CV was then performed by sweeping from 0 V to 1 V, at scan rates of 1000 mV/s, 500 mV/s, 100 mV/s, and 50 mV/s. The electrode underwent pretreatment by anodization in 1 M NaOH for 30s prior to each substrate's voltammetric titration experiment to promote efficient oxidation of the TEMPOH to TEMPO. for one substrate, which is twice the time our automated platform takes. However, our measurements were fully unsupervised, allowing these experiments to be performed passively, potentially freeing the experimenter to focus on other aspects of laboratory work. It is important to note that there is a tradeoff between the time of the experiment and experimental precautions such as cleaning the cell, priming the cell, and syringe pressure equilibration. More rigorous experiments will require even more stringent protocol for solution handling, leading to longer experimental times. Having a pH meter inside the electrochemical cell allows the solution pH to be recorded before running a CV. This enables us to examine CVs recorded in solutions with pH values closest to a specified target value, facilitating comparisons between different substrates without the influence of pH variations on the system's kinetics. Figure shows CVs of 100 mM substrate and 2 mM TEMPO, collected at scan rates of 50 mV/s in a pH-adjusted supporting electrolyte with an average pH of 9.63 ± 0.01. The CV responses for all substrates exhibit clear catalytic enhancement compared to substrate-less conditions, with many CVs demonstrating mechanistically informative non-idealities such as curve crossover at the foot of the wave (Figure ), indicating that the reaction follows the ECE' mechanism shown in Scheme 1.