1、Designation: E1086 08E1086 14Standard Test Method forAtomic Emission Vacuum Spectrometric Analysis ofAustenitic Stainless Steel by Point-to-Plane ExcitationTechniqueSpark Atomic Emission Spectrometry1This standard is issued under the fixed designation E1086; the number immediately following the desi
2、gnation indicates the year oforiginal adoption or, in the case of revision, 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 method2 covers for t
3、he atomic emission vacuum spectrometric the analysis of austenitic stainless steel in solid formby the point-to-plane excitation technique by spark atomic emission vacuum spectrometry for the following elements in theconcentration ranges shown:shownElement Concentration Range, %Element Composition R
4、ange, %Chromium 17.0 to 23.0Nickel 7.5 to 13.0Molybdenum 0.01 to 3.0Manganese 0.01 to 2.0Silicon 0.01 to 0.90Copper 0.01 to 0.30Carbon 0.005 to 0.25Phosphorus 0.003 to 0.15Sulfur 0.003 to 0.0651.2 This test method is designed for the routine analysis of chill-cast disks or inspection testing of stai
5、nless steel samples thathave a flat surface of at least 13 mm (0.5 in.) in diameter. The samples must be sufficiently massive to prevent overheating duringthe discharge and of a similar metallurgical condition and composition as the reference materials.1.3 Analytical curves are plotted using the con
6、centration ratio method as shown in Practice E158. One or more of the referencematerials must closely approximate the composition of the specimen. The technique of analyzing reference materials along withunknowns and performing the indicated mathematical corrections may also be used to correct for i
7、nterference effects and tocompensate for errors resulting from instrument drift.Avariety of such systems are commonly used.Any of these that will achieveanalytical accuracy equivalent to that reported for this test method are acceptable.1.4 This standard does not purport to address all of the safety
8、 concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:3E135 Terminology Relating to Analytic
9、al Chemistry for Metals, Ores, and Related MaterialsE158 Practice for Fundamental Calculations to Convert Intensities into Concentrations in Optical Emission SpectrochemicalAnalysis (Withdrawn 2004)4E172 Practice for Describing and Specifying the Excitation Source in Emission Spectrochemical Analysi
10、s (Withdrawn 2001)4E305 Practice for Establishing and Controlling Atomic Emission Spectrochemical Analytical CurvesE406 Practice for Using Controlled Atmospheres in Spectrochemical AnalysisE876 Practice for Use of Statistics in the Evaluation of Spectrometric Data (Withdrawn 2003)41 This test method
11、 is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and is the direct responsibility ofSubcommittee E01.01 on Iron, Steel, and Ferroalloys.Current edition approved Oct. 1, 2008March 1, 2014. Published November 2008April 2014. Originally ap
12、proved in 1985. Last previous edition approved in 20052008as E1086 94 (2005).E1086 08. DOI: 10.1520/E1086-08.10.1520/E1086-14.2 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:E02-1023.3 For referencedASTM standards, visit theAS
13、TM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an in
14、dication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be
15、 considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1E1060 Practice for Interlaboratory Testing of Spectrochemical Methods of Analysis4 (Withdrawn 1997)E1601E1329 Practice for Conducting an Interlaboratory
16、 Study to Evaluate the Performance of anAnalytical MethodVerificationand Use of Control Charts in Spectrochemical AnalysisE1806 Practice for Sampling Steel and Iron for Determination of Chemical Composition2.2 Other ASTM Documents:ASTM MNL 7 Manual on Presentation of Data and Control Chart Analysis5
17、3. Terminology3.1 DefinitionsFor definitions of terms used in this test method, refer to Terminology E135.4. Summary of Test Method4.1 A controlled discharge is produced between the flat surface of the specimen and the counter electrode. The radiant energyof selected analytical lines are converted i
18、nto electrical energies by photomultiplier tubes and stored on capacitors. The dischargeis terminated at a predetermined level of accumulated radiant energy from the internal standard iron line or after a fixedexposureintegration time. At the end of the exposureintegration period, the charge on each
19、 capacitor is measured, and displayedor recorded as a relative energy or concentration. mass fraction %.5. Significance and Use5.1 The chemical composition of stainless steels must be determined accurately in order to ensure the desired metallurgicalproperties. This procedure is suitable for manufac
