Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of semivolatile organic compounds in bottom sediment by solvent extraction, gel permeation chromatographic fractionation, and capillary-column gas chromatography/mass spectrometry

Furlong, E. T.; Vaught, D. G.; Merten, L. M.; Foreman, W. T.; Gates, P. M.

Abstract:

A method for the determination of 79 semivolatile organic compounds (SOCs) and 4 surrogate compounds in soils and bottom sediment is described. The SOCs are extracted from bottom sediment by solvent extraction, followed by partial isolation using high-performance gel permeation chromatography (GPC). The SOCs then are qualitatively identified and quantitative concentrations determined by capillary-column gas chromatography/mass spectrometry (GC/MS). This method also is designed for an optional simultaneous isolation of polychlorinated biphenyls (PCBs) and organochlorine (OC) insecticides, including toxaphene. When OCs and PCBs are determined, an additional alumina- over-silica column chromatography step follows GPC cleanup, and quantitation is by dual capillary- column gas chromatography with electron-capture detection (GC/ECD). Bottom-sediment samples are centrifuged to remove excess water and extracted overnight with dichloromethane. The extract is concentrated, centrifuged, and then filtered through a 0.2-micrometer polytetrafluoro-ethylene syringe filter. Two aliquots of the sample extract then are quantitatively injected onto two polystyrene- divinylbenzene GPC columns connected in series. The SOCs are eluted with dichloromethane, a fraction containing the SOCs is collected, and some coextracted interferences, including elemental sulfur, are separated and discarded. The SOC-containing GPC fraction then is analyzed by GC/MS. When desired, a second aliquot from GPC is further processed for OCs and PCBs by combined alumina-over-silica column chromatography. The two fractions produced in this cleanup then are analyzed by GC/ECD. This report fully describes and is limited to the determination of SOCs by GC/MS.

Genre:

USGS Numbered Series

ProdID:

21945

Citation Author:

Furlong, E. T.; Vaught, D. G.; Merten, L. M.; Foreman, W. T.; Gates, P. M.

Citation Contributing Office:

Citation Datum:

Citation Day:

Citation Edition:

Citation Editor:

Citation End Page:

Citation Issue:

Citation Keywords:

Citation Language:

ENGLISH

Citation Larger Work Title:

Citation LatN:

Citation LatS:

Citation LonE:

Citation LonW:

Citation Month:

Citation No Pagination:

Citation Number Of Pages:

Citation Online Only Flag:

Citation Phsyical Description:

vi, 67 p. :ill. ;28 cm.

Citation Projection:

Citation Public Comments:

Citation Publisher:

U.S. Geological Survey : Open-File Reports Section/ESIC [distributor],

Citation Series:

Open-File Report

Citation Series Code:

OFR

Citation Series Number:

95-719

Citation Search Results Text:

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of semivolatile organic compounds in bottom sediment by solvent extraction, gel permeation chromatographic fractionation, and capillary-column gas chromatography/mass spectrometry; 1996; OFR; 95-719; Furlong, E. T.; Vaught, D. G.; Merten, L. M.; Foreman, W. T.; Gates, P. M.