METHOD 8270C SEMIVOLATILE ORGANIC COMPOUNDS BY …

1 CD-ROM8270C - 1 Revision 3 December 1996 METHOD 8270 CSEMIVOLATILE ORGANIC COMPOUNDSBY GAS CHROMATOGRAPHY/MASS SPECTROMETRY (GC/MS) AND 8270 is used to determine the concentration of SEMIVOLATILE ORGANIC compoundsin extracts prepared from many types of solid waste matrices, soils, air sampling media and watersamples. Direct injection of a sample may be used in limited applications. The following compoundscan be determined by this METHOD :Appropriate Preparation Techniquesb 3540/CompoundsCAS No35103520354135503580aAcenaphthene83-32 -9 XXXXXA cenaphthene-d (IS)XXXXX10 Acenaphthylene208-96-8 XXXXXA cetophenone 98-86-2 XNDNDNDX2-Acetylaminofluorene 53-96-3 XNDNDNDX1-Acetyl-2-thiourea 591-08-2 LRNDNDNDLRA ldrin 309-00-2 XXXXX2-Aminoanthraquinone 117-79-3 XNDNDNDXA minoazobenzene 60-09-3 XNDNDNDX4-Aminobiphenyl 92-67-1 XNDNDNDX3-Amino-9-ethylcarbazole 132-32-1 XXNDNDNDA nilazine 101-05-3 XNDNDNDXA niline 62-53-3 XXNDXXo-Anisidine 90-04-0 XNDNDNDX Anthracene 120-12-7 XXXXXA ramite 140-57-8HS(43)NDNDNDXA roclor 101612674-11-2 XXXXXA roclor 122111104-28-2 XXXXXA roclor 123211141-16-5 XXXXXA roclor 124253469-21-9 XXXXXA roclor 124812672-29-6 XXXXXA roclor 125411097-69-1 XXXXXA roclor 126011096-82-5 XXXXXA zinphos-methyl 86-50-0HS(62)

2 NDNDNDXB arban 101-27-9 LRNDNDNDLRB enzidine 92-87-5 CPCPCPCPCPB enzoic acid 65-85-0 XXNDXXBenz(a)anthracene 56-55-3 XXXXXB enzo(b)fluoranthene 205-99-2 XXXXXB enzo(k)fluoranthene 207-08-9 XXXXXB enzo(g,h,i)perylene 191-24-2 XXXXXB enzo(a)pyrene 50-32-8 XXXXXCD-ROM8270C - 2 Revision 3 December 1996 Appropriate Preparation Techniquesb 3540/CompoundsCAS No35103520354135503580ap-Benzoquinone106 -51-4 OENDNDNDXB enzyl alcohol100-51-6 XXNDXX"-BHC319-84-6 XXXXX$-BHC319-85-7 XXXXX*-BHC319-86-8 XXXXX(-BHC (Lindane)58-89-9 XXXXXBis(2-chloroethoxy)methane111-91-1 XXXXXBis(2-chloroethyl) ether111-44-4 XXXXXBis(2-chloroisopropyl) ether108-60-1 XXXXXBis(2-ethylhexyl) phthalate117-81-7 XXXXX4-Bromophenyl phenyl ether101-55-3 XXXXXB romoxynil1689-84-5 XNDNDNDXB utyl benzyl phthalate85-68-7 XXXXXC aptafol2425-06-1HS(55)NDNDNDXC aptan133-06-2HS(40)NDNDNDXC arbaryl63-25-2 XNDNDNDXC arbofuran1563-66-2 XNDNDNDXC arbophenothion786-19-6 XNDNDNDXC hlordane (NOS)57-74-9 XXXXXC hlorfenvinphos470-90-6 XNDNDNDX4-Chloroaniline106-47-8 XNDNDNDXC hlorobenzilate510-15-6 XNDNDNDX5-Chloro-2-methylaniline95-79-4 XNDNDNDX4-Chloro-3-methylphenol59-50-7 XXXXX3-(Chloromethyl)pyridine hydrochloride6959-48-4 XNDNDNDX1-Chloronaphthalene90-13-1 XXXXX2-Chloronaphthalene91-58-7 XXXXX2-Chlorophenol95-57-8 XXXXX4-Chloro-1,2-phenylenediamine95-83- 0 XXNDNDND4-Chloro-1,3-phenylenediamine513 1-60-2 XXNDNDND4-Chlorophenyl phenyl ether7005-72-3 XXXXXC hrysene218-01-9 XXXXXC hrysene-d (IS)XXXXX12 Coumaphos56-72-4 XNDNDNDXp-Cresidine120-71-8 XNDNDNDXC rotoxyphos7700-17-6 XNDNDNDX2-Cyclohexyl-4,6-dinitro-phenol1 31-89-5 XNDNDNDLR4,4'-DDD72-54-8 XXXXX4,4'-DDE72-55-9 XXXXX4,4'-DDT50-29-3 XXXXXD emeton-O298-03-3HS(68)NDNDNDXD emeton-S126-75-0 XNDNDNDXD iallate (cis or trans))

