ASTM_D_6052_-_97_2008.pdf

Designation:D605297(Reapproved 2008)Standard Test Method forPreparation and Elemental Analysis of Liquid HazardousWaste by Energy-Dispersive X-Ray Fluorescence1This standard is issued under the fixed designation D6052;the number immediately following the designation 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 covers the determination of trace andmajor element concentrations by energy-dispersive X-ray fluo-rescence spectrometry(EDXRF)in liquid hazardous waste(LHW).1.2 This test method has been used successfully on numer-ous samples of aqueous and organic-based LHW for thedetermination of the following elements:Ag,As,Ba,Br,Cd,Cl,Cr,Cu,Fe,Hg,I,K,Ni,P,Pb,S,Sb,Se,Sn,Tl,V,and Zn.1.3 This test method is applicable for other elements(Si-U)not listed in 1.2.1.4 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 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-Ray Fluorescence(XRF)Systems(With-drawn 2008)3D1193 Specification for Reagent Water2.2 Other ASTM Documents:ASTM Data Series DS 46 X-ray Emission Wavelengths andKeV Tables for Nondiffractive Analysis43.Summary of Test Method3.1 A weighed portion of activated alumina and sample arecombined in a mixing vessel and shaken until well mixed.Thesample mixture is transferred into a disposable sample cup andplaced in the spectrometer for analysis.3.2 The K spectral emission lines are used for elementsSi-Ba.3.3 The L spectral emission lines are used for elements withatomic numbers greater than Ba.4.Significance and Use4.1 The elemental analysis of liquid hazardous waste isoften important for regulatory and process specific require-ments.This test method provides the user an accurate,rapidmethod for trace and major element determinations.5.Interferences5.1 Spectral Overlaps(Deconvolution):5.1.1 Samples containing a mixture of elements often ex-hibit X-ray emission line overlap.Modern Si(Li)detectorsgenerally provide adequate resolution to minimize the effectsof spectral overlap.In cases where emission line overlap exists,techniques of peak fitting exist for extracting corrected analyteemission line intensities.For example,the PbL“line overlapswith the AsK.”The PbL line can be used to avoid thisoverlap and the AsK lines can then be resolved from the PbLoverlap.The actual lines used for any particular element shouldbe such that overlaps are minimized.Follow the EDXRFmanufacturers recommendation concerning spectral deconvo-lution.Reference should be made to ASTM Data Series DS 46for detailed information on potential line overlaps.5.2 Matrix Interferences(Regression):5.2.1 Matrix interference in the measurement of“as re-ceived”LHW samples using EDXRF has been the principlelimitation in the development and expanding use of thisinstrumental technique.Using well understood XRF principlesfor controlling matrix effects,for example,dilution and matrixmodification using lithium borate fusion and addition of heavyabsorbers,a matrix can be stabilized.Using calcined aluminaand the above principles matrices are stabilized for quantitativeEDXRF analysis.5.2.2 The response range of this test method should belinear with respect to the elements of interest and theirregulatory or process control,or both,action thresholds.Large1This 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 Feb.1,2008.Published March 2008.Originallyapproved in 1997.Last previous edition approved in 2003 as D6052 97(2003).DOI:10.1520/D6052-97R08.2For 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 to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from ASTM Headquarters,Customer Service.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 concentration variations of element or matrix,or both,compo-nents in LHW samples can result in non-linear X-ray intensityresponse at increasing element concentrations.6.Apparatus6.1 Energy-dispersive X-ray Fluorescence Spectrometer,ca-pable of measuring the wavelengths of the elements listed in1.2.Refer to Guide C982 for system specifications.6.2 Analytical Balance,capable of weighing to 0.001 g.7.Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall beused i