Statistically designed experiments were used to optimise a Raney copper catalyst system for the water-gas shift reaction by assessing a large number of variables which contribute towards catalytic activity and stability. A 2(IIII)(I-7) fractional factorial design was employed to screen eleven preparation and four reaction process variables, of which the CO:H2O ratio, alloy particle size, caustic/soluble metal ratio and zincate leach concentration were found to significantly influence the long term final catalyst activity and the overall change in activity. A composite factorial design together with response surface methodology was used to optimise the three preparation variables with respect to maximum final activity and minimum change in activity. The results of these experiments showed that the interaction between alloy particle size and caustic/soluble metal ratio was significantly responsible for final activity. Catalyst deactivation, as measured by change in activity, was significantly influenced by the interaction of zincate concentration and the caustic/soluble metal ratio. At an operating temperature of 200 degrees C, the optimum Raney copper catalyst of composition 48.8 weight percent Cu, 15.9 weight percent Zn and 33.1 weight percent Al demonstrated a higher specific activity than an industrial low temperature shift catalyst over 960 hours-on-stream under the same conditions. The above example of catalyst optimisation thus provides an excellent example of the advantages associated with this approach to catalyst experimentation.