METHOD 8270D

SEMIVOLATILE ORGANIC COMPOUNDS BY GAS CHROMATOGRAPHY/MASS SPECTROMETRY (GC/MS)

1.0 SCOPE AND APPLICATION

1.1 Method 8270 is used to determine the concentration of semivolatile organic compounds inextracts prepared from manytypes of solid waste matrices, soils, airsampling media and water samples. Direct injection of asample may be used in limited applications. The following compounds can be determined by this method:

Appropriate Preparation Techniques"
3540/ Compounds CAS Noa 3510 3520 3541 3550 3580 Acenaphthene 83-32-9 X X X X X Acenaphthylene 208-96-8 X X X X X Acetophenone 98-86-2 X ND ND ND X 2-Acetylaminofluorene 53-96-3 X ND ND ND X 1-Acetyl-2-thiourea 591-08-2 LR ND ND ND LR Aldrin 309-00-2 X X X X X 2-Aminoanthraquinone 117-79-3 X ND ND ND X Aminoazobenzene 60-09-3 X ND ND ND X 4-Aminobiphenyl 92-67-1 X ND ND ND X 3-Amino-9-ethylcarbazole 132-32-1 X X ND ND ND Anilazine 101-05-3 

### X ND ND ND X Aniline 62-53-3 X 

### X ND 

### X X o-Anisidine 90-04-0 

### X ND ND ND 

### X Anthracene 120-12':'7 X 

### X X X X Aramite 140-57-8 HS(43) NO NO NO X Aroclor 1016 12674-11-2 

### X X X X X Aroclor 1221 11104-28-2 X 

### X X 

### X X Aroclor 1232 11141-16-5 X 

### X X X X Aroclor 1242 53469-21-9 

### X X X X X Aroclor 1248 12672-29-6 X 

### X X X X Aroclor 1254 11097-69-1 

### X X X 

### X X Aroclor 1260 11096-82-5 

### X X X 

### X X Azinphos-methyl 86-50-0 HS(62) NO NO NO 

### X Barban 101-27-9 LR NO NO NO LR Benzidine 92-87-5 CP CP CP CP CP Benzoicacid 65-85-0 

### X X ND 

### X X Benz(a)anthracene 56-55-3 X 

### X X X 

### X Benzo(b)fluoranthene 205-99-2 X 

### X X 

### X X

CD-ROM 8270D -1 Revision 4 January 1998Appropriate Preparation Techniques"


### 35401 Compounds CAS No" 3510 3520 3541 3550 3580 Benzo(k)fluoranthene 207-08-9 

### X X X X X Benzo(g,h,i)perylene 191-24-2 

### X X X 

### X X Benzo(a)pyrene 50-32-8 

### X v 

### X v V A. A. A. p-Benzoquinone 106-51-4 OE NO NO NO 

### X Benzyl alcohol 100-51-6 

### X X NO 

### X X a-BHC 319-84-6 

### X X X X 

### X**~-BHC** 319-85-7 

### X X X X X a-BHe 319-86-8 

### X X X X X y-BHC (Lindane) 58-89-9 

### X X X X X Bis(2-chloroethoxy)methane 111-91-1 

### X X X X X Bis(2-chloroethyl) ether 111-44-4 

### X X X X X Bis(2-chloroisopropyl) ether 108-60-1 

### X X X 

### X X Bis(2-ethylhexyl) phthalate 117-81-7 

### X X X X X 4-Bromophenyl phenyl ether 101-55-3 

### X X X X X Bromoxynil 1689-84-5 

### X NO NO NO 

### X Butyl benzyl phthalate 85-68-7 

### X 

### X X X X Captafol 2425-06-1

. HS(55) NO NO NO 

### X Captan 133-06-2 HS(40) NO NO NO 

### X Carbaryl 63-25-2 

### X NO NO NO 

### X Carbofuran 1563-66-2 

### X NO NO NO 

### X Carbophenothion 786-19-6 

### X NO NO NO 

### X Chlordane (NOS) 57-74-9 

### X X X 

### X X Chlorfenvinphos 470-90-6 

### X NO NO NO 

### X 4-Chloroaniline 106-47-8 

### X ND NO NO 

### X Chlorobenzilate 510-15-6 

### X NO NO NO 

### X 5-Chloro-2-methylaniline 95-79-4 

### X NO ND NO 

### X 4-Chloro-3-methylphenol 59-50-7 

### X X X X X 3-(Chloromethyl)pyridine 6959-48-4 

### X NO NO NO 

### X hydrochloride 1-Chloronaphthalene 90-13-1 

### X X X X X 2-Chloronaphthalene 91-58-7 

### X X X X X 2-Chlorophenol 95-57-8 

### X X X X X 4-Chloro-1.2-ohenvlenediamine 95-83-0 

### X X NO NO NO

- - - -- - - -, l J 4-Chloro-1,3-phenylenediamine 5131-60-2 

### X X NO NO NO 4-Chlorophenyl phenyl ether 7005-72-3 

### X X X X X Chrysene 218-01-9 

### X X X X X Coumaphos 56-72-4 

### X NO NO NO 

### X p-Cresidine 120-71-8 

### X NO NO NO 

### X Crotoxyphos 7700-17-6 

### X NO NO NO 

### X

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3540/ Compounds CAS Noa 3510 3520 3541 3550 3580 2-Cyclohexyl-4,6-dinitro-phenol 131-89-5 X ND ND ND LR 4,4'-DDD 72-54-8 X X X X X 4,4'-DDE 72-55-9 X X X X X 4,4'-DDT 50-29-3 X X X X X Demeton-O 298-03-3 HS(68) ND ND ND X Demeton-S 126-75-0 X ND ND ND X Diallate (cis ortrans) 2303-16-4 X ND ND ND X 2,4-Diaminotoluene 95-80-7 DC,OE(42) ND ND ND X Dibenz(a,j)acridine 224-42-0 X ND ND ND X Dibenz(a,h)anthracene 53-70-3 X X X X X Dibenzofuran 132-64-9 X X ND X X Dibenzo(a,e)pyrene 192-65-4 ND ND ND ND X 1,2-Dibromo-3-chloropropane 96-12-8 X X ND ND ND Di-n-butyl phthalate 84-74-2 X X X X X Dichlone 117-80-6 OE ND ND ND X 1,2-Dichlorobenzene 95-50-1 X X X X X 1,3-Dichlorobenzene 541-73-1 X X X X X 1,4-Dichlorobenzene 106-46-7 X X X X X 3,3'-Dichlorobenzidine 91-94-1 X X X X X 2,4-Dichlorophenol 120-83-2 X X X X X 2,6-Dichlorophenol 87-65-0 X ND ND ND X Dichlorovos 62-73-7 X ND ND ND X Dicrotophos 141-66-2 X ND ND ND X Dieldrin 60-57-1 X X X X X Diethyl phthalate 84-66-2 X X X X X Diethylstilbestrol 56-53-1 AW,OS(67) ND ND ND X Diethyl sulfate 64-67-5 LR ND ND ND LR Dimethoate 60-51-5 HE,HS(31) ND ND ND X 3,3'-Dimethoxybenzidine 119-90-4 X ND ND ND LR Dimethylaminoazobenzene 60-11-7 X ND ND ND X 7,12-Dimethylbenz(a)-anthracene 57-97-6 CP(45) ND ND ND CP 3,3'-Dimethylbenzidine 119-93-7 X ND ND ND X a,a-Dimethylphenethylamine 122-09-8 ND ND ND ND X 2,4-Dimethylphenol 105-67-9 X X X X X Dimethyl phthalate 131-11-3 X X X X X 1,2-Dinitrobenzene 528-29-0 X ND ND ND X 1,3-Dinitrobenzene 99-65-0 X ND ND ND X 1,4-Dinitrobenzene 100-25-4 HE(14) ND ND ND X 4,6-Dinitro-2-methylphenol 534-52-1 X X X X X

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- 3 Revision 4 January 1998Appropriate Preparation Techniques"
35401 Compounds CAS No8 3510 3520 3541 3550 3580 2,4-Dinitrophenol 51-28-5 

### X X X X X 2,4-Dinitrotoluene 121-14-2 

### X X X X X 2,6-Dinitrotoluene 606-20-2 

### X X 

### X X X Dinocap 39300-45-3 CP,HS(28) ND ND ND CP Dinoseb 88-85-7 

### X ND ND ND 

### X Diphenylamine 122-39-4 

### X X X X X 5,5-Diphenylhydantoin 57-41-0 

### X ND ND ND 

### X 1,2-Diphenylhydrazine 122-66-7 

### X X X X X Di-n-cetyl phthalate 117-84-0 

### X X X 

### X X Disulfoton 298-04-4 

### X ND ND ND 

### X Endosulfan I 959-98-8 

### X X X X X Endosulfan II 33213-65-9 

### X X X X X Endosulfan sulfate 1031-07-8 

### X X X X X Endrin 72-20-8 

### X X X X X Endrinaldehyde 7421-93-4 

### X X X X X Endrin ketone 53494-70-5 

### X X ND 

### X X EPN 2104-64-5 

### X ND ND ND 

### X Ethion 563-12-2 

### X ND ND ND 

### X Ethyl carbamate 51-79-6 DC(28) NO ND ND 

### X Ethyl methanesulfonate 62-50-0 

### X ND ND ND 

### X Famphur 52-85-7 

### X ND ND ND 

### X Fensulfothion 115-90-2 

### X ND NO ND 

### X Fenthion 55-38-9 

### X ND ND ND 

### X Fluchloralin 33245-39-5 

### X ND ND ND 

### X Fluoranthene 206-44-0 

### X X X X X Fluorene 86-73-7 

### X X X X X 2-Fluorobiphenyl (surr) 321-60-8 

### X X X X X 2-Fluorophenol (surr) 367-12-4

. 

### X X X X X Heptachlor 76-44-8 

### X X X X X Heptachlorepoxide 1024-57-3

. 

### X X X X X Hexachlorobenzene 118-74-1 

### X X X X X Hexachlorobutadiene 87-68-3 

### X X X X X Hexachtorocyclopentadiene 77-47-4 

### X X X X X Hexachloroethane 67-72-1 

### X X X X X Hexachlorophene 70-30-4 AW,CP(62) ND ND ND CP Hexachloropropene 1888-71-7 

### X ND ND ND 

### X Hexamethylphosphoramide 680-31-9 

### X ND NO ND 

### X Hydroquinone 123-31-9 ND NO NO ND 

### X Indeno(1,2,3-cd)pyrene 193-39-5 

### X X X X X

CD-ROM 82700- 4 Revision 4 January 1998Appropriate Preparation Techniques"
35401 Compounds CAS No" 3510 3520 3541 3550 3580 Isodrin 465-73-6 

### X NO ND ND 

### X Isophorone 78-59-1 

### X X X X X Isosafrole 120-58-1 OC(46) NO ND NO 

### X Kepone 143-50-0 

### X NO ND NO 

### X Leptophos 21609-90-5 

### X NO ND NO 

### X Malathion 121-75-5 HS(5) NO ND ND 

### X Maleic anhydride 108-31-6 

### HE ND ND ND 

### X Mestranol 72-33-3 

### X ND ND ND 

### X Methapyrilene 91-80-5 

### X ND ND ND 

### X Methoxychlor 72-43-5 

### X NO ND NO 

### X 3-Methylcholanthrene 56-49-5 

### X NO

. ND NO 

### X 4A'-Methylenebis (2-chloroaniline) 101-14-4 OE,OS(O) ND ND ND LR 4A'-Methylenebis(N,N-dimethyl- 101-61-1 

### X X ND ND ND aniline) Methyl methanesulfonate 66-27-3 

### X NO ND ND 

### X 2-Methylnaphthalene 91-57-6 

### X X ND 

### X X Methyl parathion 298-00-0 

### X NO ND ND 

### X 2-Methylphenol 95-48-7 

### X ND ND NO 

### X 3-Methylphenol 108-39-4 

### X NO ND ND 

### X 4-Methylphenol 106-44-5 

### X NO ND ND 

### X Mevinphos 7786-34-7 

### X ND ND ND 

### X Mexacarbate 315-18-4 HE,HS(68) ND ND ND 

### X Mirex 2385-85-5 

### X NO ND NO 

### X Monocrotophos 6923-22-4 HE NO ND NO 

### X Naled 300-76-5 

### X NO ND ND 

### X Naphthalene 91-20-3 

### X X X X X 1A-Naphthoquinone 130-15-4 

### X NO ND ND 

### X 1-Naphthylamine 134-32-7 OS(44) NO ND ND 

### X 2-Naphthylamine 91-59-8 

### X NO ND NO 

### X Nicotine 54-11-5 OE(67) ND ND ND 

### X 5-Nitroacenaphthene 602-87-9 

### X NO ND ND 

### X 2-Nitroaniline 88-74-4 

### X X ND 

### X X 3-Nitroaniline 99-09-2 

### X X ND 

### X X 4-Nitroaniline 100-01-6 

### X X ND 

### X X 5-Nitro-o-anisidine 99-59-2 

### X NO ND ND 

### X Nitrobenzene 98-95-3 

### X X X X X 4-Nitrobiphenyl 92-93-3 

### X ND ND NO 

### X Nitrofen 1836-75-5 

### X ND ND ND 

### X 2-Nitrophenol 88-75-5 

### X X X X X

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3540/ Compounds CAS No" 3510 3520 3541 3550 3580 4-Nitrophenol 100-02-7 

### X X X 

### X 

### X 5-Nitro-o-toluidine 99-55-8 

### X X NO NO X Nitroquinoline-1-oxide 56-57-5 X NO ND ND v A. N-Nitrosodi-n-butylamine 924-16-3 

### X NO NO NO X N-Nitrosodiethylamine 55-18-5 X NO NO NO X N-Nitrosodimethylamine 62-75-9 

### X X X 

### X X N-Nitrosomethylethylamine 10595-95-6 

### X NO NO NO X N-Nitrosodiphenylamine 86-30-6 X X X 

### X 

### X N-Nitrosodi-n-propylamine 621-64-7 X X X X X N-Nitrosomorpholine 59-89-2 NO ND NO NO 

### X N-Nitrosopiperidine 100-75-4 

### X NO NO NO 

### X N-Nitrosopyrrolidine 930-55-2 

### X NO NO NO 

### X Octamethyl pyrophosphoramide 152-16-9 LR NO NO NO LR 4,4'-Oxydianiline 101-80-4 X NO NO NO 

### X Parathion 56-38-2 

### X X NO NO 

### X Pentachlorobenzene 608-93-5 X NO NO NO X Pentachloronitrobenzene 82-68-8 X NO NO NO 

### X Pentachlorophenol 87-86-5 

### X X X X X Phenacetin 62-44-2 

### X NO NO NO 

### X Phenanthrene 85-01-8 

### X X X 

### X X Phenobarbital 50-06-6 X NO NO NO X Phenol 108-95-2 OC(28) X 

### X X X 1,4-Phenylenediamine 106-50-3 

### X NO NO NO X Phorate 298-02-2 X NO NO NO X Phosalone 2310-17-0 HS(65) NO NO NO 

### X Phosmet 732-11-6 HS(15) NO NO NO 

### X Phosphamidon 13171-21-6 HE(63) NO NO NO 

### X Phthalicanhydride 85-44-9 CP,HE(1) NO NO NO CP 2-Picoline (2-Methylpyridine) 109-06-8 

### X X NO NO NO Piperonyl sulfoxide 120-62-7 X NO NO NO X Pronamide 23950-58-5 

### X NO NO NO X Propylthiouracil 51-52-5 LR NO NO NO LR

D\1r'on.o. 129-00-0 

### X X X X X .I

..1 I vit"'" Resorcinol 108-46-3 OC,OE(10) NO NO NO 

### X Safrole 94-59-7 X NO NO NO, X Strychnine 57-24-9 AW,OS(55) NO NO NO X Sulfallate 95-06-7 X NO NO NO X Terbufos 13071-79-9 X NO NO NO X 1,2,4,5-Tetrachlorobenzene 95-94-3 X NO NO NO 

### X

CO-ROM 82700 - 6 Revision 4 January 1998Appropriate Preparation Techniques"
3540/ Compounds CAS Noa 3510 3520 3541 3550 3580 2,3,4,6-Tetrachlorophenol 58-90-2 X NO NO NO X Tetrachlorvinphos 961-11-5 X NO NO NO X Tetraethyl dithiopyrophosphate 3689-24-5 X X NO NO NO Tetraethyl pyrophosphate 107-49-3 X NO NO NO X Thionazine 297-97-2 X NO NO NO X Thiophenol (Benzenethiol) 108-98-5 X NO NO NO X Toluene diisocyanate 584-84-9 HE(6) NO NO NO X o-Toluidine 95-53-4 X NO NO NO X Toxaphene 8001-35-2 X X X X X 1,2,4-Trichlorobenzene 120-82-1 X X X X X 2,4,5-Trichlorophenol 95-95-4 X X NO X X 2,4,6-Trichlorophenol 88-06-2 X X X X X Trifluralin 1582-09-8 X NO NO NO X 2,4,5-Trimethylaniline 137-17-7 X NO NO NO X Trimethyl phosphate 512-56-1 HE(60) NO NO NO X 1,3,5-Trinitrobenzene 99-35-4 X NO NO NO X Tris(2,3-dibromopropyl) phosphate 126-72-7 X NO NO NO LR Tri-p-tolyl phosphate 78-32-0 X NO NO NO X O,O,O-Triethyl phosphorothioate 126-68-1 X NO NO NO X

aChemical Abstract Service Registry Number

b See Sec. 1.2 for other acceptable preparation methods.

