1、Designation: E 539 07Standard Test Method forX-Ray Fluorescence Spectrometric Analysis of 6Al-4VTitanium Alloy1This standard is issued under the fixed designation E 539; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of l
2、ast revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method2covers the X-ray fluorescence analysisof 6Al-4V titanium alloy for the following elements in therange
3、s indicated:Element Concentration Range, %Aluminum 4.6 to 7.2Chromium 0.023 to 0.071Copper 0.015 to 0.066Iron 0.1 to 0.3Manganese 0.009 to 0.068Molybdenum 0.018 to 0.072Nickel 0.026 to 0.073Silicon 0.03 to 0.06Tin 0.016 to 0.076Vanadium 2.6 to 5.4Zirconium 0.009 to 0.0641.2 This standard does not pu
4、rport to address all of 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. Specific precau-tionary statements are give
5、n in Section 10.2. Referenced Documents2.1 ASTM Standards:3E 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE 1172 Practice for Describing and Specifying aWavelength-Dispersive X-Ray SpectrometerE 1329 Practice for Verification and Use of Control Chartsin Spec
6、trochemical AnalysisE 1361 Guide for Correction of Interelement Effects inX-Ray Spectrometric AnalysisE 1621 Guide for X-Ray Emission Spectrometric Analysis3. Terminology3.1 Definitions:3.1.1 For definitions of terms used in this test method, referto Terminology E 135.4. Summary of Test Method4.1 Th
7、e specimen is finished to a clean, uniform surface andthen irradiated by high energy X-ray photons. Secondary X-rays are produced and emitted from the sample. This radiationis diffracted by means of analyzing crystals and focused on adetector which measures the count rates at specified wave-lengths.
8、 The outputs of the detectors in voltage pulses areintegrated or counted. Radiation measurements are made basedon the time required to reach a fixed number of counts, or onthe total counts obtained for a fixed time (generally expressedin counts per unit time). Concentrations of the elements aredeter
9、mined by relating the measured radiation of unknownsamples to calibration curves prepared using reference materi-als of known compositions.5. Significance and Use5.1 This method is suitable for providing data on thechemical composition of 6Al-4V titanium alloys for the scopeelements. It is intended
10、to be used for routine productioncontrol and for determination of chemical composition for thepurpose of certifying material specification compliance. Addi-tionally, the analytical performance data included with thismethod may be used as a benchmark to determine if similarX-ray spectrometers provide
11、 equivalent precision and accu-racy.6. Interferences6.1 Line overlaps, interelement effects and matrix effectsmay exist for some of the scope elements. A list of potentialline overlaps is provided in section 6.2. Modern X-ray spec-trometers provide software for generation of mathematicalcorrections
12、to model the effects of line overlaps, interelementand matrix interferences. The user of this method may chooseto use these mathematical corrections for analysis. Guide1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores and Related Materials and
13、is the directresponsibility of Subcommittee E01.06 on Ti, Zr, W, Mo, Ta, Nb, Hf, Re.Current edition approved June 1, 2007. Published June 2007. Originallyapproved in 1975. Last previous edition approved in 2006 as E 539 06.2Supporting data for this test method as determined by cooperative testing ha
14、sbeen filed at ASTM International Headquarters as two separate research reportsRR:E2-1010 and RR: RR: E01-1061.3For 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 s
