Elemental compositional characterization of (U, Pu)O₂ samples is an important aspect for quality control of nuclear fuels. A microanalytical Energy Dispersive X-ray Fluorescence (EDXRF) method has been developed for the determination of plutoniumand uranium. Themethod involves sample dissolution, addition of internal standard(s) into the sample solution, taking about 50 μg of the sample on absorbent sheets, drying and sealing the specimens in such a manner that no loose radioactive particle comes out, during the analysis. Such approach does not require putting the instrument inside the glove box. These specimens were presented for the EDXRF measurements using Rh Kα as the excitation source. The amount of uraniumand plutoniumin sampleswere calculated using two different internal standards Ga and Y. The Puweight percent (wt%)was calculatedwith respect to (U + Pu) in the samples. The results obtained were in good agreement with the biamperometric analysis results of the samples. The average precision observed was within 1% (1σ, n=4) and the deviation of the EDXRF determined values from expected values was within 2%. The detection limits obtained for Pu and U were 4 μg.