20、turing control and inspection testing.6. Apparatus6.1 Sampling and Sample Preparation Equipment:6.1.1 Refer to Practice E1806 for devices and practices to sample liquid and solid steel.6.1.2 Abrasive Grinder, a suitable belt grinder, horizontal disk grinder, or similar grinding apparatus. The result
21、ing surfaceshould be uniformly plane and free of defects. These may be either wet or dry grinding devices. Grinding materials with grit sizesranging from 60 to 180 have been found satisfactory.6.2 Excitation Source, with parameters capable of producing a usable spectrum in accordance with 11.1 and P
22、ractice E172.6.3 Excitation Stand, suitable for mounting in optical alignment, a flat surface of the specimen in opposition to a counterelectrode. The stand shall provide an atmosphere of argon and may be water cooled. Counter electrodes and argon are describedin 7.1 and 7.2.6.4 Spectrometer, having
23、 sufficient resolving power and linear dispersion to separate clearly the analytical lines from other linesin the spectrum of a specimen in the spectral region 170.0 nm to 500.0 nm. Spectrometer characteristics for two of the instrumentsused in this test method are described as having dispersion of
24、0.697 nm/mm (first order), and a focal length of 1 m. Spectral linesare listed in Table 1.6.5 Measuring System, consisting of photomultiplier tubes having individual voltage adjustment, capacitors on which the outputof each photomultiplier tube is stored and an electronic system to measure voltages
25、on the capacitors either directly or indirectly,and the necessary switching arrangements to provide the desired sequence of operation.6.6 Readout Console, capable of indicating the ratio of the analytical lines to the internal standard with sufficient precision toproduce the accuracy of analysis des
26、ired.6.7 Vacuum Pump, capable of maintaining a vacuum of 25 m Hg or less.6.8 Gas System, consisting of an argon supply with pressure and flow regulation. Automatic sequencing shall be provided toactuate the flow at a given rate for a specific time interval. The flow rate may be manually or automatic
27、ally controlled. The argonsystem shall be in accordance with Practice E406.NOTE 1It is not within the scope of this test method to prescribe all details of equipment to be used. Equipment varies among laboratories.7. Reagents and Materials7.1 Argon, either gaseous or liquid, must be of sufficient pu
28、rity to permit proper excitation of the analytical lines of interest.Argon of 99.998 % purity has been found satisfactory. Refer to Practice E406.7.2 Counter Electrodes, can vary in diameter from 1.5 mm to 6.5 mm (depending on the instrument manufacturer) and typicallyare machined to a 90 or 120 ang
29、led tip. Silver or thoriated tungsten rods are typically used. Other material may be used providedit can be shown experimentally that equivalent precision and accuracy are obtained.4 The last approved version of this historical standard is referenced on www.astm.org.Withdrawn 1997.5 ASTM Manual Seri
30、es, ASTM International, 8th edition, 2010.E1086 1428. Reference Materials8.1 Certified Reference Materials are available from the National Institute of Standards and Technology6 and other internationalcertification agencies.8.2 Reference Materials with matrices similar to that of the test specimen a
31、nd containing varying amounts of the elements tobe determined may be used provided they have been chemically analyzed in accordance withASTM standard test methods. Thesereference materials shall be homogeneous, and free of voids or porosity.8.3 The reference materials shall cover the concentration r
32、anges of the elements being sought. A minimum of three referencematerials shall be used for each element.9. Preparation of Samples9.1 The specimens and reference materials must be prepared in the same manner. A specimen cut from a large sample sectionmust be of sufficient size and thickness for prep
33、aration and to properly fit the spectrometer stand.9.2 Ensure the specimens are homogenous and free from voids and pits in the region to be excited. Grind the surface with anabrasive belt or disc. Refer to 6.1.2. Perform the final grind with a dry abrasive belt or disc.10. Preparation of Apparatus10
34、.1 Follow the manufacturers instructions for verifying the optical alignment of the entrance slit and programming theappropriate wavelengths (Table 1).11. Excitation and ExposureIntegration11.1 Electrical ParametersTwo different types of sources were employed in the testing of this test method.11.1.
