A diffractometer equipped with a gas proportional counter and pulse-height analyzer provides a very satisfactory means of recording the X-ray diffraction patterns of chromium-containing materials with Cu Kα radiation. The fluorescent chromium K radiation can be rejected along with much of the white background radiation without appreciable loss of Cu Kα intensity, and the advantages of copper over chromium or molybdenum radiation can be fully utilized. This is illustrated by an X-ray diffraction study of coprecipitated chromia-alumina catalysts, in which the chromium concentration varies between 0 and 37 w, %. At each chromium concentration the precipitate was studied in the washed and dried state, as well as after calcination at 500, 750, and 1400°C. X-ray diffraction patterns are presented to show the phase transformations and sample inhomogenelties that were observed.