1、Designation: D5839 15Standard Test Method forTrace Element Analysis of Hazardous Waste Fuel byEnergy-Dispersive X-Ray Fluorescence Spectrometry1This standard is issued under the fixed designation D5839; the number immediately following the designation indicates the year oforiginal adoption or, in th
2、e 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 method applies to the determination of traceelement concentrations by energy
3、-dispersive X-ray fluores-cence (EDXRF) spectrometry in typical liquid hazardous wastefuels (LHWF) used by industrial furnaces.1.2 This test method has been used successfully on numer-ous samples of LHWF that are mixtures of solvents, oils,paints, and pigments for the determination of the followinge
4、lements: Ag, As, Ba, Cd, Cr, Hg, Ni, Pb, Sb, Se, and Tl.1.3 This test method also may be applicable to elements notlisted above and to the analysis of trace metals in organicliquids other than those used as LHWF.1.4 This standard does not purport to address all of thesafety concerns, if any, associa
5、ted 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.2. Referenced Documents2.1 ASTM Standards:2C982 Guide for Selecting Components for Energy-Dispersive X-
6、Ray Fluorescence (XRF) Systems (With-drawn 2008)33. Summary of Test Method3.1 A weighed portion of the sample is transferred to aporcelain evaporating dish and placed on a hot plate. Thesample is heated for 15 to 30 min at a temperature notexceeding 105C to evaporate highly volatile components. Thed
7、ish is removed from the hot plate and allowed to cool.Graphite powder is blended with the evaporated sample until ahomogeneous paste is produced and the sample weight isrecorded. The blended sample is inserted in a disposablesample cup and placed in the X-ray spectrometer for analysis.3.2 The K Spec
8、tral X-ray emission lines are used forAg,As,Ba, Cd, Cr, Ni, Sb, and Se.3.3 The L spectral X-ray emission lines are used for Hg, Pb,and Tl.4. Significance and Use4.1 The analysis of trace elements is often a regulatory andprocess specific requirement for facilities utilizing LHWF.With proper instrume
9、nt standardization, set-up, and qualitycontrol, this test method provides the user an accurate, rapid,nondestructive method for trace element determinations.5. Interferences5.1 Spectral Overlaps:5.1.1 Samples containing a mixture of elements often ex-hibit X-ray emission line overlap. Modern Si (Li)
10、 detectorsgenerally provide adequate resolution to minimize the effectsof spectrum overlaps on the analytical results of the LHWF. Inthose cases where direct emission line overlap exists, spectraldeconvolution methods extract corrected analyte emission lineintensities. Table 1 lists the significant
11、line overlaps observedfor the elements analyzed in LHWF. Follow the EDXRFmanufacturers recommendations concerning spectral decon-volution of the emission lines.NOTE 1Not all possible interferences are listed in Table 1. The LHWFsamples to be analyzed may have other emission line interferences notmen
12、tioned. Consult the manufacturers recommendations for optimumdeconvolution methods.5.2 Matrix Interferences:5.2.1 Large concentration variations of metal or matrixcomponents, or both, in LHWF samples can result in non-linear metal X-ray intensity response at increasing metalconcentrations. Untreated
13、 matrix interactions may have adeleterious effect on metal determination accuracy. Matrixinteractions, if exhibited by the LHWF samples, must beaccounted for by method calibration.1This guide is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subco
14、mmittee D34.01.06 onAnalytical Methods.Current edition approved May 1, 2015. Published May 2015. Originallyapproved in 1996. Last previous edition approved in 2006 as D5839 - 96 (2006),which was withdrawn in January 2015 and reinstated in May 2015. DOI:10.1520/D5839-15.2For referenced ASTM standards
15、, 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.3The last approved version of this historical standard is referenced onwww.astm.org.Copyrig
16、ht ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16. Apparatus6.1 Energy Dispersive X-Ray Spectrometer, capable of mea-suring the wavelengths listed in Table 1. Refer to Guide C982for system specifications.6.2 Hot Plate, with temperature contr
17、ol to 105C.6.3 Analytical Balance, capable of weighing to 0.001 g.6.4 Porcelain Evaporating Dishes, 70 to 150 mL capacity.7. Reagents and Materials7.1 Purity of ReagentsUse reagent grade chemicals in alltests. Unless otherwise indicated, all reagents will conform tothe specifications of the Committe
18、e on Analytical Reagents ofthe American Chemical Society where such specifications areavailable.4Other grades may be used, provided it is firstascertained that the reagent is of sufficient high purity to permitits use without lessening the accuracy of the determination.7.2 Use graphite powder, mixin
