1、Designation: E1257 93 (Reapproved 2008)E1257 16Standard Guide forEvaluating Grinding Materials Used for Surface Preparationin Spectrochemical Analysis1This standard is issued under the fixed designation E1257; the number immediately following the designation indicates the year oforiginal adoption or
2、, 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 guide covers recommendations for the evaluation of various grinding materi
3、als used to prepare the surfaces ofspecimens to be analyzed by optical spark atomic emission or X-ray emission spectroscopy.fluorescence spectrometry.1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibilityof the user of this
4、 standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials3. Terminology3.1 For definitions o
5、f terms used in this guide, refer to Terminology E135.4. Significance and Use4.1 The grinding materials used for the preparation of the surfaces of specimens prior to analysis by optical spark atomicemission or X-ray emission spectroscopyfluorescence spectrometry can contaminate the surface and thus
6、 produce erroneousresults.This guide provides examples of the effects of these contaminations and recommendations for evaluating grinding materialsto eliminate or reduce these effects in spectrochemical analysis.4.2 The examples given in this guide are not the only contaminations whichthat can occur
7、. Especially in X-ray spectrometry,all phases of the surface preparation should be examined for potential contamination effects.4.3 Analytical significance of the contaminations observed depends on the needs of the analyst for the particular application ata given concentration position.5. Evaluation
8、 of Grinding Materials by Direct Analysis5.1 Table 1 shows an example of semiquantitative spectrographicspectrometric analysis of various grinding belts from differentproducers. An examination of these analyses identifies the elements most likely to contaminate the surface of the specimen. Themore c
9、ritical the element and the lower its concentration mass fraction in the specimen, the more important are low-levelconcentrationscontaminants in the belts.5.1.1 For example, using the 80-grit zircon belt in the determination of 0.5 % chromium, the trace level of chromium in the beltshould cause no p
10、roblem, but in the determination of 0.02 % aluminum, that belt probably will cause a problem. In thedetermination of calcium at ppmg/g levels in steel, even low levels of calcium in the belts cause problems.5.2 Figs. 1-6 show energy dispersive X-ray analyses of various belts and the same logic appli
11、ed in 5.1 can be used with theseanalyses. Major components in the belts will cause greater problems in the determination of these elements.1 This guide is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and is the direct responsibility ofS
12、ubcommittee E01.20 on Fundamental Practices.Current edition approved May 1, 2008Feb. 1, 2016. Published June 2008March 2016. Originally approved in 1988. Last previous edition approved in 20032008 asE1257 93 (2003).(2008). DOI: 10.1520/E1257-93R08.10.1520/E1257-16.2 For referencedASTM standards, vis
13、it theASTM 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 standa
14、rd an indication 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
15、is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.2.1 Direct analysis of the grinding material is particularly useful in such analyses as the determination of calcium in steel,where the analyt
16、e is generally too inhomogeneous to use the methods described in Section 6. This analysis requires a virtuallycalcium-free belt as in Fig. 2.TABLE 1 Semiquantitative (Spectrographic) Analysis of Grinding Belt AbrasivesConcentration,% 80-Grit Silicon Carbide 80-Grit Alumina 80-Grit ZirconNo. 1 No. 2
