AbstractThe anoxic–oxic activated‐sludge process has been evaluated in a laboratory investigation as a means for effective treatment of cyanide‐laden wastewaters, with phenols used as the organic carbon sources for denitrification reactions. The performance of the process was evaluated at different levels of feed cyanide concentration and mean cell residence time (MCRT). The results obtained indicate that the phenolic compounds used can be effectively used as the organic carbon sources to promote denitrification reactions. The effects of cyanide inhibition on overall TOC removal can be alleviated at longer MCRTs. Between 1.2 and 2.2 g TOC can be utilized per gram NO2+ NO3−‐N removed in the anoxic chamber depending on the prevailing MCRT. Microbial oxidation of cyanide and thiocyanate which yields ammonia is the main mechanism responsible for the removal of cyanide and thiocyanate observed in the anoxic–oxic activated‐sludge process. Excellent removal efficiencies have been observed with feed concentrations up to 60 mg CN−/L and 100 mg SCN−/L Frequent exposure of autotrophic and aerobic cyanideutilizing microbes does not impede their activities in the oxic environment. Good nitrification and denitrification efficiencies are attainable in the anoxic–oxic activated‐sludge process in the presence of high feed cyanide and thiocyanate concentrations, provided that MCRT is maintained at a desirable level. As a result, the microbial degradation of cyanide and thiocyanate in conjunction with nitrification and denitrification to produce innocuous nitrogen gas is feasible in the anoxic–oxic a