KEY TO ANALYTE LIST

AW= Adsorption to walls ofglassware during extraction and storage. CP = Nonreproducible chromatographic performance. OC Unfavorable distribution coefficient (numberin parenthesis is percent recovery). HE = Hydrolysis during extraction accelerated by acidic or basic conditions (number in parenthesis is percent recovery). HS = Hydrolysis during storage (number in parenthesis ispercent stability). LR 

# = Low response. NO

## = Not determined. OE 

# = Oxidation during extraction accelerated by basic conditions (number in parenthesis is percent recovery). OS- Oxidation during storage (number in parenthesis is percentstability).

X 

# = Greaterthan 70 percent recovery by this technique.

1.2 In addition to the sample preparation methods listed in the above analyte list, Method 3535 describes a solid-phase extraction procedure that may be applied to the extraction of semivolatiles from TCLP leachates (Tables 16 and 17 contain performance data). Method 3542

CO-ROM 82700 - 7 Revision 4 January 1998

### describes sample preparation for semivolatile organic compounds in air sampled by Method 0010 (Table 11 contains surrogate performance data), Method 3545 describes an automated solvent extractiondevice for semivolatiles in solids (Table 12 contains performance data), and Method 3561 describes asupercriticalfluid device for the extraction of PAHs from solids (see Tables 13, 14, and 15 forperformancedata). 1.3 Method 8270 can be used to quantitate most neutral, acidic, and basic organic compounds that are soluble in methylene chloride and capable of being eluted, without derivatization, as sharp peaks from a gas chromatographicfused-silica capillary column coated with a slightly polar silicone. Such compounds include polynuclear aromatic hydrocarbons, chlorinated hydrocarbonsand 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 characteristicions that have been evaluated. In most cases, Method 8270 is not appropriatefor the quantitation ofmulticomponentanalytes, e.g., Aroclors,Toxaphene, Chlordane, etc., because of limited sensitivity forthose analytes. When these analytes have been identified by another technique, Method 8270 may be appropriate for confirmation of the identification of these analytes when concentration in the extract permits. Refer to Sec. 7.0 of Methods 8081 and 8082 for guidance on calibration and quantitation of multicomponentanalytes such as the Aroclors, Toxaphene, and Chlordane.

1.4 method: The following compounds may require specialtreatment when being determined by this

1.4.1 Benzidine may be subject to oxidativelosses during solvent concentration and its chromatographicbehavior is poor. 1.4.2 Under the alkaline conditions of the extraction step from aqueous matrices, a-BHC, V-BHC, Endosulfan I and II, and Endrin are subject to decomposition. Neutral extraction should be performed if these compounds are expected.

1.4.3 Hexachlorocyclopentadiene is subject to thermal decomposition in the inlet of the gas chromatograph, chemical reaction in acetone solution, and photochemical decomposition.

1.4.4 N-nitrosodimethylamine is difficult to separate from the solvent under the chromatographicconditions described.

1.4.5 N-nitrosodiphenylamine decomposes in the gas chromatographic inlet and cannot be separated from diphenylamine.

1.4.6 Pentachlorophenol, 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, especially if the GC system is contaminated with high boiling material. 1.4.7 Pyridine may perform poorly at the GCinjection port temperatures listed in the method. Lowering the injection port temperature may reduce the amount of degradation. However, the analyst must use caution in modifying the injection port temperature, as the performance of other analytes may be adversely affected. Therefore, if pyridine is to be determined in addition to other target analytes, it maybe necessary to perform separate

CD-ROM 82700- 8 Revision 4 January 1998analyses. In addition, pyridine may be lost during the evaporative concentration of the sample extract. As a result, many of the extraction methods listed above may yield low recoveries unless great care isexercised during the concentration steps. For this reason, analysts may wish to consider the use of extractiontechniques such as pressurized fluid extraction (Method 3545) or supercritical fluid extraction, which involve smallerextract volumes, thereby reducing oreliminating the need for evaporative concentration techniquesfor many applications.

1.4.8 Toluene diisocyanate rapidly hydrolyses in water (half-life of less then 30 min.). Therefore, recoveries of this compound from aqueous matrices should not be expected. In addition, in solid matrices, toluene diisocyanate often reacts with alcohols and amines to produce urethane and ureas and consequently cannot usually coexist in a solution containing these materials.
1.4.9 In addition, analytes in the list provided above areflagged when there are limitations caused by sample preparation and/orchromatographic problems.

1.5 The estimated quantitation limit (EQL) of Method 8270 for determining an individual compound is approximately 660 J..Ig/kg (wet weight) for soil/sediment samples, 1-200 mg/kg for wastes (dependent on matrix and method of preparation), and 10 J..Ig/Lfor ground watersamples (see Table 2). EQLs will be proportionately higherforsample extractsthat require dilution to avoid saturation of the detector. 1.6 This method is restricted to use by or under the supervision ofanalysts experienced in the use of gas chromatograph/mass spectrometers and skilled in the interpretation of mass spectra. Each analyst must demonstrate the ability to generate acceptable resultswith this method.

2.0 SUMMARYOF METHOD

2.1 The samples are prepared for analysis by gas chromatography/mass spectrometry (GC/MS) using the appropriate sample preparation (refer to Method 3500) and, ifnecessary, sample cleanup procedures (refer to Method 3600).

2.2 The semivolatile compounds are introduced into the GC/MS by injecting the sample extract into a gas chromatograph (GC) with a narrow-bore fused-silica capillary column. The GC column is temperature-programmed to separatethe analytes, which are then detectedwith a mass spectrometer (MS) connected to the gas chromatograph.

2.3 Analytes eluted from the capillary column are introduced into the mass spectrometer via ajet separator or a direct connection. Identification of target analytes is accomplished by comparing their mass spectra with the electron impact (or electron impact-like) spectra ofauthentic standards. Quantitation is accomplished by comparing the response of a major (quantitation) ion relative to an internal standard using afive-point calibration curve.

2.4 The method includes specific calibration and quality control steps that supersedethe general requirements provided in Method 8000.

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### 3.0 INTERFERENCES 3.1 Raw GC/MS data from all blanks, samples, and spikes must be evaluated for interferences. Determine if the source of interference is in the preparation and/or cleanup of the samples and take corrective action to eliminatethe problem. 3.2 Contamination by carryover can occur whenever high-concentration and low-concentrationsamples are sequentially analyzed. To reduce carryover, the sample syringe must be rinsed with solventbetween sample injections. Whenever an unusually concentrated sample is encountered, it should be followed by the analysis of solvent to check for cross-contamination.

4.0 APPARATUS AND MATERIALS

4.1 Gaschromatograph/massspectrometersystem
4.1.1 Gas chromatograph - An analytical system complete with a temperature-programmablegaschromatograph suitable for splitless injection and all required accessories, including syringes, analytical columns, and gases. The capillary column should be directly coupled to the source. 4.1.2 Column - 30-m x 0.25-mm ID (or 0.32-mm ID) t-urn film thickness silicone-coated fused-silica capillary column (J&W Scientific D8-5 or equivalent).

4.1.3 Massspectrometer

4.1.3.1 Capable of scanning from 35 to 500 amu every 1 sec or less, using 70 volts (nominal) electron energy in the electron impactionization mode. The mass spectrometer must be capable of producing a mass spectrum for decafluorotriphenylphosphine (DFTPP) which meets the criteria in Table 3 when 1 IJl of the GC/MS tuning standard is injected through the GC (50 ng of DFTPP).

4.1.3.2 

### Anion trap mass spectrometermay be used if it is capable of axial modulation to reduce ion-molecule reactions and can produce electron impact-like spectra that match those in the EPAINIST Library. The massspectrometermust be capableofproducing a massspectrum for DFTPP which meets the criteria in Table 3 when 5 or 50 ng are introduced. 4.1.4 GCIMS interface- Any GC-to-MS interfacemay be used that gives acceptable calibration pointsat 50 ng per injectionfor each compound of interest and achieves acceptable tuning performance criteria. For a narrow-bore capillary column, the interface is usually capillary-direct into the mass spectrometersource. 4.1.5 Data system - A computer system should be interfaced to the mass spectrometer. The system must allow the continuous acquisition and storage on machine-readable media of all mass spectra obtained throughout the duration of the chromatographic program. The computershould have software that can search any GC/MS data file for ions of a specific mass and that can plot such ion abundances versus time or scan number. This type of plot is defined as an Extracted Ion Current Profile (EICP). Software should also be availablethat allows integratingthe abundances in any EICP between specified time or scan-number limits. The most recent version of the EPAINIST Mass Spectral Library should also be available.

CD-ROM 8270D.c10 Revision 4 January 19984.1.6 Guard column (optional)- (J&Wdeactivated fused-silica, 0.25-mm 10 x 6-m, or equivalent) between the injection port and the analytical column joined with column joiners (Hewlett-Packard Catalog No. 5062-3556, or equivalent). 4.2 Syringe - 10-1JL.

4.3 Volumetricflasks, Class A -Appropriate sizes with ground-glass stoppers.

4.4 Balance -Analytical, capable ofweighing 0.0001 g. 4.5 Bottles - glass with polytetrafluoroethylene (PTFE)-lined screw caps or crimp tops.

5.0 REAGENTS

5.1 Reagent grade inorganic chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its usewithout lessening the accuracy of the determination. 5.2 Organic-free reagent water - All references to water in this meth od refer to organic-free reagentwater, as defined in ChapterOne. 5.3 Stock standard solutions (1000 mg/L) - Standard solutions can be prepared from pure standard materials orpurchased as certified solutions.

5.3.1 Prepare stockstandard solutions by accurately weighing about 0.0100 g of pure material. Dissolve the material in pesticide quality acetone orothersuitablesolvent and dilute to volume in a 1O-mLvolumetric flask. Largervolumes can be used at the convenience of the analyst. . When compound purity is assayed to be 96% orgreater, the weight may be used without correction to calculatethe concentration of the stock standard. Commerciallyprepared stock standards may be used at any concentration if they are certified by the manufactureror by an independentsource.
5.3.2 Transfer the stock standard solutions into bottles with PTFE-lined screw-caps. Store, protected from light, at -10 0C or less or as recommended by the standard manufacturer. Stock standard solutions should be checked frequently for signs of degradation orevaporation, especiallyjust prior to preparing calibration standardsfrom them.

5.3.3 Stock standard solutions must be replaced after 1 year or sooner if comparison with quality control checksamples indicates a problem.

5.3.4 It is recommended that nitrosamine compounds be placed together in a separate calibration mix and not combined with other calibration mixes. When using a premixed certified standard, consultthe manufacturer's instructionsforadditional guidance. 5.3.5 Mixes with hydrochloride salts may contain hydrochloric acid, which can cause analytical difficulties. When using a premixed certified standard, consultthe manufacturer's instructionsfor additional guidance.

CD-ROM 82700 - 11 Revision 4 January 19985.4 Internal standard solutions - The internal standards recommended are 1,4-dichlorobenzene-d; naphthalene-d8' acenaphthene-d 10' phenanthrene-d 10' chrysene-d 12' and perylene-d., (seeTable 5). Other compounds may be used as internal standards as long as the specifications in Sec. 7.3.2 are met. 5.4.1 Dissolve 0.200 g of each compound with a small volume of carbon disulfide. Transferto a 50 mLvolumetricflaskand diluteto volume with methylene chloride sothatthe finalsolventisapproximately20% carbon disulfide. Most of the compounds are also soluble in small volumes of methanol, acetone, or toluene, except for perylene-d.; The resulting solution will contain each standard at a concentration of 4,000 

### ng/llL. Each 1-ml sample extract undergoing analysis should be spiked with 10 

### III of the internal standard solution, resulting in a concentration of 40 ng/lllofeach internal standard. Store at -1O°C or less when not in use. When using premixed certified solutions, store according to the manufacturers documented holding time and storagetemperature recommendations.

5.4.2 If a more sensitive massspectrometeris employed to achieve lowerdetection levels, amoredilute internal standard solution may be required. Area counts of the internal standard peaks shouldbebetween 50-200% of the area of thetargetanalytes in the mid-point calibration analysis.

5.5 GC/MS tuning standard - A methylene chloride solution containing 50 ng/lll of decafluorotriphenylphosphine (DFTPP) should be prepared. The standard should also contain 50 ng/llleach of4,4'-DDT, pentachlorophenol, and benzidineto verify injection portinertness and GC column performance. Store at -10°C or less when not in use. If a more sensitive mass spectrometer is employedto achieve lowerdetection levels, a more dilute turiing solution may be necessary. When using premixed certified solutions, store according to the manufacturer's documented holding time and storagetemperature recommendations.

5.6 Calibration standards - A minimum of five calibration standards should be prepared at five different concentrations. At least one of the calibration standards should correspondto asample concentration at or below that necessaryto meetthe data quality objectives ofthe project. The remaining standards shouldcorrespondto the range of concentrationsfound in actual samples but should not exceed the working range of the GC/MS system. Each standard should contain each analytefor detection by this method.

5.6.1 It is the intent of EPA that all target analytes for a particular analysis be included in the calibration standard(s). Thesetarget analytes may not includethe entire list of analytes (Sec. 1.1) for which the method has been demonstrated. However, the laboratory shall not report a quantitative result for atargetanalytethat was not included in the calibration standard(s).

5.6.2 Each 1-mlaliquot of calibration standard should be spiked with 10 

### III of the internal. standard solution prior to analysis. All standards should be stored at -1O°C or less, and should be freshly prepared once a year, orsoonerif check standards indicate a problem. The calibration verification standard should be prepared weekly and stored at 4DC. When using premixed certifiedsolutions, storeaccording to the manufacturer's documented holding time and storage temperature recommendations.

5.7 Surrogate standards- The recommended surrogates are phenol-de, 2-fluorophenol, 2,4,6-tribromophenol, nitrobenzene-d., 2-f1uorobiphenyl, and p-terphenyl-d.; See Method 3500 for instructions on preparing the surrogate solutions.

CD-ROM 82700 -12 Revision 4 January 19985.7.1 Surrogate standard check - Determine what the appropriate concentration should be for the blankextracts after all extraction, cleanup, and concentration steps. Inject this concentration into the GC/MS to determine recovery of surrogate standards. It is recommended that this check be done whenever a newsurrogate spiking solution is prepared. NOTE: Method 3561 (SFE Extraction of PAHs) recommends the use of bromobenzene and p-quaterphenyl to bettercover the range of PAHs listed in the method. 5.7.2 If a more sensitive mass spectrometer is employed to achieve lowerdetection levels, a more dilute surrogate solution may be necessary.

5.8 Matrixspike and laboratory control standards - See Method 3500 for instructions on preparing the matrix spike standard. The same standard may be used as the laboratory control standard (LCS).

5.8.1 Matrix spike check - Determine what concentration should be in the blank extracts after all extraction, cleanup, and concentration steps. Inject this concentration into the GC/MSto determine recovery. It is recommended that this check be done whenevera new matrix spiking solution is prepared. 5.8.2 If a more sensitive mass spectrometer is employed to achieve lowerdetection levels, a more dilute matrixand LCS spiking solution may be necessary. 5.8.3 Some projects may require the spiking of the specific compounds of interest, since the spiking compounds listed in Method 3500 would not be representative of the compounds of interest required for the project. When this occurs, the matrix and LCS spiking standards should be prepared in methanol, with each compound present at aconcentration appropriatefor the project.
5.9 Solvents - Acetone, hexane, methylene chloride, isooctane, carbon disulfide, toluene, and other appropriate solvents. All solvents should be pesticide quality or equivalent.

6.0 SAMPLE COLLECTION, PRESERVATION, AND HANDLING

6.1 See the introductory material to this chapter, OrganicAnalytes, Sec. 4.1. 6.2 Store the sample extracts at -10°C, protected from light, in sealed vials (e.g., screw-cap vials orcrimp-capped vials) equipped with unpierced PTFE-lined septa.

