An atomic absorption procedure was developed for the determination of titanium and vanadium in medium-purity uranium products (yellow-cakes). Samples equivalent to 4 g uranium were dissolved in 5.5 M nitric acid. Titanium and vanadium were separated from the uranium matrix by column extraction chromatography with the use of tri-<i>n</i>-butyl phosphate (TBP) supported on polytrifluorochloroetylene (Kel-F)® powder. A nitrous oxide-acetylene flame was employed to estimate the concentration of the analytes in the nitric phase. The precision was about 3% relative standard deviation for both elements, with detection limits of 60 μg/g for Ti and 30 μg/g for V. The influence of Al, Fe, and PO<sub>4</sub><sup>3-</sup> on the measured absorbance values and mutual interferences effects between Ti and V were investigated.

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