Sorption equilibrium isotherms from aqueous solution of benzene, toluene, chlorobenzene, p-xylene, carbon tetrachloride, trichloroethylene, and chloroform for various sorbents have been measured by two independent techniques: head-space gas chromatography (HSGC) and a stirred cell with on-line UV detection. Isotherms obtained by each technique showed close agreement at all concentrations. Isotherms are presented for XAD4, XAD2, AC-F400, an soli poly(styrene/divinylbenzene) copolymer microspheres. For solution concentrations <25% of the aqueous solubility of the organic, activated carbon was found to have the highest sorption capacity; however, activated carbon was surpassed in capacity by XAD4 at high thermodynamic activities for each organic solute. Thus, for concentrated (>25% saturated in organic) industrial waste streams, XAD4 would appear to be an attractive alternative to activated carbon. Sorption data for this study were best represented for solutes onto XAD4 by normalized volumetric isotherms and AC-F400 by a Polanyi potential theory correlation plot.