1、Designation: E 1085 95 (Reapproved 2004)Standard Test Method forX-Ray Emission Spectrometric Analysis of Low-AlloySteels1This standard is issued under the fixed designation E 1085; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, th
2、e 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.1. Scope1.1 This test method covers the wavelength dispersiveX-ray spectrometric analysis of low-alloy steels for the f
3、ollow-ing elements:Element Concentration Range, %Nickel 0.04 to 3.0Chromium 0.04 to 2.5Manganese 0.04 to 2.5Silicon 0.06 to 1.5Molybdenum 0.005 to 1.5Copper 0.03 to 0.6Vanadium 0.012 to 0.6Cobalt 0.03 to 0.2Sulfur 0.009 to 0.1Niobium 0.002 to 0.1Phosphorus 0.010 to 0.08Calcium 0.001 to 0.0071.2 This
4、 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 determine the applica-bility of regulatory limitations prior to use. Specific precau-tionar
5、y statements are given in Section 10.2. Referenced Documents2.1 ASTM Standards:2E 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE 305 Practice for Establishing and Controlling Spectro-chemical Analytical CurvesE 691 Practice for Conducting an Interlaboratory
6、Study toDetermine the Precision of a Test MethodE 1361 Guide for Correction of Interelement Effects inX-Ray Spectrometric AnalysisE 1622 Practice for the Correction of Spectral Line Overlapin Wavelength X-Ray Spectrometry3. Terminology3.1 For definitions of terms used in this test method, refer toTe
7、rminology 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. Thesecondary X rays produced are dispersed by means of crystals,and the intensities are measured by suitable detectors atselected wavelengths. R
8、adiation measurements are made basedon the time required to reach a fixed number of counts, or onthe total counts obtained for a fixed time. Concentrations of theelements are determined by relating the measured radiation ofunknown specimens to analytical curves prepared with suitablereference materi
9、als. Either a fixed-channel, polychromatorsystem or a sequential, monochromator system may be used toprovide simultaneous or sequential determinations of elements.5. Significance and Use5.1 This procedure is suitable for manufacturing control andfor verifying that the product meets specifications. T
10、his testmethod provides rapid, multielement determinations with suf-ficient accuracy to ensure product quality and minimize pro-duction delays. The analytical performance data may be usedas a benchmark to determine if similar X-ray spectrometersprovide equivalent precision and accuracy, or if the pe
11、rfor-mance of a particular X-ray spectrometer has changed.5.2 Calcium is sometimes added to steel to effect inclusionshape control in order to enhance certain mechanical propertiesof steel. This test method is useful for determining the residualcalcium in the steel after such treatment.5.2.1 Because
12、 calcium occurs primarily in inclusions, theprecision of this test method is a function of the distribution ofthe calcium-bearing inclusions in the steel. The variation ofdeterminations on freshly prepared surfaces will give someindication of the distribution of these inclusions.1This test method is
13、 under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry of Metals, Ores, and Related Materials and is the directresponsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.Current edition approved Oct. 1, 2004. Published November 2000. Originallyapproved in 1987. Last previous
14、 edition approved in 2000 as E 1085 95 (2000).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.1Copyright ASTM
15、 International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6. Interferences6.1 Interelement or matrix effects may exist for some of theelements in 1.1. Mathematical corrections may be used to solvefor these effects. Various mathematical correction proceduresa
16、re commonly utilized. See Guide E 1361 and Practice E 1622.Any of these procedures is acceptable that will achieveanalytical accuracy equivalent to that provided by this testmethod.6.2 Because trace amounts of calcium are being determinedwith this test method, exercise care not to contaminate thespe
17、cimen. The presence of calcium in the grinding mediumwill contaminate the specimen to the extent that erratic andincorrect results will be obtained. Therefore, the grindingmedium shall be analyzed for calcium and only those materialsthat are free of calcium shall be used.7. Apparatus7.1 Specimen Pre
