NOAA NST: 130.10: Organic contaminants in marine sediments by GC-ECD

Summary
Analytes
Revision
Data and Sites

Official Method Name

Gas chromatography electron capture detector (GC-ECD) analysis for organic contaminates in marine sediments.

Current Revision

March 1998

Media

SOILS/SEDIMENT

Instrumentation

Gas Chromatography with Electron Capture Detection

Method Subcategory

Organic

Method Source

NOAA NST

Citation

Sampling and Analytical Methods of the National Status and Trends Program Mussel Watch Project: 1993-1996 Update.
NOAA Technical Memorandum NOS ORCA 130. March 1998. Silver Spring, MD. 233pp.

Brief Method Summary

Chlorinated hydrocarbons are quantitatively determined by gas chromatography with an electron capture detector (ECD). The ECD is very sensitive and allows for detection of the chlorinated hydrocarbons at trace concentrations (ppb) in marine sediments. Silica gel/alumina cleanup with activated copper is used to remove interfering materials from the sample prior to analysis.

Scope and Application

This method quantitatively determines chlorinated pesticides and PCBs in soils and sediments using GC/ECD.

Applicable Concentration Range

5 to 200 ng/g

Interferences

Method interferences may be caused by contaminants in solvents, reagents, glassware, and other sample processing hardware, and lead to false positives during instrumental analysis. All materials used in this method are routinely demonstrated to be free from interferences by processing procedural blanks identical to samples (one blank per 20 samples or each batch whichever is more frequent). Matrix interferences result from co-extraction of compounds other than the analytes of interest. Elemental sulfur and naturally occurring lipids can cause interferences in the analysis of sediment extracts.

Quality Control Requirements

The quality assurance / quality control requirements were as follows: Initial calibration and continuing calibration checks. Method blank analysis. Surrogate compound analysis. Matrix spike analysis. Reference sample analysis.

Sample Handling

Collect samples in a glass container and store in the dark at or below -20 deg. C. Store extracts in the dark at 4 deg. C.

Maximum Holding Time

6 months (frozen)

Relative Cost

$201 to $400

Sample Preparation Methods

NOAA TM #130

This method has 32 analytes associated with it.

