METHOD 8270D

SEMIVOLATILE ORGANIC COMPOUNDS

BY GAS CHROMATOGRAPHY/MASS SPECTROMETRY (GC/MS)

1.0 SCOPE AND APPLICATION

1.1 Method 8270 is used to determine the concentration of semivolatile organic compounds

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

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

can be determined by this method:

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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(43) NO NO NO X

Aroclor 1016 12674-11-2 X X X X X

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

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

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

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

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

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

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

Barban 101-27-9 LR NO NO NO LR

Benzidine 92-87-5 CP CP CP CP CP

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

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

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

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Compounds CAS No" 3510 3520 3541 3550 3580

Benzo(k)fluoranthene 207-08-9 X X X X X

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

Benzo(a)pyrene 50-32-8 X v X v V A. A. A.

p-Benzoquinone 106-51-4 OE NO NO NO X

Benzyl alcohol 100-51-6 X X NO X X

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

~-BHC 319-85-7 X X X X X

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

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

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

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

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

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

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

Bromoxynil 1689-84-5 X NO NO NO X

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

Captafol 2425-06-1 . HS(55) NO NO NO X

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

Carbaryl 63-25-2 X NO NO NO X

Carbofuran 1563-66-2 X NO NO NO X

Carbophenothion 786-19-6 X NO NO NO X

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

Chlorfenvinphos 470-90-6 X NO NO NO X

4-Chloroaniline 106-47-8 X ND NO NO X

Chlorobenzilate 510-15-6 X NO NO NO X

5-Chloro-2-methylaniline 95-79-4 X NO ND NO X

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

3-(Chloromethyl)pyridine 6959-48-4 X NO NO NO X

hydrochloride

1-Chloronaphthalene 90-13-1 X X X X X

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

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

4-Chloro-1.2-ohenvlenediamine - - - -- - - -, l J 95-83-0 X X NO NO NO

4-Chloro-1,3-phenylenediamine 5131-60-2 X X NO NO NO

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

Chrysene 218-01-9 X X X X X

Coumaphos 56-72-4 X NO NO NO X

p-Cresidine 120-71-8 X NO NO NO X

Crotoxyphos 7700-17-6 X NO NO NO X

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Compounds CAS Noa 3510 3520 3541 3550 3580

2-Cyclohexyl-4,6-dinitro-phenol 131-89-5 X ND ND ND LR

4,4'-DDD 72-54-8 X X X X X

4,4'-DDE 72-55-9 X X X X X

4,4'-DDT 50-29-3 X X X X X

Demeton-O 298-03-3 HS(68) ND ND ND X

Demeton-S 126-75-0 X ND ND ND X

Diallate (cis or trans) 2303-16-4 X ND ND ND X

2,4-Diaminotoluene 95-80-7 DC,OE(42) ND ND ND X

Dibenz(a,j)acridine 224-42-0 X ND ND ND X

Dibenz(a, h)anthracene 53-70-3 X X X X X

Dibenzofuran 132-64-9 X X ND X X

Dibenzo(a,e)pyrene 192-65-4 ND ND ND ND X

1,2-Dibromo-3-chloropropane 96-12-8 X X ND ND ND

Di-n-butyl phthalate 84-74-2 X X X X X

Dichlone 117-80-6 OE ND ND ND X

1,2-Dichlorobenzene 95-50-1 X X X X X

1,3-Dichlorobenzene 541-73-1 X X X X X

1,4-Dichlorobenzene 106-46-7 X X X X X

3,3'-Dichlorobenzidine 91-94-1 X X X X X

2,4-Dichlorophenol 120-83-2 X X X X X

2,6-Dichlorophenol 87-65-0 X ND ND ND X

Dichlorovos 62-73-7 X ND ND ND X

Dicrotophos 141-66-2 X ND ND ND X

Dieldrin 60-57-1 X X X X X

Diethyl phthalate 84-66-2 X X X X X

Diethylstilbestrol 56-53-1 AW,OS(67) ND ND ND X

Diethyl sulfate 64-67-5 LR ND ND ND LR

Dimethoate 60-51-5 HE,HS(31) ND ND ND X

3,3'-Dimethoxybenzidine 119-90-4 X ND ND ND LR

Dimethylaminoazobenzene 60-11-7 X ND ND ND X

7,12-Dimethylbenz(a)-anthracene 57-97-6 CP(45) ND ND ND CP

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

a,a-Dimethylphenethylamine 122-09-8 ND ND ND ND X

2,4-Dimethylphenol 105-67-9 X X X X X

Dimethyl phthalate 131-11-3 X X X X X

1,2-Dinitrobenzene 528-29-0 X ND ND ND X

1,3-Dinitrobenzene 99-65-0 X ND ND ND X

1,4-Dinitrobenzene 100-25-4 HE(14) ND ND ND X

4,6-Dinitro-2-methylphenol 534-52-1 X X X X X

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Compounds CAS No8 3510 3520 3541 3550 3580

2,4-Dinitrophenol 51-28-5 X X X X X

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

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

Dinocap 39300-45-3 CP,HS(28) ND ND ND CP

Dinoseb 88-85-7 X ND ND ND X

Diphenylamine 122-39-4 X X X X X

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

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

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

Disulfoton 298-04-4 X ND ND ND X

Endosulfan I 959-98-8 X X X X X

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

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

Endrin 72-20-8 X X X X X

Endrinaldehyde 7421-93-4 X X X X X

Endrin ketone 53494-70-5 X X ND X X

EPN 2104-64-5 X ND ND ND X

Ethion 563-12-2 X ND ND ND X

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

Ethyl methanesulfonate 62-50-0 X ND ND ND X

Famphur 52-85-7 X ND ND ND X

Fensulfothion 115-90-2 X ND NO ND X

Fenthion 55-38-9 X ND ND ND X

Fluchloralin 33245-39-5 X ND ND ND X

Fluoranthene 206-44-0 X X X X X

Fluorene 86-73-7 X X X X X

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

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

Heptachlor 76-44-8 X X X X X

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

Hexachtorocyclopentadiene 77-47-4 X X X X X

Hexachloroethane 67-72-1 X X X X X

Hexachlorophene 70-30-4 AW,CP(62) ND ND ND CP

Hexachloropropene 1888-71-7 X ND ND ND X

Hexamethylphosphoramide 680-31-9 X ND NO ND X

Hydroquinone 123-31-9 ND NO NO ND X

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

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Compounds CAS No" 3510 3520 3541 3550 3580

Isodrin 465-73-6 X NO ND ND X

Isophorone 78-59-1 X X X X X

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

Kepone 143-50-0 X NO ND NO X

Leptophos 21609-90-5 X NO ND NO X

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

Maleic anhydride 108-31-6 HE ND ND ND X

Mestranol 72-33-3 X ND ND ND X

Methapyrilene 91-80-5 X ND ND ND X

Methoxychlor 72-43-5 X NO ND NO X

3-Methylcholanthrene 56-49-5 X NO . ND NO X

4A'-Methylenebis (2-chloroaniline) 101-14-4 OE,OS(O) ND ND ND LR

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

aniline)

Methyl methanesulfonate 66-27-3 X NO ND ND X

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

Methyl parathion 298-00-0 X NO ND ND X

2-Methylphenol 95-48-7 X ND ND NO X

3-Methylphenol 108-39-4 X NO ND ND X

4-Methylphenol 106-44-5 X NO ND ND X

Mevinphos 7786-34-7 X ND ND ND X

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

Mirex 2385-85-5 X NO ND NO X

Monocrotophos 6923-22-4 HE NO ND NO X

Naled 300-76-5 X NO ND ND X

Naphthalene 91-20-3 X X X X X

1A-Naphthoquinone 130-15-4 X NO ND ND X

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

2-Naphthylamine 91-59-8 X NO ND NO X

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

5-Nitroacenaphthene 602-87-9 X NO ND ND X

2-Nitroaniline 88-74-4 X X ND X X

3-Nitroaniline 99-09-2 X X ND X X

4-Nitroaniline 100-01-6 X X ND X X

5-Nitro-o-anisidine 99-59-2 X NO ND ND X

Nitrobenzene 98-95-3 X X X X X

4-Nitrobiphenyl 92-93-3 X ND ND NO X

Nitrofen 1836-75-5 X ND ND ND X

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

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Compounds CAS No" 3510 3520 3541 3550 3580

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

5-Nitro-o-toluidine 99-55-8 X X NO NO X

Nitroquinoline-1-oxide 56-57-5 X NO ND ND v

A.

N-Nitrosodi-n-butylamine 924-16-3 X NO NO NO X

N-Nitrosodiethylamine 55-18-5 X NO NO NO X

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

N-Nitrosomethylethylamine 10595-95-6 X NO NO NO X

N-Nitrosodiphenylamine 86-30-6 X X X X X

N-Nitrosodi-n-propylamine 621-64-7 X X X X X

N-Nitrosomorpholine 59-89-2 NO ND NO NO X

N-Nitrosopiperidine 100-75-4 X NO NO NO X

N-Nitrosopyrrolidine 930-55-2 X NO NO NO X

Octamethyl pyrophosphoramide 152-16-9 LR NO NO NO LR

4,4'-Oxydianiline 101-80-4 X NO NO NO X

Parathion 56-38-2 X X NO NO X

Pentachlorobenzene 608-93-5 X NO NO NO X

Pentachloronitrobenzene 82-68-8 X NO NO NO X

Pentachlorophenol 87-86-5 X X X X X

Phenacetin 62-44-2 X NO NO NO X

Phenanthrene 85-01-8 X X X X X

Phenobarbital 50-06-6 X NO NO NO X

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

1,4-Phenylenediamine 106-50-3 X NO NO NO X

Phorate 298-02-2 X NO NO NO X

Phosalone 2310-17-0 HS(65) NO NO NO X

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

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

Phthalic anhydride 85-44-9 CP,HE(1) NO NO NO CP

2-Picoline (2-Methylpyridine) 109-06-8 X X NO NO NO

Piperonyl sulfoxide 120-62-7 X NO NO NO X

Pronamide 23950-58-5 X NO NO NO X

Propylthiouracil 51-52-5 LR NO NO NO LR

.I

D\1r'on.o. ..1 I vi t"'" 129-00-0 X X X X X

Resorcinol 108-46-3 OC,OE(10) NO NO NO X

Safrole 94-59-7 X NO NO NO, X

Strychnine 57-24-9 AW,OS(55) NO NO NO X

Sulfallate 95-06-7 X NO NO NO X

Terbufos 13071-79-9 X NO NO NO X

1,2,4,5-Tetrachlorobenzene 95-94-3 X NO NO NO X

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Compounds CAS Noa 3510 3520 3541 3550 3580

2,3,4,6-Tetrachlorophenol 58-90-2 X NO NO NO X

Tetrachlorvinphos 961-11-5 X NO NO NO X

Tetraethyl dithiopyrophosphate 3689-24-5 X X NO NO NO

Tetraethyl pyrophosphate 107-49-3 X NO NO NO X

Thionazine 297-97-2 X NO NO NO X

Thiophenol (Benzenethiol) 108-98-5 X NO NO NO X

Toluene diisocyanate 584-84-9 HE(6) NO NO NO X

o-Toluidine 95-53-4 X NO NO NO X

Toxaphene 8001-35-2 X X X X X

1,2,4-Trichlorobenzene 120-82-1 X X X X X

2,4,5-Trichlorophenol 95-95-4 X X NO X X

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

Trifluralin 1582-09-8 X NO NO NO X

2,4,5-Trimethylaniline 137-17-7 X NO NO NO X

Trimethyl phosphate 512-56-1 HE(60) NO NO NO X

1,3,5-Trinitrobenzene 99-35-4 X NO NO NO X

Tris(2,3-dibromopropyl) phosphate 126-72-7 X NO NO NO LR

Tri-p-tolyl phosphate 78-32-0 X NO NO NO X

O,O,O-Triethyl phosphorothioate 126-68-1 X NO NO NO X

a Chemical Abstract Service Registry Number

b See Sec. 1.2 for other acceptable preparation methods.

KEY TO ANALYTE LIST

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

CP = Nonreproducible chromatographic performance.

OC Unfavorable distribution coefficient (number in parenthesis is percent recovery).

HE = Hydrolysis during extraction accelerated by acidic or basic conditions (number in

parenthesis is percent recovery).

HS = Hydrolysis during storage (number in parenthesis is percent stability).

LR = Low response.

NO = Not determined.

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

percent recovery).

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

X = Greater than 70 percent recovery by this technique.

1.2 In addition to the sample preparation methods listed in the above analyte list, Method

3535 describes a solid-phase extraction procedure that may be applied to the extraction of

semivolatiles from TCLP leachates (Tables 16 and 17 contain performance data). Method 3542

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describes sample preparation for semivolatile organic compounds in air sampled by Method 0010

(Table 11 contains surrogate performance data), Method 3545 describes an automated solvent

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

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

15 for performance data).

1.3 Method 8270 can be used to quantitate most neutral, acidic, and basic organic

compounds that are soluble in methylene chloride and capable of being eluted, without

derivatization, as sharp peaks from a gas chromatographic fused-silica capillary column coated with

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

hydrocarbonsand pesticides, phthalate esters, organophosphate esters, nitrosamines, haloethers,

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

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

been evaluated.

In most cases, Method 8270 is not appropriatefor 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 Sec. 7.0 of Methods 8081 and 8082 for guidance on calibration and quantitation of

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

1.4

method:

The following compounds may require specialtreatment when being determined by this

1.4.1 Benzidine may be subject to oxidativelosses during solvent concentration and

its chromatographic behavior is poor.

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

a-BHC, V-BHC, Endosulfan I and II, and Endrin are subject to decomposition. Neutral

extraction should be performed if these compounds are expected.

1.4.3 Hexachlorocyclopentadiene is subject to thermal decomposition in the inlet

of the gas chromatograph, chemical reaction in acetone solution, and photochemical

decomposition.

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

chromatographic conditions described.

1.4.5 N-nitrosodiphenylamine decomposes in the gas chromatographic inlet and

cannot be separated from diphenylamine.

1.4.6 Pentachlorophenol, 2,4-dinitrophenol, 4-nitrophenol, benzoic acid,

4,6-dinitro-2-methylphenol, 4-chloro-3'-methylphenol, 2-nitroaniline, 3-nitroaniline,

4-chloroaniline, and benzyl alcohol are subject to erratic chromatographic behavior, especially

if the GC system is contaminated with high boiling material.

1.4.7 Pyridine may perform poorly at the GC injection port temperatures listed in the

method. Lowering the injection port temperature may reduce the amount of degradation.

