Two methods were used for the analysis of submicro-crystalline copper prepared by high-pressure (6 GPa) severe plastic deformation. Conventional powder XRD study was carried in terms of the modified Williamson-Hall (WH) plots and shown large line-broadening anisotropy. A new high-resolution small-angle transmission diffuse scattering method was applied for determination of crystallite size. Two methods were used for the evaluation of the diffuse scattering - calculation of the autocorrelation function of the crystalline shape by the transformation of the measured signal and by the direct fitting. Bimodal block size distribution has to be assumed for annealed samples. This was also confirmed by classical back-reflection film method as well as by the long tails of conventional diffraction profiles.