ASTM E1587-2010 Standard Test Methods for Chemical Analysis of Refined Nickel《精制镍化学分析的标准试验方法》.pdf

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1、Designation:E158705 Designation: E1587 10Standard Test Methods forChemical Analysis of Refined Nickel1This standard is issued under the fixed designation E1587; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revis

2、ion. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1These1.1 These test methods apply to the chemical analysis of refined nickel and other forms of metallic nickel havingchemical co

3、mpositions within the following limits:Element Weight %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 0.20Nicke

4、l, min 98.0Nitrogen, less than 0.50Oxygen, 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

5、 to determine the following elements by the methods indicated below:Antimony, Arsenic, Bismuth, Cadmium, Lead, Selenium, Silver, Tellurium, Tin, and Thallium by the Electrothermal AtomicAbsorption MethodBismuth, Cadmium, Cobalt, Copper, Iron, Lead, Manganese, Silver, and Zinc by the Flame Atomic Abs

6、orption MethodCarbon, Total, by the Combustion-Instrumental MethodNickel by the Dimethylglyoxime Gravimetric MethodNitrogen by the Inert Gas Fusion Thermal Conductivity MethodOxygen by the Inert Gas Fusion MethodSulfur by the Infrared Absorption MethodTest Methods SectionsAntimony, Arsenic, Bismuth,

7、 Cadmium,Lead, Selenium, Silver, Tellurium, Tin,and Thallium by the Graphite FurnaceAtomic Absorption Spectrometric Method21-31Bismuth, Cadmium, Cobalt, Copper, Iron,Lead, Manganese, Silver, and Zinc by theFlame Atomic Absorption SpectrometricMethod9-201These test methods are under the jurisdiction

8、of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and are the direct responsibilityof Subcommittee E01.08 on Ni and Co and High Temperature Alloys.Current edition approved MayDec. 15, 2005.2010. Published June 2005.February 2011. Originally approved in 1994. Last

9、previous edition approved in 19982005 asE158794(1998).E1587 05. DOI: 10.1520/E1587-105.1This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible t

10、o adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Con

11、shohocken, PA 19428-2959, United States.Carbon, Total, by the Combustion-Instrumental Method (Refer to Test Meth-ods E1019)32Test Methods SectionsNitrogen by the Inert Gas Fusion ThermalConductivity Method (Refer to Test Meth-ods E1019)45Oxygen by the Inert Gas Fusion Method(Refer to Test Methods E1

12、019)46Phosphorus by the Phosphovanadomo-lybdate Molecular Absorption Spectromet-ric Method (Refer to Test MethodsE1019)47Sulfur by the Combustion-Infrared Ab-sorption Method (Refer to Test MethodsE1019)33Sulfur by the Methylene Blue Spectro-photometric Method After Generation ofHydrogen Sulfide34-44

13、1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish a

14、ppropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. For specific precautions, see Section 6.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data to Determine Co

15、nformance with Specifications E39Methods for ChemicalAnalysis of NickelE50 Practices forApparatus, Reagents, and Safety Considerations for ChemicalAnalysis of Metals, Ores, and Related MaterialsE60 Practice for Analysis of Metals, Ores, and Related Materials by Molecular Absorption SpectrometryE135

16、Terminology Relating to Analytical Chemistry for Metals, Ores, and Related MaterialsE1019 Test Methods for Determination of Carbon, Sulfur, Nitrogen, and Oxygen in Steel, Iron, Nickel, and Cobalt Alloys byVarious Combustion and Fusion TechniquesE1024 Guide for Chemical Analysis of Metals and Metal B

17、earing Ores by Flame Atomic Absorption SpectrophotometryE1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method2For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book

18、 of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.E1587 102Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical MethodE1917 Test Method for Determination of Phosphorus in Nickel, Ferronickel, and Nickel All

19、oys by PhosphovanadomolybdateMolecular Absorption Spectrometry2.2 ISO Standard:3ISO 5725 Precision of Test MethodsDetermination of Repeatability and Reproducibility by Interlaboratory Tests3. Terminology3.1 For definitions of terms used in this test method, refer to Terminology E135.4. Significance

20、and Use4.1 These test methods are primarily intended to test refined nickel metal for compliance with compositional specifications. Itis assumed that all who use these test methods will be trained analysts capable of performing common laboratory proceduresskillfully and safely. It is expected that t