However, the analyst must use caution in modifying the injection port temperature, as the

performance of other analytes may be adversely affected. Therefore, if pyridine is to be

determined in addition to other target analytes, it maybe necessary to perform separate

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analyses. In addition, pyridine may be lost during the evaporative concentration of the sample

extract. As a result, many of the extraction methods listed above may yield low recoveries

unless great care is exercised during the concentration steps. For this reason, analysts may

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

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

or eliminating the need for evaporative concentration techniques for many applications.

1.4.8 Toluene diisocyanate rapidly hydrolyses in water (half-life of less then 30

min.). Therefore, recoveries of this compound from aqueous matrices should not be expected.

In addition, in solid matrices, toluene diisocyanate often reacts with alcohols and amines to

produce urethane and ureas and consequently cannot usually coexist in a solution containing

these materials.

1.4.9 In addition, analytes in the list provided above are flagged when there are

limitations caused by sample preparation and/or chromatographic problems.

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

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

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

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

saturation of the detector.

1.6 This method is restricted to use by or under the supervision of analysts experienced

in the use of gas chromatograph/mass spectrometers and skilled in the interpretation of mass

spectra. Each analyst must demonstrate the ability to generate acceptable results with this method.

2.0 SUMMARY OF METHOD

2.1 The samples are prepared for analysis by gas chromatography/mass spectrometry

(GC/MS) using the appropriate sample preparation (refer to Method 3500) and, if necessary, sample

cleanup procedures (refer to Method 3600).

2.2 The semivolatile compounds are introduced into the GC/MS by injecting the sample

extract into a gas chromatograph (GC) with a narrow-bore fused-silica capillary column. The GC

column is temperature-programmed to separate the analytes, which are then detected with a mass

spectrometer (MS) connected to the gas chromatograph.

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

via a jet separator or a direct connection. Identification of target analytes is accomplished by

comparing their mass spectra with the electron impact (or electron impact-like) spectra of authentic

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

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

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

general requirements provided in Method 8000.

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3.0 INTERFERENCES

3.1 Raw GC/MS data from all blanks, samples, and spikes must be evaluated for

interferences. Determine if the source of interference is in the preparation and/or cleanup of the

samples and take corrective action to eliminate the problem.

3.2 Contamination by carryover can occur whenever high-concentration and

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

be rinsed with solventbetween sample injections. Whenever an unusually concentrated sample is

encountered, it should be followed by the analysis of solvent to check for cross-contamination.

4.0 APPARATUS AND MATERIALS

4.1 Gas chromatograph/mass spectrometer system

4.1.1 Gas chromatograph - An analytical system complete with a

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

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

be directly coupled to the source.

4.1.2 Column - 30-m x 0.25-mm ID (or 0.32-mm ID) t-urn film thickness

silicone-coated fused-silica capillary column (J&W Scientific D8-5 or equivalent).

4.1.3 Mass spectrometer

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

using 70 volts (nominal) electron energy in the electron impact ionization mode. The

mass spectrometer must be capable of producing a mass spectrum for

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

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

4.1.3.2 An ion trap mass spectrometermay be used if it is capable of axial

modulation to reduce ion-molecule reactions and can produce electron impact-like

spectra that match those in the EPAINIST Library. The mass spectrometer must be

capableof producing a mass spectrum for DFTPP which meets the criteria in Table 3

when 5 or 50 ng are introduced.

4.1.4 GCIMS interface- Any GC-to-MS interfacemay be used that gives acceptable

calibration pointsat 50 ng per injectionfor each compound of interest and achieves acceptable

tuning performance criteria. For a narrow-bore capillary column, the interface is usually

capillary-direct into the mass spectrometer source.

4.1.5 Data system - A computer system should be interfaced to the mass

spectrometer. The system must allow the continuous acquisition and storage on

machine-readable media of all mass spectra obtained throughout the duration of the

chromatographic program. The computer should have software that can search any GC/MS

data file for ions of a specific mass and that can plot such ion abundances versus time or scan

number. This type of plot is defined as an Extracted Ion Current Profile (EICP). Software

should also be availablethat allows integratingthe abundances in any EICP between specified

time or scan-number limits. The most recent version of the EPAINIST Mass Spectral Library

should also be available.

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4.1.6 Guard column (optional)- (J&W deactivated fused-silica, 0.25-mm 10 x 6-m,

or equivalent) between the injection port and the analytical column joined with column joiners

(Hewlett-Packard Catalog No. 5062-3556, or equivalent).

4.2 Syringe - 10-1JL.

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

4.4 Balance - Analytical, capable of weighing 0.0001 g.

4.5 Bottles - glass with polytetrafluoroethylene (PTFE)-lined screw caps or crimp tops.

5.0 REAGENTS

5.1 Reagent grade inorganic chemicals shall be used in all tests. Unless otherwise

indicated, it is intended that all reagents shall conform to the specifications of the Committee on

Analytical Reagents of the American Chemical Society, where such specifications are available.

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

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

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

reagent water, as defined in Chapter One.

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

standard materials or purchased as certified solutions.

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

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

dilute to volume in a 1O-mL volumetric flask. Larger volumes can be used at the convenience

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

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

manufacturer or by an independent source.

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

Store, protected from light, at -10 0

C or less or as recommended by the standard manufacturer.

Stock standard solutions should be checked frequently for signs of degradation or evaporation,

especially just prior to preparing calibration standards from them.

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

comparison with quality control check samples indicates a problem.

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

separate calibration mix and not combined with other calibration mixes. When using a

premixed certified standard, consult the manufacturer's instructions for additional guidance.

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

analytical difficulties. When using a premixed certified standard, consult the manufacturer's

instructions for additional guidance.

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5.4 Internal standard solutions - The internal standards recommended are 1,4-dichlorobenzene-d; naphthalene-d 8' acenaphthene-d 10' phenanthrene-d 10' chrysene-d 12' and perylene-d.,

(see Table 5). Other compounds may be used as internal standards as long as the specifications

in Sec. 7.3.2 are met.

5.4.1 Dissolve 0.200 g of each compound with a small volume of carbon disulfide.

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

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

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

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

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

resulting in a concentration of 40 ng/lll ofeach internal standard. Store at -1O°C or less when

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

documented holding time and storage temperature recommendations.

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

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

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

calibration analysis.

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

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

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

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

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

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

documented holding time and storage temperature recommendations.

5.6 Calibration standards - A minimum of five calibration standards should be prepared at

five different concentrations. At least one of the calibration standards should correspond to a sample

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

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

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

analyte for detection by this method.

5.6.1 It is the intent of EPA that all target analytes for a particular analysis be

included in the calibration standard(s). These target analytes may not include the entire list

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

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

standard(s).

5.6.2 Each 1-ml aliquot of calibration standard should be spiked with 10 III of the

internal. standard solution prior to analysis. All standards should be stored at -1O°C or less,

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

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

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

time and storage temperature recommendations.

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

2,4,6-tribromophenol, nitrobenzene-d., 2-f1uorobiphenyl, and p-terphenyl-d.; See Method 3500 for

instructions on preparing the surrogate solutions.

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5.7.1 Surrogate standard check - Determine what the appropriate concentration

should be for the blank extracts after all extraction, cleanup, and concentration steps. Inject

this concentration into the GC/MS to determine recovery of surrogate standards. It is

recommended that this check be done whenever a new surrogate spiking solution is prepared.

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

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

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

levels, a more dilute surrogate solution may be necessary.

5.8 Matrix spike and laboratory control standards - See Method 3500 for instructions on

preparing the matrix spike standard. The same standard may be used as the laboratory control

standard (LCS).

5.8.1 Matrix spike check - Determine what concentration should be in the blank

extracts after all extraction, cleanup, and concentration steps. Inject this concentration into the

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

matrix spiking solution is prepared.

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

levels, a more dilute matrix and LCS spiking solution may be necessary.

5.8.3 Some projects may require the spiking of the specific compounds of interest,

since the spiking compounds listed in Method 3500 would not be representative of the

compounds of interest required for the project. When this occurs, the matrix and LCS spiking

standards should be prepared in methanol, with each compound present at a concentration

appropriate for the project.

5.9 Solvents - Acetone, hexane, methylene chloride, isooctane, carbon disulfide, toluene,

and other appropriate solvents. All solvents should be pesticide quality or equivalent.

6.0 SAMPLE COLLECTION, PRESERVATION, AND HANDLING

6.1 See the introductory material to this chapter, Organic Analytes, Sec. 4.1.

6.2 Store the sample extracts at -10°C, protected from light, in sealed vials (e.g., screw-cap

vials or crimp-capped vials) equipped with unpierced PTFE-lined septa.

7.0 PROCEDURE

7.1 Sample preparation

7.1.1 Samples are normally prepared by one of the following methods prior to

GC/MS analysis.

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Matrix

Air (particulates and sorbent resin)

Water (including TCLP leachates)

Soil/sediment

Waste

Methods

3542

3510,3520,3535

3540,3541,3545,3550,3560,3561

3540,3541,3545,3550,3560,3561,3580

7.1.2 In very limited applications, direct injection of the sample into the GC/MS

system with a 10-IJL syringe may be appropriate. The detection limit is very high

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

of 10,000 IJg/L are expected.

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

GC/MS analysis.

Analytes of interest

Aniline & aniline derivatives

Phenols

Phthalate esters

Nitrosamines

Organochlorine pesticides &·PCBs

Nitroaromatics and cyclic ketones

Polynuclear aromatic hydrocarbons

Haloethers

Chlorinated hydrocarbons

Organophosphorus pesticides

Petroleum waste

All base, neutral, and acid

priority pollutants

Methods

3620

3630,3640,8041 a

3610,3620,3640

3610,3620,3640

3610,3620,3630,3660,3665

3620, 3640

3611,3630,3640

3620,3640

3620, 3640

3620

3611,3650

3640

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

are encountered on GC/FID.

7.3 Initial calibration

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

Mass range:

Scan time:

Initial temperature:

Temperature program:

Final temperature:

Injector temperature:

Transfer line temperature:

Source temperature:

Injector:

Injection volume:

Carrier gas:

Ion trap only:

35-500 amu

1 sec/scan

40°C, hold for 4 minutes

40-270°C at 10°C/min

270°C, hold until benzo[g,h,i]perylene elutes

250-300°C

250-300°C

According to manufacturer's specifications

Grob-type, splitless

1-2 IJL

Hydrogen at 50 em/sec or helium at 30 em/sec

Set axial modulation, manifold temperature, and emission

current to manufacturer's recommendations

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

7.3.1 The GC/MS system must be hardware-tuned using a 50-ng injection of

DFTPP. Analyses must not begin until the tuning criteria are met.

7.3.1.1 In the absence of specific recommendations on how to acquire the

mass spectrum of DFTPP from the instrument manufacturer, the following approach

has been shown to be useful: Three scans (the peak apex scan and the scans

immediately preceding and following the apex) are acquired and averaged.

Background subtraction is required, and must be accomplished using a single scan

acquired no more than 20 scans prior to the elution of DFTPP. The background

subtraction should be designed only to eliminate column bleed or instrument

background ions. Do not subtract part of the DFTPP peak.

7.3.1.2 Use the DFTPP mass intensity criteria in Table 3 as tuning

acceptance criteria. Alternatively, other documented tuning criteria may be used (e.g.

CLP, Method 525, or manufacturer's instructions), provided that method performance

is not adversely affected.

NOTE: All subsequent standards, samples, MS/MSDs, and blanks associated with

a DFTPP analysis must use the identical mass spectrometer instrument

conditions.

7.3.1.3 The GC/MS tuning standard solution should also be used to

assess GC column performance and injection port inertness. Degradation of DDT to

DOE and DOD should not exceed 20%. (See Sec. 8.0 of Method 8081 for the percent

breakdown calculation). Benzidine and pentachlorophenol should be present at their

normal responses, and no peak tailing should be visible.

7.3.1.4 If degradation is excessive and/or poor chromatography is noted,

the injection port may require cleaning. It may also be necessary to break off the first

6-12 in. of the capillary column. The use of a guard column (Sec. 4.1.6) between the

injection port and the analytical column may help prolong analytical column

performance.

7.3.2 The internal standards selected in Sec. 5.4 should permit most of the

components of interest in a chromatogram to have retention times of 0.80-1.20 relative to one

of the internal standards. Use the base peak ion from the specific internal standard as the

primary ion for quantitation (see Table 1). If interferences are noted, use the next most intense

ion as the quantitation ion (i.e. for 1,4-dichlorobenzene-d4 , use 152 m/z for quantitation).

7.3.3 Analyze 1-2 IJL of each calibration standard (containing internal standards)

and tabulate the area of the primary characteristic ion against concentration for each target

analyte (as indicated in Table 1). A set of at least five calibration standards is necessary (see

Sec. 5.6 and Method 8000). The injection volume must be the same for all standards and

sample extracts. Figure 1 shows a chromatogram of a calibration standard containing

base/neutral and acid analytes.

Calculate response factors (RFs) for each target analyte relative to one of the internal

standards as follows:

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RF

where:

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

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

C, = Concentration of the analyte or surrogate, in Ilg/L.

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

7.3.4 System performance check compounds (SPCCs)

7.3.4.1 A system performance check must be performed to ensure that

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

the System performance check compounds (SPCCs) are: N-nitroso-di-n-propylamine;

hexachlorocyclopentadiene; 2,4-dinitrophenol; and 4-nitrophenol.

7.3.4.2 The minimum acceptable average RF for these compounds is

0.050. These SPCCs typically have very low RFs (0.1-0.2) and tend to decrease in

response as the chromatographic system begins to deteriorate or the standard material

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

they must meet the minimum requirement when the system is calibrated.

7.3.4.3 If the minimum response factors are not met, the system must be

evaluated, and corrective action must be taken before sample analysis begins.

Possible problems include standard mixture degradation, injection port inlet

contamination, contamination at the front end of the analytical column, and active sites

in the column or chromatographic system. This check must be met before sample

analysis begins.

7.3.5 Calibration check compounds (GCGs)

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

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

indicative of system leaks or reactive sites on the column. Meeting the GGG criteria

is not a substitute for successful calibration of the target analytes using one of the

approaches described in Sec. 7.0 of Method 8000.

