NOAA NST: 130.30: Organic contaminants in marine sediments by GC-MS

Summary
Analytes
Revision
Data and Sites

Official Method Name

Gas chromatography mass spectrometry (GC-MS) analysis for organic contaminates in marine sediments.

Current Revision

March 1998

Media

SOILS/SEDIMENT

Instrumentation

Gas Chromatography with Mass Spectrometry 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

Polycyclic aromatic hydrocarbons (PAH), PCDDs, and PCDFs can be determined at low concentrations by mass spectrometry due to their strong molecular ion response. Therefore, GC/MS in the selected ion monitoring mode provides unambiguous and sensitive detection for these compounds. The availability of labeled surrogates internal standards of many of the analytes makes very accurate determinations of analyte concentrations possible. Quantitation was performed by gas chromatography mass spectrometry (GC/MS) in the selected ion monitoring (SIM) mode. Silica gel/alumina cleanup with activated copper is used to remove interfering materials from the sample prior to analysis.

Scope and Application

The quantitative method described in this document was used to determine polycyclic aromatic hydrocarbons (PAH) and their alkylated homologues in extracts of sediments. This method also provides procedures for the detection and quantitative measurement of polychlorinated dibenzo-p-dioxins (tetra- through octa-chlorinated homologues; PCDDs) and polychlorinated dibenzofurans (tetra- through octa-chlorinated homologues; PCDFs) in sediments at pg/g concentrations.

Applicable Concentration Range

1 - 1000 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 are as follows: Method blank. Laboratory blank spike. Ongoing precision and recovery analyses. Matrix spike. Duplicates. Reference material (NIST SRM 1944) analyses. Labeled compound recovery.

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

Greater than $400

Sample Preparation Methods

NOAA TM #130

This method has 43 analytes associated with it.

