A method yielding a quantitative profile analysis from electron diffraction is worked out and combined with the local information gained from transmission electron microscopy images; it is applicable to various nanomaterials. As an example, small nanocrystalline regions are analyzed that form in FeAl by severe plastic deformation. The result is unexpected as the coherently scattering domain size does not change as a function of strain. At high strains, the sample is homogeneously nanocrystalline and the results agree well with those of X-ray diffraction.