ASTM E37-2005(2011) 8750 Standard Test Methods for Chemical Analysis of Pig Lead《铅锭化学分析的标准试验方法》.pdf

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1、Designation: E37 05 (Reapproved 2011)Standard Test Methods forChemical Analysis of Pig Lead1This standard is issued under the fixed designation E37; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the year of last revision. A numbe

2、r in parentheses indicates the year of last reapproval. A superscriptepsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods cover the chemical analysis of piglead having chemical compositions within the following limits:Element Concentration Ran

3、ge, %Antimony 0.001 to 0.02Arsenic 0.0005 to 0.02Bismuth 0.002 to 0.2Copper 0.001 to 0.1Iron 0.0005 to 0.005Lead 99.5 to 99.99Silver 0.001 to 0.03Tin 0.001 to 0.02Zinc 0.001 to 0.0051.2 The test methods appear in the following order:SectionsAntimony by the Rhodamine-B Photometric Method 21-30Copper,

4、 Bismuth, Silver, and Zinc by the Atomic AbsorptionMethod10-201.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is th

5、eresponsibility of the user of this standard to consult andestablish appropriate safety and health practices and deter-mine the applicability of regulatory limitations prior to use.Specific precautionary statements are given in the individualtest methods.2. Referenced Documents2.1 ASTM Standards:2B2

6、9 Specification for Refined LeadE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE60 Practice for Analysis of Metals, Ores, an

7、d RelatedMaterials by Molecular Absorption SpectrometryE135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysis of Metals3E1601 Practice for Conducting an Interlaboratory Study toEvalu

8、ate the Performance of an Analytical Method3. Terminology3.1 For definitions of terms used in this test method, refer toTerminology E135.4. Significance and Use4.1 These test methods for the chemical analysis of metalsand alloys are primarily intended to test such materials forcompliance with compos

9、itional specifications. It is assumedthat all who use these methods will be trained analysts capableof performing common laboratory procedures skillfully andsafely. It is expected that work will be performed in a properlyequipped laboratory.5. Apparatus, Reagents, and Photometric Practice5.1 Apparat

10、us and reagents required for each determinationare listed in separate sections of each test method. Theapparatus, standard solutions, and reagents conform to therequirements prescribed in Practices E50. Photometers shallconform to the requirements prescribed in Practice E60.1These test methods are u

11、nder the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and are the directresponsibility of Subcommittee E01.05 on Cu, Pb, Zn, Cd, Sn, Be, their Alloys, andRelated Metals.Current edition approved Feb. 1, 2011. Published March 2011. Originallyapprove

12、d in 1942. Last previous edition approved in 2005 as E37 05. DOI:10.1520/E0037-05R11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary

13、page onthe ASTM website.3Formerly under the jurisdiction of Committee E01 on Analytical Chemistry forMetals, Ores, and Related Materials, this test method was withdrawn in October1998 in accordance with section 10.5.3.1 of the Regulations Governing ASTMTechnical Committees, which requires that stand

14、ards shall be updated by the end ofthe eighth year since the last approval date.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6. Safety Hazards6.1 For precautions to be observed in the use of certainreagents in these test methods,

15、refer to Practices E50.7. Sampling7.1 For procedures for sampling the material, refer toSpecification B29.8. Rounding Calculated Values8.1 Calculated values shall be rounded to the desired num-ber of places as directed in Practice E29.9. Interlaboratory Studies9.1 These test methods have been evalua

16、ted in accordancewith Practice E173, unless otherwise noted in the precisionsection.COPPER, BISMUTH, SILVER, AND ZINC BY THEATOMIC ABSORPTION METHOD10. Scope10.1 This test method covers the determination of bismuthin concentrations from 0.002 to 0.2 %, copper from 0.001 to0.1 %, silver from 0.001 to

17、 0.03 %, and zinc from 0.001 to0.005 %.11. Summary of Test Method11.1 The sample is dissolved in a nitric-perchloric acidmixture, the solution is fumed, and hydrochloric acid is addedto precipitate lead chloride. The hydrochloric-perchloric acidsolution is aspirated into the air-acetylene flame of a

18、n atomicabsorption spectrophotometer. The absorption of the resonanceline energy from the spectrum of each element is measured andcompared with that of calibration solutions of the sameelement. The lines used were Cu 324.7, Bi 223.0, Ag 328.0,and Zn 213.8 nm12. Concentration Range12.1 The concentrat

19、ion range for each element must bedetermined experimentally because the optimum range willdepend upon the individual instrument. Determine the appro-priate concentration range of each element as follows:12.1.1 Prepare a dilute standard solution as directed inSection 16. Refer to 16.1 for suggested i

