In order to obtain more accurate information of Compton profiles a new technique, the Compton fluorescence scattering (CFS), was further developed. The most important advantage of the CFS compared with the conventional x‐ray technique is that the background is small and well defined. With respect to &ggr; radiation the resolution is much better and influences of multiple scattering are less serious. As an example the results on aluminum with AgK&agr; radiation and a LiF 600 analyzer demonstrate that deviations between previous results with the MoK&agr; conventional method and 412‐ and 59‐keV &ggr; measurements respectively could be interpreted. The best agreement was found with the 412‐keV &ggr; results.