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 in extracts prepared from many types of solid waste matrices, soils, air sampling media 

and water samples. Direct injection of a sample may be used in limited applications. The following 

compounds can be determined by this method: 

Appropriate Preparation Techniquesb 

3540/
 

Compounds CAS Noa 3510 352 3541 355 3580
 

0 0
 

Acenaphthene 83-32-9 X X X X X
 

1-Acetyl-2-thiourea 591-08-2 LR ND ND ND LR
 

Barban 101-27-9 LR ND ND ND LR
 

Benzidine 92-87-5 CP CP CP CP CP
 

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
 

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) ND ND ND 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) ND ND ND X
 

Benzoic acid 65-85-0 X X ND X X
 

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Appropriate Preparation Techniquesb 

Compounds CAS Noa 3510 352 3541 355 

3540/
 

3580
 

0 0
 

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

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

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 X X X X
 

p-Benzoquinone 106-51-4 OE ND ND ND X
 

Benzyl alcohol 100-51-6 X X ND X X
 

α-BHC 319-84-6 X X X X X
 

β-BHC 319-85-7 X X X X X
 

δ-BHC 319-86-8 X X X X X
 

γ-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 ND ND ND X
 

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

Captafol 2425-06-1 HS(55) ND ND ND X
 

Captan 133-06-2 HS(40) ND ND ND X
 

Carbaryl 63-25-2 X ND ND ND X
 

Carbofuran 1563-66-2 X ND ND ND X
 

Carbophenothion 786-19-6 X ND ND ND X
 

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

Chlorfenvinphos 470-90-6 X ND ND ND X
 

4-Chloroaniline 106-47-8 X ND ND ND X
 

Chlorobenzilate 510-15-6 X ND ND ND X
 

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

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

3-(Chloromethyl)pyridine 6959-48-4 X ND ND ND 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-phenylenediamine 95-83-0 X X ND ND ND
 

4-Chloro-1,3-phenylenediamine 5131-60-2 X X ND ND ND
 

4-Chlorophenyl phenyl ether 7005-72-3 X X X X X
 

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Appropriate Preparation Techniquesb 

Compounds CAS Noa 3510 352 3541 355 

3540/
 

3580
 

0 0
 

Chrysene 218-01-9 X X X X X
 

Coumaphos 56-72-4 X ND ND ND X
 

p-Cresidine 120-71-8 X ND ND ND X
 

Crotoxyphos 7700-17-6 X ND ND ND X
 

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 or trans) 2303-16-4 X ND ND ND X
 

2,4-Diaminotoluene 95-80-7 DC,0E(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,0S(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
 

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Appropriate Preparation Techniquesb 

Compounds CAS Noa 3510 352 3541 355 

3540/
 

3580
 

0 0
 

3,3'-Dimethylbenzidine 119-93-7 X ND ND ND X

α,α-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

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-octyl 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
 

Endrin aldehyde 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) ND 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 ND 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
 

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Appropriate Preparation Techniquesb 

Compounds CAS Noa 3510 352 3541 355 

3540/
 

3580
 

0 0
 

Heptachlor 76-44-8 X X X X X
 

Heptachlor epoxide 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
 

Hexachlorocyclopentadiene 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
 

4,4'-Methylenebis 101-14-4 OE,OS(0) ND ND ND LR
 

(2-chloroaniline)
 

Hexamethylphosphoramide 680-31-9 X ND ND ND X
 

Hydroquinone 123-31-9 ND ND ND ND X
 

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

Isodrin 465-73-6 X ND ND ND X
 

Isophorone 78-59-1 X X X X X
 

Isosafrole 120-58-1 DC(46) ND ND ND X
 

Kepone 143-50-0 X ND ND ND X
 

Leptophos 21609-90-5 X ND ND ND X
 

Malathion 121-75-5 HS(5) ND 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 ND ND ND X
 

3-Methylcholanthrene 56-49-5 X ND ND ND X
 

4,4'-Methylenebis(N,N-dimethyl- 101-61-1 X X ND ND ND
 

aniline)
 

Methyl methanesulfonate 66-27-3 X ND ND ND X
 

2-Methylnaphthalene 91-57-6 X X ND X X

Methyl parathion 298-00-0 X ND ND ND X
 

2-Methylphenol 95-48-7 X ND ND ND X

3-Methylphenol 108-39-4 X ND ND ND X

4-Methylphenol 106-44-5 X ND 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 ND ND ND X
 

Monocrotophos 6923-22-4 HE ND ND ND X
 

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Appropriate Preparation Techniquesb 

Compounds CAS Noa 3510 352 3541 355 

3540/
 

3580
 

0 0
 

Naled 300-76-5 X ND ND ND X
 

Naphthalene 91-20-3 X X X X X
 

1,4-Naphthoquinone 130-15-4 X ND ND ND X

1-Naphthylamine 134-32-7 OS(44) ND ND ND X
 

2-Naphthylamine 91-59-8 X ND ND ND X

Nicotine 54-11-5 DE(67) ND ND ND X
 

5-Nitroacenaphthene 602-87-9 X ND 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 ND ND ND X
 

Nitrobenzene 98-95-3 X X X X X
 

4-Nitrobiphenyl 92-93-3 X ND ND ND X

Nitrofen 1836-75-5 X ND ND ND X
 

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

4-Nitrophenol 100-02-7 X X X X X

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

Nitroquinoline-1-oxide 56-57-5 X ND ND ND X

N-Nitrosodi-n-butylamine 924-16-3 X ND ND ND X
 

N-Nitrosodiethylamine 55-18-5 X ND ND ND X
 

N-Nitrosodimethylamine 62-75-9 X X X X X
 

N-Nitrosomethylethylamine 10595-95-6 X ND ND ND 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 ND ND ND ND X
 

N-Nitrosopiperidine 100-75-4 X ND ND ND X
 

N-Nitrosopyrrolidine 930-55-2 X ND ND ND X
 

Octamethyl pyrophosphoramide 152-16-9 LR ND ND ND LR
 

4,4'-Oxydianiline 101-80-4 X ND ND ND X

Parathion 56-38-2 X X ND ND X
 

Pentachlorobenzene 608-93-5 X ND ND ND X
 

Pentachloronitrobenzene 82-68-8 X ND ND ND X
 

Pentachlorophenol 87-86-5 X X X X X
 

Phenacetin 62-44-2 X ND ND ND X
 

Phenanthrene 85-01-8 X X X X X
 

Phenobarbital 50-06-6 X ND ND ND X
 

Phenol 108-95-2 DC(28) X X X X
 

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Appropriate Preparation Techniquesb 

Compounds CAS Noa 3510 352 3541 355 

3540/
 

3580
 

0 0
 

106-50-3 X ND ND ND X
 

Phthalic anhydride 85-44-9 CP,HE(1) ND ND ND CP
 

Propylthiouracil 51-52-5 LR ND ND ND LR
 

1,4-Phenylenediamine 

Phorate 298-02-2 X ND ND ND X
 

Phosalone 2310-17-0 HS(65) ND ND ND X
 

Phosmet 732-11-6 HS(15) ND ND ND X
 

Phosphamidon 13171-21-6 HE(63) ND ND ND X
 

2-Picoline (2-Methylpyridine) 109-06-8 X X ND ND ND
 

Piperonyl sulfoxide 120-62-7 X ND ND ND X
 

Pronamide 23950-58-5 X ND ND ND X
 

Pyrene 129-00-0 X X X X X
 

Resorcinol 108-46-3 DC,OE(10 ND ND ND X
 

)
 

Safrole 94-59-7 X ND ND ND X
 

Strychnine 57-24-9 AW,0S(55 ND ND ND X
 

)
 

Sulfallate 95-06-7 X ND ND ND X
 

Terbufos 13071-79-9 X ND ND ND 

Tetraethyl dithiopyrophosphate 3689-24-5 X X ND ND ND
 

X
 

1,2,4,5-Tetrachlorobenzene 95-94-3 X ND ND ND X
 

2,3,4,6-Tetrachlorophenol 58-90-2 X ND ND ND X

Tetrachlorvinphos 961-11-5 X ND ND ND X
 

Tetraethyl pyrophosphate 107-49-3 X ND ND ND X
 

Thionazine 297-97-2 X ND ND ND X
 

Thiophenol (Benzenethiol) 108-98-5 X ND ND ND X
 

Toluene diisocyanate 584-84-9 HE(6) ND ND ND X
 

o-Toluidine 95-53-4 X ND ND ND 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 ND X X

2,4,6-Trichlorophenol 88-06-2 X X X X X

Trifluralin 1582-09-8 X ND ND ND X
 

2,4,5-Trimethylaniline 137-17-7 X ND ND ND X

Trimethyl phosphate 512-56-1 HE(60) ND ND ND X
 

1,3,5-Trinitrobenzene 99-35-4 X ND ND ND X
 

Tris(2,3-dibromopropyl) 126-72-7 X ND ND ND LR
 

phosphate
 

CD-ROM 8270D - 7 Revision 4
 

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Appropriate Preparation Techniquesb 

Compounds CAS Noa 3510 352 

0 

3540/ 

3541 355 

0 

3580 

Tri-p-tolyl phosphate 

O,O,O-Triethyl phosphorothioate 

78-32-0 

126-68-1 

X 

X 

ND 

ND 

ND 

ND 

ND 

ND 

X 

X 

a

 Chemical Abstract Service Registry Number

b

 See Sec. 1.2 for other acceptable preparation methods.
 

KEY TO ANALYTE LIST 

AW = Adsorption to walls of glassware during extraction and storage. 

CP = Nonreproducible chromatographic performance. 

DC = Unfavorable distribution coefficient (number in 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 is percent stability). 

LR = Low response. 

ND = Not determined. 

OE = Oxidation during extraction accelerated by basic conditions (number in parenthesis is 

percent recovery). 

OS = Oxidation during storage (number in parenthesis is percent stability). 

