The major problem for Fe-0 application is the degradation of performance as time due to the formation of a surface oxide layer and that for TiO2, is the limit of the efficiency due to the recombination phenomenon. To overcome the problems as well as to improve the performance, our laboratory has been inventing a novel catalyst, which was developed by coating synthesized sol-gel-derived TiO2 nanoparticles onto the surface of Fe-0. This composite was employed on the degradation of azo dye (Acid Black-24) in the aqueous solution. Results from XPS, XRD and FE-SEM analysis indicated that the laboratory-prepared nanoscale TiO2/Fe-0 material is a composite of TiO2 and Fe-0. The nanoscale TiO2/Fe-0 composite with UV irradiation can efficiently decolour and reduce TOC from the simulated wastewater containing Acid Black-24. The efficiency of the TiO2/Fe-0 composite with UV irradiation on AB-24 reduction is much more efficient than microscale, and nanoscale Fe-0 and TiO2 particle (P-25). The evidence shows that TiO2 particles by sol-gel process were coated on the Fe-0 particles surface, which is attributed to the longer life cycle of Fe-0 reactivity. (c) 2007 Elsevier B.V. All rights reserved.