An ion interaction chromatographic separation method, coupled with UV spectroscopic detection, has been developed for the analysis of ethyl xanthate (O-ethyl dithiocarbonate) and its oxidative decomposition products in mineral flotation systems. The effects of the ion-pairing agent (tetrabutylammonium ion), pH modifier (phosphoric acid), and organic modifier (acetonitrile) in the eluant upon the retention characteristics of the ethyl xanthate oxidation products have been determined. The optimized separation procedure has been successfully applied to the analysis of ethyl xanthate and its oxidation products in a nickel-iron sulfide mineral suspension containing a number of other anionic species, including cyanide complexes of nickel and iron, as well as sulfur-oxy anions. The ethyl xanthate oxidation products investigated in this study have been isolated as pure compounds and characterized by UV-visible, FT-IR, and NMR spectroscopies. The UV-visible and FT-IR spectroscopic properties of these species are discussed in terms of the chemical modifications of the thiocarbonate group.