1、Designation: E2465 13Standard Test Method forAnalysis of Ni-Base Alloys by Wavelength Dispersive X-RayFluorescence Spectrometry1This standard is issued under the fixed designation E2465; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revisi
2、on, 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 covers the analysis of Ni-base alloysby wavelength dispersive X-ray Fluorescence Spec
3、trometry forthe determination of the following elements:Element Composition RangeManganese 0.06 % to 1.6 %Phosphorus 0.008 % to 0.015 %Silicon 0.08 % to 0.6 %Chromium 1.6 % to 22 %Nickel 23 % to 77 %Aluminum 0.20 % to 1.3 %Molybdenum 0.03 % to 10 %Copper 0.007 % to 2.5 %Titanium 0.11 % to 3.0 %Niobi
4、um 0.55 % to 5.3 %Iron 0.17 % to 46 %Tungsten 0.06 % to 0.50 %Cobalt 0.04 % 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 in
5、clude but not limited to Gage Repeatability 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 The values stated in SI units are to be regarded asstandard. No other units of measure
6、ment are included in thisstandard.1.3 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 establish appro-priate safety and health practices and to determine theapplicability of regulatory limit
7、ations prior to use.2. Referenced Documents2.1 ASTM Standards:2E135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE305 Practice for Establishing and Controlling AtomicEmission Spectrochemical Analytical CurvesE1361 Guide for Correction of Interelement Effects inX
8、-Ray Spectrometric AnalysisE1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE1622 Practice for Correction of Spectral Line Overlap inWavelength-Dispersive X-Ray Spectrometry (Withdrawn2006)32.2 Other Documents:ISO 17025 General requirements for
9、 the competence oftesting and calibration laboratories2.3 U.S. Government Standards:410 CFR Part 19 Notices, Instructions and Reports to Work-ers: Inspection and Investigations10 CFR Part 20 Standards for Protection Against Radiation3. Terminology3.1 DefinitionsFor definitions of terms used in this
10、testmethod, refer to Terminology E135.4. Summary of Test Method4.1 The 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 atsele
11、cted wavelengths. The outputs of the detectors in voltagepulses are 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 or kilocounts per unit time).4.2 Concentrations of t
12、he elements are determined by relat-ing the measured radiation of unknown specimens to analyticalcurves prepared with suitable reference materials. Either afixed-channel (simultaneous) spectrometer or a sequential1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistr
13、y 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 June 1, 2013. Published July 2013. Originally approvedin 2006. Last previous edition approved in 2011 as E2465 111. DOI: 10.1520/E2465-13
14、.2For 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 standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is re
15、ferenced onwww.astm.org.4Available from the U.S. Nuclear Regulatory Commission, Public DocumentRoom, One White Flint North, 11555 Rockville Pike, Rockville, MD 20852-2738,http:/www.nrc.gov.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United Stat
16、es1spectrometer, or an instrument combining both fixed-channelsand one or more goniometers shall be used.5. Significance and Use5.1 This procedure is suitable for manufacturing control andfor verifying that the product meets specifications. It providesrapid, multi-element determinations with suffici
17、ent accuracy toassure product quality. The analytical performance data in-cluded may be used as a benchmark to determine if similarX-ray spectrometers provide equivalent precision andaccuracy, or if the performance of a particular spectrometer haschanged.6. Interferences6.1 Interelement effects, or
18、matrix effects, exist for some ofthe elements listed. Mathematical correction may be used tosolve for these elements. Various mathematical correctionprocedures are commonly utilized. See Guide E1361 andPractice E1622. Any of these procedures that achieves analyti-cal accuracy equivalent to that prov
19、ided by this test method isacceptable.7. Apparatus7.1 Specimen Preparation Equipment:7.1.1 Surface Grinder or Sander With Abrasive Belts orDisks, or Lathe, capable of providing a flat, uniform surface onthe reference materials and test specimens. Aluminum oxideand zirconium oxide belts and discs wit
20、h 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 produce secondaryradiation of the specimen for the elements specified. Thegenerator may be equipped with a line voltage
21、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 that will excite the elements to bedetermined.7.3 Spectrometer, designed for X-ray fluorescence analysisand equipped with s
22、pecimen holders and a specimen chamber.The chamber shall contain a specimen spinner, and must beequipped for vacuum or helium-flushed operation for thedetermination of elements of atomic number 20 (calcium) orlower.7.3.1 Analyzing Crystals, flat or curved crystals with opti-mized capability for the
23、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 the divergence ofthe characteristic X-rays. Use in accordance with the equip-ment manufacturers recommendations.7.3.3
24、Detectors, sealed-gas, gas-flow scintillation countersor equivalent.7.3.4 Vacuum System, providing for the determination ofelements whose radiation is absorbed by air (for example,silicon, phosphorus, and sulfur). The system shall consist of avacuum pump, gage, and electrical controls to provide aut
25、o-matic pump down of the optical path, and maintain a controlledpressure, usually 13 Pa (100 mm Hg) or less, controlled to 63Pa (20 mm Hg). A helium-flushed system is an alternative to avacuum system.7.4 Measuring System, consisting of electronic circuits ca-pable of amplifying and integrating pulse
26、s 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 be equipped withan appropriate device.8. Reagents and Materials8.1 Detector GasesOnly gas-flow proportional countersreq
