Catalysts containing transition metals like nickel are frequently used in technical hydrogenation reactions. Typically their activity and selectivity are determined via metal dispersion. XRD, H2 TPD, volumetric chemisorption of H2 and CO pulse chemisorption were applied to determine the Ni crystallite size of Ni-containing catalysts. The methods were compared with regard to their information content and validity as well as their applicability in quality control during industrial manufacturing of catalysts. Pulse chemisorption of CO showed the best results for utilization in quality control.