19、g grade, 44 m, 325 mesh.57.3 Use oil-based Ag, As, Ba, Cd, Cr, Hg, Ni, Pb, Sb and Sestandards, 10 to 10 000 mg/kg depending on the usersanalytical requirements. If the results of this test method are tobe used for compliance purposes, standards or a commercialsource must be traceable to NIST or othe
20、r certifying body.Quality control samples for analyses done for compliancepurposes may need to be prepared with standards from adifferent vendor or lot number.7.4 Use oil or solvent-based Tl standard, 10 to 1000 mg/kgdepending on the users analytical requirements. If the resultsof this test method a
21、re to be used for compliance purposes,standards or a commercial source must be traceable to NIST orother certifying body.67.5 Use paraffinic base oil.7.6 Use sample cups, vented or unvented.7.7 Use thin-film sample support.NOTE 2The user should select a thin-film support that provides formaximum tra
22、nsmittance and is resistant to typical components in LHWF.The thin-film supports used in the development of this test method were4 m Prolene.8. Sampling8.1 Because stratification or layering of liquid samples ispossible, the laboratory sample should be thoroughly mixed byshaking prior to withdrawing
23、 a portion for testing, or use asampling method that assures all portions of the sample arerepresented.9. Preparation of Apparatus9.1 Follow the manufacturers instructions for set-up,conditioning, preparation, and maintenance of the XRF spec-trometer.9.2 Obtain reference spectra from pure element st
24、andardsfor all analytes and interelement correction metals.9.3 Address spectral interferences, as listed in 5.1.1,inaccordance with manufacturers recommendations.10. Calibration and Standardization10.1 Calibrate the spectrometer to an appropriate referenceelement at the minimum frequency specified b
25、y the manufac-turer.10.2 Analytical standards should be gravimetrically pre-pared by blending the elemental standards and graphite listedin Section 7. These preparations can contain single or multipleelements and should be prepared at combinations and ratios tomeet the users individual needs. For ex
26、ample, a Pb and Cdstandard at 125 ppm each could be prepared by gravimetricallycombining 2 g oil-based Pb standard (500 ppm), 2 g oil-basedCd standard (500 ppm) and 4 g graphite and blending to ahomogeneous mixture. For this example, the Pb concentrationis calculated as follows:Pb Standard Concentra
27、tion 5 500 ppm3Pb Std. g!graphite g!1Cd Std. g!1Pb Std. g!(1)10.3 The metals standard/graphite paste is placed in an XRFsample cup and affixed with a thin-film support. The samplecup is inverted and lightly tapped on a level surface until theblended paste makes full contact (no air spaces) with thet
28、hin-film support.10.3.1 The standard blends in the sample cups are placedinto the spectrometers designated sample holder. Avoid touch-ing the thin-film, as this can further reduce transmittance.Initiate data acquisition for the desired elements according tothe manufacturers instructions.10.4 Two alt
29、ernative standards calibration methods may beused:10.4.1 Test Method A (Empirical Calibration Method)Organic-based metals standards containing the metals of inter-est are prepared as described in 10.2. The standard metalconcentrations must bracket the unknown LHWF concentra-tion levels. If the stand
30、ard concentrations are less than 0.1 %by weight, a linear calibration method may be used to plotmetal emission intensity response against metal concentration.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reag
31、ents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.5This reagent, or its equivalent, is available from Chemple
32、x Industries, Inc., 160Marbledale Road, Tuckahoe, NY 10707.6This reagent, or its equivalent, is available from Alfa Aesar, Johnson MattheyInc., 30 Bond Street, Ward Hill, MA 01835.TABLE 1 Common Emission Line Spectral Interferences forLHWF AnalysisElementLinesDeterminedSpectral InterferencesAs K,K P
33、b L,HgL,TlL LCr K,K VK,MnKHg L,L As K,SeK,PbL,TlL,BrKNi K,K Cu K,CuKPb L,L As K,SeK Hg L Tl L,TlL,BrK,BrKSe K,K Pb L,HgL,TlLTl L,L As K,AsK,SeK,PbL,BrK,HgL,HgLD5839 15210.4.1.1 If metal concentration exceeds 0.1 % by weight,then a matrix correction technique is employed. Standardmixtures of varying
34、metal composition must be prepared thatbracket the LWHF unknown concentrations. Eq A is solved forthe slope, intercept and all alpha terms:Ci5 Bi1KiIi11(ijCj! (2)where:Ci= concentration of analyte element i,Bi= intercept term,Ki= slope term,Ii= X-ray intensity of element, i,ij= alpha coefficient des