21、he analytical work will be performed in a properly equipped laboratory under appropriatequality control practices.5. Apparatus, Reagents, and Instrumental Practices5.1 Apparatus:5.1.1 Special apparatus and reagents required for each determination are listed in the Apparatus section of each test meth

22、od.5.1.2 Glass storage containers shall be of borosilicate glass.5.1.3 Plastic containers shall be polyethylene or preferably polyetrafluoroethylene (PTFE).5.2 Reagents:5.2.1 Purity of ReagentsUnless otherwise indicated, all reagents used in these test methods shall conform to the specificationsof t

23、he Committee on Analytical Reagents of the American Chemical Society. Other chemicals may be used, provided it is firstascertained that they are of sufficiently high purity to permit their use without adversely affecting the expected performance of thedetermination, as indicated in each Precision an

24、d Bias section.5.2.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water as defined byType II of Specification D1193.5.2.3 Reagents and their preparation are described in the Reagents section in each test method.5.2.4 Instructions for the preparat

25、ion of standard solutions used in these test methods frequently call for measuring exactweights of substances of known composition so that the concentrations of the resulting standard solutions can be expressed usingsimple numbers. Small variations from these specified quantities are acceptable, pro

26、vided that the true weighed masses are usedto calculate the concentration of the prepared solutions and then these calculated values are used throughout the test methods.5.3 Instrumental PracticesInformation on the use of some instrumental techniques employed in these test methods aredescribed in Pr

27、actice E60 and in Guide E1024.6. Hazards6.1For6.1 For precautions to be observed in the use of certain reagents and equipment in these test methods, refer to PracticesE50.6.2 Where appropriate, specific precautionary information is given in the Hazards sections and in special warning paragraphs.7. S

28、ampling7.1 Sampling shall be carried out by a mutually acceptable method.7.2 The laboratory sample normally is in the form of a powder, granules, millings, or drillings and no further preparation isnecessary.7.3 If it is suspected that the laboratory sample is contaminated with oil or grease from th

29、e milling or drilling process, it maybe cleaned by washing with high-purity acetone and drying in air.7.4 If the laboratory sample contains particles or pieces of widely varying sizes, the test sample should be obtained by rifflingor coning and quartering techniques.8. Rounding Calculated Values8.1

30、Calculated values shall be rounded to the desired number of places in accordance with the rounding method in Practice E29.SILVER, BISMUTH, CADMIUM, COBALT, COPPER, IRON, MANGANESE, LEAD, AND ZINC BY THE FLAMEATOMIC ABSORPTION SPECTROMETRIC METHOD9. Scope9.1 This test method applies to the determinat

31、ion of the silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead, and3Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.E1587 103zinc contents of refined, wrought, and cast nickel metal within the following ranges

32、.Concentration Range, %Element Method A Method BAgSilver 0.0002 to 0.01 . BiSilver 0.0002 to 0.01 .Bismuth 0.0010 to 0.01 . CdBismuth 0.0010 to 0.01 .Cadmium 0.0002 to 0.0025 . CoCadmium 0.0002 to 0.0025 .Cobalt 0.0010 to 0.01 0.01 to 1.00 CuCobalt 0.0010 to 0.01 0.01 to 1.00Copper 0.0005 to 0.01 0.

33、01 to 1.00 FeCopper 0.0005 to 0.01 0.01 to 1.00Iron 0.0025 to 0.01 0.01 to 0.15 MnIron 0.0025 to 0.01 0.01 to 0.15Manganese 0.0005 to 0.01 0.01 to 0.20 PbManganese 0.0005 to 0.01 0.01 to 0.20Lead 0.0006 to 0.01 . ZnLead 0.0006 to 0.01 .Zinc 0.0005 to 0.0025 0.001 to 0.0159.2 This test method is appl

34、icable to the independent determination of any one or more of the elements listed without includingall the elements specified in the standard solutions.9.3 The lower level for iron can be extended to less than 0.0025 % provided nickel metal containing less than 0.0001 % ironis used for preparation o

35、f standards.9.4 The upper limit for the determination of cobalt and copper can be raised to 2 % by a minor modification to the test method.See Note 6.10. Summary of Test Method10.1 The sample is dissolved in dilute nitric acid,HNO3, excess acid is evaporated, and the solution diluted to a known volu

36、me.The test solution is aspirated into the air/acetylene flame of an atomic absorption spectrometer. The absorption of the resonanceline energy from the spectrum of each element is measured and compared with that from a set of calibration solutions of the sameelement in a matched nickel matrix.11. I

