A gas chromatographic procedure is described for the analysis of a variety of substituted phenols from water samples. The method was designed for situations when the sample size is very limited (0.5 to 1.0 ml), such as in laboratory microcosm experiments on transport and fate of pollutants. The phenols were extracted, derivatized, and quantified by flame ionization and electron capture detection. Toluene gave a better extraction efficiency than acetone, hexane, dichloromethane, and ethylacetate, yielding essentially the same recovery from spiked well water samples as direct acetylation with acetic anhydride. Between 5 and 35 ng/ml of different phenols were detected. The heptafluorobutyryl derivatives possessed high electron capture sensitivity, ranging from 0.1 to 7.6 pg of individual phenols.