A method in described for the simultaneous determination of trace concentrations of Ca, Cr, Cu, Fe, Mn, Ni, Mo, As, Zn, Co, Th, V and Ti in nuclear‐grade uranium oxides or other uranium compounds by x‐ray fluorescence spectrometry without the use of chemical treatment. The limits of detection are Mo 25, As 40, Cu 5, Ni 29, Co 17, Fe 5, Mn 30, Cr 8, Th 7, Zn 5, V 52, Ti 10 and Ca 80 ppm. Samples are prepared in the form of double‐layer pellets with starch as a binding agent. Standards are prepared in a U3O8 matrix, which is more chemically stable than other uranium oxides. The dynamic ranges of the calibration graphs are very large because, for all impurity elements, they are linear over three orders of magnitude of concentration. The method is fast, since it requires no chemical treatment and only limited manipulations. The method has good precision for the impurity elements.