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Method Summary

Method Source U.S. EPA Engineering and Analysis Division
Method Number1625
Revision Information40 CFR Part 136, Appendix A (Current Edition)
Method NameDescriptive Name: Semivolatiles - Base/Neutrals, Acid Extractable, GC/MS

Official Name: Semivolatile Organic Compounds by Isotope Dilution GCMS

MediaMedia: WATER
SubcategoryOrganic
Citation EPA Method Guidance CD-ROM (includes MCAWW Methods, and most current EPA Methods)
Method Download Adobe Acrobat (pdf) icon Download full method now (PDF file)
Summary of MethodStable isotopically labeled analogs of the compounds of interest are added to a 1-L wastewater sample. The sample is extracted at pH 12-13, then at pH <2 with methylene chloride using continuous extraction techniques. The extract is dried over sodium sulfate and concentrated to a volume of 1 mL. An internal standard is added to the extract and the extract is injected into the GC. The compounds are separated by GS and detected by MS. The labeled compounds serve to correct the variability of the analytical technique.
Scope and ApplicationThis method is designed to determine the semivolatile toxic organic pollutants associated with the 1976 Consent Decree and additional compounds amenable to extraction and analysis by capillary column gas chromatography-mass spectrometry (GC/MS).
Applicable Concentration RangeVaries with analyte.
Interferences(A) Artifacts: Solvents, reagents, glassware, and other sample processing hardware may yield artifacts and/or elevated baselines causing misinterpretation of chromatograms and spectra. Use of pure or purified reagents and solvent rinsed and baked glassware can minimize potential for artifacts.
(2) Matrix: Interferences coextracted from samples will vary considerably from source to source, depending on the diversity of the industrial complex or municipality being sampled.
QC RequirementsThe minimum QC requirements consist of an initial demonstration of laboratory capability, analysis of samples spiked with labeled compounds to evaluate data quality, and analysis of standards and blanks as tests of continued performance. Laboratory performance is compared against established criteria.
Sample HandlingCollect samples in glass containers. If chlorine is present, preserve with 80 mg sodium thiosulfate per liter of sample. Keep containers at 4oC during sampling and storage.
Max Holding Time7 days (sample prior to extraction); 40 days (extract)
Relative Cost/EffortGreater than $400
Sample Prep Method(s) 
 