15、tandards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.E 1621 provide a more extensive overview of mathematicalinterference correction methods.6.2 Potential line overlaps may occur directly
16、on the analyteline or may create problems with the background. Some listedinterfering elements may not be present in significant concen-trations in 6-4 titanium, but are listed for consideration. Themagnitude of the overlap will be a function of the collimationon the analyte line. Line overlaps to c
17、onsider:Analyte Interfering Element(s)V Ti (direct overlap)Cr V (direct overlap)Ni Nb, Cu (background overlaps)Mo Nb, Zr (background overlaps)Zr Cu (background overlap)7. Apparatus7.1 Specimen Preparation Equipment:7.1.1 Surface Grinder, with 60 to 600-grit silicon carbidebelts or disks capable of p
18、roviding test specimens with auniform flat finish. For silicon determinations 60-600 gritaluminum oxide or aluminum zirconium oxide belts or diskscapable of providing test specimens with a uniform flat finishshould be used. A wet belt or wet disk grinder is preferred toprevent work hardening of the
19、sample.7.1.2 Lathe, as an alternative to abrasive surfacing of testspecimens a lathe may be used to produce a uniform surface.7.2 X-ray Spectrometer:7.2.1 Practice E 1172 describes the essential components ofa wavelength-dispersive spectrometer and should be used as areference source for considerati
20、ons in selection of a suitablespectrometer for testing to this method.8. Reagents and Materials8.1 Detector GasAs specified by the spectrometer manu-facturer for use with flow proportional detectors.9. Reference Materials9.1 Certified reference materials are commercially availablefrom both domestic
21、and international sources. These should beof similar composition to 6Al-4V titanium alloy and are to beused for the development of calibration curves.9.2 Reference materials of similar composition to 6Al-4Vtitanium alloy may also be produced or obtained. Thesereference materials may be used to suppl
22、ement the certifiedreference materials used in the development of calibrationcurves.9.3 The reference materials shall cover the concentrationranges of the elements being determined. A minimum of threereference materials shall be used to develop the calibrationcurve for each element. A greater number
23、 of calibrationmaterials may be required to calculate mathematical correc-tions for interferences. See Guide E 1361.10. Hazards10.1 X-ray spectrometers produce ionizing radiation. Thismethod does not purport to address all safety considerationsrelating to the installation and use of an X-ray spectro
24、meter toperform this method. In general, however, OSHA guidelinesfor use of ionizing radiation producing equipment must be met,as well as state and local regulations relating to radiationhygiene must be followed. Additionally, the safety guidelinesestablished by the instrument manufacturer should be
25、 fol-lowed. Appropriate safety practices should be used withsample preparation equipment. Refer to Guide E 1621 foradditional information on hazards.11. Preparation of Reference Materials and TestSpecimens11.1 The reference materials and test specimens must be ofan appropriate size for fabrication i
26、nto a flat surfaced piece thatwill fit into the cup to be used to perform the test with the flatsurface completely covering the aperture of the cup. Grind orlathe mill the reference materials/specimens to provide a flat,clean area for testing. All reference materials and test speci-mens must receive
