A method has been developed for the direct determination of uranium in carbonate solutions by X-ray fluorescence. Uranium, in the concentration range 0.2–50 ppm, is first absorbed as the carbonate complex on an anion exchange resin and then determined by X-ray fluorescence. A sensitivity corresponding to 20 ppb in 250 ml solution and a precision of ±6.5% was obtained. The sensitivity was 100-fold greater than that obtained by the direct determination in solution by X-ray fluorescence.