Alumina-supported cobalt catalysts have been prepared from different cobalt precursors to study the influence of the precursor on the ultimate metal particle size. Furthermore, the effect of the particle size on the catalytic performance (activity and selectivity) during Fischer-Tropsch synthesis has been investigated. The preparation of low-loaded cobalt catalysts (2.5 wt%) by incipient wetness impregnation using cobalt EDTA and ammonium cobalt citrate precursors resulted initially in very small cobalt oxide particles, as determined by XPS. The small oxide particles reacted during the thermal treatment in a reducing gas now with the alumina support to cobalt aluminate, which was neither active nor selective during Fischer-Tropsch synthesis. The catalysts prepared with cobalt nitrate had larger particles that could be easily reduced to metallic cobalt. These catalysts were active under reaction conditions. High-loaded cobalt catalysts (5.0 wt%) prepared using ammonium cobalt citrate showed a larger particle size than the low-loaded catalyst prepared from the citrate precursor. The extent of reduction to metallic cobalt that could be achieved with the high-loaded catalyst was significantly higher than that with the low-loaded catalyst, as shown by magnetic measurements. Accordingly, the high-loaded catalyst exhibited a reasonable activity and, in addition, an interesting and remarkably high selectivity toward higher hydrocarbons, and also a very high Schultz-Flory parameter.