1、Designation: E3047 16Standard Test Method forAnalysis of Nickel Alloys by Spark Atomic EmissionSpectrometry1This standard is issued under the fixed designation E3047; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last
2、 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 method describes the spark atomic emission spec-trometric (Spark-AES) analysis of nickel alloys, such as thosespecifi
3、ed by committee B02, having chemical compositionswithin the following limits:ElementApplicationRange (MassFraction, %)Aluminum 0.005-6.00Boron 0.001-0.10Carbon 0.005-0.15Chromium 0.01-33.00Copper 0.01-35.00Cobalt 0.01-25.00Iron 0.05-55.00Magnesium 0.001-0.020Manganese 0.01-1.00Molybdenum 0.01-35.00N
4、iobium 0.01-6.0Nickel 25.00-100.0Phosphorous 0.001-0.025Silicon 0.01-1.50Sulfur 0.0001-0.01Titanium 0.0001-6.0Tantalum 0.01-0.15Tin 0.001-0.020Tungsten 0.01-5.0Vanadium 0.0005-1.0Zirconium 0.01-0.101.2 The following elements may be determined using thismethod.ElementQuantificationRange (MassFraction
5、, %)Aluminum 0.010-1.50Boron 0.004-0.025Carbon 0.014-0.15Chromium 0.09-20.0Cobalt 0.05-14.00Copper 0.03-0.6Iron 0.17-20Magnesium 0.001-0.03Manganese 0.04-0.6Molybdenum 0.07-5.0Niobium 0.02-5.5ElementQuantificationRange (MassFraction, %)Phosphorous 0.005-0.020Silicon 0.07-0.6Sulfur 0.002-0.005Tantalu
6、m 0.025-0.15Tin 0.001-0.02Titanium 0.025-3.2Tungsten 0.02-0.10Vanadium 0.005-0.25Zirconium 0.01-0.051.3 This method has been interlaboratory tested for theelements and quantification ranges specified in section 1.2. Theranges in section 1.2 indicate intervals within which resultshave been demonstrat
7、ed to be quantitative. It may be possibleto extend this method to other elements or different composi-tion ranges provided that a method validation study as de-scribed in Guide E2857 is performed and that the results of thisstudy show that the method extension is meeting laboratorydata quality objec
8、tives. Supplemental data on other elementsnot included in the scope are found in the supplemental datatables of the Precision and Bias section.1.4 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
9、d to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific safetyhazard statements are given in Section 9.2. Referenced Documents2.1 ASTM Standards:2E29 Practice for Using Significant Digits in Test Data toDetermine Confo
10、rmance with SpecificationsE135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE305 Practice for Establishing and Controlling AtomicEmission Spectrochemical Analytical Curves1This test method
11、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 April 1, 2016. Published May 2016. DOI: 10.1520/E304716.2For referen
12、ced 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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Co
13、nshohocken, PA 19428-2959. United States1E406 Practice for Using Controlled Atmospheres in Spec-trochemical AnalysisE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE1257 Guide for Evaluating Grinding Materials Used forSurface Preparation in Spectrochem
14、ical AnalysisE1329 Practice for Verification and Use of Control Charts inSpectrochemical AnalysisE1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE2857 Guide for Validating Analytical MethodsE2972 Guide for Production, Testing, and Value Assign
15、mentof In-House Reference Materials for Metals, Ores, andOther Related Materials2.2 ISO Standard:3ISO/IEC Guide 98-3:2008 Uncertainty of MeasurementPart 3: Guide to the Expression of Uncertainty in Mea-surement (GUM:1995)3. Terminology3.1 DefinitionsFor definitions of terms used in thisPractice, ref
16、er to Terminology E135.4. Summary of Test Method4.1 Acontrolled electrical discharge is produced in an argonatmosphere between the prepared flat surface of a specimenand the tip of a counter electrode. The energy of the dischargeis sufficient to ablate material from the surface of the specimen,break
17、 the chemical or physical bonds, and cause the resultingatoms or ions to emit radiant energy. The radiant energy isdispersed by a grating and energies of selected analytical linesand the internal standard line(s) are converted into electricalsignals by either photomultiplier tubes (PMTs) or a suitab
18、lesolid state detector. The detected analyte signals are integratedand converted to an intensity value. A ratio of the detectedanalyte intensity and the internal standard signal may be made.A calibration is made using a suite of reference materials withcompositional similarity to the specimens being
19、 analyzed.Calibration curves plotting analyte intensity (intensity ratio)versus analyte mass fraction are developed. Specimens aremeasured for analyte intensity and results in mass fraction aredetermined using the calibration curves.5. Significance and Use5.1 This test method for the chemical analys