27、 the same surface preparation. Care must beused in selecting the grinding media, in order to minimize thepotential for surface contamination from the media. For in-stance, aluminum oxide and aluminum zirconium oxide grind-ing belts/disks may introduce aluminum and/or zirconiumcontamination and silic
28、on carbide belts/disks may introducesilicon contamination.12. Preparation of Apparatus12.1 Install and operate the spectrometer in accordance withthe manufacturers instructions. Also refer to Guide E 1621 foradditional considerations for preparing the spectrometer.12.2 The tube power supply conditio
29、ns (kV/mA) should beoptimized according to the manufacturers recommendations.Once established the optimized current and voltage settingsshall be used for generation of calibration curves and for allsubsequent specimen determinations.12.3 Check pulse height discrimination for each detector perthe man
30、ufacturers recommendations to verify that the limitvoltages are properly established for each element beingdetermined.12.4 The crystals and X-ray lines specified in Table 1 haveTABLE 1 Suggested X-Ray LinesElementLineDesignationA2u Angle,degBWavelength,(nm)CrystalAluminum Ka 144.67 0.8339 PETAluminu
31、m Ka 142.57 08339 EDDTChromium Kb 62.36 0.2085 LiF 200Chromium Ka 69.36 0.2291 LiF 200Copper Ka 45.03 0.1542 LiF 200Iron Ka 57.52 0.1937 LiF 200Manganese Ka 62.97 0.2103 LiF 200Molybdenum Ka 20.33 0.0710 LiF 200Nickel Ka 48.67 0.1659 LiF 200Ruthenium Ka 18.42 0.0644 LiF 200Silicon Ka 109.21 0.7126 P
32、ETTin La 126.77 0.3600 LiF 200Vanadium Kb 69.13 0.2285 LiF 200Vanadium Ka 76.94 0.2505 LiF 200Yttrium Ka 23.80 0.0831 LiF 200Zirconium Ka 22.55 0.0788 LiF 200ALine designations listed in this method are based on the Siegbahn system,which has been superseded by the IUPAC Nomenclature System for X-Ray
33、Spectrometry, Jenkins, R., Manne, R., Robin, R., and Senemaud, C., Pure titanium; X-rayTABLE 4 Statistical Information for ChromiumTestMaterialNumber ofLaboratoriesChromiumFound, %MinSD(SM,E 1601)Reproducibility SD (SR,E 1601)Reproducibility Index (R,E 1601)RrelCertifiedChromium, %Number Source Desc
34、ription1 6 0.0241 0.00124 0.00259 0.00724 30.1 0.025 654B NIST Ti-6AI 4V2 6 0.0180 0.00102 0.02796 0.00783 43.4 0.015 173C NIST Ti-6AI 4V3 6 0.0125 0.00108 0.00292 0.00816 65.5 0.013 T5A Brammer Ti-6AI 4V4 6 0.0272 0.00092 0.00465 0.01303 47.9 Not Cert. HTL 601 TIMET Ti-6AI 4V5 6 0.0701 0.00127 0.00
35、511 0.01430 20.4 Not Cert. 0240 Allvac Ti-6AI 4V6 6 0.0127 0.00099 0.00313 0.00877 68.8 0.013 175A ARMI Ti-6AI 4V7 6 0.0071 0.00082 0.00378 0.01058 148.1 0.005 T20 Brammer Ti-6AI 4VTABLE 5 Statistical Information for CopperTestMaterialNumber ofLaboratoriesCopperFound, %MinSD(SM,E 1601)Reproducibilit
36、y SD (SR, E 1601)Reproducibility Index (R,E 1601)RrelCertifiedCopper, %Number Source Description1 6 0.0056 0.00016 0.00292 0.00818 145.2 0.004 654B NIST Ti-6AI 4V2 6 0.0037 0.00029 0.00286 0.00800 214.0 0.0040 173C NIST Ti-6AI 4V3 6 0.0015 0.00035 0.00270 0.00756 512.2 0.0025 T5A Brammer Ti-6AI 4V4
37、6 0.0101 0.00036 0.00311 0.00870 86.3 Not Cert. HTL 601 TIMET Ti-6AI 4V5 6 0.0655 0.00045 0.00236 0.00660 10.1 Not Cert. 0240 Allvac Ti-6AI 4V6 6 0.0034 0.00331 0.00264 0.00738 216.0 0.005 175A ARMI Ti-6AI 4V7 6 0.0117 0.00035 0.00612 0.01713 146.1 0.016 T20 Brammer Ti-6AI 4VTABLE 6 Statistical Info
38、rmation for IronTestMaterialNumber ofLaboratoriesIronFound, %MinSD(SM,E 1601)Reproducibility SD (SR,E 1601)Reproducibility Index (R,E 1601)RrelCertifiedIron, %Number Source Description1 7 0.2293 0.00127 0.00443 0.01242 5.4 0.23 654B NIST Ti-6AI 4V2 7 0.2253 0.00115 0.00577 0.01616 7.2 0.213 173C NIS
