8270 D

METHOD 8270D
SEMIVOLATILE ORGANIC COMPOUNDS

BY GAS CHROMATOGRAPHY/MASS SPECTROMETRY
SW-846 is not intended to be an analytical training manual. Therefore, method

procedures are written based on the assumption that they will be performed by analysts who are
formally trained in at least the basic principles of chemical analysis and in the use of the subject
technology.
In addition, SW-846 methods, with the exception of required method use for the analysis
of method defined parameters (MDPs), are intended to be guidance methods that contain
general information on how to perform an analytical procedure or technique, which a laboratory
can use as a basic starting point for generating its own detailed standard operating procedure
(SOP), either for its own general use or for a specific project application. The performance data
included in this method are for guidance purposes only, and are not intended to be and must not
be used as absolute quality control (QC) acceptance criteria for purposes of laboratory
accreditation.
1.0 SCOPE AND APPLICATION
1.1 This method 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 Resource Conservation and Recovery Act (RCRA) analytes have been
determined by this method:
Appropriate Preparation Techniquesb

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Compounds CAS Noa 3510 3520 3541 3550 3580
Acenaphthene 83-32-9 X X X X X
Acenaphthylene 208-96-8 X X X X X
Acetophenone 98-86-2 X ND ND ND X
2-Acetylaminofluorene 53-96-3 X ND ND ND X
1-Acetyl-2-thiourea 591-08-2 LR ND ND ND LR
Aldrin 309-00-2 X X X X X
2-Aminoanthraquinone 117-79-3 X ND ND ND X
Aminoazobenzene 60-09-3 X ND ND ND X
4-Aminobiphenyl 92-67-1 X ND ND ND X
3-Amino-9-ethylcarbazole 132-32-1 X X ND ND ND
Anilazine 101-05-3 X ND ND ND X
Aniline 62-53-3 X X ND X X
o-Anisidine 90-04-0 X ND ND ND X
Anthracene 120-12-7 X X X X X
Aramite 140-57-8 HS 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
SW-846 Update V 8270D - 1 Revision 5
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Azinphos-methyl 86-50-0 HS ND ND ND X
Barban 101-27-9 LR ND ND ND LR
Benzidine 92-87-5 CP CP CP CP CP
Benzoic acid 65-85-0 X X ND X X
Benzo(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-chloro-1-methylethyl)etherc 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 ND ND ND X
Captan 133-06-2 HS 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
hydrochloride 6959-48-4 X ND ND ND X
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
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 ND ND ND X
Demeton-S 126-75-0 X ND ND ND X
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a
Compounds CAS No 3510 3520 3541 3550 3580
Diallate (cis or trans) 2303-16-4 X ND ND ND X
2,4-Diaminotoluene 95-80-7 DC, OE 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
3,3'-Dichlorobenzidine 91-94-1 X X X X X
2,4-Dichlorophenol 120-83-2 X X X X X
2,6-Dichlorophenol 87-65-0 X ND ND ND X
Dichlorovos 62-73-7 X ND ND ND X
Dicrotophos 141-66-2 X ND ND ND X
Dieldrin 60-57-1 X X X X X
Diethyl phthalate 84-66-2 X X X X X
Diethylstilbestrol 56-53-1 AW, OS ND ND ND X
Diethyl sulfate 64-67-5 LR ND ND ND LR
Dimethoate 60-51-5 HE, HS 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 ND ND ND CP
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 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 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
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Ethyl carbamate 51-79-6 DC 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
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 ND ND ND CP
Hexachloropropene 1888-71-7 X ND ND ND X
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 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 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(2-chloroaniline) 101-14-4 OE, OS ND ND ND LR
4,4'-Methylenebis(N,N-dimethyl-
aniline) 101-61-1 X X ND ND ND
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
Mevinphos 7786-34-7 X ND ND ND X
Mexacarbate 315-18-4 HE, HS ND ND ND X
Mirex 2385-85-5 X ND ND ND X
Monocrotophos 6923-22-4 HE ND ND ND X
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 ND ND ND X
2-Naphthylamine 91-59-8 X ND ND ND X
Nicotine 54-11-5 DC ND ND ND X
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a
Compounds CAS No 3510 3520 3541 3550 3580
5-Nitroacenaphthene 602-87-9 X ND ND ND X
2-Nitroaniline 88-74-4 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-Nitrosodiphenylamine 86-30-6 X X X X X
N-Nitrosodi-n-propylamine 621-64-7 X X X X X
N-Nitrosomethylethylamine 10595-95-6 X ND ND ND 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 X X X X
1,4-Phenylenediamine 106-50-3 X ND ND ND X
Phorate 298-02-2 X ND ND ND X
Phosalone 2310-17-0 HS ND ND ND X
Phosmet 732-11-6 HS ND ND ND X
Phosphamidon 13171-21-6 HE ND ND ND X
Phthalic anhydride 85-44-9 CP, HE ND ND ND CP
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
Propylthiouracil 51-52-5 LR ND ND ND LR
Pyrene 129-00-0 X X X X X
Resorcinol 108-46-3 DC, OE ND ND ND X
Safrole 94-59-7 X ND ND ND X
Strychnine 57-24-9 AW, OS ND ND ND X
Sulfallate 95-06-7 X ND ND ND X
Terbufos 13071-79-9 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 dithiopyrophosphate 3689-24-5 X X ND ND ND
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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 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 ND ND ND X
1,3,5-Trinitrobenzene 99-35-4 X ND ND ND X
Tris(2,3-dibromopropyl)phosphate 126-72-7 X ND ND ND LR
Tri-p-tolyl phosphate 78-32-0 X ND ND ND X
O,O,O-Triethyl phosphorothioate 126-68-1 X ND ND ND X
a
Chemical Abstract Service (CAS) Registry Number
b
See Sec. 1.2 for other acceptable preparation methods.
c
Chemical name was changed by the Integrated Risk Information System (IRIS) on November
30, 2007 from Bis(2-chloroisopropyl)ether to Bis(2-chloro-1-methylethyl)ether (common name).
This compound is also known as 2,2’-oxybis(1-chloropropane) (CAS index name). See the link
at http://www.epa.gov/iris/subst/0407.htm, Section VII for the “Revision History” and Section
VIII, for “Synonyms” of this chemical.
KEY TO ANALYTE LIST
AW = Adsorption to walls of glassware during extraction and storage

CP = Non-reproducible chromatographic performance
DC = Unfavorable distribution coefficient
HE = Hydrolysis during extraction accelerated by acidic or basic conditions
HS = Hydrolysis during storage potential
LR = Low response
ND = Not determined
OE = Oxidation during extraction accelerated by basic conditions
OS = Oxidation during storage potential
X = Historically, adequate recovery can be obtained by this technique. However, actual
recoveries may vary depending on the extraction efficiency, the number of
constituents being analyzed concurrently, and the analytical instrumentation.
1.2 In addition to the sample preparation methods listed in the above analyte list,
Method 3535 describes a solid-phase extraction (SPE) procedure that may be applied to the
extraction of semivolatiles from toxicity characteristic leaching procedure (TCLP) leachates (see
Tables 16 and 17 of this method for performance data). Method 3542 describes sample
preparation for semivolatile organic compounds in air sampled by Method 0010 (see Table 10 of
this method for surrogate performance data), Method 3545 describes an automated solvent
extraction (ASE) device for semivolatiles in solids (see Table 11 of this method for performance
data), Method 3561 describes a supercritical fluid extraction (SFE) device for the extraction of
polynuclear aromatic hydrocarbons (PAHs) from solids (see Tables 12, 13, and 14 of this
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method for performance data), and Method 3546 provides an extraction procedure employing
commercially available microwave equipment to extract semivolatiles while using less solvent
and taking less time than procedures such as a Soxhlet extraction (see Tables 18 through 22 of
this method for the applicable performance data). The tabulated data are provided for guidance
purposes only.
1.3 This method can be used to quantitate most neutral, acidic, and basic organic
compounds that are soluble in methylene chloride (or other suitable solvents provided that the
desired performance data can be generated) and are 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 PAHs, 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, this method 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 permits. Refer to 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 to be present.
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. For this reason, it is acceptable to report
the combined result for n-nitrosodiphenylamine and diphenylamine for either of these
compounds as a combined concentration.
1.4.6 1,2-Diphenylhydrazine is unstable even at room temperature and readily

converts to azobenzene. Given the stability problems, it would be acceptable to calibrate
for 1,2-diphenylhydrazine using azobenzene. Under these poor compound separation
circumstances the results for either of these compounds should be reported as a
combined concentration.
1.4.7 Pentachlorophenol, 2,4-dinitrophenol, 4-nitrophenol, benzoic acid, 4,6-

dinitro-2-methylphenol, 4-chloro-3-methylphenol, 2-nitroaniline, 3-nitroaniline, 4-

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nitroaniline, and benzyl alcohol are subject to erratic chromatographic behavior, especially
if the gas chromatograph (GC) system is contaminated with high boiling material.
1.4.8 Pyridine may perform poorly at the GC injection port temperatures listed
in this 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), microwave extraction (Method 3546),
or supercritical fluid extraction, which involve smaller extract volumes, thereby reducing or
eliminating the need for evaporative concentration techniques for many applications.
1.4.9 Toluene diisocyanate rapidly hydrolyzes in water (it has a half-life of less
than 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.
1.4.10 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 lower limits of quantitation (LLOQ) for this method when determining an
individual compound are approximately 660 µg/kg (wet weight) for soil/sediment samples, 1-200
mg/kg for wastes (dependent on matrix and method of preparation), and 10 µg/L for
groundwater samples (see Table 2). LLOQ will be proportionately higher for sample extracts
that require dilution to avoid saturation of the detector. The lower limits of quantitation listed in
Table 2 are provided for guidance and may not always be achievable.
1.6 Prior to employing this method, analysts are advised to consult the base method
for each type of procedure that may be employed in the overall analysis (e.g., Methods 3500,
3600, 5000, and 8000) for additional information on QC procedures, development of QC
acceptance criteria, calculations, and general guidance. Analysts also should consult the
disclaimer statement at the front of the manual and the information in Chapter Two for guidance
on the intended flexibility in the choice of methods, apparatus, materials, reagents, and
supplies, and on the responsibilities of the analyst for demonstrating that the techniques
employed are appropriate for the analytes of interest, in the matrix of interest, and at the levels
of concern.
In addition, analysts and data users are advised that, except where explicitly specified in a
regulation, the use of SW-846 methods is not mandatory in response to Federal testing
requirements. The information contained in this method is provided by Environmental
Protection Agency (EPA or the Agency) as guidance to be used by the analyst and the
regulated community in making judgments necessary to generate results that meet the data
quality objectives (DQOs) for the intended application.
1.7 Use of this method is restricted to use by, or under supervision of, personnel
appropriately experienced and trained in the use of the GC/mass spectrometer (MS) and skilled
in the interpretation of mass spectra. Each analyst must demonstrate the ability to generate
acceptable results with this method.

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2.0 SUMMARY OF METHOD
2.1 The samples are prepared for analysis by 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 GC equipped with a narrow-bore fused-silica capillary column. The GC
column is temperature-programmed to separate the analytes, which are then detected with an
MS connected to the GC.
2.3 Analytes eluted from the capillary column are introduced into the MS 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 an appropriate calibration curve for the intended
application.
2.4 This method includes specific calibration and QC steps that supersede the general
recommendations provided in Method 8000.
3.0 DEFINITIONS
Refer to Chapter One and the manufacturer's instructions for definitions that may be
relevant to this procedure.
4.0 INTERFERENCES
4.1 Solvents, reagents, glassware, and other sample processing hardware may yield
artifacts and/or interferences to sample analysis. All of these materials must be demonstrated
to be free from interferences under the conditions of the analysis by analyzing method blanks.
Specific selection of reagents and purification of solvents by distillation in all glass systems may
be necessary. Refer to each method to be used for specific guidance on QC procedures and to
Chapter Four for general guidance on the cleaning of glassware. Also refer to Method 8000 for
a discussion of interferences.
4.2 Raw gas chromatography/mass spectrometry 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.
4.3 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 cross-
contamination.

