The use of a dual oxidation system, which combines sodium persulfate (Na2S2O8, SPS) and hydrogen peroxide (H2O2, HP) is increasing as an in-situ chemical oxidation (ISCO) process for soil and groundwater remediation. An analytical method was assessed in this study for determining individual oxidant concentration in order to understand the interactions, and variations in the concentrations, of SPS and HP in aqueous systems containing both SPS and HP. The iodometric titration method was demonstrated to be capable of measuring total oxidant (SPS + HP) concentration; while the ceric sulfate titration method can be used specifically for measuring HP in the dual oxidation system without interfering with the iodometric titration. Therefore, SPS concentration can be deduced by subtraction of the HP concentration from the total oxidant concentration. Direct iodometric titration for determination of total oxidant at concentration above 20 mM exhibited <8% concentration. Based on the results of indirect determination of SPS in the dual oxidation system, an approximate 10% concentration variation was expected. This research may serve as a reference for measuring oxidant variations in this ISCO dual oxidant application.