Few studies have investigated the use of activated carbon fibres (ACFs) impregnated with metal oxides for the catalytic oxidation of volatile organic compounds (VOCs). Thus, the effects of the ACF-supported metal oxides on toluene removal are determined in this study. Three catalysts, namely, Ce, Mn, and Cu, two pretreatment solutions NaOH and H₂O₂, and three reaction temperatures of 250°C, 300°C, and 350°C, were employed to determine toluene removal. The composition and morphology of the catalysts were analysed using Brunauer–Emmett–Teller (BET), transmission electron microscope (TEM), inductively coupled plasma (ICP), X-ray photoelectron spectroscopy (XPS), Fourier-transform infrared spectrometer (FTIR), and thermo-gravimetric analyser (TGA) to study the effects of the catalyst's characteristics on toluene removal. The results demonstrated that the metal catalysts supported on the ACFs could significantly increase toluene removal. The Mn/ACFs and Cu/ACFs were observed to be most active in toluene removal at a reaction temperature of 250°C with 10% oxygen content. Moreover, the data also indicated that toluene removal was slightly improved after pretreating the ACFs with NaOH and H₂O₂. The results suggested that surface-metal loading and the surface characteristics of the ACFs were the determinant parameters for toluene removal. Furthermore, the removal of toluene over Mn/ACFs-H₂O₂ decreased when the reaction temperature considered was>300°C.