20、is of nickelalloys is primarily intended to test material for compliance withcompositional specifications such as those under jurisdiction ofASTM committee B02. It may also be used to test compliancewith other specifications that are compatible with the testmethod.5.2 It is assumed that all who use
21、this method will be trainedanalysts capable of performing common laboratory proceduresskillfully and safely, and that the work will be performed in aproperly equipped laboratory.5.3 It is expected that laboratories using this method willprepare their own work instructions. These work instructionswil
22、l include detailed operating instructions for the specificlaboratory including information such as applicable analyticalmethods, drift correction (standardization) protocols, verifiers,and performance acceptance criteria.6. Interferences6.1 When possible, select analytical lines which are freefrom s
23、pectral interferences. However, this is not alwayspossible, and it may be necessary to apply interelementcorrections to account mathematically for the effect of theinterference on the measured intensities. If interference correc-tions are necessary, refer to Practice E305 for detailed infor-mation o
24、n the various techniques used to calculate interferencecorrections.6.2 Table 1 lists analytical lines routinely used for analysisof nickel alloys. For consistency of expression, the wave-lengths are all listed as stated in the National Institute ofStandards and Technology (NIST) Atomic Spectroscopy
25、Data-base.4In the NIST wavelength table, wavelengths 200 nmare as determined in a vacuum and wavelengths of 200 nmare as determined in air. Interference corrections, as reportedby the interlaboratory study participants, are also indicated. Itis not implied that analyses using this standard test meth
26、odmust be made with the same atmospheric conditions as statedfor the NIST stated wavelengths. Performance of the analyticalline selected should be evaluated during method developmentfor sensitivity and potential interferences.7. Apparatus7.1 Spark Atomic Emission Spectrometer, containing thefollowin
27、g basic components.7.1.1 Spark SourceThe excitation source uses computersoftware which typically produces: (1) a high-energy pre-spark(of some preset duration), (2) a spark-type discharge (of somepreset duration), (3) an arc type discharge (of some presetduration), and (4) a spark-type discharge, du
28、ring which, timeresolved measurements are made for improved detectionlimits, (this may be optional on some instruments). Thecounter-electrode serves as a conduction path for the highvoltage discharge. The counter-electrode configuration/composition is typically specified by the instrument manufac-tu
29、rer.7.1.2 Analytical StandCapable of supporting the speci-men and counter-electrode in a manner such that the dischargeof the spark source may conduct through the flat, uniformsurface of a prepared specimen. Additionally, the stand isdesigned to work in conjunction with the gas flow system.7.1.3 Gas
30、 Flow SystemDesigned to deliver pure argon gasto the spark discharge, specimen interface region. Use theminimum argon purity specified by the instrument manufac-turer. Refer to Practice E406 for practical guidance on the useof controlled atmospheres.3Available from American National Standards Instit
31、ute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.4Kramida, A., Ralchenko, Yu., Reader, J., and NIST ASD Team (2014). NISTAtomic Spectra Database (ver. 5.2), Online. Available: http:/physics.nist.gov/asd2015, July 29. National Institute of Standards and Technology, Gaither
32、sburg, MD.E3047 1627.1.4 SpectrometerHaving acceptable dispersion,resolution, and wavelength coverage for the determination ofnickel alloys. Table 1 provides guidance on the wavelengthsthat may be required.7.1.5 Optional Optical Path Purge or Vacuum SystemDesigned to enhance ultraviolet wavelength s
33、ensitivity byeither purging the optical path with a UV-transparent gas or byevacuating the optical path to remove air. The UV-transparentgas shall meet the manufacturers minimum suggested purityrequirements. Typically, the sum of the residual O2and H2Oimpurities in the UV-transparent gas should not
34、exceed 2mol/mol (ppm).7.1.6 Measuring and Control SystemsDesigned to convertemitted light intensities to a measurable electrical signal. Thesesystems will consist of either a series of photomultiplier tubes(PMT) or solid-state photosensitive arrays (Charge CoupledDevice (CCD) or Charge Injection Dev
