ASTM D8064-2016 6931 Standard Test Method for Elemental Analysis of Soil and Solid Waste by Monochromatic Energy Dispersive X-ray Fluorescence Spectrometry Using Multiple Monochrom.pdf
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1、Designation: D8064 16Standard Test Method forElemental Analysis of Soil and Solid Waste byMonochromatic Energy Dispersive X-ray FluorescenceSpectrometry Using Multiple Monochromatic ExcitationBeams1This standard is issued under the fixed designation D8064; the number immediately following the design
2、ation 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 method is based upon e
3、nergy-dispersive X-rayFluorescence (EDXRF) spectrometry using multiple mono-chromatic excitation beams for detection and quantification ofselected heavy metal elements in soil and related solid waste.1.2 This test method is also known as High Definition X-rayFluorescence (HDXRF) or Multiple Monochro
4、matic BeamEDXRF (MMB-EDXRF).1.3 This test method is applicable to various soil matricesfor the determination of Cr, Ni,As, Cd, Hg, and Pb in the rangeof 1 to 5000 mg/kg, as specified in Table 1 and determined bya ruggedness study using representative samples. The limit ofdetection (LOD) for each ele
5、ment is listed in Table 1. The LODis estimated by measuring a SiO2blank sample (see Table X1.1in Appendix X1).1.4 This test method is applicable to other elements: Sb, Cu,Se, Ag, Tl, Zn, Ba, Au, Co, V, Fe, Mn, Mo, K, Rb, Sn, Sr, andTi.1.5 X-ray NomenclatureThis standard names X-ray linesusing the Si
6、egbahn convention.21.6 UnitsThe values stated in SI units are to be regardedas standard. No other units of measurement are included in thisstandard.1.7 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 st
7、andard 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:3D653 Terminology Relating to Soil, Rock, and ContainedFluidsD4944 Test Method for Field Determination of Water (Mois-ture) C
8、ontent of Soil by the Calcium Carbide Gas PressureTesterD5283 Practice for Generation of Environmental Data Re-lated to Waste Management Activities: Quality Assuranceand Quality Control Planning and ImplementationD5681 Terminology for Waste and Waste ManagementD5847 Practice for Writing Quality Cont
9、rol Specificationsfor Standard Test Methods for Water AnalysisE1169 Practice for Conducting Ruggedness TestsE1727 Practice for Field Collection of Soil Samples forSubsequent Lead DeterminationE2554 Practice for Estimating and Monitoring the Uncer-tainty of Test Results of a Test Method Using Control
10、Chart Techniques2.2 Other Documents:ASTM DS46 X-Ray Emission Wavelengths and Kev Tablesfor Nondiffractive Analysis4ASTM MNL 7 Manual on Presentation of Data and ControlChart Analysis, 8thed.4US EPA Method, Method 6200 Field Portable X-Ray Fluo-rescence Spectrometry for the Determination of Elemental
11、Concentrations in Soil and Sediment51This test method is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34.01.06 onAnalytical Methods.Current edition approved Nov. 1, 2016. Published November 2016. DOI:10.1520/D8064-16.2Jenkins, R.,
12、Manne, R., Robin, R., and Senemaud, C., “Nomenclature Systemfor X-ray Spectroscopy,” Pure method precision is achieved with a monochromatic beamhaving an energy bandwidth (Full Width Half Maximum) lessthan 15 % relative to the selected energy and containing morethan 95 % flux of the spectrum of the
13、excitation beam which isincident on the sample.3.2.5 multiple monochromatic excitation beams, ntwo ormore monochromatic beams.3.2.6 Rayleigh scattering, nthe elastic scattering of anX-ray photon through its interaction with the bound electronsof an atom; this process is also referred to as coherents
14、cattering.3.3 Acronyms:3.3.1 ARVaccepted reference values3.3.2 EDXRFenergy dispersive X-ray fluorescence3.3.3 FPfundamental parameters3.3.4 HDXRFhigh definition X-ray fluorescence3.3.5 LODlimits of detection3.3.6 MMBmultiple monochromatic beams3.3.7 NDnon-detected3.3.8 RSDrelative standard deviation
15、4. Summary of Test Method4.1 The operating conditions presented in this test methodhave been successfully used in the determination of Cd,As, Cr,Pb, Hg, Sb, Cu, Ni, Se, Ag, Tl, Zn, Ba, Sn, and Au in soil andrelated solid waste.4.2 This technique uses one or more monochromatic exci-tation beams to qu
16、antify elemental concentrations in soil andsolid waste samples. The sample is homogenized to a reason-able degree and positioned in front of an aperture where it isexposed to one or more monochromatic X-ray beams that arefocused by X-ray optics from an X-ray source. A nearbydetector is positioned to
17、 collect fluorescent and backscatteredX rays. The X rays collected by the detector are converted toelectric pulses by a digital pulse processor. A multi-channelanalyzer separates the pulses by X-ray energy, forming themeasurement spectrum. The spectrum is processed by an FPmethod to obtain the analy
18、sis result.4.3 The apparatus is calibrated for each monochromaticbeam and the detector. The calibration may be performed bythe manufacturer or by the user.5. Significance and Use5.1 Elemental species such as Cr, Ni,As, Cd, Hg, and Pb arewidely used in many industrial processes. These elements havebe
19、en identified in many former industrial sites driving the needfor a quick, easy method for testing on-site at trace levels insoil and solid waste matrices.5.2 This method may be used for quantitative determina-tions of Cr, Ni, As, Cd, Hg, and Pb in soil matrices and solidwaste. Typical test time is
20、90 seconds to 15 minutes.6. Interferences6.1 Spectral InterferenceSpectral interferences resultfrom spectral overlaps among the X-ray lines that remainunresolved due to limited energy resolution of the detector. Forinstance, the arsenic (As) K peak directly overlaps the lead(Pb) L peak. The Pb L lin
21、e can be used to account for thisoverlap and theAs K lines can then be resolved from the Pb Loverlap. The actual lines used for any particular element shouldbe such that overlaps are minimized. Reference ASTM DataSeries DS46 for detailed information on potential line overlaps.Interactions of photons
22、 and electrons inside the detector resultin additional peaks in the spectrum known as escape peaks andsum peaks. These peaks can overlap with X-ray lines ofinterest, for example, the sum peak of iron (Fe) K can overlapwith the Pb L peak.6.2 Matrix EffectsMatrix effects, also called interelementeffec
23、ts, exist among all elements as the result of absorption offluorescent X rays (secondary X rays) by atoms in thespecimen. Absorption reduces the apparent sensitivity for theelement. In contrast, the atom that absorbs the X rays may inturn emit a fluorescent X ray, increasing apparent sensitivityfor
24、the second element. Mathematical methods may be used tocompensate for matrix effects. A number of mathematicalcorrection procedures are commonly utilized including full FPtreatments and mathematical models based on influence coef-ficient algorithms.6.3 Physical Matrix EffectsPhysical characteristics
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