The polyol process is an effective method to generate well-dispersed nanoscale active sites on a support. To study the activity of catalysts prepared by polyol process, Cu1.25Co3.75/Al2O3, Cu2.5Co2.5/Al2O3, and Cu3.75Co1.25/Al2O3 were studied in a pilot-scale incinerator system to remove benzene, toluene, ethylbenzene, xylene, and polycyclic aromatic hydrocarbons, and the effect of lead in a flue gas was also discussed. The pilot-scale experiment results indicated that Cu1.25Co3.75/Al2O3 exhibited a good performance on organic compounds removal, without being poisoned by lead. The bimetal containing Cu/Co = 1/3 exhibits a better activity and stabilization on oxidation than the others. When the Cu/Co ratio was above one, the X-ray powder diffractometer, and Fourier transform infrared spectroscopy analyses results revealed that several components (Cu-0, CuO, and CuCo2O4) of the spent catalysts disappeared. This may be due to the active sites that were covered with an amount of CH3-groups. (C) 2008 Elsevier Ltd. All rights reserved.