1、Designation: E 2465 06Standard Test Method forAnalysis of Ni-Base Alloys by X-ray FluorescenceSpectrometry1This standard is issued under the fixed designation E 2465; 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 (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the analysis of Ni-base alloysby wavelength dispersive X-ray Fluorescence Spectrometry forthe det
3、ermination of the following elements:Element Concentration RangeManganese 0.17 to 1.6 %Phosphorus 0.005 to 0.015 %Silicon 0.02 to 0.6 %Chromium 11 to 22 %Nickel 31 to 77 %Aluminum 0.12 to 1.3 %Molybdenum 0.045 to 10 %Copper 0.014 to 2.5 %Titanium 0.20 to 3.0 %Niobium 1.43 to 5.3 %Iron 2 to 46 %Tungs
4、ten 0.016 to 0.50 %Cobalt 0.014 to 0.35 %NOTE 1Unless exceptions are noted, concentration ranges can beextended by the use of suitable reference materials. Once these elementranges are extended they must be verified by some experimental means.This could include but not limited to Gage Repeatability
5、and Reproduc-ibility studies and/or Inter-laboratory Round Robin studies. Once thesestudies are completed, they will satisfy the ISO 17025 requirements forcapability.1.2 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of t
6、he user of this standard to establish appro-priate safety and health practices and to determine theapplicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE 305 Practice f
7、or Establishing and Controlling Spectro-chemical Analytical Curves3E 1361 Guide for Correction of Interelement Effects inX-Ray Spectrometric AnalysisE 1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE 1622 Practice for Correction of Spectral Li
8、ne Overlap inWavelength-Dispersive X-Ray Spectrometry32.2 Other Documents:ISO 17025 General requirements for the competence oftesting and calibration laboratories3. Terminology3.1 Definitions: For definitions of terms used in this testmethod, refer to Terminology E 135.4. Summary of Test Method4.1 T
9、he test specimen is finished to a clean, uniform surface,then irradiated with an X-ray beam of high energy. Thesecondary X-rays produced are dispersed by means of crystalsand the intensities are measured by suitable detectors atselected wavelengths. The outputs of the detectors in voltagepulses are
10、counted. Radiation measurements are made based onthe time required to reach a fixed number of counts, or on thetotal counts obtained for a fixed time (generally expressed incounts per unit time). Concentrations of the elements aredetermined by relating the measured radiation of unknownspecimens to a
11、nalytical curves prepared with suitable referencematerials. A fixed-channel, polychromator system or a sequen-tial, monochromator can be used for measurement of theelements.5. Significance and Use5.1 This procedure is suitable for manufacturing control andfor verifying that the product meets specifi
12、cations. It providesrapid, multi-element determinations with sufficient accuracy toassure product quality. The analytical performance data in-cluded may be used as a benchmark to determine if similar1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals,
13、Ores, and Related Materials and is the directresponsibility of Subcommittee E01.08 on Ni and Co and High Temperature Alloys.Current edition approved May 15, 2006. Published June 2006.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.
14、org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.X-ray spectrometers provide equivalent precision and
15、 accu-racy, or if the performance of a particular spectrometer haschanged.6. Interferences6.1 Interelement effects, or matrix effects, exist for some ofthe elements listed. Mathematical correction may be used tosolve for these elements. Various mathematical correctionprocedures are commonly utilized
16、. See Guide E 1361 andPractice E 1622. Any of these procedures that achieves ana-lytical accuracy equivalent to that provided by this test methodis acceptable.7. Apparatus7.1 Specimen Preparation Equipment:7.1.1 Surface Grinder or Sander With Abrasive Belts orDisks, or Lathe, capable of providing a
17、flat, uniform surface onthe reference materials and test specimens. Aluminum oxideand zirconium oxide belts and discs with a grit size of between60 and 180 have been found suitable.7.2 Excitation Source:7.2.1 Tube Power Supply, providing a constant potential orrectified power of sufficient energy to
18、 produce secondaryradiation of the specimen for the elements specified. Thegenerator may be equipped with a line voltage regulator andcurrent stabilizer.7.2.2 X-ray Tubes, with targets of various high-purity ele-ments that are capable of continuous operation at requiredpotentials and currents and th
