ASTM E1587-2017 Standard Test Methods for Chemical Analysis of Refined Nickel《精炼镍化学分析的标准试验方法》.pdf

1、Designation: E1587 10E1587 17Standard 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 revision. A numbe

2、r in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods apply to the chemical analysis of refined nickel and other forms of metallic nickel having chemicalcompositions within th

3、e following limits:Element Weight, %Element Mass Fraction, %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 98.0N

4、itrogen, 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 to determin

5、e the following elements by the methods indicated below:1 These test methods are under the jurisdiction ofASTM 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 editio

6、n approved Dec. 15, 2010April 1, 2017. Published February 2011June 2017. Originally approved in 1994. Last previous edition approved in 20052010 asE1587 05.E1587 10. DOI: 10.1520/E1587-10.10.1520/E1587-17.This document is not an ASTM standard and is intended only to provide the user of an ASTM stand

7、ard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to 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

8、 is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1Test Methods SectionsAntimony, Arsenic, Bismuth, Cadmium,Lead, Selenium, Silver, Tellurium, Tin,and Thallium by the Graphite FurnaceAtomic Abso

9、rption Spectrometric Method21 31Bismuth, Cadmium, Cobalt, Copper, Iron,Lead, Manganese, Silver, and Zinc by theFlame Atomic Absorption SpectrometricMethod9 20Carbon, Total, by the Combustion-Instrumental Method (Refer to Test Meth-ods E1019)32Test Methods SectionsNitrogen by the Inert Gas Fusion The

10、rmalConductivity Method (Refer to Test Meth-ods E1019)45Oxygen by the Inert Gas Fusion Method(Refer to Test Methods E1019)46Phosphorus by the Phosphovanadomo-lybdate Molecular Absorption Spectromet-ric Method (Refer to Test MethodsE1019)47Sulfur by the Combustion-Infrared Ab-sorption Method (Refer t

11、o Test MethodsE1019)33Sulfur by the Methylene Blue Spectro-photometric Method After Generation ofHydrogen Sulfide34 44Sulfur by the Methylene Blue Spectro-photometric Method After Generation ofHydrogen Sulfide32 421.3 The values stated in SI units are to be regarded as standard. No other units of me

12、asurement 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 appropriate safety and health practices and determine the applicability of regulatoryli

13、mitations prior to use. For specific precautions, see Section 6.1.5 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendation

14、s issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data to Determine Conformance with SpecificationsE50 Practices forApparatus, Reagents,

15、 and Safety Considerations for ChemicalAnalysis of Metals, Ores, and Related MaterialsE60 Practice for Analysis of Metals, Ores, and Related Materials by SpectrophotometryE135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related MaterialsE1019 Test Methods for Determination of

16、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 Bearing Ores by Flame Atomic Absorption Spectrophotometry(Withdrawn 2004)3E1601 Practice for Conducting an Interlaboratory St

17、udy to Evaluate the Performance of an Analytical MethodE1917 Test Method for Determination of Phosphorus in Nickel, Ferronickel, and Nickel Alloys by PhosphovanadomolybdateSpectrophotometry2.2 ISO Standard:4ISO 5725 Precision of Test MethodsDetermination of Repeatability and Reproducibility by Inter

18、laboratory Tests2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this historica

19、l standard is referenced on www.astm.org.4 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.E1587 1723. Terminology3.1 For definitions of terms used in this test method, refer to Terminology E135.4. Significance and Use4.1

20、 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 the analyti

21、cal 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 method.5.1.2 G

22、lass storage containers shall be of borosilicate glass.5.1.3 Plastic containers shall be polyethylene or preferably polyetrafluoroethylenepolytetrafluoroethylene (PTFE).5.2 Reagents:5.2.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, all reagents u

23、sed inthese test methods shall it is intended that all reagents conform to the specifications of the Committee on Analytical Reagents ofthe American Chemical Society. Society where such specifications are available.5 Other chemicalsgrades may be used, providedit is first ascertained that they are th

24、e reagent is of sufficiently high purity to permit theirits use without adversely affecting theexpected performance of the determination, as indicated in each Precision and Bias section.lessening the accuracy of thedetermination.5.2.2 Purity of WaterUnless otherwise indicated, references to water sh

25、all 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 preparation of standard solutions used in these test methods frequently call for measuring exa

26、ctweightsmasses of substances of known composition so that the concentrations of the resulting standard stock solutions can beexpressed using simple numbers. Small variations from these specified quantities are acceptable, provided that the true weighedmasses are used to calculate the concentration

27、of the prepared solutions and then these calculated values are used throughout thetest methods.5.3 Instrumental PracticesInformation on the use of some instrumental techniques employed in these test methods aredescribed in Practice E60 and in Guide E1024.6. Hazards6.1 For precautions to be observed

