The generation of gaseous singlet oxygen by gas‐liquid reaction of chlorine with alkaline solution of hydrogen peroxide in spray form was studied experimentally on the originally designed device with a fast separation of reacted liquid from gas. The singlet oxygen yield, residual chlorine, and water vapor content in gas were measured under different experimental conditions of the centrifugal spray singlet oxygen generator (CSSOG) using nitrogen as a dilution gas. A characteristic feature of the CSSOG is a high utilization of the chemicals and production of singlet oxygen at a very high total pressure even near the atmospheric pressure. This generator developed originally for driving a chemical oxygen‐iodine laser (COIL) could be employed also as an efficient singlet oxygen source in material science, chemical synthesis, and others.