1、Designation: E2371 13Standard Test Method forAnalysis of Titanium and Titanium Alloys by Direct CurrentPlasma and Inductively Coupled Plasma Atomic EmissionSpectrometry (Performance-Based Test Methodology)1This standard is issued under the fixed designation E2371; the number immediately following th
2、e designation indicates the year 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 method describes th
3、e analysis of titanium andtitanium alloys, such as specified by committee B10, byinductively coupled plasma atomic emission spectrometry(ICP-AES) and direct current plasma atomic emission spec-trometry (DCP-AES) for the following elements:ElementApplicationRange (wt.%)QuantitativeRange (wt.%)Aluminu
4、m 08 0.009 to 8.0Boron 00.04 0.0008 to 0.01Cobalt 0-1 0.006 to 0.1Chromium 05 0.005 to 4.0Copper 00.6 0.004 to 0.5Iron 03 0.004 to 3.0Manganese 00.04 0.003 to 0.01Molybdenum 08 0.004 to 6.0Nickel 01 0.001 to 1.0Niobium 0-6 0.008 to 0.1Palladium 0-0.3 0.02 to 0.20Ruthenium 0-0.5 0.004 to 0.10Silicon
5、00.5 0.02 to 0.4Tantalum 0-1 0.01 to 0.10Tin 04 0.02 to 3.0Tungsten 0-5 0.01 to -0.10Vanadium 015 0.01 to 15.0Yttrium 00.04 0.001 to 0.004Zirconium 05 0.003 to 4.01.2 This test method has been interlaboratory tested for theelements and ranges specified in the quantitative range part ofthe table abov
6、e. It may be possible to extend this test methodto other elements or broader mass fraction ranges as shown inthe application range part of the table above provided that testmethod validation is performed that includes evaluation ofmethod sensitivity, precision, and bias. Additionally, the vali-datio
7、n study shall evaluate the acceptability of sample prepa-ration methodology using reference materials or spike recov-eries or both. Guide E2857 provides information on validationof analytical methods for alloy analysis.1.3 Because of the lack of certified reference materials(CRMs) containing bismuth
8、, hafnium, and magnesium, theseelements were not included in the scope or the interlaboratorystudy (ILS). It may be possible to extend the scope of this testmethod to include these elements provided that method vali-dation includes the evaluation of method sensitivity, precision,and bias during the
9、development of the testing method.1.4 UnitsThe values stated in SI units are to be regardedas the standard. No other units of measurement are included inthis standard.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of
10、the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific safetyhazards statements are given in Section 9.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE50 Practi
11、ces for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE1097 Guide for Determination of Various Elements byDirect Current Plasma Atomic Emission Spectro
12、metryE1329 Practice for Verification 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 MethodE1763
13、 Guide for Interpretation and Use of Results fromInterlaboratory Testing of Chemical Analysis Methods1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and is the directresponsibility of Subcommittee E01.06 on Ti, Zr, W, M
14、o, Ta, Nb, Hf, Re.Current edition approved June 15, 2013. Published June 2013. Originallyapproved in 2004. Last previous edition approved in 2004 as E2371 - 04, which waswithdrawn in January 2013 and reinstated in June 2013. DOI: 10.1520/E2371-13.2For referenced ASTM standards, visit the ASTM websit
15、e, 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 Conshohocken, PA 19428-2959. United States1
16、E1832 Practice for Describing and Specifying a DirectCurrent Plasma Atomic Emission SpectrometerE2027 Practice for Conducting Proficiency Tests in theChemical Analysis of Metals, Ores, and Related MaterialsE2626 Guide for Spectrometric Analysis of Reactive andRefractory MetalsE2857 Guide for Validat
17、ing Analytical Methods2.2 ISO Standards:3ISO/IEC 17025 Requirements for the Competence of Cali-bration and Test LaboratoriesISO Guide 31 Reference MaterialsContents of Certificatesand LabelsISO Guide 34 General Requirements for the Competence ofReference Material ProducersISO Guide 98-3 Uncertainty
18、of measurement Part 3: Guideto the Expression of Uncertainty in Measurement (GUM:1995)First Edition3. Terminology3.1 For definitions of terms used in this test method, refer toTerminology E135.4. Summary of Test Method4.1 Amineral acid solution of the sample is aspirated into aninductively coupled p
19、lasma (ICP) or direct current plasma(DCP) spectrometer. The intensities of emission lines from thespectra of the analytes are measured and compared withcalibration curves obtained from solutions containing knownamounts of pure elements.5. Significance and Use5.1 This test method for the chemical ana
