1、Designation: E2594 09 (Reapproved 2014)Standard Test Method forAnalysis of Nickel Alloys by Inductively Coupled PlasmaAtomic Emission Spectrometry (Performance-BasedMethod)1This standard is issued under the fixed designation E2594; the number immediately following the designation indicates the year
2、oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method describes the inductively coupledplasma
3、atomic emission spectrometric analysis of nickelalloys, such as specified by Committee B02, and havingchemical compositions within the following limits:ElementApplicationRange (%)Aluminum 0.011.00Boron 0.0010.050Calcium 0.0010.05Carbon 0.100.20Chromium 0.0133.0Cobalt 0.1020.0Copper 0.013.00Iron 0.01
4、50.0Lead 0.0010.01Magnesium 0.00010.100Manganese 0.013.0Molybdenum 0.0130.0Niobium 0.016.0Nickel 25.080.0Nitrogen 0.0010.20Oxygen 0.00010.003Phosphorous 0.0010.030Sulfur 0.00010.010Silicon 0.011.50Tantalum 0.0050.10Tin 0.0010.020Titanium 0.0016.0Tungsten 0.015.0Vanadium 0.011.0Zirconium 0.010.101.2
5、The following elements may be determined using thistest method. The test method user should carefully evaluate theprecision and bias statements of this test method to determineapplicability of the test method for the intended use.ElementQuantificationRange (%)Aluminum 0.0601.40Boron 0.0020.020Calciu
6、m 0.0010.003Copper 0.0100.52ElementQuantificationRange (%)Magnesium 0.0010.10Manganese 0.0020.65Niobium 0.0205.5Phosphorous 0.0040.030Tantalum 0.0100.050Tin 0.0020.018Titanium 0.0203.1Tungsten 0.0070.11Vanadium 0.0100.50Zirconium 0.0020.101.3 This test method has only been interlaboratory tested for
7、the elements and ranges specified. It may be possible to extendthis test method to other elements or different concentrationranges provided that method validation is performed thatincludes evaluation of method sensitivity, precision, and bias asdescribed in this document. Additionally, the validatio
8、n studymust evaluate the acceptability of sample preparation method-ology using reference materials or spike recoveries, or both.The user is cautioned to carefully evaluate the validation dataagainst the laboratorys data quality objectives. Method vali-dation of scope extensions is also a requiremen
9、t of ISO/IEC 17025.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 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 standar
10、d to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific warningstatements are given in 8.2.6.3 and safety hazard statements aregiven in Section 9.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reage
11、nt Water1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and is the directresponsibility of Subcommittee E01.08 on Ni and Co and High Temperature Alloys.Current edition approved June 1, 2014. Published June 2014. Origina
12、llyapproved in 2009. Last previous edition approved in 2009 as E2594 09. DOI:10.1520/E2594-09R14.2For 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 Docum
13、ent Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1E50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE55 Practice for Sampling
14、 Wrought Nonferrous Metals andAlloys for Determination of Chemical CompositionE88 Practice for Sampling Nonferrous Metals and Alloys inCast Form for Determination of Chemical CompositionE135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE1329 Practice for Verific
15、ation and Use of Control Charts inSpectrochemical AnalysisE1479 Practice for Describing and Specifying Inductively-Coupled Plasma Atomic Emission SpectrometersE1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE2027 Practice for Conducting Profic
16、iency Tests in theChemical Analysis of Metals, Ores, and Related Materials2.2 ISO Standards:3ISO/IEC 17025 General Requirements for the Competenceof Calibration and Testing LaboratoriesISO Guide 31 Reference MaterialsContents of Certificatesand LabelsISO Guide 34 General Requirements for the Compete
17、nce ofReference Material ProducersISO Guide 98-3 Uncertainty of Measurement Part 3: Guideto the Expression of Uncertainty in Measurement(GUM:1995), First Edition3. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, refer to Terminology E135.4. Summary of Test Method4.1 Sampl
18、es are dissolved in a mixture of mineral acids andthe resulting solutions are measured using inductively coupledplasma atomic emission spectrometry.5. Significance and Use5.1 This test method for the chemical analysis of nickelalloys is primarily intended to test material for compliance withspecific