37、nterferences11.1 Elements ordinarily present in nickel metal do not present spectral interferences in the atomic absorption analysis.11.2 For the determination of silver, take care to avoid contamination of the sample and calibration solutions with chloride.11.3 Potential background absorption inter

38、ference is eliminated by use of matched matrix standards prepared from high-puritynickel metal. See Note 7.12. Apparatus12.1 Atomic Absorption Spectrometer :12.1.1 The atomic absorption spectrometer used in this test method shallshould meet the instrument performance parameters inaccordance with Gui

39、de E1024.12.1.2 The instrument shall be equipped with a burner head capable of accepting a solution containing 25 g/L of nickel, asnitrate, and suitable for an air/acetylene flame.12.1.3 The instrument should be capable of using single-element hollow cathode or electrodeless discharge lamps operated

40、 atcurrents recommended by the instrument manufacturer.13. Reagents13.1 Bismuth, Standard Stock Solution (1mL=1mgBismuth):13.1.1 Transfer a 1.00-g sample of bismuth metal (purity, 99.9 % minimum), 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 gen

41、tly until dissolution is complete. Boil gently to expel oxides ofnitrogen and cool. Transfer to a 1-L volumetric flask containing 160 mL of HNO3(1 + 1), dilute to volume with water, and mix.Store in a polyethylene or PTFE bottle.NOTE 1Use the same batch of nitric acidHNO3throughout the entire proced

42、ure. Also see Note 4.13.2 Cadmium, Standard Stock Solution (1 mL=1mgCadmium)Transfer a 1.00-g sample of cadmium metal (purity, 99.9 %minimum), weighed to the nearest 0.001 g, to a 600-mL beaker. Proceed as directed in 13.1.2.13.3 Cobalt, Standard Stock Solution (1 mL=1mg Cobalt)Transfer a 1.00-g sam

43、ple of cobalt metal (purity, 99.9 %minimum), weighed to the nearest 0.001 g, to a 600-mL beaker. Proceed as directed in 13.1.2.13.4 Copper, Standard Stock Solution (1 mL=1mg Copper)Transfer a 1.00-g sample of copper metal (purity, 99.9 %E1587 104minimum), weighed to the nearest 0.001 g, to a 600-mL

44、beaker. Proceed as directed in 13.1.2.13.5 Iron, Standard Stock Solution (1 mL=1mgIron)Transfer a 1.00-g sample of iron metal (purity, 99.9 % minimum),weighed to the nearest 0.001 g, to a 600-mL beaker. Proceed as directed in 13.1.2.13.6 Lead, Standard Stock Solution (1 mg=1mgLead)Transfer a 1.00-g

45、sample of lead metal (purity, 99.9 % minimum),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 mg Manganese)Transfer a 1.00-g sample of manganese metal (purity,99.9 % minimum), weighed to the nearest 0.001 g, to a 600

46、-mL beaker. Proceed as directed in 13.1.2.13.8 Nickel PowderHigh-purity, containing less than 0.0005 % Iron and less than 0.0001 % each of silver, bismuth, cadmium,cobalt, copper, manganese, lead, and zinc.13.9 Silver, Standard Stock Solution (1 mL=1mgSilver)Transfer a 1.00-g sample of silver metal

47、(purity, 99.9 % minimum),weighed to the nearest 0.001-g,0.001 g, to a 600-mL beaker. Proceed as directed in 13.1.2, except store in an amber glass container.13.10 Zinc, Standard Stock Solution (1 mL=1mgZinc)Transfer a 1.00-g sample of zinc metal (purity, 99.9 % minimum),weighed to the nearest 0.001

48、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 g of Silver, Bismuth, Cadmium, Cobalt, Copper, Iron, Manganese, andLead and 10 g of Zinc)Using pipets, transfer 20.0 mL of each of the standard stock solutions for Silver, B

49、ismuth, Cadmium,Cobalt, Copper, Iron, Manganese, and Lead and 10 mL of the standard stock solution for Zinc to a 1-L volumetric flask containing160 mLof HNOMixed Analyte Standard Solution A (1 mL = 20 g of silver, bismuth, cadmium, cobalt, copper, iron, manganese, and lead and 10 g of zinc)Usingpipets, transfer 20.0 mL of each of the standard stock solutions for silver, bismuth, cadmium, cobalt, copper, iron, manganese, and lead and 10 mL of the standard stocksolution for zinc to a 1-L volumetric flask containing 160 mL of HNO3(1 + 1) (Note 1). Dilute to v