1、Designation: E 572 02a (Reapproved 2006)e2Standard Test Method forAnalysis of Stainless and Alloy Steels by X-rayFluorescence Spectrometry1This standard is issued under the fixed designation E 572; the number immediately following the designation indicates the year oforiginal adoption or, in the cas
2、e of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.e1NOTEUpdated Section 2 Reference Documents in December 2006.e2NOTEMade Editorial corrections to 7.3.4
3、 in March 2007.1. Scope1.1 This test method2covers the analysis of stainless andalloy steels by wavelength dispersive X-ray FluorescenceSpectrometry for the determination of the following elements:Element Range %Chromium 2.0 to 25.0Cobalt 0.03 to 0.40Copper 0.05 to 3.50Manganese 0.3 to 5.0Molybdenum
4、 0.15 to 3.5Nickel 0.20 to 35.0Niobium 0.05 to 1.3Phosphorus 0.01 to 0.03Silicon 0.05 to 0.20Sulfur 0.02 to 0.30Titanium 0.002 to 0.04Vanadium 0.03 to 0.25NOTE 1Unless exceptions are noted, concentration ranges can beextended by the use of suitable reference materials.1.2 This standard does not purp
5、ort 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 given
6、in Section 10.2. Referenced Documents2.1 ASTM Standards:3E 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE 305 Practice for Establishing and Controlling Spectro-chemical Analytical Curves4E 691 Practice for Conducting an Interlaboratory Study toDetermine the
7、Precision of a Test MethodE 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 1621 Guide for X-Ray Emission Spectrometric AnalysisE 1806 Practice for Sampling Ste
8、el and Iron for Determi-nation of Chemical Composition3. Terminology3.1 For definitions of terms used in this test method, refer toTerminology E 135.4. Summary of Test Method4.1 The test specimen is finished to a clean, uniform surfaceand then irradiated with an X-ray beam of high energy. Theseconda
9、ry 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 counted. Radiation measurements are made based onthe time required to reach a fixed number of counts, or on thetotal c
10、ounts obtained for a fixed time (generally expressed incounts per unit time). Concentrations of the elements aredetermined by relating the measured radiation of unknownspecimens to analytical curves prepared with suitable referencematerials. A fixed-channel, polychromator system or a sequen-tial, mo
11、nochromator 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 specifications. It providesrapid, multi-element determinations with sufficient accuracy toassure product quality. The analyti
12、cal 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, Ores and Related Materials and is the directresponsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.Curr
13、ent edition approved Nov. 1, 2006. Published November 2006. Originallyapproved in 1976. Last previous edition approved in 2002 as E 572 02a.2Supporting data for this test method as determined by cooperative testing havebeen filed at ASTM International Headquarters as RR: E-1-1032.3For referenced AST
14、M 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.4Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, We
15、st Conshohocken, PA 19428-2959, United States.X-ray spectrometers provide equivalent 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
16、used tosolve for these elements. Various mathematical correctionprocedures are commonly utilized. See Guides E 1361 andE 1621. Any of these procedures that achieves analyticalaccuracy equivalent to that provided by this test method isacceptable.7. Apparatus7.1 Specimen Preparation Equipment:7.1.1 Su
17、rface 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 with a grit size of between60 and 180 have been found suitable.7.2 Excitation Source:7.2.1 X-ray
18、 Tube Power Supply, providing a constant po-tential or rectified power of sufficient energy to producesecondary radiation of the specimen for the elements specified.The generator may be equipped with a line voltage regulatorand current stabilizer.7.2.2 X-ray Tubes, with targets of various high-purit
19、y 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 emission analysis andequipped with specimen holders and a specimen chamber. Thechamber shall contain a specimen spinner, and
20、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 diffraction of the wavelengths ofinterest. The use of synthetic multilayer structures can
21、 be foundin stateoftheart equipment.7.3.2 Collimators or Slits, for controlling the 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
22、 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 auto-matic pump down of the optical path, and maintain a controlledpressure, usually 13 Pa (100 m Hg)
23、 or less, controlled to 63Pa (620 m Hg). A helium-flushed system is an alternative toa vacuum 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
24、 detectors may be required to provide moreaccurate measurements. The system shall be equipped with anappropriate 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 C
25、ertified Reference Materials are available from na-tional and international sources.9.2 Reference Materials with matrices similar to that of thetest specimen and containing varying amounts of the elementsto be determined may be used provided they have beenanalyzed in accordance with ASTM standard me
