A coupled reaction-solvent extraction process was used to remove HCl from a simulated distiller waste. The extraction performances of various extractants and diluents were compared and the apparent basicity of N235 (a mixture of tertiary amines) in various diluents was determined. The best results were obtained using N235 and isoamyl alcohol as the extractant and diluent, respectively. The yield of HCl from the coupled extraction was 75% with this extraction system. The mechanisms for the removal of HCl in both the direct and coupled extractions were investigated. For the coupled extraction, the formation of an R 3 NHCl ion-pair complex was involved in the HCl removal. For the direct extraction, the mechanism involved the formation of hydrogen bonds at high concentrations of HCl.