The mechanochemical reduction of lead sulphide with elemental iron in a high-energy mill was studied. X-ray photoelectron spectroscopy was used for characterization of obtained products of reduction. Elemental lead as well as its divalent forms were identified in the surface layer of products of mechanochemical reduction. The mechanochemical reduction of lead sulphide with elemental iron on the surface is a complicated reaction and the identification of compounds formed in the surface layer is not unambiguous. However, only 23% of elemental lead on the surface is produced. The degree of mechanochemical transformation in the surface layer is not very high under chosen conditions. Higher power input is needed for further progress of the reaction. (C) 2004 Kluwer Academic Publishers.