Cyanide compounds Lire widely used in gold ore processing plants in order to facilitate the extraction and subsequent concentration of the precious metal, Owing to the high cyanide concentrations employed in gold processing, effluents generated have high contents of free cyanide as well as metallic cyanide complexes, which lend them a high degree of toxicity. The process under study, developed in laboratory scale with the use of a distillation apparatus, consists of highly decreasing the pH of the solution by adding sulfuric acid. Thus, the cyanide present in either free form or as a metallic complex is made volatile and the resulting cyanide gas is absorbed in an alkaline solution for reutilization. This work aims at recognizing the chemical relations between the cyanide and metals during distillation. The regeneration of cyanide from gold processing proved to be a viable procedure. Cyanide recoveries pointed to the fact that if a method for reutilization of cyanide contained in mining effluents is employed, the precious metal processing will become more efficient. Also, the environmental conditions in the area of the operation will be improved. (C) 2002 Elsevier Science Ltd. All rights reserved.