7.0 PROCEDURE 7.1 Sample preparation

7.1.1 Samples are normally prepared by one of the following methods prior to GC/MSanalysis.

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### Matrix Air (particulates and sorbent resin) Water(including TCLP leachates) Soil/sediment Waste Methods

3542 3510,3520,3535 3540,3541,3545,3550,3560,3561 3540,3541,3545,3550,3560,3561,3580 7.1.2 In very limited applications, direct injection of the sample into the GC/MS system with a 10-IJL syringe may be appropriate. The detection limit is very high (approximately 10,000 IJg/L). Therefore, it is only permitted where concentrations in excess of 10,000 IJg/Lare expected. 7.2 Extract cleanup - Extracts may be cleaned up by any of the following methods prior to GC/MS analysis. Analytes ofinterest

Aniline & aniline derivatives Phenols Phthalate esters Nitrosamines Organochlorine pesticides &·PCBs Nitroaromatics and cyclic ketones Polynuclear aromatic hydrocarbons Haloethers Chlorinated hydrocarbons Organophosphorus pesticides Petroleum waste All base, neutral, and acid

priority pollutants Methods

3620 3630,3640,8041 a 

### 3610,3620,3640 3610,3620,3640 3610,3620,3630,3660,3665 3620, 3640 3611,3630,3640 3620,3640 3620, 3640 3620 3611,3650

3640

a 

### Method 8041 includes a derivatization technique and a GC/ECD analysis, if interferences

are encountered on GC/FID.

7.3 Initial calibration
Establishthe GC/MSoperating conditions, using the following recommendations as guidance. Mass range: Scan time: Initialtemperature: Temperature program: Final temperature: Injector temperature: Transferlinetemperature: 

### Sourcetemperature: Injector: Injection volume: Carrier gas: Ion trap only: 35-500 amu 1 sec/scan 40°C, hold for 4 minutes 40-270°C at 10°C/min 270°C, hold until benzo[g,h,i]peryleneelutes 250-300°C 250-300°C Accordingto manufacturer'sspecifications Grob-type, splitless 1-2 IJL Hydrogen at 50 em/sec or helium at 30 em/sec Set axial modulation, manifold temperature, and emission current to manufacturer's recommendations

CD'-ROM 8270D - 14 Revision 4 January 1998Split injection is allowed if the sensitivity of the mass spectrometer issufficient.

7.3.1 The GC/MS system must be hardware-tuned using a 50-ng injection of DFTPP. Analyses must not begin until the tuning criteria are met. 7.3.1.1 In the absence of specific recommendations on how to acquire the mass spectrum of DFTPP from the instrument manufacturer, the following approach has been shown to be useful: Three scans (the peak apex scan and the scans immediately preceding and following the apex) are acquired and averaged. Background subtraction is required, and must be accomplished using a single scan acquired no more than 20 scans prior to the elution of DFTPP. The background subtraction should be designed only to eliminate column bleed or instrument background ions. Do not subtract part of the DFTPP peak.

7.3.1.2 Use the DFTPP mass intensity criteria in Table 3 as tuning acceptance criteria. Alternatively, other documented tuning criteria may be used (e.g. CLP, Method 525, ormanufacturer's instructions), provided that method performance is not adversely affected.

NOTE: All subsequent standards, samples, MS/MSDs, and blanks associated with a DFTPP analysis must use the identical mass spectrometer instrument conditions.

7.3.1.3 The GC/MS tuning standard solution should also be used to assess GC column performance and injection port inertness. Degradation of DDT to DOE and DOD should not exceed 20%. (See Sec. 8.0 of Method 8081 for the percent breakdown calculation). Benzidine and pentachlorophenol should be present at their normal responses, and no peak tailing should be visible.

7.3.1.4 If degradation is excessive and/or poor chromatography is noted, the injection port may require cleaning. It may also be necessaryto break off the first 6-12 in. of the capillary column. The use of a guard column (Sec. 4.1.6) between the injection port and the analytical column may help prolong analytical column performance.

7.3.2 The internal standards selected in Sec. 5.4 should permit most of the components of interest in a chromatogram to have retention times of0.80-1.20 relative to one of the internal standards. Use the base peak ion from the specific internal standard as the primary ion for quantitation (see Table 1). If interferences are noted, use the next most intense ion as the quantitation ion (i.e. for 1,4-dichlorobenzene-d4, use 152 m/z for quantitation).
7.3.3 Analyze 1-2 IJL of each calibration standard (containing internal standards) and tabulate the area of the primary characteristic ion against concentration for each target analyte (as indicated in Table 1). A set of at least five calibration standards is necessary (see Sec. 5.6 and Method 8000). The injection volume must be the same for all standards and sample extracts. Figure 1 shows a chromatogram of a calibration standard containing base/neutral and acid analytes. Calculate response factors (RFs) for each target analyte relative to one of the internal standards asfollows:

CD-ROM 82700 - 15 Revision 4 January 1998RF

where: 

## As 

# = Peakarea (or height) of the analyte orsurrogate. AiS

# = Peakarea (or height) of the internal standard. 

### C, 

### = Concentration of the analyte orsurrogate, in 

### Ilg/L. Cis 

### = Concentration of the internal standard, in 

### Ilg/L.

7.3.4 System performance check compounds (SPCCs)

7.3.4.1 A system performance check must be performedto ensurethat minimum average RFs are met before the calibration curve is used. Forsemivolatiles, the System performance check compounds (SPCCs) are: N-nitroso-di-n-propylamine; hexachlorocyclopentadiene; 2,4-dinitrophenol; and 4-nitrophenol.

7.3.4.2 The minimum acceptable average RF for these compounds is 0.050. These SPCCs typically have very low RFs (0.1-0.2) and tend to decrease in response as the chromatographic systembeginsto deteriorate or the standard material begins to deteriorate. They are usually the first to show poorperformance. Therefore, they must meetthe minimumrequirementwhen the system is calibrated.

7.3.4.3 If the minimum response factors are not met, the system must be evaluated, and corrective action must be taken before sample analysis begins. Possible problems include standard mixture degradation, injection port inlet contamination, contamination at the front end of the analytical column, and active sites in the column or chromatographic system. This check must be met before sample analysis begins.

7.3.5 Calibration check compounds (GCGs) 7.3.5.1 The purpose of the CCCs are to evaluatethe calibration from the standpoint of the integrity of the system. High variabilityforthese compounds may be indicative ofsystem leaks or reactive sites on the column. Meeting the GGG criteria is not a substitute for successful calibration of the target analytes using one of the approaches described in Sec. 7.0 of Method 8000.

7.3.5.2 Calculate the mean response factorand the relative standard deviation (RSD) of the response factors for each target analyte. The RSD should be less than or equal to 15% for each target analyte. However, the RSD for each individual GGC (seeTable4) must be less than or equal to 30%.



### n n-1 n L(RFi-RF)2 i=1 SD n LRFj i=1 mean RF = RF = --

CD-ROM 8270D - 16 Revision 4 January 1998RSD 

## so =_ x RF 100

7.3.5.3 If the RSD of any CCC is greater than 30%, then the chromatographic system is too reactive for analysis to begin. Clean or replace the injector liner and/or capillary column, then repeat the calibration procedure beginning with Sec. 7.3.

7.3.5.4 If the CCCs are not included in the list of analytes for a project, and therefore not included in the calibration standards, then refer to Sec. 7.0 of Method 8000. 7.3.6 Evaluation of retention times - The relative retention time (RRT) of each target analyte in each calibration standard should agree within 0.06 RRT units. Late-eluting target analytes usually have much better agreement.

Retention time of the analyte Retention time of the internal standard RRT = --------------''----

7.3.7 Linearity of target analytes-Ifthe RSD of anytargetanalytes is 15% or less, then the relative response factor is assumed to be constant over the calibration range, and the average relative response factor may be used for quantitation (Sec. 7.6.2). 7.3.7.1 If the RSD of any target analyte isgreaterthan 15%, refer to Sec. 7.0 in Method 8000 for additional calibration options. One of the options must be applied to GC/MS calibration in this situation, or a new initial calibration must be performed.

NOTE: Method 8000 designates a linearity criterion of 20% RSD. That criterion pertains to GC and HPLC methods other than GC/MS. Method 8270 requires 15% RSD as evidence ofsufficient linearity to employ an average response factor.

7.3.7.2 When the RSD exceeds 15%, the plotting and visual inspection of a calibration curve can be a useful diagnostictool. The inspection may indicate analytical problems, including errors in standard preparation, the presence of active sites in the chromatographic system, analytes that exhibit poor chromatographic behavior, etc.
7.4 GC/MS calibration verification - Calibration verification consists of three steps that are performed at the beginning of each 12-hour analytical shift. 7.4.1 Prior to the analysis ofsamples or calibration standards, inject 50 ng of the DFTPP standard into the GC/MS system. The resultant mass spectrum for DFTPP must meet the criteria given in Table 3 before sample analysis begins. These criteria must be demonstrated each 12-hourshift during which samples are analyzed.

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### 7.4.2 The initial calibration (Sec. 7.3) for each compound of interest should be verified once every 12 hours prior to sample analysis, using the introduction technique and conditions used for samples. This is accomplished by analyzing a calibration standard at a concentration near the midpointconcentration for the calibrating range of the GC/MS. The results from the calibration standard analysis should meet the verification acceptance criteria provided in Secs. 7.4.4 through 7.4.7.

NOTE: The DFTPP and calibration verification standard may be combined into a single standard as long as both tuning andcalibrationverificationacceptance criteria for the project can bemetwithoutinterferences. 7.4.3 A method blank should be analyzed either after the calibration standard, or at any other time during the analytical shift, to ensure that the total system (introduction device, transfer lines and GC/MS system) is free of contaminants. If the method blank indicates contamination, then it may be appropriate to analyze a solvent blank to demonstratethat the contamination is not a result of carryoverfrom standards or samples. See Sec. 8.0 of Method 80008for method blank performance criteria. 7.4.4 System performance check compounds (SPCCs) 7.4.4.1 A system performancecheck must be made during every 12-hour analytical shift. Each spce in the calibration verification standard must meet a minimum response factorof0.050. This is the same checkthat is applied during the initial calibration. 7.4.4.2 If the minimum responsefactors are not met, the system mustbe evaluated, and corrective action must be taken before sample analysis begins. Possible problems include standard mixture degradation, injection port inlet contamination, contamination at the front end of the analytical column, and active sites in the column or chromatographic system. This check must be met before sample analysis begins. 7.4.5 Calibration check compounds (eees)

7.4.5.1 Afterthe system performance check is met, the CCCs listed in Table 4 are used to check the validity ofthe initial calibration. Use percent difference when performing the average response factor model calibration. Use percent drift when calibrating using a regression fit model. Refer to Sec. 7.0 of Method 8000 for guidance on calculating percent difference and drift. 7.4.5.2 If the percent difference for each eee is less than or equal to 20%, then the initial calibration is assumed to be valid. If the criterion is not met (i.e., greater than 20% differenceor drift) foranyone eee, then corrective action must be taken prior to the analysis of samples. If the cees are not included in the list of ana!ytes for a project, and therefore not included in the calibration standards, then all 

### analytes must meet the 20% difference or drift criterion.

7.4.5.3 Problems similar tothose listed under specs could affect the CCCs. If the problem cannot be corrected by other measures, a new initial calibration must be generated. The eee criteria must be met before sampleanalysis begins.

CD-ROM 82700-18 Revision 4 January 19987.4.6 Internal standard retention time - The retention times of the internal standards in the calibration verification standard must be evaluated immediately after or during data acquisition. If the retention time for any internal standard changes by more than 30 seconds from that in the mid-pointstandard level of the most recent initial calibration sequence, then the chromatographic system must be inspected for malfunctions and corrections must be made, as required. When corrections are made, reanalysis of samples analyzed while the system was malfunctioning is required.

7.4.7 Internal standard response-Ifthe EICP area for any of the internal standards in the calibration verification standard changes by afactorof two (-50% to +100%) from that in the mid-point standard level of the most recent initial calibration sequence, the mass spectrometer must be inspected for malfunctions and corrections must be made, as appropriate. When corrections are made, reanalysis ofsamples analyzed while the system was malfunctioning is required.

7.5 GC/MSanalysis of samples 7.5.1 It is highly recommended that sample extracts be screened on a GC/FID or GC/PID using the same type of capillary column used in the GC/MSsystem. This will minimize contamination of the GC/MS system from unexpectedly high concentrations of organic compounds. 7.5.2 Allow the sample extract to warm to room temperature. Just prior to analysis, add 10IJLof the internal standard solution to the 1-mL concentrated sample extract obtained from sample preparation.
7.5.3 Inject a 1-2IJLaliquot of the sample extract into the GC/MSsystem, using the same operating conditions that were used for the calibration (Sec. 7.3). The volume to be injected should contain 100 ng of base/neutral and 200 ng of acid surrogates (assuming 100% recovery), unless a more sensitive GC/MSsystem is being used and the surrogate solution is less concentrated then that listed in Sec. 5.7. The injection volume must be the same volume used for the calibration standards. 7.5.4 If the response for any quantitation ion exceeds the initial calibration range of the GC/MSsystem, the sample extract must be diluted and reanalyzed. Additional internal standard solution must be added to the diluted extract to maintain the same concentration as in the calibration standards (40ng/lJL, unless a more sensitive GC/MS system is being used). Secondary ion quantitation should be used only when there are sample interferenceswith the primary ion. NOTE: It may be a useful diagnostictool to monitor internal standard retention times and responses (area counts) in all samples, spikes, blanks, and standardsto effectively check drifting method performance, poor injection execution, and anticipatethe need for system inspection and/or maintenance. 7.5.4.1 When ions from a compound in the sample saturatethe detector, this analysis must be followed by the analysis of an instrument blank consisting of clean solvent. If the blank analysis is not free ofinterferences, then the system must be decontaminated. Sample analysis may not resume until the blank analysis is demonstrated to be free ofinterferences.

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### 7.5.4.2 All dilutions should keep the response ofthe major constituents (previously saturated peaks) in the upper half of the linearrange of the curve. 7.5.5 The use of selected ion monitoring (SlM) is acceptable for applications requiring detection limits below the normal range of electron impact mass spectrometry. However,SIM may provide a lesser degree ofconfidencein the compound identification unless multiple ions are monitored for each compound. 7.6 Qualitative analysis

7.6.1 The qualitative identification of compounds determined by this method is based on retention time and on comparison of the sample mass spectrum, after background correction, with characteristic ions in a reference mass spectrum. The reference mass spectrum must be generated by the laboratory using the conditions of this method. The characteristicions from the reference mass spectrum are defined as the three ions of greatest relative intensity, or any ions over 30% relative intensity, if tessthan three such ions occur in the reference spectrum. Compounds are identified when the following criteria are met.

7.6.1.1 The intensities of the characteristic ions of a compound must maximize in the same scan or within one scan of each other. Selection of a peak by a data system target compound search routine where the search is based on the presence of a targetchromatographic peak containing ions specific for the target compound at a compound-specific retention time will be accepted as meeting this criterion. 7.6.1.2 The RRT of the sample component is within 

### ±0.06 RRT units of the RRT of the standard component.

7.6.1.3 The relativeintensitiesof the characteristic ions agree within 30% of the relative intensities of these ions in the reference spectrum. (Example: For an ion with an abundance of 50% in the reference spectrum, the corresponding abundance in a sample spectrum can range between 20% and 80%.) 7.6.1.4 Structuralisomers that produce very .similar mass spectra should beidentifiedas individual isomersif they have sufficiently different GC retention times. Sufficient GC resolution is achieved 

### ifthe height of thevalley between two isomer peaks is less than 25% of the sum of the two peak heights. Otherwise, structural isomers are identified as isomeric pairs. Oiastereomeric pairs (e.g., Aramite and lsosafrol) that may be separable by the GC should be identified, quantitated and reported as the sum of both compounds by the GC.

7.6.1.5 Identification is hampered when sample components are not resolved chromatographically and produce mass spectra containing ions contributed by more than one analyte. When gas chromatographic peaks obviously represent more than one sample component (Le., a broadened peakwith shou!der(s) or a valley 

### between two or more maxima), appropriate selection of analyte spectra and background spectra is important. 7.6.1.6 Examination of extracted ion current profiles of appropriate ions can aid in the selectionof spectra and inqualitative identification of compounds. When analytes coelute (i.e., only one chromatographic peak is apparent), the identification

CD-ROM 82700- 20 Revision 4 January 1998criteria may be met, but each analyte spectrum will containextraneous ions contributed by the coeluting compound.

