AbstractA simple method is described for the quantitative determination of organochlorine pesticides and polychlorinated biphenyls (PCB's) in water at the sub‐ppb level. A micro gas‐phase extractor advantageously replaces other preconcentration and purification techniques. The extract is analyzed by capillary gas chromatography without further enrichment. The recovery at the ppb level was nearly 100% for organochlorine pesticides and more than 80% for PCB's. The complete procedure including sample preparation, steam distillation‐extraction, and capillary gas chromatographic analysis is carried out in less than four hours.