17、No. 3 No. 1 No. 2 No. 310+ Si Si Si Al Al, Ca Al Al, Ca, Zr110 Ca Ca Ti Si, Na, Fe0.11 Ba, Mg Fe, Al, Na Mg, Si, Ca, Ti Fe, Si, Na Ca Ti, Zn0.050.5 B Fe, B Mg0.010.1 Mn, Na B, Mg Al Ba, B Zr Na Mg0.0050.05 V, Cu, Ti, Ni Mn, Ti V, Ca, Na, Ni Mn, Zr, Cu, Na B B, Fe, Si B, Mn, SrTrace0.01 Mo, Zr, Sr Ba
18、, V, Zr, Cu,Ni, SrBa, Mn, Mg, Pb, Cr,Zr, Cu, Ti, SrNi Ba, Mn, Cr, V,Cu, Ni, SrMn, Mo, Cu,Sr, MgBa, Pb, Cr, V,Mo, CuTABLE 1 Semiquantitative (Spectrographic) Analysis of Grinding Belt AbrasivesComposition, % 80-Grit Silicon Carbide 80-Grit Alumina 80-Grit ZirconNo. 1 No. 2 No. 3 No. 1 No. 2 No. 310+
19、Si Si Si Al Al, Ca Al Al, Ca, Zr110 Ca Ca Ti Si, Na, Fe0.11 Ba, Mg Fe, Al, Na Mg, Si, Ca, Ti Fe, Si, Na Ca Ti, Zn0.050.5 B Fe, B Mg0.010.1 Mn, Na B, Mg Al Ba, B Zr Na Mg0.0050.05 V, Cu, Ti, Ni Mn, Ti V, Ca, Na, Ni Mn, Zr, Cu, Na B B, Fe, Si B, Mn, SrTrace0.01 Mo, Zr, Sr Ba, V, Zr, Cu,Ni, SrBa, Mn, M
20、g, Pb, Cr,Zr, Cu, Ti, SrNi Ba, Mn, Cr, V,Cu, Ni, SrMn, Mo, Cu,Sr, MgBa, Pb, Cr, V,Mo, CuTABLE 2 X-Ray Fluorescence Analysis of a Steel Specimen Using Various Grinding MediaApparent Concentration, %, UsingElement Si C Belt Alumina Belt Zircon Belt Resin BondedDiamond Metal BondedDiamond Diamond Paste
21、 Surface GrinderMolybdenum 0.057 0.056 0.058 0.057 0.057 0.057 0.058Niobium 0.034 0.032 0.032 0.033 0.032 0.032 0.033Copper 0.315 0.310 0.320 0.316 0.317 0.316 0.317Nickel 0.297 0.296 0.292 0.295 0.322A 0.296 0.295Cobalt 0.014 0.011 0.010 0.011 0.010 0.011 0.012Manganese 1.39 1.40 1.39 1.40 1.39 1.4
22、0 1.40Chromium 0.197 0.193 0.197 0.196 0.195 0.196 0.195Vanadium 0.061 0.059 0.060 0.059 0.060 0.059 0.059Titanium 0.024 0.025 0.024 0.024 0.025 0.024 0.024Phosphorus 0.012 0.011 0.012 0.011 0.012 0.012 0.011Silicon 0.444A 0.234 0.234 0.245A 0.293A 0.235 0.236Antimony 0.006 0.005 0.005 0.005 0.006 0
23、.005 0.006Tin 0.023 0.022 0.023 0.023 0.022 0.023 0.022Aluminum 0.016 0.070A 0.085A 0.026A 0.090A 0.015 0.030AZirconium 0.050 0.051 0.066A 0.051 0.050 0.051 0.050TABLE 2 X-Ray Fluorescence Analysis of a Steel Specimen Using Various Grinding MediaApparent Composition, %, UsingElement Si C Belt Alumin
24、a Belt Zircon Belt Resin BondedDiamond Metal BondedDiamond Diamond Paste Surface GrinderMolybdenum 0.057 0.056 0.058 0.057 0.057 0.057 0.058Niobium 0.034 0.032 0.032 0.033 0.032 0.032 0.033Copper 0.315 0.310 0.320 0.316 0.317 0.316 0.317Nickel 0.297 0.296 0.292 0.295 0.322A 0.296 0.295Cobalt 0.014 0
25、.011 0.010 0.011 0.010 0.011 0.012Manganese 1.39 1.40 1.39 1.40 1.39 1.40 1.40Chromium 0.197 0.193 0.197 0.196 0.195 0.196 0.195Vanadium 0.061 0.059 0.060 0.059 0.060 0.059 0.059Titanium 0.024 0.025 0.024 0.024 0.025 0.024 0.024Phosphorus 0.012 0.011 0.012 0.011 0.012 0.012 0.011Silicon 0.444A 0.234
26、 0.234 0.245A 0.293A 0.235 0.236Antimony 0.006 0.005 0.005 0.005 0.006 0.005 0.006Tin 0.023 0.022 0.023 0.023 0.022 0.023 0.022Aluminum 0.016 0.070A 0.085A 0.026A 0.090A 0.015 0.030AZirconium 0.050 0.051 0.066A 0.051 0.050 0.051 0.050A Elements that exhibit contamination from grinding media.E1257 16
27、26. Evaluation of Grinding Materials by Specimen Examination6.1 The effect of grinding materials depends on the analytical method. In optical spark atomic emission analysis, the preburnwill, in general, volatilize the grinding material left on or driven into the surface (see 6.3). For X-ray emission
28、fluorescence analysis,the material left on the surface will be analyzed as being specimen material.FIG. 1 EDX Analysis of Silicon Carbide Grinding Belt, 60-GritFIG. 2 EDX Analysis of Silicon Carbide Grinding Belt, 240-GritFIG. 3 EDX Analysis of Alumina Grinding Belt, 60-GritE1257 1636.2 Table 2 show
