The application of gas chromatography/Fourier transform infrared (GC/FT-IR) data to regulatory decisions requires, among other things, the availability of validated analytical protocols. Such protocols are necessary for the generation of reliable analytical data. A GC/FT-IR protocol is described which is applicable to the determination of semivolatile organic compounds in wastewater, soils, sediments, and solid wastes. The protocol is designed for the high-throughput automated analysis of multicomponent environmental and hazardous waste extracts. With the use of capillary GC/FT-IR techniques, wastewater identification limits of 150 to 400 ppb can be achieved with this method, while the corresponding identification limits for solid samples are 3 to 88 ppm. Automated packed-column GC/FT-IR identification limits are approximately a factor of five higher than the corresponding capillary GC/FT-IR values.