We describe a method for determination of cyanide in whole blood, erythrocytes, and plasma after stabilization of cyanide by addition of silver ions. The cyanide is then transferred from the acidified sample, by aeration, into sodium hydroxide and quantified by the König reaction, with sodium hypochlorite as the chlorinating agent. A rapid loss of measurable cyanide found when cyanide was added to plasma in the absence of silver ions was attributed to a reaction with serum albumin. Cyanide added to whole blood was bound to a saturable component in erythrocytes, which we identified as methemoglobin.