Method Semivolatiles - Base/Neutrals, Acid Extractable, GC/MS has 177 analytes associated with it.

Analyte


Detection
Level


Bias Precision Pct False
Positive
Herbicides
(E-12839)
N/AN/AN/A 
Organochlorine pesticides
(E-12851)
N/AN/AN/A 
Organics, semivolatile
(E-12884)
N/AN/AN/A 
Volatile organic compounds
(E-12419)
N/AN/AN/A 
Pentachlorophenol
(87-86-5)
50 ug/LN/AN/A 
2-Methyl-4,6-dinitrophenol
(534-52-1)
20 ug/LN/AN/A 
4-Nitrophenol
(100-02-7)
50 ug/LN/AN/A 
2,4-Dinitrophenol
(51-28-5)
50 ug/LN/AN/A 
2,3,6-Trichlorophenol
(933-75-5)
10 ug/LN/AN/A 
2,4,5-Trichlorophenol
(95-95-4)
10 ug/LN/AN/A 
2,4,6-Trichlorophenol
(88-06-2)
10 ug/LN/AN/A 
4-Chloro-3-methylphenol
(59-50-7)
10 ug/LN/AN/A 
2,4-Dichlorophenol
(120-83-2)
10 ug/LN/AN/A 
2-Nitrophenol
(88-75-5)
20 ug/LN/AN/A 
2-Chlorophenol
(95-57-8)
10 ug/LN/AN/A 
2-Bromochlorobenzene
(694-80-4)
N/AN/AN/A 
2-(Methylthio)benzothiazole
(615-22-5)
N/AN/AN/A 
2,6-di-tert-Butyl-p-benzoquinone
(719-22-2)
N/AN/AN/A 
2-Methylbenzothiazole
(120-75-2)
N/AN/AN/A 
2-Isopropylnaphthalene
(2027-17-0)
N/AN/AN/A 
3-Chloronitrobenzene
(121-73-3)
N/AN/AN/A 
3-Bromochlorobenzene
(108-37-2)
N/AN/AN/A 
3,6-Dimethylphenanthrene
(1576-67-6)
N/AN/AN/A 
3,3'-Dimethoxybenzidine
(119-90-4)
N/AN/AN/A 
2-Methylnaphthalene
(91-57-6)
N/AN/AN/A 
1,3-Dichloro-2-propanol
(96-23-1)
N/AN/AN/A 
1,3,5-Trithiane
(291-21-4)
N/AN/AN/A 
1,3-Dinitrobenzene
(99-65-0)
N/AN/AN/A 
2,4,5-Trimethylaniline
(137-17-7)
N/AN/AN/A 
2,3-Dichloronitrobenzene
(3209-22-1)
N/AN/AN/A 
2,3-Dichloroaniline
(608-27-5)
N/AN/AN/A 
2,3-Benzofluorene
(243-17-4)
N/AN/AN/A 
1-Phenylnaphthalene
(605-02-7)
N/AN/AN/A 
1-Methylphenanthrene
(832-69-9)
N/AN/AN/A 
1-Methyl-9H-fluorene
(1730-37-6)
N/AN/AN/A 
1,5-Naphthalenediamine
(2243-62-1)
N/AN/AN/A 
1,4-Naphthoquinone
(130-15-4)
N/AN/AN/A 
1,4-Dinitrobenzene
(100-25-4)
N/AN/AN/A 
2,4-Diaminotoluene
(95-80-7)
N/AN/AN/A 
3-Nitroaniline
(99-09-2)
N/AN/AN/A 
3-Methylcholanthrene
(56-49-5)
N/AN/AN/A 
4-Aminobiphenyl
(92-67-1)
N/AN/AN/A 
4,5-Methylene phenanthrene
(203-64-5)
N/AN/AN/A 
4,4'-Methylenebis(2-chloroaniline)
(101-14-4)
N/AN/AN/A 
4-Chloro-2-nitroaniline
(89-63-4)
N/AN/AN/A 
7,12-Dimethylbenz(a)anthracene
(57-97-6)
N/AN/AN/A 
5-Nitro-o-toluidine
(99-55-8)
N/AN/AN/A 
5-Chloro-o-toluidine
(95-79-4)
N/AN/AN/A 
4-Nitrobiphenyl
(92-93-3)
N/AN/AN/A 
Acetophenone
(98-86-2)
N/AN/AN/A 
alpha-Naphthylamine
(134-32-7)
N/AN/AN/A 
Isosafrole
(120-58-1)
N/AN/AN/A 
2-Phenylnaphthalene
(612-94-2)
N/AN/AN/A 
2-Nitroaniline
(88-74-4)
N/AN/AN/A 
Aniline
(62-53-3)
N/AN/AN/A 
Benzenethiol
(108-98-5)
N/AN/AN/A 
Benzanthrone
(82-05-3)
N/AN/AN/A 
Butyl benzyl phthalate
(85-68-7)
