ASTM E1587-2005 Standard Test Methods for Chemical Analysis of Refined Nickel《精炼镍化学分析的标准试验方法》.pdf

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1、Designation: E 1587 05Standard Test Methods forChemical Analysis of Refined Nickel1This standard is issued under the fixed designation E 1587; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in p

2、arentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods apply to the chemical analysis ofrefined nickel and other forms of metallic nickel havingchemical compositions within the foll

3、owing limits:Element Weight %Antimony, less than 0.005Arsenic, less than 0.005Bismuth, less than 0.01Cadmium, less than 0.0025Carbon, max 0.03Cobalt, max 1.00Copper, max 1.00Hydrogen, max 0.003Iron, max 0.15Lead, less than 0.01Manganese, less than 0.20Nickel, min 98.0Nitrogen, less than 0.50Oxygen,

4、less than 0.03Phosphorus, less than 0.005Selenium, less than 0.0010Silicon, less than 0.005Silver, less than 0.01Sulfur, max 0.01Tellurium, less than 0.0010Thallium, less than 0.0010Tin, less than 0.005Zinc, less than 0.0151.2 These test methods may be used to determine thefollowing elements by the

5、methods indicated below:Antimony, Arsenic, Bismuth, Cadmium, Lead, Selenium,Silver, Tellurium, Tin, and Thallium by the ElectrothermalAtomic Absorption MethodBismuth, Cadmium, Cobalt, Copper, Iron, Lead, Manga-nese, Silver, and Zinc by the Flame Atomic AbsorptionMethodCarbon, Total, by the Combustio

6、n-Instrumental MethodNickel by the Dimethylglyoxime Gravimetric MethodNitrogen by the Inert Gas Fusion Thermal ConductivityMethodOxygen by the Inert Gas Fusion MethodSulfur by the Infrared Absorption MethodSulfur by the Methylene Blue SpectrophotometricMethod After Generation of Hydrogen Sulfide1.3

7、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 theresponsibility of the user of this standard to establish appro-pr

8、iate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specificprecautions, see Section 6.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data toDetermine Conform

9、ance with SpecificationsE39 Methods for Chemical Analysis of Nickel3E50 Practices for Apparatus, Reagents, and Safety Precau-tions for Chemical Analysis of MetalsE60 Practice for Photometric and SpectrophotometricMethods for Chemical Analysis of MetalsE 135 Terminology Relating to Analytical Chemist

10、ry forMetals, Ores and Related MaterialsE 1019 Test Methods for Determination of Carbon, Sulfur,Nitrogen, Oxygen, and Hydrogen in Steel and in Iron,Nickel, and Cobalt AlloysE 1024 Guide for Chemical Analysis of Metals and MetalBearing Ores by Flame Absorption SpectrophotometryE 1601 Practice for Con

11、ducting an Interlaboratory Study toEvaluate the Performance of an Analytical Method2.2 ISO Standard:ISO 5725 Precision of Test MethodsDetermination ofRepeatability and Reproducibility by InterlaboratoryTests43. Terminology3.1 For definitions of terms used in this test method, refer toTerminology E 1

12、35.1These test methods are under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and are the directresponsibility of Subcommittee E01.08 on Ni and Co and High-TemperatureAlloys.Current edition approved May 15, 2005. Published June 2005. Originall

13、yapproved in 1994. Last previous edition approved in 1998 as E 1587 94 (1998)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 page ont

14、he ASTM website.3Withdrawn.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036 (www.ansi.org).1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4. Significance and Use4.1 These tes

15、t methods are primarily intended to test refinednickel metal for compliance with compositional specifications.It is assumed that all who use these test methods will be trainedanalysts capable of performing common laboratory proceduresskillfully and safely. It is expected that the analytical work wil

16、lbe performed in a properly equipped laboratory under appro-priate quality control practices.5. Apparatus, Reagents, and Instrumental Practices5.1 Apparatus:5.1.1 Special apparatus and reagents required for eachdetermination are listed in the Apparatus section of each testmethod.5.1.2 Glass storage

