A solvent extraction process is described for the preparation of very high-purity beryllium compounds. The process involves extraction of beryllium from an aqueous solution containing sufficient ethylenediaminetetra-acetic acid (EDTA) to complex all extractable impurities. The extractant used is a kerosene solution of 2-ethylhexoic acid. Further purification is accomplished by scrubbing the organic phase with 4-M sulfuric acid. The purified beryllium can be removed either with strong aqueous HCl or HF. Fifteen pounds of beryllium sulfate tetrahydrate, to which various impurities were added, were treated by this process in three batches, and converted to ammonium beryllium fluoride of high purity. Analyses of these products are given.