35、ice (CID) and integrat-ing electronics. Dedicated computer software is used to controlanalytical method conditions, source operation, dataacquisition, and the conversion of intensity data to massfraction.7.1.7 Other SoftwareDesigned to coordinate instrumentfunction. At a minimum, the instruments sof
36、tware shouldinclude functions for calibration, routine instrument drift cor-rection (standardization) and routine measurement. Additionalsoftware features may include functionality for tasks such ascontrol charting.7.2 Specimen Preparation EquipmentA grinder or lathecapable of machining nickel alloy
37、 specimens to produce aclean, flat analytical surface.8. Reagents and Materials8.1 Reference Materials (RMs):8.1.1 Certified Reference Materials (CRMs) should be usedas calibration reference materials (RMs), if available. Thesecertified reference materials should be of similar compositionTABLE 1 Ana
38、lytical Lines for the Analysis of Nickel Alloys and Potential InterferencesElement Wavelength, nm Potential Interference Element Wavelength, nm Potential InterferenceAluminum 308.22 Cr, Mo, Nb, Ti Nickel 150.00Aluminum 309.28 Cu, Fe, Mo, Nb, Nickel 166.66Aluminum 394.40 Co, Cr, Cu, Fe, Mo,Nb, Si, WN
39、ickel 182.31Aluminum 616.43 Nickel 208.08Arsenic 189.04 Fe Nickel 210.58Boron 182.64 Co, Cr, Fe, Mn, Mo,Ti, WNickel 214.78Boron 345.13 Nickel 218.55Calcium 396.85 Nickel 226.14Calcium 393.37 Fe Nickel 232.27Carbon 193.09 Al, Fe Nickel 243.79Carbon 165.70 Fe Nickel 282.13Cobalt 228.62 Cr, Fe, Mo, Nb,
40、 W, Ti, Nickel 301.91Cobalt 258.03 Fe, Mo,Nb, W Nickel 304.50Cobalt 345.35 Cr, Fe, ,Mo,Nb,Ti, W, Nickel 309.71Cobalt 384.55 Cr,Fe,Mo,Ti,W Nickel 310.55Cobalt 184.59 Al, Fe Ti, Nickel 346.95Chromium 267.72 Cu, Mo, Nb Nickel 376.95Chromium 298.92 Al,Co,Fe,Ti,W Nickel 380.71Copper 199.97 Fe, Mo, Nb Nic
41、kel 471.44Copper 212.30 Co, Mn, Ti, Si, Sn Phosphorous 177.49 Cu, Mo, Nb, WCopper 224.26 Ni, W Phosphorous 178.28 Cr, Fe, Mo, Nb, WCopper 282.44 Silver 338.29 Co, CrCopper 324.75 Fe, Nb, W Silver 328.07 MoCopper 510.55 Co, Cr,Mo,Nb, W, Silicon 212.41 Cr, Co, Fe, Mo, Nb,WIron 260.02 Co, Cr, Cu, W Sil
42、icon 288.16 Al, CrIron 273.07 Co,Cr,Ti,W,Mo, Nb Sulfur 180.73 Al, Co, Cr, Mn, Mo,Nb, Ni, Ti, WIron 275.57 Al, Co, Cu,Mn, Mo, NbTi, W,Tantalum 240.06 CoIron 371.99 Tantalum 293.27 Cr, Nb, Ni, WIron 492.39 Tantalum 331.12 Cr, Nb, W, ZrMagnesium 279.08 Fe Tin 189.99 Cr, Mo,Nb, Ti,VManganese 263.82 Al,
43、Cr, Fe, Mo, W Tin 300.91 Cr, Fe, MoManganese 273.09 Cr, Fe, Ti Tin 317.50 FeManganese 293.93 Titanium 308.81 Co, Cu, Fe, Mo, W,Molybdenum 202.03 Cr, Mn, Ni, W Titanium 324.20 Co, Cr, Fe, Mo,Nb,WMolybdenum 281.61 Al, Co, Cr, Fe Vanadium 311.07 Al, Co, Cr, Cu, Fe,Mo, Nb, Ti,Molybdenum 290.91 Cr, Fe, W
44、 Tungsten 220.45 Al, Co, Cr, MoMolybdenum 308.76 Cr, Fe, W Tungsten 400.90 Co, Cr, Fe, Mo, Nb, TiMolybdenum 369.26 Fe Zirconium 343.82 Co, Cr, Fe, Mo, Ta, Ti,WNiobium 319.50 W Zirconium 349.62 Co, Cr, Mn, MoZirconium 468.84E3047 163to the alloys being analyzed. In cases where CRMs are notavailable f
45、or the element and/or alloy being analyzed or ifavailable CRMs do not adequately cover the intended analyti-cal range, it is acceptable to use other reference materials forcalibration.8.1.2 In-house RMsSome laboratories may have the re-sources to produce in-house RMs for nickel alloys. It isacceptab
46、le to use these RMs for calibration of Spark-AESinstruments provided that the in-house RMs have been devel-oped following technically sound development protocols, suchas those described in Practice E2972.8.1.3 Instrument Manufacturer Provided RMsSomemanufacturers perform factory calibrations which m
47、ay includereference materials owned by the manufacturer. The laboratoryshould make reasonable attempts to secure certificates ofanalysis for each of these RMs and to evaluate the acceptabilityof these certificates in conjunction with the laboratorys qualitypolicies.8.2 Grinding MediaIf grinding is u
48、sed as the specimenpreparation technique, belts or disks of appropriate grit shall beprovided. Aluminum oxide and silicon carbide based abrasivematerials have been found to be acceptable for grinding nickelalloys. Typically 60 grit or finer abrasive materials are found tobe acceptable. Guide E1257 m
49、ay be consulted for guidance inevaluating grinding materials.8.3 Lathe ToolingIf lathe turning is used for specimenpreparation then tools appropriate for cutting nickel alloys shallbe provided.8.4 Drift Correction (Standardization) SamplesSelect asuite of drift correction samples. This suite of samples shouldbe of similar composition to the alloys being analyzed andshould contain analyte levels near the extremes of the calibra-tion range for each analyte. Drift correction involves a calcu-lated adjustment to calibration slope and intercept based onint
