The mass of volatile organic compounds emitted to the atmosphere during solvent sublation was determined experimentally, using toluene as a test compound. It is shown that the emission of toluene to the atmosphere can be significantly reduced by using solvent sublation instead of air stripping under the same experimental conditions. The parameters which affect emission are the air flow rate, the nature and thickness of the organic layer, and the nature and concentrations of the co-solutes. Emissions are reduced as the thickness of the organic layer on the top of the column is increased. The use of decyl alcohol as the layer compound decreases emission to a greater extent than does paraffin oil. The emission of toluene during solvent sublation is further reduced as the air flow rate is lowered. The rate of toluene removal from water in solvent sublation is somewhat higher than in air stripping under the same experimental conditions. The effect of added anionic or cationic surfactants or alcohol was to improve the efficiency of water separation, but it also allowed more of the toluene to be emitted from the system.