17、containers shall be of borosilicate glass.5.1.3 Plastic containers shall be polyethylene or preferablypolyetrafluoroethylene (PTFE).5.2 Reagents:5.2.1 Purity of ReagentsUnless otherwise indicated, allreagents used in these test methods shall conform to thespecifications of the Committee on Analytica

18、l Reagents of theAmerican Chemical Society. Other chemicals may be used,provided it is first ascertained that they are of sufficiently highpurity to permit their use without adversely affecting theexpected performance of the determination, as indicated ineach Precision and Bias section.5.2.2 Purity

19、of WaterUnless otherwise indicated, refer-ences to water shall be understood to mean reagent water asdefined by Type II of Specification D 1193.5.2.3 Reagents and their preparation are described in theReagents section in each test method.5.2.4 Instructions for the preparation of standard solutionsus

20、ed in these test methods frequently call for measuring exactweights of substances of known composition so that theconcentrations of the resulting standard solutions can beexpressed using simple numbers. Small variations from thesespecified quantities are acceptable, provided that the trueweighed mas

21、ses are used to calculate the concentration of theprepared solutions and then these calculated values are usedthroughout the test methods.5.3 Instrumental PracticesInformation on the use of someinstrumental techniques employed in these test methods aredescribed in Practice E60and in Guide E 1024.6.

22、Hazards6.1 For precautions to be observed in the use of certainreagents and equipment in these test methods, refer to PracticesE50.6.2 Where appropriate, specific precautionary informationis given in the Hazards sections and in special warningparagraphs.7. Sampling7.1 Sampling shall be carried out b

23、y a mutually acceptablemethod.7.2 The laboratory sample normally is in the form of apowder, granules, millings, or drillings and no further prepa-ration is necessary.7.3 If it is suspected that the laboratory sample is contami-nated with oil or grease from the milling or drilling process, itmay be c

24、leaned by washing with high-purity acetone anddrying in air.7.4 If the laboratory sample contains particles or pieces ofwidely varying sizes, the test sample should be obtained byriffling or coning and quartering techniques.8. Rounding Calculated Values8.1 Calculated values shall be rounded to the d

25、esired num-ber of places in accordance with the rounding method inPractice E29.SILVER, BISMUTH, CADMIUM, COBALT, COPPER,IRON, MANGANESE, LEAD, AND ZINC BY THEFLAME ATOMIC ABSORPTION METHOD9. Scope9.1 This test method applies to the determination of thesilver, bismuth, cadmium, cobalt, copper, iron,

26、manganese,lead, and zinc contents of refined, wrought, and cast nickelmetal within the following ranges.Concentration Range, %Element Method A Method BAg 0.0002 to 0.01 .Bi 0.0010 to 0.01 .Cd 0.0002 to 0.0025 .Co 0.0010 to 0.01 0.01 to 1.00Cu 0.0005 to 0.01 0.01 to 1.00Fe 0.0025 to 0.01 0.01 to 0.15

27、Mn 0.0005 to 0.01 0.01 to 0.20Pb 0.0006 to 0.01 .Zn 0.0005 to 0.0025 0.001 to 0.0159.2 This test method is applicable to the independent deter-mination of any one or more of the elements listed withoutincluding all the elements specified in the standard solutions.9.3 The lower level for iron can be

28、extended to less than0.0025 % provided nickel metal containing less than 0.0001 %iron is used for preparation of standards.9.4 The upper limit for the determination of cobalt andcopper can be raised to 2 % by a minor modification to the testmethod. See Note 6.10. Summary of Test Method10.1 The sampl

29、e is dissolved in dilute nitric acid, excessacid is evaporated, and the solution diluted to a known volume.The test solution is aspirated into the air/acetylene flame of anatomic absorption spectrometer. The absorption of the reso-nance line energy from the spectrum of each element ismeasured and co