7.3.5.2 Calculate the mean response factor and the relative standard

deviation (RSD) of the response factors for each target analyte. The RSD should be

less than or equal to 15% for each target analyte. However, the RSD for each

individual GGC (see Table 4) must be less than or equal to 30%.

n n-1

n

L(RFi-RF)2

i=1 SD

n

LRFj

i=1 mean RF = RF = --

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RSD =_

so x

RF

100

7.3.5.3 If the RSD of any CCC is greater than 30%, then the

chromatographic system is too reactive for analysis to begin. Clean or replace the

injector liner and/or capillary column, then repeat the calibration procedure beginning

with Sec. 7.3.

7.3.5.4 If the CCCs are not included in the list of analytes for a project,

and therefore not included in the calibration standards, then refer to Sec. 7.0 of Method

8000.

7.3.6 Evaluation of retention times - The relative retention time (RRT) of each target

analyte in each calibration standard should agree within 0.06 RRT units. Late-eluting target

analytes usually have much better agreement.

Retention time of the analyte

Retention time of the internal standard

RRT = --------------''----

7.3.7 Linearity of target analytes -If the RSD of any target analytes is 15% or less,

then the relative response factor is assumed to be constant over the calibration range, and the

average relative response factor may be used for quantitation (Sec. 7.6.2).

7.3.7.1 If the RSD of any target analyte is greater than 15%, refer to Sec.

7.0 in Method 8000 for additional calibration options. One of the options must be

applied to GC/MS calibration in this situation, or a new initial calibration must be

performed.

NOTE: Method 8000 designates a linearity criterion of 20% RSD. That criterion

pertains to GC and HPLC methods other than GC/MS. Method 8270 requires

15% RSD as evidence of sufficient linearity to employ an average response

factor.

7.3.7.2 When the RSD exceeds 15%, the plotting and visual inspection

of a calibration curve can be a useful diagnostic tool. The inspection may indicate

analytical problems, including errors in standard preparation, the presence of active

sites in the chromatographic system, analytes that exhibit poor chromatographic

behavior, etc.

7.4 GC/MS calibration verification - Calibration verification consists of three steps that are

performed at the beginning of each 12-hour analytical shift.

7.4.1 Prior to the analysis of samples or calibration standards, inject 50 ng of the

DFTPP standard into the GC/MS system. The resultant mass spectrum for DFTPP must meet

the criteria given in Table 3 before sample analysis begins. These criteria must be

demonstrated each 12-hour shift during which samples are analyzed.

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7.4.2 The initial calibration (Sec. 7.3) for each compound of interest should be

verified once every 12 hours prior to sample analysis, using the introduction technique and

conditions used for samples. This is accomplished by analyzing a calibration standard at a

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

results from the calibration standard analysis should meet the verification acceptance criteria

provided in Secs. 7.4.4 through 7.4.7.

NOTE: The DFTPP and calibration verification standard may be combined into a single

standard as long as both tuning and calibration verification acceptance criteria for the

project can be met without interferences.

7.4.3 A method blank should be analyzed either after the calibration

standard, or at any other time during the analytical shift, to ensure that the total system

(introduction device, transfer lines and GC/MS system) is free of contaminants. If the method

blank indicates contamination, then it may be appropriate to analyze a solvent blank to

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

See Sec. 8.0 of Method 80008 for method blank performance criteria.

7.4.4 System performance check compounds (SPCCs)

7.4.4.1 A system performancecheck must be made during every 12-hour

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

minimum response factor of0.050. This is the same check that is applied during the

initial calibration.

7.4.4.2 If the minimum responsefactors are not met, the system must be

evaluated, and corrective action must be taken before sample analysis begins.

Possible problems include standard mixture degradation, injection port inlet

contamination, contamination at the front end of the analytical column, and active sites

in the column or chromatographic system. This check must be met before sample

analysis begins.

7.4.5 Calibration check compounds (eees)

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

Table 4 are used to check the validity ofthe initial calibration. Use percent difference

when performing the average response factor model calibration. Use percent drift

when calibrating using a regression fit model. Refer to Sec. 7.0 of Method 8000 for

guidance on calculating percent difference and drift.

7.4.5.2 If the percent difference for each eee is less than or equal to

20%, then the initial calibration is assumed to be valid. If the criterion is not met (i.e.,

greater than 20% difference or drift) for anyone eee, then corrective action must be

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

ana!ytes for a project, and therefore not included in the calibration standards, then all

analytes must meet the 20% difference or drift criterion.

7.4.5.3 Problems similar to those listed under specs could affect the

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

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

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7.4.6 Internal standard retention time - The retention times of the internal standards

in the calibration verification standard must be evaluated immediately after or during data

acquisition. If the retention time for any internal standard changes by more than 30 seconds

from that in the mid-point standard level of the most recent initial calibration sequence, then

the chromatographic system must be inspected for malfunctions and corrections must be

made, as required. When corrections are made, reanalysis of samples analyzed while the

system was malfunctioning is required.

7.4.7 Internal standard response -If the EICP area for any of the internal standards

in the calibration verification standard changes by a factor of two (-50% to +100%) from that

in the mid-point standard level of the most recent initial calibration sequence, the mass

spectrometer must be inspected for malfunctions and corrections must be made, as

appropriate. When corrections are made, reanalysis of samples analyzed while the system

was malfunctioning is required.

7.5 GC/MS analysis of samples

7.5.1 It is highly recommended that sample extracts be screened on a GC/FID or

GC/PID using the same type of capillary column used in the GC/MS system. This will minimize

contamination of the GC/MS system from unexpectedly high concentrations of organic

compounds.

7.5.2 Allow the sample extract to warm to room temperature. Just prior to analysis,

add 10 IJL of the internal standard solution to the 1-mL concentrated sample extract obtained

from sample preparation.

7.5.3 Inject a 1-2 IJL aliquot of the sample extract into the GC/MS system, using the

same operating conditions that were used for the calibration (Sec. 7.3). The volume to be

injected should contain 100 ng of base/neutral and 200 ng of acid surrogates (assuming 100%

recovery), unless a more sensitive GC/MS system is being used and the surrogate solution is

less concentrated then that listed in Sec. 5.7. The injection volume must be the same volume

used for the calibration standards.

7.5.4 If the response for any quantitation ion exceeds the initial calibration range

of the GC/MS system, the sample extract must be diluted and reanalyzed. Additional internal

standard solution must be added to the diluted extract to maintain the same concentration as

in the calibration standards (40 ng/lJL, unless a more sensitive GC/MS system is being used).

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

primary ion.

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

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

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

for system inspection and/or maintenance.

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

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

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

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

demonstrated to be free of interferences.

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7.5.4.2 All dilutions should keep the response ofthe major constituents

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

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

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

However,SIM may provide a lesser degree of confidence in the compound identification unless

multiple ions are monitored for each compound.

7.6 Qualitative analysis

7.6.1 The qualitative identification of compounds determined by this method is

based on retention time and on comparison of the sample mass spectrum, after background

correction, with characteristic ions in a reference mass spectrum. The reference mass

spectrum must be generated by the laboratory using the conditions of this method. The

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

relative intensity, or any ions over 30% relative intensity, if tessthan three such ions occur in

the reference spectrum. Compounds are identified when the following criteria are met.

7.6.1.1 The intensities of the characteristic ions of a compound must

maximize in the same scan or within one scan of each other. Selection of a peak by

a data system target compound search routine where the search is based on the

presence of a target chromatographic peak containing ions specific for the target

compound at a compound-specific retention time will be accepted as meeting this

criterion.

7.6.1.2 The RRT of the sample component is within ± 0.06 RRT units of

the RRT of the standard component.

7.6.1.3 The relative intensities of the characteristic ions agree within 30%

of the relative intensities of these ions in the reference spectrum. (Example: For an

ion with an abundance of 50% in the reference spectrum, the corresponding

abundance in a sample spectrum can range between 20% and 80%.)

7.6.1.4 Structuralisomers that produce very .similar mass spectra should

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

Sufficient GC resolution is achieved ifthe height of the valley between two isomer

peaks is less than 25% of the sum of the two peak heights. Otherwise, structural

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

lsosafrol) that may be separable by the GC should be identified, quantitated and

reported as the sum of both compounds by the GC.

7.6.1.5 Identification is hampered when sample components are not

resolved chromatographically and produce mass spectra containing ions contributed

by more than one analyte. When gas chromatographic peaks obviously represent

more than one sample component (Le., a broadened peak with shou!der(s) or a valley

between two or more maxima), appropriate selection of analyte spectra and

background spectra is important.

7.6.1.6 Examination of extracted ion current profiles of appropriate ions

can aid in the selectionof spectra and in qualitative identification of compounds. When

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

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

by the coeluting compound.

7.6.2 For samples containing components not associated with the calibration

standards, a library search may be made for the purpose of tentative identification. The

necessity to perform this type of identification will be determined by the purpose of the

analyses being conducted. Data system library search routines should not use normalization

routines that would misrepresent the library or unknown spectra when compared to each other.

For example, the ReRA permit or waste delisting requirements may require the

reporting of non-target analytes. Only after visual comparison of sample spectra with the

nearest library searches may the analyst assign a tentative identification. Guidelines for

tentative identification are:

(1) Relative intensities of major ions in the reference spectrum (ions> 10% of the

most abundant ion) should be present in the sample spectrum.

(2) The relative intensities of the major ions should agree within ± 20%. (Example:

For an ion with an abundance of 50% in the standard spectrum, the corresponding

sample ion abundance must be between 30 and 70%.)

(3) Molecular ions present in the reference spectrum should be present in the sample

spectrum.

(4) Ions present in the sample spectrum but not in the reference spectrum should be

reviewed for possible background contamination or presence of coeluting

compounds.

(5) Ions present in the reference spectrum but not in the sample spectrum should be

reviewed for possible subtraction from the sample spectrum because of

background contamination or coeluting peaks. Data system library reduction

programs can sometimes create these discrepancies.

7.7 Quantitative analysis

7.7.1 Once a compound has been identified, the quantitation of that compound will

be based on the integrated abundance of the primary characteristic ion from the EICP.

7.7.2 If the RSD of a compound's response factor is 15% or less, then the

concentration in the extract may be determined using the average response factor (RF) from

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

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

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

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

following modifications: The areas Ax and As should be from the total ion chromatograms, and

the RF for the compound should be assumed to be 1.

7.7.4 The resulting concentration should be reported indicating: (1) that the value

is an estimate, and (2) which internal standard was used to determine concentration. Use the

nearest internal standard free of interferences.

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7.7.5 Quantitation of multicomponent compounds (e.g., Toxaphene, Aroclors, etc.)

is beyond the scope of Method 8270. Normally, quantitation is performed using a GC/ECD,

by Methods 8081 or 8082. However, Method 8270 may be used to confirm the identification

of these compounds, when the concentrations are at least 10 ng/~L in the concentrated

sample extract.

7.7.6 Structural isomers that produce very similar mass spectra should be

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

Sufficient GC resolution is achieved if the height of the valley between two isomer peaks is less

than 25% of the sum of the two peak heights. Otherwise, structural isomers are quantitated

as isomeric pairs. Diastereomericpairs (e.g., Aramite and Isosafrol) that may be separable

by the GC should be summed and reported as the sum of both compounds.

8.0 QUALITY CONTROL

8.1 Refer to Chapter One and Method 8000 for specific quality control (QC) procedures.

Quality control procedures to ensure the proper operation of the various sample preparation and/or

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

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

quality of the data generated.

8.2 Qualitycontrol procedures necessary to evaluate the GC system operation are found

in Sec. 7.0 of Method 8000 and include calibration verification and chromatographic analysis of

samples. In addition, instrument QC requirements may be found in the following 'sections of Method

8270:

8.2.1 The GC/MS system must be tuned to meet the DFTPP criteria discussed in

Sees. 7.3.1 and 7.4.1.

8.2.2 There must bean initial calibration of the GC/MS system as described in Sec.

7.3.

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

in Sec. 7.4, each 12 hours.

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

standard component provided in Sec. 7.6.1.

8.3 Initialdemonstrationof proficiency - Each laboratory must demonstrate initial proficiency

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

of acceptable accuracy and precision for target analytes in a dean matrix. The laboratory must also

repeat the followinq operations whenever new staff are trained or significant changes in

instrumentation are made. See Method 8000, Sec. 8.0 for information on how to accomplish this

demonstration.

8.4 Sample quality control for preparation and analysis - The laboratory must also have

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

and detection limit). At a minimum, this includes the analysis of QC samples including a method

blank, matrix spike, a duplicate, and a laboratory control sample (LCS) in each analytical batch and

the addition of surrogates to each field sample and QC sample.

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

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

reagents are under control. Each time a set of samples is analyzed or there is a change in

reagents, a method blank should be analyzed as a safeguard against chronic laboratory

contamination. The blanks should be carried through all stages of sample preparation and

measurement.

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

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

pair. The decision on whether to prepare and analyze duplicate samples or a matrix

spike/matrix spike duplicate must be based on a knowledge of the samples in the sample

batch. If samples are expected to contain target analytes, then laboratories may use one

matrix spike and a duplicate analysis of an unspiked field sample. If samples are not expected

to contain target analytes, laboratories should use a matrix spike and matrix spike duplicate

pair.

8.4.3 A laboratory control sample (LCS) should be included with each analytical

batch. The LCS consists of an aliquot of a clean (control) matrix similar to the sample matrix

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

concentrations as the matrix spike. When the results of the matrix spike analysis indicate a

potential problem due to the sample matrix itself, the LCS results are used to verify that the

laboratory can perform the analysis in a clean matrix.

8.4.4 See Method 8000, Sec. 8.0 for the details on carrying out sample quality

control procedures for preparation and analysis.

8.5 Surrogate recoveries - The laboratory must evaluate surrogate recovery data from

individual samples versus the surrogate control limits developed by the laboratory. See Method

8000, Sec. 8.0 for information on evaluating surrogate data and developing and updating surrogate

limits.

8.6 The experience of the analyst performing GC/MS analyses is invaluable to the success

of the methods. Each day that analysis is performed, the calibration verification standard should be

evaluated to determine if the chromatographic system is operating properly. Questions that should

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

from previous calibrations? Careful examination of the standard chromatogram can indicate whether

the column is still performing acceptably, the injector is leaking, the injector septum needs replacing,

etc. If any changes are made to the system (e.g., the column changed, a septum is changed), see

the guidance in Sec 8.2 of Method 8000 regarding whether recalibration of the system must take

place.

8.7 It is recommended that the laboratory adopt additional quality assurance practices for

use with this method. The specific practices that are most productive depend upon the needs of the

laboratory and the nature of the samples. Whenever possible, the laboratory should analyze

standard reference materials and participate in relevant performance evaluation studies.

