1、Designation: E 2594 09Standard Test Method forAnalysis of Nickel Alloys by Inductively Coupled PlasmaAtomic Emission Spectrometry (Performance-BasedMethod)1This standard is issued under the fixed designation E 2594; the number immediately following the designation indicates the year oforiginal adopt
2、ion 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 atomic emission
3、spectrometric analysis of nickel al-loys, such as specified by Committee B02, and having chemi-cal 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 0.0150.0Lead 0.0
4、010.01Magnesium 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 The followin
5、g 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 0.0020.020Calcium 0.0010.003
6、Copper 0.0100.52Magnesium 0.0010.10Manganese 0.0020.65Niobium 0.0205.5ElementQuantificationRange (%)Phosphorous 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 forthe elements
7、 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 validation studymust
8、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 requirement of ISO/IEC
9、 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 standard to establi
10、sh 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:2D 1193 Specification for Reagent WaterE50
11、 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE55 Practice for Sampling Wrought Nonferrous Metals and1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Mate
12、rials and is the directresponsibility of Subcommittee E01.08 on Ni and Co and High Temperature Alloys.Current edition approved March 15, 2009. Published April 2009.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Boo
13、k of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Alloys for Determination of Chemical CompositionE88 Practice for Sampling Nonferro
14、us Metals and Alloysin Cast Form for Determination of Chemical CompositionE 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE 1329 Practice for Verification and Use of Control Chartsin Spectrochemical AnalysisE 1479 Practice for Describing and Specifying Induct
15、ively-Coupled Plasma Atomic Emission SpectrometersE 1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE 2027 Practice for Conducting Proficiency Tests in theChemical Analysis of Metals, Ores, and Related Materials2.2 ISO Standards:3ISO/IEC 17025
16、General Requirements for the Competenceof Calibration and Testing LaboratoriesISO Guide 31 Reference MaterialsContents of Certifi-cates and LabelsISO Guide 34 General Requirements for the Competence ofReference Material ProducersISO Guide 98-3 Uncertainty of Measurement Part 3: Guideto the Expressio
17、n of Uncertainty in Measurement(GUM:1995), First Edition3. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, refer to Terminology E 135.4. Summary of Test Method4.1 Samples are dissolved in a mixture of mineral acids andthe resulting solutions are measured using inductively
18、 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 withspecifications such as those under jurisdiction of ASTMCommittee B02. It may also be used to test compliance wit
19、hother 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 skillfully and safely, and that the work will beperformed in a properly equipped laboratory.5.3 This is a perfo
20、rmance-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 will prepare their own workinstructions. These work instructions will include detailedoperating instruc
21、tions for the specific laboratory, the specificreference materials employed, and performance acceptancecriteria. It is also expected that, when applicable, each labora-tory will participate in proficiency test programs, such asdescribed in Practice E 2027, and that the results from theparticipating
22、laboratory will be satisfactory.6. Interferences6.1 Practice E 1479 describes the typical interferences en-countered during the inductively coupled plasma spectrometricanalysis of metal alloys. The user is responsible for ensuringthe absence of or for compensating for interferences that maybias test
23、 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 solutions transport efficiencies.6.3 Shifts in background intensity levels because of, forexample, recombina
24、tion effects or molecular band contribu-tions, or both, may be corrected by the use of an appropriatebackground correction technique. Direct spectral overlaps arebest addressed by selecting alternative wavelengths. Spectralinterference studies should be conducted on all new matrices todetermine the
25、interference correction factor(s) that must beapplied to concentrations obtained from certain spectral lineintensities to minimize biases. Some instrument manufacturersoffer software options which mathematically correct for directspectral overlaps, but the user is cautioned to carefully evaluatethis
26、 approach to spectral correction.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 examine thisinformation to ascertain the need for background correctionand the correct placement of back
