Sample preparation for analyzing polycyclic aromatic hydrocarbons and polychlorinated dibenzo-p-dioxins and dibenzofurans in sediment by gas chromatography/mass spectrometry

Journal Article · Wed Dec 01 00:00:00 EST 1993 · Estuaries; (United States)

DOI:https://doi.org/10.2307/1352590· OSTI ID:7035058

Tan, Y L; Kong, Ada; Chiu, Yue-On ^[1]

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1. Department of Energy, New York, NY (United States)

A sample preparation technique was developed to isolate and separate two classes of combustion-produced pollutants: three- to six-ring polycyclic aromatic hydrocarbons (PAH) and polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/F), from sediment samples for interference-free analyses by gas chromatography/mass spectrometry (GC/MS). The method involves soxhlet extraction with methylene chloride, sulfur removal with activated copper powder, gel filtration chromatography with Sephadex LH-20, polarity separation of PAH and PCDD/F with prepacked silica gel solid-phase extraction columns, and isolation of PCDD/F from polychlorinated biphenyls with microalumina columns. Stringent procedural controls were established to achieve clean isolations and recoveries of 70% or better for each step in the method. The prepared sample extracts were analyzed by capillary GC and GC/MS. Electron impact ionization was used for PAH, and negative chemical ionization with methane as a reagent gas was used for PCDD/F. Reproducible results were obtained. The method is sample and has the advantage of conserving sample consumption since two classes of compounds can be analyzed from the same sample. This can be critical in sediment core analyses were sample size is usually limited. 23 refs., 3 tabs.

• OSTI ID: 7035058
• Journal Information: Estuaries; (United States), Vol. 16:3A; ISSN 0160-8347
• Country of Publication: United States
• Language: English

Related Subjects

54 ENVIRONMENTAL SCIENCES
DIOXIN
SAMPLE PREPARATION
FURANS
POLYCHLORINATED BIPHENYLS
POLYCYCLIC AROMATIC HYDROCARBONS
SEDIMENTS
CHEMICAL ANALYSIS
COMBUSTION PRODUCTS
GAS CHROMATOGRAPHY
AROMATICS
CHLORINATED AROMATIC HYDROCARBONS
CHROMATOGRAPHY
HALOGENATED AROMATIC HYDROCARBONS
HETEROCYCLIC COMPOUNDS
HYDROCARBONS
ORGANIC CHLORINE COMPOUNDS
ORGANIC COMPOUNDS
ORGANIC HALOGEN COMPOUNDS
ORGANIC OXYGEN COMPOUNDS
SEPARATION PROCESSES
540220* - Environment
Terrestrial- Chemicals Monitoring & Transport- (1990-)