A fast energy dispersive x-ray fluorescence (EDXRF) method requiring only microgram amounts of analytes, i.e. uranium (U) and thorium (Th), in their mixtures in solution form is described. Calibration solutions and samples covering the fuel composition range (0–5%of U in U+Th) of advanced heavy water reactor (AHWR) were prepared by mixing uranium and thorium solutions. A known fixed amount of internal standard yttrium (Y) was added to these solutions. EDXRF spectra of calibration solutions and samples were measured by taking 20 μl aliquots on 30mmdiameter filter papers, after drying, using a Rh target tube operated at 40 kV and 500 μA. Calibration plots were made by plotting U/Y, U/Th and Th/Y amount ratios against the respective intensity ratios of Th Lα, U Lα and Y Kα. In the first set, U was determined using Y as an internal standard, and for Th determination, U, thus determined, was used as an internal standard since the amounts of Th and Y were kept constant in the calibration solutions and samples. In the second set, both U and Th were varied and determined using Y as internal standard. The results of U and Th determinations showed a precision of about 3% (1s) and the results deviated from the expected values by < 3% in most of the cases. This approach has an advantage that it requires only microgram amounts of sample, thus mitigating radiation hazards associated with radioactive samples as well as the amount of radioactive analytical waste generated is quite less.