PT/AL2O3–CEO2 NANO CATALYST WITH PT LOADING OF 1% AND CERIA LOADING OF 30% WERE SUCCESSFULLY PREPARED VIA ULTRASOUND-ENHANCED IMPREGNATION METHOD TO BE UTILIZED IN TOTAL CATALYTIC OXIDATION OF TOLUENE. THE NANOCATALYST WAS CHARACTERIZED USING XRD, FESEM, BET AND FTIR TECHNIQUES. THE XRD PATTERNS CONFIRMED THE FORMATION OF CERIUM OXIDE AS THE CRYSTALLINE PHASE ON ALUMINA WITH AN AVERAGE CRYSTALLITE SIZE BETWEEN 8.1- 8.7 NM, DERIVED BY SCHERRER EQUATION. FESEM IMAGES CONFIRMED THAT THIS NANO CATALYST HAD CERIA AND PT PARTICLES IN NANO-RANGES. BET SURFACE AREA PRESENTED LARGE SURFACE AREA FOR NANOCATALYST. THEREFORE, THESE PATTERNS REVEALED THE PROMOTING EFFECT OF ULTRASOUND IRRADIATION ON THE SURFACE PROPERTIES. THE RESULTS OF TOLUENE OXIDATION INDICATED THAT THE SYNTHESIZED NANOCATALYST WAS HIGHLY ACTIVE AND ABLE TO REMOVE NEARLY 100% OF TOLUENE AS REPRESENTATIVE VOCS. THE PRESENCE OF NANOPARTICLES ALONG WITH GOOD CHARACTERISTICS OF THE SYNTHESIZED NANOCATALYST PRESENTED IT AS A HIGHLY EFFICIENT MATERIAL FOR CATALYTIC OXIDATION OF VOCS.