X = Greater than 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 

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 

extraction device for semivolatiles in solids (Table 12 contains performance data), and Method 3561 

describes a supercritical fluid device for the extraction of PAHs from solids (see Tables 13, 14, and 

15 for performance data). 

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 chromatographic fused-silica capillary column coated with 

a slightly polar silicone. Such compounds include polynuclear aromatic hydrocarbons, chlorinated 

hydrocarbons and pesticides, phthalate esters, organophosphate esters, nitrosamines, haloethers, 

aldehydes, ethers, ketones, anilines, pyridines, quinolines, aromatic nitro compounds, and phenols, 

including nitrophenols. See Table 1 for a list of compounds and their characteristic ions that have 

been evaluated. 

In most cases, Method 8270 is not appropriate for the quantitation of multicomponent 

analytes, e.g., Aroclors, Toxaphene, Chlordane, etc., because of limited sensitivity for those 

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 

CD-ROM 8270D - 8 Revision 4 

January 1998 
 

permits. Refer to Sec. 7.0 of Methods 8081 and 8082 for guidance on calibration and quantitation 

of multicomponent analytes such as the Aroclors, Toxaphene, and Chlordane. 

1.4 The following compounds may require special treatment when being determined by 

this method: 

1.4.1 Benzidine may be subject to oxidative losses during solvent concentration 

and its chromatographic behavior is poor. 

1.4.2 Under the alkaline conditions of the extraction step from aqueous matrices, 

α-BHC, γ-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 

chromatographic conditions 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 GC injection 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 may be necessary to perform separate 

analyses. 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 is exercised during the concentration steps. For this reason, analysts may 

wish to consider the use of extraction techniques such as pressurized fluid extraction (Method 

3545) or supercritical fluid extraction, which involve smaller extract volumes, thereby reducing 

or eliminating the need for evaporative concentration techniques for 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 are flagged when there are 

limitations caused by sample preparation and/or chromatographic problems. 

1.5 The estimated quantitation limit (EQL) of Method 8270 for determining an individual 

compound is approximately 660 μg/kg (wet weight) for soil/sediment samples, 1-200 mg/kg for 

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January 1998 
 

 

 

wastes (dependent on matrix and method of preparation), and 10 μg/L for ground water samples 

(see Table 2). EQLs will be proportionately higher for sample extracts that require dilution to avoid 

saturation of the detector. 

1.6 This method is restricted to use by or under the supervision of analysts 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 results with this method. 

2.0 SUMMARY OF 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, if necessary, 

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 separate the analytes, which are then detected with a mass 

spectrometer (MS) connected to the gas chromatograph. 

2.3 Analytes eluted from the capillary column are introduced into the mass spectrometer 

via a jet 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 of authentic 

standards. Quantitation is accomplished by comparing the response of a major (quantitation) ion 

relative to an internal standard using a five-point calibration curve. 

2.4 The method includes specific calibration and quality control steps that supersede the 

general requirements provided in Method 8000. 

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 eliminate the problem. 

3.2 Contamination by carryover can occur whenever high-concentration and 

low-concentration samples are sequentially analyzed. To reduce carryover, the sample syringe 

must be rinsed with solvent between sample injections. Whenever an unusually concentrated 

sample is encountered, it should be followed by the analysis of solvent to check for crosscontamination. 

4.0 APPARATUS AND MATERIALS 

4.1 Gas chromatograph/mass spectrometer system 

4.1.1 Gas chromatograph - An analytical system complete with a 

temperature-programmable gas chromatograph suitable for splitless injection and all required 

accessories, including syringes, analytical columns, and gases. The capillary column should 

be directly coupled to the source. 

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4.1.2 Column - 30-m x 0.25-mm ID (or 0.32-mm ID) 1-μm film thickness 

silicone-coated fused-silica capillary column (J&W Scientific DB-5 or equivalent). 

4.1.3 Mass spectrometer 

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 impact ionization mode. The 

mass spectrometer must be capable of producing a mass spectrum for 

decafluorotriphenylphosphine (DFTPP) which meets the criteria in Table 3 when 1 μL 

of the GC/MS tuning standard is injected through the GC (50 ng of DFTPP). 

4.1.3.2 An ion trap mass spectrometer may 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 EPA/NIST Library. The mass spectrometer 

must be capable of producing a mass spectrum for DFTPP which meets the criteria 

in Table 3 when 5 or 50 ng are introduced. 

4.1.4 GC/MS interface - Any GC-to-MS interface may be used that gives 

acceptable calibration points at 50 ng per injection for 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 spectrometer source. 

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 computer should 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 available that allows integrating the abundances in any EICP 

between specified time or scan-number limits. The most recent version of the EPA/NIST 

Mass Spectral Library should also be available. 

4.1.6 Guard column (optional) - (J&W deactivated fused-silica, 0.25-mm ID 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-μL. 

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

4.4 Balance - Analytical, capable of weighing 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. 

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Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high 

purity to permit its use without lessening the accuracy of the determination. 

5.2 Organic-free reagent water - All references to water in this method refer to organic-free 

reagent water, as defined in Chapter One. 

5.3 Stock standard solutions (1000 mg/L) - Standard solutions can be prepared from pure 

standard materials or purchased as certified solutions. 

5.3.1 Prepare stock standard solutions by accurately weighing about 0.0100 g of 

pure material. Dissolve the material in pesticide quality acetone or other suitable solvent and 

dilute to volume in a 10-mL volumetric flask. Larger volumes can be used at the convenience 

of the analyst. When compound purity is assayed to be 96% or greater, the weight may be 

used without correction to calculate the concentration of the stock standard. Commerciallyprepared stock standards may be used at any concentration if they are certified by the 

manufacturer or by an independent source. 

5.3.2 Transfer the stock standard solutions into bottles with PTFE-lined 

screw-caps. Store, protected from light, at -10EC or less or as recommended by the standard 

manufacturer. Stock standard solutions should be checked frequently for signs of 

degradation or evaporation, especially just prior to preparing calibration standards from them. 

5.3.3 Stock standard solutions must be replaced after 1 year or sooner if 

comparison with quality control check samples 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, consult the manufacturer's instructions for additional guidance. 

5.3.5 Mixes with hydrochloride salts may contain hydrochloric acid, which can 

cause analytical difficulties. When using a premixed certified standard, consult the 

manufacturer's instructions for additional guidance. 

5.4 Internal standard solutions - The internal standards recommended are 1,4-dichlorobenzene-d4, naphthalene-d8, acenaphthene-d10, phenanthrene-d10, chrysene-d12, and perylene-d12 

(see Table 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. 

Transfer to a 50 mL volumetric flask and dilute to volume with methylene chloride so that the 

final solvent is approximately 20% carbon disulfide. Most of the compounds are also soluble 

in small volumes of methanol, acetone, or toluene, except for perylene-d12. The resulting 

solution will contain each standard at a concentration of 4,000 ng/μL. Each 1-mL sample 

extract undergoing analysis should be spiked with 10 μL of the internal standard solution, 

resulting in a concentration of 40 ng/μL of each internal standard. Store at -10EC or less 

when not in use. When using premixed certified solutions, store according to the 

manufacturer's documented holding time and storage temperature recommendations. 

5.4.2 If a more sensitive mass spectrometer is employed to achieve lower 

detection levels, a more dilute internal standard solution may be required. Area counts of the 

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internal standard peaks should be between 50-200% of the area of the target analytes in the 

mid-point calibration analysis. 

5.5 GC/MS tuning standard - A methylene chloride solution containing 50 ng/μL of 

decafluorotriphenylphosphine (DFTPP) should be prepared. The standard should also contain 50 

ng/μL each of 4,4'-DDT, pentachlorophenol, and benzidine to verify injection port inertness and GC 

column performance. Store at -10EC or less when not in use. If a more sensitive mass 

spectrometer is employed to achieve lower detection levels, a more dilute tuning solution may be 

necessary. When using premixed certified solutions, store according to the manufacturer's 

documented holding time and storage temperature 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 correspond to a 

sample concentration at or below that necessary to meet the data quality objectives of the project. 

The remaining standards should correspond to the range of concentrations found in actual samples 

but should not exceed the working range of the GC/MS system. Each standard should contain 

each analyte for 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). These target analytes may not include the entire list 

of analytes (Sec. 1.1) for which the method has been demonstrated. However, the laboratory 

shall not report a quantitative result for a target analyte that was not included in the calibration 

standard(s). 

5.6.2 Each 1-mL aliquot of calibration standard should be spiked with 10 μL of the 

internal standard solution prior to analysis. All standards should be stored at -10EC or less, 

and should be freshly prepared once a year, or sooner if check standards indicate a problem. 

The calibration verification standard should be prepared weekly and stored at 4EC. When 

using premixed certified solutions, store according to the manufacturer's documented holding 

time and storage temperature recommendations. 

5.7 Surrogate standards - The recommended surrogates are phenol-d6, 2-fluorophenol, 

2,4,6-tribromophenol, nitrobenzene-d5, 2-fluorobiphenyl, and p-terphenyl-d14. See Method 3500 for 

instructions on preparing the surrogate solutions. 

5.7.1 Surrogate standard check - Determine what the appropriate concentration 

should be for the blank extracts 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 new surrogate spiking solution is 

prepared. 

NOTE:	 Method 3561 (SFE Extraction of PAHs) recommends the use of bromobenzene and 

p-quaterphenyl to better cover the range of PAHs listed in the method. 

5.7.2 If a more sensitive mass spectrometer is employed to achieve lower 

detection levels, a more dilute surrogate solution may be necessary. 

5.8 Matrix spike 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). 

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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/MS to determine recovery. It is recommended that this check be done whenever a 

new matrix spiking solution is prepared. 

5.8.2 If a more sensitive mass spectrometer is employed to achieve lower 

detection levels, a more dilute matrix and 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 a concentration 

appropriate for 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, Organic Analytes, Sec. 4.1. 

6.2 Store the sample extracts at -10EC, protected from light, in sealed vials (e.g., screwcap vials or crimp-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/MS analysis. 

