In situ monitoring of peroxodisulfate anion production

A direct, continuous method for the measurement of peroxodisulfate anion has been devised and assessed. The approach is based upon the reduction of the anion under mass transfer limiting conditions at an amalgamated copper rotating disk electrode. The preparation of the disk electrode by Hg electroplating was examined in detail in order to generate a reproducible surface. The system was calibrated by demonstrating that the limiting current density for peroxodisulfate reduction was directly proportional to its bulk solution concentration. An electrochemical cell arrangement was then developed to permit the continuous, in situ measurement of peroxodisulfate concentration during electrochemical synthesis.