Analyte	Detection Level	Bias	Precision
1,2,3,4,6,7,8-Heptachlorodibenzo-p-dioxin(35822-46-9) 1,2,3,4,6,7,8-HEPTACHLORODIBENZODIOXIN 1,2,3,4,6,7,8-Heptachlorodibenzo-p-dioxin 1,2,3,4,6,7,8-HpCDD Dibenzo[b,e][1,4]dioxin, 1,2,3,4,6,7,8-heptachloro-	1.000 ng/g	N/A	N/A
1,2,3,4,6,7,8-Heptachlorodibenzofuran(67562-39-4) 1,2,3,4,6,7,8-Heptachlorodibenzofuran 1,2,3,4,6,7,8-HpCDF	1.000 ng/g	N/A	N/A
1,2,3,4,7,8,9-Heptachlorodibenzofuran(55673-89-7) 1,2,3,4,7,8,9-Heptachlorodibenzofuran 1,2,3,4,7,8,9-HpCDF	1.000 ng/g	N/A	N/A
1,2,3,4,7,8-Hexachlorodibenzo-p-dioxin(39227-28-6) 1,2,3,4,7,8-Hexachlorodibenzo-p-dioxin 1,2,3,4,7,8-Hexachlorodibenzo[1,4]dioxin 1,2,3,4,7,8-HxCDD Dibenzo[b,e][1,4]dioxin, 1,2,3,4,7,8-hexachloro- Hexachlorodibenzo(b,e)(1,4)dioxin,1,2,3,4,7,8-	1.000 ng/g	N/A	N/A
1,2,3,4,7,8-Hexachlorodibenzofuran(70648-26-9) 1,2,3,4,7,8-Hexachlorodibenzofuran 1,2,3,4,7,8-HxCDF Dibenzofuran, 1,2,3,4,7,8-hexachloro-	1.000 ng/g	N/A	N/A
1,2,3,6,7,8-Hexachlorodibenzo-p-dioxin(57653-85-7) 1,2,3,6,7,8-Hexachlorodibenzo-p-dioxin 1,2,3,6,7,8-HxCDD	1.000 ng/g	N/A	N/A
1,2,3,6,7,8-Hexachlorodibenzofuran(57117-44-9) 1,2,3,6,7,8-Hexachlorodibenzofuran 1,2,3,6,7,8-HxCDF	1.000 ng/g	N/A	N/A
1,2,3,7,8,9-Hexachlorodibenzo-p-dioxin(19408-74-3) 1,2,3,7,8,9-Hexachlorodibenzo-p-dioxin 1,2,3,7,8,9-HxCDD Hexachlorodibenzo-p-dioxin, mixture Hexachlorodibenzo-p-dioxin,123789	1.000 ng/g	N/A	N/A
1,2,3,7,8,9-Hexachlorodibenzofuran(72918-21-9) 1,2,3,7,8,9-Hexachlorodibenzofuran 1,2,3,7,8,9-HxCDF	1.000 ng/g	N/A	N/A
1,2,3,7,8-Pentachlorodibenzo-p-dioxin(40321-76-4) 1,2,3,7,8-PeCDD 1,2,3,7,8-PeDD 1,2,3,7,8-Pentachlorodibenzo-p-dioxin 1,2,3,7,8-Pentachlorodibenzodioxin	1.000 ng/g	N/A	N/A
1,2,3,7,8-Pentachlorodibenzofuran(57117-41-6) 1,2,3,7,8-PeCDF 1,2,3,7,8-Pentachlorodibenzofuran	1.000 ng/g	N/A	N/A
1,2-Dichloropropane(78-87-5) 1,2-Dichloropropane Dichloropropane,alpha,beta- Nemex Propane, 1,2-dichloro- Propylene chloride Propylene dichloride	1.000 ng/g	N/A	N/A
1,6,7-Trimethylnaphthalene(2245-38-7) 1,6,7-Trimethylnaphthalene 2,3,5-Trimethylnaphthalene Naphthalene, 1,6,7-Trimethyl	0.400 ng/g	N/A	N/A
1-Methylphenanthrene(832-69-9) 1-Methylphenanthrene Phenanthrene, 1-methyl-	1.000 ng/g	N/A	N/A
2,3,4,6,7,8-Hexachlorodibenzofuran(60851-34-5) 2,3,4,6,7,8-Hexachlorodibenzofuran 2,3,4,6,7,8-HxCDF	1.000 ng/g	N/A	N/A
2,3,4,7,8-Pentachlorodibenzofuran(57117-31-4) 2,3,4,7,8-PeCDF 2,3,4,7,8-Pentachlorodibenzofuran Pentachlorodibenzofurans	1.000 ng/g	N/A	N/A
2,3,7,8-Tetrachlorodibenzo-p-dioxin(1746-01-6) 2,3,7,8-TCDD 2,3,7,8-Tetrachlorodibenzo-p-dioxin Dibenzo-p-dioxin, 2,3,7,8-tetrachloro- Dibenzo[b,e][1,4]dioxin, 2,3,7,8-tetrachloro- Dioxin Tetrachlorodibenzo-1,4-dioxin,2,3,7,8-	1.000 ng/g	N/A	N/A
2,3,7,8-Tetrachlorodibenzofuran(51207-31-9) 2,3,7,8-TCDF 2,3,7,8-Tetrachlorodibenzofuran Dibenzofuran, 2,3,7,8-tetrachloro-	1.000 ng/g	N/A	N/A
2,6-Dimethylnaphthalene(581-42-0) 2,6-Dimethylnaphthalene	0.600 ng/g	N/A	N/A
2-Methylnaphthalene(91-57-6) 2-Methylnaphthalene Naphthalene, 2-methyl beta-Methylnaphthalene	0.700 ng/g	N/A	N/A
Acenaphthene(83-32-9) 1,2-Dihydroacenaphthylene 1,8-Ethylenenaphthalene Acenaphthene Acenaphthene,1,2-dihydro- Acenaphthylene, 1,2-dihydro- Periethylenenaphthalene	0.500 ng/g	N/A	N/A