Matrix Methods 

Air (particulates and sorbent resin) 3542 

Water (including TCLP leachates) 3510, 3520, 3535 

Soil/sediment 3540, 3541, 3545, 3550, 3560, 3561 

Waste 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-μL syringe may be appropriate. The detection limit is very high 

(approximately 10,000 μg/L). Therefore, it is only permitted where concentrations in excess 

of 10,000 μg/L are expected. 

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7.2 Extract cleanup - Extracts may be cleaned up by any of the following methods prior 

to GC/MS analysis. 

Analytes of interest	 Methods 

Aniline & aniline derivatives 3620
 

Phenols 3630, 3640, 8041a
 

Phthalate esters 3610, 3620, 3640
 

Nitrosamines 3610, 3620, 3640
 

Organochlorine pesticides & PCBs 3610, 3620, 3630, 3660, 3665
 

Nitroaromatics and cyclic ketones 3620, 3640
 

Polynuclear aromatic hydrocarbons 3611, 3630, 3640
 

Haloethers 3620, 3640
 

Chlorinated hydrocarbons 3620, 3640
 

Organophosphorus pesticides 3620
 

Petroleum waste 3611, 3650
 

All base, neutral, and acid 

priority pollutants	 3640 

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

are encountered on GC/FID. 

7.3 Initial calibration 

Establish the GC/MS operating conditions, using the following recommendations as guidance. 

Mass range: 35-500 amu 

Scan time: 1 sec/scan 

Initial temperature: 40EC, hold for 4 minutes

 Temperature program: 40-270EC at 10EC/min 

Final temperature: 270EC, hold until benzo[g,h,i]perylene elutes 

Injector temperature: 250-300EC 

Transfer line temperature: 250-300EC 

Source temperature: According to manufacturer's specifications 

Injector: Grob-type, splitless 

Injection volume: 1-2 μL 

Carrier gas: Hydrogen at 50 cm/sec or helium at 30 cm/sec 

Ion trap only: Set axial modulation, manifold temperature, and emission 

current to manufacturer's recommendations 

Split injection is allowed if the sensitivity of the mass spectrometer is sufficient. 

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 

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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, or manufacturer'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 

DDE and DDD 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 necessary to 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 of 0.80-1.20 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 μL 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 as follows: 

RF ' As × Cis 

Ais × Cs 

where: 

As = Peak area (or height) of the analyte or surrogate. 

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Ais = Peak area (or height) of the internal standard.
 

Cs = Concentration of the analyte or surrogate, in μg/L.
 

Cis = Concentration of the internal standard, in μg/L.
 

7.3.4 System performance check compounds (SPCCs) 

7.3.4.1 A system performance check must be performed to ensure that 

minimum average RFs are met before the calibration curve is used. For semivolatiles, 

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 system begins to deteriorate or the standard 

material begins to deteriorate. They are usually the first to show poor performance. 

Therefore, they must meet the minimum requirement when 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 (CCCs) 

7.3.5.1 The purpose of the CCCs are to evaluate the calibration from the 

standpoint of the integrity of the system. High variability for these compounds may be 

indicative of system leaks or reactive sites on the column. Meeting the CCC 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 factor and 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 CCC (see Table 4) must be less than or equal to 30%. 

n n

j RFi j (RFi

&RF)

2 

mean RF ' RF ' i'1 i'1 

SD ' n n&1 

SD RSD ' × 100
 

RF
 

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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 RRT ' Retention time of the internal standard 

7.3.7 Linearity of target analytes - If the RSD of any target analytes 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 is greater than 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 of sufficient 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 diagnostic tool. 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 of samples 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-hour shift during which samples are analyzed. 

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 midpoint concentration for the calibrating range of the GC/MS. The 

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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 and calibration verification acceptance criteria for 

the project can be met without interferences. 

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 

demonstrate that the contamination is not a result of carryover from standards or samples. 

See Sec. 8.0 of Method 8000B for method blank performance criteria. 

7.4.4	 System performance check compounds (SPCCs) 

7.4.4.1 A system performance check must be made during every 12-hour 

analytical shift. Each SPCC in the calibration verification standard must meet a 

minimum response factor of 0.050. This is the same check that is applied during the 

initial calibration. 

7.4.4.2 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. 

7.4.5	 Calibration check compounds (CCCs) 

7.4.5.1 After the system performance check is met, the CCCs listed in 

Table 4 are used to check the validity of the 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 CCC 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% difference or drift) for any one CCC, then corrective action must be 

taken prior to the analysis of samples. If the CCCs are not included in the list of 

analytes 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 to those listed under SPCCs could affect the 

CCCs. If the problem cannot be corrected by other measures, a new initial calibration 

must be generated. The CCC criteria must be met before sample analysis begins. 

7.4.6 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-point standard level of the most recent initial calibration 

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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 - If the EICP area for any of the internal standards 

in the calibration verification standard changes by a factor of 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 of samples analyzed while the system 

was malfunctioning is required. 

7.5 GC/MS analysis 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/MS system. 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 10 μL of the internal standard solution to the 1-mL concentrated sample extract obtained 

from sample preparation. 

7.5.3 Inject a 1-2 μL aliquot of the sample extract into the GC/MS system, 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/MS system 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/MS system, 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 (40 ng/μL, unless a more sensitive GC/MS system is being used). 

Secondary ion quantitation should be used only when there are sample interferences with the 

primary ion. 

NOTE:	 It may be a useful diagnostic tool to monitor internal standard retention times and 

responses (area counts) in all samples, spikes, blanks, and standards to effectively 

check drifting method performance, poor injection execution, and anticipate the 

need for system inspection and/or maintenance. 

7.5.4.1 When ions from a compound in the sample saturate the detector, 

this analysis must be followed by the analysis of an instrument blank consisting of 

clean solvent. If the blank analysis is not free of interferences, then the system must 

be decontaminated. Sample analysis may not resume until the blank analysis is 

demonstrated to be free of interferences. 

7.5.4.2 All dilutions should keep the response of the major constituents 

(previously saturated peaks) in the upper half of the linear range of the curve. 

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7.5.5 The use of selected ion monitoring (SIM) is acceptable for applications 

requiring detection limits below the normal range of electron impact mass spectrometry. 

However, SIM may provide a lesser degree of confidence in 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 

characteristic ions from the reference mass spectrum are defined as the three ions of greatest 

relative intensity, or any ions over 30% relative intensity, if less than 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 target chromatographic 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 relative intensities of 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 Structural isomers that produce very similar mass spectra should 

be identified as individual isomers if they have sufficiently different GC retention times. 

Sufficient GC resolution 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 

isomers are identified as isomeric pairs. Diastereomeric pairs (e.g., Aramite and 

Isosafrol) 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 (i.e., a broadened peak with shoulder(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 selection of spectra and in qualitative identification of compounds. 

When analytes coelute (i.e., only one chromatographic peak is apparent), the 

identification criteria may be met, but each analyte spectrum will contain extraneous 

ions contributed by the coeluting compound. 

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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 RCRA 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, the quantitation 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 (&R&F) from 

initial calibration data (Sec. 7.3.5). See Method 8000, Sec. 7.0, for the equations describing 

internal standard calibration and either linear or non-linear calibrations. 

7.7.3 Where applicable, the concentration of any non-target analytes identified in 

the sample (Sec. 7.6.2) should be estimated. The same formulae should be used with the 

following modifications: The areas Ax and Ais should 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. 

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7.7.5 Quantitation of multicomponent 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/μL 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 GC resolution 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 isomers are 

quantitated as isomeric pairs. Diastereomeric pairs (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 the various sample preparation and/or 

sample introduction techniques can be found in Method 3500. Each laboratory should maintain 

a formal quality assurance program. The laboratory should also maintain records to document the 

quality of the data generated. 

8.2 Quality control procedures necessary to 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/MS system must be tuned to meet the DFTPP criteria discussed in 

Secs. 7.3.1 and 7.4.1. 

8.2.2 There must be an initial calibration of the GC/MS system as described in 

Sec. 7.3. 

8.2.3 The GC/MS system must meet the calibration verification acceptance criteria 

in Sec. 7.4, each 12 hours. 

8.2.4 The RRT of the sample component must fall within the RRT window of the 

standard component provided in Sec. 7.6.1. 

8.3 Initial demonstration of proficiency - Each laboratory must demonstrate initial 

proficiency with each sample preparation and determinative method combination it utilizes, by 

generating data of acceptable accuracy and precision for target analytes in a clean matrix. The 

laboratory must also repeat the following 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 

procedures for documenting the effect of the matrix on method performance (precision, accuracy, 

and detection limit). At a minimum, this includes the 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 - 23 Revision 4 

January 1998 
 

 

 

 

8.4.1 Before processing any samples, the analyst should demonstrate, through the 

analysis of a method blank, that interferences from the analytical system, glassware, and 

reagents are under control. Each time a set of samples 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 of sample preparation and 

measurement. 

8.4.2 Documenting the effect of the matrix should include the analysis of at least 

one matrix spike and one duplicate unspiked sample or one matrix spike/matrix spike 

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. If samples are not 

expected to contain target analytes, laboratories should use a matrix spike 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) matrix similar to the sample matrix 

and of the same weight or volume. The LCS is spiked with the same analytes at the same 

concentrations as the matrix spike. When the results of the matrix spike 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 procedures for 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 invaluable to 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. Questions that 

should be asked are: Do the peaks look normal? Is the response obtained comparable to the 

response from previous calibrations? Careful examination of the standard chromatogram can 

indicate whether the column is still performing acceptably, the injector is leaking, the injector 

septum needs replacing, etc. If any changes are made to the system (e.g., the column changed, 

a septum 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 most productive 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 

CD-ROM 8270D - 24 Revision 4 

January 1998 
 

 

 

wastewaters spiked at six concentrations ranging from 5 to 1,300 μg/L. Single operator accuracy 

and precision, and method accuracy were found to be directly related to the concentration of the 

analyte and essentially independent of the sample matrix. Linear equations to describe these 

relationships are presented in Table 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. (See Method 8000.) 