9.0 METHOD PERFORMANCE

9.1 Method 8250 (the packed column version of Method 8270) was tested by 15

laboratories using organic-free reagent water, drinking water, surface water, and industrial

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

CD-ROM 82700 - 23 Revision 4

January 1998
and precision, and method accuracy were found to be directly related to the concentration of the

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

relationships are presented in Table 7. These values are presented as guidance only and are not

intended as absolute acceptance criteria. Laboratories should generate their own acceptance

criteria for capillary column method performance... (See Method 8000.)

9.2 Chromatograms from calibration standards analyzed with Day 0 and Day 7 samples

were compared to detect possible deterioration of GC performance. These recoveries (using

Method 3510 extraction) are presented in Table 8.

9.3 Method performance data using Method 3541 (automated Soxhlet extraction) are

presented in Table 9. Single laboratory accuracy and precision data were obtained for semivolatile

organics in a clay soil by spiking at a concentration of 6 mg/kg for each compound. The spiking

solution was mixed into the soif during addition and then allowed to equilibrate for approximately 1

hour prior to extraction. The spiked samples were then extracted by Method 3541 (Automated

Soxhlet). Three extractions were performed and each extract was analyzed by gas

chromatography/mass spectrometry following Method 8270. The low recovery of the more volatile

compounds is probably due to volatilization losses during equilibration. These data are listed in

Table 10 and were taken from Reference 7.

9.4 Surrogate precision and accuracy data are presented in Table 11 from a field dynamic

spiking study based on air sampling by Method 0010. The trapping mediawere prepared for analysis

by Method 3542 and subsequently analyzed by Method 8270.

9.5 Single laboratory precision and bias data using Method 3545 (pressurized fluid

extraction) for semivolatile organic compounds are presented in Table 12. The samples were

conditioned spiked samples prepared and certified by a commercial supplier that contained 57

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

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

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

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

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

replicates relative to the automated Soxhlet data are as foUows: clay 96.8%, loam 98.7% and sand

102.1%. The average recoveries from the three concentrations also relative to the automated

Soxhlet data are as follows: low-101.2%, mid-97.2% and high-99.2%.

9.6 Single laboratoryprecision and bias data using Method 3561 (SFE extraction of PAHs

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

extraction of two certified referencematerials( EC-1, a lake sediment from Environment Canada and

HS-3, a marine sedimentfrom the National Science and Engineering Research Council of Canada,

both naturally-contaminated with PAHs). The SFE instrument used for these extractions was a

Hewlett-Packard Model 7680. Analysis was by GC/MS. Average recoveries from six replicate

extractions range from 85 to 148% (overall average of 100%) based on the certified value (or a

Soxhlet value if a certified value was unavailable for a specific analyte) for the lake sediment.

Average recoveries from three replicate extractions range from 73 to 133% (overall average of 92%)

based on the certified value for the marine sediment. The data are found in Tables 13 and 14 and

were taken from Reference 10.

9.7 Single laboratory precision and accuracy data using Method 3561 (SFE extraction of

PAHs with a fixed restrictor and liquid trapping) were obtained for twelve of the method analytes by

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

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

CD-ROM 8270D - 24 Revision 4

January 1998
Average recoveries from four replicate extractions range from 60 to 122% (overall average of 89%)

based on the certified value. Following are the instrument conditions that were utilized to extract a

3.4 g sample: Pressure - 300 atm; Time - 60 min.; Extraction fluid - CO2; Modifier - 10% 1:1 (v/v)

methanol/methylene chloride; Oven temperature - 80°C; Restrictor temperature - 120°C; and,

Trapping fluid - chloroform (methylene chloride has also been used). The data are found in Table

15 and were taken from Reference 11.

9.8 Tables 16 and 17 contain single-laboratory precision and accuracy data for solid-phase

extraction of TCLP buffer solutions spiked at two levels and extracted using Method 3535.

9.9 Table 18 contains multiple-laboratory data for solid-phase extraction of spiked TCLP

soil leachates extracted using Method 3535.

10.0 REFERENCES

1. Eichelberger, J.W., Harris, L.E., and Budde, W.L., "Reference Compound to Calibrate Ion

Abundance Measurement in Gas Chromatography-Mass Spectrometry Systems", Analytical

Chemistry, 47, 995-1000, 1975.

2. "Method Detection Limit for Methods 624 and 625", Olynyk, P., Budde, W.L., and Eichelberger,

J.W., unpublished report, October 1980. .

3. "Interlaboratory Method Study for EPA Method 625-Base/Neutrals, Acids, and Pesticides",

Final Report for EPA Contract 68-03-3102.

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

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

5. Lucas, S.v., Kornfeld, RA., "GC-MS Suitability Testing of RCRA Appendix VIII and Michigan

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

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

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

Organic Compounds for Extractability and Aqueous Stability by SW-846, Method 3510", U.S.

Environmental Protection Agency, Environmental Monitoring and Support Laboratory,

Cincinnati, OH 45268, June 5, 1987, Contract 68-03-3224.

7. Lopez-Avila, V. (W. Beckert, Project Officer); "Development of a Soxtec Extraction Procedure

for Extraction of Organic Compounds from Soils and Sediments"; U.S. Environmental

Protection Agency, Environmental Monitoring and Support Laboratory, Las Vegas, NV,

October 1991; EPA 600/X-91/140.

8. Bursey, J., Merrill, R, McAllister, R, and McGaughey, J., "Laboratory Validation of VOST and

SemiVOST for Halogenated Hydrocarbons from the Clean Air Act Amendments List", Vol. 1

and 2, U.S. Environmental Protection Agency, EPA 600/R-93/123a and b, (NTIS PB 93-227163

and 93-27171), Research Triangle Park, NC, July 1993.

9. Richter, B., Ezzell, J., and Felix, D., "Single Laboratory Method Validation Report: Extraction

of Target Compound List/Priority Pollutant List BNAs and Pesticides using Accelerated Solvent

Extraction (ASE) with Analytical Validation by GC/MS and GC/ECD", Document 101124,

Dionex Corporation, Salt Lake City, UT, June 16, 1994.

CD-ROM 8270D - 25 Revision 4

January 1998
10. Lee, H.B., Peart, T.E., Hong-You, R.L., and Gere, D.R., "Supercritical Carbon Dioxide

Extraction of Polycyclic Aromatic Hydrocarbons from Sediments", J. Chromatography, A 653

83-91 (1993).

11. Warner, S., "SFE Extraction of PNAs from Solid Matrices Using the Dionex 703M SFE

Extractor and a Liquid Trap," EPA Region III, Central Regional Laboratory, 839 BestgateRoad,

Annapolis, MD 21401, December 12,1994.

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

CD-ROM 8270D - 26 Revision 4

January 1998
TABLE 1

CHARACTERISTIC IONS FOR SEMIVOLATILE COMPOUNDS

Compound

2-Picoline

Aniline

. Phenol

Bis(2-chloroethyl) ether

2-Chlorophenol

1,3-Dichlorobenzene

1,4-Dichlorobenzene-d4 (IS)

1,4-Dichlorobenzene

Benzyl alcohol

1,2-Dichlorobenzene

N-Nitrosomethylethylamine

Bis(2-chloroisopropyl) ether

Ethyl carbamate

Thiophenol (Benzenethiol)

Methyl methanesulfonate

N-Nitrosodi-n-propylamine

Hexachloroethane

Maleic anhydride

Nitrobenzene

Isophorone

N-Nitrosodiethylamine

2-Nitrophenol

2,4-Dimethylphenol

p-Benzoquinone

Bis(2-chloroethoxy)methane

Benzoic acid

2,4-Dichlorophenol

Trimethyl phosphate

Ethyl methanesulfonate

1,2,4-Trichlorobenzene

Naphthalene-d, (IS)

Naphthalene

Hexachlorobutadiene

Tetraethyl pyrophosphate

Diethyl sulfate

4-Chloro-3-methylphenol

2-Methylnaphthalene

2-Methyl phenol

Hexachloropropene

Hexachlorocyclopentadiene

N-Nitrosopyrrolidine

Acetophenone

CD-ROM

Retention Primary

Time (min) Ion

3.758 93

5.68 93

5.77 94

5.82 93

5.97 128

6.27 146

6.35 152

6.40 146

6.78 108

6.85 146

6.97 88

7.22 45

7.27 62

7.42 110

7.48 80

7.55 70

7.65 117

7.6554

7.87 77

8.53 82

8.70 102

8.75 139

9.03 122

9.13 108

9.23 93

9.38 122

9.48 162

9.53 110

9.62 79

9.67 180

9.75 136

9.82 128

10.43 225

11.07 99

11.37 139

11.68 107

11.87 142

12.40 107

12.45 213

12.60 237

12.65 100

12.67 105

82700 - 27

Secondary lon(s)

66,92

66,65

65,66

63,95

64,130

148,111

150,115

148,111

79,77

148,111

42,43,56

77,121

44,45,74

66,109,84

79,65,95

42,101,130

201,199

98,53,44

123,65

95,138

42,57,44,56

109,65

107,121

54,82,80

95,123

105,77

164,98

79,95,109,140

109,97,45,65

182,145

68

129,127

223,227

155,127,81,109

45,59,99,111,125

144,142

141

108,77,79,90

211,215,117,106,141

235,272

41,42,68,69

71,51,120

Revision 4

January 1998
Compound

4-Methylphenol

2A,6-Trichlorophenol

o-Toluidine

3-Methylphenol

2-Chloronaphthalene

N-Nitrosopiperidine

1A-Phenylenediamine

1-Chloronaphthalene

2-Nitroaniline

5-Chloro-2-methylaniline

Dimethyl phthalate

Acenaphthylene

2,6-Dinitrotoluene

Phthalic anhydride

o-Anisidine

3-Nitroaniline

Acenaphthene-d., (IS)

Acenaphthene

2,4-Dinitrophenol

2,6-Dinitrophenol

4-Chloroaniline

lsosafrole

Dibenzofuran

2A-Diaminotoluene

2A-Dinitrotoluene

4-Nitrophenol

2-Naphthylamine

1A-Naphthoquinone

p-Cresidine

Dichlorovos

Diethyl phthalate

Fluorene

2,4,5-Trimethylaniline

N-Nitrosodi-n-butylamine

4-Chlorophenyl phenyl ether

Hydroquinone

4,6-Dinitro-2-methylphenol

Resorcinol

N-Nitrosodiphenylamine

Safrole

Hexamethyl phosphoramide

3-(Chloromethyl)pyridine hydrochloride

Diphenylamine

CD-'ROM

TABLE 1

(continued)

Retention Primary

Time (min) Ion

12.82 107

12.85 196

12.87 106

12.93 107

13.30 162

13.55 114

13.62 108

13.65a 162

13.75 65

14.28 106

14.48 163

14.57 152

14.62 165

14.62 104

15.00 108

15.02 138

15.05 164

15.13 154

15.35 184

15.47 162

15.50 127

15.60 162

15.63 168

15.78 121

15.80 165

15.80 139

16.00a 143

16.23 158

16.45 122

16.48 109

16.70 149

16.70 166

16.70 120

16.73 84

16.78 204

16.93 110

17.05 198

17.13 110

17.17 169

17.23 162

17.33 135

17.50 92

17.54a 169

8270D - 28

Secondary lon(s)

108,77,79,90

198,200

107,77,51,79

108,77,79,90

127,164

42,55,56,41

80,53,54,52

127,164

92,138

141,140,77,89

194,164

151,153

63,89

76,50,148

80,123,52

108,92

162,160

153,152

63,154

164,126,98,63

129,65,92

131,104,77,51

139

122,94,77,104

63,89

109,65

115,116

104,102,76,50,130

94,137,77,93

185,79,145

177,150

165,167

135,134,91,77

57,41,116,158

206,141

81,53,55

51,105

81,82,53,69

168,167

104,77,103,135

44,179,92,42

127,129,65,39

168,167

Revision 4

January 1998
TABLE 1

(continued)

Retention Primary Secondary lon(s)

Compound Time (min) Ion

1,2,4,5-Tetrachlorobenzene 17.97 216 214,179,108,143,218

1-Naphthylamine 18.20 143 115,89,63

1-Acetyl-2-thiourea 18.22 118 43,42,76

4-Bromophenyl phenyl ether 18.27 248 250,141

Toluene diisocyanate 18.42 174 145,173,146,132,91

2,4,5-Trichlorophenol 18.47 196 198,97,132,99

Hexach!orobenzene 18.65 284 142,249

Nicotine 18.70 84 133,161,162

Pentachlorophenol 19.25 266 264,268

5-Nitro-o-toluidine 19.27 152 77,79,106,94

Thionazine 19.35 107 96,97,143,79,68

4-Nitroaniline 19.37 138 65,108,92,80,39

Phenanthrene-d.; (IS) 19.55 188 94,80

Phenanthrene 19.62 178 179,176

Anthracene 19.77 178 176,179

1,4-Dinitrobenzene 19.83 168 75,50,76,92,122

Mevinphos 19.90 127 192,109,67,164

Naled 20.03 109 145,147,301,79,189

1,3-Dinitrobenzene 20.18 168 76,50,75,92,122

Diallate (cis or trans) 20.57 86 234,43,70

1,2-Dinitrobenzene 20.58 168 50,63,74

Diallate (trans or cis) 20.78 86 234,43,70

Pentachlorobenzene 21.35 250 252,108,248,215,254

5-Nitro-o-anisidine 21.50 168 79,52,138,153,77

Pentachloronitrobenzene 21.72 237 142,214,249,295,265

4-Nitroquinoline-1-oxide 21.73 174 101,128,75,116

Di-n-butyl phthalate 21.78 149 150,104

2,3,4,6-Tetrachlorophenol 21.88 232 131,230,166,234,168

Dihydrosaffrole 22.42 135 64,77

Demeton-O 22.72 88 89,60,61,115,171

Fluoranthene 23.33 202 101,203

1,3,5-Trinitrobenzene 23.68 75 74,213,120,91,63

Dicrotophos 23.82 127 67,72,109,193,237

Benzidine 23.87 184 92,185

Trifluralin 23.88 306 43,264,41,290

Bromoxynil 23.90 277 279,88,275,168

Pyrene 24.02 202 200,203

Monocrotophos 24.08 127 192,67,97,109

Phorate 24.10 75 121,97,93,260

Sulfallate 24.23 188 88,72,60,44

Demeton-S 24.30 88 60,81,89,114,115

Phenacetin 24.33 108 180,179,109,137,80

Dimethoate 24.70 87 93,125,143,229

CD-ROM 8270D - 29 Revision 4

January 1998
TABLE 1

(continued)

