This paper summarizes the results of research on the treatment of synthetically prepared aqueous solutions of trinitrotoluene (TNT) and cyclotrimethylene–trinitramine (RDX) in the weight ratio 70%/30% representing a typical munitions wastewater, by a combination of ozone and ultrasound. A parametric study investigated the relationship among the variables: (1) initial solution pH (5.84 → 10.0); (2) ultrasound power level (5 → 50 watts at 852.0 to 863.0 kHz);(3) ultrasound frequency level (60.6 → 1,007.0 kHz); (4) solution concentration (70/30 mg/l TNT/RDX solutions volumetrically diluted with distilled water in the ratios 1/0, 1/1, 1/3); (5) reaction temperature (25 → 59°C). Removal rates of both TNT and TOC increased directly with increases in reaction temperature and initial solution pH. Likewise, increased sound power level produced enhanced system kinetic responses; however, these were attributed to reaction mass temperature increases. Ultrasound was found to inhibit reaction kinetics at high temperatures and pH because it promoted radical–radical extinguishment reaction.