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5.0 SAFETY
This method does not address all safety issues associated with its use. The laboratory is
responsible for maintaining a safe work environment and a current awareness file of
Occupational Safety and Health Administration (OSHA) regulations regarding the safe handling
of the chemicals listed in this method. A reference file of material safety data sheets (MSDSs)
should be available to all personnel involved in these analyses.
6.0 EQUIPMENT AND SUPPLIES
The mention of trade names or commercial products in this manual is for illustrative
purposes only, and does not constitute an EPA endorsement or exclusive recommendation for
use. The products and instrument settings cited in SW-846 methods represent those products
and settings used during method development or subsequently evaluated by the Agency.
Glassware, reagents, supplies, equipment, and settings other than those listed in this manual
may be employed provided that method performance appropriate for the intended application
has been demonstrated and documented.
This section does not list common laboratory glassware (e.g., beakers and flasks).
6.1 Gas chromatograph/mass spectrometer system
6.1.1 GC - An analytical system equipped with a temperature programmable

GC suitable for splitless injection and all required accessories, including syringes,
analytical columns, and gases. The capillary column should be directly coupled to the
source.
6.1.2 Column - 30 m x 0.25 mm ID (or 0.32 mm ID) 0.25, 0.5, or 1 µm film

thickness silicone-coated fused-silica capillary column (J&W Scientific DB-5 or equivalent).
The columns listed in this section were the columns used in developing the method. The
listing of these columns in this method is not intended to exclude the use of other columns
that may be developed. Laboratories may use these columns or other capillary columns
provided that the laboratories document method performance data (e.g., chromatographic
resolution, analyte breakdown, and sensitivity) that are appropriate for the intended
application.
6.1.3 Mass spectrometer
6.1.3.1 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 MS must be capable of producing a mass spectrum for
decafluorotriphenylphosphine (DFTPP) which meets the criteria as outlined in Sec.
11.3.1.
6.1.3.2 An ion trap MS 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/National Institute of Standards and Technology (NIST)
Library. The MS must be capable of producing a mass spectrum for DFTPP which
meets the criteria as outlined in Sec. 11.3.1.

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6.1.4 GC/MS interface - Any GC-to-MS interface may be used that gives
acceptable calibration points 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 MS source.
6.1.5 Data system - A computer system should be interfaced to the MS. 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 gas chromatography/mass
spectrometry 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/National Institute of Standards and Technology (NIST) Mass Spectral Library should
also be available.
6.1.6 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
connectors (Agilent Catalog No. 5062-3556, or equivalent).
6.2 Syringe - 10 µL
6.3 Volumetric flasks, Class A - Appropriate sizes equipped with ground-glass stoppers
6.4 Balance - Analytical, capable of weighing 0.0001 g
6.5 Bottles - Glass equipped with polytetrafluoroethylene (PTFE)-lined screw caps or

crimp tops
7.0 REAGENTS AND STANDARDS
7.1 Reagent-grade chemicals must be used in all tests. Unless otherwise indicated, it
is intended that all reagents conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society (ACS), where such specifications are available.
Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination. Reagents should be
stored in glass to prevent the leaching of contaminants from plastic containers.
7.2 Organic-free reagent water - All references to water in this method refer to organic-
free reagent water.
7.3 Standard solutions
The following sections describe the preparation of stock, intermediate, and working
standards for the compounds of interest. This discussion is provided as an example, and other
approaches and concentrations of the target compounds may be used, as appropriate for the
intended application. See Method 8000 for additional information on the preparation of
calibration standards.
7.4 Stock standard solutions (1000 mg/L) - Standard solutions can be prepared from
pure standard materials or purchased as certified solutions.

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7.4.1 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. Commercially prepared stock standards may be used at any concentration if
they are certified by the manufacturer or by an independent source.
7.4.2 Transfer the stock standard solutions into bottles equipped with PTFE-
lined screw caps. Store, protected from light, at ≤6 °C 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.
7.4.3 Stock standard solutions must be replaced after one year or sooner if
comparison with QC check samples indicates a problem.
7.4.4 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.
7.4.5 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.
7.5 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 criteria in Sec. 11.3.2 are met.
7.5.1 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 away from any light source at ≤6 °C when not in use (−10 °C is
recommended). When using premixed certified solutions, store according to the
manufacturer's documented holding time and storage temperature recommendations.
7.5.2 If a more sensitive MS is employed to achieve lower quantitation levels, a

more dilute internal standard solution may be required. Area counts of the internal
standard peaks should be between 50-200% of the area of the target analytes in the mid-
point calibration analysis.
7.6 GC/MS tuning standard - A methylene chloride solution containing 50 ng/µL of

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.
Alternate concentrations may be used to compensate for different injection volumes if the total
amount injected is 50 ng or less. Store away from any light source at ≤6 °C when not in use (-
10 °C is recommended). If a more sensitive MS is employed to achieve lower quantitation
levels, a more dilute tuning solution may be necessary. When using premixed certified
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solutions, store according to the manufacturer's documented holding time and storage
temperature recommendations.
7.7 Calibration standards - A minimum of five calibration standards should be prepared

at different concentrations. At least one of the calibration standards should correspond to a
sample concentration at or below that necessary to meet the DQOs 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 and/or series of
calibration standards prepared at a given concentration should contain all the desired project-
specific target analytes for which quantitation and quantitative results are to be reported by this
method.
7.7.1 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).
7.7.2 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 away from
any light source at ≤6 °C when not in use (−10 °C is recommended), and should be freshly
prepared once a year, or sooner if check standards indicate a problem. The calibration
verification standard should be prepared, as necessary, and stored at ≤6 °C. When using
premixed certified solutions, store according to the manufacturer's documented holding
time and storage temperature recommendations.
7.8 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.
NOTE: In the presence of samples containing residual chlorine, phenol-d6 has been known to
react to form chlorinated phenolic compounds that are not detected as the original
spiked surrogate. Sample preservation precautions outlined in Chapter Four should be
used when residual chlorine is known to be present in order to minimize degradation of
deuterated phenols or any other susceptible target analyte.
7.8.1 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.

more dilute surrogate solution may be necessary.
7.9 Matrix spike and laboratory control standards (LCSs) - See Method 3500 for
instructions on preparing the matrix spike standard. The same standard may be used as the
LCS and the spiking solution should be the same source as used for the initial calibration
standards to restrict the influence of standard accuracy on the determination of recovery
through preparation and analysis.

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7.9.1 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.

more dilute matrix and LCS spiking solution may be necessary.
7.9.3 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.
7.10 Solvents - Acetone, hexane, methylene chloride, isooctane, carbon disulfide,

toluene, and other appropriate solvents may be used. All solvents should be pesticide quality or
equivalent. Solvents may be degassed prior to use, if necessary.
8.0 SAMPLE COLLECTION, PRESERVATION, AND STORAGE
8.1 See the introductory material to Chapter Four, "Organic Analytes."
8.2 Store the sample extracts at ≤6 °C, protected from light, in sealed vials (e.g.,
screw-cap vials or crimp-capped vials) equipped with unpierced PTFE-lined septa.
9.0 QUALITY CONTROL
9.1 Refer to Chapter One for guidance on quality assurance (QA) and QC protocols.
When inconsistencies exist between QC guidelines, method-specific QC criteria take
precedence over both technique-specific criteria and those criteria given in Chapter One, and
technique-specific QC criteria take precedence over the criteria in Chapter One. Any effort
involving the collection of analytical data should include development of a structured and
systematic planning document, such as a quality assurance project plan (QAPP) or a sampling
and analysis plan (SAP), which translates project objectives and specifications into directions for
those that will implement the project and assess the results. Each laboratory should maintain a
formal QA program. The laboratory should also maintain records to document the quality of the
data generated. All data sheets and QC data should be maintained for reference or inspection.
9.2 Refer to Method 8000 for specific determinative method QC procedures. Refer to
Method 3500 or 5000 for QC procedures to ensure the proper operation of the various sample
preparation techniques. If an extract cleanup procedure is performed, refer to Method 3600 for
the appropriate QC procedures. Any more specific QC procedures provided in this method will
supersede those noted in Methods 8000, 5000, 3500, or 3600.
9.3 QC procedures necessary to evaluate the GC system operation are found in

Method 8000 and include evaluation of retention time windows, calibration verification and
chromatographic analysis of samples. In addition, discussions regarding the instrument QC
requirements listed below can be found in the referenced sections of this method:
9.3.1 The GC/MS must be tuned to meet the recommended DFTPP criteria
prior to the initial calibration and for each twelve-hour period during which analyses are
performed. See Secs. 11.3.1 and 11.4.1 for further details.

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9.3.2 There must be an initial calibration of the GC/MS system as described in
Sec. 11.3. In addition, the initial calibration curve should be verified immediately after
performing the standard analyses using a second source standard (prepared using
standards different from the calibration standards). The suggested acceptance limits for
this initial calibration verification analysis are 70-130%. Alternative acceptance limits
may be appropriate based on the desired project-specific DQOs. Quantitative sample
analyses should not proceed for those analytes that fail the second source standard
initial calibration verification. However, analyses may continue for those analytes that
fail the criteria with an understanding these results could be used for screening purposes
and would be considered estimated values.
9.3.3 The GC/MS system must meet the calibration verification acceptance
criteria in Sec. 11.4.
9.3.4 The relative retention time (RRT) of the sample component must fall
within the RRT window of the standard component provided in Sec. 11.6.1.
9.4 Initial demonstration of proficiency (IDP)
Prior to implementation of a method, each laboratory must perform an IDP consisting of at

least four replicate reference samples spiked into a clean matrix taken through the entire
sample preparation and analysis. Whenever a significant change to instrumentation or
procedure occurs, the laboratory must demonstrate that acceptable precision and bias can still
be obtained by the changed conditions. Whenever new staff members are trained, an analyst
IDP must be performed. See Method 8000 for more information on how to accomplish an IDP.
9.4.1 Demonstration of proficiency for new analysts - Each laboratory should

have a training program which documents that a new analyst is capable of performing the
method, or portion of the method, for which the analyst is responsible. This demonstration
should document that the new analyst is capable of successfully following the SOP
established by the laboratory.
9.5 Initially, before processing any samples, the analyst should demonstrate that all
parts of the equipment in contact with the sample and reagents are interference-free. This is
accomplished through the analysis of a method blank. As a continuing check, each time
samples are extracted, cleaned up, and analyzed, a method blank must be prepared and
analyzed for the compounds of interest as a safeguard against chronic laboratory
contamination. If a peak is observed within the retention time window of any analyte that would
prevent the determination of that analyte, determine the source and eliminate it, if possible,
before processing the samples. The blanks should be carried through all stages of sample
preparation and analysis. When new reagents or chemicals are received, the lab should
monitor the preparation and/or analysis blanks associated with samples for any signs of
contamination. It is not necessary to test every new batch of reagents or chemicals prior to
sample preparation if the source shows no prior problems. However, if reagents are changed
during a preparation batch, separate blanks need to be prepared for each set of reagents.

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9.6 Sample QC for preparation and analysis
The laboratory must also have procedures for documenting the effect of the matrix on
method performance (precision, accuracy, method sensitivity). At a minimum, this should
include the analysis of QC samples including a method blank, a matrix spike, a duplicate, and a
LCS in each analytical batch and the addition of surrogates to each field sample and QC sample
when surrogates are used. Any method blanks, matrix spike samples, and replicate samples
should be subjected to the same analytical procedures (Sec. 11.0) as those used on actual
samples.
9.6.1 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 knowledge of the samples in the
sample batch. If samples are expected to contain target analytes, laboratories may use a
matrix spike and a duplicate analysis of an unspiked field sample. If samples are not
expected to contain target analytes, then laboratories should use a matrix spike and matrix
spike duplicate pair. Consult Method 8000 for information on developing acceptance
criteria for the matrix spike and matrix spike duplicate.
9.6.2 An 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 appropriate. 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. Consult Method 8000 for
information on developing acceptance criteria for the LCS.
9.6.3 Also see Method 8000 for the details on carrying out sample QC
procedures for preparation and analysis. In-house method performance criteria for
evaluating method performance should be developed using the guidance found in Method
8000.
9.6.4 Blanks – Before processing any samples, the analyst should demonstrate
through the analysis of a method blank that equipment and reagents are free from
contaminants and interferences. If a peak is found in the blank that would prevent the
identification or bias the measurement of an analyte, the analyst should determine the
source and eliminate it, if possible. As a continuing check, each time a batch of samples
is extracted, cleaned up, and analyzed, and when there is a change in reagents, a method
blank must be prepared and analyzed for the compounds of interest as a safeguard
against chronic laboratory contamination. Method blanks, trip blanks, and other field
blanks should be carried through all stages of sample preparation and analysis. At least
one method blank or instrument blank must be analyzed on every instrument after
calibration standard(s) and prior to the analysis of any samples.
9.6.5 Blanks are generally considered to be acceptable if target analyte

concentrations are less than one-half the LLOQ or are less than project-specific
requirements. Blanks may contain analyte concentrations greater than acceptance limits if
the associated samples in the batch are unaffected (i.e., targets are not present in
samples or sample concentrations are ≥10X the blank). Other criteria may be used
depending on the needs of the project.
9.6.6 If an analyte of interest is found in a sample in the batch near a

concentration confirmed in the blank (refer to Sec. 9.5.2), the presence and

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or/concentration of that analyte should be considered suspect and may require
qualification. Contaminants in the blank should meet most or all of the qualitative
identifiers in Section 11.6 to be considered. Samples may require re-extraction and/or re-
analysis if the blanks do not meet lab established or project specific criteria. Re-extraction
and/or re-analysis is not necessary if the analyte concentration falls well below the action
or regulatory limit or if the analyte is deemed not important for the project.
9.6.7 When new reagents or chemicals are received, the lab should monitor the
blanks associated with samples for any signs of contamination. It is not necessary to test
every new batch of reagents or chemicals prior to sample preparation if the source shows
no prior problems. However, if reagents are changed during a preparation batch, separate
blanks need to be prepared for each set of reagents.
9.6.8 Method and/or solvent blanks may also be used to check for
contamination by carryover from a high-concentration sample into subsequent samples
(Sec. 4.2). When analysis of such blanks is not possible, such as when an unattended
autosampler is employed, the analyst should carefully review the results for at least the
next sample after the high-concentration sample. If analytes in the high-concentration
sample are not present in the subsequent sample, then lack of carryover has been
demonstrated. If there is evidence that carryover may have occurred, then the affected
samples should be reanalyzed.
9.7 Surrogate recoveries
If surrogates are used, the laboratory should evaluate surrogate recovery data from
individual samples versus the surrogate control limits developed by the laboratory. See Method
8000 for information on evaluating surrogate data and developing and updating surrogate limits.
Procedures for evaluating the recoveries of multiple surrogates and the associated corrective
actions should be defined in an approved project plan.
9.8 The experience of the analyst performing gas chromatography/mass spectrometry