Retention Primary Secondary lanes)

Compound Time (min) Ion

Phenobarbital 24.70 204 117,232,146,161

Carbofuran 24.90 164 149,131,122

Octamethyl pyrophosphoramide 24.95 135 44,199,286,153,243

4-Aminobiphenyl 25.08 169 168,170,115

Dioxathion 25.25 97 125,270,153

Terbufos 25.35 231 57,97,153,103

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

Pronamide 25.48 173 175,145,109,147

Aminoazobenzene 25.72 197 92,120,65,77

Dichlone 25.77 191 163,226,228,135,193

Dinoseb 25.83 211 163,147,117,240

Disulfoton 25.83 88 97,89,142,186

Fluchloralin 25.88 306 63,326,328,264,65

Mexacarbate 26.02 165 150,134,164,222

4,4'-Oxydianiline 26.08 200 108,171,80,65

Butyl benzyl phthalate 26.43 149 91,206

4-Nitrobiphenyl 26.55 199 152,141,169,151

Phosphamidon 26.85 127 264,72,109,138

2-Cyclohexyl-4,6-Dinitrophenol 26.87 231 185,41,193,266

Methyl parathion 27.03 109 125,263,79,93

Carbaryl 27.17 144 115,116;201

Dimethylaminoazobenzene 27.50 225 120,77,105,148,42

Propylthiouracil 27.68 170 142,114,83

Benz(a)anthracene 27.83 228 229,226

Chrysene-d., (IS) 27.88 240 120,236

3,3'-Dichlorobenzidine 27.88 252 254,126

Chrysene 27.97 228 226,229

Malathion 28.08 173 125,127,93,158

Kepone 28.18 272 274,237,178,143,270

Fenthion 28.37 278 125,109,169,153

Parathion 28.40 109 97,291,139,155

Anilazine 28.47 239 241,143,178,89

Bis(2-ethylhexyl) phthalate 28.47 149 167,279

3,3'-Dimethylbenzidine 28.55 212 106,196,180

Carbophenothion 28.58 157 97,121,342,159,199

5-Nitroacenaphthene 28.73 199 152,169,141,115

Methapyrilene 28.77 97 50,191,71

Isodrin 28.95 193 66,195,263,265,147

Captan 29.47 79 149,77,119,117

Chlorfenvinphos 29.53 267 269,323,325,295

Crotoxyphos 29.73 127 105,193,166

Phosmet 30.03 160 77,93,317,76

EPN 30.11 157 169,185,141,323

CD-ROM 8270D - 30 Revision4

January 1998
TABLE 1

(continued)

Retention Primary Secondary lon(s)

Compound Time (min) Ion

Tetrachlorvinphos 30.27 329 109,331,79,333

Di-n-octyl phthalate 30.48 149 167,43

2-Aminoanthraquinone 30.63 223 167,195

Barban 30.83 222 51,87,224,257,153

Aramite 30.92 185 191,319,334,197,321

Benzo(b)fluoranthene 31.45 252 253,125

Nitrofen 31.48 283 285,202,139,253

Benzo(k)fluoranthene 31.55 252 253,125

Chlorobenzilate 31.77 251 139,253,111,141

Fensulfothion 31.87 293 97,308,125,292

Ethion 32.08 231 97,153,125,121

Diethylstilbestrol 32.15 268 145,107,239,121,159

Famphur 32.67 218 125,93,109,217

Tri-p-tolyl phosphate" 32.75 368 367,107,165,198

Benzo(a)pyrene 32.80 252 253,125

Perylene-d., (IS) 33.05 264 260,265

7,12-Dimethylbenz(a)anthracene 33.25 256 241,239,120

5,5-Diphenylhydantoin 33.40 180 104,252,223,209

Captafol 33.47 79 77,80,107

Dinocap 33.47 69 41,39

Methoxychlor 33.55 227 228,152,114,274,212

2-Acetylaminofluorene 33.58 181 180,223,152

4,4'-Methylenebis(2-chloroaniline) 34.38 231 266,268,140,195

3,3'-Dimethoxybenzidine 34.47 244 201,229

3-Methylcholanthrene 35.07 268 252,253,126,134,113

Phosalone 35.23 182 184,367,121,379

Azinphos-methyl 35.25 160 132,93,104,105

Leptophos 35.28 171 377,375,77,155,379

Mirex 35.43 272 237,274,270,239,235

Tris(2,3-dibromopropyl) phosphate 35.68 201 137,119,217,219,199

Dibenz(a,j)acridine 36.40 279 280,277,250

Mestranol 36.48 277 310,174,147,242

Coumaphos 37.08 362 226,210,364,97,109

Indeno(1,2,3-cd)pyrene 39.52 276 138,227

Dibenz(a,h)anthracene 39.82 278 139,279

Benzo(g,h,i)perylene 41.43 276 138,277

1,2:4,5-Dibenzopyrene 41.60 302 151,150,300

Strychnine 45.15 334 334,335,333

Piperonyl sulfoxide 46.43 162 135,105,77

Hexachlorophene 47.98 196 198,209,211,406,408

Aldrin 66 263,220

Aroclor 1016 222 260,292

Aroclor 1221 190 224,260

CD-ROM 82700 - 31 Revision 4

January 1998
Compound

Aroclor 1232

Aroclor 1242

Aroclor 1248

Aroclor 1254

Aroclor 1260

a-SHC

~-BHC

a-BHC

V-BHC (Lindane)

4,4'-DDD

4,4'-DDE

4,4'-DDT

Dieldrin

1,2-Diphenylhydrazine

Endosulfan I

Endosulfan 1\

Endosulfan sulfate

Endrin

Endrin aldehyde

Endrin ketone

2-Ftuorobiphenyl (surr)

2-Fluorophenol (surr)

Heptachlor

Heptachlor epoxide

Nitrobenzene-d, (surr)

N-Nitrosodimethylamine

Phencl-d, (surr)

Terphenyl-d., (surr)

2,4,6-Tribromophenol (surr)

Toxaphene

TABLE 1

(continued)

Retention Primary Secondary lon(s)

Time (min) Ion

190 224,260

222 256,292

292 362,326

292 362,326

360 362,394

183 181,109

181 183,109

183 181,109

183 181,109

235 237,165

246 248,176

235 237,165

79 263,279

77 105,182

195 339,341

337 339,341

272 387,422

263 82,81

67 345,250

317 67,319

172 171

112 64

100 272,274

353 355,351

82 128,54

42 74,44

99 42,71

244 122,212

330 332,141

159 231,233

IS =internal standard

surr =surrogate

"Estimated retention times

bSubstitute for the non-specific mixture, tricresyl phosphate

CD-ROM 8270D - 32 Revision 4

January 1998
TABLE 2

ESTIMATED QUANTITATION LIMITS (EQLs) FOR SEMIVOLATILE ORGANICS

Estimated Quantitation Limits"

Compound

Acenaphthene

Acenaphthylene

Acetophenone

1-Acetyl-2-thiourea

2-Aminoanthraquinone

Aminoazobenzene

4-Aminobiphenyl

Anilazine

o-Anisidine

Anthracene

Aramite

Azinphos-methyl

Barban

Benz(a)anthracene

Benzo(b)fluoranthene

Benzo(k)fluoranthene

Benzoic acid

Benzo(g,h,i)perylene

Benzo(a)pyrene

p-Benzoquinone

Benzyl alcohol

Bis(2-chloroethoxy)methane

Bis(2-chloroethyl) ether

Bis(2-chloroisopropyl) ether

4-Bromophenyl phenyl ether

Bromoxynil

Butyl benzyl phthalate

Captafol

Captan

Carbaryl

Carbofuran

Carbophenothion

Chlorfenvinphos

4-Chloroaniline

Chlorobenzilate

5-Chloro-2-methylaniline

CD-ROM

Ground water Low Soil/Sediment"

(1-l9/L) (1-l9/kg)

10 660

10 660

10 NO

')n f\ln L..V ........ 1000 NO

20 NO

10 NO

20 NO

100 NO

10 NO

10 660

20 NO

100 NO

200 NO

10 660

10 660

10 660

50 3300

10 660

10 660

10 NO

20 1300

10 660

10 660

10 660

10 660

10 NO

10 660

20 NO

50 NO

"1n f\ln IU ........

10 NO

10 NO

20 NO

20 1300

10 NO

10 NO

82700 - 33 Revision 4

January 1998
Compound

4-Chloro-3-methylphenol

3-(Chloromethyl)pyridine hydrochloride

2-Chloronaphthalene

2-Chlorophenol

4-Chiorophenyi phenyl ether

Chrysene

Coumaphos

p-Cresidine

Crotoxyphos

2-Cyclohexyl-4,6-dinitrophenol

Demeton-O

Demeton-S

Diallate (cis or trans)

Diallate (trans or cis)

2A-Diaminotoluene

Dibenz(a,j)acridine

Dibenz(a,h)anthracene

Dibenzofuran

Dibenzo(a,e)pyrene

Di-n-butyl phthalate

Dichlone

1,2-Dichlorobenzene

1,3-Dichlorobenzene

1A-Dichlorobenzene

3,3'-Dichlorobenzidine

2A-Dichlorophenol

2,6-Dichlorophenol

Dichlorovos

Dicrotophos

Diethy! phthalate

Diethylstilbestrol

Diethyi sulfate

Dimethoate

3,3'-Dimethoxybenzidine

Dimethylaminoazobenzene

7,12-Dimethy!benz(a)anthracene

3,3'-Dimethylbenzidine

2A-Dimethylphenol

CD"ROM

TABLE 2

(Continued)

Estimated Quantitation Limits"

Ground water Low Soil/Sediment"

(1-l9/L) (1-l9/kg)

20 1300

100 ND

10 660

10 660

'10 660

10 660

40 ND

10 ND

20 ND

100 ND

10 ND

10 ND

10 ND

10 ND

20 ND

10 ND

10 660

10 660

10 ND

10 ND

NA ND

10 660

10 660

10 660

20 1300

10 660

10 ND

10 NO

'10 NO

10 660

20 ND

100 ND

20 ND

100 ND

10 NO

10 ND

10 ND

10 660

8270D -34 Revision 4

January 1998
Compound

Dimethyl phthalate

1,2-Dinitrobenzene

1,3-Dinitrobenzene

1A-Dinitrobenzene

4,6-Dinitro-2-methyiphenoi

2A-Dinitrophenol

2,4-Dinitrotoluene

2,6-Dinitrotoluene

Dinocap

Dinoseb

5,S-Diphenylhydantoin

Di-n-cetyl phthalate

Disulfoton

EPN

Ethion

Ethyl carbamate

Bis(2-ethylhexyl) phthalate

Ethyl methanesulfonate

Famphur

Fensulfothion

Fenthion

Fluchloralin

Fluoranthene

Fluorene

Hexachlorobenzene

Hexachlorobutadiene

Hexachlorocyclopentadiene

Hexachloroethane

Hexachlorophene

Hexachloropropene

Hexamethylphosphoramide

indeno(1,2,3-cd)pyrene

Isodrin

Isophorone

Isosafrole

Kepone

Leptophos

Malathion

CD-ROM

TABLE 2

(Continued)

Estimated Quantitation Limits"

Ground water Low Soil/Sediment"

(lJg/L) (1J9/kg)

10 660

40 ND

20 ND

40 ND rr rv "'-""'Inn OU ,),)UU

50 3300

10 660

10 660

100 ND

20 ND

20 ND

10 660

10 ND

10 ND

10 ND

50 ND

10 660

20 ND

20 ND

40 ND

10 ND

20 ND

10 660

10 660

10 660

10 660

10 660

10 660

50 ND

10 ND

20 ND

10 660

20 ND

10 660

10 ND

20 ND

10 ND

50 ND

8270D - 35 Revision 4

January 1998
Compound

Mestranol

Methapyrilene

Methoxychlor

3-Methylcholanthrene

Methyl methanesuifonate

2-Methylnaphthalene

Methyl parathion

2-Methylphenol

3-Methylphenol

4-Methylphenol

Mevinphos

Mexacarbate

Mirex

Monocrotophos

Naled

Naphthalene

1A-Naphthoquinone

1-Naphthylamine

2-Naphthylamine

Nicotine

5-Nitroacenaphthene

2-Nitroaniline

3-Nitroaniline

4-Nitroanifine

5-Nitro-o-anisidine

Nitrobenzene

4-Nitrobiphenyl

Nitrofen

2-Nitrophenol

4-Nitrophenol

5-Nitro-o-toluidine

4-Nitroquinoiine-1-oxide

N-Nitrosodi-n-butylamine

N-Nitrosodiethylamine

N-Nitrosodiphenylamine

N-Nitroso-di-n-propylamine

N-Nitrosopiperidine

N-Nitrosopyrrolidine

CD-ROM

TABLE 2

(Continued)

Estimated Quantitation Limits"

Ground water Low Soil/Sediment"

(lJg/L) (lJg/kg)

20 NO

100 NO

10 NO

10 NO

10 ND

10 660

10 NO

10 660

10 NO

10 660

10 NO

20 NO

10 NO

40 NO

20 ND

10 660

10 NO

10 NO

10 NO

20 NO

10 NO

50 3300

50 3300

20 NO

10 NO

10 660

10 NO

20 NO

10 660

50 3300

10 NO

40 ND

10 NO

20 NO

10 660

10 660

20 NO

40 NO

82700 - 36 Revision 4

J.anuary 1998
Compound

actamethyl pyrophosphoramide

4,4'-Oxydianiline

Parathion

Pentachlorobenzene

Pentachioronitrobenzene

Pentachlorophenol

Phenacetin

Phenanthrene

Phenobarbital

Phenol

1,4-Phenylenediamine

Phorate

Phosalone

Phosmet

Phosphamidon

Phthalic anhydride

2-Picoline

Piperonyl sulfoxide

Pronamide

Propylthiouracil

Pyrene

Resorcinol

Safrole

Strychnine

Sulfallate

Terbufos

1,2,4,5-Tetrachlorobenzene

2,3,4,6-Tetrachlorophenol

Tetrachlorvinphos

Tetraethyl pyrophosphate

Thionazine

Thiophenoi (Benzenethioi)

o-Toluidine

1,2,4-Trichlorobenzene

2,4,5-Trichlorophenol

2,4,6-Trichlorophenol

Trifluralin

2,4,5-Trimethylaniline

CD-ROM

TABLE 2

(Continued)

Estimated Quantitation Limits"

Ground water Low Soil/Sediment''

(lJg/L) (lJg/kg)

200 NO

20 NO

10 NO

10 NO

20 ND

50 3300

20 NO

10 660

10 NO

10 660

10 NO

10 NO

100 NO

40 NO

100 NO

100 NO

NO NO

100 NO

10 NO

100 NO

10 660

100 NO

10 NO

40 NO

10 NO

20 NO

10 NO

10 NO

20 NO

40 NO

20 NO

20 NO

10 NO

10 660

10 660

10 660

10 NO

10 NO

82700 - 37 Revision 4

January 1998
TABLE 2

(Continued)

Estimated Quantitation Limits"

Compound

Ground water Low Soil/Sediment"

(!Jg/L) (!Jg/kg)

Trimethyl phosphate

1,3,5-Trinitrobenzene

Tris(2,3-dibromopropyl) phosphate

Tri-p..:tolyl phosphate(h)

10

10

200

10

NO

NO

NO

NO

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

may not always be achievable.