9.2 Chromatograms from 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 soil 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 Surrogate precision and accuracy data are presented in Table 11 from a field dynamic 

spiking study based on air sampling by Method 0010. The trapping media were 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 supplier that contained 57 

semivolatile organics at three concentrations (250, 2500, and 12,500 μg/kg) on three types of soil 

(clay, loam and sand). Spiked samples were extracted both by the Dionex Accelerated Solvent 

Extraction system and by the Perstorp Environmental SoxtecTM (automated Soxhlet). The data in 

Table 12 represent seven replicate extractions and analyses for each individual sample and were 

taken from reference 9. The average recoveries from the three matrices for all analytes and all 

replicates relative to the automated Soxhlet data are as follows: clay 96.8%, 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 laboratory precision and bias data using Method 3561 (SFE extraction of PAHs 

with a variable restrictor and solid trapping material) were obtained for the method analytes by the 

extraction of two certified reference materials ( EC-1, a lake sediment from Environment Canada 

and HS-3, a marine sediment from 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 three replicate extractions 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 a fixed restrictor and liquid trapping) were obtained for twelve of the method analytes 

CD-ROM 8270D - 25 Revision 4 

January 1998 
by the extraction of a certified reference material (a soil naturally contaminated with PAHs). The 

SFE instrument used for these extractions was a Dionex Model 703-M. Analysis was by GC/MS. 

Average recoveries from four replicate extractions range from 60 to 122% (overall average of 89%) 

based on the certified value. Following are the instrument conditions that were 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 - 80EC; Restrictor temperature - 120EC; 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 solidphase extraction of TCLP buffer solutions spiked at two levels and extracted using Method 3535. 

9.9 Table 18 contains multiple-laboratory data for solid-phase extraction of spiked 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 Report for EPA Contract 68-03-3102. 

4.	 Burke, J.A., "Gas Chromatography for Pesticide Residue Analysis: Some Practical Aspects", 

Journal of the Association of Official Analytical Chemists (AOAC), 48, 1037, 1965. 

5.	 Lucas, S.V., Kornfeld, R.A., "GC-MS Suitability Testing of RCRA Appendix VIII and Michigan 

List Analytes ", U.S. Environmental Protection Agency, Environmental Monitoring and Support 

Laboratory, Cincinnati, OH 45268, February 20, 1987, Contract No. 68-03-3224. 

6.	 Engel, T.M., Kornfeld, R.A., Warner, J.S., and Andrews, K.D., "Screening of Semivolatile 

Organic Compounds for 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., "Laboratory Validation of VOST and 

SemiVOST for Halogenated Hydrocarbons from 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. 

CD-ROM 8270D - 26 Revision 4 

January 1998 
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. 

10.	 Lee, H.B., Peart, T.E., Hong-You, R.L., and Gere, D.R., "Supercritical Carbon Dioxide 

Extraction of Polycyclic Aromatic Hydrocarbons from 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 Bestgate 

Road, Annapolis, MD 21401, December 12, 1994. 

12.	 Markell, C., "3M Data Submission to EPA," letter to B. Lesnik, June 27, 1995. 

CD-ROM 8270D - 27 Revision 4 

January 1998 
TABLE 1
 

CHARACTERISTIC IONS FOR SEMIVOLATILE COMPOUNDS
 

Retention Primary Secondary Ion(s) 

Compound Time (min) Ion 

2-Picoline 3.75a 93 66,92 

Aniline 5.68 93 66,65 

Phenol 5.77 94 65,66 

Bis(2-chloroethyl) ether 5.82 93 63,95 

2-Chlorophenol 5.97 128 64,130 

1,3-Dichlorobenzene 6.27 146 148,111 

1,4-Dichlorobenzene-d4 (IS) 6.35 152 150,115 

1,4-Dichlorobenzene 6.40 146 148,111 

Benzyl alcohol 6.78 108 79,77 

1,2-Dichlorobenzene 6.85 146 148,111 

N-Nitrosomethylethylamine 6.97 88 42,43,56 

Bis(2-chloroisopropyl) ether 7.22 45 77,121 

Ethyl carbamate 7.27 62 44,45,74 

Thiophenol (Benzenethiol) 7.42 110 66,109,84 

Methyl methanesulfonate 7.48 80 79,65,95 

N-Nitrosodi-n-propylamine 7.55 70 42,101,130 

Hexachloroethane 7.65 117 201,199 

Maleic anhydride 7.65 54 98,53,44 

Nitrobenzene 7.87 77 123,65 

Isophorone 8.53 82 95,138 

N-Nitrosodiethylamine 8.70 102 42,57,44,56 

2-Nitrophenol 8.75 139 109,65 

2,4-Dimethylphenol 9.03 122 107,121 

p-Benzoquinone 9.13 108 54,82,80 

Bis(2-chloroethoxy)methane 9.23 93 95,123 

Benzoic acid 9.38 122 105,77 

2,4-Dichlorophenol 9.48 162 164,98 

Trimethyl phosphate 9.53 110 79,95,109,140 

Ethyl methanesulfonate 9.62 79 109,97,45,65 

1,2,4-Trichlorobenzene 9.67 180 182,145 

Naphthalene-d8 (IS) 9.75 136 68 

Naphthalene 9.82 128 129,127 

Hexachlorobutadiene 10.43 225 223,227 

Tetraethyl pyrophosphate 11.07 99 155,127,81,109 

Diethyl sulfate 11.37 139 45,59,99,111,125 

4-Chloro-3-methylphenol 11.68 107 144,142 

2-Methylnaphthalene 11.87 142 141 

2-Methylphenol 12.40 107 108,77,79,90 

Hexachloropropene 12.45 213 211,215,117,106,141 

Hexachlorocyclopentadiene 12.60 237 235,272 

N-Nitrosopyrrolidine 12.65 100 41,42,68,69 

CD-ROM 8270D - 28 Revision 4 

January 1998 
TABLE 1 

(continued) 

Retention Primary Secondary Ion(s) 

Compound Time (min) Ion 

Acetophenone 12.67 105 71,51,120 

4-Methylphenol 12.82 107 108,77,79,90 

2,4,6-Trichlorophenol 12.85 196 198,200 

o-Toluidine 12.87 106 107,77,51,79 

3-Methylphenol 12.93 107 108,77,79,90 

2-Chloronaphthalene 13.30 162 127,164 

N-Nitrosopiperidine 13.55 114 42,55,56,41 

1,4-Phenylenediamine 13.62 108 80,53,54,52 

1-Chloronaphthalene 13.65a 162 127,164 

2-Nitroaniline 13.75 65 92,138 

5-Chloro-2-methylaniline 14.28 106 141,140,77,89 

Dimethyl phthalate 14.48 163 194,164 

Acenaphthylene 14.57 152 151,153 

2,6-Dinitrotoluene 14.62 165 63,89 

Phthalic anhydride 14.62 104 76,50,148 

o-Anisidine 15.00 108 80,123,52 

3-Nitroaniline 15.02 138 108,92 

Acenaphthene-d10 (IS) 15.05 164 162,160 

Acenaphthene 15.13 154 153,152 

2,4-Dinitrophenol 15.35 184 63,154 

2,6-Dinitrophenol 15.47 162 164,126,98,63 

4-Chloroaniline 15.50 127 129,65,92 

Isosafrole 15.60 162 131,104,77,51 

Dibenzofuran 15.63 168 139 

2,4-Diaminotoluene 15.78 121 122,94,77,104 

2,4-Dinitrotoluene 15.80 165 63,89 

4-Nitrophenol 15.80 139 109,65 

2-Naphthylamine 16.00a 143 115,116 

1,4-Naphthoquinone 16.23 158 104,102,76,50,130 

p-Cresidine 16.45 122 94,137,77,93 

Dichlorovos 16.48 109 185,79,145 

Diethyl phthalate 16.70 149 177,150 

Fluorene 16.70 166 165,167 

2,4,5-Trimethylaniline 16.70 120 135,134,91,77 

N-Nitrosodi-n-butylamine 16.73 84 57,41,116,158 

4-Chlorophenyl phenyl ether 16.78 204 206,141 

Hydroquinone 16.93 110 81,53,55 

4,6-Dinitro-2-methylphenol 17.05 198 51,105 

Resorcinol 17.13 110 81,82,53,69 

N-Nitrosodiphenylamine 17.17 169 168,167 

Safrole 17.23 162 104,77,103,135 

Hexamethyl phosphoramide 17.33 135 44,179,92,42 

CD-ROM 8270D - 29 Revision 4 

January 1998 
TABLE 1 

(continued) 

Retention Primary Secondary Ion(s) 

Compound Time (min) Ion 

3-(Chloromethyl)pyridine hydrochloride 17.50 92 127,129,65,39 

Diphenylamine 17.54a 169 168,167 

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 

Hexachlorobenzene 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-d10 (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 

CD-ROM 8270D - 30 Revision 4 

January 1998 
TABLE 1 

(continued) 

Compound 

Retention 

Time (min) 

Primary 

Ion 

Secondary Ion(s) 

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 

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 

α,α-Dimethylphenylamine 25.43 58 91,65,134,42 

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-d12 (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 

CD-ROM 8270D - 31 Revision 4 

January 1998 
TABLE 1 

(continued) 

Retention Primary Secondary Ion(s) 

Compound Time (min) Ion 

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 

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 phosphateb 32.75 368 367,107,165,198 

Benzo(a)pyrene 32.80 252 253,125 

Perylene-d12 (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 

CD-ROM 8270D - 32 Revision 4 

January 1998 
TABLE 1 

(continued) 

Retention Primary Secondary Ion(s) 

