The TEMPO-functionalized layers obtained from these solutions, by applying a potential of -0.4 V for 15 minutes, were analyzed by cyclic voltammetry under the same conditions as previously described (Figure ). As shown by the cyclic voltammograms (blue dashed line), the inclusion of a Lewis acid during the electroreduction of dC12TEMPONOBF4 significantly enhances the surface concentration of TEMPO entities, increasing it from 1.1 ± 0.1 × 10⁻¹⁰ mol•cm⁻² under previously established conditions to 3.0 ± 0.3 × 10⁻¹⁰ mol•cm⁻² in the presence of acid. This value is comparable to the surface concentration achieved through the electroreduction of dC12TEMPOtBuONO/BF3 under the same prior conditions. In the presence of free radical TEMPO (red dashed line), the surface concentration, as deduced from the voltammograms, decreased significantly after the electroreduction of dC12TEMPOtBuONO/BF3, dropping from 3.0 ± 0.3 × 10⁻¹⁰ mol•cm⁻² to 1.0 ± 0.1 × 10⁻¹⁰ mol•cm⁻². This lower value closely matches the surface concentration observed when immobilizing dC12TEMPONOBF4 without the addition of free radical TEMPO. Similarly, the presence of bare TEMPO radicals during the electroreduction of dC12TEMPONOBF4 reduced the surface concentration by approximately half (not shown).