X-ray diffraction (XRD) is a major tool employed to identify and characterize catalytic materials. A brief review of the diffraction phenomenon and the effect of crystallite size is presented.Appli cations of XRD to catalyst characterization are illustrated, including correlation of XRD powder patterns to molecular structural features, deter mination of Pt crystallite size and others. Factors that affect the appearance of XRD powder patterns, such as framework structure perturbations, extra framework material, crystal morphology, impurities, sample preparation, instrument configurations, and x-ray sources, are discussed.X-ray diffraction (XRD), in particular x-ray powder diffraction, has been used extensively to identify and characterize materials used as catalysts in the petroleum refining and petrochemical industries. This is not surprising, since many of the materials are crystalline; i.e., the atoms can be arranged in threedimensional periodic arrays. Every atom in a crystalline solid contributes to the observed XRD pattern, thus making the pattern characteristic of the material-a virtual fingerprint. The diffraction data obtained for catalytic materials can tell us many things about these materials, ranging from the structural nature of the crystalline components to the average Pt crystallite size on a supported-metal catalyst. It can be used to monitor and correlate molecular structural features to catalytic process and reaction variables, or to specify composition for patent definition. In short, XRD is an invaluable technique in catalyst research and development. This discussion will illustrate some of the applications of XRD to catalyst characterization and point out some of the factors that affect the appearance of x-ray powder diffraction patterns of these materials.