A fly ash sample found to contain polychlorinated dioxins and dibenzofurans was analyzed for brominated analytes. Bromochloro-polynuclear aromatic hydrocarbons, dioxins and dibenzofurans, as well as bromo PAH were found in ppt to ppb concentrations. Analytical results were confirmed by high-resolution mass spectrometric accurate mass determinations and by tandem mass spectrometry.
Groundwater at or near Superfund sites often contains
much organic matter, as indicated by total organic
carbon (TOC) measurements. Analyses by standard GC
and GC/MS methodology often miss the more polar
or nonvolatile of these organic compounds. The
identification of the highly polar or ionic compounds
may be needed to assess toxicity more reliably, to
plan remediation, and to establish the possible source
of a waste and the responsible party. This study
characterized water samples from two Superfund sites
for organic components where routine methods had
failed to account for a majority of the TOC.
Carboxylic acids, alcohols, and ketones were detected
by GC/MS using a new capillary column designed
for polar organic compounds. Particle beam LC/MS
allowed for identifying several additional compounds.
Finally, thermospray LC/MS was shown to be an
excellent means of detecting ionic constituents, such
as aromatic sulfonic acids, in the water samples.
Vacuum distillation of water, soil, oil, and fish samples is presented as an alternative technique for determining volatile organic compounds (VOCs). Analyses of samples containing VOCs and non-VOCs at 50 ppb concentrations were performed to evaluate method limitations. Analyte recoveries were found to relate closing with boiling point unless a compound's water solubility exceeded 5 g/L. Recovery, precision, and method detection limits for VOCs demonstrate this technology is appropriate for environmental samples.Determining volatile organic compound (VOC) concentrations in environmental matrices is one of the most important and routine analyses. VOCs are addressed as a major group of analytes for the Comprehensive Environmental Response Compensation and Liability Act (CERCLA), Resource Conversation and Recovery Act (RCRA), and the Clean Water Act (CWA). The widespread occurrence of VOCs in the environment and the potential of using VOCs as indicator parameters for contamination plumes from point sources make their accurate and routine measurement an important issue. These considerations make any improvements in VOC determinations worthwhile to the EPA and relevant to the analytical community.The most widespread technology used to determine VOCs is purge and trap, developed by the EPA to determine VOCs in water.1'2 3Purge and trap is incorporated into EPA methods for water and soil.3-5 This technique is optimal for drinking water, but has difficulties when purging is hindered by elevated organic content. The trapping material also introduces difficulties that have been summarized.6Vacuum distillation was developed as an alternative technique for determining VOCs in nonwater environmental matrices. The vacuum distillation of sediments and fish tissues provided greater VOC recoveries compared to purge and trap.7
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