AbstractScreening procedures have been developed by the U.S. Environmental Protection Agency (EPA) to isolate and tentatively identify nonpolar organic chemicals in effluent and sediment samples with high potential to form chemical residues in aquatic organisms. The objective of this study was to determine if the sample components tentatively identified by the effluent‐and sediment‐screening procedures actually form chemical residues in aquatic organisms. This evaluation consisted of analyzing effluent and sediment samples from a field site with discharges from two coke‐manufacturing facilities using the screening procedures. Effluent, sediment, crayfish (Decapoda), and sunfish (Lepomis sp.) samples from the field site were also prepared using conventional sample preparation procedures and analyzed for the tentatively identified chemicals (TIDs) reported by the screening procedures. Results of the screening procedures were then compared to the results of the analyses on the samples prepared using the conventional sample preparation procedures. For the effluent‐screening procedure, 182 of 183 TIDs in Coke Plant 1 effluent and all of the 7 TIDs in Coke Plant 2 effluent were found in the crayfish, sunfish, and/or sediment samples downstream of the discharges. For the sediment‐screening procedure, 92 of 93 TIDs and all of 47 TIDs in sediment samples from two sampling stations downstream of the discharges were found in the crayfish and/or sunfish samples.