A novel liquid–liquid separation for the recovery of free or liberated gold from mixtures of fine particles was evaluated. The separation, conducted at 295 K and carbon dioxide vapor pressure of 6.0 MPa, was based on the difference in wettability of precious metals and minerals. Contact angle results indicated that in the presence of water and liquid CO 2, gold was slightly hydrophobic. The addition of CO 2-soluble fluoroalkyl or fluoroether thiols increased the hydrophobicity of gold exposed to water and CO 2 to a greater extent than alkylthiols. Minerals, including quartz, pyrite and magnetite, were hydrophilic. During the separation an aqueous slurry of fine mineral and gold particles was mixed with liquid carbon dioxide. Fine gold particles, −325 mesh, dispersed in the liquid CO 2 or agglomerated at the H 2O–CO 2 interface. The minerals tended to remain in the aqueous phase. Poor results were obtained, however, when attempts were made to recover gold from an Australian gold-mining gravity concentrate. This was attributed to the gold particles in the concentrate being too large, agglomerated in slimes, or coated with minerals.