A new procedure was developed for the waste treatment of radioactive phenol on a laboratory scale. Waste phenol was dissolved in water (2% as phenol), and ferrous ion (10 mg/l as Fe2+) was added. Hydrogen peroxide (6% as H2O2) was added separately in three steps, 20, 30, and 50% of the volume, in order to avoid rapid reaction. The solution was heated at 80-90 degrees C for several hours in a beaker covered with a watch glass till the color of the solution changes from red purple to pale yellow. Then, the solution was neutralized with sodium hydroxide and heated for 1 h to decompose excess hydrogen peroxide. When the procedure is carried out with four 2 l beakers on a hot plate, 100 ml of phenol (1,200 ml of the aqueous solution saturated with phenol) can be oxidized simultaneously.