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

weight basis, therefore, EQLs will be higher based on the % dry weight of each sample. These

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

NO = Not Determined

NA = Not Applicable

Other Matrices

High-concentration soil and sludges by ultrasonic extractor

Non-water miscible waste

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

Factor

7.5

75

CD·HOM 82700- 38 Revision 4

January 1998
TABLE 3

DFTPP KEY IONS AND ION ABUNDANCE CRITERIAa,b

Mass Ion Abundance Criteria

51 30-60% of mass 198

68 < 2% of mass 69

70 < 2% of mass 69

127 40-60% of mass 198

-107 <' -10/.. ,...f rY'\-:>c-c- -10Q 1-.;;..11 .... I IU VI 1II00vv I \JU

198 Base peak, 100% relative abundance

199 5-9% of mass 198

275 10-30% of mass 198

365 > 1% of mass 198

441 Present but less than mass 443

442 > 40% of mass 198

443 17-23% of mass 442

a Data taken from Reference 3.

b Alternate tuning criteria may be employed,

(e.g., CLP, Method 525, or manufacturers'

instructions), provided that method

performance is not adversely affected.

TABLE 4

CALIBRATION CHECK COMPOUNDS (CCC)

CD-ROM

Base/Neutral Fraction

Acenaphthene

1,4-Dichlorobenzene

Hexachlorobutadiene

Diphenylamine

Di-n-octyl phthalate

Fluoranthene

Benzo(a)pyrene

Acid Fraction

4-Chloro-3-methylphenol

2,4-Dichlorophenol

2-Nitrophenol

Phenol

Pentachlorophen01

2,4,6-Trichlorophenol

82700 - 39 Revision 4

January 1998
TABLE 5

SEMIVOLATILE INTERNAL STANDARDS WITH CORRESPONDING ANALYTES

ASSIGNED FOR QUANTITATION

1,4-Dichlorobenzene-d4

Aniiine

Benzyl alcohol

Bis(2-chloroethyl) ether

Bis(2-chloroisopropyl) ether

2-Chlorophenol

1,3-Dichlorobenzene

1,4-Dichlorobenzene

1,2-Dichlorobenzene

Ethyl methanesulfonate

2-Fluorophenol (surr)

Hexachloroethane

Methyl methanesulfonate

2-Methylphenol

4-Methylphenol

N-Nitrosodimethylamine

N-Nitroso-di-n-propylamine

Phenol

Phenol-d, (surr)

2-Picoline

(surr) =surrogate

CD-ROM

Naphthalene-d,

Acetophenone

Benzoic acid

Bis(2-chloroethoxy)methane

4-Chloroaniline

4-Chloro-3-methylphenol

2,4-Dichlorophenol

2,6-Dichlorophenol

a,a-Dimethylphenethylamine

2,4-Dimethylphenol

Hexachlorobutadiene

Isophorone

2-Methylnaphthalene

Naphthalene

Nitrobenzene

Nitrobenzene-d, (surr)

2-Nitrophenol

N-Nitrosodi-n-butylamine

N-Nitrosopiperidine

1,2,4-Trichlorobenzene

8270D - 40

Acenaphthene-d.,

Acenaphthene

Acenaphthylene

1-Chloronaphthalene

2-Chloronaphthalene

4-Chlorophenyl phenyl ether

Dibenzofuran

Diethyl phthalate

Dimethyl phthalate

2,4-Dinitrophenol

2,4-Dinitrotoluene

2,6-Dinitrotoluene

Fluorene

2-Fluorobiphenyl (surr)

Hexachlorocyclopentadiene

1-Naphthylamine

2-Naphthylamine

2-Nitroaniline

3-Nitroaniline

4-Nitroaniline

4-Nitrophenol

Pentachlorobenzene

1,2,4,5-Tetrachlorobenzene

2,3,4,6-Tetrachlorophenol

2,4,6-Tribromophenol (surr)

2,4,6-Trichlorophenol

2,4,5-Trichlorophenol

Revision 4

January 1998
TABLE 5

(continued)

Phenanthrene-d., Chrysene-d.,

4-Aminobiphenyl Benzidine

Anthracene Benzo(a)anthracene

4-Bromophenyl phenyl ether Bis(2-ethylhexyl) phthalate

Di-n-butyl phthalate Butyl benzyl phthalate

4,6-Dinitro-2-methylphenol Chrysene

Diphenylamine 3,3'-Dichlorobenzidine

Perylene-d.,

Benzo(b)fluoranthene

Benzo(k)fluoranthene

Benzo(g,h,i)perylene

Benzo(a)pyrene

Dibenz(a,j)acridine

Dibenz(a,h)anthracene

Fluoranthene

Hexachlorobenzene

N-Nitrosodiphenylamine

Pentachlorophenol

Pentachloronitrobenzene

Phenacetin

Phenanthrene

Pronamide

(surr) =surrogate

CD-ROM

p-Dimethyl aminoazobenzene

Pyrene

Terphenyl-d., (surr)

7,12-Dimethylbenz(a)

anthracene

Di-n-cetyl phthalate

Indeno(1,2,3-cd) pyrene

3-Methylcholanthrene

82700 - 41 Revision 4

January 1998
TABLE 6

MULTILABORATORY PERFORMANCE DATN

Test cone. Limit for Range for x Range

Compound (lJg/L) s (lJg/L) (lJg/L) p, ps(%)

Acenaphthene 100 27.6 60.1-132.3 47-145

Acenaphthylene 100 40.2 53.5-126.0 33-145

Aldrin 100 39.0 7.2-152.2 0-166

Anthracene 100 32.0 43.4-118.0 27-133

Benz(a)anthracene 100 27.6 41.8-133.0 33-143

Benzo(b}fluoranthene 100 38.8 42.0-140.4 24-159

Benzo(k}fluoranthene 100 32.3 25.2-145.7 11-162

Benzo(a)pyrene 100 39.0 31.7-148.0 17-163

Benzo(g,h,i)perylene 100 58.9 0-195.0 0-219

Benzyl butyl phthalate 100 23.4 0-139.9 0-152

f3-BHC 100 31.5 41.5-130.6 24-149

a-BHC 100 21.6 0-100.0 0-110

Bis(2-chloroethyl) ether 100 55.0 42.9-126.0 12-158

Bis(2-chloroethoxy)methane 100 34.5 49.2-164.7 33-184

Bis(2-chloroisopropyl) ether 100 46.3 62.8-138.6 36-166

Bis(2-ethylhexyl) phthalate 100 41.1 28.9-136.8 8-158

4-Bromophenyl phenyl ether 100 23.0 64.9-114.4 53-127

2-Chloronaphthalene 100 13.0 64.5-113.5 60-118

4-Chlorophenyl phenyl ether 100 33.4 38.4-144.7 25-158

Chrysene 100 48.3 44.1-139.9 17-168

4A'-DDD 100 31.0 0-134.5 0-145

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

4A'-DDT 100 61.6 0-170.6 0-203

Dibenzo(a,h)anthracene 100 70.0 0-199.7 0-227

DI-n-butyl phthalate 100 16.7 8.4-111.0 1-118

1,2-Dichlorobenzene 100 30.9 48.6-112.0 32-129

1,3-Dichlorobenzene 100 41.7 16.7-153.9 0-172

1A-Dichlorobenzene 100 32.1 37.3-105.7 20-124

3,3'-Dichlorobenzidine 100 71.4 8.2-212.5 0-262

Dieldrin 100 30.7 44.3-119.3 29-136

Diethyl phthalate 100 26.5 0-100.0 0-114

Dimethyl phthalate 100 23.2 0-100.0 0-112

2A-Dinitrotoluene 100 21.8 47.5-126.9 39-139

2,6-0initrotoluene 100 29.6 68.1-136.7 50-158

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

Endosulfan sulfate 100 16.7 0-103.5 0-107

Endrin aldehyde 100 32.5 0-188.8 0-209

Fluoranthene 100 32.8 42.9-121.3 26-137

CD-ROM 82700 - 42 Revision 4

January 1998
TABLE 6

Ccontinued)

Compound

Fluorene

Heptachlor

Heptachlor epoxide

Hexachlorobenzene

Hexachlorobutadiene

Hexachloroethane

Indeno(1,2,3-cd)pyrene

Isophorone

Naphthalene

Nitrobenzene

N-Nitrosodi-n-propylamine

Arocior 1260

Phenanthrene

Pyrene

1,2,4-Trichlorobenzene

4-Chloro-3-methylphenol

2-Chlorophenol

2,4-Chlorophenol

2,4-0imethylphenol

2,4-0initrophenol

2-Methyl-4,6-dinitrophenol

2-Nitrophenol

4-Nitrophenol

Pentachlorophenol

Phenol

2,4,6-Trichlorophenol

Test cone.

ClJg/L)

100

100

100

100

100

100

100

100

100

100

100

100

100

100

100

100

100

100

100

100

100

100

100

100

100

100

Limit for

s ClJg/L)

20.7

37.2

54.7

24.9

26.3

24.5

44.6

63.3

30.1

39.3

55.4

54.2

20.6

25.2

28.1

37.2

28.7

26.4

26.1

49.8

93.2

35.2

47.2

48.9

22.6

31.7

Range for x

ClJg/L)

71.6-108.4

0-172.2

70.9-109.4

7.8-141.5

37.8-102.2

55.2-100.0

0-150.9

46.6-180.2

35.6-119.6

54.3-157.6

13.6-197.9

19.3-121.0

65.2-108.7

69.6-100.0

57.3-129.2

40.8-127.9

36.2-120.4

52.5-121.7

41.8-109.0

0-172.9

53.0-100.0

45.0-166.7

13.0-106.5

38.1-151.8

16.6-100.0

52.4-129.2

Range

p, pS(%)

59-121

0-192

26.155

0-152

24-116

40-113

0-171

21-196

21-133

35-180

0-230

0-164

54-120

52-115

44-142

22-147

23-134

39-135

32-119

0-191

0-181

29-182

0-132

14-176

5-112

. 37-144

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

-

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

p, Ps = Measured percent recovery

D

a Criteria from 40 CFR Part 136 for Method 625, using a packed GC column. These criteria are

based directly on the method performance data in Table 7. Where necessary, the limits for

recovery have been broadened to assure applicability of the limits to concentrations below those

used to develop Table 7. These values are for guidance only. Appropriate derivation of

acceptance criteria for capillary columns should result in much narrower ranges. See Method 8000

for information on developing and updating acceptance criteria for method performance.

CO-ROM 82700 - 43 Revision 4

January 1998
TABLE 7

METHOD ACCURACY AND PRECISION AS FUNCTIONS OF CONCENTRATIONa

Compound

Acenaphthene

Acenaphthylene

Aldrin

Anthracene

Benz(a)anthracene

Benzo(b)flu oranthene

Benzo(k)fluoranthene

Benzo(a)pyrene

Benzo(g,h,i)perylene

Benzyl butyl phthalate

~-BHC

B-BHC

Bis(2-chloroethyl) ether

Bis(2-chloroethoxy}methane

Bis(2-chloroisopropyl) ether

Bis(2-ethylhexyl) phthalate

4-Bromophenyl phenyl ether

2-Chloronaphthalene

4-Chlorophenyl phenyl ether

Chrysene

4A'-DDD

4,4'-DDE

4A'-DDT

Dibenzo{a,h}anthracene

Di-n-butyl phthalate

1,2-Dichlorobenzene

1,3-Dichlorobenzene

1A-Dichlorobenzene

3,3'-Dichlorobenzidine

Dieldrin

Diethyl phthalate

Dimethyl phthalate

2,4-Dinitrotoluene

2,6-Dinitrotoluene

Di-n-octyl phthalate

Endosulfan sulfate

Endrin aldehyde

Fluoranthene

Fluorene

Accuracy, as

recovery, x' (!Jg/L)

0.96C+0.19

0.89C+0.74

0.78C+1.66

0:80C+0.68

0.88C-0.60

0.93C-1.80

0.87C-1.56

0.90C-0.13

0.98C-0.86

0.66C-1.68

0.87C-0.94

0.29C-1.09

0.86C-1.54

1.12C-5.04

1.03C-2.31

0.84C-1.18

0.91C-1.34

0.89C+O.01

0.91C+0.53

0.93C-1.00

0.56C-0.40

0.70C-0.54

0.79C-3.28

0.88C+4.72

0.59C+0.71

0.80C+0.28

0.86C-0.70

0.73C-1.47

1.23C-12.65

0.82C-0.16

0.43C+1.00

0.20C+1.03

0.92C-4.81

1.06C-3.60

0.76C-0.79

0.39C+0.41

0.76C-3.86

0.81C+1.10

0.90C-0.00

Single analyst

precision, s,' (!Jg/L)

0.15x-O.12

0.24x-1.06

0.27x-1.28

0.21x-0.32

0.15x+0.93

0.22x+0.43

0.19x+1.03

0.22x+0.48

0.29x+2.40

0.18x+0.94

0.20x-0.58

0.34x+0.86

0.35x-0.99

0.16x+1.34

0.24x+0.28

0.26x+0.73

0.13x+0.66

0.07x+0.52

0.20x-0.94

0.28x+0.13

0.29x-0.32

0.26x-1.17

0.42x+0.19

0,30x+8.51

0.13x+1.16

0.20x+0.47

0.25x+0.68

0.24x+0.23

0.28x+7.33

0.20x-0.16

0.28x+1.44

0.54x+0.19

0.12x+1.06

0.14x+1.26

0.21x+1.19

0.12x+2.47

0.18x+3.91

0.22x-0.73

0.12x+0.26

Overall precision,

S' (!Jg/L)

