Simultaneous Determination of Hydrogen Peroxide, Hydroxylamine and Iodate in Basic Media by Differential Pulse Polarography
Abstract
The study of a new process for iodine management during nuclear spent fuel reprocessing has shown the necessity to develop a reproducible, accurate and rapid determination of iodate, hydroxylamine and hydrogen peroxide in the liquid wastes. If possible, the analysis should be performed at high pH for species stability reasons. Differential pulse polarography using LiOH 0.1 mol(.)l(-1) as supporting electrolyte appeared to be a sensitive technique for the simultaneous analysis of the three compounds. The species electrochemical behaviours were studied independently and the chemical interactions were determined. Because of numerous interactions occurring between the species, analyses by the standard addition technique was excluded and rigorous operating conditions must be applied. Simultaneous analysis was performed by adding small amounts of sample in 10ml LiOH 0.1mol(.)l(-1) deaerated supporting electrolyte and using calibrations curves. The three species could be detennined in one cathodic scan with satisfying sensitivity (limit of detection=1 X 10(-6) mol(.)l(-1)), reproducibility (relative standard deviation < 8% for ten measurements) and selectivity.