7.6.2 For samples containing components not associated with the calibration standards, a library search may be made for the purpose of tentative identification. The necessity to perform this type of identification will be determined by the purpose of the analyses being conducted. Data system library search routines should not use normalization routines that would misrepresent the library or unknown spectra when compared to each other. For example, the ReRA permit or waste delisting requirements may require the reporting of non-target analytes. Only after visual comparison of sample spectra with the nearest library searches may the analyst assign a tentative identification. Guidelines for tentative identification are: (1) Relative intensities of major ions in the reference spectrum (ions> 10% of the most abundant ion) should be present in the sample spectrum. (2) The relative intensities of the major ions should agree within ± 20%. (Example: For an ion with an abundance of 50% in the standard spectrum, the corresponding sample ion abundance must be between 30 and 70%.) (3) Molecular ions present in the reference spectrum should be present in the sample spectrum. (4) Ions present in the sample spectrum but not in the reference spectrum should be reviewed for possible background contamination or presence of coeluting compounds. (5) Ions present in the reference spectrum but not in the sample spectrum should be reviewed for possible subtraction from the sample spectrum because of background contamination or coeluting peaks. Data system library reduction programs can sometimes create these discrepancies.

7.7 Quantitative analysis 7.7.1 Once a compound has been identified, thequantitation of that compound will be based on the integrated abundance of the primary characteristic ion from the EICP.

7.7.2 If the RSD of a compound's response factor is 15% or less, then the concentration in the extract may be determined using the average response factor (RF) from initial calibration data (Sec. 7.3.5). See Method 8000, Sec. 7.0, for the equations describing internal standard calibration and eitherlinear or non-linearcalibrations.
7.7.3 Where applicable, the concentration of any non-targetanalytes identified in the sample (Sec. 7.6.2) should be estimated. The same formulae should be used with the following modifications: The areas

## Axand

## Asshould be from the total ion chromatograms, and the RF for the compound should be assumed to be 1.
7.7.4 The resulting concentration should be reported indicating: (1) that the value is an estimate, and (2) which internal standard was used to determine concentration. Use the nearest internal standard free of interferences.

CD-ROM 82700-21 Revision 4 January 19987.7.5 Quantitation ofmulticomponent compounds (e.g., Toxaphene, Aroclors, etc.) is beyond the scope of Method 8270. Normally, quantitation is performed using a GC/ECD, by Methods 8081 or 8082. However, Method 8270 may be used to confirm the identification of these compounds, when the concentrations are at least 10**ng/~L** in the concentrated sample extract.
7.7.6 Structural isomers that produce very similar mass spectra should be quantitated as individual isomers if they have sufficiently different GC retention times. Sufficient GCresolution is achieved if the height of the valley between two isomer peaks is less than 25% of the sum of the two peak heights. Otherwise, structural isomersare quantitated as isomeric pairs. Diastereomericpairs (e.g., Aramite and Isosafrol)that may be separable by the GC should be summed and reported as the sum of both compounds.

8.0 QUALITY CONTROL 8.1 Refer to Chapter One and Method 8000 for specific quality control (QC) procedures. Quality control procedures to ensure the proper operation of thevarioussample preparation and/or sample introductiontechniques can be found inMethod3500. Each laboratoryshould maintain a formal qualityassurance program. The laboratory should also maintain records to documentthe quality ofthedata generated. 8.2 Qualitycontrol procedures necessaryto evaluate the GC system operation are found in Sec. 7.0 of Method 8000 and include calibration verification and chromatographic analysis of samples. In addition, instrument QC requirements may be found in the following 'sections of Method 8270:

8.2.1 The GC/MSsystem must be tuned to meet the DFTPP criteria discussed in Sees. 7.3.1 and 7.4.1.

8.2.2 There mustbean initial calibration of the GC/MSsystem as described in Sec. 7.3.

8.2.3 The GC/MSsystem must meet the calibrationverification acceptance criteria in Sec. 7.4, each 12 hours. 8.2.4 The RRT of the sample component mustfall within the RRTwindow of the standard component provided in Sec. 7.6.1. 8.3 Initialdemonstrationof proficiency - Each laboratory must demonstrate initial proficiency with each sample preparation and determinativemethod combination it utilizes, bygenerating data of acceptable accuracy and precision for target analytes in adean matrix. The laboratory must also repeat the followinq operations whenever new staff are trained or significant changes in instrumentation are made. See Method 8000, Sec. 8.0 for information on how to accomplish this 

### demonstration.

8.4 Sample quality control for preparation and analysis - The laboratory must also have proceduresfor documenting the effect of the matrixon method performance (precision, accuracy, and detection limit). At a minimum, this includesthe analysis of QC samples including a method blank, matrix spike, a duplicate, and a laboratory control sample (LCS) in each analytical batch and the addition of surrogates to each field sample and QC sample.

CD-ROM 8270D - 22 Revision 4 January 19988.4.1 Before processing any samples, the analystshould demonstrate, through the analysis of a method blank, that interferences from the analytical system, glassware, and reagents are under control. Each time a set ofsamples is analyzed or there is a change in reagents, a method blank should be analyzed as a safeguard against chronic laboratory contamination. The blanks should be carried through all stages ofsample preparation and measurement.

8.4.2 Documenting the effect of the matrix should includethe analysis of at least one matrix spike and one duplicate unspiked sample or one matrix spike/matrixspike duplicate pair. The decision on whether to prepare and analyze duplicate samples or a matrix spike/matrix spike duplicate must be based on a knowledge of the samples in the sample batch. If samples are expected to contain target analytes, then laboratories may use one matrix spike and a duplicate analysis of an unspiked field sample. Ifsamples are notexpected to contain target analytes, laboratories should use a matrixspike and matrix spike duplicate pair.

8.4.3 A laboratory control sample (LCS) should be included with each analytical batch. The LCS consists of an aliquot of a clean (control) matrixsimilarto the sample matrix and of the same weight or volume. The LCS is spiked with the same analytes at the same concentrations as the matrixspike. When the results of the matrixspike analysis indicate a potential problem due to the sample matrix itself, the LCS results are used to verify that the laboratory can perform the analysis in a clean matrix.
8.4.4 See Method 8000, Sec. 8.0 for the details on carrying out sample quality control proceduresfor preparation and analysis.

8.5 Surrogate recoveries

- The laboratory must evaluate surrogate recovery data from individual samples versus the surrogate control limits developed by the laboratory. See Method 8000, Sec. 8.0 for information on evaluating surrogate data and developing and updating surrogate limits.8.6 The experience of the analyst performing GC/MS analyses is invaluableto the success of the methods. Each day that analysis is performed, the calibration verification standard should be evaluated to determine if the chromatographic system is operating properly. Questionsthat should be asked are: Do the peaks look normal? Is the response obtained comparable to the response from previous calibrations? Careful examination of the standardchromatogram can indicatewhether the column is still performing acceptably, the injector is leaking, the injectorseptum needs replacing, etc. If any changes are made to the system (e.g., the column changed, aseptum is changed), see the guidance in Sec 8.2 of Method 8000 regarding whether recalibration of the system must take place.

8.7 It is recommended that the laboratory adopt additional quality assurance practices for use with this method. The specific practices that are mostproductive depend upon the needs of the laboratory and the nature of the samples. Whenever possible, the laboratory should analyze standard reference materials and participate in relevant performance evaluation studies.

9.0 METHOD PERFORMANCE

9.1 Method 8250 (the packed column version of Method 8270) was tested by 15 laboratories using organic-free reagent water, drinking water, surface water, and industrial wastewaters spiked at six concentrations ranging from 5 to 1,300 IJg/L. Single operatoraccuracy

CD-ROM 82700- 23 Revision 4 January 1998

### and precision, and method accuracy were found to be directly related tothe concentration ofthe analyte and essentially independent of the sample matrix. Linear equations te- describe these relationships arepresented 

### inTable 7. These values are presented as guidance only and are not intended as absolute acceptance criteria. Laboratories should generate their own acceptance criteria for capillary column method performance... (SeeMethod 8000.)

9.2 Chromatogramsfrom calibration standards analyzed with Day 0 and Day 7 samples were compared to detect possible deterioration of GC performance. These recoveries (using Method 3510 extraction) are presented in Table 8. 9.3 Method performance data using Method 3541 (automated Soxhlet extraction) are presented in Table 9. Single laboratory accuracy and precision data were obtained for semivolatile organics in a clay soil by spiking at a concentration of 6 mg/kg for each compound. The spiking solution was mixed into the soif during addition and then allowed to equilibrate for approximately 1 hour prior to extraction. The spiked samples were then extracted by Method 3541 (Automated Soxhlet). Three extractions were performed and each extract was analyzed by gas chromatography/mass spectrometry following Method 8270. The low recovery of the more volatile compounds is probably due to volatilization losses during equilibration. These data are listed in Table 10 and were taken from Reference 7. 9.4 Surrogateprecision and accuracy data are presented in Table 11 from a field dynamic spiking study based on airsampling by Method 0010. The trapping mediawere prepared for analysis by Method 3542 and subsequently analyzed by Method 8270.

9.5 Single laboratory precision and bias data using Method 3545 (pressurized fluid extraction) for semivolatile organic compounds are presented in Table 12. The samples were conditioned spiked samples prepared and certified by a commercial supplierthat contained 57 semivolatile organics at three concentrations (250, 2500, and 12,500 IJg/kg) on three types of soil (clay, loam and sand). Spiked sampleswere extracted both by the DionexAccelerated Solvent Extraction system and by the Perstorp Environmental SoxtecTM (automated Soxhlet). The data in Table 12 representseven replicate extractions and analyses for each individual sample and were taken from reference 9. The average recoveriesfrom the three matrices for all analytes and all replicates relative to the automated Soxhlet data are asfoUows: clay96.8%, loam 98.7% and sand 102.1%. The average recoveries from the three concentrations also relative to the automated Soxhlet data are as follows: low-101.2%, mid-97.2% and high-99.2%. 9.6 Single laboratoryprecision and bias data usingMethod 3561 (SFE extraction of PAHs with avariable restrictor and solid trapping material) were obtained for the method analytes by the extraction of two certified referencematerials( EC-1, a lake sediment from Environment Canada and HS-3, a marine sedimentfrom the National Science and Engineering Research Council of Canada, both naturally-contaminated with PAHs). The SFE instrument used for these extractions was a Hewlett-Packard Model 7680. Analysis was by GC/MS. Average recoveries from six replicate extractions range from 85 to 148% (overall average of 100%) based on the certified value (or a Soxhlet value if a certified value was unavailable for a specific analyte) for the lake sediment. Average recoveries from threereplicateextractions range from 73 to 133% (overall average of 92%) based on the certified value for the marine sediment. The data are found in Tables 13 and 14 and were taken from Reference 10. 9.7 Single laboratory precision and accuracy data using Method 3561 (SFE extraction of PAHs with afixed restrictor and liquid trapping) were obtained for twelve of the method analytes by the extraction of a certified reference material (a soil naturallycontaminated with PAHs). The SFE instrument used for these extractions was a Dionex Model 703-M. Analysis was by GC/MS.

CD-ROM 8270D

- 24 Revision 4 January 1998Average recoveriesfrom four replicate extractions range from 60 to 122% (overall average of 89%) based on the certifiedvalue. Following are the instrumentconditionsthatwere utilized to extract a 3.4 g sample: Pressure - 300 atm; Time

- 60 min.; Extraction fluid - CO2; Modifier- 10% 1:1 (v/v) methanol/methylene chloride; Oven temperature

- 80°C; Restrictor temperature

- 120°C; and, Trapping fluid - chloroform (methylene chloride has also been used). The data are found in Table 15 and were taken from Reference 11. 9.8 Tables 16 and 17 contain single-laboratory precision and accuracy data for solid-phase extraction of TCLP buffersolutions spiked at two levels and extracted using Method 3535.

9.9 Table 18 contains multiple-laboratory data forsolid-phase extraction ofspiked TCLP soil leachates extracted using Method 3535.

10.0 REFERENCES

1. Eichelberger, J.W., Harris, L.E., and Budde, W.L., "Reference Compound to Calibrate Ion Abundance Measurement in Gas Chromatography-Mass Spectrometry Systems", Analytical Chemistry, 47, 995-1000, 1975. 2. "Method Detection Limit for Methods 624 and 625", Olynyk, P., Budde, W.L., and Eichelberger, J.W., unpublished report, October 1980.

. 3. "Interlaboratory Method Study for EPA Method 625-Base/Neutrals, Acids, and Pesticides", Final Reportfor EPA Contract68-03-3102.
4. Burke,JA, "Gas Chromatographyfor Pesticide Residue Analysis: Some Practical Aspects", Journal of the Association of Official Analytical Chemists (AOAC), 48, 1037, 1965.
5. Lucas, S.v., Kornfeld, 

### RA., "GC-MS SuitabilityTesting of RCRAAppendixVIII and Michigan List Analytes ", U.S. Environmental ProtectionAgency, Environmental Monitoring and Support Laboratory, Cincinnati, OH 45268, February20, 1987, Contract No. 68-03-3224.

6. Engel, T.M., Kornfeld, 

### RA., Warner, J.S., and Andrews, K.D., "Screening of Semivolatile OrganicCompoundsfor Extractability and Aqueous Stability by SW-846, Method 3510", U.S. Environmental Protection Agency, Environmental Monitoring and Support Laboratory, Cincinnati, OH 45268, June 5, 1987, Contract 68-03-3224.
7. Lopez-Avila, V. (W. Beckert, Project Officer); "Development of a Soxtec Extraction Procedure for Extraction of Organic Compounds from Soils and Sediments"; U.S. Environmental Protection Agency, Environmental Monitoring and Support Laboratory, Las Vegas, NV, October 1991; EPA 600/X-91/140.
8. Bursey, J., Merrill, 

### R, McAllister, 

### R, and McGaughey, J., "LaboratoryValidation ofVOST and SemiVOST for Halogenated Hydrocarbonsfrom the Clean Air Act Amendments List", Vol. 1 and 2, U.S. Environmental Protection Agency, EPA 600/R-93/123a and b, (NTIS PB 93-227163 and 93-27171), Research Triangle Park, NC, July 1993.
9. Richter, B., Ezzell, J., and Felix, D., "Single Laboratory Method Validation Report: Extraction of Target Compound List/Priority Pollutant List BNAs and Pesticides using Accelerated Solvent Extraction (ASE) with Analytical Validation by GC/MS and GC/ECD", Document 101124, Dionex Corporation, Salt Lake City, UT, June 16, 1994.

CD-ROM 8270D - 25 Revision 4 January 199810. Lee, H.B., Peart, T.E., Hong-You, R.L., and Gere, D.R., "Supercritical Carbon Dioxide Extraction of PolycyclicAromatic Hydrocarbonsfrom Sediments", J. Chromatography, A 653 83-91 (1993).

11. Warner, S., "SFE Extraction of PNAs from Solid Matrices Using the Dionex 703M SFE Extractor and a Liquid Trap," EPA Region III, Central Regional Laboratory, 839 BestgateRoad, Annapolis, MD 21401, December 12,1994.
12. Markell, C., "3M Data Submission to EPA," letter to B. Lesnik, June 27, 1995.