19、at will excite the elements to bedetermined.7.3 Spectrometer, designed for X-ray emission analysis andequipped with specimen holders and a specimen chamber. Thechamber shall contain a specimen spinner, and must beequipped for vacuum or helium-flushed operation for thedetermination of elements of ato
20、mic number 20 (calcium) orlower.7.3.1 Analyzing Crystals, flat or curved crystals with opti-mized capability for the diffraction of the wavelengths ofinterest. The use of synthetic multilayer structures can also befound in some state-of-the-art-equipment.7.3.2 Collimators or Slits, for controlling t
21、he divergence ofthe characteristic X-rays. Use per the equipment manufactur-ers recommendations.7.3.3 Detectors, sealed or gas-flow proportional type, scin-tillation counters or equivalent.7.3.4 Vacuum System, providing for the determination ofelements whose radiation is absorbed by air (for example
22、,silicon, phosphorus, and sulfur). The system shall consist of avacuum pump, gage, and electrical controls to provide auto-matic pump down of the optical path, and maintain a controlledpressure, usually 13Pa (100 mm Hg) or less, controlled to 63Pa (20 mm Hg). A helium-flushed system is an alternativ
23、e to avacuum system.7.4 Measuring System, consisting of electronic circuits ca-pable of amplifying and integrating pulses received from thedetectors. For some measurements, a pulse height selector inconjunction with the detectors may be used to remove highorder lines and background. The system shall
24、 be equipped withan appropriate device.8. Reagents and Materials8.1 Detector Gas (P-10), consisting of a mixture of 90 %argon and 10 % methane, for use with gas-flow proportionalcounters only.9. Reference Materials9.1 Certified Reference Materials are available from na-tional metrology institutes, i
25、nternational research institutes,and commercial sources.9.2 Reference Materials with matrices similar to that of thetest specimens and containing varying amounts of the elementsin the scope of this test method may be used provided theyhave been analyzed using validated standard methods of test.These
26、 reference materials shall be homogeneous and free ofvoids and porosity.9.3 The reference materials shall cover the concentrationranges of the elements being sought. A minimum of threereference materials shall be used for each element. A greaternumber of calibrants may be required if the analyst cho
27、oses toperform mathematical corrections for interelement effects. SeeGuide E 1361.10. Hazards10.1 OSHA Standards for ionizing radiation4shall be ob-served at all X-ray emission spectrometer installations. It isalso recommended that operating and maintenance personnelfollow the guidelines of safe ope
28、rating procedures given incurrent handbooks and publications from National Institute ofStandards and Technology and the U.S. Government PrintingOffice, or similar handbooks on radiation safety.10.2 X-ray equipment shall be used only under the guidanceand supervision of a responsible, qualified perso
29、n.10.3 Monitoring Devices, either film badges or dosimeters5may be worn by all operating and maintenance personnel.Safety regulations shall conform to applicable local, state, andfederal regulations.11. Preparation of Reference Materials and TestSpecimens11.1 The analyst must choose a measurement ar
30、ea ordiameter from the options built into the spectrometer. All testspecimens and reference materials must have a flat surface ofgreater diameter than the chosen viewed area.11.2 Prepare the reference materials and test specimens toprovide a clean, flat uniform surface to be exposed to the X-raybeam
31、. One surface of a reference material may be designatedby the producer as the certified surface. The same preparationmedium shall be used for all reference materials and testspecimens.11.3 Refinish the surface of the reference materials and testspecimens as needed to eliminate oxidation.4Federal Reg
32、ister, Vol. 36, No. 105, May 1971, Section 1910.96 or of latestissue of Subpart G, or National Bureau of Standards Handbook 111, ANSIN43.2-1971, available from Superintendent of Documents, U.S.Government Print-ing Office, Washington DC 20025.5Available from Siemens Gammasonics, Inc., 2000 Nuclear Dr
33、ive, Des PlainesIl 60018.E246506212. Preparation of Apparatus12.1 Prepare and operate the spectrometer in accordancewith the manufacturers instructions.NOTE 2It is not within the scope of this test method to prescribeminute details relative to the preparation of the apparatus. For a descrip-tion and
34、 specific details concerning the operation of a particular spectrom-eter, refer to the manufacturers manual.12.1.1 Start-upTurn on the power supply and electroniccircuits and allow sufficient time for instrument warm-up priorto taking measurements.12.2 Tube Power SupplyThe power supply conditionssho
