An analytical procedure has been developed for the age determination of highly enriched uranium samples exploiting the mother/daughter pair 235U/231Pa. Protactinium is separated from bulk uranium through highly selective sorption to silica gel and is subsequently quantified using alpha-spectrometry. The method has been validated using uranium standard reference materials of known ages. It affords decontamination factors exceeding 2.5 x 10(7), overall recoveries in the range of 80-85%, and a combined uncertainty below 5%.