3 2303-16-4 XNDNDNDXCD-ROM8270C - 3 Revision 3 December 1996 Appropriate Preparation Techniquesb 3540/CompoundsCAS No35103520354135503580a2,4-Diaminotoluen e95-80-7DC,0E(42)NDNDNDXD ibenz(a,j)acridine224-42-0 XNDNDNDXD ibenz(a,h)anthracene53-70-3 XXXXXD ibenzofuran132-64-9 XXNDXXD ibenzo(a,e)pyrene192-65-4 NDNDNDNDX1,2-Dibromo-3-chloropropane96-1 2-8 XXNDNDNDDi-n-butyl phthalate84-74-2 XXXXXD ichlone117-80-6 OENDNDNDX1,2-Dichlorobenzene95-50-1 XXXXX1,3-Dichlorobenzene541-73-1 XXXXX1,4-Dichlorobenzene106-46-7 XXXXX1,4-Dichlorobenzene-d (IS)XXXXX43,3'-Dichlorobenzidine91-94-1 XXXXX2,4-Dichlorophenol120-83-2 XXXXX2,6-Dichlorophenol87-65-0 XNDNDNDXD ichlorovos62-73-7 XNDNDNDXD icrotophos141-66-2 XNDNDNDXD ieldrin60-57-1 XXXXXD iethyl phthalate84-66-2 XXXXXD iethylstilbestrol56-53-1AW,0S(67)NDNDNDX D iethyl sulfate64-67-5 LRNDNDNDLRD ihydrosaffrole56312-13-1 NDNDNDNDNDD imethoate60-51-5HE,HS(31)NDNDNDX3,3'-Dim ethoxybenzidine119-90-4 XNDNDNDLRD imethylaminoazobenzene60-11-7 XNDNDNDX7,12-Dimethylbenz(a)- anthracene57-97-6CP(45)NDNDNDCP3,3'-Dime thylbenzidine119-93-7 XNDNDNDX","-Dimethylphenethylamine122-09 -8 NDNDNDNDX2,4-Dimethylphenol105-67-9 XXXXXD imethyl phthalate131-11-3 XXXXX1,2-Dinitrobenzene528-29-0 XNDNDNDX1,3-Dinitrobenzene99-65-0 XNDNDNDX1,4-Dinitrobenzene100-25-4HE(14) NDNDNDX4,6-Dinitro-2-methylphenol534-52- 1 XXXXX2,4-Dinitrophenol51-28-5 XXXXX2,4-Dinitrotoluene121-14-2 XXXXX2,6-Dinitrotoluene606-20-2 XXXXXD inocap39300-45-3CP,HS(28)