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. When any changes
are made to the system (e.g., the column is changed, a septum is changed), see the guidance
in Method 8000 regarding whether recalibration of the system must take place.
9.9 It is recommended that the laboratory adopt additional QA 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.
9.10 Lower Limit of Quantitation (LLOQ)
The LLOQ is the lowest concentration at which the laboratory has demonstrated target
analytes can be reliably measured and reported with a certain degree of confidence, which must
be ≥ the lowest point in the calibration curve. The laboratory shall establish the LLOQ at
concentrations where both quantitative and qualitative requirements can consistently be met
(see Sections 9.9 and 11.6). The laboratory shall verify the LLOQ at least annually, and
whenever significant changes are made to the preparation and/or analytical procedure, to

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demonstrate quantitation capability at lower analyte concentration levels. The verification is
performed by the extraction and/or analysis of an LCS (or matrix spike) at 0.5-2 times the
established LLOQ. Additional LLOQ verifications may be useful on a project-specific basis if a
matrix is expected to contain significant interferences at the LLOQ. The verification may be
accomplished with either clean control material (e.g., reagent water, solvent blank, Ottawa sand,
diatomaceous earth) or a representative sample matrix, free of target compounds. Optimally,
the LLOQ should be less than the desired decision level or regulatory action level based on the
stated DQOs.
9.10.1 LLOQ Verification – The verification of LLOQs using spiked clean control
material represents a best-case scenario because it does not evaluate the potential matrix
effects of real-world samples. For the application of LLOQs on a project-specific basis,
with established DQOs, a representative matrix-specific LLOQ verification may provide a
more reliable estimate of the lower quantitation limit capabilities.
9.10.2 The LLOQ verification (to be performed after the initial calibration) is
prepared by spiking a clean control material with the analyte(s) of interest at 0.5-2 times
the LLOQ concentration level(s). Alternatively, a representative sample matrix free of
targets may be spiked with the analytes of interest at 0.5-2 times the LLOQ concentration
levels. The LLOQ check is carried through the same preparation and analytical
procedures as environmental samples and other QC samples. It is recommended to
analyze the LLOQ verification on every instrument where data is reported; however, at a
minimum, the lab should rotate the verification among similar analytical instruments such
that all are included within 3 years. Frequently performed analyses, such as 8270D,
should have an LLOQ check standard be verified, at minimum, once a year.
9.10.3 Recovery of target analytes in the LLOQ verification should be within

established in-house limits or within other such project-specific acceptance limits to
demonstrate acceptable method performance at the LLOQ. Until the laboratory has
sufficient data to determine acceptance limits, the LCS criteria ± 20% (i.e., lower limit
minus 20% and upper limit plus 20%) may be used for the LLOQ acceptance criteria. This
practice acknowledges the potential for greater uncertainty at the low end of the calibration
curve. Where practical, historically based LLOQ acceptance criteria should be determined
once sufficient data points have been acquired.
9.10.4 Reporting concentrations below LLOQ - Concentrations that are below

the established LLOQ may still be reported; however, these analytes must be qualified as
estimated. The procedure for reporting analytes below the LLOQ should be documented
in the laboratory’s SOP or in a project-specific plan. Analytes below the LLOQ that are
reported should meet most or all of the qualitative identification requirements in Sec. 11.
10.0 CALIBRATION AND STANDARDIZATION
See Sec 11.3 for information on calibration and standardization.
11.0 PROCEDURE
11.1 Sample preparation
11.1.1 Samples are normally prepared by one of the following methods prior to
gas chromatography/mass spectrometry analysis.

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Matrix Methods
Air (particulates and sorbent resin) 3542

Water (including TCLP leachates) 3510, 3520, 3535
Soil/sediment 3540, 3541, 3545, 3546, 3550, 3560, 3561
Waste 3540, 3541, 3545, 3546, 3550, 3560, 3561,
3580
11.1.2 In very limited applications, direct injection of the sample into the GC/MS
system with a 10-µL syringe may be appropriate. The quantitation limit is very high
(approximately 10,000 µg/L) when this procedure is used. Therefore, it is only appropriate
where concentrations in excess of 10,000 µg/L are expected.
11.2 Extract cleanup - Cleanup procedures may not be necessary for a relatively clean
sample matrix, but most extracts from environmental and waste samples will require additional
preparation before analysis. The specific cleanup procedure used will depend on the nature of
the sample to be analyzed and the DQOs for the measurements. General guidance for sample
extract cleanup is provided in this section and in Method 3600.
Extracts may be cleaned up by any of the following methods prior to gas

chromatography/mass spectrometry analysis.
Analytes of Interest Methods
Aniline and aniline derivatives 3620

Phenols 3630, 3640, 8041a
Phthalate esters 3610, 3620, 3640
Nitrosamines 3610, 3620, 3640
Organochlorine pesticides 3610, 3620, 3630, 3640, 3660
PCBs 3620, 3630, 3660, 3665
Nitroaromatics and cyclic ketones 3620, 3640
PAHs 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/electron capture detector
(ECD) analysis, if interferences are encountered on GC/flame ionization detector (FID).
11.3 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: 40 °C, hold for 4 min
Temperature program: 40-320 °C at 10 °C/min
Final temperature: 320 °C, hold until 2 min after benzo[g,h,i]perylene elutes
Injector temperature: 250-300 °C
Transfer line temperature: 250-300 °C
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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 MS is sufficient.
11.3.1 The GC/MS system must be hardware-tuned such that injecting 50 ng or

less of DFTPP meets the manufacturer's specified acceptance criteria or as listed in Table
3. The tuning criteria as outlined in Table 3 were developed using quadrupole MS
instrumentation and it is recognized that other tuning criteria may be more effective
depending on the type of instrumentation (e.g., Time-of-Flight, Ion Trap, etc.). In these
cases it would be appropriate to follow the manufacturer's tuning instructions or some
other consistent tuning criteria. However, no matter which tuning criteria is selected, the
system calibration must not begin until the tuning acceptance criteria are met with the
sample analyses performed under the same conditions as the calibration standards.
11.3.1.1 In the absence of specific recommendations on how to acquire

the mass spectrum of DFTPP from the instrument manufacturer, the following
approach should be used: 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 within 20 scans of the elution of DFTPP. The background subtraction
should be designed only to eliminate column bleed or instrument background ions.
Do not subtract part of the DFTPP peak or any other discrete peak that does not
coelute with DFTPP.
11.3.1.2 Use the DFTPP mass intensity criteria in the manufacturer's

instructions as primary tuning acceptance criteria or those in Table 3 as default
tuning acceptance criteria if the primary tuning criteria are not available.
Alternatively, other documented tuning criteria may be used (e.g., Contract
Laboratory Program (CLP) or Method 625), provided that method performance is
not adversely affected. The analyst is always free to choose criteria that are tighter
than those included in this method or to use other documented criteria provided
they are used consistently throughout the initial calibration, calibration verification,
and sample analyses.
NOTE: All subsequent standards, samples, matrix spikes/matrix spike duplicates,

and blanks associated with a DFTPP analysis must use identical MS
instrument conditions.
11.3.1.3 The GC/MS tuning standard solution should also be used to

assess the GC column performance and injection port inertness. Degradation of
dichlorodiphenyltrichloroethane (DDT) to dichlorodiphenyldichloroethylene (DDE)
and dichlorodiphenyldichloroethane (DDD) should not exceed 20%. (See Method
8081 for the percent breakdown calculation.) Benzidine and pentachlorophenol
should be present at their normal responses, and should not exceed a tailing factor
of 2 given by the following equation:
BC
Tailing Factor =
AB

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where the peak is defined as follows: AC is the width at 10% height; DE is the
height of peak and B is the height at 10% of DE. This equation compares the width
of the back half of the peak to the width of the front half of the peak at 10% of the
height. (See Figure 1 for an example tailing factor calculation.)
11.3.1.4 If degradation is excessive and/or poor chromatography is

noted, the injection port may require cleaning. It may also be necessary to cut off
the first 6 to 12 in. of the capillary column to remove high boiling contaminants in
the column. The use of a guard column (Sec. 6.1.6) between the injection port and
the analytical column may help prolong analytical column performance life.
11.3.2 The internal standards selected in Sec. 7.5 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 (e.g., for 1,4-dichlorobenzen-d4, use
m/z 150 for quantitation).
11.3.3 Analyze a consistent volume (typically 1-2 µL) of each calibration

standard (i.e., containing the compounds for quantitation and the appropriate surrogates
and internal standards) and tabulate the area of the primary ion against concentration for
each target analyte (as indicated in Table 1). A set of at least five calibration standards
is necessary (see Sec. 7.7 and Method 8000). Alternate injection volumes may be used
if the applicable QC requirements for using this method are met. The injection volume
must be the same for all standards and sample extracts. Figure 2 shows a
chromatogram of a calibration standard containing base/neutral and acid analytes.
11.3.4 Initial calibration calculations
Calculate response factors (RFs) for each target analyte relative to one of the
internal standards (see Table 4) as follows:
A s × C is
RF =
A is × C s
where:
As = Peak area (or height) of the analyte or surrogate
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
11.3.4.1 Calculate the mean RF and the relative standard deviation

(RSD) of the RFs for each target analyte using the following equations. The RSD
should be less than or equal to 20% for each target analyte. It is also
recommended that a minimum RF for the most common target analytes, as noted
in Table 4, be demonstrated for each individual calibration level as a means to
ensure that these compounds are behaving as expected. In addition, meeting the
minimum RF criteria for the lowest calibration standard is critical in establishing
and demonstrating the desired sensitivity. Due to the large number of compounds
that may be analyzed by this method, some compounds will fail to meet these
criteria. For these occasions, it is acknowledged that the failing compounds may
not be critical to the specific project and therefore they may be used as qualified
data or estimated values for screening purposes. The analyst should also strive to
place more emphasis on meeting the calibration criteria for those compounds that