20、nitial concentrations.12.1.2 Prepare the instrument for use as directed in 18.1.Measure the instrument response while aspirating water, thecalibration solution with the lowest concentration, and the twowith the highest concentrations. Determine the minimumresponse and the curve linearity as directed

21、 in 14.1.1 and14.1.2, respectively.12.1.3 If the instrument meets or surpasses the minimumresponse and curve linearity criteria, the initial concentrationrange may be considered suitable for use. In this case proceedas directed in 12.1.5.12.1.4 If the minimum response is not achieved, prepareanother

22、 dilute standard solution to provide a higher concentra-tion range, and repeat 12.1.2 and 12.1.3. If the calibration curvedoes not meet the linearity criterion, prepare another dilutestandard solution to provide a lower concentration range, andrepeat 12.1.2 and 12.1.3. If a concentration range canno

23、t befound for which both criteria can be met, do not use thismethod until the performance of the apparatus has beenimproved.12.1.5 Perform the stability test as directed in 14.1.3.Ifeither of the minimum stability requirements is not met, do notuse this method until the repeatability of the readings

24、 has beensuitably improved.13. Interferences13.1 Elements ordinarily present do not interfere if theirconcentrations are under the maximum limits shown in 1.1.14. Apparatus14.1 Atomic Absorption SpectrophotometerUse hollow-cathode lamps, operated in accordance with manufacturersrecommendations as so

25、urces for the following lines: Cu 324.7,Bi 223.0, Ag 328.0, and Zn 213.8 nm. Aspirate the solutionsinto an air-acetylene flame of a premix burner. Determine thatthe atomic absorption spectrophotometer is satisfactory for usein this method by proceeding as directed in 14.1.1-14.1.3.NOTE 1Optimum sett

26、ings for the operating parameters of the atomicabsorption spectrophotometer vary from instrument to instrument.14.1.1 Minimum Response Calculate the difference be-tween the readings of the two highest of five equally spaced(16.2) calibration solutions. This difference must be at least 40scale units.

27、NOTE 2The scale unit is defined as the smallest numerical intervalthat is estimated in taking each reading on the instrument. If the scale isnon-linear, the largest unit defined in this manner is used.14.1.2 Curve Linearity Calculate the difference betweenthe scale readings obtained with water and t

28、he lowest of thefive equally spaced calibration solutions. If necessary, convertthis difference and the difference calculated in 14.1.1 toabsorbance. Divide the difference for the highest interval bythat for the lowest interval. If this ratio is not 0.70 or greater,proceed as directed in 12.1.4.E37

29、05 (2011)214.1.3 Minimum StabilityIf the variability of the readingsof the highest calibration solution and of water is not less than1.8 % and 1.4 %, respectively, as calculated below, proceed asdirected in 12.1.5.VC5100C(C C!2n 1(1)Vo5100C(O O!2n 1(2)where:VC= percent variability of the highest cal

30、ibrationreadings,C= average absorbance value for the highestcalibration solution,( (CX)2= sum of the squares of the n differencesbetween the absorbance readings of the high-est calibration solution and their average,VO= percent variability of the readings on waterrelative to C,O= average absorbance

31、value of water,(OO)2= sum of the squares of the n difference be-tween the absorbance readings of water andtheir average, andn = number of determinations, three or more.15. Reagents15.1 Bismuth, Standard Solution (1 mL = 1 mg Bi)Transfer1gofbismuth (purity: 99.9 % min) to a 400-mLbeaker and dissolve

32、in 50 mL of HNO3(1 + 1), heating gentlyif necessary. When dissolution is complete, cool, transfer to a1-L volumetric flask, add 100 mL of HNO3(1 + 1), dilute tovolume, and mix. Store in a polyethylene bottle.15.2 Copper, Standard Solution (1 mL = 1 mg Cu)Proceed as directed in 15.1, but substitute1g

33、ofcopper (purity:99.9 % min) for the bismuth.15.3 Silver, Standard Solution (1 mL = 1 mg Ag)Proceedas directed in 15.1 but substitute1gofsilver (purity: 99.9 %min) for the bismuth.15.4 Zinc, Standard Solution (1 mL = 0.1 mg Zn)Proceedas directed in 15.1 but substitute 0.1 g of zinc (purity: 99.9 %mi

34、n) for the bismuth.16. Calibration16.1 Dilute Standard SolutionUsing pipets, transfer to500-mL volumetric flasks the following volumes of eachstandard solution: bismuth, 20 mL; copper, 10 mL; silver, 5mL; and zinc, 10 mL. Dilute to volume and mix. Adjust theconcentration of a dilute standard solutio