0.21x-0.67

0.26x-0.54

0.43 x+1.13

0.27x-0.64

0.26x-0.21

0.29x+0.96

0.35x+0.40

0.32x+1.35

0.51 x-0.44

0.53x+0.92

0.30x+1.94

0.93x-0.17

0.35x+0.10

0.26x+2.01

0.25x+1.04

0.36x+0.67

0.16x+0.66

0.13x+0.34

0.30x-0.46

0.33x-0.09

0.66x-0.96

0.39x-1.04

0.65x-0.58

0.59x+0.25

0.39x+0.60

0.24x+0.39

0.41x+0.11

0.29x+0.36

0.47x+3.45

0.26x-0.07

0.52x+0.22

1.05x-0.92

0.21 x+1.50

0.19x+0.35

0.37x+1.19

0.63x-1.03

0.73x-0.62

0.28x-0,60

0.13x+0.61

CD-ROM 82700 - 44 Revision 4

January 1998
Compound

Heptachlor

Heptachlor epoxide

Hexachlorobenzene

Hexachlorobutadiene

Hexachloroethane

Indeno(1,2,3-cd)pyrene

Isophorone

Naphthalene

Nitrobenzene

N-Nitrosodi-n-propylamine

Aroclor 1260

Phenanthrene

Pyrene

1,2,4-Trichlorobenzene

4-Chloro-3-methylphenol

2-Chlorophenol

2,4-0ichlorophenol

2,4-0imethylphenol

2,4-0initrophenol

2-Methyl-4,6-dinitrophenol

2-Nitrophenol

4-Nitrophenol

Pentachlorophenol

Phenol

2,4,6-Trichlorophenol

TABLE 7

(Continued)

Accuracy, as

recovery, x' (~g/L)

0.87C-2.97

0.92C-1.87

0.74C+0.66

0.71 C-1.01

0.73C-0.83

0.78C-3.10

1.12C+1.41

0.76C+1.58

1.09C-3.05

1.12C-6.22

0.81C-10.86

0.87C+0.06

0.84C-0.16

0.94C-0.79

0.84C+0.35

0.78C+0.29

0.87C-0.13

0.71C+4.41

0.81C-18.04

1.04C-28.04

0.07C-1.15

0.61C-1.22

0.93C+1.99

0.43C+1.26

0.91C-0.18

Single analyst

precision, s,' (~g/L)

0.24x-0.56

0.33x-0.46

0.18x-0.10

0.19x+0.92

0.17x+0.67

0.29x+1.46

0.27x+0.77

0.21 x-0.41

0.19x+0.92

0.27x+0.68

0.35x+3.61

0.12x+0.57

0.16x+0.06

0:15x+0.85

0.23x+0.75

0.18x+1.46

0.15x+1.25

0.16x+1.21

0.38x+2.36

0.10x+42.29

0.16x+1.94

0.38x+2.57

0.24x+3.03

0.26x+0.73

0.16x+2.22

Overall precision,

S' (~g/L)

0.50x-0.23

0.28x+0.64

0.43x-0.52

0.26x+0.49

0.17x+0.80

0.50x-0.44

0.33x+0.26

0.30x-0.68

0.27x+0.21

0.44x+0.47

0.43x+1.82

0.15x+0.25

0.15x+0.31

0.21x+0.39

0.29x+1.31

0.28x+0.97

0.21x+1.28

0.22x+1.31

0.42x+26.29

0.26x+23.10

0.27x+2.60

0.44x+3.24

0.30x+4.33

0.35x+0.58

0.22x+1.81

x' =

s'r =

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

C, in ~g/L.

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

X, in ~g/L.

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

found of X, in ~g/L.

C = True value for the concentration, in ~g/L. -

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

~g/L.

a Criteria from 40 CFR Part 136 for Method 625, using a packed GC column. These criteria are

based directlyon the method performance data in Table 7. These values are for guidance

only. Appropriate derivation of acceptance criteria for capillary columns should result in much

narrower ranges. See Method 8000 for information on developing and updating acceptance

criteria for method performance.

CD-ROM' 82700 - 45 Revision 4

January 1998
TABLE 8

EXTRACTION EFFICIENCY AND AQUEOUS STABILITY RESULTS

Percent Recovery, Day 0 Percent Recovery, Day 7

Compound Mean RSD Mean RSD

3-Amino-9-ethylcarbazole 80 8 73 3

4-Chloro-1,2-phenylenediamine 91 1 108 4

4-Chloro-1,3-phenylenediamine 84 3 70 3

1,2-Dibromo-3-chioropropane 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-o4oluidine 99 10 93 4

2-Picoline 80 4 83 4

Tetraethyl dithiopyrophosphate 92 7 70 1

Data taken from Reference 6.

CD-ROM 8270D- 46 Revision 4

January 1998
TABLE 9

MEAN PERCENT RECOVERIES AND PERCENT RSD VALUES FOR SEMIVOLATILE ORGANICS

FROM SPIKED CLAY SOIL AND TOPSOIL BY AUTOMATED SOXHLET EXTRACTION

(METHOD 3541) WITH HEXANE-ACETONE (1 :1)8

Clay Soil Topsoil

Mean RSD Mean RSD

Compound Recovery Recovery

1,3-Dichlorobenzene 0 0

1,2-Dichlorobenzene 0 0

Nitrobenzene 0 0

Benzal chloride 0 0

Benzotrichloride 0 0

4-Chloro-2-nitrotoluene 0 0

Hexachlorocyclopentadiene 4.1 15 7.8 23

2,4-Dichloronitrobenzene 35.2 7.6 21.2 15

3,4-Dichloronitrobenzene 34.9 15 20.4 11

Pentachlorobenzene 13.7 7.3 14.8 13

2,3,4,5-Tetrachloronitrobenzene 55.9 6.7 50.4 6.0

Benefin 62.6 4.8 62.7 2.9

alpha-BHC 58.2 7.3 54.8 4.8

Hexachlorobenzene 26.9 13 25.1 5.7

delta-BHC 95.8 4.6 99.2 1.3

Heptachlor 46.9 9.2 49.1 6.3

Aldrin 97.7 12 102 7.4

Isopropalin 102 4.3 105 2.3

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

8 The operating conditions for the Soxtec apparatus were as follows: immersion time 45 min;

extraction time 45 min; the sample size was 10 g; the spiking concentration was 500 ng/g, except

for the surrogate compounds at 1000 ng/g, 2,5-0ichlorophenyl-4-nitrophenyl ether, 2,3,6-

Trichlorophenyl-4-nitrophenyl ether, and 2,3,4-Trichlorophenyl-4-nitrophenyl ether at 1500 ng/g,

Nitrobenzene at 2000 ng/g, and 1,3-Dichlorobenzene and 1,2-Dichlorobenzene at 5000 ng/g.

CD-ROM 82700 - 47 Revision 4

January 1998
TABLE 10

SINGLE LABORATORY ACCURACY AND PRECISION DATA FOR THE EXTRACTION

OF SEMIVOLATILE ORGANICS FROM SPIKED CLAY BY

AUTOMATED SOXHLET (METHOD 3541)a

Compound Mean Recovery RSD

Phenol 47.8 5.6

Bis(2-chloroethyl)ether 25.4 13

2-Chlorophenol 42.7 4.3

Benzyl alcohol tzt: o 7") ,J,J.v I.L..

2-Methylphenol 17.6 6.6

Bis(2-chloroisopropyl)ether 15.0 15

4-Methylphenol 23.4 6.7

N-Nitroso-di-n-propylamine 41.4 6.2

Nitrobenzene 28.2 7.7

Isophorone 56.1 4.2

2-Nitrophenol 36.0 6.5

2,4-Dimethylphenol 50.1 5.7

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

3-Nitroaniline 77.6 5.3

Acenaphthene 79.2 4.0

2,4-Dinitrophenol 91.9 8.9

4-Nitrophenol a") o -1a VL...v IV

Dibenzofuran 82.1 5.9

2,4-Dinitrotoluene 84.2 5.4

2,6-Dinitrotoluene 68.3 5.8

Diethyl phthalate 74.9 5.4

4.,Chlorophenyl-phenyl ether 67.2 3.2

Fluorene 82.1 3.4

CD-ROM 82700 - 48 Revision 4

January 1998
Compound

4-Nitroaniline

4,6-Dinitro-2-methylphenol

N-Nitrosodiphenylamine

4-Bromophenyl-phenyl ether

Hexachlorobenzene

Pentachlorophenol

Phenanthrene

Anthracene

Di-n-butyl phthalate

Fluoranthene

Pyrene

Butyl benzyl phthalate

3,3'-Dichlorobenzidine

Benzo(a)anthracene

Bis(2-ethylhexyl) phthalate

Chrysene

Di-n-cetyl phthalate

Benzo(b)fluoranthene

Benzo(k)fluoranthene

Benzo(a)pyrene

Indeno(1,2,3-cd)pyrene

Dibenzo(a,h)anthracene

Benzo(g,h,i)perylene

1,2-Dichlorobenzene

1,3-Dichlorobenzene

1A-Dichlorobenzene

Hexachloroethane

Hexachlorobutadiene

TABLE 10

(continued)

Mean Recovery

79.0

63.4

77.0

62.4

72.6

62.7

83.9

96.3

78.3

87.7

102

66.3

25.2

73.4

77.2

76.2

83.1

82.7

71.7

71.7

72.2

66.7

63.9

a

o

o

o

o

RSD

7.9

6.8

3.4

3.0

3.7

6.1

5.4

3.9

40

6.9

0.8

5.2

11

3.8

4.8

4.4

4.8

5.0

4.1

4.1

4.3

6.3

8.0

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

as follows: immersion time 45 min; extraction time 45 min; the sample size was 10 9 clay soil; the

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

after spiking.

Data taken from Reference 7.

CD-ROM 82700 - 49 Revision 4

January 1998
TABLE 11

PRECISION AND BIAS VALUES FOR METHOD 35421

Compound Mean Recovery Standard Deviation % RSD

2-Fluorophenol 74.6 28.6 38.3

Phenol-d, 77.8 27.7 35.6

Nitrobenzene-d, 65.6 32.5 49.6

2-Fluorobiphenyl 75.9 30.3 39.9

2,4,6-Tribromophenol 67.0 34.0 50.7

Terphenyl-d., 78.6 32.4 41.3

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

0010 matrices in a field dynamic spiking study.

CD-ROM 8270D - 50 Revision 4

January 1998
TABLE 12

ACCELERATED SOLVENT EXTRACTION (METHOD 3545) RECOVERY VALUES

AS PERCENT OF SOXTECTM

Clay Loam Sand Mean

Compound Low Mid High Low Mid High Low Mid High Rec.

Phenol 93.3 78.7 135.9 73.9 82.8 124.6 108.8 130.6 89.7 102.0

Bis(2-chloroethyl) ether 102.1 85.1 109.1 96.0 88.0 103.6 122.3 119.9 90.8 101.9

2-Chlorophenol 100.8 82.6 115.0 93.8 88.9 111.1 115.0 115.3 91.9 101.6

1,3-Dichlorobenzene 127.7 129.7 110.0 *364.2 129.9 119.0 *241.3 *163.7 107.1 120.6

1,4-Dichlorobenzene 127.9 127.0 110.5 *365.9 127.8 116.4 *309.6 *164.1 105.8 119.2

1,2-Dichlorobenzene 116.8 115.8 101.3 *159.2 113.4 105.5 *189.3 134.0 100.4 112.5

2-Methylphenol 98.9 82.1 119.7 87.6 89.4 111.0 133.2 128.0 92.1 104.7

Bis(2-chloroisopropyl)ether 109.4 71.5 108.0 81.8 81.0 88.6 118.1 148.3 94.8 100.2

o-Toluidine 100.0 89.7 117.2 100.0 *152.5 120.3 100.0 *199.5 102.7 110.3

N-Nitroso-di-n-propylamine 103.0 79.1 107.7 83.9 88.1 96.2 109.9 123.3 91.4 98.1

Hexachloroethane 97.1 125.1 111.0 *245.4 117.1 128.1 *566.7 147.9 103.7 118.6

Nitrobenzene 104.8 82.4 106.6 86.8 84.6 101.7 119.7 122.1 93.3 100.2

Isophorone 100.0 86.4 98.2 87.1 87.5 109.7 135.5 118.4 92.7 101.7

2,4-Dimethylphenol 100.0 104.5 140.0 100.0 114.4 123.1 100.0 *180.6 96.3 109.8

2-Nitrophenol 80.7 80.5 107.9 91.4 86.7 103.2 122.1 107.1 87.0 96.3

Bis(chloroethoxy)methane 94.4 80.6 94.7 86.5 84.4 99.6 130.6 110.7 93.2 97.2

2,4-Dichlorophenol 88.9 87.8 111.4 85.9 87.6 103.5 123.3 107.0 92.1 98.6

1,2,4-Trichlorobenzene 98.0 97.8 98.8 123.0 93.7 94.5 137.0 99.4 95.3 104.2

Naphthalene 101.7 97.2 123.6 113.2 102.9 129.5 *174.5 114.0 89.8 106.1

4-Chloroaniline 100.0 *150.2 *162.4 100.0 125.5 *263.6 100.0 *250.8 114.9 108.1

Hexachlorobutadiene 101.1 98.7 102.2 124.1 90.3 98.0 134.9 96.1 96.8 104.7

4-Chloro-3-methylphenol 90.4 80.2 114.7 79.0 85.2 109.8 131.6 116.2 90.1 99.7

2-Methylnaphthalene 93.2 89.9 94.6 104.1 92.2 105.9 146.2 99.1 93.3 102.1

Hexachlorocyclopentadiene 100.0 100.0 0.0 100.0 100.0 6.8 100.0 100.0 *238.3 75.8

2,4,6-Trichlorophenol 94.6 90.0 112.0 84.2 91.2 103.6 101.6 95.9 89.8 95.9

2,4,5-Trichlorophenol 84.4 91.9 109.6 96.1 80.7 103.6 108.9 83.9 87.9 94.1

2-Chloronaphthalene 100.0 91.3 93.6 97.6 93.4 98.3 106.8 93.0 92.0 96.2

2-Nitroaniline 90.0 83.4 97.4 71.3 88.4 89.9 112.1 113.3 87.7 92.6

2,6-Dinitrotoluene 83.1 90.6 91.6 86.4 90.6 90.3 104.3 84.7 90.9 90.3

Acenaphthylene 104.9 95.9 100.5 99.0 97.9 108.8 118.5 97.8 92.0 101.7

3-Nitroaniline *224.0 115.6 97.6 100.0 111.8 107.8 0.0 111.7 99.0 92.9

Acenaphthene 102.1 92.6 97.6 97.2 96.9 104.4 114.2 92.0 89.0 98.4

4-Nitrophenol 0.0 93.2 121.5 18.1 87.1 116.6 69.1 90.5 84.5 75.6

2,4-Dinitrotoluene 73.9 91.9 100.2 84.7 93.8 98.9 100.9 84.3 87.3 90.7

CD-ROM 82700 - 51 Revision 4

January 1998
TABLE 12

(continued)

Clay Loam Sand Mean

Compound Low Mid High Low Mid High Low Mid High Rec.