19、ations such as those under jurisdiction of ASTMCommittee B02. It may also be used to test compliance withother specifications that are compatible with the test method.5.2 It is assumed that all who use this test method will betrained analysts capable of performing common laboratoryprocedures skillfu
20、lly and safely, and that the work will beperformed in a properly equipped laboratory.5.3 This is a performance-based test method that relies moreon the demonstrated quality of the test result than on strictadherence to specific procedural steps. It is expected thatlaboratories using this test method
21、 will prepare their own workinstructions. These work instructions will include detailedoperating instructions for the specific laboratory, the specificreference materials employed, and performance acceptancecriteria. It is also expected that, when applicable, each labora-tory will participate in pro
22、ficiency test programs, such asdescribed in Practice E2027, and that the results from theparticipating laboratory will be satisfactory.6. Interferences6.1 Practice E1479 describes the typical interferences en-countered during the inductively coupled plasma spectrometricanalysis of metal alloys. The
23、user is responsible for ensuringthe absence of or for compensating for interferences that maybias test results obtained using their particular spectrometer.6.2 The use of an internal standard may compensate for thephysical interferences resulting from differences betweensample and calibration soluti
24、ons transport efficiencies.6.3 Shifts in background intensity levels because of, forexample, recombination effects or molecular bandcontributions, or both, may be corrected by the use of anappropriate background correction technique. Direct spectraloverlaps are best addressed by selecting alternativ
25、e wave-lengths. Spectral interference studies should be conducted onall new matrices to determine the interference correctionfactor(s) that must be applied to concentrations obtained fromcertain spectral line intensities to minimize biases. Someinstrument manufacturers offer software options which m
26、ath-ematically correct for direct spectral overlaps, but the user iscautioned to carefully evaluate this approach to spectralcorrection.6.4 Modern instruments have software that allows compari-son of a sample spectrum to the spectrum obtained from ablank solution. The user of this test method must e
27、xamine thisinformation to ascertain the need for background correctionand the correct placement of background points.6.5 Table 1 suggests wavelengths that the user may use foranalysis of nickel alloys. Each line was used by at least onelaboratory during the interlaboratory phase of test methoddevelo
28、pment and provided statistically valid results. Informa-tion for the suggested analytical wavelengths was collectedfrom each laboratory and has been converted to wavelengths asannotated in the National Institute of Standards and Technol-ogy (NIST) Atomic Spectra Database.4In this database,wavelength
29、s of less than 200 nm were measured in vacuumand wavelengths greater than or equal to 200 nm were mea-sured in air. Software tables for individual instruments may listwavelengths somewhat differently, as instrument optical pathatmospheric conditions may vary.6.6 Information on potential spectral int
30、erfering elementswas provided by the laboratories participating in the interlabo-ratory study and may have originated from sources such asrecognized wavelength reference tables, instrument manufac-turers software wavelength tables, or an individual laborato-rys wavelength research studies, or combin
31、ations thereof.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.4Ralchenko, Yu, Kramida, A. E., Reader, J., and NIST ASD Team (2008). NISTAtomic Spectra Database (version 3.1.5), National Institute of Standards andTechnolo
32、gy, Gaithersburg, MD.Available online: http:/physics.nist.gov/asd3 2008,October 28.E2594 09 (2014)26.7 The user must verify that the selected wavelengthperforms acceptably in their lab, preferably during methodvalidation (see Section 15). The user also may choose to usemultiple wavelengths to help v
33、erify that line selection isoptimized for the particular alloy being determined. It isrecommended that when wavelengths and appropriate spectralcorrections are determined, the user of this test method shouldspecify this information or reference instrument programs thatinclude this information in the
34、ir laboratory analysis proce-dures.7. Apparatus7.1 Inductively Coupled Plasma Atomic EmissionSpectrometersUsed to perform analysis by this test methodmay conform to the specifications given in Practice E1479.Suitability of a specific instrument for testing to this testmethod will be established usin
