The application of scanning nuclear microprobe for study a radiation-induced migration of impurities at the grain boundaries in structural materials was considered. The work describes the sample preparation for a further irradiation of microscopic areas which include a few grains. Copper samples with deposited sulfur film were used in the present work. Determinations of a chemical composition of the samples, as well as a mapping of the element distribution, were based on the analysis of characteristic paticle induced X-ray emission (PIXE). Two-dimensional distribution maps of elements, that revealed a presence of randomly distributed inclusions of silicon as a result of mechanical treatment, were obtained using the method of micro-PIXE. The quality difference of sulfur films deposited by thermal evaporation and a drop method was shown.