18、paration Equipment:7.1.1 Surface Grinder or Sander With Abrasive Belts, Disks,or Lathe, capable of providing a flat, uniform surface on thereference materials and test specimens.7.1.1.1 When calcium is to be determined, 240-grit,calcium-free silicon carbide belts or disks shall be used.7.2 Excitatio
19、n Source:7.2.1 X-Ray 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 o
20、f various high-purityelements, that are capable of continuous operation at requiredpotentials and currents, and will excite the elements to bedetermined.7.2.2.1 For the determination of calcium only chromiumtarget tubes were tested. Other targets shall be tested prior touse.7.3 Spectrometer, designe
21、d for X-ray emission analysis, andequipped with specimen holders and a specimen chamber. Thechamber may 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 curv
22、ed crystals with opti-mized capability for the diffraction of the wavelengths ofinterest.7.3.2 Collimator, for limiting the characteristic X rays to aparallel bundle when flat crystals are used in the instrument.For curved crystal optics, a collimator is not necessary.7.3.3 Detectors, sealed or gas-
23、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,calcium, silicon, phosphorus, and sulfur). The system shallconsist of a vacuum pump, gage, and electrical controls toprovide
24、automatic pumpdown of the optical path and maintaina controlled pressure, usually 13 Pa (100 m Hg) or less,controlled to 63Pa(620 m Hg).7.4 Measuring System, consisting of electronic circuits ca-pable of amplifying and integrating pulses received from thedetectors. For some measurements, pulse heigh
25、t analyzers maybe required to provide more accurate measurements. Thesystem shall be equipped with an appropriate recording 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 Mat
26、erials9.1 Certified Reference Materials are available from theNational Institute of Standards and Technology3and otherinternational certification agencies.9.2 Reference Materials with matrices similar to that of thetest specimen and containing varying amounts of the elementsto be determined may be u
27、sed provided they have beenchemically analyzed in accordance with ASTM standard testmethods. These reference materials shall be homogeneous, andfree of voids or porosity.9.3 The reference materials shall cover the concentrationranges of the elements being sought. A minimum of threereference material
28、s shall be used for each element.10. Hazards10.1 Occupational Health and Safety standards for ionizingradiation4shall be observed at all X-ray emission spectrometerinstallations. It is also recommended that operating and main-tenance personnel follow the guidelines of safe operatingprocedures given
29、in current handbooks and publications fromthe National Institute of Standards and Technology5,6and theU.S. Government Printing Office,7or similar handbooks onradiation safety.10.2 X-ray equipment shall be used only under the guidanceand supervision of a responsible, qualified person.10.3 Monitoring
30、Devices, either film badges or dosimetersmay be worn by all operating and maintenance personnel.Safety regulations shall conform to applicable local, state, andfederal regulations. To meet local, state, and federal radiationstandards, periodic radiation surveys of the equipment for leaksand excessiv
31、e scattered radiation shall be made by a qualifiedperson using an ionization-chamber detector. The personal filmbadge survey record, the radiation survey record, and anequipment maintenance record shall be available upon request.3Office of Standard Reference Materials, National Institute of Standard
32、s andTechnology, U.S. Department of Commerce, Gaithersburg, MD 20899.4ANSI/NBS Handbook 114, General Safety Standard for Installations UsingNon-Medical X-Ray and Sealed Gamma-Ram Sources, available from AmericanNational Standards Institute, 11 W. 42nd St., 13th Floor, New York, NY 10036.5NBS Handboo
33、k 76, Medical X-Ray Protection Up to Three Million Volts,available as NCRP 33 from NCRP Publications, 7910 Woodmont Ave., Suite 1016,Bethesda, MD 20814.6ANSI N43.2-1977/NBS Handbook 111, Radiation Safety for X-Ray Diffractionand Fluorescence Analysis, available from American National Standards Insti
