Abstract: Disclosed is a process for recovery of cyanide and metals from a liquor containing complexes of cyanide and metal typically generated by a metallurgical or industrial process. The process involves electrochemical dissociation of the metal-cyanide complex and electrowinning of the metal while free cyanide generated in the process is recovered in a membrane treatment step for re-use in a metallurgical process utilising it. An electrochemical apparatus, which may be used in the process, forms a further aspect of the invention. A membrane process alone, for separation of cyanide, from liquors containing cyanide complexes is a further aspect of the invention.