The process of oxidation of ammonia proceeds in 800-900 degrees C with high reactivity hydrogen discharge. Extremely aggressive environment and temperature require using the most chemically resistant materials with catalysis properties. One of the main groups of those materials is palladium-nickel alloys. In our investigation we focused on analysis of PdNi5 degradation during catalysis process. The investigation was performed on 78 mu m diameter wires after long exposition to chemically aggressive environment. The samples were prepared with focused ion beam ( FIB) system. The observations of surface and wire cross sections were executed using a scanning electron microscope (SEM) with energy dispersive spectroscopy (EDS) device, which allowed defining chemical composition. The effect of a grain orientation on sensitivity to reaction with ammonia gas was tested by mapping with electron backscatter diffraction (EBSD) techniques. Significant change of wire cross section after long exposition was determined by 3D X-ray computer tomography (XCT). The obtained results can be basis of further investigation on improvement of strength of PdNi alloys in high temperature chemical application. (C) 2012 Elsevier B.V. All rights reserved.