The distribution of pesticides and other synthetic organic compounds in water, sediment, and biota in the upper Illinois River Basin in Illinois, Indiana, and Wisconsin was examined from 1987 through 1990 as part of the pilot National Water-Quality Assesssment Program conducted by the U.S. Geological Survey. Historical data for water and sediment collected from 1975 through 1986 were similar to data collected from 1987 through 1990. Some compounds were detected in concentrations that exceed U.S. Environmental Protection Agency water-quality criteria. Results from pesticide sampling at four stations in 1988 and 1989 identified several agricultural pesticides that were detected more frequently and at higher concentrations in urban areas than in agricultural areas. Results from herbicide sampling at 17 stations in the Kankakee and Iroquois River Basins in 1990 indicated that atrazine concentrations exceeded the U.S. Environmental Protection Agency's maximum contaminant level for drinking water during runoff periods. Results from sampling for volatile and semivolatile organic compounds in water indicate that, with one exception, all stations at which more than one compound was detected were within 2 miles downstream from the nearest point source. Detections at two stations in the Chicago urban area accounted for 37 percent of the total number of detections. Concentrations of tetrachloroethylene, trichloroethylene, and 1,2-dichlorethane from stations in the Des Plaines River Basin exceeded the U.S. Environmental Protection Agency's maximum contaminant level for drinking water in one and two samples from the two stations in the Chicago area. Phenols and pentachlorophenols were detected most frequently in the Des Plaines River Basin where point-source discharges were common. Phenol concentrations were significantly different among the Des Plaines, Kankakee, and Fox River Basins. Phenols and pentachlorophenols never exceeded the general use and secondary contact standards. Results from a 1989 synoptic survey of semivolatile organic compounds in sediment indicate that these compounds were detected most frequently at sites in the Chicago urban area. Of the 17 stations at which 10 or more compounds were detected, 14 were located in the Des Plaines River subbasin, and 1 was on the Illinois River mainstem. As was the case with organic compounds in water, each of these sites was located within 2 miles downstream from point sources. Biota samples were collected and analyzed for organochlorines and polynuclear aromatic hydrocarbons in 1989 and 1990. The most commonly detected compound in both years was p,p'-DDE. National Academy of Science recommendations for chlordane and dieldrin for protection of predators were exceeded in 19 and 10 samples, respectively, when the 1989 and 1990 data were combined. In the nine fish-fillet samples collected in 1989, concentrations exceeded U.S. Environmental Protection Agency fish-tissue criteria in nine fillets for p,p'-DDE and five fillets for dieldrin.