ASTM_D_7363_-_13a.pdf

Designation:D736313aStandard Test Method forDetermination of Parent and Alkyl Polycyclic Aromatics inSediment Pore Water Using Solid-Phase Microextractionand Gas Chromatography/Mass Spectrometry in SelectedIon Monitoring Mode1,2This standard is issued under the fixed designation D7363;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.NoteBalloted information was included and the year date changed on May 17,2013.1.Scope1.1 The U.S.Environmental Protection Agency(USEPA)narcosis model for benthic organisms in sediments contami-nated with polycyclic aromatic hydrocarbons(PAHs)is basedon the concentrations of dissolved PAHs in the interstitialwater or“pore water”in sediment.This test method covers theseparation of pore water from PAH-impacted sedimentsamples,the removal of colloids,and the subsequent measure-ment of dissolved concentrations of the required 10 parentPAHs and 14 groups of alkylated daughter PAHs in the porewater samples.The“24 PAHs”are determined using solid-phasemicroextraction(SPME)followedbyGasChromatography/Mass Spectrometry(GC/MS)analysis in se-lected ion monitoring(SIM)mode.Isotopically labeled ana-logs of the target compounds are introduced prior to theextraction,and are used as quantification references.1.2 Lower molecular weight PAHs are more water solublethan higher molecular weight PAHs.Therefore,USEPA-regulated PAH concentrations in pore water samples varywidely due to differing saturation water solubilities that rangefrom 0.2 g/L for indeno1,2,3-cdpyrene to 31 000 g/L fornaphthalene.This method can accommodate the measurementof microgram per litre concentrations for low molecular weightPAHs and nanogram per litre concentrations for high molecularweight PAHs.1.3 The USEPA narcosis model predicts toxicity to benthicorganisms if the sum of the toxic units(TUc)calculated for all“34 PAHs”measured in a pore water sample is greater than orequal to 1.For this reason,the performance limit required forthe individual PAH measurements was defined as the concen-tration of an individual PAH that would yield134of a toxic unit(TU).However,the focus of this method is the 10 parent PAHsand 14 groups of alkylated PAHs(Table 1)that contribute 95%of the toxic units based on the analysis of 120 background andimpacted sediment pore water samples.3The primary reasonsfor eliminating the rest of the 5-6 ring parent PAHs are:(1)these PAHs contribute insignificantly to the pore water TU,and(2)these PAHs exhibit extremely low saturation solubilitiesthat will make the detection of these compounds difficult inpore water.This method can achieve the required detectionlimits,which range from approximately 0.01 g/L,for highmolecular weight PAHs,to approximately 3 g/L for lowmolecular weight PAHs.1.4 The test method may also be applied to the determina-tion of additional PAH compounds(for example,5-and 6-ringPAHs as described in Hawthorne et al.).4However,it is theresponsibility of the user of this standard to establish thevalidity of the test method for the determination of PAHs otherthan those referenced in 1.1 and Table 1.1.5 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.6 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is the1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.06 on Methods forAnalysis forOrganic Substances in Water.Current edition approved May 17,2013.Published November 2013.Originallyapproved in 2007.Last previous edition approved in 2013 as D7363 13.DOI:10.1520/D7363-13A.2Standard methods under the jurisdiction of ASTM Committee D19 may bepublished for a limited time preliminary to the completion of full collaborative studyvalidation.Such standards are deemed to have met all other D19 qualifyingrequirements but have not completed the required validation studies to fullycharacterize the performance of the test method across multiple laboratories andmatrices.Preliminary publication is done to make current technology accessible tousers of standards,and to solicit additional input from the user community.3Hawthorne,S.B.,Grabanski,C.B.,and Miller,D.J.,“Measured PartitioningCoefficients for Parent and Algae Polycyclic Aromatic Hydrocarbons in 114Historically Contaminated Sediments:Part I,Koc Values,”Environmental Toxicol-ogy and Chemistry,Vol 25,2006,pp.29012911.4Hawthorne,S.B.,Grabanski,C.B.,Miller,D.J.,and Kreitinger,J.P.,“SolidPhase Microextraction Measurement of Parent and Akyl Polycyclic AromaticHydrocarbons in Milliliter Sediment Pore Water Samples and Determination ofKDOCValues,”Environmental Science Technology,Vol 39,2005,pp.27952803.Copyright ASTM Internat