N/AN/AN/A 
Carbazole
(86-74-8)
20 ug/LN/AN/A 
Methapyrilene
(91-80-5)
N/AN/AN/A 
Mestranol
(72-33-3)
N/AN/AN/A 
Benzyl alcohol
(100-51-6)
N/AN/AN/A 
bis(2-Chloroethoxy)methane
(111-91-1)
10 ug/LN/AN/A 
Dibenzo(a,h)anthracene
(53-70-3)
20 ug/LN/AN/A 
DBCP
(96-12-8)
N/AN/AN/A 
Crotoxyphos
(7700-17-6)
N/AN/AN/A 
Diphenyl disulfide
(882-33-7)
N/AN/AN/A 
Dimethyl sulfone
(67-71-0)
N/AN/AN/A 
Ethylenethiourea
(96-45-7)
N/AN/AN/A 
Ethyl methanesulfonate
(62-50-0)
N/AN/AN/A 
Erythritol anhydride
(1464-53-5)
N/AN/AN/A 
Dichloran
(99-30-9)
N/AN/AN/A 
Malachite green
(569-64-2)
N/AN/AN/A 
Longifolene
(475-20-7)
N/AN/AN/A 
Methyl methanesulfonate
(66-27-3)
N/AN/AN/A 
n-Dodecane
(112-40-3)
10 ug/LN/AN/A 
n-Docosane
(629-97-0)
10 ug/LN/AN/A 
N,N-Dimethylformamide
(68-12-2)
N/AN/AN/A 
n-Tetradecane
(629-59-4)
10 ug/LN/AN/A 
n-Octacosane
(630-02-4)
10 ug/LN/AN/A 
N-Nitrosopiperidine
(100-75-4)
N/AN/AN/A 
N-Nitrosomorpholine
(59-89-2)
N/AN/AN/A 
N-Nitrosomethylphenylamine
(614-00-6)
N/AN/AN/A 
N-Nitrosomethylethylamine
(10595-95-6)
N/AN/AN/A 
N-Nitrosodimethylamine
(62-75-9)
50 ug/LN/AN/A 
N-Nitrosodiethylamine
(55-18-5)
N/AN/AN/A 
N-Nitrosodi-n-propylamine
(621-64-7)
20 ug/LN/AN/A 
Indeno(1,2,3-cd)pyrene
(193-39-5)
20 ug/LN/AN/A 
Hexachloropropene
(1888-71-7)
N/AN/AN/A 
p-Nitroaniline
(100-01-6)
N/AN/AN/A 
p-Dimethylaminoazobenzene
(60-11-7)
N/AN/AN/A 
p-Chloroaniline
(106-47-8)
N/AN/AN/A 
o-Toluidine
(95-53-4)
N/AN/AN/A 
o-Cresol
(95-48-7)
N/AN/AN/A 
o-Anisidine
(90-04-0)
N/AN/AN/A 
Pentachloroethane
(76-01-7)
N/AN/AN/A 
Pentachlorobenzene
(608-93-5)
N/AN/AN/A 
Phenacetin
(62-44-2)
N/AN/AN/A 
Perylene
(198-55-0)
N/AN/AN/A 
Pentamethylbenzene
(700-12-9)
N/AN/AN/A 
Pronamide
(23950-58-5)
N/AN/AN/A 
Phenothiazine
(92-84-2)
N/AN/AN/A 
Phenol
(108-95-2)
10 ug/LN/AN/A 
N-Nitrosodi-n-butylamine
(924-16-3)
N/AN/AN/A 
n-Hexacosane
(630-01-3)
N/AN/AN/A 
Safrole
(94-59-7)
N/AN/AN/A 
Resorcinol
(108-46-3)
N/AN/AN/A 
Pyridine
(110-86-1)
N/AN/AN/A 
Thioxanthone
(492-22-8)
N/AN/AN/A 
Thioacetamide
(62-55-5)
N/AN/AN/A 
Thianaphthene
(95-15-8)
N/AN/AN/A 
Squalene
(7683-64-9)
N/AN/AN/A 
Tripropyleneglycol methyl ether
(20324-33-8)
N/AN/AN/A 
Triphenylene
(217-59-4)
N/AN/AN/A 
Aramite
(140-57-8)
N/AN/AN/A 
1,2,4,5-Tetrachlorobenzene
(95-94-3)
N/AN/AN/A 
1,2,3-Trimethoxybenzene
(634-36-6)
20 ug/LN/AN/A 
1,2,3-Trichlorobenzene
(87-61-6)
10 ug/LN/AN/A 
1,2,3,5-Tetrachlorobenzene
(634-90-2)
N/AN/AN/A 
1,2,3,4-Tetrachlorobenzene
(634-66-2)
N/AN/AN/A 
2,4-Dimethylphenol
(105-67-9)
10 ug/L97.9 % Rec (ML)14 % RSD (ML)100 ug/L
2-Chloronaphthalene
(91-58-7)
10 ug/L133.1 % Rec (ML)36.9 % RSD (ML)100 ug/L