35、uld be set according to the manufacturers recommenda-tions.12.2.1 The voltage and current established as optimum forthe X-ray tube power supply in an individual laboratory shallbe reproduced for subsequent measurements.12.3 Proportional Counter Gas FlowWhen a gas-flowproportional counter is used, ad
36、just the flow of the P-10 gas inaccordance with the equipment manufacturers instructions.When changing P-10 tanks, the detectors should be adequatelyflushed with detector gas before the instrument is used. Afterchanging P-10 tanks, check the pulse height selector accordingto the manufacturers instru
37、ctions.12.4 Measurement ConditionsThe K-L2,3(Ka) lines foreach element are used. When using a sequential spectrometer,measurement angles shall be calibrated according to themanufacturers guidelines.12.4.1 Crystals and DetectorsThe following crystals anddetectors are used for the elements indicated:E
38、lement Crystal DetectorChromium L1,L2 SP,Sc,FPCobalt L1,L2 SP,Sc,FPCopper L1,L2 SP,Sc,FPManganese L1,L2 SP,Sc,FPMolybdenum L1,L2 ScNickel L1,L2 SP,Sc,FPNiobium L1,L2 ScPhosphorus Ge FP,SPSilicon PET,InSb FP,SPTitanium L1,L2 SP,Sc,FPAluminum PET Sc,FPIron L1,L2 SP,ScTungsten L1,L2 SP,ScL1 = LiF200 SP
39、 = Sealed ProportionalL2 = LiF220 Sc = ScintillationFP = Flow Proportional12.4.2 Counting TimeCollect a sufficient number ofcounts so that the precision of the analysis will not be affectedby the variation in the counting statistics. A minimum of10,000 counts is required for one percent precision of
40、 thecounting statistics, 40,000 for one-half percent.13. Calibration and Standardization13.1 Calibration (Preparation of Analytical Curves)Using the conditions given in Section 12, measure a series ofreference materials that cover the required concentrationranges. Use at least three reference materi
41、als for each element.Prepare an analytical curve for each element being determined(refer to Practice E 305). For information on correction ofinterelement effects in X-ray Spectrometric Analysis refer toGuide E 1361. Information on correction of spectral lineoverlap in wavelength dispersive X-ray spe
42、ctrometry can befound in Practice E 1622.13.2 Standardization (Analytical Curve Adjustment)Using a control reference material, check the calibration of theX-ray spectrometer at a frequency consistent with SPC practiceor when the detector gas or major components have beenchanged. If the calibration c
43、heck indicates that the spectrom-eter has drifted, make appropriate adjustments according to theinstructions in the manufacturers manual. Refer to PracticeE 305 for frequency of verification of standardization.14. Procedure14.1 Specimen LoadingPlace the reference materials andtest specimens in the a
44、ppropriate specimen holding container.If the spectrometer is equipped with an automated loadingdevice, loading and unloading all specimens from the sameholder may improve repeatability. The container shall have asuitable opening to achieve the required precision in anacceptable amount of time. The h
45、older must be equipped tokeep the specimen from moving inside the holder.14.2 ExcitationExpose the specimen to primary X radia-tion in accordance with Section 12.14.3 Radiation MeasurementsObtain and record thecounting rate measurement for each element. Either fixed countor fixed time modes may be u
46、sed. Obtain at least the prede-termined minimum counts for all specimens.14.4 Spectral InterferencesSome X-ray spectrometerswill not completely resolve radiation from several elementcombinations (for example, molybdenum and sulfur; molyb-denum and phosphorus, and iron and cobalt). Therefore caremust
47、 be exercised in the interpretation of intensities when bothelements are present. Mathematical calculations must be usedto correct for interferences.14.5 Replicate MeasurementsMake a single measurementon each test specimen. The performance of an X-ray spectrom-eter is not improved significantly by m
48、aking multiple measure-ments on the same surface of the specimen. Confidence in theaccuracy of analysis will improve by making multiple mea-surements on freshly prepared surfaces of the same specimen.15. Calculation of Results15.1 Using the radiation measurements for the test specimenand the appropr
49、iate analytical curves, determine the concen-trations of the various elements.15.1.1 If mathematical calculations must be made to correctthe concentrations for interelement effects, any of a number ofcorrection procedures may be employed. Refer to the equip-ment manufacturers manual for the recommended procedurefor the instrument being used. See Guide E 1361.16. Precision and Bias616.1 PrecisionAn acceptable number of laboratoriestested this method in accordance with Practice E 1601. Preci-sion data, including R and Rrelare provided in Tables 1-13.6Supporting da
