A series of gold/iron-oxide catalysts has been prepared by an inverse co-precipitation method from a mixture of HAuCl(4)(.)3H(2)O and Fe(NO3)(3)(.)9H(2)O. Samples calcined at 400 degreesC for 3h exhibited poor activity towards CO oxidation, whereas uncalcined materials that had only been dried at 120 degreesC for 16 h exhibited a far superior catalytic activity. The most active material of this latter type is shown to have 100% CO conversion at 20 degreesC for at least 10 h. Detailed characterisation of the dried and the calcined materials using ICP and BET analysis, XRD, HREM, STEM-EDX and Mossbauer spectroscopy has shown significant differences in their microstructure. The dried materials consist of micron scale agglomerates of 4-8 nm disordered Fe(5)HO(8)(.)4H(2)O particles on which the An is uniformly dispersed in the form of a mixture AuOOH(.)xH(2)O and Au-0. By comparison, the calcined materials are comprised solely of 3-5 nm cuboctahedral metallic Au particles supported on 20 nm diameter well-crystalline alpha-Fe2O3 particles. Our microstructural observations and catalytic measurements are discussed in the context of the Bond-Thompson mixed Aux+/Au-0 model for the low-temperature CO oxidation catalyst.