Synchronous ultraviolet-visible (US-vis) fluorescence spectrometry is currently being evaluated as a field screening technology by the U.S. Environmental Protection Agency's (EPA) Environmental Monitoring Systems Laboratory in Las Vegas, Nevada (EMSL-LV). A prototype field-portable spectrofluorometer capable of excitation, emission, and synchronous scans was field tested at the American Creosote Works Superfund Site (a wood preservation facility) in Jackson, Tennessee. The instrument was also tested in the laboratory with sediment samples collected from Antarctica. The results of the study demonstrate the utility of synchronous fluorescence to provide evidence of the presence and identity of hydrocarbon contamination in environmental samples. The technique allows flexibility in selection of optimum extraction and instrumental procedures for site-specific matrices.