The near quantitative separation, purification, and recovery of 211At has been demonstrated through an extraction chromatography process which utilizes porous beads impregnated with 3-octanone, resulting in an elution yield of 92–95%. Moreover, the rapid nature of this process, <20 min, was achieved after dissolution of a Bi metal target in HNO3 following retrieval from the beamline after α-particle bombardment. The solution was directly loaded onto the column with no volume or acidity adjustment. The column was washed with HNO3 and H2O, and 211At was eluted with ethanol, collecting roughly 87–93% in 1 mL. This process of recovering high purity 211At, in near quantitative yields, represents a significant advance in At separations.