Acenaphthylene(208-96-8) Acenaphthalene Acenaphthylene Cyclopenta(de)naphthalene	0.300 ng/g	N/A	N/A
Anthracene(120-12-7) Anthracene Anthracin Green oil Paranaphthalene Tetra olive n2g	2.300 ng/g	N/A	N/A
Benz[a]anthracene(56-55-3) 1,2-Benzanthracene 2,3-Benzphenanthrene Benz[a]anthracene Benzanthrene Benzo(a)anthracene Benzoanthracene Naphthanthracene Tetraphene	0.200 ng/g	N/A	N/A
Benzo(a)pyrene(50-32-8) 3,4-Benzopyrene 3,4-Benzpyrene BP BaP Benzo(a)pyrene Benzo[a]pyrene	0.300 ng/g	N/A	N/A
Benzo(b)fluoranthene(205-99-2) 2,3-Benzofluoranthene 3,4-Benzfluoranthene 3,4-Benzofluoranthene B(b)F Benz[e]acephenanthrylene Benzo(b)fluoranthene Benzo(e)fluoranthene Benzo[b]fluoranthene	0.300 ng/g	N/A	N/A
Benzo(g,h,i)perylene(191-24-2) 1,12-Benzoperylene 1,12-Benzperylene B(ghi)P Benzo(g,h,i)perylene Benzo(ghi)perylene	1.300 ng/g	N/A	N/A
Benzo(k)fluoranthene(207-08-9) 11,12-Benzofluoranthene B(k)F Benz(k)fluoranthene Benzo(k)fluoranthene	0.300 ng/g	N/A	N/A
Benzo[e]pyrene(192-97-2) 2,3-Benzofluoranthene 3,4-Benzfluoranthene 4,5-Benzopyrene B[E]P Benzo[e]pyrene	0.200 ng/g	N/A	N/A
Biphenyl(92-52-4) 1,1'-Biphenyl Bibenzene Biphenyl Diphenyl Phenylbenzene	0.300 ng/g	N/A	N/A
Chrysene(218-01-9) 1,2,5,6-Dibenzonaphthalene 1,2-Benzophenanthrene 1,2-Benzphenanthrene Benz(a)phenanthrene Benzo(a)phenanthrene Chrysene	0.300 ng/g	N/A	N/A
Dibenzo(a,h)anthracene(53-70-3) 1,2:5,6-Dibenzanthracene DB(a,h)A Dibenz(a,h)anthracene Dibenzo(a,h)anthracene	0.400 ng/g	N/A	N/A
Fluoranthene(206-44-0) 1,2-Benzacenaphthene Benzo(j,k)fluorene Fluoranthene Idryl	0.300 ng/g	N/A	N/A
Fluorene(86-73-7) 2,2'-Methylenebiphenyl 9H-Fluorene Diphenylenemethane Fluorene o-Biphenylenemethane	0.500 ng/g	N/A	N/A
Indeno(1,2,3-cd)pyrene(193-39-5) 1,10-(1,2-Phenylene)pyrene 2,3-Phenylenepyrene Indeno(1,2,3-cd)pyrene o-Phenylenepyrene	0.300 ng/g	N/A	N/A
Naphthalene(91-20-3) Moth balls Naphthalene Naphthalin Naphthene Tar camphor White tar	1.100 ng/g	N/A	N/A
Octachlorodibenzo-p-dioxin(3268-87-9) 1,2,3,4,6,7,8,9-Octachlorodibenzo-p-dioxin Dibenzo-p-dioxin, octachloro- Dibenzo[b,e][1,4]dioxin, octachloro- OCDD Octachlorodibenzo-p-dioxin Octachlorodibenzo-p-dioxins	1.000 ng/g	N/A	N/A
Organics, semivolatile(E-12884) Organics, semivolatile Semi-volatile organics Semivolatile organics	N/A	N/A	N/A
PAHs(130498-29-2) Aromatic hydrocarbons, polycyclic PAH PAH's PAHs PNA's Polycyclic organic matter Polynuclear aromatic hydrocarbons	0.400 ng/g	N/A	N/A
Perylene(198-55-0) Dibenz(de,k)anthracene Dibenz(de,kl)anthracene Perylene peri-Dinaphthalene	0.400 ng/g	N/A	N/A
Phenanthrene(85-01-8) Phenanthrene Phenathrin	0.600 ng/g	N/A	N/A
Pyrene(129-00-0) Benzo[def]phenanthrene Pyrene Pyrene[def]phenanthrene	0.400 ng/g	N/A	N/A
Volatile organic compounds(E-12419) Organic compounds, volatile VOCs Volatile organic compounds	N/A	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 1994 volume 49, number 209:1

Revision	PDF/Link
March 1998

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NOAA NST: 130.30: Organic contaminants in marine sediments by GC-MS

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