1、Designation: E 322 96 (Reapproved 2004)Standard Test Method forX-Ray Emission Spectrometric Analysis of Low-Alloy Steelsand Cast Irons1This standard is issued under the fixed designation E 322; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、 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.1. Scope1.1 This test method covers the X-ray emission spectromet-ric analysis of low-alloy steels and cas
3、t irons for the followingelements in the ranges indicated:Elements Concentration Range, %Manganese 0.20 to 1.50Nickel 0.10 to 1.00Chromium 0.10 to 1.00Molybdenum 0.04 to 0.40Copper 0.05 to 0.30Vanadium 0.03 to 0.25NOTE 1These concentration ranges can be extended by the use ofsuitable standards. The
4、detection limit for the elements is lower than thelisted value. The ranges represent the actual levels at which this testmethod was tested.1.2 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
5、 establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE 350 Test Methods for Chemical Analysis of
6、Carbon Steel,Low Alloy Steel, Silicon Electrical Steel, Ingot Iron, andWrought IronE 351 Test Methods for Chemical Analysis of Cast IronAll TypesE 882 Guide for Accountability and Quality Control in theChemical Analysis Laboratory3. Terminology3.1 All terms used in this test method are in conformanc
7、ewith Terminology E 135.4. Summary of Test Method4.1 The sample is finished to a clean, uniform surface, andthen irradiated by an X-ray beam of high energy. The second-ary X rays produced are dispersed by means of a crystal and theintensities are measured by a detector at selected wavelengths.The re
8、sults are obtained by relating measured intensities to anappropriate calibration curve.5. Significance and Use5.1 This test method is a comparative method intended foruse as a routine method to test materials for compliance withcompositional specifications. It is assumed that all who use thistest me
9、thod will be trained analysts capable of performingskillfully and safely. It is expected that work will be performedin a properly equipped laboratory under appropriate qualitycontrol practices, such as those described in Guide E 882.6. Apparatus6.1 Specimen Preparation Equipment:6.1.1 Disk or Belt S
10、ander, capable of providing test speci-mens with a uniform, clean surface finish, or other equivalentfinishing device.6.2 Excitation Source:6.2.1 X-ray Generator, with a full-wave rectified powersupply, or constant potential power supply.6.2.2 X-ray Tube, with a high-purity tungsten target.6.3 Spect
11、rometer:6.3.1 Analyzing Crystal, lithium fluoride, flat or curvedhaving a 2d spacing of 0.40276 nm.6.3.2 CollimationProvide appropriate collimation toachieve the required resolution. For curved optics, no collima-tion is required.6.3.3 GoniometerA goniometer that provides an angularscan from 10 to 1
12、48.6.3.4 Detectors, proportional or scintillation counter.1This 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.Current edition approved O
13、ct. 1, 2004. Published Oct. 1, 2004. Originallyapproved in 1967. Last previous edition approved in 1996 as E 322 96e1.2For 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 t
14、o the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.4 Measuring UnitAn electronic circuit panel capable ofamplifying, counting, or integrating pulses received from thedetector tu
15、be. In addition, a pulse height analyzer should beavailable for pulse energy discrimination if needed. Goodprecision and accuracy have been obtained without the use ofa pulse height analyzer.7. Reference Materials7.1 Certified Reference Materials Low-alloy steel andcast iron certified reference mate
16、rials are commercially avail-able from a number of sources.7.2 Low-Alloy Steel Reference MaterialsLow-alloy steeland cast iron reference materials can be used. They should beanalyzed and thoroughly evaluated in accordance with TestMethods E 350 and E 351.8. Safety Precautions8.1 Normal safety precau
17、tions for X-ray spectrographicinstallations are to be observed. It is recommended that suitablemonitoring devices (film badges and dosimeters) be availableand worn by all participating personnel. Accurate control andregulation of monitoring devices at all times is recommended.9. Preparation of Refer
18、ence Materials and Specimens9.1 Using the belt sander equipped with aluminum oxideabrasive paper, prepare a smooth, clean surface on the testspecimen having a minimum area of 25 mm2. Use 240 grit orfiner, but after a grit has been selected, the same grit numbershould always be used. Other equivalent