CD-ROM 8270D - 26 Revision 4 January 1998TABLE 1
CHARACTERISTIC IONS FOR SEMIVOLATILE COMPOUNDS

Compound 2-Picoline Aniline

. Phenol

Bis(2-chloroethyl) ether 2-Chlorophenol 1,3-Dichlorobenzene 1,4-Dichlorobenzene-d4 (IS) 1,4-Dichlorobenzene Benzyl alcohol 1,2-Dichlorobenzene N-Nitrosomethylethylamine Bis(2-chloroisopropyl) ether Ethyl carbamate Thiophenol (Benzenethiol) Methyl methanesulfonate N-Nitrosodi-n-propylamine Hexachloroethane Maleic anhydride Nitrobenzene Isophorone N-Nitrosodiethylamine 2-Nitrophenol 2,4-Dimethylphenol p-Benzoquinone Bis(2-chloroethoxy)methane Benzoic acid 2,4-Dichlorophenol Trimethyl phosphate Ethyl methanesulfonate 1,2,4-Trichlorobenzene Naphthalene-d, (IS) Naphthalene Hexachlorobutadiene Tetraethyl pyrophosphate Diethyl sulfate 4-Chloro-3-methylphenol 2-Methylnaphthalene 2-Methyl phenol Hexachloropropene Hexachlorocyclopentadiene N-Nitrosopyrrolidine Acetophenone

CD-ROM Retention Primary Time (min) Ion 3.758 93 5.68 93 5.77 94 5.82 93 5.97 128 6.27 146 6.35 152 6.40 146 6.78 108 6.85 146 6.97 88 7.22 45 7.27 62 7.42 110 7.48 80 7.55 70 7.65 117 7.6554 7.87 77 8.53 82 8.70 102 8.75 139 9.03 122 9.13 108 9.23 93 9.38 122 9.48 162 9.53 110 9.62 79 9.67 180 9.75 136 9.82 128 10.43 225 11.07 99 11.37 139 

### 11.68 107 11.87 142 12.40 107 12.45 213 12.60 237 12.65 100 12.67 105

82700

- 27 Secondary lon(s)

66,92 66,65 65,66 63,95 64,130 148,111 150,115 148,111 79,77 148,111 42,43,56 77,121 44,45,74 66,109,84 79,65,95 42,101,130 201,199 98,53,44 123,65 95,138 42,57,44,56 109,65 107,121 54,82,80 95,123 105,77 164,98 79,95,109,140 109,97,45,65 182,145 68 129,127 223,227 155,127,81,109 45,59,99,111,125 144,142 141 108,77,79,90 211,215,117,106,141 235,272 41,42,68,69 71,51,120

Revision 4 January 1998

### Compound 4-Methylphenol 

### 2A,6-Trichlorophenol o-Toluidine 3-Methylphenol 2-Chloronaphthalene N-Nitrosopiperidine 1

### A-Phenylenediamine 1-Chloronaphthalene 2-Nitroaniline 5-Chloro-2-methylaniline Dimethyl phthalate Acenaphthylene 2,6-Dinitrotoluene Phthalic anhydride o-Anisidine 3-Nitroaniline Acenaphthene-d., (IS) Acenaphthene 2,4-Dinitrophenol 2,6-Dinitrophenol 4-Chloroaniline lsosafrole Dibenzofuran 2A-Diaminotoluene 2A-Dinitrotoluene 4-Nitrophenol 2-Naphthylamine 1A-Naphthoquinone p-Cresidine Dichlorovos Diethyl phthalate Fluorene 2,4,5-Trimethylaniline N-Nitrosodi-n-butylamine 4-Chlorophenyl phenyl ether Hydroquinone 4,6-Dinitro-2-methylphenol Resorcinol N-Nitrosodiphenylamine Safrole Hexamethyl phosphoramide 3-(Chloromethyl)pyridine hydrochloride Diphenylamine

CD-'ROM TABLE 1 (continued)
Retention Primary Time (min) Ion 12.82 107 12.85 196 12.87 106 12.93 107 13.30 162 13.55 114 13.62 108 13.65a 

### 162 13.75 65 14.28 106 14.48 163 14.57 152 14.62 165 14.62 104 15.00 108 15.02 138 15.05 164 15.13 154 15.35 184 15.47 162 15.50 127 15.60 162 15.63 168 15.78 121 15.80 165 15.80 139 16.00a 

### 143 16.23 158 16.45 122 16.48 109 16.70 149 16.70 166 16.70 120 16.73 84 16.78 204 16.93 110 17.05 198 17.13 110 17.17 169 17.23 162 17.33 135 17.50 92 17.54a 

### 169

8270D - 28 Secondary lon(s)

108,77,79,90 198,200 107,77,51,79 108,77,79,90 127,164 42,55,56,41 80,53,54,52 127,164 92,138 141,140,77,89 194,164 151,153 63,89 76,50,148 80,123,52 108,92 162,160 153,152 63,154 164,126,98,63 129,65,92 131,104,77,51 139 122,94,77,104 63,89 109,65 115,116 104,102,76,50,130 94,137,77,93 185,79,145 177,150 165,167 135,134,91,77 57,41,116,158 206,141 81,53,55 51,105 81,82,53,69 168,167 104,77,103,135 44,179,92,42 127,129,65,39 168,167

Revision 4 January 1998TABLE 1 (continued)

Retention Primary Secondary lon(s) Compound Time (min) Ion 1,2,4,5-Tetrachlorobenzene 17.97 216 214,179,108,143,218 1-Naphthylamine 18.20 143 115,89,63 1-Acetyl-2-thiourea 18.22 118 43,42,76 4-Bromophenyl phenyl ether 18.27 248 250,141 Toluene diisocyanate 18.42 174 145,173,146,132,91 2,4,5-Trichlorophenol 18.47 196 198,97,132,99 Hexach!orobenzene 18.65 284 142,249 Nicotine 18.70 84 133,161,162 Pentachlorophenol 19.25 266 264,268 5-Nitro-o-toluidine 19.27 152 77,79,106,94 Thionazine 19.35 107 96,97,143,79,68 4-Nitroaniline 19.37 138 65,108,92,80,39 Phenanthrene-d.; (IS) 19.55 188 94,80 Phenanthrene 19.62 178 179,176 Anthracene 19.77 178 176,179 1,4-Dinitrobenzene 19.83 168 75,50,76,92,122 Mevinphos 19.90 127 192,109,67,164 Naled 20.03 109 145,147,301,79,189 1,3-Dinitrobenzene 20.18 168 76,50,75,92,122 Diallate (cis or trans) 20.57 86 234,43,70 1,2-Dinitrobenzene 20.58 168 50,63,74 Diallate (trans or cis) 20.78 86 234,43,70 Pentachlorobenzene 21.35 250 252,108,248,215,254 5-Nitro-o-anisidine 21.50 168 79,52,138,153,77 Pentachloronitrobenzene 21.72 237 142,214,249,295,265 4-Nitroquinoline-1-oxide 21.73 174 101,128,75,116 Di-n-butyl phthalate 21.78 149 150,104 2,3,4,6-Tetrachlorophenol 21.88 232 131,230,166,234,168 Dihydrosaffrole 22.42 135 64,77 Demeton-O 22.72 88 89,60,61,115,171 Fluoranthene 23.33 202 101,203 1,3,5-Trinitrobenzene 23.68 75 74,213,120,91,63 Dicrotophos 23.82 127 67,72,109,193,237 Benzidine 23.87 184 92,185 Trifluralin 23.88 306 43,264,41,290 Bromoxynil 23.90 277 279,88,275,168 Pyrene 24.02 202 200,203 Monocrotophos 24.08 127 192,67,97,109 Phorate 24.10 75 121,97,93,260 Sulfallate 24.23 188 88,72,60,44 Demeton-S 24.30 88 60,81,89,114,115 Phenacetin 24.33 108 180,179,109,137,80 Dimethoate 24.70 87 93,125,143,229

CD-ROM 8270D

- 29 Revision 4 January 1998TABLE 1 (continued)

Retention Primary Secondary lanes) Compound Time (min) Ion Phenobarbital 24.70 204 117,232,146,161 Carbofuran 24.90 164 149,131,122 Octamethyl pyrophosphoramide 24.95 135 44,199,286,153,243 4-Aminobiphenyl 25.08 169 168,170,115 Dioxathion 25.25 97 125,270,153 Terbufos 25.35 231 57,97,153,103

rt rY_niml"thvlnhl"nvl:::lminl" 25.43 58 Q1 RI:\ 1**~LI.** LI.? -'0,

........

_ ....- .... ",J"r"""-' 'J ._•• ,•••-

.... • ,--, "'-.'J .- Pronamide 25.48 173 175,145,109,147 Aminoazobenzene 25.72 197 92,120,65,77 Dichlone 25.77 191 163,226,228,135,193 Dinoseb 25.83 211 163,147,117,240 Disulfoton 25.83 88 97,89,142,186 Fluchloralin 25.88 306 63,326,328,264,65 Mexacarbate 26.02 165 150,134,164,222 4,4'-Oxydianiline 26.08 200 108,171,80,65 Butyl benzyl phthalate 26.43 149 91,206 4-Nitrobiphenyl 26.55 199 152,141,169,151 Phosphamidon 26.85 127 264,72,109,138 2-Cyclohexyl-4,6-Dinitrophenol 26.87 231 185,41,193,266 Methyl parathion 27.03 109 125,263,79,93 Carbaryl 27.17 144 115,116;201 Dimethylaminoazobenzene 27.50 225 120,77,105,148,42 Propylthiouracil 27.68 170 142,114,83 Benz(a)anthracene 27.83 228 229,226 Chrysene-d., (IS) 27.88 240 120,236 3,3'-Dichlorobenzidine 27.88 252 254,126 Chrysene 27.97 228 226,229 Malathion 28.08 173 125,127,93,158 Kepone 28.18 272 274,237,178,143,270 Fenthion 28.37 278 125,109,169,153 Parathion 28.40 109 97,291,139,155 Anilazine 28.47 239 241,143,178,89 Bis(2-ethylhexyl) phthalate 28.47 149 167,279 3,3'-Dimethylbenzidine 28.55 212 106,196,180 Carbophenothion 28.58 157 97,121,342,159,199 5-Nitroacenaphthene 28.73 199 152,169,141,115 Methapyrilene 28.77 97 50,191,71 Isodrin 28.95 193 66,195,263,265,147 Captan 29.47 79 149,77,119,117 Chlorfenvinphos 29.53 267 269,323,325,295 Crotoxyphos 29.73 127 105,193,166 Phosmet 30.03 160 77,93,317,76 EPN 30.11 157 169,185,141,323

CD-ROM 8270D - 30 Revision4 January 1998TABLE 1 (continued)

Retention Primary Secondary lon(s) Compound Time (min) Ion Tetrachlorvinphos 30.27 329 109,331,79,333 Di-n-octyl phthalate 30.48 149 167,43 2-Aminoanthraquinone 30.63 223 167,195 Barban 30.83 222 51,87,224,257,153 Aramite 30.92 185 191,319,334,197,321 Benzo(b)fluoranthene 31.45 252 253,125 Nitrofen 31.48 283 285,202,139,253 Benzo(k)fluoranthene 31.55 252 253,125 Chlorobenzilate 31.77 251 139,253,111,141 Fensulfothion 31.87 293 97,308,125,292 Ethion 32.08 231 97,153,125,121 Diethylstilbestrol 32.15 268 145,107,239,121,159 Famphur 32.67 218 125,93,109,217 Tri-p-tolyl phosphate" 32.75 368 367,107,165,198 Benzo(a)pyrene 32.80 252 253,125 Perylene-d., (IS) 33.05 264 260,265 7,12-Dimethylbenz(a)anthracene 33.25 256 241,239,120 5,5-Diphenylhydantoin 33.40 180 104,252,223,209 Captafol 33.47 79 77,80,107 Dinocap 33.47 69 41,39 Methoxychlor 33.55 227 228,152,114,274,212 2-Acetylaminofluorene 33.58 181 180,223,152 4,4'-Methylenebis(2-chloroaniline) 34.38 231 266,268,140,195 3,3'-Dimethoxybenzidine 34.47 244 201,229 3-Methylcholanthrene 35.07 268 252,253,126,134,113 Phosalone 35.23 182 184,367,121,379 Azinphos-methyl 35.25 160 132,93,104,105 Leptophos 35.28 171 377,375,77,155,379 Mirex 35.43 272 237,274,270,239,235 Tris(2,3-dibromopropyl) phosphate 35.68 201 137,119,217,219,199 Dibenz(a,j)acridine 36.40 279 280,277,250 Mestranol 36.48 277 310,174,147,242 Coumaphos 37.08 362 226,210,364,97,109 Indeno(1,2,3-cd)pyrene 39.52 276 138,227 Dibenz(a,h)anthracene 39.82 278 139,279 Benzo(g,h,i)perylene 41.43 276 138,277 1,2:4,5-Dibenzopyrene 41.60 302 151,150,300 Strychnine 45.15 334 334,335,333 Piperonyl sulfoxide 46.43 162 135,105,77 Hexachlorophene 47.98 196 198,209,211,406,408 Aldrin 66 263,220 Aroclor 1016 222 260,292 Aroclor 1221 190 224,260

CD-ROM 82700 - 31 Revision 4 January 1998Compound Aroclor 1232 Aroclor 1242 Aroclor 1248 Aroclor 1254 Aroclor 1260 a-SHC**~-BHC** a-BHC V-BHC (Lindane) 4,4'-DDD 4,4'-DDE 4,4'-DDT Dieldrin 1,2-Diphenylhydrazine Endosulfan I Endosulfan 

### 1\ Endosulfansulfate Endrin Endrin aldehyde Endrin ketone 2-Ftuorobiphenyl (surr) 2-Fluorophenol (surr) Heptachlor Heptachlor epoxide 

### Nitrobenzene-d, (surr) N-Nitrosodimethylamine Phencl-d, (surr) Terphenyl-d., (surr) 2,4,6-Tribromophenol (surr) Toxaphene TABLE 1 (continued)
Retention Primary Secondary lon(s) Time (min) Ion 190 224,260 222 256,292 292 362,326 292 362,326 360 362,394 183 181,109 181 183,109 183 181,109 183 181,109 235 237,165 246 248,176 235 237,165

79 263,279 77 105,182 195 339,341 337 339,341 272 387,422 263 82,81

67 345,250 317 67,319 172 171 112 64 100 272,274 353 355,351

82 128,54 42 74,44 99 42,71 244 122,212 330 332,141 159 231,233

IS 

# =internal standard surr

# =surrogate "Estimated retention times bSubstitute for the non-specific mixture, tricresyl phosphate

CD-ROM 8270D - 32 Revision 4 January 1998TABLE 2

ESTIMATED QUANTITATION LIMITS (EQLs) FOR SEMIVOLATILE ORGANICS

Estimated Quantitation Limits"
Compound Acenaphthene Acenaphthylene Acetophenone
1-Acetyl-2-thiourea 2-Aminoanthraquinone Aminoazobenzene 4-Aminobiphenyl Anilazine o-Anisidine Anthracene Aramite Azinphos-methyl Barban Benz(a)anthracene Benzo(b)fluoranthene Benzo(k)fluoranthene Benzoicacid Benzo(g,h,i)perylene Benzo(a)pyrene p-Benzoquinone Benzyl alcohol Bis(2-chloroethoxy)methane Bis(2-chloroethyl) ether Bis(2-chloroisopropyl) ether 4-Bromophenyl phenyl ether Bromoxynil Butyl benzyl phthalate Captafol Captan Carbaryl Carbofuran Carbophenothion Chlorfenvinphos 4-Chloroaniline Chlorobenzilate 5-Chloro-2-methylaniline

CD-ROM Ground water Low Soil/Sediment" (1-l9/L) (1-l9/kg) 10 660 10 660 10 NO ')n f\ln L..V 

## ........ 1000 NO 20 NO 10 NO 20 NO 100 NO

10 NO 10 660 20 NO 100 NO 200 NO

10 660 10 660 10 660 50 3300 10 660 10 660 10 NO 20 1300 10 660 10 660 10 660 10 660 10 NO 10 660 20 NO 50 NO
"1n f\ln IU 

## ........ 10 NO 10 NO 20 NO 20 1300 10 NO 10 NO

82700 - 33 Revision 4 January 1998Compound 4-Chloro-3-methylphenol 3-(Chloromethyl)pyridine hydrochloride 2-Chloronaphthalene 2-Chlorophenol 4-Chiorophenyi phenyl ether Chrysene Coumaphos p-Cresidine Crotoxyphos 2-Cyclohexyl-4,6-dinitrophenol Demeton-O Demeton-S Diallate (cis or trans) Diallate (trans or cis) 2A-Diaminotoluene Dibenz(a,j)acridine Dibenz(a,h)anthracene Dibenzofuran Dibenzo(a,e)pyrene Di-n-butyl phthalate Dichlone 1,2-Dichlorobenzene 1,3-Dichlorobenzene 1A-Dichlorobenzene 3,3'-Dichlorobenzidine 2A-Dichlorophenol 2,6-Dichlorophenol Dichlorovos Dicrotophos Diethy! phthalate Diethylstilbestrol Diethyi sulfate Dimethoate 3,3'-Dimethoxybenzidine Dimethylaminoazobenzene 7,12-Dimethy!benz(a)anthracene 3,3'-Dimethylbenzidine 2A-Dimethylphenol

CD"ROM TABLE 2 (Continued)

Estimated Quantitation Limits" Ground water Low Soil/Sediment" 

### (1-l9/L) (1-l9/kg) 20 1300 100 ND

10 660 10 660 '10 

### 660 10 660 40 ND 10 ND 20 ND 100 ND

10 ND 10 ND 10 ND 10 ND 20 ND 10 ND 10 660 10 660 10 ND 10 ND NA ND 10 660 10 660 10 660 20 1300 10 660 10 ND 10 NO '10 NO 10 660 20 ND 

### 100 ND

20 ND 100 ND

10 NO 10 ND 10 ND 10 660

8270D -34 Revision 4 January 1998Compound Dimethyl phthalate 1,2-Dinitrobenzene 1,3-Dinitrobenzene 1A-Dinitrobenzene 4,6-Dinitro-2-methyiphenoi 2A-Dinitrophenol 2,4-Dinitrotoluene 2,6-Dinitrotoluene Dinocap Dinoseb 5,S-Diphenylhydantoin Di-n-cetyl phthalate Disulfoton EPN Ethion Ethyl carbamate Bis(2-ethylhexyl) phthalate Ethyl methanesulfonate Famphur Fensulfothion Fenthion Fluchloralin Fluoranthene Fluorene Hexachlorobenzene Hexachlorobutadiene Hexachlorocyclopentadiene Hexachloroethane Hexachlorophene Hexachloropropene Hexamethylphosphoramide indeno(1,2,3-cd)pyrene Isodrin Isophorone Isosafrole Kepone Leptophos Malathion