Compound Time (min) Ion 

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 

Aroclor 1232 -- 190 224,260 

Aroclor 1242 -- 222 256,292 

Aroclor 1248 -- 292 362,326 

Aroclor 1254 -- 292 362,326 

Aroclor 1260 -- 360 362,394 

α-BHC -- 183 181,109 

β-BHC -- 181 183,109 

δ-BHC -- 183 181,109 

γ-BHC (Lindane) -- 183 181,109 

4,4'-DDD -- 235 237,165 

4,4'-DDE -- 246 248,176 

4,4'-DDT -- 235 237,165 

Dieldrin -- 79 263,279 

1,2-Diphenylhydrazine -- 77 105,182 

Endosulfan I -- 195 339,341 

Endosulfan II -- 337 339,341 

Endosulfan sulfate -- 272 387,422 

Endrin -- 263 82,81 

Endrin aldehyde -- 67 345,250 

Endrin ketone -- 317 67,319 

2-Fluorobiphenyl (surr) -- 172 171 

2-Fluorophenol (surr) -- 112 64 

Heptachlor -- 100 272,274 

Heptachlor epoxide -- 353 355,351 

Nitrobenzene-d5 (surr) -- 82 128,54 

N-Nitrosodimethylamine -- 42 74,44 

Phenol-d6 (surr) -- 99 42,71 

Terphenyl-d14 (surr) -- 244 122,212 

2,4,6-Tribromophenol (surr) -- 330 332,141 

Toxaphene -- 159 231,233 

IS = internal standard 

surr = surrogate 

a

Estimated retention times 

b

Substitute for the non-specific mixture, tricresyl phosphate 

CD-ROM 8270D - 33 Revision 4 

January 1998 
TABLE 2
 

ESTIMATED QUANTITATION LIMITS (EQLs) FOR SEMIVOLATILE ORGANICS
 

Estimated Quantitation Limitsa 

Compound 

Ground water 

(μg/L) 

Low Soil/Sedimentb 

(μg/kg) 

Acenaphthene 10 660 

Acenaphthylene 10 660 

Acetophenone 10 ND 

2-Acetylaminofluorene 20 ND 

1-Acetyl-2-thiourea 1000 ND 

2-Aminoanthraquinone 20 ND 

Aminoazobenzene 10 ND 

4-Aminobiphenyl 20 ND 

Anilazine 100 ND 

o-Anisidine 10 ND 

Anthracene 10 660 

Aramite 20 ND 

Azinphos-methyl 100 ND 

Barban 200 ND 

Benz(a)anthracene 10 660 

Benzo(b)fluoranthene 10 660 

Benzo(k)fluoranthene 10 660 

Benzoic acid 50 3300 

Benzo(g,h,i)perylene 10 660 

Benzo(a)pyrene 10 660 

p-Benzoquinone 10 ND 

Benzyl alcohol 20 1300 

Bis(2-chloroethoxy)methane 10 660 

Bis(2-chloroethyl) ether 10 660 

Bis(2-chloroisopropyl) ether 10 660 

4-Bromophenyl phenyl ether 10 660 

Bromoxynil 10 ND 

Butyl benzyl phthalate 10 660 

Captafol 20 ND 

Captan 50 ND 

Carbaryl 10 ND 

Carbofuran 10 ND 

Carbophenothion 10 ND 

Chlorfenvinphos 20 ND 

4-Chloroaniline 20 1300 

Chlorobenzilate 10 ND 

CD-ROM 8270D - 34 Revision 4 

January 1998 
TABLE 2 

(Continued) 

Estimated Quantitation Limitsa 

Compound 

Ground water 

(μg/L) 

Low Soil/Sedimentb 

(μg/kg) 

5-Chloro-2-methylaniline 10 ND 

4-Chloro-3-methylphenol 20 1300 

3-(Chloromethyl)pyridine hydrochloride 100 ND 

2-Chloronaphthalene 10 660 

2-Chlorophenol 10 660 

4-Chlorophenyl phenyl ether 10 660 

Chrysene 10 660 

Coumaphos 40 ND 

p-Cresidine 10 ND 

Crotoxyphos 20 ND 

2-Cyclohexyl-4,6-dinitrophenol 100 ND 

Demeton-O 10 ND 

Demeton-S 10 ND 

Diallate (cis or trans) 10 ND 

Diallate (trans or cis) 10 ND 

2,4-Diaminotoluene 20 ND 

Dibenz(a,j)acridine 10 ND 

Dibenz(a,h)anthracene 10 660 

Dibenzofuran 10 660 

Dibenzo(a,e)pyrene 10 ND 

Di-n-butyl phthalate 10 ND 

Dichlone NA ND 

1,2-Dichlorobenzene 10 660 

1,3-Dichlorobenzene 10 660 

1,4-Dichlorobenzene 10 660 

3,3'-Dichlorobenzidine 20 1300 

2,4-Dichlorophenol 10 660 

2,6-Dichlorophenol 10 ND 

Dichlorovos 10 ND 

Dicrotophos 10 ND 

Diethyl phthalate 10 660 

Diethylstilbestrol 20 ND 

Diethyl sulfate 100 ND 

Dimethoate 20 ND 

3,3'-Dimethoxybenzidine 100 ND 

Dimethylaminoazobenzene 10 ND 

7,12-Dimethylbenz(a)anthracene 10 ND 

CD-ROM 8270D - 35 Revision 4 

January 1998 
TABLE 2 

(Continued) 

Estimated Quantitation Limitsa 

Compound 

Ground water 

(μg/L) 

Low Soil/Sedimentb 

(μg/kg) 

3,3'-Dimethylbenzidine 10 ND 

2,4-Dimethylphenol 10 660 

Dimethyl phthalate 10 660 

1,2-Dinitrobenzene 40 ND 

1,3-Dinitrobenzene 20 ND 

1,4-Dinitrobenzene 40 ND 

4,6-Dinitro-2-methylphenol 50 3300 

2,4-Dinitrophenol 50 3300 

2,4-Dinitrotoluene 10 660 

2,6-Dinitrotoluene 10 660 

Dinocap 100 ND 

Dinoseb 20 ND 

5,5-Diphenylhydantoin 20 ND 

Di-n-octyl phthalate 10 660 

Disulfoton 10 ND 

EPN 10 ND 

Ethion 10 ND 

Ethyl carbamate 50 ND 

Bis(2-ethylhexyl) phthalate 10 660 

Ethyl methanesulfonate 20 ND 

Famphur 20 ND 

Fensulfothion 40 ND 

Fenthion 10 ND 

Fluchloralin 20 ND 

Fluoranthene 10 660 

Fluorene 10 660 

Hexachlorobenzene 10 660 

Hexachlorobutadiene 10 660 

Hexachlorocyclopentadiene 10 660 

Hexachloroethane 10 660 

Hexachlorophene 50 ND 

Hexachloropropene 10 ND 

Hexamethylphosphoramide 20 ND 

Indeno(1,2,3-cd)pyrene 10 660 

Isodrin 20 ND 

Isophorone 10 660 

Isosafrole 10 ND 

CD-ROM 8270D - 36 Revision 4 

January 1998 
TABLE 2 

(Continued) 

Estimated Quantitation Limitsa 

Compound 

Ground water 

(μg/L) 

Low Soil/Sedimentb 

(μg/kg) 

Kepone 20 ND 

Leptophos 10 ND 

Malathion 50 ND 

Mestranol 20 ND 

Methapyrilene 100 ND 

Methoxychlor 10 ND 

3-Methylcholanthrene 10 ND 

Methyl methanesulfonate 10 ND 

2-Methylnaphthalene 10 660 

Methyl parathion 10 ND 

2-Methylphenol 10 660 

3-Methylphenol 10 ND 

4-Methylphenol 10 660 

Mevinphos 10 ND 

Mexacarbate 20 ND 

Mirex 10 ND 

Monocrotophos 40 ND 

Naled 20 ND 

Naphthalene 10 660 

1,4-Naphthoquinone 10 ND 

1-Naphthylamine 10 ND 

2-Naphthylamine 10 ND 

Nicotine 20 ND 

5-Nitroacenaphthene 10 ND 

2-Nitroaniline 50 3300 

3-Nitroaniline 50 3300 

4-Nitroaniline 20 ND 

5-Nitro-o-anisidine 10 ND 

Nitrobenzene 10 660 

4-Nitrobiphenyl 10 ND 

Nitrofen 20 ND 

2-Nitrophenol 10 660 

4-Nitrophenol 50 3300 

5-Nitro-o-toluidine 10 ND 

4-Nitroquinoline-1-oxide 40 ND 

N-Nitrosodi-n-butylamine 10 ND 

N-Nitrosodiethylamine 20 ND 

CD-ROM 8270D - 37 Revision 4 

January 1998 
TABLE 2 

(Continued) 

Estimated Quantitation Limitsa 

Compound 

Ground water 

(μg/L) 

Low Soil/Sedimentb 

(μg/kg) 

N-Nitrosodiphenylamine 10 660 

N-Nitroso-di-n-propylamine 10 660 

N-Nitrosopiperidine 20 ND 

N-Nitrosopyrrolidine 40 ND 

Octamethyl pyrophosphoramide 200 ND 

4,4'-Oxydianiline 20 ND 

Parathion 10 ND 

Pentachlorobenzene 10 ND 

Pentachloronitrobenzene 20 ND 

Pentachlorophenol 50 3300 

Phenacetin 20 ND 

Phenanthrene 10 660 

Phenobarbital 10 ND 

Phenol 10 660 

1,4-Phenylenediamine 10 ND 

Phorate 10 ND 

Phosalone 100 ND 

Phosmet 40 ND 

Phosphamidon 100 ND 

Phthalic anhydride 100 ND 

2-Picoline ND ND 

Piperonyl sulfoxide 100 ND 

Pronamide 10 ND 

Propylthiouracil 100 ND 

Pyrene 10 660 

Resorcinol 100 ND 

Safrole 10 ND 

Strychnine 40 ND 

Sulfallate 10 ND 

Terbufos 20 ND 

1,2,4,5-Tetrachlorobenzene 10 ND 

2,3,4,6-Tetrachlorophenol 10 ND 

Tetrachlorvinphos 20 ND 

Tetraethyl pyrophosphate 40 ND 

Thionazine 20 ND 

Thiophenol (Benzenethiol) 20 ND 

o-Toluidine 10 ND 

CD-ROM 8270D - 38 Revision 4 

January 1998 
 

TABLE 2 

(Continued) 

Estimated Quantitation Limitsa 

Compound 

Ground water 

(μg/L) 

Low Soil/Sedimentb 

(μg/kg) 

1,2,4-Trichlorobenzene 10 660 

2,4,5-Trichlorophenol 10 660 

2,4,6-Trichlorophenol 10 660 

Trifluralin 10 ND 

2,4,5-Trimethylaniline 10 ND 

Trimethyl phosphate 10 ND 

1,3,5-Trinitrobenzene 10 ND 

Tris(2,3-dibromopropyl) phosphate 200 ND 

Tri-p-tolyl phosphate(h) 10 ND 

a	 Sample EQLs are highly 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 higher based on the % dry weight of each sample. These 

EQLs are based on a 30-g sample and gel permeation chromatography cleanup. 