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are critical project compounds, rather than meeting the criteria for those less
important compounds.
n n
∑ RF
i =1
i ∑(RF − RF)
i
2
mean RF = RF = SD = i =1
n n -1
SD
RSD = × 100
RF
where:
RFi = RF for each of the calibration standards
RF = mean RF for each compound from the initial calibration
n = Number of calibration standards, e.g., 5
SD = Standard deviation
11.3.4.2 If more than 10% of the compounds included with the initial
calibration exceed the 20% RSD limit and do not meet the minimum correlation
coefficient (0.99) for alternative curve fits, then the chromatographic system is
considered too reactive for analysis to begin. Clean or replace the injector liner
and/or capillary column, then repeat the calibration procedure beginning with Sec.
11.3.
11.3.5 Evaluation of retention times - The 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
11.3.6 Linearity of target analytes - If the RSD of any target analyte is 20% or
less, then the relative RF is assumed to be constant over the calibration range, and the
average relative RF may be used for quantitation (Sec. 11.7.2).
11.3.6.1 If the RSD of any target analyte is greater than 20%, refer to
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. The RF should not be used for compounds that have an RSD greater
than 20% unless the concentration is reported as estimated.
11.3.6.2 When the RSD exceeds 20%, 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.
11.3.6.3 Due to the large number of compounds that may be analyzed

by this method, some compounds may fail to meet either the 20% RSD, minimum
correlation coefficient criteria (0.99), or the acceptance criteria for alternative
calibration procedures in Method 8000. Any calibration method described in
Method 8000 may be used, but it should be used consistently. It is considered
inappropriate once the calibration analyses are completed to select an alternative
calibration procedure in order to pass the recommended criteria on a case-by-case
basis. If compounds fail to meet these criteria, the associate concentrations may
July 2014
still be determined but they must be reported as estimated. In order to report non-
detects, it must be demonstrated that there is adequate sensitivity to detect the
failed compounds at the applicable lower quantitation limit.
11.4 GC/MS calibration verification - Calibration verification consists of three steps that
are performed at the beginning of each twelve hour analytical shift.
11.4.1 Prior to the analysis of samples or calibration standards, inject 50 ng or

less of the DFTPP standard into the GC/MS system. The resultant mass spectrum for
DFTPP must meet the criteria as outlined in Sec. 11.3.1 before sample analysis begins.
These criteria must be demonstrated each twelve hour shift during which samples are
analyzed.
11.4.2 The initial calibration function for each target analyte should be checked
immediately after the first occurrence in the region of the middle of the calibration range
with a standard from a source different from that used for the initial calibration. The value
determined from the second source check should be within 30% of the expected
concentration. An alternative recovery limit may be appropriate based on the desired
project-specific DQOs. Quantitative sample analyses should not proceed for those
analytes that fail the second source standard initial calibration verification. However,
analyses may continue for those analytes that fail the criteria with an understanding that
these results could be used for screening purposes and would be considered estimated
values.
11.4.3 The initial calibration (Sec. 11.3) for each compound of interest should be
verified once every twelve hours prior to sample analysis, using the introduction technique
and conditions used for samples. This is accomplished by analyzing a calibration
standard (containing all the compounds for quantitation) at a concentration either near the
midpoint concentration for the calibrating range of the GC/MS or near the action level for
the project. The results must be compared against the most recent initial calibration curve
and should meet the verification acceptance criteria provided in Secs. 11.4.5 through
11.4.7.
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.
11.4.4 A method blank should be analyzed prior to sample analyses in order to

ensure that the total system (i.e., 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 Method 8000 for information regarding
method blank performance criteria.
11.4.5 Calibration verification standard criteria
11.4.5.1 Each of the most common target analytes in the calibration

verification standard should meet the minimum RFs as noted in Table 4. This
criterion is particularly important when the common target analytes are also critical
project-required compounds. This is the same check that is applied during the
initial calibration.
11.4.5.2 If the minimum RFs are not met, the system should be
evaluated, and corrective action should be taken before sample analysis begins.

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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.
11.4.5.3 All target compounds of interest must be evaluated using a

20% criterion. Use percent difference when performing the RF model calibration.
Use percent drift when calibrating using a regression fit model. Refer to Method
8000 for guidance on calculating percent difference and drift.
11.4.5.4 If the percent difference or percent drift for a compound is less

than or equal to 20%, then the initial calibration for that compound is assumed to
be valid. Due to the large numbers of compounds that may be analyzed by this
method, it is expected that some compounds will fail to meet the criterion. If the
criterion is not met (i.e., greater than 20% difference or drift) for more than 20% of
the compounds included in the initial calibration, then corrective action must be
taken prior to the analysis of samples. In cases where compounds fail, they may
still be reported as non-detects if it can be demonstrated that there was adequate
sensitivity to detect the compound at the applicable quantitation limit. For
situations when the failed compound is present, the concentrations must be
reported as estimated values.
11.4.5.5 Problems similar to those listed under initial calibration could

affect the ability to pass the calibration verification standard analysis. If the
problem cannot be corrected by other measures, a new initial calibration must be
generated. The calibration verification criteria must be met before sample analysis
begins.
11.4.5.6 The method of linear regression analysis has the potential for
a significant bias to the lower portion of a calibration curve, while the relative
percent difference and quadratic methods of calibration do not have this potential
bias. When calculating the calibration curves using the linear regression model, a
minimum quantitation check on the viability of the lowest calibration point should be
performed by re-fitting the response from the low concentration calibration
standard back into the curve (see Method 8000 for additional details). It is not
necessary to re-analyze a low concentration standard; rather the data system can
recalculate the concentrations as if it were an unknown sample. The recalculated
concentration of the low calibration point should be within ± 30% of the standard's
true concentration. Other recovery criteria may be applicable depending on the
project's DQOs and for those situations the minimum quantitation check criteria
should be outlined in a laboratory SOP, or a project-specific QAPP. Analytes
which do not meet the minimum quantitation calibration re-fitting criteria should be
considered "out of control" and corrective action such as redefining the LLOQ
and/or reporting those "out of control" target analytes as estimated when the
concentration is at or near the lowest calibration point may be appropriate.
11.4.6 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 absolute retention time for any internal standard changes by
more than 30 sec from that in the mid-point standard level of the most recent initial
calibration sequence, then the chromatographic system must be inspected for
malfunctions and corrections must be made, as required. When corrections are made,
reanalysis of samples analyzed while the system was malfunctioning is required.

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11.4.7 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 MS 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.
11.5 Gas chromatography/mass spectrometry analysis of samples
11.5.1 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.
11.5.2 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 of concentrated sample
extract obtained from sample preparation.
11.5.3 Inject an aliquot of the sample extract into the GC/MS system, using the
same operating conditions that were used for the calibration (Sec. 11.3). The volume to
be injected should include an appropriate concentration that is within the calibration range
of base/neutral and acid surrogates using the surrogate solution as noted in Sec. 7.8. The
injection volume must be the same volume that was used for the calibration standards.
11.5.4 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 (usually 40 ng/µL, or other
concentrations as appropriate, if 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 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. Internal standard responses (area counts) should
be monitored in all samples, spikes and blanks for similar reasons. If the EICP
area for any of the internal standards in samples, spikes, and blanks changes by a
factor of two (−50% to +100%) from the areas determined in the continuing
calibration analyzed that day, corrective action should be taken. The samples,
spikes, or blanks should be reanalyzed or the data should be qualified.
11.5.4.1 When ions from a compound in the sample saturate the

detector, this analysis should 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. Contamination from
one sample to the next on the instrument usually takes place in the syringe. If
adequate syringe washers are employed, then carryover from high concentration
samples can usually be avoided.
11.5.4.2 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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11.5.5 The use of a selected ion monitoring (SIM) technique is acceptable for
applications requiring quantitation limits below the normal range of electron impact mass
spectrometry. However, SIM may provide a lesser degree of confidence in the compound
identification, since less mass spectral information is available. Using the primary ion for
quantitation and the secondary ions for confirmation, set up the collection groups based on
their retention times. The selected ions are nominal ions and most compounds have small
mass defect, usually less than 0.2 amu, in their spectra. These mass defects should be
used in the acquisition table. The dwell time may be automatically calculated by the
laboratory's GC/MS software or manually calculated using the following formula. The total
scan time should be less than 1,000 msec and produce at least 5 to 10 scans per
chromatographic peak. The start and stop times for the SIM groups are determined from
the full scan analysis using the formula below:
Scan Time (msec)

Dwell Time for the Group =
Total Ions in the Group
Additional guidance for performing SIM analyses, in particular for PAHs and phenol target
analyte compounds, can be found in the most recent CLP semivolatile organic methods
statement of work (SOW). See the SIM sections from the following CLP SOW for further
details: EPA CLP Organics SOW (Reference 14).
11.6 Analyte identification
11.6.1 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.
11.6.1.1 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.
11.6.1.2 The RRT of the sample component is within ± 0.06 RRT units
of the RRT of the standard component.
11.6.1.3 The relative intensities of the characteristic ions agree within

30% of the relative intensities of these ions in the reference spectrum. For
example, an ion with an abundance of 50% in the reference spectrum, the
corresponding abundance in a sample spectrum can range between 20% and
80%. Use professional judgment in interpretation where interferences are
observed.
11.6.1.4 Structural isomers that produce very similar mass spectra

should be identified as individual isomers if they have sufficiently different gas
chromatographic retention times. Sufficient gas chromatographic resolution is
achieved if the height of the valley between two isomer peaks is less than 50% of

July 2014
the average of the two peak heights. Otherwise, structural isomers are identified as
isomeric pairs. The resolution should be verified on the mid-point concentration of
the initial calibration as well as the laboratory designated continuing calibration
verification level if closely eluting isomers are to be reported (e.g.,
benzo(b)fluoranthene and benzo(k)fluoranthene).
11.6.1.5 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.
11.6.1.6 Examination of extracted ion current profiles of appropriate

ions can aid in the selection of spectra and in qualitative identification of
compounds. When analytes co-elute (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 co-eluting compound.
11.6.2 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 (i.e., 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 ± 30%. For
example, an ion with an abundance of 50% in the standard spectrum must
have a corresponding sample ion abundance between 20 and 80%.
(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
co-eluting 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 co-eluting peaks. Data system
library reduction programs can sometimes create these discrepancies.

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11.7 Quantitation
11.7.1 Once a target compound has been identified, the quantitation of that
compound will be based on the integrated abundance of the primary characteristic ion
from the EICP.
11.7.1.1 It is highly recommended to use the integration produced by

the software if the integration is correct because the software should produce more
consistent integrations than an analyst will manually. However, manual
integrations may be necessary when the software does not produce proper
integrations because baseline selection is improper; the correct peak is missed; a
coelution is integrated; the peak is partially integrated; etc. The analyst is
responsible for ensuring that the integration is correct whether performed by the
software or done manually.
11.7.1.2 Manual integrations should not be substituted for proper

maintenance of the instrument or setup of the method (e.g., retention time updates,
integration parameter files, etc.). The analyst should seek to minimize manual
integration by properly maintaining the instrument, updating retention times, and
configuring peak integration parameters.
11.7.2 If the RSD of a compound's RF is 20% or less, then the concentration in

the extract may be determined using the RF from initial calibration data (Sec. 11.3.4). See
Method 8000 for the equations describing internal standard calibration and either linear or
non-linear calibrations.
11.7.3 Where applicable, the concentration of any non-target analytes identified

in the sample (Sec. 11.6.2) should be estimated. The same formula as in Sec. 11.3.4
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.
11.7.4 The resulting concentration should be reported indicating that the value is
an estimate. Use the nearest internal standard free of interferences.
11.7.5 Quantitation of multicomponent compounds (e.g., toxaphene, Aroclors,

etc.) is beyond the scope of Method 8270. Normally, quantitation is performed using a
GC/ECD, for example by Methods 8081 or 8082. However, this 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.
11.7.6 Quantitation of multicomponent parameters such as diesel range organics

(DROs) and total petroleum hydrocarbons (TPH) using the Method 8270 recommended
internal standard quantitation technique is beyond the scope of this method. Typically,
analyses for these parameters are performed using GC/FID or GC with a MS detector
capability that is available with Method 8015.
11.7.7 Structural isomers that produce very similar mass spectra should be
quantitated as individual isomers if they have sufficiently different gas chromatographic
retention times. Sufficient gas chromatographic resolution is achieved if the height of the
valley between two isomer peaks is less than 50% of the average of the two peak heights.
Otherwise, structural isomers are identified as isomeric pairs. The resolution should be
verified on the mid-point concentration of the initial calibration as well as the laboratory
designated continuing calibration verification level if closely eluting isomers are to be
reported (e.g., benzo(b)fluoranthene and benzo(k)fluoranthene).
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12.0 DATA ANALYSIS AND CALCULATIONS
See Sec. 11.7 and Method 8000 for information on data analysis and calculations.
13.0 METHOD PERFORMANCE
13.1 Performance data and related information are provided in SW-846 methods only as
examples and guidance. The data do not represent required performance criteria for users of
the methods. Instead, performance criteria should be developed on a project-specific basis,
and the laboratory should establish in-house QC performance criteria for the application of this
method. These performance data are not intended to be and must not be used as absolute QC
acceptance criteria for purposes of laboratory accreditation.
13.2 Single laboratory initial demonstration of capability data were generated from five
replicate measurements using a modified continuous liquid-liquid extractor (Method 3520) with
hydrophobic membrane. In this case only a single acid pH extraction was performed using the
CLP calibration criteria and the applicable CLP target analytes. These data are presented in
Table 6. Laboratories should generate their own acceptance criteria depending on the
extraction and instrument conditions. See Method 8000 for more detailed guidance.
13.3 Chromatograms from calibration standards analyzed with Day 0 and Day 7
samples were compared to detect possible deterioration of gas chromatographic performance.
These recoveries (using Method 3510 extraction) are presented in Table 7. These data are
provided for guidance purposes only.
13.4 Method performance data using Method 3541 (i.e., automated Soxhlet extraction)
are presented in Tables 8 and 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 one 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 GC/MS following Method 8270. The low recovery of the more volatile
compounds is probably due to volatilization losses during equilibration. These data as listed
were taken from Reference 7 and are provided for guidance purposes only.
13.5 Surrogate precision and accuracy data are presented in Table 10 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 this method (i.e., 8270).
These data are provided for guidance purposes only.
13.6 Single laboratory precision and bias data using Method 3545 (i.e., pressurized fluid
extraction) for semivolatile organic compounds are presented in Table 11. The samples were
conditioned spiked samples prepared and certified by a commercial supplier that contained 57
semivolatile organics at three concentrations (i.e., 250, 2500, and 12,500 µg/kg) on three types
of soil (i.e, clay, loam, and sand). Spiked samples were extracted both by the Dionex ASE
system and by the Perstorp Environmental SoxtecTM (i.e., automated Soxhlet). The data in
Table 11 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%.
These data are provided for guidance purposes only.