CD-ROM TABLE 2 (Continued)

Estimated Quantitation Limits" Ground water Low Soil/Sediment" (lJg/L) (1J9/kg) 10 660 40 ND 20 ND 40 ND

rr rv "'-""'Inn OU ,),)UU 50 3300 10 660 10 660 100 ND

20 ND 20 ND 10 660 10 ND 10 ND 10 ND 50 ND 10 660 20 ND 20 ND 40 ND 10 ND 20 ND 10 660 10 660 10 660 10 660 10 660 10 660 50 ND 10 ND 20 ND 10 660 20 ND 10 660 10 ND 20 ND 10 ND 50 ND

8270D - 35 Revision 4 January 1998Compound Mestranol Methapyrilene Methoxychlor 3-Methylcholanthrene Methyl methanesuifonate 2-Methylnaphthalene Methyl parathion 2-Methylphenol 3-Methylphenol 4-Methylphenol Mevinphos Mexacarbate Mirex Monocrotophos Naled Naphthalene 1A-Naphthoquinone 1-Naphthylamine 2-Naphthylamine Nicotine 5-Nitroacenaphthene 2-Nitroaniline 3-Nitroaniline 4-Nitroanifine 5-Nitro-o-anisidine Nitrobenzene 4-Nitrobiphenyl Nitrofen 2-Nitrophenol 4-Nitrophenol 5-Nitro-o-toluidine 4-Nitroquinoiine-1-oxide N-Nitrosodi-n-butylamine N-Nitrosodiethylamine N-Nitrosodiphenylamine N-Nitroso-di-n-propylamine N-Nitrosopiperidine N-Nitrosopyrrolidine

CD-ROM TABLE 2 (Continued)

Estimated Quantitation Limits" Ground water Low Soil/Sediment" (lJg/L) (lJg/kg) 20 NO 100 NO

10 NO 10 NO 10 ND 10 660 10 NO 10 660 10 NO 10 660 10 NO 20 NO 10 NO 40 NO 20 

### ND 10 660 10 NO 10 NO 10 NO 20 NO 10 NO 50 3300 50 3300 20 NO 10 NO 10 660 10 NO 20 NO 10 660 50 3300 10 NO 40 ND 10 NO 20 NO 10 660 10 660 20 NO 40 NO

82700- 36 Revision 4 J.anuary 1998Compound actamethyl pyrophosphoramide 4,4'-Oxydianiline Parathion Pentachlorobenzene Pentachioronitrobenzene Pentachlorophenol Phenacetin Phenanthrene Phenobarbital Phenol 1,4-Phenylenediamine Phorate Phosalone Phosmet Phosphamidon Phthalic anhydride 2-Picoline Piperonyl sulfoxide Pronamide Propylthiouracil Pyrene Resorcinol Safrole Strychnine Sulfallate Terbufos 1,2,4,5-Tetrachlorobenzene 2,3,4,6-Tetrachlorophenol Tetrachlorvinphos Tetraethyl pyrophosphate Thionazine Thiophenoi (Benzenethioi) o-Toluidine 1,2,4-Trichlorobenzene 2,4,5-Trichlorophenol 2,4,6-Trichlorophenol Trifluralin 2,4,5-Trimethylaniline

CD-ROM TABLE 2 (Continued)

Estimated Quantitation Limits" Ground water Low Soil/Sediment'' (lJg/L) (lJg/kg) 200 

### NO

20 

### NO 10 

### NO 10 

### NO 20 ND 50 3300 20 

### NO 10 660 10 

### NO 10 660 10 

### NO 10 

### NO 100 

### NO

40 

### NO 100 

### NO 100 

### NO NO NO 100 

### NO

10 

### NO 100 

### NO

10 660 100 

### NO

10 

### NO 40 

### NO 10 

### NO 20 

### NO 10 

### NO 10 

### NO 20 

### NO 40 

### NO 20 

### NO 20 NO 10 

### NO 10 660 10 660 10 660 10 

### NO 10 

### NO

82700- 37 Revision 4 January 1998TABLE 2 (Continued)

Estimated Quantitation Limits"
Compound Ground water Low Soil/Sediment" (!Jg/ 

### L) (!Jg/kg) Trimethyl phosphate 1,3,5-Trinitrobenzene Tris(2,3-dibromopropyl) phosphate Tri-p

..:tolyl phosphate(h) 10 10 200

10 

### NO NO NO NO

a Sample EQLs arehighly matrix-dependent. The EQLs listed here are provided for guidance and

may not always be achievable.

b EQLs listed for soil/sediment are based on wet weight. Normally, data are reported on a dry

weight basis, therefore, EQLs will be higherbased on the 

### % dryweightof each sample. These EQLs are based on a30-g sample and gel permeation chromatography cleanup.


### NO 

# = Not Determined

NA 

# = NotApplicable

OtherMatrices High-concentration soil and sludges by ultrasonicextractor Non-watermisciblewaste
CEQL

# =(EQLfor Low Soil/Sedimentgiven above inTable 2) x (Factor) Factor

7.5 75

CD·HOM 82700- 38 Revision

### 4 January 1998TABLE 3
DFTPP KEY IONS AND IONABUNDANCE CRITERIAa,b

Mass IonAbundance Criteria 51 30-60% of mass 198
68 < 2% ofmass 69
70 < 2% of mass 69
127 40-60% of mass 198

-107 <' -10/.. ,...f rY'\-:>c-c- -10Q 1-.;;..11

.... I IU VI 1II00vv I \JU 198 Base peak, 100% relative abundance
199 5-9% of mass 198
275 10-30% of mass 198
365 > 1% of mass 198
441 Present but less than mass 443
442 >40% of mass 198
443 17-23% of mass 442

a Data taken from Reference 3. b Alternate tuning criteria may be employed,

(e.g., CLP, Method 525, or manufacturers' instructions), provided that method performance is not adversely affected.

TABLE4

CALIBRATION CHECK COMPOUNDS (CCC)

CD-ROM Base/Neutral Fraction Acenaphthene 1,4-Dichlorobenzene Hexachlorobutadiene Diphenylamine Di-n-octyl phthalate Fluoranthene Benzo(a)pyrene Acid Fraction 4-Chloro-3-methylphenol 2,4-Dichlorophenol 2-Nitrophenol Phenol Pentachlorophen

### 01 2,4,6-Trichlorophenol

82700- 39 Revision 4 January 1998TABLE 5
SEMIVOLA TILE INTERNAL STANDARDS WITH CORRESPONDINGANALYTES ASSIGNED FOR QUANTITATION

1,4-Dichlorobenzene-d4 Aniiine Benzyl alcohol Bis(2-chloroethyl) ether Bis(2-chloroisopropyl) ether 2-Chlorophenol 1,3-Dichlorobenzene 1,4-Dichlorobenzene 1,2-Dichlorobenzene Ethyl methanesulfonate 2-Fluorophenol (surr) Hexachloroethane Methyl methanesulfonate 2-Methylphenol 4-Methylphenol N-Nitrosodimethylamine N-Nitroso-di-n-propylamine Phenol Phenol-d, (surr) 2-Picoline

(surr)

# =surrogate

CD-ROM Naphthalene-d, Acetophenone Benzoicacid Bis(2-chloroethoxy)methane 4-Chloroaniline 4-Chloro-3-methylphenol 2,4-Dichlorophenol 2,6-Dichlorophenola,a-Dimethylphenethylamine 2,4-Dimethylphenol Hexachlorobutadiene Isophorone 2-Methylnaphthalene Naphthalene Nitrobenzene Nitrobenzene-d, (surr) 2-Nitrophenol N-Nitrosodi-n-butylamine N-Nitrosopiperidine 1,2,4-Trichlorobenzene

8270D - 40 Acenaphthene-d., Acenaphthene Acenaphthylene 1-Chloronaphthalene 2-Chloronaphthalene 4-Chlorophenyl phenyl ether Dibenzofuran Diethyl phthalate Dimethyl phthalate 2,4-Dinitrophenol 2,4-Dinitrotoluene 2,6-Dinitrotoluene Fluorene 2-Fluorobiphenyl (surr) Hexachlorocyclopentadiene 1-Naphthylamine 2-Naphthylamine 2-Nitroaniline 3-Nitroaniline 4-Nitroaniline 4-Nitrophenol Pentachlorobenzene 1,2,4,5-Tetrachlorobenzene 2,3,4,6-Tetrachlorophenol 2,4,6-Tribromophenol (surr) 2,4,6-Trichlorophenol 2,4,5-Trichlorophenol

Revision 4 January 1998TABLE 5 (continued)

Phenanthrene-d., Chrysene-d., 4-Aminobiphenyl Benzidine
Anthracene Benzo(a)anthracene 4-Bromophenyl phenyl ether Bis(2-ethylhexyl) phthalate Di-n-butyl phthalate Butyl benzyl phthalate 4,6-Dinitro-2-methylphenol Chrysene Diphenylamine 3,3'-Dichlorobenzidine Perylene-d., Benzo(b)fluoranthene Benzo(k)fluoranthene Benzo(g,h,i)perylene Benzo(a)pyrene Dibenz(a,j)acridine Dibenz(a,h)anthracene
Fluoranthene
Hexachlorobenzene N-Nitrosodiphenylamine
Pentachlorophenol

Pentachloronitrobenzene
Phenacetin
Phenanthrene
Pronamide

(surr)

## =surrogate

CD-ROM p-Dimethyl aminoazobenzene Pyrene Terphenyl-d., (surr) 7,12-Dimethylbenz(a) anthracene Di-n-cetyl phthalate Indeno(1,2,3-cd) pyrene 3-Methylcholanthrene

82700 - 41 Revision 4 January 1998TABLE 6
MULTILABORATORY PERFORMANCE DATN

Test cone. Limit for Range for x Range Compound (lJg/L) s (lJg/L) (lJg/L) p, ps(%) Acenaphthene 100 27.6 60.1-132.3 47-145 Acenaphthylene 100 40.2 53.5-126.0 33-145 Aldrin 100 39.0 7.2-152.2 0-166 Anthracene 100 32.0 43.4-118.0 27-133 Benz(a)anthracene 100 27.6 41.8-133.0 33-143 Benzo(b}fluoranthene 100 38.8 42.0-140.4 24-159 Benzo(k}fluoranthene 100 32.3 25.2-145.7 11-162 Benzo(a)pyrene 100 39.0 31.7-148.0 17-163 Benzo(g,h,i)perylene 100 58.9 0-195.0 0-219 Benzyl butyl phthalate 100 23.4 0-139.9 0-152 f3-BHC 100 31.5 41.5-130.6 24-149 a-BHC 100 21.6 0-100.0 0-110 Bis(2-chloroethyl) ether 100 55.0 42.9-126.0 12-158 Bis(2-chloroethoxy)methane 100 34.5 49.2-164.7 33-184 Bis(2-chloroisopropyl) ether 100 46.3 62.8-138.6 36-166 Bis(2-ethylhexyl) phthalate 100 41.1 28.9-136.8 8-158 4-Bromophenyl phenyl ether 100 23.0 64.9-114.4 53-127 2-Chloronaphthalene 100 13.0 64.5-113.5 60-118 4-Chlorophenyl phenyl ether 100 33.4 38.4-144.7 25-158 Chrysene 100 48.3 44.1-139.9 17-168 4A'-DDD 100 31.0 0-134.5 0-145 4,4'-DDE 100 32.0 19.2-119.7 4-136 

### 4A'-DDT 100 61.6 0-170.6 0-203 Dibenzo(a,h)anthracene 100 70.0 0-199.7 0-227 DI-n-butyl phthalate 100 16.7 8.4-111.0 1-118 1,2-Dichlorobenzene 100 30.9 48.6-112.0 32-129 1,3-Dichlorobenzene 100 41.7 16.7-153.9 0-172 1A-Dichlorobenzene 100 32.1 37.3-105.7 20-124 3,3'-Dichlorobenzidine 100 71.4 8.2-212.5 0-262 Dieldrin 100 30.7 44.3-119.3 29-136 Diethyl phthalate 100 26.5 0-100.0 0-114 Dimethyl phthalate 100 

### 23.2 0-100.0 0-112 2A-Dinitrotoluene 100 21.8 47.5-126.9 39-139 2,6-0initrotoluene 100 29.6 68.1-136.7 50-158 Di-n-cetyl phthalate 100 31.4 18.6-131.8 4-146 Endosulfan sulfate 100 16.7 0-103.5 0-107 Endrin aldehyde 100 32.5 0-188.8 0-209 Fluoranthene 100 32.8 42.9-121.3 26-137

CD-ROM 82700

-42 Revision 4 January 1998TABLE 6 C continued)

Compound Fluorene Heptachlor Heptachlorepoxide Hexachlorobenzene Hexachlorobutadiene Hexachloroethane Indeno(1,2,3-cd)pyrene Isophorone Naphthalene Nitrobenzene N-Nitrosodi-n-propylamine Arocior 1260 Phenanthrene Pyrene 1,2,4-Trichlorobenzene 4-Chloro-3-methylphenol 2-Chlorophenol 2,4-Chlorophenol 2,4-0imethylphenol 2,4-0initrophenol 2-Methyl-4,6-dinitrophenol 2-Nitrophenol 4-Nitrophenol Pentachlorophenol Phenol 2,4,6-Trichlorophenol Testcone. ClJg/L)

100 100 100 100 100 100 

### 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 Limit for s ClJg/L) 20.7 37.2 54.7 24.9 26.3 24.5 44.6 63.3 30.1 39.3 55.4 54.2 20.6 25.2 28.1 37.2 28.7 26.4 26.1 49.8 93.2 35.2 47.2 48.9 22.6 31.7 Range for x ClJg/L) 71.6-108.4 0-172.2 70.9-109.4

7.8-141.5 37.8-102.2 55.2-100.0 0-150.9 46.6-180.2 35.6-119.6 54.3-157.6 13.6-197.9 19.3-121.0 65.2-108.7 69.6-100.0 57.3-129.2 40.8-127.9 36.2-120.4 52.5-121.7 41.8-109.0 0-172.9 53.0-100.0 45.0-166.7 13.0-106.5 38.1-151.8 16.6-100.0 52.4-129.2 Range

p, pS(%) 59-121

0-192 26.155

0-152 24-116 40-113

0-171 21-196 21-133 35-180

0-230 0-164 54-120 52-115 44-142 22-147 23-134 39-135 32-119

0-191 0-181 29-182

0-132 14-176

5-112

.37-144

s 

## = Standard deviation of four recovery measurements, in IJg/L

-x 

# = Average recovery for four recovery measurements, in IJg/L

p, 

### Ps

# = Measured percent recovery
D

a Criteria from 40 CFR Part 136 for Method 625, using a packed GC column. These criteria are based directly on the method performance data in Table 7. Where necessary, the limits for recovery have been broadened to assure applicability of the limits to concentrations below those used to develop Table 7. These values are for guidance only. Appropriate derivation of acceptance criteria for capillary columns should result in much narrower ranges. See Method 8000 for information on developing and updating acceptance criteria for method performance.