35、cribing the matrix interaction ofelement j on analyte i, andCj= concentration of matrix element j.10.4.2 Test Method B (Fundamental Parameters Method)Some instrument vendors provide software capable of estimat-ing matrix interferences with a minimum number of standards.A high and low standard concen
36、tration mixture or a mid-rangeconcentration mixture gives the fundamental parametersmethod an initial emission response determination. Using thisinformation and calculations using the principles of X-rayabsorption and emission, a data matrix is created sufficient tosolve equations of the form in Eq
37、2 for all sample matrixinteractions.10.4.2.1 Follow the software manufacturers fundamentalparameters set-up recommendations on the number of standardmixtures and the nature of the matrix balance estimate (usuallya stoichiometric combination of carbon, hydrogen, and oxy-gen) for LWHF.10.4.3 Calibrati
38、on should be repeated at least every twoweeks or whenever quality control results as specified inSection 13 are outside data quality objectives as determined bythe user.11. Procedure11.1 Mix the LHWF sample thoroughly, see 8.1.11.1.1 To a clean, dry, and tared evaporating dish, add 10 gof the LHWF s
39、ample and weigh to the nearest 0.001 g. Recordthe mass.11.1.2 Place the dish on a hot plate at a temperature suchthat the sample material does not exceed 105C. Samplescontaining significant levels of very volatile components mayneed to be heated initially at a lower temperature. If spatteringof the
40、sample is observed, the sample should be removed fromthe hot plate and allowed to cool slightly. Adjust the hot plateto a lower temperature and replace evaporating dish andsample on the hot plate and continue heating. The heating ofthe sample is a concentration step, so the heating time is not acrit
41、ical factor. Generally, the time required to evaporate thevolatile fraction from most LHWF is approximately 15 to 30min.11.1.3 Remove the dish from the hot plate and allow to coolto the touch.11.1.4 If the evaporated sample appears to contain large orvariable sized solid material, it may be necessar
42、y to grind thesample in a mortar and pestle or other suitable device.11.1.5 Mix graphite into the evaporated sample with a labspatula or equivalent device until a homogeneous paste resultsthat has no clumping, and when allowed to stand briefly,exhibits no visible liquid phase separation. An approxim
43、ateamount of 4 to6gofgraphite is normally sufficient. Weigh thegraphite/sample mixture and record.11.1.6 Mount the graphite/sample preparation in an XRFsample cup as described in 10.3.11.1.7 Place the mounted sample preparation into the spec-trometers designated sample holder. Avoid touching the thi
44、n-film, as this can reduce transmittance. Initiate data acquisitionfor the desired elements according to the manufacturersinstructions.11.1.8 After instrument analysis is completed, process ana-lytical results in accordance with Section 12.12. Calculation12.1 The analytical results for each element
45、obtained byeither empirical calibration or fundamental parameters modelsin 11.1.8 should be corrected for the sample preparationdilution as follows:Corrected concentration mg/kg! 5 Analytical Result mg/kg! (3)3Mass of graphite g! and sample mix g!Initial mass of LHWF g!13. Quality Control13.1 Before
46、 using this test method, fully investigate anyspecific regulatory quality control requirements.13.2 Process a minimum of one quality control checkstandard, matrix spike/matrix spike duplicate and one analyti-cal blank consisting of graphite powder/analyte-free paraffinicoil blend with each batch of
47、LHWF samples.13.3 Evaluate quality control sample with each batch ofanalyzed samples. These results will verify that user defineddata quality objectives have been met.14. Precision and Bias14.1 PrecisionNo statement is made about precision atthis time.An interlaboratory test study will be conducted
48、in thefuture.14.2 BiasNo statement is made about bias at this time. Aninterlaboratory test study will be conducted in the future.14.3 Appendix X1 contains analytical results following thistest method (10.4.2) on typical LHWF, MS/MSD, checkstandard, and blank. Lower Limits of Detections also are list
49、ed.15. Keywords15.1 EDXRF; hazardous waste fuel; spectrometry; spectros-copy; trace elements; XRFD5839 153APPENDIX(Nonmandatory Information)X1. ANALYTICAL AND QUALITY CONTROL RESULTS AND LOWER LIMITS OF DETECTION FOR LHWFLHWF Sample No. 1ElementVCrTiNiCuZnSeAsTlPbHgAgCdSbBaSnBlank (ppm) 13.0 3.0 8.0 6.0 8.0 7.0 3.0 16.0 6.0 4.0 3.0 3.0 2.0 8.0 34.0 4.0Check standard recovery (%) 102.1 106.1 110.0 94.5 102.8 102.8 115.0 124.8 . 104.6 110.0 100.3 105.8 108.0 130.0104.8MS/MSD-RPD1(%) 2.1 1.2 8.2 9.9 0.2 1.5
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