During the dissolution of gold in fully aerated cyanide solutions the CN ion is the active agent, and consequently the usual method of evaluating the dissolving power of such solutions is to determine the CN- concentration analytically. The presence in the solutions of copper and/or zinc which themselves form complex cyanides, may result in erroneous conclusions as to the free cyanide ion concentration determined by titration.In this paper the theory of titration of such solutions has been developed, and potentiometric methods have been used to follow the behaviour of complex cyanides of copper and zinc. The results for cuprocyanides show Cu (CN)s to be the most important copper complex, and in addition they explain the reported low rates of solution of gold in copperbearing solutions which when titrated in the usual way, appear to have adequate free cyanide. An explanation of the misleading value of the titration is given, and suggestions for recognition of the condition are offered. Preliminary results for zinc-bearing solutions show that there is no satisfactory end-point for the titration of CN- in excess of that in the complex Zn (CN) 4=, which dissociates to CN and Zn(CN)g-.