CO-ROM 82700 - 43 Revision 4 January 1998TABLE 7
METHODACCURACYAND PRECISION AS FUNCTIONS OF CONCENTRATIONa

Compound Acenaphthene Acenaphthylene Aldrin Anthracene Benz(a)anthracene Benzo(b)fluoranthene Benzo(k)fluoranthene Benzo(a)pyrene Benzo(g,h,i)perylene Benzyl butyl phthalate**~-BHC** B-BHC Bis(2-chloroethyl) ether Bis(2-chloroethoxy}methane Bis(2-chloroisopropyl) ether Bis(2-ethylhexyl) phthalate 4-Bromophenyl phenyl ether 2-Chloronaphthalene 4-Chlorophenyl phenyl ether Chrysene 4A'-DDD 4,4'-DDE 4A'-DDT Dibenzo{a,h}anthracene Di-n-butyl phthalate 1,2-Dichlorobenzene 1,3-Dichlorobenzene 1A-Dichlorobenzene 3,3'-Dichlorobenzidine Dieldrin Diethyl phthalate Dimethyl phthalate 2,4-Dinitrotoluene 2,6-Dinitrotoluene Di-n-octyl phthalate Endosulfan sulfate Endrin aldehyde Fluoranthene Fluorene Accuracy, as recovery, x' 

### (!Jg/L) 0.96C+0.19 0.89C+0.74 0.78C+1.66 0:80C+0.68 0.88C-0.60 0.93C-1.80 0.87C-1.56 0.90C-0.13 0.98C-0.86 0.66C-1.68 0.87C-0.94 0.29C-1.09 0.86C-1.54 1.12C-5.04 1.03C-2.31 0.84C-1.18 0.91C-1.34 0.89C+O.01 0.91C+0.53 0.93C-1.00 0.56C-0.40 0.70C-0.54 0.79C-3.28 0.88C+4.72 0.59C+0.71 0.80C+0.28 0.86C-0.70 0.73C-1.47 1.23C-12.65 0.82C-0.16 0.43C+1.00 0.20C+1.03 0.92C-4.81 1.06C-3.60 0.76C-0.79 0.39C+0.41 0.76C-3.86 0.81C+1.10 0.90C-0.00 Single analyst precision, s,' 

### (!Jg/L) 0.15x-O.12 0.24x-1.06 0.27x-1.28 0.21x-0.32 0.15x+0.93 0.22x+0.43 0.19x+1.03 0.22x+0.48 0.29x+2.40 0.18x+0.94 0.20x-0.58 0.34x+0.86 0.35x-0.99 0.16x+1.34 0.24x+0.28 0.26x+0.73 0.13x+0.66 0.07x+0.52 0.20x-0.94 0.28x+0.13 0.29x-0.32 0.26x-1.17 0.42x+0.19 0,30x+8.51 0.13x+1.16 0.20x+0.47 0.25x+0.68 0.24x+0.23 0.28x+7.33 0.20x-0.16 0.28x+1.44 0.54x+0.19 0.12x+1.06 0.14x+1.26 0.21x+1.19 0.12x+2.47 0.18x+3.91 0.22x-0.73 0.12x+0.26 Overall precision, S' 

### (!Jg/L) 0.21x-0.67 0.26x-0.54 0.43x+1.13 0.27x-0.64 0.26x-0.21 0.29x+0.96 0.35x+0.40 0.32x+1.35 0.51 x-0.44 0.53x+0.92 0.30x+1.94 0.93x-0.17 0.35x+0.10 0.26x+2.01 0.25x+1.04 0.36x+0.67 0.16x+0.66 0.13x+0.34 0.30x-0.46 0.33x-0.09 0.66x-0.96 0.39x-1.04 0.65x-0.58 0.59x+0.25 0.39x+0.60 0.24x+0.39 0.41x+0.11 0.29x+0.36 0.47x+3.45 0.26x-0.07 0.52x+0.22 1.05x-0.92 0.21 x+1.50 0.19x+0.35 0.37x+1.19 0.63x-1.03 0.73x-0.62 0.28x-0,60 0.13x+0.61

CD-ROM 82700 - 44 Revision 4 January 1998Compound Heptachlor Heptachlorepoxide Hexachlorobenzene Hexachlorobutadiene Hexachloroethane Indeno(1,2,3-cd)pyrene Isophorone Naphthalene Nitrobenzene N-Nitrosodi-n-propylamine Aroclor 1260 Phenanthrene Pyrene 1,2,4-Trichlorobenzene 4-Chloro-3-methylphenol 2-Chlorophenol 2,4-0ichlorophenol 2,4-0imethylphenol 2,4-0initrophenol 2-Methyl-4,6-dinitrophenol 2-Nitrophenol 4-Nitrophenol Pentachlorophenol Phenol 2,4,6-Trichlorophenol TABLE 7 (Continued)

Accuracy, as recovery, x'**(~g/L)** 0.87C-2.97 0.92C-1.87 0.74C+0.66 0.71 C-1.01 0.73C-0.83 0.78C-3.10 1.12C+1.41 0.76C+1.58 1.09C-3.05 1.12C-6.22 0.81C-10.86 0.87C+0.06 0.84C-0.16 0.94C-0.79 0.84C+0.35 0.78C+0.29 0.87C-0.13 0.71C+4.41 0.81C-18.04 1.04C-28.04 0.07C-1.15 0.61C-1.22 0.93C+1.99 0.43C+1.26 0.91C-0.18 Single analyst precision, 

### s,'**(~g/L)** 0.24x-0.56 0.33x-0.46 0.18x-0.10 0.19x+0.92 0.17x+0.67 0.29x+1.46 0.27x+0.77 0.21 x-0.41 0.19x+0.92 0.27x+0.68 0.35x+3.61 0.12x+0.57 0.16x+0.06 0:15x+0.85 0.23x+0.75 0.18x+1.46 0.15x+1.25 0.16x+1.21 0.38x+2.36 0.10x+42.29 0.16x+1.94 0.38x+2.57 0.24x+3.03 0.26x+0.73 0.16x+2.22 Overall precision, S'**(~g/L)** 0.50x-0.23 0.28x+0.64 0.43x-0.52 0.26x+0.49 0.17x+0.80 0.50x-0.44 0.33x+0.26 0.30x-0.68 0.27x+0.21 0.44x+0.47 0.43x+1.82 0.15x+0.25 0.15x+0.31 0.21x+0.39 0.29x+1.31 0.28x+0.97 0.21x+1.28 0.22x+1.31 0.42x+26.29 0.26x+23.10 0.27x+2.60 0.44x+3.24 0.30x+4.33 0.35x+0.58 0.22x+1.81

x' 

# =

s' 

# =

r Expected recovery for one or more measurements of asample containing aconcentration of 

### C, in**~g/L.** Expected single analyst standard deviation of measurements at an average concentration of 

### X, in**~g/L.** S' 

# = Expected interlaboratory standard deviation of measurements at an average concentration found ofX, in**~g/L.** C 

# = Truevalue forthe concentration, in**~g/L.**

-

### x = Average recovery' found for measurements of samples containing a concentration of C, in**~g/L.** a Criteria from 40 CFR Part 136 for Method 625, using a packed GC column. These criteria are based directlyon the method performance data in Table 7. Thesevalues are forguidance only. Appropriate derivation of acceptance criteria for capillary columns should result in much narrower ranges. See Method 8000for information on developing and updating acceptance criteriafor method performance.

CD-ROM' 82700 - 45 Revision 4 January 1998TABLE 8
EXTRACTION EFFICIENCYAND AQUEOUS STABILITY RESULTS

Percent Recovery, Day 0 Percent Recovery, Day 7 Compound Mean RSD Mean RSD 3-Amino-9-ethylcarbazole 80 8 73 3 4-Chloro-1,2-phenylenediamine 91 1 108 4 4-Chloro-1,3-phenylenediamine 84 3 70 3
1,2-Dibromo-3-chioropropane 97 2 98 5
Dinoseb 99 3 97 6
Parathion 100 2 103 4 4,4'-Methylenebis(N,N-d

### imethylaniline) 108 4 90 4
5-Nitro-o4oluidine 99 10 93 4
2-Picoline 80 4 83 4 Tetraethyl dithiopyrophosphate 92 7 70 1

Data taken from Reference 6.

CD-ROM 8270D-46 Revision 4 January 1998TABLE 9
MEAN PERCENT RECOVERIES AND PERCENT RSD VALUES FOR SEMIVOLATILE ORGANICS FROM SPIKED CLAY SOIL AND TOPSOIL BYAUTOMATED SOXHLET EXTRACTION (METHOD 3541) WITH HEXANE-ACETONE (1 :1)8

Clay Soil Topsoil
Mean RSD Mean RSD Compound Recovery Recovery 1,3-Dichlorobenzene 0 0 1,2-Dichlorobenzene 0 0 Nitrobenzene 0 0 Benzal chloride 0 0 Benzotrichloride 0 0 4-Chloro-2-nitrotoluene 0 0 Hexachlorocyclopentadiene 4.1 15 7.8 23 2,4-Dichloronitrobenzene 35.2 7.6 21.2 15 3,4-Dichloronitrobenzene 34.9 15 20.4 11 Pentachlorobenzene 13.7 7.3 14.8 13 2,3,4,5-Tetrachloronitrobenzene 55.9 6.7 50.4 6.0 Benefin 62.6 4.8 62.7 2.9 alpha-BHC 58.2 7.3 54.8 4.8 Hexachlorobenzene 26.9 13 25.1 5.7 delta-BHC 95.8 4.6 99.2 1.3 Heptachlor 46.9 9.2 49.1 6.3 Aldrin 97.7 12 102 7.4 Isopropalin 102 4.3 105 2.3 Heptachlorepoxide 90.4 4.4 93.6 2.4 trans-Chlordane 90.1 4.5 95.0 2.3 Endosulfan I 96.3 4.4 101 2.2 Dieldrin 129 4.7 104 1.9 2,5-Dichlorophenyl-4-nitrophenyl ether 110 4.1 112 2.1 Endrin 102 4.5 106 3.7 Endosulfan II 104 4.1 105 0.4 p,p'-DDT 134 2.1 111 2.0 2,3,6-Trichlorophenyl-4'-nitrophenyl ether 110 4.8 110 2.8 2,3,4-Trichlorophenyl-4'-nitrophenyl ether 112 4.4 112 3.3 Mirex 104 5.3 108 2.2

8 The operating conditions for the Soxtec apparatus were as follows: immersion time 45 min; extraction time 45 min; the sample size was 10 g; the spiking concentration was 500 ng/g, except for the surrogate compounds at 1000 ng/g, 2,5-0ichlorophenyl-4-nitrophenyl ether, 2,3,6- Trichlorophenyl-4-nitrophenyl ether, and 2,3,4-Trichlorophenyl-4-nitrophenyl ether at 1500 ng/g, Nitrobenzene at 2000 ng/g, and 1,3-Dichlorobenzene and 1,2-Dichlorobenzene at 5000 ng/g.

CD-ROM 82700- 47 Revision 4 January 1998TABLE 10
SINGLE LABORATORYACCURACYAND PRECISION DATA FOR THE EXTRACTION OF SEMIVOLA TILE ORGANICS FROM SPIKED CLAY BY AUTOMATED SOXHLET (METHOD 3541)a

Compound Mean Recovery RSD Phenol 47.8 5.6 Bis(2-chloroethyl)ether 25.4 13 2-Chlorophenol 42.7 4.3 Benzyl alcohol tzt: o 7") ,J,J.v I.L.. 2-Methylphenol 17.6 6.6 Bis(2-chloroisopropyl)ether 15.0 15 4-Methylphenol 23.4 6.7 N-Nitroso-di-n-propylamine 41.4 6.2 Nitrobenzene 28.2 7.7 Isophorone 56.1 4.2 2-Nitrophenol 36.0 6.5 2,4-Dimethylphenol 50.1 5.7 Benzoicacid 40.6 7.7 Bis(2-chloroethoxy)methane 44.1 3.0 2,4-Dichlorophenol 55.6 4.6 1,2,4-Trichlorobenzene 18.1 31 Naphthalene 26.2 15 4-Chloroaniline 55.7 12 4-Chloro-3-methylphenol 65.1 5.1 2-Methylnaphthalene 47.0 8.6 Hexachlorocyclopentadiene 19.3 19 2,4,6-Trichlorophenol 70.2 6.3 2,4,5-Trichlorophenol 26.8 2.9 2-Chloronaphthalene 61.2 6.0 2-Nitroaniline 73.8 6.0 Dimethyl phthalate 74.6 5.2 Acenaphthylene 71.6 5.7 3-Nitroaniline 77.6 5.3 Acenaphthene 79.2 4.0 2,4-Dinitrophenol 91.9 8.9 4-Nitrophenol a") o -1a VL...v IV Dibenzofuran 82.1 5.9 2,4-Dinitrotoluene 84.2 5.4 2,6-Dinitrotoluene 68.3 5.8 Diethyl phthalate 74.9 5.4 4.,Chlorophenyl-phenyl ether 67.2 3.2 Fluorene 82.1 3.4

CD-ROM 82700

-48 Revision 4 January 1998Compound 4-Nitroaniline 4,6-Dinitro-2-methylphenol N-Nitrosodiphenylamine 4-Bromophenyl-phenyl ether Hexachlorobenzene Pentachlorophenol Phenanthrene Anthracene Di-n-butyl phthalate Fluoranthene Pyrene Butyl benzyl phthalate 3,3'-Dichlorobenzidine Benzo(a)anthracene Bis(2-ethylhexyl) phthalate Chrysene Di-n-cetyl phthalate Benzo(b)fluoranthene Benzo(k)fluoranthene Benzo(a)pyrene Indeno(1,2,3-cd)pyrene Dibenzo(a,h)anthracene Benzo(g,h,i)perylene 1,2-Dichlorobenzene 1,3-Dichlorobenzene 1A-Dichlorobenzene Hexachloroethane Hexachlorobutadiene TABLE 10 (continued)

Mean Recovery 79.0 63.4 77.0 62.4 72.6 62.7 83.9 96.3 78.3 87.7 102

66.3 

### 25.2 73.4 77.2 76.2 83.1 82.7 71.7 71.7 

### 72.2 66.7 63.9



# a o 

# o o 

# o RSD 7.9 6.8 3.4 3.0 3.7 6.1 5.4 3.9 40

6.9 0.8 

### 5.2 11

3.8 4.8 4.4 4.8 5.0 4.1 4.1 4.3 6.3 8.0

a Numberof determinationswas three. The operating conditionsfor the Soxtecapparatuswere as follows: immersion time 45 min; extraction time 45 min; the sample size was 10 

### 9 clay soil; the spike concentration was 6 mg/kg percompound. The sample was allowed to equilibrate 1 hour after spiking.

Data taken from Reference

### 7.

CD-ROM 

### 82700

-49 Revision 4 January 1998TABLE 11

PRECISION AND BIAS VALUES FOR METHOD 35421

Compound Mean Recovery Standard Deviation % RSD 2-Fluorophenol 74.6 28.6 38.3 Phenol-d, 77.8 27.7 35.6 Nitrobenzene-d, 65.6 32.5 49.6 2-Fluorobiphenyl 75.9 30.3 39.9 2,4,6-Tribromophenol 67.0 34.0 50.7 

### Terphenyl-d., 78.6 32.4 41.3

1Thesurrogate values shown inTable 11 represent mean recoveries forsurrogates in all Method 0010 matrices in a field dynamicspiking study.

CD-ROM 8270D- 50 Revision 4 January 1998TABLE 12
ACCELERATED SOLVENT EXTRACTION (METHOD 3545) RECOVERYVALUES AS PERCENTOF SOXTECTM

Clay Loam Sand Mean Compound Low Mid High Low Mid High Low Mid High Rec.

Phenol 93.3 78.7 135.9 73.9 82.8 124.6 108.8 130.6 89.7 102.0 Bis(2-chloroethyl) ether 102.1 85.1 109.1 96.0 88.0 103.6 122.3 119.9 90.8 101.9 2-Chlorophenol 100.8 82.6 115.0 93.8 88.9 111.1 115.0 115.3 91.9 101.6 1,3-Dichlorobenzene 127.7 129.7 110.0 *364.2 129.9 119.0 *241.3 *163.7 107.1 120.6 1,4-Dichlorobenzene 127.9 127.0 110.5 *365.9 127.8 116.4 *309.6 *164.1 105.8 119.2 1,2-Dichlorobenzene 116.8 115.8 101.3 *159.2 113.4 105.5 *189.3 134.0 100.4 112.5 2-Methylphenol 98.9 82.1 119.7 87.6 89.4 111.0 133.2 128.0 92.1 104.7 Bis(2-chloroisopropyl)ether 109.4 71.5 108.0 81.8 81.0 88.6 118.1 148.3 94.8 100.2 o-Toluidine 100.0 89.7 117.2 100.0 *152.5 120.3 100.0 *199.5 102.7 110.3 N-Nitroso-di-n-propylamine 103.0 79.1 107.7 83.9 88.1 96.2 109.9 123.3 91.4 98.1 Hexachloroethane 97.1 125.1 111.0 *245.4 117.1 128.1 *566.7 147.9 103.7 118.6 Nitrobenzene 104.8 82.4 106.6 86.8 84.6 101.7 119.7 122.1 93.3 100.2 Isophorone 100.0 86.4 98.2 87.1 87.5 109.7 135.5 118.4 92.7 101.7 2,4-Dimethylphenol 100.0 104.5 140.0 100.0 114.4 123.1 100.0 *180.6 96.3 109.8 2-Nitrophenol 80.7 80.5 107.9 91.4 86.7 103.2 122.1 107.1 87.0 96.3 Bis(chloroethoxy)methane 94.4 80.6 94.7 86.5 84.4 99.6 130.6 110.7 93.2 97.2 2,4-Dichlorophenol 88.9 87.8 111.4 85.9 87.6 103.5 123.3 107.0 92.1 98.6 1,2,4-Trichlorobenzene 98.0 97.8 98.8 123.0 93.7 94.5 137.0 99.4 95.3 104.2 Naphthalene 101.7 97.2 123.6 113.2 102.9 129.5 *174.5 114.0 89.8 106.1 4-Chloroaniline 100.0 *150.2 *162.4 100.0 125.5 *263.6 100.0 *250.8 114.9 108.1 Hexachlorobutadiene 101.1 98.7 102.2 124.1 90.3 98.0 134.9 96.1 96.8 104.7 4-Chloro-3-methylphenol 90.4 80.2 114.7 79.0 85.2 109.8 131.6 116.2 90.1 99.7 2-Methylnaphthalene 93.2 89.9 94.6 104.1 92.2 105.9 146.2 99.1 93.3 102.1 Hexachlorocyclopentadiene 100.0 100.0 0.0 100.0 100.0 6.8 100.0 100.0 *238.3 75.8 2,4,6-Trichlorophenol 94.6 90.0 112.0 84.2 91.2 103.6 101.6 95.9 89.8 95.9 2,4,5-Trichlorophenol 84.4 91.9 109.6 96.1 80.7 103.6 108.9 83.9 87.9 94.1 2-Chloronaphthalene 100.0 91.3 93.6 97.6 93.4 98.3 106.8 93.0 92.0 96.2 2-Nitroaniline 90.0 83.4 97.4 71.3 88.4 89.9 112.1 113.3 87.7 92.6 2,6-Dinitrotoluene 83.1 90.6 91.6 86.4 90.6 90.3 104.3 84.7 90.9 90.3 Acenaphthylene 104.9 95.9 100.5 99.0 97.9 108.8 118.5 97.8 92.0 101.7 3-Nitroaniline *224.0 115.6 97.6 100.0 111.8 107.8 0.0 111.7 99.0 92.9 Acenaphthene 102.1 92.6 97.6 97.2 96.9 104.4 114.2 92.0 89.0 98.4 4-Nitrophenol 0.0 93.2 121.5 18.1 87.1 116.6 69.1 90.5 84.5 75.6 2,4-Dinitrotoluene 73.9 91.9 100.2 84.7 93.8 98.9 100.9 84.3 87.3 90.7

CD-ROM 82700 - 51 Revision 4 January 

### 1998TABLE 12 (continued)

Clay Loam Sand Mean Compound Low Mid High Low Mid High Low Mid High Rec.