ND = Not Determined 

NA = Not Applicable 

Other Matrices	 Factorc 

High-concentration soil and sludges by ultrasonic extractor 7.5 

Non-water miscible waste 75 

c

EQL = (EQL for Low Soil/Sediment given above in Table 2) x (Factor) 

CD-ROM 8270D - 39 Revision 4 

January 1998 
TABLE 3
 

DFTPP KEY IONS AND ION ABUNDANCE CRITERIAa,b
 

Mass Ion Abundance Criteria 

51 30-60% of mass 198
 

68 < 2% of mass 69
 

70 < 2% of mass 69
 

127 40-60% of mass 198 

197 < 1% of mass 198 

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. 

TABLE 4 

CALIBRATION CHECK COMPOUNDS (CCC) 

Base/Neutral Fraction Acid Fraction 

Acenaphthene 

1,4-Dichlorobenzene 

Hexachlorobutadiene 

Diphenylamine 

Di-n-octyl phthalate 

Fluoranthene 

Benzo(a)pyrene 

4-Chloro-3-methylphenol 

2,4-Dichlorophenol 

2-Nitrophenol 

Phenol 

Pentachlorophenol 

2,4,6-Trichlorophenol 

CD-ROM 8270D - 40 Revision 4 

January 1998 
TABLE 5
 

SEMIVOLATILE INTERNAL STANDARDS WITH CORRESPONDING ANALYTES
 

ASSIGNED FOR QUANTITATION
 

1,4-Dichlorobenzene-d4 Naphthalene-d8 Acenaphthene-d10 

Aniline Acetophenone Acenaphthene 

Benzyl alcohol Benzoic acid Acenaphthylene 

Bis(2-chloroethyl) ether Bis(2-chloroethoxy)methane 1-Chloronaphthalene 

Bis(2-chloroisopropyl) ether 4-Chloroaniline 2-Chloronaphthalene 

2-Chlorophenol 4-Chloro-3-methylphenol 4-Chlorophenyl phenyl ether 

1,3-Dichlorobenzene 2,4-Dichlorophenol Dibenzofuran 

1,4-Dichlorobenzene 2,6-Dichlorophenol Diethyl phthalate 

1,2-Dichlorobenzene α,α-Dimethyl- Dimethyl phthalate 

Ethyl methanesulfonate phenethylamine 2,4-Dinitrophenol 

2-Fluorophenol (surr) 2,4-Dimethylphenol 2,4-Dinitrotoluene 

Hexachloroethane Hexachlorobutadiene 2,6-Dinitrotoluene 

Methyl methanesulfonate Isophorone Fluorene 

2-Methylphenol 2-Methylnaphthalene 2-Fluorobiphenyl (surr) 

4-Methylphenol Naphthalene Hexachlorocyclopentadiene 

N-Nitrosodimethylamine Nitrobenzene 1-Naphthylamine 

N-Nitroso-di-n-propylamine Nitrobenzene-d8 (surr) 2-Naphthylamine 

Phenol 2-Nitrophenol 2-Nitroaniline 

Phenol-d6 (surr) N-Nitrosodi-n-butylamine 3-Nitroaniline 

2-Picoline N-Nitrosopiperidine 4-Nitroaniline 

1,2,4-Trichlorobenzene 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 

(surr) = surrogate 

CD-ROM 8270D - 41 Revision 4 

January 1998 
TABLE 5 

(continued) 

Phenanthrene-d10 Chrysene-d12 Perylene-d12 

4-Aminobiphenyl Benzidine Benzo(b)fluoranthene 

Anthracene Benzo(a)anthracene Benzo(k)fluoranthene 

4-Bromophenyl phenyl 

ether 

Bis(2-ethylhexyl) phthalate Benzo(g,h,i)perylene 

Di-n-butyl phthalate Butyl benzyl phthalate Benzo(a)pyrene 

4,6-Dinitro-2-methylphenol Chrysene Dibenz(a,j)acridine 

Diphenylamine 3,3'-Dichlorobenzidine Dibenz(a,h)anthracene 

Fluoranthene p-Dimethyl aminoazobenzene 

Hexachlorobenzene Pyrene 

N-Nitrosodiphenylamine Terphenyl-d14 (surr) 

Pentachlorophenol 7,12-Dimethylbenz(a) 

anthracene 

Pentachloronitrobenzene Di-n-octyl phthalate 

Phenacetin Indeno(1,2,3-cd) pyrene 

Phenanthrene 3-Methylcholanthrene 

Pronamide 

(surr) = surrogate 

CD-ROM 8270D - 42 Revision 4 

January 1998 
TABLE 6
 

MULTILABORATORY PERFORMANCE DATAa 

Test conc. Limit for Range for x& Range 

Compound (μg/L) s (μg/L) (μg/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 D-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 D-195.0 D-219
 

Benzyl butyl phthalate 100 23.4 D-139.9 D-152
 

β-BHC 100 31.5 41.5-130.6 24-149
 

δ-BHC 100 21.6 D-100.0 D-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
 

4,4'-DDD 100 31.0 D-134.5 D-145
 

4,4'-DDE 100 32.0 19.2-119.7 4-136
 

4,4'-DDT 100 61.6 D-170.6 D-203
 

Dibenzo(a,h)anthracene 100 70.0 D-199.7 D-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 D-172
 

1,4-Dichlorobenzene 100 32.1 37.3-105.7 20-124
 

3,3'-Dichlorobenzidine 100 71.4 8.2-212.5 D-262
 

Dieldrin 100 30.7 44.3-119.3 29-136
 

Diethyl phthalate 100 26.5 D-100.0 D-114
 

Dimethyl phthalate 100 23.2 D-100.0 D-112
 

2,4-Dinitrotoluene 100 21.8 47.5-126.9 39-139
 

2,6-Dinitrotoluene 100 29.6 68.1-136.7 50-158
 

Di-n-octyl phthalate 100 31.4 18.6-131.8 4-146
 

Endosulfan sulfate 100 16.7 D-103.5 D-107
 

Endrin aldehyde 100 32.5 D-188.8 D-209
 

Fluoranthene 100 32.8 42.9-121.3 26-137
 

CD-ROM 8270D - 43 Revision 4 

January 1998 
TABLE 6 

(continued) 

Compound 

Test conc. 

(μg/L) 

Limit for 

s (μg/L) 

Range for x&

(μg/L) 

Range 

p, ps (%) 

Fluorene 100 20.7 71.6-108.4 59-121 

Heptachlor 100 37.2 D-172.2 D-192 

Heptachlor epoxide 100 54.7 70.9-109.4 26.155 

Hexachlorobenzene 100 24.9 7.8-141.5 D-152 

Hexachlorobutadiene 100 26.3 37.8-102.2 24-116 

Hexachloroethane 100 24.5 55.2-100.0 40-113 

Indeno(1,2,3-cd)pyrene 100 44.6 D-150.9 D-171 

Isophorone 100 63.3 46.6-180.2 21-196 

Naphthalene 100 30.1 35.6-119.6 21-133 

Nitrobenzene 100 39.3 54.3-157.6 35-180 

N-Nitrosodi-n-propylamine 100 55.4 13.6-197.9 D-230 

Aroclor 1260 100 54.2 19.3-121.0 D-164 

Phenanthrene 100 20.6 65.2-108.7 54-120 

Pyrene 100 25.2 69.6-100.0 52-115 

1,2,4-Trichlorobenzene 100 28.1 57.3-129.2 44-142 

4-Chloro-3-methylphenol 100 37.2 40.8-127.9 22-147 

2-Chlorophenol 100 28.7 36.2-120.4 23-134 

2,4-Chlorophenol 100 26.4 52.5-121.7 39-135 

2,4-Dimethylphenol 100 26.1 41.8-109.0 32-119 

2,4-Dinitrophenol 100 49.8 D-172.9 D-191 

2-Methyl-4,6-dinitrophenol 100 93.2 53.0-100.0 D-181 

2-Nitrophenol 100 35.2 45.0-166.7 29-182 

4-Nitrophenol 100 47.2 13.0-106.5 D-132 

Pentachlorophenol 100 48.9 38.1-151.8 14-176 

Phenol 100 22.6 16.6-100.0 5-112 

2,4,6-Trichlorophenol 100 31.7 52.4-129.2 37-144 

s = Standard deviation of four recovery measurements, in μg/L 

&x = Average recovery for four recovery measurements, in μg/L 

p, ps = Measured percent recovery 

D = Detected; result must be greater than zero 

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. 

