A solvent extraction-distillation process for recovery of chloroform in aqueous effluent was developed. Sulfonated kerosene was used for extraction of chloroform. When the flow ratio of organic phase to aqueous phase is 0.1, the chloroform concentration in the aqueous effluent can be decreased from 10 g/L to about 100 mg/L by 3-stage countercurrent extraction. The distribution ratio of chloroform between sulfonated kerosene and water is about 50. Sodium sulfate in the aqueous effluent will enhance the distribution. A small amount of water was added to the distillation column for stripping chloroform in sulfonated kerosene. RPC was used as a commercial extractor. Scale-up from the data of the pilot test was based on the Karr correlation. Recovery of chloroform was over 90%, and residual kerosene in the aqueous effluent from the extraction was lower than 70 mg/L. It is expected that the technique can be used for the recovery of other organic solvents miscible with kerosene.