4 NDNDNDCPD inoseb88-85-7 XNDNDNDXD ioxathion78-34-2 NDNDNDNDNDD iphenylamine122-39-4 XXXXX5,5-Diphenylhydantoin57-41-0 XNDNDNDX1,2-Diphenylhydrazine122-66-7 XXXXXCD-ROM8270C - 4 Revision 3 December 1996 Appropriate Preparation Techniquesb 3540/CompoundsCAS No35103520354135503580aDi-n-octyl phthalate117-84-0 XXXXXD isulfoton298-04-4 XNDNDNDXE ndosulfan I 959-98-8 XXXXXE ndosulfan II33213-65-9 XXXXXE ndosulfan sulfate1031-07-8 XXXXXE ndrin72-20-8 XXXXXE ndrin aldehyde7421-93-4 XXXXXE ndrin ketone53494-70-5 XXNDXXEPN2104-64-5 XNDNDNDXE thion563-12-2 XNDNDNDXE thyl carbamate51-79-6DC(28)NDNDNDXE thyl methanesulfonate62-50-0 XNDNDNDXF amphur52-85-7 XNDNDNDXF ensulfothion115-90-2 XNDNDNDXF enthion55-38-9 XNDNDNDXF luchloralin33245-39-5 XNDNDNDXF luoranthene206-44-0 XXXXXF luorene86-73-7 XXXXX2-Fluorobiphenyl (surr)321-60-8 XXXXX2-Fluorophenol (surr)367-12-4 XXXXXH eptachlor76-44-8 XXXXXH eptachlor epoxide1024-57-3 XXXXXH exachlorobenzene118-74-1 XXXXXH exachlorobutadiene87-68-3 XXXXXH exachlorocyclopentadiene77-47-4 XXXXXH exachloroethane67-72-1 XXXXXH exachlorophene70-30-4AW,CP(62)NDNDNDCPH exachloropropene1888-71-7 XNDNDNDXH examethylphosphoramide680-31-9 XNDNDNDXH ydroquinone123-31-9 NDNDNDNDXI ndeno(1,2,3-cd)pyrene193-39-5 XXXXXI sodrin465-73-6 XNDNDNDXI sophorone78-59-1 XXXXXI sosafrole120-58-1DC(46)NDNDNDXK epone143-50-0 XNDNDNDXL eptophos21609-90-5 XNDNDNDXM alathion121-75-5HS(5)NDNDNDXM aleic anhydride108-31-6 HENDNDNDXM estranol72-33-3 XNDNDNDXM ethapyrilene91-80-5 XNDNDNDXM ethoxychlor72-43-5 XNDNDNDX3-Methylcholanthrene56-49-5 XNDNDNDX4,4'-Methylenebis (2-chloroaniline)101-14-4OE,OS(0)

5 NDNDNDLRCD-ROM8270C - 5 Revision 3 December 1996 Appropriate Preparation Techniquesb 3540/CompoundsCAS No35103520354135503580a4,4'-Methylenebis (N,N-dimethylaniline)101-61-1 XXNDNDNDM ethyl methanesulfonate66-27-3 XNDNDNDX2-Methylnaphthalene91-57-6 XXNDXXM ethyl parathion298-00-0 XNDNDNDX2-Methylphenol95-48-7 XNDNDNDX3-Methylphenol108-39-4 XNDNDNDX4-Methylphenol106-44-5 XNDNDNDXM evinphos7786-34-7 XNDNDNDXM exacarbate315-18-4HE,HS(68)NDNDNDXM irex2385-85-5 XNDNDNDXM onocrotophos6923-22-4 HENDNDNDXN aled300-76-5 XNDNDNDXN aphthalene91-20-3 XXXXXN aphthalene-d (IS)XXXXX81,4-Naphthoquinone130-15-4 XNDNDNDX1-Naphthylamine134-32-7OS(44)NDN DNDX2-Naphthylamine91-59-8 XNDNDNDXN icotine54-11-5DE(67)NDNDNDX5-Nitroacenap hthene602-87-9 XNDNDNDX2-Nitroaniline88-74-4 XXNDXX3-Nitroaniline99-09-2 XXNDXX4-Nitroaniline100-01-6 XXNDXX5-Nitro-o-anisidine99-59-2 XNDNDNDXN itrobenzene98-95-3 XXXXXN itrobenzene-d (surr)XXXXX54-Nitrobiphenyl92-93-3 XNDNDNDXN itrofen1836-75-5 XNDNDNDX2-Nitrophenol88-75-5 XXXXX4-Nitrophenol100-02-7 XXXXX5-Nitro-o-toluidine99-55-8 XXNDNDXN itroquinoline-1-oxide56-57-5 XNDNDNDXN-Nitrosodi-n-butylamine924-16-3 XNDNDNDXN-Nitrosodiethylamine55-18-5 XNDNDNDXN-Nitrosodimethylamine62-75-9 XXXXXN-Nitrosomethylethylamine10595-95-6 XNDNDNDXN-Nitrosodiphenylamine86-30-6 XXXXXN-Nitrosodi-n-propylamine621-64-7 XXXXXN-Nitrosomorpholine59-89-2 NDNDNDNDXN-Nitrosopiperidine100-75-4 XNDNDNDXN-Nitrosopyrrolidine930-55-2 XNDNDNDXO ctamethyl pyrophosphoramide152-16-9 LRNDNDNDLR4,4'-Oxydianiline101-80-4 XNDNDNDXCD-ROM8270C - 6 Revision 3 December 1996 Appropriate Preparation Techniquesb 3540/CompoundsCAS No35103520354135503580aParathion56-38-2 XXNDNDXP entachlorobenzene608-93-5 XNDNDNDXP entachloronitrobenzene82-68-8 XNDNDNDXP entachlorophenol87-86-5 XXXXXP erylene-d (IS)

