An amperometric sensor system, based on a repetitive double step potential method at a glassy carbon electrode, has been developed for the simultaneous measurement of hydrogen peroxide and oxygen concentrations. The current measured at a potential of À1 V (vs. AgyAgClysaturated Cl À ) corresponds to the sum of the reduction currents of hydrogen peroxide and dissolved oxygen. The current measured at À0.55 V (vs. AgyAgClysaturated Cl À ) is due to the reduction of dissolved oxygen to hydrogen peroxide. Alternatively, the concentration of dissolved oxygen can also be determined using a Clark electrode. The concentration of hydrogen peroxide and dissolved oxygen during enzymatic conversion of glucose can be followed on line and be used to control the process.