Automated electrochemistry experiments were performed using a modified version of our previously reported eLab platform, using a SY01B pump-valve combo to replace the separate SY08 pump and SV07 valve. All electrochemical measurements were conducted using a CH Instruments 760E bipotentiostat in a three-electrode configuration, controlled by the Hard Potato library. The setup used a 3 mm diameter glassy carbon working electrode, a graphite rod counter electrode, and an Ag/AgCl reference electrode (3 M KCl) with a salt bridge. A buffer consisting of 0.1 M sodium bicarbonate and 0.1 M sodium carbonate (pH 9.8) was used as an electrolyte. Prior to performing a set of automated experiments electrodes were preconditioned by applying an oxidative potential of 1.5 V vs. Ag/AgCl for 30 s, followed by reductive cycling from 0 V vs. Ag/AgCl to -1 V s. Ag/AgCl and back (Figure ). CVs of TEMPO Experiments were performed at room temperature without gas purging, and all cyclic voltammograms are presented following the IUPAC convention. Autonomous experiments had the same concentration bounds as the digital twin, but possible scan rates were constrained between 5 mV/s and 5 V/s.