34、tute,11 W. 42nd St., 13th Floor, New York, NY 10036.7Moore, T. M., and McDonald, D. J., Radiation Safety Recommendations forX-Ray Diffraction and Spectrographic Equipment, MORP 68-14, 1968, availablefrom National Technical Information Service, Springfield, VA 22161.E 1085 95 (2004)210.4 Special prec
35、autions for operators and maintenancepersonnel shall be posted at the equipment site.10.5 Radiation caution signs shall be posted near the X-rayequipment and at all entrances to the radiation area, consistentwith state and federal regulations.10.6 Fail-safe “X-Ray On” warning lights shall be used on
36、the equipment.11. Preparation of Reference Materials and TestSpecimens11.1 Prepare the reference materials and test specimens toprovide a clean, flat uniform surface to be exposed to the X-raybeam. For abrasive sanding, select a grit size, and use that gritand size exclusively for all reference mate
37、rials and testspecimens.11.2 Refinish the surface of the reference materials and testspecimens as needed to eliminate surface contamination.12. Preparation of Apparatus12.1 Prepare and operate the spectrometer in accordancewith the manufacturers instructions.NOTE 1It is not within the scope of this
38、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 manufacturers manual.12.1.1 Start-upTurn on the power supply and electroniccircuits and allow sufficient t
39、ime for instrument warm-up priorto taking measurements.12.2 Tube Power SupplyAdjust the voltage of the powersupply to produce optimum conditions.12.2.1 The voltage and current established as optimum forthe X-ray emission power supply in an individual laboratoryshall be reproduced for subsequent meas
40、urements.12.3 Proportional Counter Gas Flow When a gas-flowproportional counter is used, adjust 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 and adjusted before the instrument isu
41、sed.12.4 Measurement ConditionsThe K-a lines for eachelement are used. The peak location, when using a scanningspectrometer, should be determined for each instrument.12.4.1 Crystals and DetectorsThe following crystals anddetectors are used for the elements indicated:Element CrystalADetectorANickel L
42、1, L2 SP, Sc, FPChromium L1, L2 SP, Sc, FPManganese L1, L2 SP, Sc, FPSilicon PET, InSb FPMolybdenum L1, L2 ScCopper L1, L2 SP, Sc, FPVanadium L1, L2 SP, Sc, FPCobalt L1, L2 SP, Sc, FPSulfur Ge FPNiobium L1, L2 ScPhosphorus Ge FPCalcium L1 FP_AL1 = LiF(200), L2 = LiF(220), SP = Sealed Proportional, S
43、c = 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 minimum of10 000 counts is required for 1 % precision of the countingstatistics and 40 000 fo
44、r 0.5 %.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 materials for each element.Measure the reference ma
45、terials at least two different times oneach of two separate days. Prepare an analytical curve for eachelement being determined (refer to Practice E 305).13.2 Standardization (Analytical Curve Adjustment)Using a control reference material, check the calibration of theX-ray spectrometer at a frequency
46、 consistent with statisticalprocess control practice, or when the detector gas or majorcomponents have been changed. If the calibration checkindicates that the spectrometer has drifted, make appropriateadjustments in accordance with the instructions in the manu-facturers manual. Refer to Practice E
47、305 for frequency ofverification of standardization.14. Procedure14.1 Specimen LoadingOrient the reference materials andtest specimens in the specimen chamber so that the relationshipbetween the X-ray beam and the grinding striations is the samefor all measurements. This is an essential requirement
48、if thespectrometer is not equipped with a specimen spinner, but isnot necessary when a spinner is used.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 cou
49、ntor 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 elementalcombinations (for example, molybdenum and sulfur; molyb-denum and phosphorus; iron and cobalt). Therefore, exercisecare in the interpretation of intensities when both elements arepresent. Use mathematical calculations to correct for suchinterferences. See Practice E 1622.14.5 Replicate MeasurementsMake a single measurementon each test specimen. T
