Transmission X-ray microscopy has been used to investigate individual Co/TiO2 Fischer-Tropsch (FT) catalyst particles in 2-D and 3-D with 30 nm spatial resolution. Tomographic elemental mapping showed that Co is heterogeneously concentrated in the centre of the catalyst particles. In addition, it was found that Co is mostly metallic during FT at 250 °C and 10 bar. No evidence for Co oxidation was found.