The present work investigates the possibility of nitrocarburising in ammonia-acetylene-hydrogen and ammonia-propene-hydrogen gas mixtures, where unsaturated hydrocarbon gas is the carbon source during nitrocarburising. Consequently, nitrocarburising is carried out in a reducing atmosphere and straightforward control of the carburising and nitriding potentials is in principle possible. The nitrocarburising response of unalloyed (ARMCO) Fe was investigated in a thermobalance during controlled nitrocarburising at 580°C. The “cases” obtained on nitrocarburised iron were characterized by reflected light microscopy and X-ray diffraction analysis. It is shown that the use of unsaturated hydrocarbon gas in nitrocarburising processes is a viable alternative to traditional nitrocarburising methods.