[en] A procedure was developed for separating rubidium from irradiated aluminum encapsulated uranium. The separations procedure produces a final ultra-high purity RbCl product for subsequent high performance mass spectrometric analysis. The procedure involves first removing most of the macro-components and fission products by strong base anion exchange using, first, concentrated HCl, then oxalic acid media and second, selectively separating rubidium from alkaline-earth ions and other alkali-metal ions, including cesium, using Bio-Rex-40 cation-exchange resin. The resultant RbCl is then put through a final vacuum sublimation step. Ultra-pure reagents and specially clean glassware are used throughout the procedure to minimize contamination by naturally-occurring rubidium