26、thods orsimilar procedures established by the certifying body. Thesereference materials shall be homogeneous and free of voids andporosity.9.3 The reference materials shall cover the concentrationranges of the elements being sought. A minimum of threereference materials shall be used for each elemen
27、t. A greaternumber of calibrants may be required if the analyst chooses toperform mathematical corrections for interelement effects. SeeGuide E 1361.10. Hazards10.1 OSHA Standards for ionizing radiation5shall be ob-served at all X-ray emission spectrometer installations. It isalso recommended that o
28、perating and maintenance personnelfollow the guidelines of safe operating procedures given incurrent handbooks and publications from National Institute ofStandards and Technology6and the U.S. Government PrintingOffice7, or similar handbooks on radiation safety.10.2 X-ray equipment shall be used only
29、 under the guidanceand supervision of a responsible, qualified person.10.3 Monitoring Devices, either film badges or dosimeters8may be worn by all operating and maintenance personnel.Safety regulations shall conform to applicable local, state, andfederal regulations.11. Preparation of Reference Mate
30、rials 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 diameter than the chosen viewed area.11.2 Prepare the reference materials and test specimens to
31、provide a clean, flat uniform surface to be exposed to the X-ray5Federal Register, Vol 36, No. 105, May 1971, Section 1910.96 or of latest issueof Subpart G, available from Superintendent of Documents, U.S. GovernmentPrinting Office, Washington, DC 20025; or National Bureau of Standards Handbook111,
32、 ANSI N43.2-1971.6Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http:/www.dodssp.daps.mil.7Available from U.S. Department of Health, Education, and Welfare, Rockville,MD 20850.8The sole source of supply of the apparatus
33、 known to the committee at this timeis available from Seimens Gammasonics, Inc., 2000 Nuclear Drive, Des Plaines, IL60018. If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of t
34、he responsible technical committee,1which you may attend.E 572 02a (2006)e22beam. One surface of a reference material may be designatedby the producer as the certified surface. The same surfacepreparation medium shall be used for all reference materialsand test specimens.11.3 Refinish the surface of
35、 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 scope of this test method to prescribeminute details relative to the preparati
36、on of the apparatus. For a descrip-tion and 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
37、 Power SupplyThe power supply conditionsshould 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
38、 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 before the instrument is used. Afterchanging P-10 tanks, check pulse height select
39、or according tothe manufacturers instructions.12.4 Measurement ConditionsThe KL2,3(Ka) lines foreach element are used. When using a scanning (sequential)spectrometer, locations shall be calibrated according to themanufacturers guidelines.12.4.1 Crystals and DetectorsThe following crystals anddetecto
40、rs are used for the elements indicated:Element 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 Fb, SPSulfur Ge FP, SPTitanium L1, L2
41、 SP, Sc, FPVanadium L1, L2 SP, Sc, FPL1 = LiF(200),L2 = LiF(220),SP = Sealed Proportional,Sc = Scintillation, andFP = Flow Proportional.12.4.2 Counting TimeCollect a sufficient number ofcounts so that the precision of the analysis will not be affectedby the variation in the counting statistics. A mi
42、nimum of10 000 counts is required for one percent precision of 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 req
43、uired concentrationranges. Use at least three reference materials 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 correct
44、ion of spectral lineoverlap in wavelength dispersive X-ray spectrometry can befound in Practice E 1621.13.2 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
45、gas or major components have beenchanged. If the calibration check 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 L
46、oadingPlace the reference materials andtest specimens in the appropriate specimen holding container.If the spectrometer is equipped with an automated loadingdevice, repeatability may be improved by loading and unload-ing all specimens from the same holder. The container shallhave a suitable opening
47、to achieve the required precision in anacceptable 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 12.14.3 Radiation MeasurementsObtain and record thecounting rate measu
48、rement for each element. Either fixed countor fixed time modes may be used. Obtain at least the prede-termined minimum counts for all specimens.14.4 Spectral InterferencesSome X-ray spectrometerswill not completely resolve radiation from several metalcombinations (for example, molybdenum and sulfur;
49、 molyb-denum and phosphorus; and iron and cobalt). Therefore, caremust be exercised in the interpretation of intensities when bothelements are present. Mathematical calculations must be usedto correct for the interferences.14.5 Replicate MeasurementsMake a single measurementon each test specimen. The performance of an X-ray spectrom-eter is not improved significantly by making 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
