Wastewater from the Afyon Alkaloids Factory (Afyon, Turkey) was subjected to low-pressure catalytic wet-air oxidation (CWAO) using Fenton's reagent, and the optimal reaction conditions were investigated. The CWAO using Fenton's reagent was applied to the factory effluent, diluted factory effluent, and aerobically pretreated wastewater. To find the optimum quantities of reagents, ferrous iron (Fe 12 )-to-substrate ratios of 1:10, 1:25, and 1:50 and hydrogen peroxide (H 2 O 2 )-to-Fe 12 ratios of 1, 5, and 10 were investigated, and the treatment was carried out at different temperatures. High chemical oxygen demand (COD) removals were obtained at 508C, with the Fe 12 -to-substrate ratio range between 1:10 and 1:25. The change in H 2 O 2 -to-Fe 12 ratios did not cause any considerable effect. Also, the percentages of COD removals were nearly the same, so the ratio H 2 O 2 :Fe 12 :1 is recommended. Aerobic pretreatment seems to be effective. On the other hand, no enhancement was observed in the case of the diluted wastewater. Water Environ. Res., 80, 540 (2008).