Analyte	Detection Level	Bias	Precision
2,2',3,3',4,4',5,5',6,6'-Decachlorobiphenyl(2051-24-3) 2,2',3,3',4,4',5,5',6,6'-Decachlorobiphenyl Decachlorobiphenyl	1.000 ng/g	N/A	N/A
2,2',3,3',4,4',5,5',6-Nonachlorobiphenyl(40186-72-9) 2,2',3,3',4,4',5,5',6-Nonachlorobiphenyl PCB 206	1.000 ng/g	N/A	N/A
2,2',3,3',4,4',5,6-Octachorobiphenyl(52663-78-2) 2,2',3,3',4,4',5,6-Octachorobiphenyl PCB 195	1.000 ng/g	N/A	N/A
2,2',3,3',4,4',5-Heptachlorobiphenyl(35065-30-6) 2,2',3,3',4,4',5-Heptachlorobiphenyl PCB 170	1.000 ng/g	N/A	N/A
2,2',3,3',4,4'-Hexachlorobiphenyl(38380-07-3) 2,2',3,3',4,4'-Hexachlorobiphenyl 2,2',3,3',4,4'-PCB PCB 128	1.000 ng/g	N/A	N/A
2,2',3,4',5,5',6-Heptachlorobiphenyl(52663-68-0) 1,1'-Biphenyl, 2,2',3,4,5,5',6-heptachloro- 2,2',3,4',5,5',6-Heptachlorobiphenyl PCB 187	1.000 ng/g	N/A	N/A
2,2',3,4,4',5'-Hexachlorobiphenyl(35065-28-2) 2,2',3,4,4',5'-Hexachlorobiphenyl PCB 138	1.000 ng/g	N/A	N/A
2,2',3,5'-Tetrachlorobiphenyl(41464-39-5) 2,2',3,5'-Tetrachlorobiphenyl PCB 44	1.000 ng/g	N/A	N/A
2,2',4,4',5,5'-Hexachlorobiphenyl(35065-27-1) 2,2',4,4',5,5'-Hexachlorobiphenyl 2,2',4,4',5,5'-hexachloro-1,1'-Biphenyl 2,4,5,2',4',5'-PCB 2,4,5,2',4',5'-hexachlorobiphenyl PCB 153	1.000 ng/g	N/A	N/A
2,2',4,5,5'-Pentachlorobiphenyl(37680-73-2) 2,2',4,5,5'-Pentachlorobiphenyl 2,4,5,2',5'-PCB PCB 101	1.000 ng/g	N/A	N/A
2,2',5,5'-Tetrachlorobiphenyl(35693-99-3) 2,2',5,5'-PCB 2,2',5,5'-Tetrachlorobiphenyl 2,2',5,5'-tetrachloro-1,1'-Biphenyl PCB 52	1.000 ng/g	N/A	N/A
2,2',5-Trichlorobiphenyl(37680-65-2) 2,2',5-Trichlorobiphenyl	1.000 ng/g	N/A	N/A
2,3',4,4',5-Pentachlorobiphenyl(31508-00-6) 2',3,4,4',5'-PCB 2,3',4,4',5-Pentachlorobiphenyl PCB 118	1.000 ng/g	N/A	N/A
2,3',4,4'-Tetrachlorobiphenyl(32598-10-0) 2,3',4,4'-PCB 2,3',4,4'-Tetrachlorobiphenyl PCB 66	1.000 ng/g	N/A	N/A
2,3,3',4,4'-Pentachlorobiphenyl(32598-14-4) 2,3,3',4,4' PCB 2,3,3',4,4'-Pentachlorobiphenyl PCB 105	1.000 ng/g	N/A	N/A
2,4' -DDD(53-19-0) 1,1-Dichloro-2,2-bis(2,4'-dichlorophenyl)ethane 1,1-Dichloro-2-(o-chlorophenyl)-2-(p-chlorophenyl)ethane 2,4' -DDD 2,4'-Dichlorodiphenyldichloroethane o,p'-DDD o,p'-TDE	0.600 ng/g	N/A	N/A
2,4'-DDE(3424-82-6) 1,1-Dichloro-2-(o-chlorophenyl)-2-(p-chlorophenyl) ethylene 1-chloro-2-(2,2-dichloro-1-(4-chlorophenyl)ethenyl)benzene 2,4'-DDE o,p'-DDE	0.300 ng/g	N/A	N/A
2,4'-Dichlorobiphenyl(34883-43-7) 2,4'-Dichlorobiphenyl 2,4'-PCB	1.000 ng/g	N/A	N/A
2,4,4'-Trichlorobiphenyl(7012-37-5) 2,4,4'-PCB 2,4,4'-Trichlorobiphenyl PCB 28	1.000 ng/g	N/A	N/A
3,3',4,4',5-Pentachlorobiphenyl(57465-28-8) 1,1'-Biphenyl, 3,3',4,4',5-pentachloro- 3,3',4,4',5-Pentachlorobiphenyl PCB 126	1.000 ng/g	N/A	N/A
3,3',4,4'-Tetrachlorobiphenyl(32598-13-3) 3,3',4,4'-PCB 3,3',4,4'-Tetrachlorobiphenyl 3,3',4,4'-tetrachloro-1,1'-Biphenyl PCB 77	1.000 ng/g	N/A	N/A
4,4'-DDD(72-54-8) 1,1-Dichloro-2,2-bis(p-chlorophenyl)ethane 4,4'-DDD Benzene, 1,1'-(2,2-dichloroethylidene)bis[4-ch Benzene, 1,1'-(2,2-dichloroethylidene)bis[4-chloro- Dichloro-2,2-bis(p-chlorophenyl)ethane,1,1- Dichlorodiphenyldichloroethane Ethane, 1,1-dichloro-2,2-bis(p-chlorophenyl)- Rhothane TDE Tetrachlorodiphenylethane p,p'-DDD p,p'-Dichlorodiphenyl dichloroethane p,p'-TDE	0.110 ng/g	N/A	N/A