35、1 Directional Self-Initiating Capacitor Discharge Source:6 Available from National Institute of Standards and Technology (NIST), 100 Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http:/www.nist.gov.TABLE 1 Analytical and Internal Standard LinesElement Wavelength, nmConcentration Mass Fraction%
36、Switch OverPointsChromium 298.919Nickel 243.789227.021218.549216.910Molybdenum 202.030 1 %308.561 1 %369.265Manganese 293.306Silicon 251.612A288.158Copper 327.396 0.10 %224.699 0.10 %Carbon 193.092Phosphorus 178.287ASulfur 180.731IronB 271.441322.775A Silicon 251.612 can have a small but significant
37、 interference from molybdenum251.611. Phosphorus 178.287 may show small but significant interferences fromunlisted lines or background due to molybdenum, chromium, and manganese.Interference corrections will not be necessary if: separate silicon and phosphoruscurves are used for 316 and 317 alloys;
38、the manganese content varies onlybetween 0.7 % and 1.5 %; and the chromium concentration is held between 17 %and 20 %.B Either iron line 271.441 or 322.775 with narrow entrance and exit slits to avoidinterference from manganese 322.809 can be used as internal standard with anyof the listed analytica
39、l lines. Iron 271.441 is not appropriate for tungsten tool steelsor super alloys with high cobalt because of interference from cobalt 271.442.E1086 143Capacitance, F 0.015Inductance, L1, H 310Inductance, L2, H 20Resistance, residualPotential, V 13 500Peak Current, A 90First Valley Current, A 60Curre
40、nt pulse duration, s 120Number of discharges/s 24011.1.1.1 ExposureExcitation Conditions:Flush, s 7 Argon Flow 0.42 m3/hPreburn, s 20 Argon Flow 0.42 m3/hIntegration, s 20 Argon Flow 0.42 m3/h11.1.2 Triggered Capacitor Discharge Source:Preburn ExposurePreburn IntegrationPulse Output:Capacitance, F (
41、d-c charged) 7.5 2.5Inductance, H 50 50Resistance, residual residualPotential, V 950 950Peak Current, A 275 100Current pulse duration, s 250 130Number of discharges/s 120 120Trigger:Capacitance (d-c charged), F 1.2 .Inductance, H residual .Resistance, residual .Potential, V 425 .11.1.2.1 ExposureExc
42、itation Conditions:Flush, s 2 Argon Flow0.56 m3/hPreburn, s 10 Argon Flow0.56 m3/hExposure, s 10 or 15 Argon Flow0.56 m3/hIntegration, s 10 or 15 Argon Flow0.56 m3/h12. Calibration, Standardization, and Verification12.1 CalibrationUsing the conditions given in 11.1, excite each calibrant and standar
43、dant drift correction sample two to fourtimes and bracket these with similar excitations of any verifiers.Averifier may be used as a calibrant even though it is burned onlyas a verifier. There shall be at least three calibrants for each element, spanning the required concentration range. If the spec
44、trometersystem and software permits, perform random excitations of each calibrant and drift correction sample and repeat with differentrandom sequences at least four times. Follow the procedure for the concentration-ratio method in accordance with Practicespec-trometer manufacturers software procedu
45、res to convert sample intensities into E158. mass fraction %. Using the averages of thedata for each point, determine analytical curves in accordance with Practice E305.12.2 StandardizationFollowing the manufacturers recommendations, standardize on an initial setup or anytime that it isknown or susp
46、ected that readings have shifted. Make the necessary corrections either by adjusting the controls on the readout orby applying arithmetic corrections. Standardization will be done anytime verification indicates that readings have gone out ofstatistical control.12.3 VerificationAnalyze verifiers in r
47、eplicate to confirm that they read within expected confidence interval, in accordancewith 12.4.12.3.1 Each laboratory should determine the frequency of verification necessary based on statistical analysis. Typically, every4 h to 8 hoursh is practical and adequate (or if the instrument has been idle
48、for more than 1 hour). If the results are not within thecontrol limits established in 12.4, perform a standardization and then repeat verification. Repeat standardization as necessary soverifications are within control limits or investigate further for instrument problems.12.4 The confidence interva
49、l will be established from observations of the repeatability of the verifiers and determining theconfidence interval for some acceptable confidence level in accordance with Practice E876 or by establishingutilizing the upperand lower limit of a control chart in accordance with Practice E1329 or ASTM Manual MNL7A.MNL The latter is the preferableapproach since it also monitors the consistency of the statistics of the measurements and provides a way of maintaining a recordof performance.7.13. Procedure for Excitation and Radiation Measurement13.1 Produ
