A simple and rapid method for the extraction is described for the separation of beryllium (II) and aluminium (III) from aqueous sulphate solution with Bis-2 ethylhexyl phosphoric acid (HDEHP) in toluene. A systematic study of the solvent extraction of chemically similar elements, beryllium (II) and aluminium (III) was carried out separately and it has been observed that under certain specific conditions beryllium (II) and aluminium (III) can be separated in a short period from their mixture using HDEHP as an extractant.