29、s X-ray emissionfluorescence analyses of a steel specimen after surfacing with various grinding materials. Bytabulating the results in this manner, it becomes obvious what problems are occurring from the various grinding materials. Wherethere is no change from material to material, beyond the precis
30、ion of the method of analysis and the homogeneity of the material,no contamination has occurred. But where the concentrationcomposition of a given element appears higher, there has beencontamination. Such is the case with the determination of silicon using the silicon carbide belt and the bonded dia
31、mond wheels;FIG. 4 EDX Analysis of Alumina Grinding Belt, 120-GritFIG. 5 EDX Analysis of Zircon Grinding Belt, 60-GritFIG. 6 EDX Analysis of Zircon Grinding Belt, 120-GritE1257 164with the determination of zirconium using zircon belts; with the determination of aluminum using the alumina and zircon
32、belts,the bonded diamond wheels, and the surface grinder; and with the determination of nickel using the metal bonded diamond wheel.6.2.1 This method requires the use of homogeneous materials to attain the required precision to detect low levels ofcontamination. Materials should be examined by repli
33、cate determinations using the same grinding material beforehand to assurethat they are homogeneous. If inhomogeneity seems to be excessive for one element, that may come from the grinding material,for example, silicon from silicon carbide, repeat the examination using a different grinding material.6
34、.2.2 Generally this method is convenient because it determines the contamination which actually occurs in the type of materialbeing analyzed and does not require analysis of the grinding material itself. An exception is the calcium determination mentionedin 5.2.1.6.3 In optical spark atomic emission
35、 analysis, a finite time is required to clean the specimen surface (by volatilization).Intensity-time studies show that preburn periods as long as 20 s can be required to reach stable intensity ratios for elementscomprising the grinding matrix. Fig. 7 shows time studies for carbon in a specimen surf
36、aced with silicon carbide, alumina, zircon,and a lathe. Fig. 8 shows the time studies for aluminum. Under the conditions used for these tests, a total of 4800 dischargesoccurred in the 20-s period. Sources running at lower rates may require longer preburn periods. Fig. 8 shows that, compared toa spe
37、cimen surfaced with lathe, the aluminum value found at the end of the preburn period can be higher on the alumina and zirconground specimens. Analytical significance will depend on the concentrationcomposition level. Similar results can be shown forother elements, especially silicon and zirconium un
38、der the conditions used. Different source conditions may show different results.6.3.1 Although the preburn generally removes most of the grinding material, in analyses where the highest accuracy is desired,grinding materials containing the analyte element should be avoided.7. Keywords7.1 grinding ma
39、terial; specimen preparation; spectrochemical analysisFIG. 7 Time Studies: CarbonOptical CarbonSpark Atomic Emission Analysis of High-Purity IronE1257 165ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard.
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43、en, 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 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 8 Time Studies: AluminumOptical AluminumSpark Atomic Emission Analysis of High-Purity IronE1257 166