30、mpared with that from a set of calibrationsolutions of the same element in a matched nickel matrix.11. Interferences11.1 Elements ordinarily present in nickel metal do notpresent spectral interferences in the atomic absorption analysis.11.2 For the determination of silver, take care to avoidcontamin

31、ation of the sample and calibration solutions withchloride.11.3 Potential background absorption interference is elimi-nated by use of matched matrix standards prepared fromhigh-purity nickel metal. See Note 7.E158705212. Apparatus12.1 Atomic Absorption Spectrometer:12.1.1 The atomic absorption spect

32、rometer used in this testmethod shall meet the instrument performance parameters inaccordance with Guide E 1024.12.1.2 The instrument shall be equipped with a burner headcapable of accepting a solution containing 25 g/L of nickel, asnitrate, and suitable for an air/acetylene flame.12.1.3 The instrum

33、ent should be capable of using single-element hollow cathode or electrodeless discharge lampsoperated at currents recommended by the instrument manufac-turer.13. Reagents13.1 Bismuth, Standard Stock Solution (1 mL = 1 mg Bis-muth):13.1.1 Transfer a 1.00-g sample of bismuth metal (purity,99.9 % minim

34、um), weighed to the nearest 0.001 g, to a 600-mLbeaker.13.1.2 Add 40 mL of HNO3(1+1)(Note 1) and heat gentlyuntil dissolution is complete. Boil gently to expel oxides ofnitrogen and cool. Transfer to a 1-L volumetric flask containing160 mLof HNO3(1 + 1), dilute to volume with water, and mix.Store in

35、 a polyethylene or PTFE bottle.NOTE 1Use the same batch of nitric acid throughout the entireprocedure. Also see Note 4.13.2 Cadmium, Standard Stock Solution (1 mL = 1 mgCadmium)Transfer a 1.00-g sample of cadmium metal(purity, 99.9 % minimum), weighed to the nearest 0.001 g, toa 600-mL beaker. Proce

36、ed as directed in 13.1.2.13.3 Cobalt, Standard Stock Solution (1 mL = 1 mgCobalt)Transfer a 1.00-g sample of cobalt metal (purity,99.9 % minimum), weighed to the nearest 0.001 g, to a 600-mLbeaker. Proceed as directed in 13.1.2.13.4 Copper, Standard Stock Solution (1 mL = 1 mgCopper)Transfer a 1.00-

37、g sample of copper metal (purity,99.9 % minimum), weighed to the nearest 0.001 g, to a 600-mLbeaker. Proceed as directed in 13.1.2.13.5 Iron, Standard Stock Solution (1 mL = 1 mg Iron)Transfer a 1.00-g sample of iron metal (purity, 99.9 % mini-mum), weighed to the nearest 0.001 g, to a 600-mL beaker

38、.Proceed as directed in 13.1.2.13.6 Lead, Standard Stock Solution (1 mg = 1 mg Lead)Transfer a 1.00-g sample of lead metal (purity, 99.9 % mini-mum), weighed to the nearest 0.001 g, to a 600-mL beaker.Proceed as directed in 13.1.2.13.7 Manganese, Standard Stock Solution (1 mL = 1 mgManganese)Transfe

39、r a 1.00-g sample of manganese metal(purity, 99.9 % minimum), weighed to the nearest 0.001 g, toa 600-mL beaker. Proceed as directed in 13.1.2.13.8 Nickel PowderHigh-purity, containing less than0.0005 % Iron and less than 0.0001 % each of silver, bismuth,cadmium, cobalt, copper, manganese, lead, and

40、 zinc.13.9 Silver, Standard Stock Solution (1 mL = 1 mg Silver)Transfer a 1.00-g sample of silver metal (purity, 99.9 %minimum), weighed to the nearest 0.001-g, to a 600-mLbeaker. Proceed as directed in 13.1.2, except store in an amberglass container.13.10 Zinc, Standard Stock Solution (1 mL = 1 mg