6 XXXXX12 Phenacetin62-44-2 XNDNDNDXP henanthrene85-01-8 XXXXXP henanthrene-d (IS)XXXXX10 Phenobarbital50-06-6 XNDNDNDXP henol108-95-2DC(28)XXXXP henol-d (surr)DC(28)XXXX61,4-Phenylenediamine106 -50-3 XNDNDNDXP horate298-02-2 XNDNDNDXP hosalone2310-17-0HS(65)NDNDNDXP hosmet732-11-6HS(15)NDNDNDXP hosphamidon13171-21-6HE(63)NDNDNDXP hthalic anhydride85-44-9CP,HE(1)NDNDNDCP2-Picoli ne (2-Methylpyridine)109-06-8 XXNDNDNDP iperonyl sulfoxide120-62-7 XNDNDNDXP ronamide23950-58-5 XNDNDNDXP ropylthiouracil51-52-5 LRNDNDNDLRP yrene129-00-0 XXXXXP yridine110-86-1 NDNDNDNDNDR esorcinol108-46-3DC,OE(10)NDNDNDXS afrole94-59-7 XNDNDNDXS trychnine57-24-9AW,0S(55)NDNDNDXS ulfallate95-06-7 XNDNDNDXT erbufos13071-79-9 XNDNDNDXT erphenyl-d(surr)1718-51-0 XXNDXX141,2,4,5-Tetrachlorobenzene95-94- 3 XNDNDNDX2,3,4,6-Tetrachlorophenol58-90-2 XNDNDNDXT etrachlorvinphos961-11-5 XNDNDNDXT etraethyl dithiopyrophosphate3689-24-5 XXNDNDNDT etraethyl pyrophosphate107-49-3 XNDNDNDXT hionazine297-97-2 XNDNDNDXT hiophenol (Benzenethiol)108-98-5 XNDNDNDXT oluene diisocyanate584-84-9HE(6)NDNDNDXo-Toluid ine95-53-4 XNDNDNDXT oxaphene8001-35-2 XXXXX2,4,6-Tribromophenol (surr)118-79-6 XXXXX1,2,4-Trichlorobenzene120-82-1 XXXXX2,4,5-Trichlorophenol95-95-4 XXNDXX2,4,6-Trichlorophenol88-06-2 XXXXXT rifluralin1582-09-8 XNDNDNDXCD-ROM8270C - 7 Revision 3 December 1996 Appropriate Preparation Techniquesb 3540/CompoundsCAS No35103520354135503580a2,4,5-Trimethylan iline137-17-7 XNDNDNDXT rimethyl phosphate512-56-1HE(60)NDNDNDX1,3,5-Trin itrobenzene99-35-4 XNDNDNDXTris(2,3-dibromopropyl)