4,4'-DDE(72-55-9) 1,1'-(-Dichloroethenylidene)bis(4-chlorobenzene) 4,4'-DDE 4,4'-DDE, DDT, DDD Benzene, 1,1'-(dichloroethenylidene)bis[4-chlo Benzene, 1,1'-(dichloroethenylidene)bis[4-chloro- Ethylene, 1,1-dichloro-2,2-bis(p-chlorophenyl)- bis(p-Chlorophenyl)-1,1-dichloroethylene,2,2- p,p'-DDE p,p'-Dichlorodiphenyldichloroethylene	0.060 ng/g	N/A	N/A
Aldrin(309-00-2) Aldrex Aldrin Aldrin-R Aldrite Aldrosol HHDN Hexachlorohexahydro-endo-exo-dimethanonaphthalene Octalene Seedrin liquid	0.040 ng/g	N/A	N/A
Dieldrin(60-57-1) 1,2,3,4,10,10-Hexachloro-6,7-epoxy-1,4,4a,5, 6 1,2,3,4,10,10-Hexachloro-6,7-epoxy-1,4,4a,5, 6,7,8, ... 2,7:3,6-Dimethanonaphth(2,3-b)oxirene, 3,4,5,6 2,7:3,6-Dimethanonaphth(2,3-b)oxirene, 3,4,5,6,9,9- ... Alvit Dieldrin Dieldrin (hexachloroepoxyoctahydro-endo,exo- ... Dieldrin/aldrin Dimethanonaphthalene, 1,2,3,4,10,10-hexachloro-6,7- ... Heod Octalox	0.040 ng/g	N/A	N/A
Endrin(72-20-8) 2,7:3,6-Dimethanonaphth[2,3-b]oxirene, 3,4,5,6,9,9- ... 3,4,5,6,9,9-Hexachloro-1a,2,2a,3,6,6a,7,7a-oct 3,4,5,6,9,9-Hexachloro-1a,2,2a,3,6,6a,7,7a-octahydro ... Compound 269 Endrin Hexachloroepoxyoctahydro-endo,endo-dimethanonaphthalene Hexadrin Mendrin Nendrin	0.800 ng/g	N/A	N/A
Heptachlor(76-44-8) 1,4,5,6,7,8,8-Heptachlorotetrahydro-4,7-methanoindene Drinox Heptachlor Heptachlor [1,4,5,6,7,8,8-heptachloro-3a,4,7,7a- ... Heptachlor/Heptachlor epoxide (SARA 110) Heptachlorodicyclopentadiene Heptagran Heptamul Velsicol-104	0.050 ng/g	N/A	N/A
Heptachlor epoxide(1024-57-3) Heptachlor epoxide Velsicol 53-CS-17 Vesicol 53-CS-17	0.570 ng/g	N/A	N/A
Organochlorine pesticides(E-12851) Organochlorine pesticides Pesticides, organochlorine	N/A	N/A	N/A
PCBs(1336-36-3) 1,1'-Biphenyl, chloro derivs. Aroclors PCB PCBs Polychlorinated biphenyl Polychlorinated biphenyl, NOS Polychlorinated biphenyls Polychlorobiphenyl	0.050 ng/g	N/A	N/A
alpha-Chlordane(5103-71-9) 4,7-Methano-1H-indene 1,2,4,5,6,7,8,8-octachlo Methanoindan, 1-alpha,2-alpha,4-beta,5,6,7-beta,8,8- ... Methanoindan,alpha-1,2,4,5,6,7,8,8-octachloro-3a- ... alpha-Chlordane cis-4,7-Methano-1H-indene 1,2,4,5,6,7,8,8-octachloro ... cis-Chlordane	0.040 ng/g	N/A	N/A
p,p'-DDT(50-29-3) 1,1,1-Trichloro-2,2-bis(p-chlorophenyl)ethane 4,4'-DDT Benzene, 1,1'-(2,2,2-trichloroethylidene)bis[4-chloro- Chlorophenothane DDT Dichlorodiphenyltrichloroethane Ethane, 1,1,1-trichloro-2,2-bis(p-chlorophenyl)- bis(p-Chlorophenyl)-2,2,2-trichloroethane,1,1- p,p'-DDT p,p'-Dichlorodiphenyltrichloroethane	0.080 ng/g	N/A	N/A

Precision Descriptor Notes:	Precision and accuracy data were obtained from NOAA's NS&T interlaboratory validation QA program. NOAA Technical memorandum NOS ORCA 138 "National Status and Trends Program for Marine Environmental Quality, NIST/NOAA NS&T Intercomparison Exercise Program for Organic Contaminants in the Marine Envoronment Description and Results of 1998 Organic Intercomparison Exercises".
Detection Level Note:	Federal Register (1984), Vol. 49, No. 209: 198-199

Revision	PDF/Link
March 1998

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NOAA NST: 130.10: Organic contaminants in marine sediments by GC-ECD

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