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Headspace sampling combined with capillary column gas chromatography-mass spectrometry analysis was evaluated for use in the investigation of priority pollutants in water and wastewater. A 3 mL sample loop and cryogenic trapping at minus 80 degrees C were employed to increase the sensitivity into the nanogram-per-liter range. Separations were accomplished with a coated 30-m x 0.32-mm fused silica capillary column. Mass spectral data were acquired by selective ion monitoring form 50 to 500 amu. The method was applied to water and wastewater samples with good results. Includes 7 references, tables, figures.