A) Cyclic step chronoamperometric (CSCA) analysis of TEMPO (3 mM), following sequential addition of 1 equiv HCl (at 1 min) and HNO3 (at 13 min) to the aerobic reaction mixture. Inset shows representative limiting anodic and cathodic currents for two CSCA steps. B) Concentration profiles of TEMPO and TEMPO+ based on the median Ic and Ia measured at −0.18 and 0.52 V vs. Fc0/+, respectively, for each potential step in (A). Conditions: 0.1 M NBu4PF6, CH3CN, 1000 RPM.