Abstract. A method for the preparation of beryllium oxide of high purity is presented. Beryllium basic acetate (BeO-3Be(C2H3O2)2) is prepared from the metal or a convenient salt, a chloroform solution of this material extracted with redistilled water, the dried basic acetate distilled in a quartz apparatus, and this purified material converted to the oxide by fuming down with sulfuric acid and igniting at 1000 degrees C. Impurities detectable spectrographically were reduced to a very low level.