Deionized water was oxidized to form ozone at the anode while oxygen was reduced to hydrogen peroxide at the cathode in a proton-exchange-membrane electrochemical flow reactor. The conditions for simultaneous generation of these oxidants were determined as a function of the applied voltage, electrode materials (lead dioxide for ozone evolution; gold, carbon, or graphite for peroxide evolution), and electrode configurations. Measured and calculated quantities included cell current, liquid-and gas-phase ozone concentrations, hydrogen peroxide concentrations, current efficiency for ozone and peroxide evolution, and ozone and peroxide production rates. An applied potential of 4.5 V resulted in a current density of 2 A/cm z, yielding maximum gas-and liquid-phase ozone concentrations of 60 and 3.1 mg/liter at the anode (4.5% current efficiency) and hydrogen peroxide concentrations between 3 and 5 mg/liter at the cathode (0.8% current efficiency).The simultaneous synthesis of ozone and hydrogen peroxide in a proton-exchange-membrane (PEM) electrochemical flow reactor was explored. The research methodology for the paired synthesis was split into four reaction systems: 1, oxygen evolution at the anode and hydrogen evolution at the cathode (water electrolysis); 2, ozone + oxygen evolution at the anode and hydrogen evolution at the cathode; 3, oxygen reduction at the cathode (hydrogen peroxide synthesis) and oxygen evolution at the anode; and 4, simultaneous synthesis of ozone and hydrogen peroxide.Preliminary studies on the first two reaction systems I and detailed studies on reaction systems 2 ~ and 33 have been conducted. This paper describes the simultaneous oxidation of water at the anode to form ozone while reducing humidified oxygen at the cathode to form hydrogen peroxide (reaction system 4).Although there have been investigations on the individual electrochemical synthesis of ozone and hydrogen peroxide in aqueous electrolytes (acidic electrolytes for ozone, 4 and acidic and basic electrolytes for hydrogen peroxide), 5-~ very little information exists on the generation of ozone in pure water. 9'I° Also, other than the authors' own work, ~ no information exists on the generation of hydrogen peroxide using oxygen as the reactant and a proton exchange membrane as the electrolyte. Furthermore, no study has been performed to date on the design and development of a process to synthesize simultaneously ozone and hydrogen peroxide electrochemically.Ozone evolution occurs at E ° = 1.51 V vs. NHE, while hydrogen peroxide is produced at a much lower potential, E ° = 0.682 V vs. NHE. This large difference in the standard potentials suggests that high current efficiencies for hydrogen peroxide will not be obtained at potentials at which ozone is formed (due to the reduction of oxygen and hydrogen peroxide to water and possible hydrogen evolution at higher potentials). Although this large difference exists, the paired synthesis of these oxidants will eliminate the use of two separate cells where ozone is an anodic product (with ...