27、uire a detector gas. Use the gas and purity of gas specifiedby the instrument manufacturer. Typical gases specified includeP-10 or P-5. P-10 consists of a mixture of 90 % argon and 10% methane and P-5 consists of a mixture of 95 % argon and 5% methane. Other gases may be specified as well.9. Referen
28、ce Materials9.1 Certified Reference Materials are available from na-tional metrology institutes, international 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
29、 method may be used provided theyhave been analyzed using validated standard methods of test.These 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 material
30、s shall be used for each element. A greaternumber of calibrants may be required if the analyst chooses toperform mathematical corrections for interelement effects. SeeGuide E1361.10. Hazards10.1 U.S. Nuclear Regulatory standards for ionizing radia-tion as found in the Code of Federal Regulations, 10
31、 CFR Part19 and 10 CFR Part 20 shall be observed at all X-ray emissionspectrometer installations in the United States. It is alsorecommended that operating and maintenance personnel fol-low the guidelines of safe operating procedures given in similarhandbooks on radiation safety.10.2 Exposure to exc
32、essive quantities of high energy radia-tion such as those produced by X-ray spectrometers is injuriousto health. The operator should take appropriate actions to avoidexposing any part of their body, not only to primary X-rays, butalso to secondary or scattered radiation that might be present.The X-r
33、ay spectrometer should be operated in accordance withthe regulations governing the use of ionizing radiation. Manu-facturers of X-ray fluorescence spectrometers generally buildappropriate shielding/safety interlocks into X-ray equipmentduring manufacturing that minimize the risk of excessiveradiatio
34、n exposure to operators. Operators should not attemptto bypass or defeat these safety devices. Only authorizedpersonnel should service X-ray spectrometers.E2465 13210.3 Monitoring Devices, either film badges or dosimeters5may be worn by all operating and maintenance personnel.Safety regulations shal
35、l conform to applicable local, state, andfederal regulations.11. Preparation of Reference Materials and TestSpecimens11.1 The analyst must choose a measurement area ordiameter from the options built into the spectrometer. All testspecimens and reference materials must have a flat surface ofgreater d
36、iameter 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. One surface of a reference material may be designatedby the producer as the certified surface. The same preparationmedium shall be used
37、for all reference materials and testspecimens.11.3 Refinish the surface of the reference materials and testspecimens as needed to eliminate oxidation.12. Preparation of Apparatus12.1 Prepare and operate the spectrometer in accordancewith the manufacturers instructions.NOTE 2It is not within the scop
38、e of this test method to prescribeminute details relative to the preparation of the apparatus. For a descrip-tion and specific details concerning the operation of a particularspectrometer, refer to the manufacturers manual.12.1.1 Start-upTurn on the power supply and electroniccircuits and allow suff
39、icient time for instrument warm-up priorto taking measurements.12.2 Tube Power SupplyThe power supply conditionsshould be set in accordance with the manufacturers recom-mendations.12.2.1 The voltage and current established as optimum forthe X-ray tube power supply in an individual laboratory shallbe
40、 reproduced for subsequent measurements.12.3 Proportional Counter Gas FlowWhen a gas-flowproportional counter is used, adjust 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 befo
41、re the instrument is used. Afterchanging P-10 tanks, check the pulse height selector inaccordance with the manufacturers instructions.12.4 Measurement ConditionsThe K-L2,3(K) lines foreach element are used, except for tungsten. For tungsten, theL3-M5(L) line is used. When using a sequential spectrom
42、eter,measurement angles shall be calibrated in accordance with themanufacturers guidelines.12.4.1 Crystals and DetectorsThe following crystals anddetectors are suggested for the elements indicated:Element Crystal DetectorChromium L1,L2 SP,Sc,FPCobalt L1,L2 SP,Sc,FPCopper L1,L2 SP,Sc,FPManganese L1,L
43、2 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 = Sealed ProportionalL2 = LiF220 Sc = ScintillationFP = Flow Proportional12.4.2 Counting TimeCollect
44、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 relative precision ofthe counting statistics and 40,000 for one-half percent relative.If fixed time measurements a
45、re used, the measurement timescan be derived from the measured intensity (counts per second)and the minimum number of required counts (that is, 10,000 or40,000). Alternatively, measurement times of 10 s for each ofthe elements are a good starting point.13. Calibration and Standardization13.1 Calibra
46、tion (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 materials for each element.Prepare an analytical curve for each element being determined(refer to Practice
47、 E305). For information on correction ofinterelement effects in X-ray Spectrometric Analysis refer toGuide E1361. Information on correction of spectral lineoverlap in wavelength dispersive X-ray spectrometry can befound in Practice E1622.13.2 Standardization (Analytical Curve Adjustment)Usinga contr
48、ol reference material, check the calibration of the X-rayspectrometer at a frequency consistent with SPC practice orwhen the detector gas or major components have beenchanged. If the calibration check indicates that the spectrom-eter has drifted, make appropriate adjustments in accordancewith the in
49、structions in the manufacturers manual. Refer toPractice E305 for frequency of verification of standardization.14. Procedure14.1 Specimen LoadingPlace the reference materials andtest specimens in the appropriate 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 holder must be equipped tokeep the specimen from moving inside t
