The formation of a compound, “white” layer on the surface of Fe-7wt.% Cr alloy, by exposure to a gas mixture of ammonia and hydrogen at 580°C, was investigated. The microstructure of the surface layer was analysed employing light and scanning electron microscopy, X-ray diffraction and electron probe microanalysis. For the first time a quantitative (phase) analysis of such a white layer was carried out, demonstrating the presence of a dispersed CrN phase within a γ | iron-nitride matrix.