2,6-Dinitrotoluene
(606-20-2)
10 ug/L106.2 % Rec (ML)11 % RSD (ML)100 ug/L
3,3'-Dichlorobenzidine
(91-94-1)
50 ug/L109.7 % Rec (ML)15.8 % RSD (ML)100 ug/L
1,2-Diphenylhydrazine
(122-66-7)
20 ug/L127.9 % Rec (ML)34 % RSD (ML)100 ug/L
1,2-Dichlorobenzene
(95-50-1)
10 ug/L103.8 % Rec (ML)11.4 % RSD (ML)100 ug/L
1,4-Dichlorobenzene
(106-46-7)
10 ug/L119.3 % Rec (ML)21.6 % RSD (ML)100 ug/L
1,3-Dichlorobenzene
(541-73-1)
10 ug/L114.8 % Rec (ML)20.7 % RSD (ML)100 ug/L
2,4-Dinitrotoluene
(121-14-2)
10 ug/L109.1 % Rec (ML)11.2 % RSD (ML)100 ug/L
4-Bromophenyl phenyl ether
(101-55-3)
10 ug/L82.1 % Rec (ML)21.1 % RSD (ML)100 ug/L
4-Chlorophenylphenyl ether
(7005-72-3)
10 ug/L112.5 % Rec (ML)17.5 % RSD (ML)100 ug/L
Acenaphthene
(83-32-9)
10 ug/L102.8 % Rec (ML)10.2 % RSD (ML)100 ug/L
Acenaphthylene
(208-96-8)
10 ug/L114.8 % Rec (ML)18.5 % RSD (ML)100 ug/L
alpha-Picoline
(109-06-8)
50 ug/L95 % Rec (ML)17.6 % RSD (ML)100 ug/L
Benzo(a)anthracene
(56-55-3)
10 ug/L105.7 % Rec (ML)14.7 % RSD (ML)100 ug/L
Benzo(g,h,i)perylene
(191-24-2)
20 ug/L107.8 % Rec (ML)12.8 % RSD (ML)100 ug/L
Benzo(b)fluoranthene
(205-99-2)
10 ug/L142.2 % Rec (ML)54.6 % RSD (ML)100 ug/L
Benzo(k)fluoranthene
(207-08-9)
10 ug/L92.2 % Rec (ML)15.2 % RSD (ML)100 ug/L
alpha-Terpineol
(98-55-5)
10 ug/L101 % Rec (ML)22.4 % RSD (ML)100 ug/L
Benzidine
(92-87-5)
50 ug/L101.2 % Rec (ML)59.6 % RSD (ML)100 ug/L
Benzo(a)pyrene
(50-32-8)
10 ug/L112 % Rec (ML)19.1 % RSD (ML)100 ug/L
bis(2-Chloroethyl) ether
(111-44-4)
10 ug/L105.6 % Rec (ML)20.6 % RSD (ML)100 ug/L
bis(2-Chloroisopropyl) ether
(108-60-1)
10 ug/L105.8 % Rec (ML)9.1 % RSD (ML)100 ug/L
bis(2-Ethylhexyl) phthalate
(117-81-7)
10 ug/L124.6 % Rec (ML)19.6 % RSD (ML)100 ug/L
Biphenyl
(92-52-4)
10 ug/L105.3 % Rec (ML)13.2 % RSD (ML)100 ug/L
beta-Naphthylamine
(91-59-8)
50 ug/L127.3 % Rec (ML)61.5 % RSD (ML)100 ug/L
Di-n-butyl phthalate
(84-74-2)
10 ug/L112.7 % Rec (ML)11.7 % RSD (ML)100 ug/L
Di-n-octyl phthalate
(117-84-0)
10 ug/L112 % Rec (ML)12.5 % RSD (ML)100 ug/L
Dibenzothiophene
(132-65-0)
10 ug/L109.3 % Rec (ML)12.9 % RSD (ML)100 ug/L
Dibenzofuran
(132-64-9)
10 ug/L107.6 % Rec (ML)9 % RSD (ML)100 ug/L
Chrysene
(218-01-9)
10 ug/L106.2 % Rec (ML)23.8 % RSD (ML)100 ug/L
Diethyl phthalate
(84-66-2)
10 ug/L122.4 % Rec (ML)19.1 % RSD (ML)100 ug/L
Dimethyl phthalate
(131-11-3)
10 ug/L119.5 % Rec (ML)17.2 % RSD (ML)100 ug/L
Diphenylamine
(122-39-4)
20 ug/L110.8 % Rec (ML)20.6 % RSD (ML)100 ug/L
Diphenyl ether
(101-84-8)
10 ug/L105.6 % Rec (ML)8.9 % RSD (ML)100 ug/L
Fluorene
(86-73-7)
10 ug/L103.5 % Rec (ML)12 % RSD (ML)100 ug/L
Fluoranthene
(206-44-0)