20、lysis of titaniumand titanium alloys is primarily intended to test material forcompliance with specifications of chemical composition suchas those under the jurisdiction of ASTM Committee B10. Itmay also be used to test compliance with other specificationsthat are compatible with the test method.5.2
21、 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 performance-based test method that relies moreon the demonstrated qualit
22、y 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 instructions for the specific laboratory, the specificreference materials
23、used, and performance acceptance criteria.It is also expected that, when applicable, each laboratory willparticipate in proficiency test programs, such as described inPractice E2027, and that the results from the participatinglaboratory will be satisfactory.6. Interferences6.1 In Practice E1479, the
24、 typical interferences encounteredduring inductively coupled plasma spectrometric analysis ofmetal alloys are described. In Guide E1097, the typicalinterferences encountered during direct current plasma emis-sion spectrometric analysis of metal alloys are described. Theuser is responsible for ensuri
25、ng the absence of, or compensat-ing for, interferences that may bias test results obtained usingtheir 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
26、 Shifts in background intensity levels because of recom-bination effects or molecular band contributions or both may becorrected by the use of an appropriate background correctiontechnique. Direct spectral overlaps are best addressed byselecting alternative wavelengths. Spectral interference studies
27、should be conducted on all new matrices to determine theinterference correction factor(s) that shall be applied to con-centrations obtained from certain spectral line intensities tominimize biases. Some instrument manufacturers offer soft-ware options that mathematically correct for direct spectralo
28、verlaps, but the user is cautioned to evaluate carefully thisapproach 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 shall examine thisinformation to ascertain the ne
29、ed for background correctionand the correct placement of background points.6.5 In Table 1, wavelengths that may be used for analysis oftitanium alloys are suggested. Each line was used by at leastone laboratory during the interlaboratory phase of test methoddevelopment and provided statistically val
30、id results.Additionalelements and wavelengths may be added if proficiency isdemonstrated. Information for the suggested analytical wave-lengths was collected from each laboratory and has beenconverted to wavelengths as annotated in the NIST AtomicSpectra Database.4In this database, wavelengths of le
31、ss than200 nm were measured in vacuum and wavelengths greaterthan or equal to 200 nm were measured in air.Additionally, theMIT Wavelength Tables5were used. Tables for individualinstruments may list wavelengths somewhat differently, asinstrument optical path atmospheric conditions may vary.6.6 Inform
32、ation on potential spectral interfering elementswas provided by the laboratories participating in the interlabo-ratory study (ILS) and may have originated from sources suchas recognized wavelength reference tables, instrument manu-facturers software wavelength tables, and/or an individuallaboratorys
33、 wavelength research studies.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 NISTASD Team, NIST AtomicSpectra Database (version 3.1.5), 2008, online. Available: http:/physi
34、cs.nist.gov/asd3 2008, October 28. National Institute of Standards and Technology,Gaithersburg, MD.5Harrison, G. R., MIT Wavelength Tables, John Wiley the details are given in ASTM Research Report No.E01-1112.18.2 A new study was performed in 2011 to demonstratemethod precision and bias for an expan
35、ded scope. Additionalanalytes included cobalt, lead, niobium, palladium, ruthenium,tantalum, and tungsten. In Tables 16-21, the summaries of datafor this additional study are presented. Nine laboratories wereasked to report triplicate results, for six elements, obtainedfrom five different titanium a
36、lloy samples. One laboratoryE2371 136TABLE 2 Aluminum in Titanium and Titanium Alloys by Atomic Emission SpectrometryTestMaterialNumber ofLaboratoriesAluminumFound, %Minimum SD(sM, E1479)Reproducibility SD(sR, E1479)Reproducibility Index(R, E1479)Rrel%6541326666660.0003830.03390.0993.1366.4357.7230.
37、0008040.0009690.001680.03710.04780.05890.001610.002990.005450.06320.1330.1280.004510.008390.01520.1770.3730.3591177.24.715.45.65.84.6TestMaterialCertifiedAluminum, %Bias, %Material Identification(Source)Description(Uncertainty or Standard Deviation)1234563.087.636.360.0960.0310.00010.0830.1020.0750.