Dibenzofuran 89.5 91.7 109.3 98.5 92.2 j 11.4 113.8 92.7 90.4 98.8 4-Chlorophenyl phenyl 83.0 94.5 98.7 95.7 94.3 94.2 111.4 87.7 90.3 94.4 ether Fluorene 85.2 94.9 89.2 102.0 95.5 93.8 121.3 85.7 90.9 95.4 4-Nitroaniline 77.8 114.8 94.5 129.6 103.6 95.4 *154.1 89.3 87.5 99.1 N-Nitrosodiphenylamine 82.6 96.7 93.8 92.9 93.4 116.4 97.5 110.9 86.7 96.8 4-Bromophenyl phenyl 85.6 92.9 92.8 91.1 107.6 89.4 118.0 97.5 87.1 95.8 ether Hexachlorobenzene 95.4 91.7 92.3 95.4 93.6 83.7 106.8 94.3 90.0 93.7 Pentachlorophenol 68.2 85.9 107.7 53.2 89.8 88.1 96.6 59.8 81.3 81.2 Phenanthrene 92.1 93.7 93.3 100.0 97.8 113.3 124.4 101.0 89.9 100.6 Anthracene 101.6 95.0 93.5 92.5 101.8 118.4

. 123.0 94.5 90.6 101.2 Carbazole 94.4 99.3 96.6 105.5 96.7 111.4 115.7 83.2 88.9 99.1 Fluoranthene 109.9 101.4 94.3 111.6 96.6 109.6 123.2 85.4 92.7 102.7 Pyrene 106.5 105.8 107.6 116.7 90.7 127.5 103.4 95.5 93.2 105.2 3,3'-Dichlorobenzidine 100.0 *492.3 131.4 100.0 *217.6 *167.6 100.0 *748.8 100.0 116.5 Benzo(a)anthracene 98.1 107.0 98.4 119.3 98.6 104.0 105.0 93.4 89.3 101.5 Chrysene 100.0 108.5 100.2 116.8 93.0 117.0 106.7 93.6 90.2 102.9 Benzo(b)f1uoranthene 106.6 109.9 75.6 121.7 100.7 93.9 106.9 81.9 93.6 99.0 Benzo(k)f1uoranthene 102.4 105.2 88.4 125.5 99.4 95.1 144.7 89.2 78.1 103.1 Benzo(a)pyrene 107.9 105.5 80.8 122.3 97.7 104.6 101.7 86.2 92.0 99.9 Indeno(1,2,3-cd)pyrene 95.1 105.7 93.8 126.0 105.2 9004 133.6 82.6 91.9 102.7 Dibenz(a,h)anthracene 85.0 102.6 82.0 118.8 100.7 91.9 142.3 71.0 93.1 98.6 Benzo(g,h,OperyIene 98.0 0.0 81.2 0.0 33.6 78.6 128.7 83.0 94.2 6604 Mean 95.1 94.3 101.0 95.5 96.5 104.1 113.0 100.9 92.5

*Valuesgreaterthan 150% were not used to determine the averages, but the 0% values were used.

CD-ROM 

### 82700- 52 Revision 4 January 1998TABLE 13
SINGLE LABORATORYACCURACYAND PRECISION FOR THE EXTRACTION OF PAHs FROM A CERTIFIED REFERENCE SEDIMENT EC-1, USING METHOD 3561 (SFE

- SOLID TRAP)

Certified Value SFE Value" Percentof SFE Compound (mg/kg) (mg/kg) Certified Value RSD Naphthalene (27.9)b 41.3 ± 3.6 (148) 8.7 Acenaphthylene (0.8) 0.9 ± 0.1 (112) 11.1 Acenaphthene In "l\ rv

### "'.1 rv

### n,. r.... f"\f'\\ rv ,,1= \U.L) U.L I U.U I \ I UU) u.u;';
Fluorene (15.3) 15.6 ± 1.8 (102) 11.5
Phenanthrene 15.8±1.2 16.1±1.8 102 11.2
Anthracene (1.3) 1.1 ± 0.2 (88) 18.2
Fluoranthene 23.2 ± 2.0 24.1±2.1 104 8.7 Pyrene 16.7 ± 2.0 17.2 ± 1.9 103 11.0 Benz(a)anthracene 8.7± 0.8 8.8 ± 1.0 101 11.4 Chrysene (9.2) 7.9 ± 0.9 (86) 11.4 Benzo(b)fluoranthene 7.9 ± 0.9 8.5 ± 1.1 108 12.9 Benzo(k)fluoranthene 4.4 ± 0.5 4.1 ± 0.5 91 12.2 Benzo(a)pyrene 5.3

### ±0.7 5.1 ± 0.6 96 11.8 Indeno(1,2,3-cd)pyrene 5.7 ± 0.6 5.2 ± 0.6 91 11.5 Benzo(g,h,i)perylene 4.9 ± 0.7 4.3 ± 0.5 88 11.6 Dibenz(a,h)anthracene (1.3) 1.1±0.2 (85) 18.2

a Relative standard deviationsfor the SFE values are based on six replicate extractions.

b Values in parentheses were obtained from, or compared to, Soxhlet extraction results which were not certified.

Data are taken from Reference 10.

CD-ROM 8270D

- 53 Revision 4 January 1998

### TABLE 14
SINGLE LABORATORY ACCURACY AND PRECISION FOR THE EXTRACTION OF PAHs FROM A CERTIFIEDREFERENCE SEDIMENT HS-3, USING METHOD 3561 (SFE

- SOLID TRAP)

Certified Value SFE Value" Percent of SFE Compound (mg/kg) (mg/kg) Certified Value RSD Naphthalene 9.0 ± 0.7 7.4 ± 0.6 82 8.1 Acenaphthylene 0.3± 0.1 0.4 ± 0.1 133 25.0 Acenaphthene 4.5 ± 1.5 3.3± 0.3 73 9.0
Fluorene 13.6 ± 3.1 10.4±1.3 77 12.5
Phenanthrene 85.0 ± 20.0 86.2 ± 9.5 101 11.0
Anthracene 13.4 ± 0.5 12.1 ± 1.5 90 12.4
Fluoranthene 60.0± 9.0 54.0 ± 6.1 90 11.3 Pyrene 39.0± 9.0 '32.7± 3.7 84 11.3 Benz(a)anthracene 14.6 ± 2.0 12.1±1.3 83 10.7 Chrysene 14.1 ± 2.0 12.0 ± 1.3 85 10.8 Benzo(b)f1uoranthene 7.7 ± 1.2 8.4± 0.9 109 10.7 Benzo(k)f1uoranthene 2.8±2.0 3.2 ± 0.5 114 15.6 Benzo(a)pyrene 7.4 ± 3.6 6.6 ± 0.8 89 12.1 Indeno(1,2,3-cd)pyrene 5.0 ± 2.0 4.5±0.6 90 13.3 Benzo(g,h,i)perylene 5.4 ± 1.3 4.4 ± 0.6 82 13.6 Dibenz(a,h) anthracene 1.3 ± 0.5 1.1 ± 0.3 85 27.3

a 

### Relative standard deviations fortheSFE values are based on three replicate extractions.

Data aretakenfrom Reference 10.

CD-ROM 82700- 54 Revision 4 January 1998TABLE 15

SINGLE LABORATORYACCURACYAND PRECISION FOR THE EXTRACTION OF PAHs FROM A CERTIFIED REFERENCE SOIL SRS103-100, USING METHOD 3561 (SFE - LIQUID TRAP)

Certified Value SFE Value" Percentof SFE Compound (mg/kg) (mg/kg) Certified Value RSD Naphthalene 32.4 ± 8.2 29.55 91 10.5 2-Methylnaphthalene 62.1 ± 11.5 76.13 122 2.0 Acenaphthene 632 ± 105 577.28 91 2.9
Dibenzofuran 307 ± 49 302.25 98 4.1
Fluorene 492 ± 78 427.15 87 3.0
Phenanthrene 1618 ± 340 1278.03 79 3.4
Anthracene 422 ± 49 400.80 95 2.6
Fluoranthene 1280 ± 220 1019.13 80 4.5 Pyrene 1033 ± 285 911.82 88 3.1 Benz(a)anthracene 252± 8 225.50 89 4.8 Chrysene 297 ± 26 283.00 95 3.8 Benzo(a)pyrene 97.2 ± 17.1 58.28 60 6.5 Benzo(b)fluoranthene

### + 153 ± 22 130.88 86 10.7 Benzo(k)fluoranthene

a Relative standard deviationsfor the SFE values are based on four replicate extractions.

Data are taken from Reference 11.

CD-ROM 82700-55 Revision 4 January 1998TABLE 16

SINGLE LABORATORY RECOVERY DATA FOR SOLID-PHASE EXTRACTION OF BASE/NEUTRAUACID EXTRACTABLES FROM SPIKEDTCLP BUFFERS LOWSPIKE LEVEL

Buffer 1 (pH 

### = 2.886) Buffer2 (pH

# =4.937) Spike Level Analyte (lJg/L) Recovery (%) RSD Recovery (%) RSD

1,4-Dichlorobenzene 3,750 63 10 63 9
Hexachloroethane 1,500 55 6 77 4
Nitrobenzene 1,000 82 10 100 5
Hexachlorobutadiene 250 65 3 56 4 2,4-Dinitrotoluene 65 89 4 101 5
Hexachlorobenzene 65 98 5 95 6
o-Cresol 100,000 83 10 85 5
m-Cresol* 100,000 86 8 85 3 p-Cresol* 100,000 * * * * 2,4,6-Trichlorophenol 1,000 84 12 95 12 2,4,5-Trichlorophenol 200,000 83 11 88 3 Pentachlorophenol 50,000 82 9 78 9

Resultsfrom seven replicate spiked buffer samples.
* In this study, m-cresol and p-cresol co-eluted and were quantitated as a mixture of both isomers.

Data from Reference 12.

8270D - 56 Revision 4 January 1998TABLE 17

SINGLE LABORATORY RECOVERY DATA FOR SOLID-PHASE EXTRACTION OF BASE/NEUTRAL/ACID EXTRACTABLES FROM SPIKED TCLP BUFFERS HIGH SPIKE LEVEL

CD-ROM 82700

- 57 Revision 4 January 1998TABLE 18

RECOVERY DATA FROM THREE LABORATORIES FOR SOLID-PHASE EXTRACTION OF BASE/NEUTRAL/ACID EXTRACTABLES FROM SPIKEDTCLP LEACHATES FROM SOIL SAMPLES

Buffer 1 pH 

### =2.886 Lab 1 Lab 2 Lab 3 Spike Level Analyte (wg/L)* %R RSD n %R RSD n %R RSD n
o-Cresol 200,000 86 8 7 35.3 0.7 3 7.6 6 3 m-Cresol**



### -- 77 

### 8 7 p-Cresol**



## -- 

# -- -- -- -- 

# --**~-** 7.7 11 3 2,4,6-Trichlorophenol 2,000 106 6 7 96.3 3.9 3 44.8 5 3 2,4,5-Trichlorophenol 400,000 93 3 7 80.5 4.5 3 63.3 11 3 Pentachlorophenol 100,000 79 2 7 33.8 12.2 3 29.2 13 3 1,4-Dichlorobenzene 7,500 51 5 7 81.3 5.3 3 19.2 7 3 Hexachloroethane 3,000 50 5 7 66.2 2.1 3 12.6 11 3 Nitrobenzene 2,000 80 8 7 76.3 5.3 3 63.9 12 3 Hexachlorobutadiene 500 53 8 7 63.3 4.8 3 9.6 9 3 2,4-Dinitrotoluene 130 89 8 7 35.7 2.6 3 58.2 17 3
Hexachlorobenzene 130 84 21 7 92.3 1.6 3 71.7 9 3 (continued)

CD"ROM 82700 - 58 Revision 4 January 1998TABLE 18 (continued)

Buffer2 pH

## =4.937 Lab 1 Lab 2 Lab 3 Spike Level Analyte (fJg/L)* %R RSD n %R RSD n %R RSD n o-Cresol 200,00 97 13 7 37.8 4.5 3 6.1 24 3
m-Cresol**



## -- 83 

### 4 7



## -- -- 

## -- 6.0 25 3 p-Cresol** 2,4,6-Trichlorophenol 2,000 104 

### 4 7 91.7 8.0 3**~17.7** 25 3 2,4,5-Trichlorophenol 400,000 94 4 7 85.2 0,4 3 E>4,4 10 3 Pentachlorophenol 100,000 109 11 7 41.9 28.2 3**~16.6** 32 3 1,4-Dichlorobenzene 7,500 50 5 7 79.7 1.0 3 26.5 68 3
Hexachloroethane 3,000 51 3 7 64.9 2.0 3 20.3 90 3
Nitrobenzene 2,000 80 4 7 79.0 2.3 3**~)9,4** 6 3
Hexachlorobutadiene 500 57 5 7 60 3.3 3 116.6 107 3 2,4-Dinitrotoluene 130 86 6 7 38.5 5.2 3 62.2 6 

### 3
Hexachlorobenzene 130 86 7 7 91.3 0.9 

### 3 75.5 5 3

* 250-mL aliquots of leachate were spiked. Lab 1 spiked at one-halfthese levels.
** m-Cresol and p-Cresol coelute. Lab 1 and Lab 3 reported o-Cresol and the sum of m- and p-CresoL Lab 2 reported the sum of all three isomers of Cresol.

Data from Reference 12.

CD-ROM 82700 - 59 Revision 4 January 1998RIC FIGURE 1 GAS CHROMATOGRAM OF BASE/NEUTRALAND ACID CALIBRATION STANDARD

RIC (

..Ii<. 51flHS0007S6 It 2"'l TO2788**afYIi7/~** S:2b:OO (HLl:**51~7S6** .3 St<HPLE: BASE**~ID 5TD.2\1J~:i1l4·LL**  CCWS.:**~:** C**1.2799~:** H fl. 4.0 0LiHIi: Ii O. 1.0 J 

### e Bi6£: U216. 3



### zsee 41:40

CD-ROM 

### 82700-60' Revision 4 January 

### 1998METHOD 82700 SEMIVOLATILE ORGANIC COMPOUNDS BY GAS CHROMATOGRAPHY/MASS SPECTROMETRY (GC/MS)

7.1 Prepare sample

using appropriate 3500 series method.

7.2 If necessary, cleanup extract using

appropriate 3600

series method.

7.3 Establish GC/MS operating conditions. Tune to DFTPP.

Perform initial

calibration.

7.4 Perform daily calibration verification with SPCCs and CCCs

prior to analysis of samples.

CD-ROM 7.5.1 Screen extract on GC/FID or GC/PID

to identify highly contaminated samples.

Dilute those samples as needed.

7.5.3 Analyze extract by GC/MS.

7.6 Identify analyte

by comparing the sample and standard mass spectra.

7.7 Calculate concentration of each individual analvte

confirmed present. Report results.

82700

- 61 7.5.4 Dilute extract.

Revision 4 January 

### 1998