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13.7 Single laboratory precision and bias data using Method 3561 (i.e., 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 (i.e., 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 ranged from 85 to 148%, with an 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 ranged from 73 to 133%, with an overall average of 92%, based on the
certified value for the marine sediment. The data are found in Tables 12 and 13 and were taken
from Reference 10. These data are provided for guidance purposes only.
13.8 Single laboratory precision and accuracy using Method 3561 (i.e., SFE extraction
of PAHs with a fixed restrictor and liquid trapping) were obtained for twelve of the method
analytes by the extraction of a certified reference material (i.e., 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 ranged from 60 to
122%, with an overall average of 89%, based on the certified value. The instrument conditions
that were utilized to extract a 3.4 g sample were as follows: Pressure - 300 atm; time - 60 min;
extraction fluid - CO2; modifier - 10% 1:1 (v/v) methanol/methylene chloride; Oven temperature -
80 °C; Restrictor temperature - 120 °C; and, trapping fluid - chloroform (methylene chloride has
also been used). The data are found in Table 14 and were taken from Reference 11. These
data are provided for guidance purposes only.
13.9 Tables 15 and 16 contain single-laboratory precision and accuracy data for solid-
phase extraction of TCLP buffer solutions spiked at two levels and extracted using Method
3535. These data are provided for guidance purposes only.
13.10 Table 17 contains multiple-laboratory data for solid-phase extraction of spiked

TCLP soil leachates extracted using Method 3535. These data are provided for guidance
purposes only.
13.11 Tables 18 through 22 contain single-laboratory PAH recovery data for microwave
extraction of contaminated soils and standard reference materials using Method 3546. These
data are provided for guidance purposes only.
14.0 POLLUTION PREVENTION
14.1 Pollution prevention encompasses any technique that reduces or eliminates the
quantity and/or toxicity of waste at the point of generation. Numerous opportunities for pollution
prevention exist in laboratory operations. The EPA has established a preferred hierarchy of
environmental management techniques that places pollution prevention as the management
option of first choice. Whenever feasible, laboratory personnel should use pollution prevention
techniques to address their waste generation. When wastes cannot be feasibly reduced at the
source, the Agency recommends recycling as the next best option.
14.2 For information about pollution prevention that may be applicable to laboratories
and research institutions consult Less is Better: Laboratory Chemical Management for Waste
Reduction, a free publication available from the ACS, Committee on Chemical Safety,
http://portal.acs.org/portal/fileFetch/C/WPCP_012290/pdf/WPCP_012290.pdf.

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15.0 WASTE MANAGEMENT
The EPA requires that laboratory waste management practices be conducted consistent
with all applicable rules and regulations. The Agency urges laboratories to protect the air,
water, and land by minimizing and controlling all releases from hoods and bench operations,
complying with the letter and spirit of any sewer discharge permits and regulations, and by
complying with all solid and hazardous waste regulations, particularly the hazardous waste
identification rules and land disposal restrictions. For further information on waste
management, consult The Waste Management Manual for Laboratory Personnel available from
the ACS at the web address listed in Sec. 14.2.
16.0 REFERENCES
1. J. W. Eichelberger, L. E. Harris, and W. L. Budde, "Reference Compound to Calibrate Ion

Abundance Measurement in Gas Chromatography-Mass Spectrometry Systems,"
Analytical Chemistry, 47, 995-1000, 1975.
2. P. Olynk, W. L. Budde, and J. W. Eichelberger, "Method Detection Limit for Methods 624
and 625," 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. J. A. Burke, "Gas Chromatography for Pesticide Residue Analysis: Some Practical

Aspects," Journal of the Association of Official Analytical Chemists (AOAC), 48, 1037,
1965.
5. S. V. Lucas, R. A. Kornfeld, "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, Contract No. 68-03-3224, February 20,
1987.
6. T. M. Engel, R. A. Kornfeld, J. S. Warner, and K. D. Andrews, "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, Contract 68-03-3224, June 5, 1987.
7. V. Lopez-Avila (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, EPA 600/X-91/140, October 1991.
8. J. Bursey, R. Merrill, R. McAllister, and J. McGaughey, "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.
9. B. Richter, J. Ezzell, and D. Felix, "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.

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10. H. B. Lee, T. E. Peart, R. L. Hong-You, and D. R. Gere, "Supercritical Carbon Diozide
Extraction of Polycyclic Aromatic Hydrocarbons from Sediments," J. Chromatography, A,
653, 83-91 (1993).
11. S. Warner, "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. C. Markell, "3M Data Submission to EPA," letter to B. Lesnik, June 27, 1995.
13. U.S. EPA Method 525.2, "Determination of Organic Compounds in Drinking Water by
Liquid-Solid Extraction and Capillary Column Gas Chromatography/Mass Spectrometry,"
Environmental Monitoring Systems Laboratory, Office of Research and Development, US
EPA, Cincinnati, OH, Revision 2.0, March 1995.
14. USEPA, Superfund Analytical Services/Contract Laboratory Program (CLP), Multi-Media,

Multi-Concentration Organics Analysis, SOM01.X, Exhibit D - Analytical Methods,
"Analytical Method for the Analysis of Semivolatile Organic Compounds," November,
2003.
17.0 TABLES, DIAGRAMS, FLOW CHARTS, AND VALIDATION DATA
The following pages contain the tables and figures referenced by this method.

July 2014
TABLE 1
CHARACTERISTIC IONS FOR SEMIVOLATILE COMPOUNDS IN APPROXIMATE

RETENTION TIME ORDER a
Compound Primary Ion Secondary Ion(s)

2-Picoline 93 66,92
Aniline 93 66,65
Phenol 94 65,66
Bis(2-chloroethyl) ether 93 63,95
2-Chlorophenol 128 64,130
1,3-Dichlorobenzene 146 148,111
1,4-Dichlorobenzene-d4 (IS) 152 150,115
Benzyl alcohol 108 79,77
N-Nitrosomethylethylamine 88 42,43,56
Bis(2-chloro-1-methylethyl)ether 45 77,121
Ethyl carbamate 62 44,45,74
Thiophenol (Benzenethiol) 110 66,109,84
Methyl methanesulfonate 80 79,65,95
N-Nitrosodi-n-propylamine 70 42,101,130
Hexachloroethane 117 201,199
Maleic anhydride 54 98,53,44
Nitrobenzene 77 123,65
Isophorone 82 95,138
N-Nitrosodiethylamine 102 42,57,44,56
2-Nitrophenol 139 109,65
2,4-Dimethylphenol 122 107,121
p-Benzoquinone 108 54,82,80
Bis(2-chloroethoxy)methane 93 95,123
Benzoic acid 122 105,77
2,4-Dichlorophenol 162 164,98
Trimethyl phosphate 110 79,95,109,140
Ethyl methanesulfonate 79 109,9745,65
1,2,4-Trichlorobenzene 180 182,145
Naphthalene-d8 (IS) 136 68
Naphthalene 128 129,127
Hexachlorobutadiene 225 223,227
Tetraethyl pyrophosphate 99 155,127,81,109
Diethyl sulfate 139 45,59,99,111,125
4-Chloro-3-methylphenol 107 144,142
2-Methylnaphthalene 142 141
2-Methylphenol 107 108,77,79,90
Hexachloropropene 213 211,215,117,106,141
Hexachlorocyclopentadiene 237 235,272
N-Nitrosopyrrolidine 100 41,42,68,69
Acetophenone 105 71,51,120
3/4-Methylphenol b 107 108,77,79,90
2,4,6-Trichlorophenol 196 198,200
o-Toluidine 106 107,77,51,79
2-Chloronaphthalene 162 127,164
N-Nitrosopiperidine 114 42,55,56,41
July 2014
1,4-Phenylenediamine 108 80,53,54,52
1-Chloronaphthalene 162 127,164
2-Nitroaniline 65 92,138
5-Chloro-2-methylaniline 106 141,140,77,89
Dimethyl phthalate 163 194,164
Acenaphthylene 152 151,153
2,6-Dinitrotoluene 165 63,89
Phthalic anhydride 104 76,50,148
o-Anisidine 108 80,123,52
3-Nitroaniline 138 108,92
Acenanaphthene-d10 (IS) 164 162,160
Acenaphthene 154 153,152
2,4-Dinitrophenol 184 63,154
2,6-Dinitrophenol 162 164,126,98,63
4-Chloroaniline 127 129,65,92
Isosafrole 162 131,104,77,51
Dibenzofuran 168 139
2,4-Diaminotoluene 121 122,94,77,104
2,4-Dinitrotoluene 165 63,89
4-Nitrophenol 139 109,65
2-Naphthylamine 143 115,116
1,4-Naphthoquinone 158 104,102,76,50,130
p-Cresidine 122 94,137,77,93
Dichlorovos 109 185,79,145
Diethyl phthalate 149 177,150
Fluorene 166 165,167
2,4,5-Trimethylaniline 120 135,134,91,77
N-Nitrosodi-n-butylamine 84 57,41,116,158
4-Chlorophenyl phenyl ether 204 206,141
Hydroquinone 110 81,53,55
4,6-Dinitro-2-methylphenol 198 51,105
Resorcinol 110 81,82,53,69
N-Nitrosodiphenylamine 169 168,167
Safrole 162 104,77,103,135
Hexamethyl phosphoramide 135 44,179,92,42
3-(Chloromethyl)pyridine hydrochloride 92 127,129,65,39
Diphenylamine 169 168,167
1,2,4,5-Tetrachlorobenzene 216 214,179,108,143,218
1-Naphthylamine 143 115,89,63
1-Acetyl-2-thiourea 118 43,42,76
4-Bromophenyl phenyl ether 248 250,141
Toluene diisocyanate 174 145,173,146,132,91
2,4,5-Trichlorophenol 196 198,97,132,99
Hexachlorobenzene 284 142,249
Nicotine 84 133,161,162
Pentachlorophenol 266 264,268
5-Nitro-o-toluidine 152 77,79,106,94
Thionazine 107 96,97,143,79,68
4-Nitroaniline 138 65,108,92,80,39
Phenanthrene-d10 (IS) 188 94,80
Phenanthrene 178 179,176
Anthracene 178 176,179
July 2014
1,4-Dinitrobenzene 168 75,50,76,92,122
Mevinphos 127 192,109,67,164
Naled 109 145,147,301,79,189
1,3-Dinitrobenzene 168 76,50,75,92,122
Diallate (cis or trans) 86 234,43,70
1,2-Dinitrobenzene 168 50,63,74
Diallate (trans or cis) 86 234,43,70
Pentachlorobenzene 250 252,108,248,215,254
5-Nitro-o-anisidine 168 79,52,138,153,77
Pentachloronitrobenzene 237 142,214,249,295,265
4-Nitroquinoline-1-oxide 174 101,128,75,116
Di-n-butyl phthalate 149 150,104
2,3,4,6-Tetrachlorophenol 232 131,230,166,234,168
Dihydrosaffrole 135 64,77
Demeton-O 88 89,60,61,115,171
Fluoranthene 202 101,203
1,3,5-Trinitrobenzene 75 74,213,120,91,63
Dicrotophos 127 67,72,109,193,237
Benzidine 184 92,185
Trifluralin 306 43,264,41,290
Bromoxynil 277 279,88,275,168
Pyrene 202 200,203
Monocrotophos 127 192,67,97,109
Phorate 75 121,97,93,260
Sulfallate 188 88,72,60,44
Demeton-S 88 60,81,89,114,115
Phenacetin 108 180,179,109,137,80
Dimethoate 87 93,125,143,229
Phenobarbital 204 117,232,146,161
Carbofuran 164 149,131,122
Octamethyl pyrophosphoramide 135 44,199,286,153,243
4-Aminobiphenyl 169 168,170,115
Dioxathion 97 125,270,153
Terbufos 231 57,97,153,103
α,α-Dimethylphenylamine 58 91,65,134,42
Pronamide 173 175,145,109,147
Aminoazobenzene 197 92,120,65,77
Dichlone 191 163,226,228,135,193
Dinoseb 211 163,147,117,240
Disulfoton 88 97,89,142,186
Fluchloralin 306 63,326,328,264,65
Mexacarbate 165 150,134,164,222
4,4'-Oxydianiline 200 108,171,80,65
Butyl benzyl phthalate 149 91,206
4-Nitrobiphenyl 199 152,141,169,151
Phosphamidon 127 264,72,109,138
2-Cyclohexyl-4,6-Dinitrophenol 231 185,41,193,266
Methyl parathion 109 125,263,79,93
Carbaryl 144 115,116,201
Dimethylaminoazobenzene 225 120,77,105,148,42
Propylthiouracil 170 142,114,83
Benz(a)anthracene 228 229,226
July 2014
Chrysene-d12 (IS) 240 120,236
3,3'-Dichlorobenzidine 252 254,126
Chrysene 228 226,229
Malathion 173 125,127,93,158
Kepone 272 274,237,178,143,270
Fenthion 278 125,109,169,153
Parathion 109 97,291,139,155
Anilazine 239 241,143,178,89
Bis(2-ethylhexyl)phthalate 149 167,279
3,3'-Dimethylbenzidine 212 106,196,180
Carbophenothion 157 97,121,342,159,199
5-Nitroacenaphthene 199 152,169,141,115
Methapyrilene 97 50,191,71
Isodrin 193 66,195,263,265,147
Captan 79 149,77,119,117
Chlorfenvinphos 267 269,323,325,295
Crotoxyphos 127 105,193,166
Phosmet 160 77,93,317,76
EPN 157 169,185,141,323
Tetrachlorvinphos 329 109,331,79,333
Di-n-octyl phthalate 149 167,43
2-Aminoanthraquinone 223 167,195
Barban 222 51,87,224,257,153
Aramite 185 191,319,334,197,321
Benzo(b)fluoranthene 252 253,125
Nitrofen 283 285,202,139,253
Benzo(k)fluoranthene 252 253,125
Chlorobenzilate 251 139,253,111,141
Fensulfothion 293 97,308,125,292
Ethion 231 97,153,125,121
Diethylstilbestrol 268 145,107,239,121,159
Famphur 218 125,93,109,217
Tri-p-tolyl phosphatec 368 367,107,165,198
Benzo(a)pyrene 252 253,125
Perylene-d12 (IS) 264 260,265
7,12-Dimethylbenz(a)anthracene 256 241,239,120
5,5-Diphenylhydantoin 180 104,252,223,209
Captafol 79 77,80,107
Dinocap 69 41,39
Methoxychlor 227 228,152,114,274,212
2-Acetylaminofluorene 181 180,223,152
4,4'-Methylenebis(2-chloroaniline) 231 266,268,140,195
3,3'-Dimethoxybenzidine 244 201,229
3-Methylcholanthrene 268 252,253,126,134,113
Phosalone 182 184,367,121,379
Azinphos-methyl 160 132,93,104,105
Leptophos 171 377,375,77,155,379
Mirex 272 237,274,270,239,235
Tris(2,3-dibromopropyl)phosphate 201 137,119,217,219,199
Dibenz(a,j)acridine 279 280,277,250
Mestranol 277 310,174,147,242
Coumaphos 362 226,210,364,97,109
July 2014
Indeno(1,2,3-cd)pyrene 276 138,277
Dibenz(a,h)anthracene 278 139,279
Benzo(g,h,i)perylene 276 138,277
1,2:4,5-Dibenzopyrene 302 151,150,300
Strychnine 334 334,335,333
Piperonyl sulfoxide 162 135,105,77
Hexachlorophene 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
The data presented are representative of DB-5 type analytical columns.
b
Compounds cannot be separated for quantitation
c
Substitute for the non-specific mixture, tricresyl phosphate

