Capillary column gas chromatography-mass spectrometry, utilizing electron impact, chemical ionization and accurate mass determinations, was applied to the broad spectrum analysis of synthetic organic chemicals (SOCs) in a river located in the North Carolina Piedmont. The river was sampled at three locations several times during a thirteen-month period. The SOCs were isolated by either resin adsorption or direct methylene chloride liquid-liquid extraction. Of the 48 distinct SOCs detected, those found most frequently included atrazine and methyl atraton (triazine herbicides), dimethyl dioxane, 1,2,4-trichlorobenzen, tributylphosphate, triethylphosphate, trimethylindolinone, and tris(chlorpropyl)phosphate. Many of these chemicals are indigenous to industrial and agricultural activities in the Piedmont. Concentrations of the SOCs were in the ng/l to μg/l range. The qualitative and quantitative data were similar for both extraction methods, but the resin method was more tedious and introduced more artifacts. © 1988.