The recovery of microgram and submicrogram quantities of U by electroplating has been studied, using radioactive U‐233 as a tracer with and without the presence of microgram quantities of natural U as carrier. Optimum results were obtained in an ammonium oxalate medium with electrolysis at 80°–85°C being performed first in acidic solution and then in alkaline solution. A small Pt disk which fitted into a flow counter was used as cathode, and a Pt spiral served as anode. With 20 µg of U carrier present and a volume of 25 ml, an average recovery, based on alpha counting, of was obtained for amounts of U‐233 ranging from 0.03 to 0.13 µg.