Innovative and efficient electroanalytical approach for determining persulfate in aqueous solutions using a gold...

Persulfate (PDS), peroxodisulfate, peroxydisulfate, peroxodisulfuric acid, is an oxidant that can be generated by direct oxidation of sulfate ions or indirectly via reaction with hydroxyl radicals in anodes with high oxygen overpotential. Quantitative methods for determining/quantifying PDS in the presence of other strong oxidants or other anions in eco-friendly applications do not give reliable results because of these interferents. Therefore, an additional method is needed to improve the efficacy to determine/quantify the PDS concentration in oxidative environments. In this frame, an alternative sensing approach was developed based on the electroreduction of PDS in the polycrystalline gold electrode using the square wave voltammetry (SWV) technique for its detection and quantification. Then, the procedure was evaluated in terms of its effectiveness for determining PDS in complex matrices, such as in the electrolysis of sulfate ion precursor solutions using anodes with high oxygen overpotential (e.g.: diamond electrode) capable of generating other strong oxidants. Based on the results obtained, it was confirmed that only the direct electron transfer step is attained when PDS is electrochemically synthetized at the surface of the polycrystalline gold electrode, contributing to its detection and quantification by SWV. It was also observed that at acidic conditions, the PDS electroreduction process is controlled by mass transfer while that the sensitivity for PDS detection is improved, achieving detection limits of about 14 and 19 μM for perchloric and sulfuric acids medium, respectively. When the electrolysis of sulfate-based solution at acidic conditions was performed to determine the electrochemical production of PDS by SWV approach with Au sensor, the concentration of PDS was effectively determined and no interferences were assessed by other strong oxidants generated during the electrolysis. Conversely, the spectrophotometric method showed that, the results of the PDS concentration were overestimated and other strong oxidants significantly interfere with its determination during the electrolysis of sulfuric acid solutions. Therefore, the electroanalytical method presented here is a suitable alternative for determining PDS during the applicability of the environmental-electrochemical technologies.