A simple electrochemical method has been proposed for the preparation of silver nanoparticles that can be used for the detection of cyanide. Both the electrochemical behavior and morphology of the Ag nanoparticles have been characterized in the presence of KCN or diethyl cyanophosphonate (DECP) as well as in alkaline media. These were investigated by cyclic voltammetry and scanning electron microscopy (SEM). DECP is a simulant of the chemical warfare agent tabun.