28、in the use of certain reagents and equipment in these test methods, refer to Practices E50.6.2 Where appropriate, specific precautionary information is given in the Hazards sections and in special warning paragraphs.7. Sampling7.1 Sampling shall be carried out by a mutually acceptable method.7.2 The

29、 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 the milling or drilling process, it maybe cleaned by washing with high-purity acet

30、one 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 Calculated values shall be rounded to the desired number of places in accordance

31、 with the rounding method in Practice E29.5 Available from Fisher Scientific Co., 2000 Park Lane Dr., Pittsburgh, PA 15275, .Reagent Chemicals, American Chemical Society Specifications,American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by the American Ch

32、emical Society, see the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.E1587 173SILVER, BISMUTH, CADMIUM, COBALT, COPPER, IRON, MANGANESE, LEAD, AND ZINC BY THE FLAMEATOMIC ABSORPTION SPECTROMETRIC METHODSPECTROMETRY9. Scope9.1 This test m

33、ethod applies to the determination of the silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead, andzinc contents of refined, wrought, and cast nickel metal within the following ranges.Concentration Range, %Mass Fraction Range, %Element Method A Method BSilver 0.0002 to 0.01 .Bismuth 0.001

34、0 to 0.01 .Cadmium 0.0002 to 0.0025 .Cobalt 0.0010 to 0.01 0.01 to 1.00Copper 0.0005 to 0.01 0.01 to 1.00Iron 0.0025 to 0.01 0.01 to 0.15Manganese 0.0005 to 0.01 0.01 to 0.20Lead 0.0006 to 0.01 .Zinc 0.0005 to 0.0025 0.001 to 0.0159.2 This test method is applicable to the independent determination o

35、f any one or more of the elements listed without includingall the elements specified in the standardcalibration 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 of standards.calibration soluti

36、ons.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.SeeFor Note 6.test samples containing greater than 0.25 % and less than 2 % of cobalt or copper, further dilutions of the testsolution with HNO3 (1 + 19) may be made. Th

37、e nickel content of the calibration solutions should be matched with those of thetest solutions.9.5 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Stan

38、dards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.10. Summary of Test Method10.1 The sample is dissolved in dilute HNO3, excess acid is evaporated, and the solution diluted to a known volume. The testsolution is aspirated into the air

39、/acetylene flame of an atomic absorption spectrometer. The absorption of the resonance line energyfrom the spectrum of each element is measured and compared with that from a set of calibration solutions of the same elementin a matched nickel matrix.11. Interferences11.1 Elements ordinarily present i

40、n 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 interference is eliminated by use of matched matrix

41、 standards calibration solutionsprepared from high-purity nickel metal. See Note 71.NOTE 1In this test method, any effect of nonspecific absorption and light scatter is compensated for by matching the matrix of the calibration solutionswith the test solutions.Also, since the same lot of HNO3 is used

42、 for both calibration and test solutions, the reagent blank is incorporated in the calibrationcurve. Thus, the calibration curve may not pass through the origin.12. Apparatus12.1 Atomic Absorption Spectrometer:12.1.1 The atomic absorption spectrometer used in this test method should meet the instrum

43、ent performance parameters inaccordance with Guide E1024.12.1.2 The instrument shall be equipped with a burner head capable of accepting a solution containing 25 gL of nickel, asnitrate, and suitable for an air/acetylene flame.12.1.3 The instrument should be capable of using single-element hollow ca

44、thode or electrodeless discharge lamps operated atcurrents recommended by the instrument manufacturer.13. Reagents13.1 Bismuth, Standard Stock Solution (1 mL = 1 mg Bismuth):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.E

45、1587 17413.1.2 Add 40 mL of HNO3 (1 + 1) (Note 1) and heat gently 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. Use the

46、 same batch of HNO3 throughout the entire procedure.NOTE 1Use the same batch of HNO3 throughout the entire procedure. Also see Note 4.13.1.3 If inhomogeneity is suspected in the test sample, or if the sample pieces are relatively large, a larger sample mass shouldbe used to prepare the test solution

47、. Under such circumstances, a sample mass of 25 g in a final volume of 1000-mL may be used.The amount of HNO3 should be increased in proportion. Even larger sample masses can be used, with greater amounts of HNO3to prepare a more concentrated nickel test solution. However, an aliquot portion to corr

48、espond to a 5-g sample must be taken fromsuch a solution and processed in accordance with the procedure given to give a test solution containing 25 g/L of nickel to matchthe calibration solutions.13.2 Cadmium, Standard Stock Solution (1 mL = 1 mg Cadmium)Transfer a 1.00-g sample of cadmium metal (pu

49、rity, 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 = 1 mg Cobalt)Transfer a 1.00-g sample 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 = 1 mg Copper)Transfer a 1.00-g sample of copper metal (purity, 99.9 %minimum), weighed to the nearest 0.001 g, to a 600-mL beaker. Proceed as directed in 13.1.2.13.5 Iron, Standard Stock Solut