Abstract: | Efficient and stable electrocatalytic activity for the reduction of O2 at activated screen‐printed carbon electrodes modified with palladium nanoparticles (SPE*‐Pd) was demonstrated in this study. X‐ray photoelectron spectroscopy confirmed the formation of >C?O functional group on electrode surface during the preanodization procedure at 2.0 V (vs. Ag/AgCl). The existence of chloride moieties was also identified possibly from the organic binder of carbon ink used in SPE fabrication. Both >C?O and chloride functional groups were essential for the excellent stability of the SPE*‐Pd. Electrochemical impedance spectroscopy verified the enhanced kinetic rate of oxygen reduction reaction at the as‐prepared Pd nanoparticles. The SPE*‐Pd showed ca. 250 mV positive shift in peak potential together with twice increase in peak current compared to those observed at a SPE‐Pt. The calibration plot was linear up to 8 ppm of DO with sensitivity and regression coefficient of 4.49 μA/ppm and 0.9936, respectively. The variation coefficient of ipc for 7 DO determinations with O2‐saturated pH 7.4 PBS was 2.1%. Real sample assays for ground and tap waters gave consistent values to those measured by a commercial dissolved oxygen meter. |