well. Transfer into a1L plastics, stoppered container.NOTEThese solutions are stable for at least24hours.4 Apparatus4.1 Atomic absorption spectrophotometer, incorporating a 10scale expansion faci

30、lity, fitted with an electrothermal atomizer (e.g.graphite furnace), a strip chart or other recording system for peak measurement and electrodeless discharge (ED) and hollow cathode (HC) lamps.NOTEElectrodeless discharge tube equipment is essential for the determination of arsenic, selenium and tell

31、urium, but hollow cathode lamps may be adequate for the determination of antimony, bismuth, lead and tin.antimony arsenic lead6 4g/g(0.0006%m/m) maximum for each elementbismuth selenium tellurium3 4g/g(0.0003%m/m) maximum for each elementtin 204g/g(0.0020%m/m) maximum1) For information on the availa

32、bility of copper of suitable purity, apply to Enquiry Section, BSI, Linford Wood, Milton Keynes MK146LE, enclosing a stamped addressed envelope for reply.BS7317-4:19902 BSI 01-20004.2 Laboratory glasswareNOTEIt is recommended that new glassware, dedicated to this specific purpose, is used.4.3 Polyst

33、yrene or polycarbonate tubes, calibrated to contain10mL, such as are generally available for clinical use. Do not use polyolefine ware.5 Procedure5.1 GeneralScrupulously clean all glassware in aqua regia, i.e.1part of concentrated nitric acid(3.2) and3 parts of concentrated hydrochloric acid(3.5), f

34、or16h, and rinse with water immediately before use.5.2 Preparation of solutions5.2.1 Stock reference solutions. Prepare seven stock reference solutions (solutions5.2.1.1 to5.2.1.7) by the following method and use within24h to avoid deterioration.Into seven separate100mL volumetric flasks transfer, u

35、sing a micropipette,1004L of the bismuth(3.10.3), selenium(3.10.5) and tellurium(3.10.6) primary calibration solutions,2004L of the antimony(3.10.1), arsenic(3.10.2) and lead(3.10.4) primary calibration solutions and5004L of the tin(3.10.7) primary calibration solution. Dilute each solution to the m

36、ark with water and mix well.NOTEThe concentrations of the resulting stock reference solutions will be such that1mL is equivalent in each case to: These solutions have to be used as soon as possible and at latest within8h of preparation.5.2.2 Calibration solutions. Prepare five calibration solutions

37、(solutions5.2.2.1 to5.2.2.5) by the following method, and use them in the same period as that in which the test portions (see5.2.3) and the reagent blank (see5.2.4) are prepared and measured.Into five10mL calibrated tubes(4.3) add by pipette1mL of copper solution(3.9). Add to each container the amou

38、nts of each reference solution given in Table 1. Dilute to the mark and mix well.5.2.3 Test portions. Prepare three test portions (solutions5.2.3.1 to5.2.3.3) by the following method.Weigh three0.1g portions of the analysis sample (previously cleaned in hydrochloric acid solution and dried, as descr

39、ibed in3.9), and transfer them to three10mL calibrated tubes(4.3). Add1mL of nitric acid solution(3.3) to each and allow to dissolve without heating. Cool, dilute to the mark with water and mix well.NOTEWhere the sample is in a suitable homogeneous form the use of0.1g sample masses, diluted finally

40、to10mL has been found to be preferable in minimizing pick up and speed of dissolution. Other higher sample masses may be necessary because of the sampling method. These may be used with proportionately greater volumes of acid for dissolution and correspondingly greater final dilution.Do not use poly

41、olefin ware.5.2.4 Reagent blank. Transfer to a10mL calibrated tube(4.3)1mL of nitric acid solution(3.3) and1004L of copper solution(3.9). Dilute to the mark with water and mix well.NOTEThe addition of copper solution to the reagent blank is necessary to prevent loss of impurity elements in the “ash”

42、 stage of analysis.Table 1 Calibration solutionsbismuth (5.2.1.3)1 4gselenium (5.2.1.5)tellurium (5.2.1.6)antimony (5.2.1.1)2 4garsenic (5.2.1.2)lead (5.2.1.4)tin (5.2.1.7) 5 4gCalibration solutionAddition of stock reference solutions (5.2.1.1to5.2.1.7)Equivalent concentration for a0.1g sampleSeleni

43、um tellurium and bismuthArsenic antimony and leadTin5.2.2.15.2.2.25.2.2.35.2.2.45.2.2.54L0.01002003004004g/g0.001.002.003.004.004g/g0.002.004.006.008.004g/g0.005.0010.0015.0020.00NOTESolution5.2.2.1 is the calibration blank.BS7317-4:1990 BSI 01-2000 3Table 2 Typical electrothermal atomization measur

44、ement conditions5.3 Adjustment of apparatusAdjust the atomic absorption spectrophotometer in accordance with the recommendations of the instrument supplier. Use automatic background correction.5.4 Determinations5.4.1 Instrumental conditions. The optimum instrumental conditions will vary with the ins

45、truments used. Follow the manufacturers instructions for the drying time and temperature, the ashing time and temperature and the atomization temperature. Typical measurement conditions are given, for guidance, in Table 2.Follow the manufacturers instructions for the sample volume to be used.Whichev

46、er apparatus is used it is essential that the peak absorbance obtained for the impurity elements when measuring calibration solution5.2.2.2 is not less than those in Table 3. Table 3 Minimum sensitivity Table 4 Maximum mean differences for impurity elements5.4.2 Measurement. Measure the atomic absor

47、ption peaks, height or area, of each of the impurity elements three times for each of the calibration solutions(5.2.2.1 to5.2.2.5), three times for each of the test portions (5.2.3.1 to5.2.3.3) and three times for the reagent blank(5.2.4).6 Calculation and expression of results6.1 Calibration calcul

48、ationsFor each impurity element, calculate the arithmetic means of the three absorbance measurements for each of the calibration solutions(5.2.2.1 to5.2.2.5). Subtract the mean absorbance value for the calibration blank solution (5.2.2.1) from the mean absorbance values for each of the other calibra

49、tion solutions(5.2.2.2 to5.2.2.5) and use the resulting values to construct or calculate a calibration curve (mean absorbance plotted against calibration solution concentration) for each element, using a least squares (second order) fit.Impurity element WavelengthLamp Sample volumeDrying stage Ashing stage Atomizing temperatureHC ED Temperature Time Temperature TimeAntimonyArsenicBismuthLeadSeleniumTelluriumTinnm231.1193.7223.1283.3196.0214.3224.64L15101010151510C120120120120120120120s30202020303020C6004005004004005