A direct, continuous method for the measurement of peroxodisulfate ani
on has been devised and assessed. The approach is based upon the reduc
tion of the anion under mass transfer limiting conditions at an amalga
mated copper rotating disk electrode. The preparation of the disk elec
trode by He electroplating was examined in detail in order to generate
a reproducible surface. The system was calibrated by demonstrating th
at the limiting current density for peroxodisulfate reduction was dire
ctly proportional to its bulk solution concentration. An electrochemic
al cell arrangement was then developed to permit the continuous, in si
tu measurement of peroxodisulfate concentration during electrochemical
synthesis.