Removal efficiencies from a three-phase continuous, countercurrent solvent sublation of pyrene and pentachlorophenol from water are presented and compare well with Series CSTR Model predictions. The effects of the air-to-water flow ratio, the solvent flow rate, and the gas sparger design are discussed. Steady-state efficiencies as high as 96% for pyrene and 94% for pentachlorophenol are reported for an annular shear gas sparger. These results demonstrate the superiority of solvent sublation over bubble fractionation which is shown to be limited to a removal efficiency of 68% or less for these compounds. Moreover, analyses of the solvent (mineral oil) phase show that the separation factor (ratio of the solvent effluent concentration to the water effluent concentration) in solvent sublation can be as high as 300, which is distinctly greater than that observed in solvent extraction.