38、0030.00290.000283NIST 649NIST 2433NIST 173bHTL 572HTL AA16#4HTL 559Ti-15V-3Al-3Cr-3Sn (0.02)Ti-8Al-1Mo-1V (0.05)Ti-6Al-4V (0.04)TIMET ILT, Ti-CP (0.009)TIMET Internal, Ti-CP (0.001)TIMET Electro-refined (no data)NoteThe General Analytical Error model estimates relative errors decrease above 0.1 % Al
39、 to a minimum of 5.2 %.TABLE 3 Boron in Titanium and Titanium Alloys by Atomic Emission SpectrometryTestMaterialNumber ofLaboratoriesBoronFound, %Minimum SD(sM, E1479)Reproducibility SD(sR, E1479)Reproducibility Index(R, E1479)Rrel%341265750.0000950.004870.004880.008220.0000940.0004580.0000760.00039
40、30.0001370.0004620.0003400.0004800.0003840.001290.000950.00134404.26.619.516.3TestMaterialCertifiedBoron, %Bias, %Material Identification(Source)Description(Uncertainty or Standard Deviation)12340.00480.00930.00010.00520.00007-0.001080.0000-0.00033HTL 572HTL AA16#4HTL 559HTL 573TIMET ILT, Ti-CP (0.0
41、09)TIMET Internal, Ti-CP (0.001)TIMET Electro-refined (no data)TIMET ILT, Ti-6Al-4V (0.0003)NoteThe General Analytical Error model estimates relative errors decrease above 0.002 % to a minimum of 18.5 %.TABLE 4 Chromium in Titanium and Titanium Alloys by Atomic Emission SpectrometryTestMaterialNumbe
42、r ofLaboratoriesChromiumFound, %Minimum SD(sM, E1479)Reproducibility SD(sR, E1479)Reproducibility Index(R, E1479)Rrel%432155550.000350.01490.02453.8090.0003350.0001910.0002030.018780.0008620.0006000.0016330.033630.002410.001680.004570.0942692.11.318.72.47TestMaterialCertifiedChromium, %Bias, %Materi
43、al Identification(Source)Description(Uncertainty or Standard Deviation)12343.840.0250.01450.0003-0.031-0.00050.00040.00005NIST 648NIST 173bHTL 572HTL 559Ti-5Al-2Sn-2Zr-4Cr-4Mo (0.03)Ti-6Al-4V (NIST 654B, 0.002)TIMET ILT, Ti-CP (0.0005)TIMET Electro-refined (no data)NoteThe General Analytical Error m
44、odel estimates relative errors decrease above 0.1 % Cr to a minimum of 2.5 %.TABLE 5 Copper in Titanium and Titanium Alloys by Atomic Emission SpectrometryTestMaterialNumber ofLaboratoriesCopperFound, %Minimum SD(sM, E1479)Reproducibility SD(sR, E1479)Reproducibility Index(R, E1479)Rrel%41352577660.
45、0003530.004100.02060.02110.4730.000380.000330.000570.000580.009380.000660.001700.002810.002150.02180.001850.004760.007860.006010.0610524.116.38.228.512.9TestMaterialCertifiedCopper, %Bias, %Material Identification(Source)Description(Uncertainty or Standard Deviation)123450.0080.490.0250.00010.025-0.
46、0039-0.017-0.00440.0003-0.0039NIST 173bIARM-178AHTL 572HTL 559HTL 573Ti-6Al-4V(0.001) NIST 654B(0.0040.001)ARMI RM Ti-6Al-6V-2Sn (0.028)TIMET ILT, Ti-CP (0.003)TIMET Electro-refined (no data)TIMET ILT, Ti-6Al-4V (0.001)NoteThe General Analytical Error model estimates relative errors decrease above 0
47、.015 % Cu to a minimum of 13 %.E2371 137TABLE 6 Iron in Titanium and Titanium Alloys by Atomic Emission SpectrometryTestMaterialNumber ofLaboratoriesIronFound, %Minimum SD(sM, E1479)Reproducibility SD(sR, E1479)Reproducibility Index(R, E1479)Rrel%432166660.001880.04440.2271.7060.000150.000920.001960
48、.01080.000730.001440.006960.02050.002030.004040.01950.0575108.9.18.63.37TestMaterialCertifiedIron, %Bias, %Material Identification(Source)Description(Uncertainty or Standard Deviation)12341.770.230.0480.0011-0.064-0.003-0.00360.00078NIST 2432NIST 173bHTL 572HTL 559Ti-10V-2Fe-3Al (0.05)Ti-6Al-4V (0.0
49、1)TIMET ILT, Ti-CP (0.003)TIMET Electro-refined (no data)NoteThe General Analytical Error model estimates relative errors decrease above 0.06 % Fe to a minimum of 3.5 %.TABLE 7 Manganse in Titanium and Titanium Alloys by Atomic Emission SpectrometryTestMaterialNumber ofLaboratoriesManganseFound, %Minimum SD(sM, E1479)Reproducibility SD(sR, E1479)Reproducibility Index(R, E1479)Rrel%43125555-0.000710.003880.004200.012770.0000080.0000300.0000430.0001240.000560.000460.000500.000410.001570.001280.001400.00115219.33.033.39.0TestMaterialCertifiedManganse, %Bias,
