This report contains data from the survey of manmade nonagricultural volatile and semivolatile organic chemicals in surface water in the upper Illinois River basin from May 1988 through March l990. In addition to the data, sampling methods and quality-assurance procedures are described. The survey was part of the upper Illinois River basin pilot project of the National Water-Quality Assessment program conducted by the U.S. Geological Survey. The organic chemicals analyzed from the water samples were those expected to be associated primarily with effluent from point sources in urban areas. A low-flow synoptic investigation of 52 volatile and 54 semivolatile organic chemicals was conducted at 31 sites in July 1988. Additional samples were collected monthly at two sites to continue to test for the presence of 43 volatile organic chemicals from December 1988 through March l990, and of all semivolatile organic chemicals at two sites from August through September 1988.