A series of nanosized iron-doped anatase TiO2 Catalysts with different iron content (between 0.4 and 5.1 wt.%) has been prepared by a microemulsion method and examined with respect to their behaviour for UV photocatalytic degradation of aqueous phenol. The activity results have been correlated with structural, electronic and surface examinations of the catalysts done with XRD, Raman, UV-vis, EPR, N-2 physisorption and NH3 chemisorption. An enhancement of the photocatalytic activity is observed for doping levels up to ca. 1 wt.% which is attributable to the effective introduction of Fe3+ cations into the anatase structure along with associated modifications of the surface acid/base properties. Achievement of relatively high levels of surface segregation of oxidic iron-containing amorphous phases for higher doping levels results however detrimental to the photoactivity. (c) 2006 Elsevier B.V. All rights reserved.