It is reported that Mo and Co powders had been recovered from spent hydrogenation and desulphurization catalysts. In use these become 'poisoned' by deposited C. The process is described and involves size reduction and size separation, chemical leaching, roasting to oxide and reduction to metal with H. Effects of process variables were studied, recovery of 94% is reported and powders of high purity were obtained. The powders were characterized and compaction tests were done.