Laboratory testwork has been performed on ancient residues from the cyanidation of a previously roasted gold-containing pyrite and arsenopyrite ore. By grinding to 95 per cent minus 60 microns, and after a strong aeration conditioning of the pulp, a gold recovery of approximately 67 per cent was obtained by cyanidation. This recovery was brought up to 80 per cent by leaching with thiourea, after a preleaching step with sulphuric acid under severe conditions of acidity and temperature. To avoid excessive capital costs bound to such processes, it was decided to investigate the possibility of applying flotation after grinding at a size similar or finer than the one used for the leaching tests. The method turned out to give interesting results because of the natural flotability observed at pH values lower than two for particles rich in gold present in the residue. After two cleaning steps, a final concentrate, representing around one weight per cent of the feed, was obtained with an approximate gold content of 350 g/t, representing a batch recovery of gold of about 50 per cent. Apart from sulphuric acid, whose addition was very high (flotation slurries at 25 g/l H2SO4), other reagents were not found necessary. Additional flotation tests were carried out to examine whether the recycling of the cleaner tails was justified but the gain observed appeared insufficient.