July 2014
TABLE 2
EXAMPLE LOWER LIMITS OF QUANTITATION FOR SEMIVOLATILE ORGANICS
Lower Limits of Quantitationa

Ground water Low Soil/Sedimentb
Compound (µg/L) (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-chloro-1-methylethyl)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
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
July 2014
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
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
3,3'-Dimethylbenzidine 10 ND
2,4-Dimethylphenol 10 660
Dimethyl phthalate 10 660
1,2-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
July 2014
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
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
N-Nitrosodiphenylamine 10 660
N-Nitroso-di-n-propylamine 10 660
July 2014
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
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

July 2014
a
Sample LLOQs are highly matrix-dependent and those listed here are provided for guidance
and may not always be achievable.
b
LLOQs listed for soil/sediment are based on wet weight. When data are reported on a dry
weight basis, the lower limits will be higher based on the % dry weight of each sample. These
lower limits 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 extraction 7.5

Non-water miscible waste 75
c
LLOQ=(LLOQ for low soil/sediment given above in Table 2) x (Factor)

July 2014
TABLE 3
DFTPP KEY IONS AND ION ABUNDANCE CRITERIAa,b
Mass Ion Abundance Criteria

51 10-80% of Base Peak
68 < 2% of mass 69
70 < 2% of mass 69
197 < 2% of mass 198
198 Base peak, or > 50% of Mass 442
199 5-9% of mass 198
365 > 1% of mass 198
441 present but < 24% of mass 442
442 Base Peak, or > 50% of mass 198
443 15-24% of mass 442
a
The majority of the data are taken from Reference 13 (Method 525.2).
b
The criteria in this table are intended to be used as default criteria for quadrupole
instrumentation if optimized manufacturer's operating conditions are not available.
Alternate tuning criteria may be employed (e.g., CLP or Method 625), provided that
method performance is not adversely affected. See Sec. 11.3.1.

July 2014
TABLE 4
RECOMMENDED MINIMUM RESPONSE FACTOR CRITERIA FOR INITIAL AND

CONTINUING CALIBRATION VERIFICATION USING THE SUGGESTED IONS
FROM TABLE 1
Minimum Response
Semivolatile Compounds
Factor (RF)
Benzaldehyde 0.010
Phenol 0.800
Bis(2-chloroethyl)ether 0.700
2-Chlorophenol 0.800
2-Methylphenol 0.700
2,2'-Oxybis-(1-chloropropane) 0.010
Acetophenone 0.010
4-Methylphenol 0.600
N-Nitroso-di-n-propylamine 0.500
Hexachloroethane 0.300
Nitrobenzene 0.200
Isophorone 0.400
2-Nitrophenol 0.100
2,4-Dimethylphenol 0.200
Bis(2-chloroethoxy)methane 0.300
2,4-Dichlorophenol 0.200
Naphthalene 0.700
4-Chloroaniline 0.010
Hexachlorobutadiene 0.010
Caprolactam 0.010
4-Chloro-3-methylphenol 0.200
2-Methylnaphthalene 0.400
Hexachlorocyclopentadiene 0.050
2,4,6-Trichlorophenol 0.200
2,4,5-Trichlorophenol 0.200
1,1'-Biphenyl 0.010
2-Chloronaphthalene 0.800
2-Nitroaniline 0.010
Dimethyl phthalate 0.010
2,6-Dinitrotoluene 0.200
Acenaphthylene 0.900
Acenaphthene 0.900
2,4-Dinitrophenol 0.010
4-Nitrophenol 0.010
Dibenzofuran 0.800
2,4-Dinitrotoluene 0.200
Diethyl phthalate 0.010
1,2,4,5-Tetrachlorobenzene 0.010
4-Chlorophenyl-phenyl ether 0.400
Fluorene 0.900
4,6-Dinitro-2-methylphenol 0.010
4-Bromophenyl-phenyl ether 0.100
N-Nitrosodiphenylamine 0.010
Hexachlorobenzene 0.100

July 2014
Minimum Response
Semivolatile Compounds
Factor (RF)
Atrazine 0.010
Pentachlorophenol 0.050
Phenanthrene 0.700
Anthracene 0.700
Carbazole 0.010
Di-n-butyl phthalate 0.010
Fluoranthene 0.600
Pyrene 0.600
Butyl benzyl phthalate 0.010
3,3'-Dichlorobenzidine 0.010
Benzo(a)anthracene 0.800
Chrysene 0.700
Bis-(2-ethylhexyl)phthalate 0.010
Di-n-octyl phthalate 0.010
Benzo(b)fluoranthene 0.700
Benzo(k)fluoranthene 0.700
Benzo(a)pyrene 0.700
Indeno(1,2,3-cd)pyrene 0.500
Dibenz(a,h)anthracene 0.400
Benzo(g,h,i)perylene 0.500
2,3,4,6-Tetrachlorophenol 0.010

July 2014
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-chloro-1-methylethyl)
4-Chloroaniline 2-Chloronaphthalene
ether
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-Dimethylphenethylamine Dimethyl phthalate
Ethyl methanesulfonate 2,4-Dimethylphenol 2,4-Dinitrophenol
2-Fluorophenol (surr) Hexachlorobutadiene 2,4-Dinitrotoluene
Hexachloroethane Isophorone 2,6-Dinitrotoluene
Methyl methanesulfonate 2-Methylnaphthalene Fluorene
2-Methylphenol Naphthalene 2-Fluorobiphenyl (surr)
4-Methylphenol Nitrobenzene Hexachlorocyclopentadiene
N-Nitrosodimethylamine Nitrobenzene-d8 (surr) 1-Naphthylamine
N-Nitroso-di-n-propylamine 2-Nitrophenol 2-Naphthylamine
Phenol N-Nitrosodi-n-butylamine 2-Nitroaniline
Phenol-d6 (surr) N-Nitrosopiperidine 3-Nitroaniline
2-Picoline 1,2,4-Trichlorobenzene 4-Nitroaniline
4-Nitrophenol
Pentachlorobenzene
1,2,4,5-Tetrachlorobenzene
2,3,4,6-Tetrachlorophenol
2,4,6-Tribromophenol (surr)
2,4,6-Trichlorophenol
2,4,5-Trichlorophenol
(surr) = surrogate

July 2014
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 7,12-Dimethylbenz(a)anthracene
Hexachlorobenzene Pyrene Di-n-octyl phthalate
N-Nitrosodiphenylamine Terphenyl-d14 (surr) Indeno(1,2,3-cd)pyrene
Pentachlorophenol 3-Methylcholanthrene
Pentachloronitrobenzene
Phenacetin
Phenanthrene
Pronamide
(surr) = surrogate

July 2014
TABLE 6
EXAMPLE SINGLE LABORATORY PERFORMANCE DATAa
Test conc. x of 5 % Recovery

Compound replicates
(µg/L) of Avg.
(µg/L)
Acenaphthene 50 46.7 93.4
Acenaphthylene 50 46.1 92.2
Aniline 50 8.3 16.7
Anthracene 50 48.4 96.8
Benzoic acid 50 43.7 87.4
Benzo(a)anthracene 50 49.6 99.2
Benzo(b)fluoranthene 50 49.8 99.6
Benzo(k)fluoranthene 50 50.6 101
Benzo(a)pyrene 50 47.7 95.5
Benzo(g,h,i)perylene 50 52.6 105
Benzyl alcohol 50 44.4 88.8
Bis(2-chloroethyl)ether 50 44.2 88.4
Bis(2-chloroethoxy)methane 50 46.6 93.1
Bis(2-chloro-1-methylethyl)ether 50 43.4 86.8
Bis(2-ethylhexyl)phthalate 50 50.2 100
4-Bromophenyl phenyl ether 50 48.6 97.2
Butyl benzyl phthalate 50 49.6 99.3
Carbazole 50 52.1 104
2-Chloroaniline 50 38.9 77.7
4-Chloro-3-methylphenol 50 47.3 94.6
2-Chloronaphthalene 50 45.3 90.8
2-Chlorophenol 50 43.1 86.2
4-Chlorophenyl phenyl ether 50 47.3 94.6
Chrysene 50 50.3 101
Dibenzofuran 50 47.4 94.7
Dibenz(a,h)anthracene 50 51.6 103
Di-n-butyl phthalate 50 50.5 101
1,2-Dichlorobenzene 50 35.8 71.6
3,3'-Dichlorobenzidine 50 32.0 64.0
2,4-Dichlorophenol 50 47.4 94.8
Diethyl phthalate 50 50.0 99.9
Dimethyl phthalate 50 48.5 97.0
2,4-Dimethylphenol 50 31.2 62.3
4,6-Dinitro-2-methylphenol 50 57.6 115
2,4-Dinitrophenol 50 58.7 117
2,4-Dinitrotoluene 50 51.3 103
2,6-Dinitrotoluene 50 50.2 100
Di-n-octyl phthalate 50 51.1 102
Fluoranthene 50 51.0 102
July 2014
Test conc. x of 5 % Recovery
Compound replicates
(µg/L) of Avg.
(µg/L)
Fluorene 50 48.5 97.0
Hexachlorobenzene 50 49.0 97.9
Hexachlorobutadiene 50 34.7 69.5
Hexachlorocyclopentadiene 50 1.9 3.8
Hexachloroethane 50 29.9 58.8
Indeno(1,2,3-cd)pyrene 50 51.7 103
Isophorone 50 47.1 94.3
2-Methylnaphthalene 50 44.7 89.4
2-Methylphenol 50 41.7 83.4
4-Methylphenol 50 42.6 85.2
Naphthalene 50 43.4 86.8
2-Nitroaniline 50 48.4 96.7
3-Nitroaniline 50 46.8 93.6
4-Nitroaniline 50 56.1 112
Nitrobenzene 50 47.1 94.1
2-Nitrophenol 50 47.3 94.6
4-Nitrophenol 50 55.4 111
N-Nitrosodiphenylamine 50 46.7 93.4
N-Nitroso-di-propylamine 50 44.6 89.3
Pentachlorophenol 50 56.9 114
Phenanthrene 50 49.7 99.4
Phenol 50 40.9 81.8
Pyrene 50 49.2 98.4
1,2,4-Trichlorobenzene 50 39.1 78.2
2,4,5-Trichlorophenol 50 47.7 95.4
2,4,6-Trichlorophenol 50 49.2 98.4
x =Average recovery for five initial demonstrations of capability measurements, in µg/L

a
Extraction using acidic pH only with a modified continuous liquid-liquid extractor with
hydrophobic membrane according to Method 3520. These values are for guidance only.
Appropriate derivation of acceptance criteria for similar extraction conditions may result in much
different recovery ranges. See Method 8000 for information on developing and updating
acceptance criteria for method performance.