35、g the performance criteriadescribed in 12.1. The sample introduction system shall becapable of handling solutions containing up to 5 % HF.7.2 Sample Preparation EquipmentMachine tools capableof removing surface oxides and other contamination from theas-received sample shall be used to produce chips
36、or millingsfor analysis.8. Reagents and Materials8.1 Reagents:8.1.1 Purity of ReagentsReagent 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 w
37、heresuch specifications are available.5Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.8.1.2 Purity of WaterUnless otherwise indicated, refer-ences to water shall be understo
38、od to mean reagent water asdefined by Type II of Specification D1193. The water purifi-cation method used must be capable of removal of all elementsin concentrations that might bias the test results.8.1.3 Internal StandardThe use of an internal standard isoptional. However, the use of an internal st
39、andard maycompensate for the physical interferences resulting from dif-ferences in sample and calibration solutions transport effi-ciency.8.2 Calibration Solutions:8.2.1 In this test method, calibration is based on laboratory-prepared, alloy matrix-matched calibration solutions. Alloymatrix-matched
40、calibration solutions are solutions that containthe approximate amounts of the major alloying elementsnickel, chromium, cobalt, molybdenum, and iron found intypical sample solutions. They are intended to model thephysical behavior of sample solutions in the plasma. Thematrix solutions are prepared w
41、ith starting materials of knownpurity and are then spiked with aliquots of single elementcertified reference material (CRM) solutions that contain theanalytes to be quantified. The CRMs shall be compliant withISO Guide 31 and ISO Guide 34. It may be possible to analyzedifferent alloys using common m
42、atrix-matched calibrationsolutions provided method validation studies demonstrate ac-ceptable data.8.2.2 Steps 8.2.3 and following describe the preparation ofalloy matrix-matched calibration solutions for analysis ofsample solutions that contain 1 g alloy/100 mL final dilution. Itis acceptable to va
43、ry the sample weight and final volume aslong as the users method demonstrates adequate sensitivityand precision (see 12.1).8.2.3 Calculate the nominal amounts of the alloying metalsnickel, chromium, cobalt, molybdenum, and iron in 1 g of the5Reagent Chemicals, American Chemical Society Specification
44、s, AmericanChemical Society, Washington, DC, www.chemistry.org. For suggestions on thetesting of reagents not listed by the American Chemical Society, see the UnitedStates Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention,Inc. (USPC), Rockville, MD, http:/www.usp.org.TABLE 1 Suggest
45、ed Wavelengths/InterferencesElementWavelength(nm)Potential InterferenceAluminum 396.152Aluminum 394.401 NickelAluminum 237.312Aluminum 176.638Aluminum 167.079Boron 182.641 Molybdenum, Cobalt, ChromiumBoron 182.591 Molybdenum, Cobalt, ChromiumBoron 136.246 CobaltCalcium 396.847Calcium 393.366 CobaltC
46、opper 327.396 Titanium, Niobium, GadoliniumCopper 224.700 Molybdenum, IronCopper 219.958 TantalumCopper 218.172Copper 217.894Copper 213.598Magnesium 383.829Magnesium 280.270 CobaltMagnesium 279.553Manganese 283.930Manganese 257.610 Cerium, Cobalt, TungstenNiobium 319.498Niobium 309.418 Chromium, Van
47、adiumNiobium 294.154 VanadiumNiobium 269.706Niobium 210.942Phosphorous 178.766Phosphorous 178.284 CobaltPhosphorous 177.495 Nickel, CopperTantalum 263.558 MolybdenumTantalum 240.063 Cobalt, Chromium, VanadiumTantalum 226.230Tin 189.991 TitaniumTin 175.800Tin 140.052Titanium 350.489Titanium 338.376Ti
48、tanium 337.280 NiobiumTitanium 323.228Titanium 321.827Tungsten 207.912Tungsten 202.999Vanadium 437.924Vanadium 375.087Vanadium 309.311Vanadium 292.464Vanadium 292.402Zirconium 357.247Zirconium 343.823 NiobiumZirconium 327.305 Chromium, EuropiumZirconium 256.887E2594 09 (2014)3alloy to be analyzed. U
49、se a source of each metal that containsa known, low concentration of each analyte to be determined.8.2.4 Calculate the amount of analyte contained in eachmatrix metal. This quantity of analyte will be present in thecalibration solutions. Total the amount of analyte from thesesources and adjust the stated concentration of each calibrationsolution accordingly.NOTE 1Powdered metals have been found acceptable for preparingmatrix solutions. Select powdered metals that do not exhibit excessivesurface oxidation. However, do not use