CD-ROM 8270D - 44 Revision 4 

January 1998 
TABLE 7
 

METHOD ACCURACY AND PRECISION AS FUNCTIONS OF CONCENTRATIONa
 

Accuracy, as Single analyst Overall precision, 

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 

β-BHC 

δ-BHC 

Bis(2-chloroethyl) ether 

Bis(2­

recovery, x’ (μg/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 

precision, sr

’ (μg/L) 

0.15 x&-0.12 

0.24 x&-1.06 

0.27 x&-1.28 

0.21 x&-0.32 

0.15 x&+0.93 

0.22 x&+0.43 

0.19 x&+1.03 

0.22 x&+0.48 

0.29 x&+2.40 

0.18 x&+0.94 

0.20 x&-0.58 

0.34 x&+0.86 

0.35 x&-0.99 

0.16 x&+1.34 

S’ (μg/L) 

0.21 x&-0.67 

0.26 x&-0.54 

0.43 x&+1.13 

0.27 x&-0.64 

0.26 x&-0.21 

0.29 x&+0.96 

0.35 x&+0.40 

0.32 x&+1.35 

0.51 x&-0.44 

0.53 x&+0.92 

0.30 x&+1.94 

0.93 x&-0.17 

0.35 x&+0.10 

0.26 x&+2.01 

chloroethoxy)methane 

Bis(2-chloroisopropyl) ether 

Bis(2-ethylhexyl) phthalate 

4-Bromophenyl phenyl 

1.03C-2.31 

0.84C-1.18 

0.91C-1.34 

0.24 x&+0.28 

0.26 x&+0.73 

0.13 x&+0.66 

0.25 x&+1.04 

0.36 x&+0.67 

0.16 x&+0.66 

ether 

2-Chloronaphthalene 

4-Chlorophenyl phenyl 

0.89C+0.01 

0.91C+0.53 

0.07 x&+0.52 

0.20 x&-0.94 

0.13 x&+0.34 

0.30 x&-0.46 

ether 

Chrysene 

4,4'-DDD 

4,4'-DDE 

4,4'-DDT 

Dibenzo(a,h)anthracene 

Di-n-butyl phthalate 

1,2-Dichlorobenzene 

1,3-Dichlorobenzene 

1,4-Dichlorobenzene 

3,3'-Dichlorobenzidine 

Dieldrin 

Diethyl phthalate 

Dimethyl phthalate 

2,4-Dinitrotoluene 

2,6-Dinitrotoluene 

Di-n-octyl phthalate 

Endosulfan sulfate 

Endrin aldehyde 

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 

0.28 x&+0.13 

0.29 x&-0.32 

0.26 x&-1.17 

0.42 x&+0.19 

0.30 x&+8.51 

0.13 x&+1.16 

0.20 x&+0.47 

0.25 x&+0.68 

0.24 x&+0.23 

0.28 x&+7.33 

0.20 x&-0.16 

0.28 x&+1.44 

0.54 x&+0.19 

0.12 x&+1.06 

0.14 x&+1.26 

0.21 x&+1.19 

0.12 x&+2.47 

0.18 x&+3.91 

0.33 x&-0.09 

0.66 x&-0.96 

0.39 x&-1.04 

0.65 x&-0.58 

0.59 x&+0.25 

0.39 x&+0.60 

0.24 x&+0.39 

0.41 x&+0.11 

0.29 x&+0.36 

0.47 x&+3.45 

0.26 x&-0.07 

0.52 x&+0.22 

1.05 x&-0.92 

0.21 x&+1.50 

0.19 x&+0.35 

0.37 x&+1.19 

0.63 x&-1.03 

0.73 x&-0.62 

CD-ROM 8270D - 45 Revision 4 

January 1998 
TABLE 7 

(Continued) 

Accuracy, as Single analyst Overall precision, 

Compound 

Fluoranthene 

Fluorene 

Heptachlor 

Heptachlor epoxide 

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-Dichlorophenol 

2,4-Dimethylphenol 

2,4-Dinitrophenol 

2-Methyl-4,6-dinitrophenol 

2-Nitrophenol 

4-Nitrophenol 

Pentachlorophenol 

Phenol 

2,4,6-Trichlorophenol 

recovery, x’ (μg/L) 

0.81C+1.10 

0.90C-0.00 

0.87C-2.97 

0.92C-1.87 

0.74C+0.66 

0.71C-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 

precision, sr

’ (μg/L) 

0.22 x&-0.73 

0.12 x&+0.26 

0.24 x&-0.56 

0.33 x&-0.46 

0.18 x&-0.10 

0.19 x&+0.92 

0.17 x&+0.67 

0.29 x&+1.46 

0.27 x&+0.77 

0.21 x&-0.41 

0.19 x&+0.92 

0.27 x&+0.68 

0.35 x&+3.61 

0.12 x&+0.57 

0.16 x&+0.06 

0.15 x&+0.85 

0.23 x&+0.75 

0.18 x&+1.46 

0.15 x&+1.25 

0.16 x&+1.21 

0.38 x&+2.36 

0.10 x&+42.29 

0.16 x&+1.94 

0.38 x&+2.57 

0.24 x&+3.03 

0.26 x&+0.73 

0.16 x&+2.22 

S’ (μg/L) 

0.28 x&-0.60 

0.13 x&+0.61 

0.50 x&-0.23 

0.28 x&+0.64 

0.43 x&-0.52 

0.26 x&+0.49 

0.17 x&+0.80 

0.50 x&-0.44 

0.33 x&+0.26 

0.30 x&-0.68 

0.27 x&+0.21 

0.44 x&+0.47 

0.43 x&+1.82 

0.15 x&+0.25 

0.15 x&+0.31 

0.21 x&+0.39 

0.29 x&+1.31 

0.28 x&+0.97 

0.21 x&+1.28 

0.22 x&+1.31 

0.42 x&+26.29 

0.26 x&+23.10 

0.27 x&+2.60 

0.44 x&+3.24 

0.30 x&+4.33 

0.35 x&+0.58 

0.22 x&+1.81 

x' =	 Expected recovery for one or more measurements of a sample containing a concentration 

of C, in μg/L. 

sr

' =	 Expected single analyst standard deviation of measurements at an average concentration 

of x&, in μg/L. 

S' =	 Expected interlaboratory standard deviation of measurements at an average concentration 

found of x&, in μg/L. 

C =	 True value for the concentration, in μg/L.

&x = Average recovery found for measurements of samples containing a concentration of C, in 

μg/L. 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. 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. 

CD-ROM 8270D - 46 Revision 4 

January 1998 
TABLE 8
 

EXTRACTION EFFICIENCY AND 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-chloropropane 97 2 98 5 

Dinoseb 99 3 97 6 

Parathion 100 2 103 4 

4,4'-Methylenebis(N,N- 108 4 90 4 

dimethylaniline) 

5-Nitro-o-toluidine 99 10 93 4 

2-Picoline 80 4 83 4 

Tetraethyl dithiopyrophosphate 92 7 70 1 

Data taken from Reference 6. 

CD-ROM 8270D - 47 Revision 4 

January 1998 
TABLE 9 

MEAN PERCENT RECOVERIES AND PERCENT RSD VALUES FOR SEMIVOLATILE
 

ORGANICS FROM SPIKED CLAY SOIL AND TOPSOIL BY AUTOMATED SOXHLET
 

EXTRACTION (METHOD 3541) WITH HEXANE-ACETONE (1:1)a
 

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 

Heptachlor epoxide 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 

a	 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-Dichlorophenyl-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 8270D - 48 Revision 4 

January 1998 
TABLE 10 

SINGLE LABORATORY ACCURACY AND PRECISION DATA FOR THE EXTRACTION
 

OF SEMIVOLATILE ORGANICS FROM SPIKED CLAY BY
 

AUTOMATED SOXHLET (METHOD 3541)a
 

Compound Mean Recovery RSD 

Phenol 47.8 5.6 

Bis(2-chloroethyl)ether 

2-Chlorophenol 

Benzyl alcohol 

2-Methylphenol 

Bis(2-chloroisopropyl)ether 

4-Methylphenol 

N-Nitroso-di-n-propylamine 

Nitrobenzene 

25.4 

42.7 

55.9 

17.6 

15.0 

23.4 

41.4 

28.2 

13 

4.3 

7.2 

6.6 

15 

6.7 

6.2 

7.7 

Isophorone 

2-Nitrophenol 

2,4-Dimethylphenol 

Benzoic acid 

56.1 

36.0 

50.1 

40.6 

4.2 

6.5 

5.7 

7.7 

Bis(2-chloroethoxy)methane 

2,4-Dichlorophenol 

1,2,4-Trichlorobenzene 

44.1 

55.6 

18.1 

3.0 

4.6 

31 

Naphthalene 

4-Chloroaniline 

26.2 

55.7 

15 

12 

4-Chloro-3-methylphenol 

2-Methylnaphthalene 

Hexachlorocyclopentadiene 

2,4,6-Trichlorophenol 

2,4,5-Trichlorophenol 

2-Chloronaphthalene 

2-Nitroaniline 

65.1 

47.0 

19.3 

70.2 

26.8 

61.2 

73.8 

5.1 

8.6 

19 

6.3 

2.9 

6.0 

6.0 

Dimethyl phthalate 

Acenaphthylene 

3-Nitroaniline 

74.6 

71.6 

77.6 

5.2 

5.7 

5.3 

Acenaphthene 

2,4-Dinitrophenol 

4-Nitrophenol 

Dibenzofuran 

79.2 

91.9 

62.9 

82.1 

4.0 

8.9 

16 

5.9 

2,4-Dinitrotoluene 84.2 5.4 

2,6-Dinitrotoluene 68.3 5.8 

Diethyl phthalate 

4-Chlorophenyl-phenyl ether 

74.9 

67.2 

5.4 

3.2 

CD-ROM 8270D - 49 Revision 4 

January 1998 
TABLE 10 

(continued) 

Compound Mean Recovery RSD 

Fluorene 82.1 3.4 

4-Nitroaniline 79.0 7.9 

4,6-Dinitro-2-methylphenol 63.4 6.8 

N-Nitrosodiphenylamine 77.0 3.4 

4-Bromophenyl-phenyl ether 62.4 3.0 

Hexachlorobenzene 72.6 3.7 

Pentachlorophenol 62.7 6.1 

Phenanthrene 83.9 5.4 

Anthracene 96.3 3.9 

Di-n-butyl phthalate 78.3 40 

Fluoranthene 87.7 6.9 

Pyrene 102 0.8 

Butyl benzyl phthalate 66.3 5.2 

3,3'-Dichlorobenzidine 25.2 11 

Benzo(a)anthracene 73.4 3.8 

Bis(2-ethylhexyl) phthalate 77.2 4.8 

Chrysene 76.2 4.4 

Di-n-octyl phthalate 83.1 4.8 

Benzo(b)fluoranthene 82.7 5.0 

Benzo(k)fluoranthene 71.7 4.1 

Benzo(a)pyrene 71.7 4.1 

Indeno(1,2,3-cd)pyrene 72.2 4.3 

Dibenzo(a,h)anthracene 66.7 6.3 

Benzo(g,h,i)perylene 63.9 8.0 

1,2-Dichlorobenzene 0 -­

1,3-Dichlorobenzene 0 -­

1,4-Dichlorobenzene 0 -­

Hexachloroethane 0 --

Hexachlorobutadiene 0 -­

a	 Number of determinations was three. The operating conditions for the Soxtec apparatus were 

as follows: immersion time 45 min; extraction time 45 min; the sample size was 10 g clay soil; 

the spike concentration was 6 mg/kg per compound. The sample was allowed to equilibrate 1 

hour after spiking. 