Dibenzofuran 89.5 91.7 109.3 98.5 92.2 j 11.4 113.8 92.7 90.4 98.8

4-Chlorophenyl phenyl 83.0 94.5 98.7 95.7 94.3 94.2 111.4 87.7 90.3 94.4

ether

Fluorene 85.2 94.9 89.2 102.0 95.5 93.8 121.3 85.7 90.9 95.4

4-Nitroaniline 77.8 114.8 94.5 129.6 103.6 95.4 *154.1 89.3 87.5 99.1

N-Nitrosodiphenylamine 82.6 96.7 93.8 92.9 93.4 116.4 97.5 110.9 86.7 96.8

4-Bromophenyl phenyl 85.6 92.9 92.8 91.1 107.6 89.4 118.0 97.5 87.1 95.8

ether

Hexachlorobenzene 95.4 91.7 92.3 95.4 93.6 83.7 106.8 94.3 90.0 93.7

Pentachlorophenol 68.2 85.9 107.7 53.2 89.8 88.1 96.6 59.8 81.3 81.2

Phenanthrene 92.1 93.7 93.3 100.0 97.8 113.3 124.4 101.0 89.9 100.6

Anthracene 101.6 95.0 93.5 92.5 101.8 118.4 . 123.0 94.5 90.6 101.2

Carbazole 94.4 99.3 96.6 105.5 96.7 111.4 115.7 83.2 88.9 99.1

Fluoranthene 109.9 101.4 94.3 111.6 96.6 109.6 123.2 85.4 92.7 102.7

Pyrene 106.5 105.8 107.6 116.7 90.7 127.5 103.4 95.5 93.2 105.2

3,3'-Dichlorobenzidine 100.0 *492.3 131.4 100.0 *217.6 *167.6 100.0 *748.8 100.0 116.5

Benzo(a)anthracene 98.1 107.0 98.4 119.3 98.6 104.0 105.0 93.4 89.3 101.5

Chrysene 100.0 108.5 100.2 116.8 93.0 117.0 106.7 93.6 90.2 102.9

Benzo(b)f1uoranthene 106.6 109.9 75.6 121.7 100.7 93.9 106.9 81.9 93.6 99.0

Benzo(k)f1uoranthene 102.4 105.2 88.4 125.5 99.4 95.1 144.7 89.2 78.1 103.1

Benzo(a)pyrene 107.9 105.5 80.8 122.3 97.7 104.6 101.7 86.2 92.0 99.9

Indeno(1,2,3-cd)pyrene 95.1 105.7 93.8 126.0 105.2 9004 133.6 82.6 91.9 102.7

Dibenz(a,h)anthracene 85.0 102.6 82.0 118.8 100.7 91.9 142.3 71.0 93.1 98.6

Benzo(g,h,OperyIene 98.0 0.0 81.2 0.0 33.6 78.6 128.7 83.0 94.2 6604

Mean 95.1 94.3 101.0 95.5 96.5 104.1 113.0 100.9 92.5

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

CD-ROM 82700 - 52 Revision 4

January 1998
TABLE 13

SINGLE LABORATORY ACCURACY AND PRECISION FOR THE EXTRACTION OF PAHs

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

Certified Value SFE Value" 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 In "l\ rv "'.1 rv n,. r.... f"\f'\\ rv ,,1= \U.L) U.L I U.U I \ I UU) u.u;';

Fluorene (15.3) 15.6 ± 1.8 (102) 11.5

Phenanthrene 15.8±1.2 16.1±1.8 102 11.2

Anthracene (1.3) 1.1 ± 0.2 (88) 18.2

Fluoranthene 23.2 ± 2.0 24.1±2.1 104 8.7

Pyrene 16.7 ± 2.0 17.2 ± 1.9 103 11.0

Benz(a)anthracene 8.7± 0.8 8.8 ± 1.0 101 11.4

Chrysene (9.2) 7.9 ± 0.9 (86) 11.4

Benzo(b)fluoranthene 7.9 ± 0.9 8.5 ± 1.1 108 12.9

Benzo(k)fluoranthene 4.4 ± 0.5 4.1 ± 0.5 91 12.2

Benzo(a)pyrene 5.3 ± 0.7 5.1 ± 0.6 96 11.8

Indeno(1,2,3-cd)pyrene 5.7 ± 0.6 5.2 ± 0.6 91 11.5

Benzo(g,h,i)perylene 4.9 ± 0.7 4.3 ± 0.5 88 11.6

Dibenz(a,h)anthracene (1.3) 1.1±0.2 (85) 18.2

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

b Values in parentheses were obtained from, or compared to, Soxhlet extraction results which were

not certified.

Data are taken from Reference 10.

CD-ROM 8270D - 53 Revision 4

January 1998
TABLE 14

SINGLE LABORATORY ACCURACY AND PRECISION FOR THE EXTRACTION OF PAHs

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

Certified Value SFE Value" Percent of SFE

Compound (mg/kg) (mg/kg) Certified Value RSD

Naphthalene 9.0 ± 0.7 7.4 ± 0.6 82 8.1

Acenaphthylene 0.3± 0.1 0.4 ± 0.1 133 25.0

Acenaphthene 4.5 ± 1.5 3.3± 0.3 73 9.0

Fluorene 13.6 ± 3.1 10.4±1.3 77 12.5

Phenanthrene 85.0 ± 20.0 86.2 ± 9.5 101 11.0

Anthracene 13.4 ± 0.5 12.1 ± 1.5 90 12.4

Fluoranthene 60.0± 9.0 54.0 ± 6.1 90 11.3

Pyrene 39.0± 9.0 '32.7 ± 3.7 84 11.3

Benz(a)anthracene 14.6 ± 2.0 12.1±1.3 83 10.7

Chrysene 14.1 ± 2.0 12.0 ± 1.3 85 10.8

Benzo(b)f1uoranthene 7.7 ± 1.2 8.4± 0.9 109 10.7

Benzo(k)f1uoranthene 2.8± 2.0 3.2 ± 0.5 114 15.6

Benzo(a)pyrene 7.4 ± 3.6 6.6 ± 0.8 89 12.1

Indeno(1,2,3-cd)pyrene 5.0 ± 2.0 4.5± 0.6 90 13.3

Benzo(g,h,i)perylene 5.4 ± 1.3 4.4 ± 0.6 82 13.6

Dibenz(a,h) anthracene 1.3 ± 0.5 1.1 ± 0.3 85 27.3

a Relative standard deviations for theSFE values are based on three replicate extractions.

Data are taken from Reference 10.

CD-ROM 82700 - 54 Revision 4

January 1998
TABLE 15

SINGLE LABORATORY ACCURACY AND PRECISION FOR THE EXTRACTION OF PAHs

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

(SFE - LIQUID TRAP)

Certified Value SFE Value" Percent of SFE

Compound (mg/kg) (mg/kg) Certified Value RSD

Naphthalene 32.4 ± 8.2 29.55 91 10.5

2-Methylnaphthalene 62.1 ± 11.5 76.13 122 2.0

Acenaphthene 632 ± 105 577.28 91 2.9

Dibenzofuran 307 ± 49 302.25 98 4.1

Fluorene 492 ± 78 427.15 87 3.0

Phenanthrene 1618 ± 340 1278.03 79 3.4

Anthracene 422 ± 49 400.80 95 2.6

Fluoranthene 1280 ± 220 1019.13 80 4.5

Pyrene 1033 ± 285 911.82 88 3.1

Benz(a)anthracene 252± 8 225.50 89 4.8

Chrysene 297 ± 26 283.00 95 3.8

Benzo(a)pyrene 97.2 ± 17.1 58.28 60 6.5

Benzo(b)fluoranthene + 153 ± 22 130.88 86 10.7

Benzo(k)fluoranthene

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

Data are taken from Reference 11.

CD-ROM 82700- 55 Revision 4

January 1998
TABLE 16

SINGLE LABORATORY RECOVERY DATA FOR SOLID-PHASE EXTRACTION OF

BASE/NEUTRAUACID EXTRACTABLES FROM SPIKED TCLP BUFFERS

LOW SPIKE LEVEL

Buffer 1 (pH = 2.886) Buffer 2 (pH =4.937)

Spike Level

Analyte (lJg/L) Recovery (%) RSD Recovery (%) RSD

1,4-Dichlorobenzene 3,750 63 10 63 9

Hexachloroethane 1,500 55 6 77 4

Nitrobenzene 1,000 82 10 100 5

Hexachlorobutadiene 250 65 3 56 4

2,4-Dinitrotoluene 65 89 4 101 5

Hexachlorobenzene 65 98 5 95 6

o-Cresol 100,000 83 10 85 5

m-Cresol* 100,000 86 8 85 3

p-Cresol* 100,000 * * * *

2,4,6-Trichlorophenol 1,000 84 12 95 12

2,4,5-Trichlorophenol 200,000 83 11 88 3

Pentachlorophenol 50,000 82 9 78 9

Results from seven replicate spiked buffer samples.

* In this study, m-cresol and p-cresol co-eluted and were quantitated as a mixture of both isomers.

Data from Reference 12.

8270D - 56 Revision 4

January 1998
TABLE 17

SINGLE LABORATORY RECOVERY DATA FOR SOLID-PHASE EXTRACTION OF

BASE/NEUTRAL/ACID EXTRACTABLES FROM SPIKED TCLP BUFFERS

HIGH SPIKE LEVEL

CD-ROM 82700 - 57 Revision 4

January 1998
TABLE 18

RECOVERY DATA FROM THREE LABORATORIES FOR SOLID-PHASE EXTRACTION

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

Buffer 1 pH = 2.886 Lab 1 Lab 2 Lab 3

Spike Level

Analyte (wg/L)* %R RSD n %R RSD n %R RSD n

o-Cresol 200,000 86 8 7 35.3 0.7 3 7.6 6 3

m-Cresol** -- 77 8 7

p-Cresol** -- -- -- -- -- -- ~- 7.7 11 3

2,4,6-Trichlorophenol 2,000 106 6 7 96.3 3.9 3 44.8 5 3

2,4,5-Trichlorophenol 400,000 93 3 7 80.5 4.5 3 63.3 11 3

Pentachlorophenol 100,000 79 2 7 33.8 12.2 3 29.2 13 3

1,4-Dichlorobenzene 7,500 51 5 7 81.3 5.3 3 19.2 7 3

Hexachloroethane 3,000 50 5 7 66.2 2.1 3 12.6 11 3

Nitrobenzene 2,000 80 8 7 76.3 5.3 3 63.9 12 3

Hexachlorobutadiene 500 53 8 7 63.3 4.8 3 9.6 9 3

2,4-Dinitrotoluene 130 89 8 7 35.7 2.6 3 58.2 17 3

Hexachlorobenzene 130 84 21 7 92.3 1.6 3 71.7 9 3

(continued)

CD"ROM 82700 - 58 Revision 4

January 1998
TABLE 18

(continued)

Buffer 2 pH =4.937 Lab 1 Lab 2 Lab 3

Spike Level

Analyte (fJg/L)* %R RSD n %R RSD n %R RSD n

o-Cresol 200,00 97 13 7 37.8 4.5 3 6.1 24 3

m-Cresol** -- 83 4 7 -- -- -- 6.0 25 3

p-Cresol**

2,4,6-Trichlorophenol 2,000 104 4 7 91.7 8.0 3 ~17.7 25 3

2,4,5-Trichlorophenol 400,000 94 4 7 85.2 0,4 3 E>4,4 10 3

Pentachlorophenol 100,000 109 11 7 41.9 28.2 3 ~16.6 32 3

1,4-Dichlorobenzene 7,500 50 5 7 79.7 1.0 3 26.5 68 3

Hexachloroethane 3,000 51 3 7 64.9 2.0 3 20.3 90 3

Nitrobenzene 2,000 80 4 7 79.0 2.3 3 ~)9,4 6 3

Hexachlorobutadiene 500 57 5 7 60 3.3 3 116.6 107 3

2,4-Dinitrotoluene 130 86 6 7 38.5 5.2 3 62.2 6 3

Hexachlorobenzene 130 86 7 7 91.3 0.9 3 75.5 5 3

* 250-mL aliquots of leachate were spiked. Lab 1 spiked at one-half these levels.

** m-Cresol and p-Cresol coelute. Lab 1 and Lab 3 reported o-Cresol and the sum of m- and p-CresoL Lab 2 reported the sum of all three

isomers of Cresol.

Data from Reference 12.

CD-ROM 82700 - 59 Revision 4

January 1998
RIC

FIGURE 1

GAS CHROMATOGRAM OF BASE/NEUTRAL AND ACID CALIBRATION STANDARD

RIC (..Ii<. 51flHS0007S6 It 2"'l TO 2788 afYIi7/~ S:2b:OO (HLl: 51~7S6 .3

St<HPLE: BASE ~ID 5TD.2\1J~:i1l4·LL

CCWS. : ~: C 1.2799~: H fl. 4.0 0LiHIi: Ii O. 1.0 J e Bi6£: U 216. 3

zsee

41:40

CD-ROM 82700- 60' Revision 4

January 1998
METHOD 82700

SEMIVOLATILE ORGANIC COMPOUNDS BY GAS CHROMATOGRAPHY/MASS

SPECTROMETRY (GC/MS)

7.1 Prepare sample

using appropriate

3500 series method.

7.2 If necessary,

cleanup extract using

appropriate 3600

series method.

7.3 Establish GC/MS

operating conditions.

Tune to DFTPP.

Perform initial

calibration.

7.4 Perform daily

calibration verification

with SPCCs and CCCs

prior to analysis of

samples.

CD-ROM

7.5.1 Screen extract

on GC/FID or GC/PID

to identify highly

contaminated samples.

Dilute those samples

as needed.

7.5.3 Analyze

extract by GC/MS.

7.6 Identify analyte

by comparing the

sample and standard

mass spectra.

7.7 Calculate

concentration of

each individual analvte

confirmed present.

Report results.

82700 - 61

7.5.4 Dilute

extract.

Revision 4

January 1998