27、ground 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 methoddevelopment and provided statistically valid results. Informa-tion for the suggested analytical wavelengths w
28、as 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,wavelengths of less than 200 nm were measured in vacuumand wavelengths greater than or equal to 200 nm were mea-s
29、ured in air. Software tables for individual instruments may listwavelengths somewhat differently, as instrument optical pathatmospheric conditions may vary.6.6 Information on potential spectral interfering elementswas provided by the laboratories participating in the interlabo-ratory study and may h
30、ave originated from sources such asrecognized wavelength reference tables, instrument manufac-turers software wavelength tables, or an individual laborato-rys wavelength research studies, or combinations thereof.6.7 The user must verify that the selected wavelengthperforms acceptably in their lab, p
31、referably during methodvalidation (see Section 15). The user also may choose to usemultiple wavelengths to help verify that line selection isoptimized for the particular alloy being determined. It isrecommended that when wavelengths and appropriate spectralcorrections are determined, the user of thi
32、s test method should3Available 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 NISTASD Team (2008). NISTAtomic Spectra Database (version 3.1.5), National Institute of Standards andTechn
33、ology, Gaithersburg, MD.Available online: http:/physics.nist.gov/asd3 2008,October 28.E2594092specify this information or reference instrument programs thatinclude this information in their laboratory analysis proce-dures.7. Apparatus7.1 Inductively Coupled Plasma Atomic EmissionSpectrometersUsed to
34、 perform analysis by this test methodmay conform to the specifications given in Practice E 1479.Suitability of a specific instrument for testing to this testmethod will be established using the performance criteriadescribed in 12.1. The sample introduction system shall becapable of handling solution
35、s containing up to 5 % HF.7.2 Sample Preparation EquipmentMachine tools ca-pable of removing surface oxides and other contaminationfrom the as-received sample shall be used to produce chips ormillings for analysis.8. Reagents and Materials8.1 Reagents:8.1.1 Purity of ReagentsReagent grade chemicals
36、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 first ascertained that the reag
37、ent 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 understood to mean reagent water asdefined by Type II of Specification D 1193. The water purifi-cation method used mus
38、t 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 standard maycompensate for the physical interferences resulting from dif-ferences in sample and calibration sol
39、utions 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 calibration solutions are solutions that containthe approximate amounts of the major alloying elementsnickel,
40、 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 with starting materials of knownpurity and are then spiked with aliquots of single elementcertified reference
41、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 matrix-matched calibrationsolutions provided method validation studies demonstrate ac-ceptable data.8.2.2 Step
42、s 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 vary the sample weight and final volume aslong as the users method demonstrates adequate sensitivityand precisi
43、on (see 12.1).8.2.3 Calculate the nominal amounts of the alloying metalsnickel, chromium, cobalt, molybdenum, and iron in 1 g of thealloy to be analyzed. Use a source of each metal that containsa known, low concentration of each analyte to be determined.8.2.4 Calculate the amount of analyte containe
44、d 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 preparing5Reagent Chemicals, Ame
45、rican Chemical Society Specifications, AmericanChemical Society, Washington, DC, http:/pubs.acs.org/reagents/index.html. Forsuggestions on the testing of reagents not listed by the American Chemical Society,see the United States Pharmacopeia and National Formulary, U.S. PharmacopeialConvention, Inc.
46、 (USPC), Rockville, MD, http:/www.usp.org.TABLE 1 Suggested 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, ChromiumB
47、oron 136.246 CobaltCalcium 396.847Calcium 393.366 CobaltCopper 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, Cob
48、alt, TungstenNiobium 319.498Niobium 309.418 Chromium, VanadiumNiobium 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 Titaniu
49、mTin 175.800Tin 140.052Titanium 350.489Titanium 338.376Titanium 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 256.887E2594093matrix solutions. Select powdered metals that do not exhibit excessivesurface oxidation. However, do not use powdered metals to make analyteadditions as oxidation can lead to significant error in the amount o
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