Data taken from Reference 7. 

CD-ROM 8270D - 50 Revision 4 

January 1998 
TABLE 11
 

PRECISION AND BIAS VALUES FOR METHOD 35421
 

Compound Mean Recovery Standard Deviation % RSD 

2-Fluorophenol 74.6 28.6 38.3 

Phenol-d5 77.8 27.7 35.6 

Nitrobenzene-d5 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-d14 78.6 32.4 41.3 

1

 The surrogate values shown in Table 11 represent mean recoveries for surrogates in all 

Method 0010 matrices in a field dynamic spiking study. 

CD-ROM 8270D - 51 Revision 4 

January 1998 
TABLE 12
 

ACCELERATED SOLVENT EXTRACTION (METHOD 3545) RECOVERY VALUES
 

AS PERCENT OF 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 

Hexachlorocyclopentadien 100.0 100.0 0.0 100.0 100.0 6.8 100.0 100.0 *238.3 75.8 

e 

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 8270D - 52 Revision 4 

January 1998 
TABLE 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 92.2 111.4 113.8 92.7 90.4 98.8 

4-Chlorophenyl phenyl 

ether 

83.0 94.5 98.7 95.7 94.3 94.2 111.4 87.7 90.3 94.4 

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)fluoranthene 106.6 109.9 75.6 121.7 100.7 93.9 106.9 81.9 93.6 99.0 

Benzo(k)fluoranthene 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 90.4 133.6 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,i)perylene 98.0 0.0 81.2 0.0 33.6 78.6 128.7 83.0 94.2 66.4 

Mean 95.1 94.3 101.0 95.5 96.5 104.1 113.0 100.9 92.5 

* Values greater than 150% were not used to determine the averages, but the 0% values were used. 

CD-ROM 8270D - 53 Revision 4 

January 1998 
TABLE 13 

SINGLE LABORATORY ACCURACY AND PRECISION FOR THE EXTRACTION OF PAHs 

FROM A CERTIFIED REFERENCE SEDIMENT EC-1, USING METHOD 3561 (SFE - SOLID 

TRAP) 

Certified Value SFE Valuea Percent of 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 (0.2) 0.2 ± 0.01 (100) 0.05 

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 deviations for 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 - 54 Revision 4 

January 1998 
TABLE 14 

SINGLE LABORATORY ACCURACY AND PRECISION FOR THE EXTRACTION OF PAHs 

FROM A CERTIFIED REFERENCE SEDIMENT HS-3, USING METHOD 3561 (SFE - SOLID 

TRAP) 

Certified Value SFE Valuea 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)fluoranthene 7.7 ± 1.2 8.4 ± 0.9 109 10.7 

Benzo(k)fluoranthene 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 for the SFE values are based on three replicate extractions. 

Data are taken from Reference 10. 

CD-ROM 8270D - 55 Revision 4 

January 1998 
TABLE 15
 

SINGLE LABORATORY ACCURACY AND PRECISION FOR THE EXTRACTION OF PAHs
 

FROM A CERTIFIED REFERENCE SOIL SRS103-100, USING METHOD 3561
 

(SFE - LIQUID TRAP)
 

Compound 

Naphthalene 

2-Methylnaphthalene 

Acenaphthene 

Dibenzofuran 

Certified Value 

(mg/kg) 

32.4 ± 8.2 

62.1 ± 11.5 

632 ± 105 

307 ± 49 

SFE Valuea 

(mg/kg) 

29.55 

76.13 

577.28 

302.25 

Percent of 

Certified Value 

91 

122 

91 

98 

SFE 

RSD 

10.5 

2.0 

2.9 

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 

Benz(a)anthracene 

Chrysene 

Benzo(a)pyrene 

Benzo(b)fluoranthene + 

Benzo(k)fluoranthene 

1033 ± 285 

252 ± 8 

297 ± 26 

97.2 ± 17.1 

153 ± 22 

911.82 

225.50 

283.00 

58.28 

130.88 

88 

89 

95 

60 

86 

3.1 

4.8 

3.8 

6.5 

10.7 

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

Data are taken from Reference 11. 

CD-ROM 8270D - 56 Revision 4 

January 1998 
TABLE 16
 

SINGLE LABORATORY RECOVERY DATA FOR SOLID-PHASE EXTRACTION OF
 

BASE/NEUTRAL/ACID EXTRACTABLES FROM SPIKED TCLP BUFFERS
 

LOW SPIKE LEVEL
 

Analyte 

Spike Level 

(μg/L) 

Buffer 1 (pH = 2.886) 

Recovery (%) RSD 

Buffer 2 (pH = 4.937) 

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 

Results from 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. 

CD-ROM 8270D - 57 Revision 4 

January 1998 
TABLE 17
 

SINGLE LABORATORY RECOVERY DATA FOR SOLID-PHASE EXTRACTION OF
 

BASE/NEUTRAL/ACID EXTRACTABLES FROM SPIKED TCLP BUFFERS
 

HIGH SPIKE LEVEL
 

Analyte 

Spike Level 

(μg/L) 

Buffer 1 (pH = 2.886) 

Recovery (%) RSD 

Buffer 2 (pH = 4.937) 

Recovery (%) RSD 

1,4-Dichlorobenzene 15,000 63 10 63 9 

Hexachloroethane 6,000 54 7 46 7 

Nitrobenzene 4,000 81 4 81 13 

Hexachlorobutadiene 1,000 81 5 70 11 

2,4-Dinitrotoluene 260 99 8 98 3 

Hexachlorobenzene 260 89 8 91 9 

o-Cresol* 400,000 92 15 90 4 

m-Cresol* 400,000 95 8 82 6 

p-Cresol* 400,000 82 14 84 7 

2,4,6-Trichlorophenol 4,000 93 12 104 12 

2,4,5-Trichlorophenol 800,000 93 14 97 23 

Pentachlorophenol 200,000 84 9 73 8 

Results from seven replicate spiked buffer samples. 

* In this study, recoveries of these compounds were determined from triplicate spikes of the 

individual compounds into separate buffer solutions. 

Data from Reference 12. 

CD-ROM 8270D - 58 Revision 4 

January 1998 
TABLE 18
 

RECOVERY DATA FROM THREE LABORATORIES FOR SOLID-PHASE EXTRACTION

OF BASE/NEUTRAL/ACID EXTRACTABLES FROM SPIKED TCLP LEACHATES FROM SOIL SA

Buffer 1 pH = 2.886 Lab 1 Lab 2 

Spike 

Analyte Level %R RSD n %R RSD n %R 

(μg/L)* 

o-Cresol 200,000 86 8 7 35.3 0.7 3 7.6 m-Cresol** -- 77 8 7 -- -- -- -- 

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

CD-ROM 8270D - 59 
TABLE 18 

(continued) 

Buffer 2 pH = 4.937 Lab 1 Lab 2 

Spike 

Analyte Level %R RSD n %R RSD n %R 

(μg/L)* 

o-Cresol 200,00 97 13 7 37.8 4.5 3 6.1 m-Cresol** -- 83 4 7 -- -- -- 6.0 p-Cresol** -- -- -- -- -- -- -- -- 2,4,6-Trichlorophenol 2,000 104 4 7 91.7 8.0 3 37.7 2,4,5-Trichlorophenol 400,000 94 4 7 85.2 0.4 3 64.4 Pentachlorophenol 100,000 109 11 7 41.9 28.2 3 36.6 1,4-Dichlorobenzene 7,500 50 5 7 79.7 1.0 3 26.5 Hexachloroethane 3,000 51 3 7 64.9 2.0 3 20.3 Nitrobenzene 2,000 80 4 7 79.0 2.3 3 59.4 Hexachlorobutadiene 500 57 5 7 60 3.3 3 16.6 2,4-Dinitrotoluene 130 86 6 7 38.5 5.2 3 62.2 Hexachlorobenzene 130 86 7 7 91.3 0.9 3 75.5 

* 250-mL aliquots of leachate were spiked. Lab 1 spiked at one-half these 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 rthree isomers of Cresol.
 Data from Reference 12.
 

CD-ROM 8270D - 60 
FIGURE 1
 

GAS CHROMATOGRAM OF BASE/NEUTRAL AND ACID CALIBRATION STANDARD
 

CD-ROM 8270D - 61 Revision 4
 

January 1998
 
METHOD 8270D
 

SEMIVOLATILE ORGANIC COMPOUNDS BY GAS CHROMATOGRAPHY/MASS
 

SPECTROMETRY (GC/MS)
 

CD-ROM 8270D - 62 Revision 4 

January 1998