ASTM E1587-17 Standard Test Methods for Chemical Analysis of Refined Nickel.pdf

1、Designation: E1587 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 number in par

2、entheses 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 ofrefined nickel and other forms of metallic nickel havingchemical compositions within the followi

3、ng limits: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 98.0Nitrogen, less than 0.50Oxy

4、gen, 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

5、 the methods indicated below:Test Methods SectionsAntimony, Arsenic, Bismuth, Cadmium,Lead, Selenium, Silver, Tellurium, Tin,and Thallium by the Graphite FurnaceAtomic Absorption Spectrometric Method2131Bismuth, Cadmium, Cobalt, Copper, Iron,Lead, Manganese, Silver, and Zinc by theFlame Atomic Absor

6、ption SpectrometricMethod920Sulfur by the Methylene Blue Spectro-photometric Method After Generation ofHydrogen Sulfide32421.3 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

7、thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specificprecautions, see Section 6.1.5 This international stand

8、ard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Re

9、ferenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE29 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 MaterialsE6

10、0 Practice for Analysis of Metals, Ores, and RelatedMaterials by SpectrophotometryE135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE1024 Guide for Chemical Analysis of Metals and MetalBearing Ores by Flame Atomic Absorption Spectropho-tometry (Withdrawn 2004)3E

11、1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical Method2.2 ISO Standard:4ISO 5725 Precision of Test MethodsDetermination of Re-peatability and Reproducibility by Interlaboratory Tests1These test methods are under the jurisdiction of ASTM Committee E01

12、 onAnalytical Chemistry for Metals, Ores, and Related Materials and are the directresponsibility of Subcommittee E01.08 on Ni and Co and High Temperature Alloys.Current edition approved April 1, 2017. Published June 2017. Originallyapproved in 1994. Last previous edition approved in 2010 as E1587 10

13、. DOI:10.1520/E1587-17.2For 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 onthe ASTM website.3The last approved version of this his

14、torical standard is referenced onwww.astm.org.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis internati

15、onal standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committ

16、ee.13. Terminology3.1 For definitions of terms used in this test method, refer toTerminology E135.4. Significance and Use4.1 These test methods are primarily intended to test refinednickel metal for compliance with compositional specifications.It is assumed that all who use these test methods will b

17、e trainedanalysts capable of performing common laboratory proceduresskillfully and safely. It is expected that the analytical work willbe performed in a properly equipped laboratory under appro-priate quality control practices.5. Apparatus, Reagents, and Instrumental Practices5.1 Apparatus:5.1.1 Spe

18、cial apparatus and reagents required for eachdetermination are listed in the Apparatus section of each testmethod.5.1.2 Glass storage containers shall be of borosilicate glass.5.1.3 Plastic containers shall be polyethylene or preferablypolytetrafluoroethylene (PTFE).5.2 Reagents:5.2.1 Purity of Reag

19、entsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.5Other grades may be used,provided it is fir

20、st ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.5.2.2 Purity of WaterUnless otherwise indicated, refer-ences to water shall be understood to mean reagent water asdefined by Type II of Specification D1193.5.2.3 Reagent

21、s and their preparation are described in theReagents section in each test method.5.2.4 Instructions for the preparation of standard solutionsused in these test methods frequently call for measuring exactmasses of substances of known composition so that theconcentrations of the resulting standard sto

22、ck solutions can beexpressed using simple numbers. Small variations from thesespecified quantities are acceptable, provided that the trueweighed masses are used to calculate the concentration of theprepared solutions and then these calculated values are usedthroughout the test methods.5.3 Instrument

23、al PracticesInformation on the use of someinstrumental techniques employed in these test methods aredescribed in Practice E60 and in Guide E1024.6. 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

24、, specific precautionary informationis given in the Hazards sections and in special warningparagraphs.7. Sampling7.1 Sampling shall be carried out by a mutually acceptablemethod.7.2 The laboratory sample normally is in the form of apowder, granules, millings, or drillings and no further prepa-ration

25、 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 cleaned by washing with high-purity acetone anddrying in air.7.4 If the laboratory sample contains particles or pieces ofwidely varying sizes, the test s

26、ample should be obtained byriffling or coning and quartering techniques.8. Rounding Calculated Values8.1 Calculated values shall be rounded to the desired num-ber of places in accordance with the rounding method inPractice E29.SILVER, BISMUTH, CADMIUM, COBALT, COPPER,IRON, MANGANESE, LEAD, AND ZINC

27、BY FLAMEATOMIC ABSORPTION SPECTROMETRY9. Scope9.1 This test method applies to the determination of thesilver, bismuth, cadmium, cobalt, copper, iron, manganese,lead, and zinc contents of refined, wrought, and cast nickelmetal within the following ranges.Mass Fraction Range, %Element Method A Method

28、BSilver 0.0002 to 0.01 .Bismuth 0.0010 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 applicab

29、le to the independent deter-mination of any one or more of the elements listed withoutincluding all the elements specified in the calibration solutions.9.3 The lower level for iron can be extended to less than0.0025 % provided nickel metal containing less than 0.0001 %iron is used for preparation ca

30、libration solutions.9.4 The upper limit for the determination of cobalt andcopper can be raised to 2 % by a minor modification to the testmethod. For test samples containing greater than 0.25 % andless than 2 % of cobalt or copper, further dilutions of the testsolution with HNO3(1 + 19) may be made.