7 Phosphate126-72-7 XNDNDNDLRTri-p-tolyl phosphate78-32-0 XNDNDNDXO,O,O-Triethyl phosphorothioate126-68-1 XNDNDNDX Chemical Abstract Service Registry Numbera See Sec. for other acceptable preparation TO ANALYTE LISTIS=This compound may be used as an internal compound may be used as a to walls of glassware during extraction and chromatographic distribution coefficient (number in parenthesis is percent recovery).HE=Hydrolysis during extraction accelerated by acidic or basic conditions (number inparenthesis is percent recovery).HS=Hydrolysis during storage (number in parenthesis is percent stability).LR=Low during extraction accelerated by basic conditions (number in parenthesis ispercent recovery).OS=Oxidation during storage (number in parenthesis is percent stability).X=Greater than 70 percent recovery by this addition to the sample preparation methods listed in the above analyte list, Method3542 describes sample preparation for SEMIVOLATILE ORGANIC COMPOUNDS in air sampled by Method0010 (Table 11 contains surrogate performance data), METHOD 3545 describes an automated solventextraction device for semivolatiles in solids (Table 12 contains performance data), and METHOD 3561describes a supercritical fluid extraction of solids for PAHs (see Tables 13, 14, and 15 forperformance data).

8 8270 can be used to quantitate most neutral, acidic, and basic organiccompounds that are soluble in methylene chloride and capable of being eluted, withoutderivatization, as sharp peaks from a gas chromatographic fused-silica capillary column coated witha slightly polar silicone. Such COMPOUNDS include polynuclear aromatic hydrocarbons, chlorinatedhydrocarbons and pesticides, phthalate esters, organophosphate esters, nitrosamines, haloethers,aldehydes, ethers, ketones, anilines, pyridines, quinolines, aromatic nitro COMPOUNDS , and phenols,including nitrophenols. See Table 1 for a list of COMPOUNDS and their characteristic ions that havebeen - 8 Revision 3 December 1996In most cases, METHOD 8270 is not appropriate for the quantitation of multicomponent analytes, , Aroclors, Toxaphene, Chlordane, etc., because of limited sensitivity for those analytes. Whenthese analytes have been identified by another technique, METHOD 8270 is appropriate forconfirmation of the presence of these analytes when concentration in the extract permits.

9 Refer toSec. of Methods 8081 and 8082 for guidance on calibration and quantitation of multicomponentanalytes such as the Aroclors, Toxaphene, and following COMPOUNDS may require special treatment when being determined by thismethod: may be subject to oxidative losses during solvent concentration andits chromatographic behavior is poor. the alkaline conditions of the extraction step from aqueous matrices,"-BHC, (-BHC, Endosulfan I and II, and Endrin are subject to decomposition. Neutralextraction should be performed if these COMPOUNDS are is subject to thermal decomposition in the inlet of thegas chromatograph, chemical reaction in acetone solution, and photochemical is difficult to separate from the solvent under thechromatographic conditions described. decomposes in the gas chromatographic inlet and cannotbe separated from diphenylamine. , 2,4-dinitrophenol, 4-nitrophenol, benzoic acid,4,6-dinitro-2-methylphenol, 4-chloro-3-methylphenol, 2-nitroaniline, 3-nitroaniline,4-chloroaniline, and benzyl alcohol are subject to erratic chromatographic behavior, especiallyif the GC system is contaminated with high boiling material.)

10 May perform poorly at the GC injection port temperatures listed in themethod. Lowering the injection port temperature may reduce the amount of degradation. Theanalyst needs to use caution if modifying the injection port temperature as the performance ofother analytes may be adversely diisocyanate rapidly hydrolyses in water (half-life of less then 30 min.).Therefore, recoveries of this compound from aqueous matrices should not be expected. Inaddition, in solid matrices, toluene diisocyanate often reacts with alcohols and amines toproduce urethane and ureas and consequently cannot usually coexist in a solution containingthese additio