39、T Ti-6AI 4V3 7 0.1745 0.00134 0.00718 0.02010 11.5 0.170 T5A Brammer Ti-6AI 4V4 7 0.1998 0.00283 0.00635 0.01777 8.9 Not Cert. HTL 601 TIMET Ti-6AI 4V5 7 0.2336 0.00108 0.00448 0.01254 5.4 Not Cert. 0240 Allvac Ti-6AI 4V6 7 0.1935 0.00138 0.00690 0.01933 10.0 0.20 175A ARMI Ti-6AI 4V7 7 0.0845 0.000
40、85 0.00996 0.02790 33.0 0.089 T20 Brammer Ti-6AI 4VTABLE 7 Statistical Information for ManganeseTestMaterialNumber ofLaboratoriesManganeseFound, %MinSD(SM, E 1601)Reproducibility SD (SR,E 1601)Reproducibility Index (R,E 1601)RrelCertifiedManganese, %Number Source Description1 7 0.0034 0.00059 0.0019
41、9 0.00558 166.0 Not Cert. 654B NIST Ti-6AI 4V2 7 0.0029 0.00042 0.00197 0.00550 188.6 Not Cert. 173C NIST Ti-6AI 4V3 6 0.0013 0.00031 0.00151 0.00424 319.3 0.002 T5A Brammer Ti-6AI 4V4 6 0.0037 0.00045 0.00222 0.00621 168.6 Not Cert. HTL 601 TIMET Ti-6AI 4V5 6 0.0679 0.00101 0.00188 0.00527 7.8 Not
42、Cert. 0240 Allvac Ti-6AI 4V6 6 0.0019 0.00034 0.00187 0.00523 282.7 Not Cert. 175A ARMI Ti-6AI 4V7 6 0.0263 0.00060 0.00541 0.01514 57.6 0.03 T20 Brammer Ti-6AI 4VE539074TABLE 8 Statistical Information for MolybdenumTestMaterialNumber ofLaboratoriesMolybdenum Found, %MinSD(SM,E 1601)Reproducibility
43、SD (SR,E 1601)Reproducibility Index (R,E 1601)RrelCertifiedMolybdenum, %Number Source Description1 7 0.0122 0.00007 0.00114 0.00320 26.3 0.013 654B NIST Ti-6AI 4V2 6 0.0074 0.00003 0.00213 0.00597 80.9 0.0068 173C NIST Ti-6AI 4V3 7 0.0053 0.00032 0.00290 0.00811 153.9 0.004 T5A Brammer Ti-6AI 4V4 7
44、0.0189 0.00028 0.00215 0.00603 31.8 Not Cert. HTL 601 TIMET Ti-6AI 4V5 6 0.0716 0.00063 0.00336 0.00940 13.1 Not Cert. 0240 Allvac Ti-6AI 4V6 6 0.0069 0.00005 0.00226 0.00632 91.8 0.008 175A ARMI Ti-6AI 4V7 6 0.0244 0.00026 0.00145 0.00405 16.6 0.021 T20 Brammer Ti-6AI 4VTABLE 9 Statistical Informat
45、ion for NickelTestMaterialNumber ofLaboratoriesNickelFound, %MinSD(SM,E 1601)Reproducibility SD (SR,E 1601)Reproducibility Index (R,E 1601)RrelCertifiedNickel, %Number Source Description1 7 0.0282 0.00035 0.00087 0.00243 8.6 0.028 654B NIST Ti-6AI 4V2 7 0.0214 0.00034 0.00282 0.00790 36.9 0.0203 173
46、C NIST Ti-6AI 4V3 7 0.0147 0.00039 0.00346 0.00969 66.1 0.012 T5A Brammer Ti-6AI 4V4 6 0.0165 0.00027 0.00101 0.00284 17.2 Not Cert. HTL 601 TIMET Ti-6AI 4V5 6 0.0732 0.00017 0.00369 0.01033 14.1 Not Cert. 0240 Allvac Ti-6AI 4V6 7 0.0123 0.00040 0.00127 0.00355 28.8 0.012 175A ARMI Ti-6AI 4V7 7 0.00
47、37 0.00029 0.00458 0.01281 342 0.002 T20 Brammer Ti-6AI 4VTABLE 10 Statistical Information for TinTestMaterialNumber ofLaboratoriesTinFound, %MinSD(SM,E 1601)Reproducibility SD (SR,E 1601)Reproducibility Index (R,E 1601)RrelCertifiedTin, %Number Source Description1 6 0.0231 0.00043 0.00092 0.00257 1
48、1.1 0.023 654B NIST Ti-6AI 4V2 6 0.0111 0.00040 0.00131 0.00368 33.1 0.010 173C NIST Ti-6AI 4V3 6 0.0113 0.00039 0.00142 0.00397 35.2 0.009 T5A Brammer Ti-6AI 4V4 6 0.0216 0.00044 0.00106 0.00296 13.7 Not Cert. HTL 601 TIMET Ti-6AI 4V5 7 0.0761 0.00042 0.00795 0.02225 29.3 Not Cert. 0240 Allvac Ti-6
49、AI 4V6 6 0.0150 0.00028 0.00125 0.00351 23.4 0.016 175A ARMI Ti-6AI 4V7 7 0.0264 0.00088 0.00302 0.00847 32.1 0.03 T20 Brammer Ti-6AI 4VTABLE 11 Statistical Information for VanadiumTestMaterialNumber ofLaboratoriesVanadiumFound, %MinSD(SM,E 1601)Reproducibility SD (SR,E 1601)Reproducibility Index (R,E 1601)RrelCertifiedVanadium, %Number Source Description1 6 4.334 0.00376 0.04865 0.13570 3.1 4.31 654B NIST Ti-6AI 4V2 7 4.194 0.00719 0.02301 0.06443 1.5 4.154 173C NIST Ti-6AI 4V3 7 4.089 0.00887 0.03043 0.08521 2.1 4.10 T5A Brammer Ti-6AI 4V4 7 3.967 0.00610 0.04754 0.13311 3.4 Not
