The redox reactions of two main components of reactive oxygen species (ROS), superoxide and hydrogen peroxide, along with oxygen in aqueous solutions were investigated using a conventional electrochemical technique, differential pulse voltammetry (DPV). Superoxide undergoes oxidation at a Pt working electrode biased at 0.055 V versus Ag/AgCl, while hydrogen peroxide can be oxidized and reduced at 0.817 and –0.745 V, respectively. Oxygen in the solutions is reduced at the electrode with an applied potential of –0.455 V. Based on these results, hydrogen peroxide and superoxide released from live cells can be successfully monitored, identified, and mapped using scanning electrochemical microscopy (SECM) at different potentials. Single human bladder (T24) cells were imaged using a 5 μm diameter SECM probe biased at –0.400, –0.600, and –0.800 V. Oxygen reduction that seems an interference can be discriminated from that of hydrogen peroxide by means of SECM.