31、 The nickel contentof the calibration solutions should be matched with those of thetest solutions.9.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for the5Reagent Chemicals, American

32、Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see the United States Pharmacopeia andNational Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.E1587 172Development o

33、f International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.10. Summary of Test Method10.1 The sample is dissolved in dilute HNO3, excess acid isevaporated, and the solution diluted to a known volume. Thetest solution is as

34、pirated 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 compared with that from a set of calibrationsolutions of the same element in a matched nickel matrix.11. Interferences11.1 Elements

35、ordinarily present in nickel metal do notpresent spectral interferences in the atomic absorption analysis.11.2 For the determination of silver, take care to avoidcontamination of the sample and calibration solutions withchloride.11.3 Potential background absorption interference is elimi-nated by use

36、 of matched matrix calibration solutions preparedfrom high-purity nickel metal. See Note 1.NOTE 1In this test method, any effect of nonspecific absorption andlight scatter is compensated for by matching the matrix of the calibrationsolutions with the test solutions. Also, since the same lot of HNO3i

37、s usedfor both calibration and test solutions, the reagent blank is incorporated inthe calibration curve. Thus, the calibration curve may not pass through theorigin.12. Apparatus12.1 Atomic Absorption Spectrometer:12.1.1 The atomic absorption spectrometer used in this testmethod should meet the inst

38、rument performance parameters inaccordance with Guide E1024.12.1.2 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 instrument should be capable of using single-element hollow

39、 cathode or electrodeless discharge lampsoperated at currents recommended by the instrument manufac-turer.13. Reagents13.1 Bismuth, Standard Stock Solution (1mL=1mgBis-muth):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

40、.1.2 Add 40 mL of HNO3(1 + 1) and heat gently untildissolution is complete. Boil gently to expel oxides of nitrogenand cool. Transfer to a 1-L volumetric flask containing 160 mLof HNO3(1 + 1), dilute to volume with water, and mix. Storein a polyethylene or PTFE bottle. Use the same batch of HNO3thro

41、ughout the entire procedure.13.1.3 If inhomogeneity is suspected in the test sample, or ifthe sample pieces are relatively large, a larger sample massshould be used to prepare the test solution. Under suchcircumstances, a sample mass of 25 g in a final volume of1000-mL may be used. The amount of HNO

42、3should beincreased in proportion. Even larger sample masses can beused, with greater amounts of HNO3to prepare a moreconcentrated nickel test solution. However, an aliquot portionto correspond to a 5-g sample must be taken from such asolution and processed in accordance with the procedure givento g

43、ive a test solution containing 25 g/L of nickel to match thecalibration solutions.13.2 Cadmium, Standard Stock Solution (1mL=1mgCadmium)Transfer a 1.00-g sample of cadmium metal(purity, 99.9 % minimum), weighed to the nearest 0.001 g, to a600-mL beaker. Proceed as directed in 13.1.2.13.3 Cobalt, Sta

44、ndard Stock Solution (1mL=1mgCobalt)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 (1mL=1mgCopper)Transfer a 1.00-g sample of copper metal (purity,99.9 % minimum),

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

46、 Solution (1mg=1mgLead)Transfer a 1.00-g sample of lead metal (purity, 99.9 %minimum), weighed to the nearest 0.001 g, to a 600-mLbeaker.Proceed as directed in 13.1.2.13.7 Manganese, Standard Stock Solution (1 mL = 1 mgManganese)Transfer a 1.00-g sample of manganese metal(purity, 99.9 % minimum), we

47、ighed to the nearest 0.001 g, to a600-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 zinc.13.9 Silver, Standard Stock Solution (1mL=1mgSilver)Transf

48、er 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 amber glasscontainer.13.10 Zinc, Standard Stock Solution (1mL=1mgZinc)Transfer a 1.00-g sample of zinc metal (purity, 99.9 %minimum), weighe

49、d to the nearest 0.001 g, to a 600-mLbeaker.Proceed as directed in 13.1.2.13.11 Working Solutions:13.11.1 Mixed Analyte Standard Solution A (1mL=20gof silver, bismuth, cadmium, cobalt, copper, iron, manganese,and lead and 10 g of zinc)Using pipets, transfer 20.0 mL ofeach of the standard stock solutions for silver, bismuth,cadmium, cobalt, copper, iron, manganese, and lead and 10 mLof the standard stock solution for zinc to a 1-L volumetric flaskcontaining 160 mL of HNO3(1 + 1). Use the same batch ofHNO3throughout the entire procedure. Dilute