ASTM_D_4657_-_92_1998.pdf

Designation:D 4657 92(Reapproved 1998)An American National StandardStandard Test Method forPolynuclear Aromatic Hydrocarbons in Water1This standard is issued under the fixed designation D 4657;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(e)indicates an editorial change since the last revision or reapproval.1.Scope1.1 This test method covers the determination of certainpolynuclear aromatic hydrocarbons(PAHs)in water andwastewater.The following compounds may be determined bythis test method:acenaphthene,acenaphthylene,anthracene,benzo(a)anthracene,benzo(a)pyrene,benzo(b)fluoranthene,benzo(ghi)perylene,benzo(k)fluoranthene,chrysene,diben-zo(ah)anthracene,fluoranthene,fluorene,indeno(1,2,3-cd)pyrene,naphthalene,phenathrene,and pyrene.AdditionalPAHs may also be determined;however,the analyst shoulddemonstrate that the test method is in fact applicable to thespecific PAH(s)of interest before applying it to sampleanalysis.This test method has high sensitivity for the com-pounds of interest.It is limited to use by analysts familiar withhigh-performance liquid chromatography(HPLC)or workingunder close supervision of such persons.1.2 This test method is applicable to the determination ofthe compounds in 1.1 in water and wastewater.This testmethod has been successfully used with distilled water,tapwater,surface water,and the following wastewaters:effluentfrom an oil refinery,blast furnace,and combined coke ovenand blast furnace.It is the users responsibility to ensure thevalidity of this test method for waters of untested matrices.Itpresupposes a high expectation of finding the specific com-pounds of interest.If the user is attempting to screen samplesfor any or all of the compounds above,component identitiesshould be verified by using two different types of reverse phaseHPLC columns,both ultraviolet and fluorescence detection,orgas chromatography/mass spectrometry-spectroscopy screen-ing procedures,or both.1.3 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.Specific hazardsstatements are given in Section 9.2.Referenced Documents2.1 ASTM Standards:D 1129 Terminology Relating to Water2D 1192 Specification for Equipment for Sampling Waterand Steam in Closed Conduits2D 1193 Specification for Reagent Water2D 1253 Test Method for Residual Chlorine in Water2D 3370 Practices for Sampling Water from Closed Con-duits2D 3856 Guide for Good Laboratory Practices in Laborato-ries Engaged in Sampling and Analysis of Water2D 4210 Practice for Intralaboratory Quality Control Proce-dures and a Discussion on Reporting Low-Level Data23.Terminology3.1 DefinitionsFor definitions of terms used in this testmethod,refer to Terminology D 1129.4.Summary of Test Method4.1 This test method consists of the extraction of 1 L ofwater with methylene chloride.This extract is then reduced involume using Kuderna-Danish(K-D)evaporation followed bycolumn chromatography on silica gel.The appropriate fractionfrom the silica gel chromatography containing the PAHs isagain reduced in volume using K-D evaporation and is solventexchanged with acetonitrile to an exact volume of 1 mL.Thisconcentrated extract is then analyzed for PAH using high-performance liquid chromatography(HPLC).4.2 The HPLC analysis utilizes reverse phase chromatogra-phy using a combination of isocratic and gradient elution.Acetonitrile and water are used as the mobile phase on a PerkinElmer PAH/10 reverse phase column.3Other C-18 reversephase columns may be used,provided that they yield adequateresolution of the PAHs of interest.Fluorescence or ultravioletdetection depending on the needs is used to monitor the PAHof interest;quantitation is by peak area integration or peakheight measurement.Results are reported in micrograms perlitre.1This test method is under the jurisdiction of ASTM Committee D-19 on Waterand is the direct responsibility of Subcommittee D19.06 on Methods forAnalysis forOrganic Substances in Water.Current edition approved Oct.15,1992.Published January 1993.Originallypublished as D 4657 87.Last previous edition D 4657 91.2Annual Book of ASTM Standards,Vol 11.01.3Perkin-Elmer PAH/10 reverse phase column is available from Perkin-ElmerCorporation,761 Main Ave.,Norwalk,CT 06859.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.4.3 If interferences are encountered,this test method pro-vides a selected general purpose cleanup procedure to aid theanalyst in their elimination.5.Significance and Use5.1 Prominent among the group of compounds found invarious water supplies and considered to be potential healthrisks are the p