10 ug/L113 % Rec (ML)16.9 % RSD (ML)100 ug/L
n-Decane
(124-18-5)
10 ug/L71.7 % Rec (ML)36.8 % RSD (ML)100 ug/L
n-Eicosane
(112-95-8)
10 ug/L122.1 % Rec (ML)29.8 % RSD (ML)100 ug/L
n-Tetracosane
(646-31-1)
10 ug/L105.7 % Rec (ML)8.4 % RSD (ML)100 ug/L
n-Octadecane
(593-45-3)
10 ug/L120.8 % Rec (ML)42.1 % RSD (ML)100 ug/L
N-Nitrosodiphenylamine
(86-30-6)
20 ug/L96.2 % Rec (ML)11.9 % RSD (ML)100 ug/L
Hexachlorobenzene
(118-74-1)
10 ug/L106.1 % Rec (ML)6.3 % RSD (ML)100 ug/L
Hexachlorobutadiene
(87-68-3)
10 ug/L116 % Rec (ML)29.1 % RSD (ML)100 ug/L
Hexachlorocyclopentadiene
(77-47-4)
10 ug/L100 % Rec (ML)7.9 % RSD (ML)100 ug/L
Hexachloroethane
(67-72-1)
10 ug/L159.4 % Rec (ML)68.1 % RSD (ML)100 ug/L
Isophorone
(78-59-1)
10 ug/L109.7 % Rec (ML)13.2 % RSD (ML)100 ug/L
p-Cymene
(99-87-6)
10 ug/L103.4 % Rec (ML)10.1 % RSD (ML)100 ug/L
Nitrobenzene
(98-95-3)
10 ug/L105.3 % Rec (ML)7.3 % RSD (ML)100 ug/L
Phenanthrene
(85-01-8)
10 ug/L105 % Rec (ML)5.4 % RSD (ML)100 ug/L
Pyrene
(129-00-0)
10 ug/L107.6 % Rec (ML)11.6 % RSD (ML)100 ug/L
n-Hexadecane
(544-76-3)
10 ug/L114.6 % Rec (ML)14.2 % RSD (ML)100 ug/L
n-Triacontane
(638-68-6)
10 ug/L112.5 % Rec (ML)20.9 % RSD (ML)100 ug/L
Naphthalene
(91-20-3)
10 ug/L106.1 % Rec (ML)10.4 % RSD (ML)100 ug/L
Styrene
(100-42-5)
10 ug/L111 % Rec (ML)24.3 % RSD (ML)100 ug/L
1,2,4-Trichlorobenzene
(120-82-1)
10 ug/L105.7 % Rec (ML)8.8 % RSD (ML)100 ug/L
Anthracene
(120-12-7)
10 ug/L102.3 % Rec (ML)21 % RSD (ML)100 ug/L
export_analytes
Precision Descriptor NotesSummarized data results are based on quantification by isotope dilution. Precision and accuracy data were obtained from "Interlaboratory Validation of U.S. Environmental Protection Agency Method 1625A" (July 1984). Study data were collected for samples analyzed at 11-13 laboratories, depending on compounds. Approximately twenty-three percent of laboratories could not quantify or detect compounds by isotope dilution, so these laboratories were excluded from method summaries (the need for these exclusions was primarily based on lack of experience with the method at the time of the 1984 study).
Detection Level Note(1) The values given are the minimum level at which the entire GC/MS system must give recognizable mass spectra (background corrected) and acceptable calibration points.
(2) The values given refer to one of three techniques for each compound: internal standard quantification, labeled compound quantification, and isotope dilution quantification. Consult Table 3 of the method for information on specific compounds.
 
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