July 2014
TABLE 7
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-
dimethylaniline) 108 4 90 4
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.

July 2014
TABLE 8
MEAN PERCENT RECOVERIES AND PERCENT RSD VALUES FOR SEMIVOLATILE

ORGANIC FROM SPIKED CLAY SOIL AND TOPSOIL BY AUTOMATED SOXHLET
(SOXTEC) EXTRACTION (METHOD 3541) WITH HEXANE-ACETONE (1:1)a
Clay Soil Top Soil

Mean Mean
RSD 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;
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.

July 2014
TABLE 9
SINGLE LABORATORY ACCURACY AND PRECISION DATA FOR THE EXTRACTION

OF SEMIVOLATILE ORGANICS FROM SPIKED CLAY BY
AUTOMATED SOXHLET (SOXTEC) (METHOD 3541)a
Compound Mean Recovery RSD

Phenol 47.8 5.6
Bis(2-chloroethyl) ether 25.4 13
2-Chlorophenol 42.7 4.3
Benzyl alcohol 55.9 7.2
2-Methylphenol 17.6 6.6
Bis(2-chloro-1-methylethyl)ether 15.0 15
4-Methylphenol 23.4 6.7
N-Nitroso-di-n-propylamine 41.4 6.2
Nitrobenzene 28.2 7.7
Isophorone 56.1 4.2
2-Nitrophenol 36.0 6.5
2,4-Dimethylphenol 50.1 5.7
Benzoic acid 40.6 7.7
Bis(2-chloroethoxy)methane 44.1 3.0
2,4-Dichlorophenol 55.6 4.6
1,2,4-Trichlorobenzene 18.1 31
Naphthalene 26.2 15
4-Chloroaniline 55.7 12
4-Chloro-3-methylphenol 65.1 5.1
2-Methylnaphthalene 47.0 8.6
Hexachlorocyclopentadiene 19.3 19
2,4,6-Trichlorophenol 70.2 6.3
2,4,5-Trichlorophenol 26.8 2.9
2-Chloronaphthalene 61.2 6.0
2-Nitroaniline 73.8 6.0
Dimethyl phthalate 74.6 5.2
Acenaphthylene 71.6 5.7
Acenaphthene 79.2 4.0
2,4-Dinitrophenol 91.9 8.9
4-Nitrophenol 62.9 16
Dibenzofuran 82.1 5.9
2,4-Dinotrotoluene 84.2 5.4
2,6-Dinitrotoluene 68.3 5.8
Diethyl phthalate 74.9 5.4
4-Chlorophenyl-phenyl ether 67.2 3.2
Fluorene 82.1 3.4
4,6-Dinitro-2-methylphenol 63.4 6.8
N-Nitrosodiphenylamine 77.0 3.4
4-Bromophenyl-phenyl ether 62.4 3.0

July 2014
Compound Mean Recovery RSD
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
Dibenz(a,h)anthracene 66.7 6.3
Benzo(g,h,i)perylene 63.9 8.0
1,2-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; 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.

July 2014
TABLE 10
PRECISION AND BIAS VALUES FOR METHOD 3542a
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
a
The surrogate values shown in Table 10 represent mean recoveries for surrogates in all
Method 0010 matrices in a field dynamic spiking study.

July 2014
TABLE 11
PRESSURIZED FLUID 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-chloro-1-methylethyl)
109.4 71.5 108.0 81.8 81.0 88.6 118.1 148.3 94.8 100.2
ether
o-Toluidine 100.0 89.7 117.2 100.0 *152.5 120.3 100.0 *199.5 102.7 110.3
N-Nitroso-di-n-propylamine 103.0 79.1 107.7 83.9 88.1 96.2 109.9 123.3 91.4 98.1
Hexachloroethane 97.1 125.1 111.0 *245.4 117.1 128.1 *566.7 147.9 103.7 118.6
Nitrobenzene 104.8 82.4 106.6 86.8 84.6 101.7 119.7 122.1 93.3 100.2
Isophorone 100.0 86.4 98.2 87.1 87.5 109.7 135.5 118.4 92.7 101.7
2,4-Dimethylphenol 100.0 104.5 140.0 100.0 114.4 123.1 100.0 *180.6 96.3 109.8
2-Nitrophenol 80.7 80.5 107.9 91.4 86.7 103.2 122.1 107.1 87.0 96.3
Bis(chloroethoxy)methane 94.4 80.6 94.7 86.5 84.4 99.6 130.6 110.7 93.2 97.2
2,4-Dichlorophenol 88.9 87.8 111.4 85.9 87.6 103.5 123.3 107.0 92.1 98.6
1,2,4-Trichlorobenzene 98.0 97.8 98.8 123.0 93.7 94.5 137.0 99.4 95.3 104.2
Naphthalene 101.7 97.2 123.6 113.2 102.9 129.5 *174.5 114.0 89.8 106.1
4-Chloroaniline 100.0 *150.2 *162.4 100.0 125.5 *263.6 100.0 *250.8 114.9 108.1
Hexachlorobutadiene 101.1 98.7 102.2 124.1 90.3 98.0 134.9 96.1 96.8 104.7
4-Chloro-3-methylphenol 90.4 80.2 114.7 79.0 85.2 109.8 131.6 116.2 90.1 99.7
2-Methylnaphthalene 93.2 89.9 94.6 104.1 92.2 105.9 146.2 99.1 93.3 102.1
Hexachlorocyclopentadiene 100.0 100.0 0.0 100.0 100.0 6.8 100.0 100.0 *238.3 75.8
2,4,6-Trichlorophenol 94.6 90.0 112.0 84.2 91.2 103.6 101.6 95.9 89.8 95.9
2,4,5-Trichlorophenol 84.4 91.9 109.6 96.1 80.7 103.6 108.9 83.9 87.9 94.1
2-Chloronaphthalene 100.0 91.3 93.6 97.6 93.4 98.3 106.8 93.0 92.0 96.2
2-Nitroaniline 90.0 83.4 97.4 71.3 88.4 89.9 112.1 113.3 87.7 92.6
2,6-Dinitrotoluene 83.1 90.6 91.6 86.4 90.6 90.3 104.3 84.7 90.9 90.3
Acenaphthylene 104.9 95.9 100.5 99.0 97.9 108.8 118.5 97.8 92.0 101.7
3-Nitroaniline *224.0 115.6 97.6 100.0 111.8 107.8 0.0 111.7 99.0 92.9
Acenaphthene 102.1 92.6 97.6 97.2 96.9 104.4 114.2 92.0 89.0 98.4
4-Nitrophenol 0.0 93.2 121.5 18.1 87.1 116.6 69.1 90.5 84.5 75.6
2,4-Dinitrotoluene 73.9 91.9 100.2 84.7 93.8 98.9 100.9 84.3 87.3 90.7
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 ether 85.6 92.9 92.8 91.1 107.6 89.4 118.0 97.5 87.1 95.8
Hexachlorobenzene 95.4 91.7 92.3 95.4 93.6 83.7 106.8 94.3 90.0 93.7
July 2014
Clay Loam Sand Mean
Compound
Low Mid High Low Mid High Low Mid High Rec.
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.

July 2014
TABLE 12
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
RSDs 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.

July 2014
TABLE 13

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

Compound
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
RSDs for the SFE values are based on three replicate extractions.

July 2014
TABLE 14

FROM A CERTIFIED REFERENCE SOIL SRS103-100, USING METHOD 3561
(SFE – LIQUID TRAP)

Compound
Naphthalene 32.4 ± 8.2 29.55 91 10.5
2-Methylnaphthalene 62.1 ± 11.5 76.13 122 2.0
Acenaphthene 632 ± 105 577.28 91 2.9
Dibenzofuran 307 ± 49 302.25 98 4.1
Fluorene 492 ± 78 427.15 87 3.0
Phenanthrene 1618 ± 340 1278.03 79 3.4
Anthracene 422 ± 49 400.80 95 2.6
Fluoranthene 1280 ± 220 1019.13 80 4.5
Pyrene 1033 ± 285 911.82 88 3.1
Benz(a)anthracene 252 ± 8 225.50 89 4.8
Chrysene 297 ± 26 283.00 95 3.8
Benzo(a)pyrene 97.2 ± 17.1 58.28 60 6.5
Benzo(b)fluoranthene +
153 ± 22 130.88 86 10.7
Benzo(k)fluoranthene
a
RSDs for the SFE values are based on four replicate extractions.

July 2014
TABLE 15
SINGLE LABORATORY RECOVERY DATA FOR SPE (METHOD 3535) OF

BASE/NEUTRAL/ACID EXTRACTABLES FROM SPIKED TCLP BUFFERS
LOW SPIKE LEVEL
Spike Buffer 1 (pH=2.886) Buffer 2 (pH=4.937)

Analyte Level
(µg/L) Recovery (%) RSD Recovery (%) RSD
1,4-Dichlorobenzene 3,750 63 10 63 9
Hexachloroethane 1,500 55 6 77 4
Nitrobenzene 1,000 82 10 100 5
Hexachlorobutadiene 250 65 3 56 4
2,4-Dinitrotoluene 65 89 4 101 5
Hexachlorobenzene 65 98 5 95 6
o-Cresol 100,000 83 10 85 5
m-Cresol* 100,000 86 8 85 3
p-Cresol* 100,000 * * * *
2,4,6-Trichlorophenol 1,000 84 12 95 12
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 quantified as a mixture of both isomers.
Data from Reference 12.

July 2014
TABLE 16
SINGLE LABORATORY RECOVERY DATA FOR SPE (METHOD 3535) OF

BASE/NEUTRAL/ACID EXTRACTABLES FROM SPIKED TCLP BUFFERS
HIGH SPIKE LEVEL
Spike Buffer 1 (pH=2.886) Buffer 2 (pH=4.937)

Analyte Level
(µg/L) Recovery (%) RSD 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
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.

