Comparisons are made between GC/FT-IR, HPLC/FT-IR, and GC/MS concerning the capability of each as analytical techniques in the analysis of an industrial wastewater effluent. Shown is the capability of infrared spectroscopy to identify specific isomers which is not accomplished by mass spectroscopy. Spectral data obtained from GC/FT-IR and GC/MS are complementary, making possible precise identifications which would otherwise be impossible. Fewer sample components are identified by HPLC/FT-IR than GC/FT-IR as a consequence of the decreased sensitivity of the former and the presence of opaque solvent band regions in the spectra. The sample isomers of chloronitrobenzene are better separated by HPLC than packed column GC, demonstrating the difference in selectivity of the two types of chromatography. Infrared reconstructed chromatograms are used in locating scan sets of maximum SIN, comparing the sensitivities of HPLC/FT-IR and GC/FT-IR, and monitoring the effect of the GC and HPLC interfaces on chromatographic peak shape. A major limitation to rapid and positive identification by GC/FT-IR is the lack of adequate vapor phase spectra. © 1979, Oxford University Press. All rights reserved.