41、Zinc)Transfer a 1.00-g sample of zinc metal (purity, 99.9 % mini-mum), weighed to the nearest 0.001 g, to a 600-mL beaker.Proceed as directed in 13.1.2.13.11 Working Solutions:13.11.1 Mixed Analyte Standard Solution A (1 mL = 20 gof Silver, Bismuth, Cadmium, Cobalt, Copper, Iron, Manga-nese, and Lea

42、d and 10 g of Zinc)Using pipets, transfer 20.0mL of each of the standard stock solutions for Silver, Bismuth,Cadmium, Cobalt, Copper, Iron, Manganese, and Lead and 10mL of the standard stock solution for Zinc to a 1-L volumetricflask containing 160 mL of HNO3(1+1)(Note 1). Dilute tovolume with water

43、 and mix. Store in a glass container.13.11.2 Mixed Analyte Standard Solution B (1 mL = 100 gof Cobalt, Copper, Iron, and Manganese and 10 g of Zinc)Using pipets, transfer 50.0 mL of the Cobalt, Copper, Iron, andManganese standard stock solutions and 5.0 mL of the Zincstandard stock solution to a 500

44、-mL volumetric flask. Dilute tovolume and mix. Store in a polyethylene or PTFE container.14. Calibration Solutions14.1 Set A:14.1.1 This set corresponds to 0, 0.2, 0.5, 1.0, 1.5, 2.0, and2.5 g/mL each of silver, bismuth, cadmium, cobalt, copper,iron, manganese, and lead and 0, 0.1, 0.25, 0.5, 0.75,

45、1.0, and1.25 g/L of Zinc.Analyte Concentration g/mLNo.Aliquot ofSolution A, mLSilver, Bismuth, Cadmium,Cobalt, Copper, Iron, Manga-nese and Lead Zinc10 0 02 2.0 0.2 0.13 5.0 0.5 0.254 10.0 1.0 0.55 15.0 1.5 0.756 20.0 2.0 1.07 25.0 2.5 1.2514.1.2 Weigh, to the nearest 0.01 g, seven separate 5.0-gpor

46、tions of high-purity nickel powder and transfer to 600-mLbeakers. Treat as directed in 15.2 to the point of dilution.14.1.3 Add, using a buret graduated in 0.05-mL divisions, 0,2.0, 5.0, 10.0, 15.0, 20.0, and 25.0 mL respectively of themixed Analyte Standard Solution A to the 200-mL volumetricflasks

47、. Dilute to volume with water and mix.NOTE 2The solution with zero addition is the reagent blank. See 15.3and Note 5.14.2 Set B:14.2.1 This set corresponds to 0, 2.5, 5.0, 10.0, 15.0, 20.0,and 25.0 g/mL of cobalt, copper, iron, and manganese, and 0,0.25, 0.5, 1.0, 1.5, 2.0, and 2.5 g/mL of Zinc.Anal

48、yte Concentration g/mLNo.Aliquot of Mixed Ana-lyte StandardSolution B, mLColbalt, Copper, Iron,and Manganese Zinc10 0 02 5.0 2.5 0.253 10.0 5.0 0.54 20.0 10.0 1.05 30.0 15.0 1.56 40.0 20.0 2.07 50.0 25.0 2.5E158705314.2.2 Weigh, to the nearest 0.005 g, seven separate 2.00-gportions of high-purity ni

49、ckel powder and transfer to 400-mLbeakers. Dissolve as directed in 16.2.2.14.2.3 Using a buret, add 0, 5.0, 10.0, 20.0, 30.0, 40.0, and50.0 mL respectively of the mixed Analyte Standard ReferenceSolution B to the 200-mL volumetric flasks. Dilute to volumewith water and mix. The solution with no analyte added is theblank. See Note 5.NOTE 3For convenience, 80 g of nickel/L stock nickel nitrate solutionmay be prepared by dissolving 20.0 g of nickel powder in water and 120mL of HNO3(1 + 1) in an 800-mL beaker and filtering through acid-washed glass wool or a