July 2014
TABLE 17
RECOVERY DATA FROM THREE LABORATORIES FOR SPE (METHOD 3535)

OF BASE/NEUTRAL/ACID/EXTRACTABLES FROM SPIKED TCLP LEACHATES FROM SOIL
SAMPLES
Buffer 1 pH=2.886 Lab 1 Lab 2 Lab 3

Spike
Level
Analyte (µg/L)* %R RSD n %R RSD n %R RSD n
o-Cresol 200,000 86 8 7 35.3 0.7 3 7.6 6 3

m-Cresol** -- 77 8 7 -- -- -- -- -- --
p-Cresol** -- -- -- -- -- -- -- 7.7 11 3
2,4,6-Trichlorophenol 2,000 106 6 7 96.3 3.9 3 44.8 5 3
Pentachlorophenol 100,000 79 2 7 33.8 12.2 3 29.2 13 3
1,4-Dichlorobenzene 7,500 51 5 7 81.3 5.3 3 19.2 7 3
Hexachloroethane 3,000 50 5 7 66.2 2.1 3 12.6 11 3
Nitrobenzene 2,000 80 8 7 76.3 5.3 3 63.9 12 3
Hexachlorobutadiene 500 53 8 7 63.3 4.8 3 9.6 9 3
2,4-Dinitrotoluene 130 89 8 7 35.7 2.6 3 58.2 17 3
Hexachlorobenzene 130 84 21 7 92.3 1.6 3 71.7 9 3
(continued)

July 2014
TABLE 17
(continued)
Buffer 2 pH=4.937 Lab 1 Lab 2 Lab 3

Spike
Level
Analyte (µg/L)* %R RSD n %R RSD n %R RSD n
o-Cresol 200,000 97 13 7 37.8 4.5 3 6.1 24 3

m-Cresol** -- 83 4 7 -- -- -- 6.0 25 3
p-Cresol** -- -- -- -- -- -- -- -- -- --
Pentachlorophenol 100,000 109 11 7 41.9 28.2 3 36.6 32 3
1,4-Dichlorobenzene 7,500 50 5 7 79.7 1.0 3 26.5 68 3
Hexachloroethane 3,000 51 3 7 64.9 2.0 3 20.3 90 3
Nitrobenzene 2,000 80 4 7 79.0 2.3 3 59.4 6 3
Hexachlorobutadiene 500 57 5 7 60 3.3 3 16.6 107 3
2,4-Dinitrotoluene 130 86 6 7 38.5 5.2 3 62.2 6 3
Hexachlorobenzene 130 86 7 7 91.3 0.9 3 75.5 5 3
* 250-mL aliquots of leachate were spiked. Lab 1 spiked at one-half these levels.
** m-Cresol and p-Cresol co-elute. Lab 1 and Lab 3 reported o-Cresol and the sum of m- and p-
Cresol. Lab 2 reported the sum of all three isomers of Cresol.

July 2014
TABLE 18
SINGLE LABORATORY PAH ANALYSIS DATA FROM:

A REAL SOIL CONTAMINATED WITH CREOSOTE, USING METHOD 3546
(MICROWAVE EXTRACTION)
Compound Concentration (µg/kg) RSD (%) REAC values (µg/kg)

Naphthalene 2,170 12.4 710,000
2-Methylnaphthalene 28,710 3.1 N/R
1-Methylnaphthalene 33,180 2.4 N/R
Biphenyl 13,440 6.0 N/R
2,6-Dimethylnaphthalene 52,990 3.8 N/R
Acenaphthylene 16,320 3.1 21,000
Acenaphthene 801,210 6.0 1,700,000
Fluorene 789,980 3.4 990,000
Phenanthrene 1,627,480 0.7 3,300,00
Anthracene 346,010 4.0 360,000
Benzo(a)anthracene 300,380 2.7 310,000
Fluoranthene 1,331,690 1.6 1,600,000
Pyrene 1,037,710 3.0 1,100,000
Chrysene 293,200 3.4 320,000
Benzo(b)fluoranthene 152,000 3.8 140,000
Benzo(k)fluoranthene 127,740 3.6 130,000
Benzo(e)pyrene 87,610 3.9 N/R
Benzo(a)pyrene 128,330 3.9 110,000
Perylene 35,260 4.3 N/R
Indeno(1,2,3-cd)pyrene 63,900 5.0 25,000
Dibenz(a,h)anthracene 17,290 6.9 N/R
Benzo(g,h,i)perylene 42,270 6.9 20,000
n=4
Soil samples obtained from U.S. EPA Emergency Response Center archive bank through their
Response Engineering and Analytical Contract (REAC) laboratory (Edison, NJ). The standard
Soxhlet extraction procedures were performed by REAC three years earlier; this long storage
period is believed to account for the low naphthalene recovery data in the present study.
REAC data labeled N/R = not reported

July 2014
TABLE 19
SINGLE LABORATORY PAH RECOVERY DATA FROM:

HS-5 MARINE SEDIMENT MATERIALS, USING METHOD 3546
Compound Certified Confidence Recovery

Value Interval (%)
(µg/kg) (µg/kg)
Naphthalene 250 180 - 320 76

Acenaphthylene 150 * 107
Acenaphthene 230 130 - 330 61
Fluorene 400 300 - 500 63
Phenanthrene 5,200 4,200 - 6,200 72
Anthracene 380 230 - 530 84
Fluoranthene 8,400 5,800 - 10,000 81
Pyrene 5,800 4,000 - 7,600 69
Benzo(a)anthracene 2,900 1,700 - 4,100 53
Chrysene 2,800 1,900 - 3,700 76
Benzo(b)fluoranthene 2,000 1,000 - 3,000 84
Benzo(k)fluoranthene 1,000 600 - 1,400 137
Benzo(a)pyrene 1,700 900 - 2,500 52
Indeno(1,2,3-cd)pyrene 1,300 600 - 2,000 63
Dibenz(a,h)anthracene 200 100 - 300 125
Benzo(g,h,i)perylene 1,300 1000 - 1600 64
n=3
* values not certified
The uncertainties represent 90% confidence intervals.

July 2014
TABLE 20

Certified Confidence Recovery

Compound Value Interval (%)
(µg/kg) (µg/kg)
Naphthalene 150 * 54
Acenaphthylene 150 * 82
Acenaphthene 150 * 63
Fluorene 150 * 81
Phenanthrene 680 600 - 760 81
Anthracene 140 70 - 210 108
Fluoranthene 1250 1,150 - 1,350 84
Pyrene 940 820 - 1,060 85
Benzo(a)anthracene 530 470 - 580 78
Chrysene 650 570 - 730 84
Benzo(b)fluoranthene 700 550 - 850 84
Benzo(k)fluoranthene 360 310 - 410 156
Benzo(a)pyrene 650 570 - 730 73
Indeno(1,2,3-cd)pyrene 510 360 - 660 88
Dibenz(a,h)anthracene 120 70 - 170 117
Benzo(g,h,i)perylene 580 360 - 800 91
n=3

July 2014
TABLE 21

Certified Confidence Recovery

Compound Value Interval (%)
(µg/kg) (µg/kg)
Naphthalene 9,000 8300 - 9,700 61

Acenaphthylene 300 200 - 400 199
Acenaphthene 4,500 3,000 - 6,000 80
Fluorene 13,300 10,200 - 16,400 58
Phenanthrene 85,000 65000 - 105,000 87
Anthracene 13,400 12,900 - 13,900 47
Fluoranthene 60,000 51,000 - 69,000 91
Pyrene 39,000 30,000 - 48,000 86
Benzo(a)anthracene 14,600 12,600 - 16,600 78
Chrysene 14,100 12,100 - 16,100 91
Benzo(b)fluoranthene 7,700 6,500 - 8,900 101
Benzo(k)fluoranthene 2,800 800 - 4,800 275
Benzo(a)pyrene 7,400 3,000 - 7,000 74
Indeno(1,2,3-cd)pyrene 5,400 4,100 - 6,700 100
Dibenz(a,h)anthracene 1,300 800 - 1,800 118
Benzo(g,h,i)perylene 5,000 3,000 - 7,000 99
n=3

July 2014
TABLE 22

SRM 1941 MARINE SEDIMENT MATERIALS, USING METHOD 3546
Certified Value Recovery

Compound (µg/kg) (%)
Naphthalene 1010 97.4

Fluorene 100 100.0
Phenanthrene 490 102.0
Fluoranthene 980 116.7
Pyrene 810 97.3
Benzo(a)anthracene 430 89.8
Chrysene 380 130.3
Benzo(b)fluoranthene 740 95.8
Benzo(k)fluoranthene 360 130.2
Benzo(e)pyrene 550 81.0
Benzo(a)pyrene 630 76.0
Perylene 450 72.4
Indeno(1,2,3-cd)pyrene 500 126.0
Dibenz(a,h)anthracene 110 78.7
Benzo(g,h,i)perylene 530 85.2
n=3
All RSDs < 10%.

July 2014
FIGURE 1
TAILING FACTOR CALCULATION

July 2014
FIGURE 2
GAS CHROMATOGRAM OF BASE/NEUTRAL AND ACID CALIBRATION STANDARD

July 2014
Appendix A:
Summary of Revisions to Method 8270D (From Revision 4 Feb 2007)
1. Improved overall method formatting for consistency with new SW-846 methods style
guidance. The format was updated to Microsoft Word .docx.
2. Many minor editorial and technical revisions were made throughout to improve method
clarity.
3. The revision number was changed to 5 and the date published was changed to July
2014.
4. This appendix was added showing changes from the previous revision.
5. Chemical name was changed by the Integrated Risk Information System (IRIS) on
November 30, 2007 from Bis(2-chloroisopropyl)ether to Bis(2-chloro-1-methylethyl)ether
(common name). This compound is also known as 2,2’-oxybis(1-chloropropane) (CAS
index name). See the link at http://www.epa.gov/iris/subst/0407.htm, Section VII for the
“Revision History” and Section VIII, for “Synonyms” of this chemical.
6. Updated information on LLOQ and method blank evaluation was included based on
language found in Method 8000D.

July 2014

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METHOD 8270D

SEMIVOLATILE ORGANIC COMPOUNDS

SW-846 is not intended to be an analytical training manual. Therefore, method

1.0 SCOPE AND APPLICATION

1.1 This method is used to determine the concentration of semivolatile organic

Appropriate Preparation Techniquesb

KEY TO ANALYTE LIST

AW = Adsorption to walls of glassware during extraction and storage

1.4.1 Benzidine may be subject to oxidative losses during solvent concentration

1.4.3 Hexachlorocyclopentadiene is subject to thermal decomposition in the

1.4.4 N-Nitrosodimethylamine is difficult to separate from the solvent under the

1.4.5 N-Nitrosodiphenylamine decomposes in the gas chromatographic inlet

1.4.6 1,2-Diphenylhydrazine is unstable even at room temperature and readily

1.4.7 Pentachlorophenol, 2,4-dinitrophenol, 4-nitrophenol, benzoic acid, 4,6-

SW-846 Update V 8270D - 7 Revision 5

SW-846 Update V 8270D - 8 Revision 5

SW-846 Update V 8270D - 9 Revision 5

6.0 EQUIPMENT AND SUPPLIES

6.1 Gas chromatograph/mass spectrometer system

6.1.1 GC - An analytical system equipped with a temperature programmable

6.1.2 Column - 30 m x 0.25 mm ID (or 0.32 mm ID) 0.25, 0.5, or 1 µm film

6.1.3 Mass spectrometer

6.1.3.1 Capable of scanning from 35 to 500 amu every 1 sec or less,

6.1.3.2 An ion trap MS may be used if it is capable of axial modulation

SW-846 Update V 8270D - 10 Revision 5

6.1.6 Guard column (optional) - (J&W deactivated fused-silica, 0.25 mm ID x 6

6.4 Balance - Analytical, capable of weighing 0.0001 g

6.5 Bottles - Glass equipped with polytetrafluoroethylene (PTFE)-lined screw caps or

7.0 REAGENTS AND STANDARDS

7.3 Standard solutions

SW-846 Update V 8270D - 11 Revision 5

7.4.4 It is recommended that nitrosamine compounds be placed together in a

7.5 Internal standard solutions - The internal standards recommended are:

7.5.1 Dissolve 0.200 g of each compound with a small volume of carbon

7.5.2 If a more sensitive MS is employed to achieve lower quantitation levels, a

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

7.7 Calibration standards - A minimum of five calibration standards should be prepared

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

7.8 Surrogate standards - The recommended surrogates are: phenol-d6, 2-

7.8.1 Surrogate standard check - Determine what the appropriate concentration

7.8.2 If a more sensitive MS is employed to achieve lower quantitation levels, a

SW-846 Update V 8270D - 13 Revision 5

7.9.2 If a more sensitive MS is employed to achieve lower quantitation levels, a

7.10 Solvents - Acetone, hexane, methylene chloride, isooctane, carbon disulfide,

8.0 SAMPLE COLLECTION, PRESERVATION, AND STORAGE

8.1 See the introductory material to Chapter Four, "Organic Analytes."

9.0 QUALITY CONTROL

9.3 QC procedures necessary to evaluate the GC system operation are found in

SW-846 Update V 8270D - 14 Revision 5

9.4 Initial demonstration of proficiency (IDP)

Prior to implementation of a method, each laboratory must perform an IDP consisting of at

9.4.1 Demonstration of proficiency for new analysts - Each laboratory should

SW-846 Update V 8270D - 15 Revision 5

9.6.5 Blanks are generally considered to be acceptable if target analyte

9.6.6 If an analyte of interest is found in a sample in the batch near a

SW-846 Update V 8270D - 16 Revision 5

9.7 Surrogate recoveries

9.8 The experience of the analyst performing gas chromatography/mass spectrometry

9.10 Lower Limit of Quantitation (LLOQ)