19、 finish-machiningmethods can be used.NOTE 2Any facets or imperfections in the flatness of the finishedsurface have been found to give marked changes in response.9.2 Repolish the reference materials as needed to eliminateoxidized surfaces.10. Preparation of Apparatus10.1 Prepare the apparatus as foll
20、ows:Voltage, kV 50 (Note 3)Current, mA 40 (Note 3)Detector scintillation or proportionalNOTE 3Lower values for voltage and current have been foundsatisfactory.11. Excitation and Radiation Measurement11.1 ExcitationPlace the specimen into the instrument,taking care not to contaminate the specimen sur
21、face. Generatethe secondary fluorescence using the settings listed in Section9.11.2 Radiation MeasurementsMake radiation measure-ment of the analytical lines listed in Table 1 using the settingslisted in Section 9.NOTE 4The listed degree 2 u peaks represent the theoretical valuesfor a lithium fluori
22、de crystal. The actual goniometer setting for these peaksmust be determined experimentally within each laboratory. Periodicchecks to verify this setting are advisable.11.2.1 Obtain the radiation measurement for each element.Collect sufficient counts to produce the required statisticalprecision. Use
23、the following to determine the minimum num-ber of counts required:Element Total CountsNickel 64 000Manganese 64 000Chromium 64 000Molybdenum 32 000Copper 32 000Vanadium 16 000NOTE 5Larger numbers than the above listed total counts have beenaccumulated within a reasonable counting time by various ins
24、truments.12. Calibration and Standardization12.1 CalibrationMake measurements on a sufficient num-ber of reference materials to establish the calibration curve.Prepare the calibration curves for each element by plotting theintensity versus concentration values.12.2 StandardizationWhenever samples ar
25、e to be ana-lyzed, run at least a high- and low-concentration material toascertain that the calibration is current.13. Calculation13.1 The concentrations are determined from the preparedcalibration curves.14. Precision and Bias14.1 PrecisionPrecision data are shown in Table 2.14.2 BiasRepresentative
26、 bias data are shown in Table 3.14.2.1 It is unlikely that any results using this test methodwill deviate more than the maximum deviation shown in Table3, provided the operating parameters are as specified.TABLE 1 Analytical PeaksElement Shell Order2u(Note 5)Wave-length, nmCrystalNickel K 1 48.61 0.
27、1659 LiFManganese K 1 62.91 0.2103 LiFChromium K 1 69.29 0.2291 LiFMolybdenum K 1 20.28 0.0710 LiFCopper K 1 44.96 0.1542 LiFVanadium K 1 76.84 0.2505 LiFTABLE 2 Precision DataAElementConcentrationRange, %Relative Standard Deviation,RSD %BManganese 0.52 to 1.41 0.60Nickel 0.23 to 0.79 0.83Chromium 0
28、.21 to 0.86 0.88Molybdenum 0.05 to 0.35 1.02Copper 0.06 to 0.27 1.04Vanadium 0.03 to 0.22 1.16AThe values were obtained by pooling data from five laboratories.BRelative standard deviation, RSD, in this method, is calculated as follows:RSD 5 100/X! = (d2/n 2 1!where:X= average concentration, %,d = di
29、fference of the determination from the mean, andn = number of determinations.E 322 96 (2004)2NOTE 6The bias approaches the precision when the reference mate-rials and the unknown are similar in composition. When referencematerials and unknowns are not alike, one must verify the absence ofinterferenc
30、es such as zirconium on molybdenum Ka, the absence ofinter-element effects such as molybdenum and nickel on chromium, andthe absence of differences due to metallurgical history or condition of thesample.15. Keywords15.1 cast iron; low-alloy steel; spectrometric analysis;X-ray emissionASTM Internatio
31、nal takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their
32、 own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be
33、 addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards
34、, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9
35、585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).TABLE 3 Bias DataElementEstablishedValue,A%Deviation ofX-ray ValueBfrom Estab-lished Value,relative %MaximumObservedDeviationfromEstablishedValue, %Manganese 0.6400.9101.1201.140.550.960.030.020.0
36、25Nickel 0.3250.5200.6951.420.230.070.010.0050.007Chromium 0.3500.5150.7000.492.350.740.010.0150.03Molybdenum 0.1000.1950.2951.903.330.580.0050.0080.005Copper 0.0600.0800.1753.830.630.970.0050.0040.007Vanadium 0.0450.14512.440.680.010.008AThe samples used for this program are secondary standards whose values areaverages from chemical analyses performed by eight laboratories.BThese values were calculated from the total results reported from threeseparate days of study, and five participating laboratories.E 322 96 (2004)3