35、n if the proper rangeis not obtained when the 5, 10, 15, 20, and 25-mL portions arediluted to 100 mL and tested.16.2 Calibration SolutionsPrepare five calibration solu-tions for each element to be determined. Using pipets, transfer5, 10, 15, 20, and 25-mL portions of the appropriate dilutestandard s

36、olution to 100-mL volumetric flasks. Add sufficientvolumes of HCl and HClO4to each flask to yield final acidconcentrations equal to that of the corresponding test solution,dilute to volume, and mix. Do not use solutions that have stoodmore than 24 h.17. Procedure17.1 Test Solution:17.1.1 Transfer a

37、10 g sample, weighed to the nearest 10mg, to a 300-mL Erlenmeyer flask (Note 3). Add 3 mL ofHNO3and 15 mL of HClO4, and heat until dissolution iscomplete. Evaporate to strong fumes of perchloric acid andcool.NOTE 3Due to the limited solubility of silver chloride, the silverconcentration in the sampl

38、e solution should be less than 1 mg/100 mL. Ifthe expected silver concentration is higher than 0.01 %, choose a sampleweight that limits the silver concentration to less than 1 mg/100 mL.17.1.2 Add 50 mL of water and, while swirling, heat toboiling. Add 25 mL of HCl. If less than a 10-g sample is us

39、ed,add 20 mL HCl plus 0.5 mL for each gram of sample used.Heat again to boiling and cool to room temperature.17.1.3 Transfer the solution and precipitate to a 100-mLvolumetric flask, dilute to volume with water, and mix thor-oughly. Allow the precipitated lead chloride to settle. Use thesupernatant

40、solution, or dilute an appropriate aliquot of thesupernatant solution to provide a concentration of the elementbeing measured which lies within the concentration rangedetermined in Section 12.17.2 Reagent Blank SolutionPrepare a reagent blank byadding 3 mL of HNO3and 15 mL of HClO4to a 300-mLErlenme

41、yer flask and proceed as directed in 17.1.18. Measurement18.1 Instrument AdjustmentOptimize the response of theinstrument as directed in 18.1.1-18.1.4.18.1.1 Set the instrument parameters approximately at thevalues obtained in 14.1, and light the burner.18.1.2 Adjust the instrument to the approximat

42、e wavelengthfor the element to be determined, permit the instrument toreach thermal equilibrium, and complete the wavelength ad-justment to obtain maximum absorption while aspirating thehighest calibration solution.18.1.3 Optimize fuel, air, and burner adjustments whileaspirating the highest calibra

43、tion solution.18.1.4 Aspirate water long enough to establish that theabsorbance reading is stable and then set the initial reading(approximately zero absorbance or 100 % transmittance).18.2 Photometry:18.2.1 Aspirate the test solution and note, but do not recordthe reading.NOTE 4Avoid transferring p

44、articles of precipitated lead chloride thatmay clog the aspirator during the measurements of the test solution.18.2.2 Aspirate water until the initial reading is againobtained. Aspirate the calibration solutions and test solution inorder of increasing instrument response, starting with thereagent bl

45、ank. When a stable response is obtained for eachsolution, record the reading.18.2.3 Proceed as directed in 18.2.2 at least twice more.19. Calculations19.1 Calculate the variability of the readings for water andthe highest calibration solution as directed in 14.1.3 to deter-mine whether they are less

46、 than 1.4 % and 1.8 %, respectively.E37 05 (2011)3If they are not, disregard the data, readjust the instrument, andproceed again as directed in 18.2.19.2 If necessary, convert the average of the readings foreach calibration solution to absorbance. Calculate the netabsorbance of the test solution by

47、subtracting the absorbance ofthe reagent blank solution.19.3 Prepare a calibration curve by plotting the absorbancevalues for the calibration solutions against milligrams of theelements per millilitre.19.4 Convert the net absorbance value of the test solution tomilligrams of the element per millilit

48、re by means of theappropriate calibration curve.19.5 Calculate the percentage of the element as follows(Note 5):Element, % 5 A 3 B 3 0.977!/C 3 100 (3)where:A = milligrams of element per millilitre,B = final volume of test solution in millilitres, andC = milligrams of sample represented in final vol

49、ume oftest solution.NOTE 5The factor 0.977 is used to compensate for the volume errorin the 100 mL of final test solution caused by the 13.1 g of lead chlorideprecipitate. If less than 10 g of sample is used, calculate and apply anappropriate factor.20. Precision and Bias20.1 PrecisionSeven laboratories cooperated in testingthis method, with one laboratory reporting a second pair ofvalues; the data are summarized in Table 1.20.2 BiasThe accuracy of this method could not beevaluated because adequate certified reference materials wereunav