The nickel part of a new, nonpyrophoric Raney-type catalyst was characterized by using anomalous small-angle X-ray scattering. The mean particle size distribution determined by the method as meant by C. G. Shull and L. C. Roess (J. Appl. Phys. 18,295 (1947)) was in good agreement with the domain size obtained from the broadening of the (111) Bragg reflection peak of the metallic nickel using the Scherrer equation and with the size observed by TEM. Moreover, it was found that the nickel particles have a cylindrical shape and do not exhibit surface fractal behavior.