A sensitive new ultraviolet-fluorescent labeling technique has been developed for the analysis of environmentally important phenols in aqueous media using 2-fluorenesulfonyl chloride as the derivatizing agent. The phenols are allowed to react with the sulfonyl chloride, and the labeled sulfonates are subsequently analyzed by high performance liquid chromatography employing fluorescence and UV detection. Use of the fluorenyl derivatives and fluorescence detection has lowered the detection limits ca. ten times that of conventional UV detection systems to a minimum detectable quantity of 0.05 ng at signal-tonoise ratio of 5:1. In addition, the chromatographic properties of the derivatives allow the option of using millilitersize injection loops without significant band spreading. A typical determination of phenolic content requires ca. 2 hr.