Cyclic voltammetry is the most versatile electroanalytical technique used for investigating the mechanisms of electroactive species. In this laboratory experiment, we utilize the FeIII(CN)63-/FeII(CN)64 couple as an example of an electrochemically reversible redox system to introduce some fundamental concepts of cyclic voltammetry. Through this experiment, students will become familiar with the basic principles of voltammetry and should be able to determine the following parameters: the formal reduction potential (Eo′); the number of electrons transferred in the redox process (n); the diffusion coefficient (D); electrochemical reversibility; and the effects of varying concentration (C) and scan rate (ν).