1、Designation: E2465 111Standard 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 revis
2、ion, 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.1NOTEEditorial corrections were made in August 2011.1. Scope1.1 This test method covers the analysis of Ni-base a
3、lloysby wavelength dispersive X-ray Fluorescence Spectrometry forthe determination of the following elements:Element Concentration Range %Manganese 0.17 to 1.6Phosphorus 0.005 to 0.015Silicon 0.02 to 0.6Chromium 11 to 22Nickel 31 to 77Aluminum 0.12 to 1.3Molybdenum 0.045 to 10Copper 0.014 to 2.5Tita
4、nium 0.20 to 3.0Niobium 1.43 to 5.3Iron 2 to 46Tungsten 0.016 to 0.50Cobalt 0.014 to 0.35NOTE 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 coul
5、d include 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 This standard does not purport to address all of thesafety concerns, if any, assoc
6、iated 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 limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E135 Terminology Relating to Analytical Chemistry forMeta
7、ls, Ores, and Related MaterialsE305 Practice for Establishing and Controlling AtomicEmission Spectrochemical Analytical CurvesE1361 Guide for Correction of Interelement Effects inX-Ray Spectrometric AnalysisE1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analy
8、tical MethodE1622 Practice for Correction of Spectral Line 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, r
9、efer 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 atselected waveleng
10、ths. 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 the elements a
11、re determined by relat-ing the measured radiation of unknown specimens to analyticalcurves prepared with suitable reference materials. Either afixed-channel (simultaneous) spectrometer or a sequentialspectrometer, or an instrument combining both fixed-channelsand one or more goniometers shall be use
12、d.5. Significance and Use5.1 This procedure is suitable for manufacturing control andfor verifying that the product meets specifications. It provides1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and is the directrespo
13、nsibility of Subcommittee E01.08 on Ni and Co and High Temperature Alloys.Current edition approved May 1, 2011. Published June 2011. Originallyapproved in 2006. Last previous edition approved in 2006 as E2465 06. DOI:10.1520/E2465-11.2For referenced ASTM standards, visit the ASTM website, www.astm.o
14、rg, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.1Copyright ASTM International, 1
15、00 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.rapid, multi-element determinations with sufficient accuracy toassure product quality. The analytical performance data in-cluded may be used as a benchmark to determine if similarX-ray spectrometers provide equivalent
16、 precision and 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 com
17、monly utilized. See Guide E1361 andPractice E1622. Any of these procedures that achieves analyti-cal accuracy equivalent to that provided 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
18、providing a 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 sufficie
19、nt energy to 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 cur
20、rents and that will excite the elements to bedetermined.7.3 Spectrometer, designed for X-ray fluorescence analysisand equipped with specimen holders and a specimen chamber.The chamber shall contain a specimen spinner, and must beequipped for vacuum or helium-flushed operation for thedetermination of
21、 elements of atomic 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, f
22、or controlling the divergence ofthe characteristic X-rays. Use in accordance with the equip-ment manufacturers recommendations.7.3.3 Detectors, sealed-gas, gas-flow scintillation countersor equivalent.7.3.4 Vacuum System, providing for the determination ofelements whose radiation is absorbed by air
23、(for example,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 a
24、n alternative 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
25、system shall be equipped withan appropriate device.8. Reagents and Materials8.1 Detector GasesOnly gas-flow proportional countersrequire 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
26、 % 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. Reference Materials9.1 Certified Reference Materials are available from na-tional metrology institutes, international research institutes,and commercial sources.9.2 Reference
27、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 reference materials shall be homogeneous and free ofvoids and porosit
28、y.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 chooses toperform mathematical corrections for interelement effects. SeeG
29、uide E1361.10. 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 operating procedures given incurrent handbooks and publications from Natio
30、nal Institute ofStandards and Technology and the U.S. Government PrintingOffice, or similar handbooks on radiation safety.10.2 Exposure to excessive quantities of high energy radia-tion such as those produced by X-ray spectrometers is injuriousto health. The operator should take appropriate actions
31、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-ray spectrometer should be operated in accordance withthe regulations governing the use of ionizing radiation. Manu-facturers of X-ray fluorescence spectromete
32、rs generally buildappropriate shielding/safety interlocks into X-ray equipmentduring manufacturing that minimize the risk of excessiveradiation exposure to operators. Operators should not attemptto bypass or defeat these safety devices. Only authorizedpersonnel should service X-ray spectrometers.4Fe
33、deral Register, 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.E2465 111210.3 Monitoring Devices, either film ba
34、dges 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 area ordiameter from the options built into
35、 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. One surface of a reference material may
36、 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.12. Preparation of Apparatus12.1 Prepare and operate
37、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 specific details concerning the operation of a particular spectrom-eter, refer to the
38、 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 conditionsshould be set in accordance with the manufacturers recom-mendations.12.2.1 The voltage an
39、d 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, adjust the flow of the P-10 gas inaccordance with the equipment manufacturers inst
40、ructions.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 inaccordance with the manufacturers instructions.12.4 Measurement ConditionsThe K-L2,3(Ka) lines foreach element are
41、 used, except for tungsten. For tungsten, theL3-M5(La) line is used. When using a sequential spectrometer,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:El
42、ement 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
43、= 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 relative prec
44、ision ofthe counting statistics and 40,000 for one-half percent relative.If fixed time measurements are 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 1
45、0 s for each ofthe elements are a good starting point.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 mater
46、ials for each element.Prepare an analytical curve for each element being determined(refer to Practice 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 spec
47、trometry can befound in Practice E1622.13.2 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 che
48、ck indicates that the spectrom-eter has drifted, make appropriate adjustments in accordancewith the instructions in the manufacturers manual. Refer toPractice E305 for frequency of verification of standardization.14. Procedure14.1 Specimen LoadingPlace the reference materials andtest specimens in th
49、e 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 an5Available from Siemens Gammasonics, Inc., 2000 Nuclear Drive, Des PlainesIl 60018.E2465 1113acceptable amount of time. The holder 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.
