This report presents the results of experimental studies of the fluid phase in the Fe-C-S system at high P and T values (5.3 GPa and 1300°C) conforming to diamond synthesis. The samples for experiments were mounted on air; therefore, the volatile compounds detected after the experiments are characterized by a wide variety and complicated composition involving both inorganic and organic components. Among the inorganic compounds, CO 2 , H 2 O, N 2 , SO 2 , CS 2 , and COS were detected. The GC/MS analysis revealed hydrocarbons (paraffins, olefins, and arenes), including high molecular compounds. The formation of heavy hydrocarbons confirms their thermodynamic stability under high pressure. Oxygenated hydrocarbons (alco hols, aldehydes, ketones, carboxylic acids, and ethers) were also detected.