Uranium is the most common element in the nuclear fuel cycle. Different techniques have been used for analyzing the isotopic composition of uranium. Precise determination of uranium isotopic ratios for an efficient control of nuclear material was carried out through the modification of the used chromatographic method of uranium. Alpha spectrometry was utilized to identify different types of natural, depleted and enriched samples for safeguard purposes. Uranium element was extracted from other interfering radionuclides, purified, electrodeposited on a stainless-steel disc, and measured using alpha-spectrometer, then isotopic ratios were calculated. For comparison purposes, the samples were also measured using a hyper pure germanium (HPGe) spectrometer and the uranium isotopic ratios were obtained. The results obtained by both techniques were in agreement within difference ranged from -8.7 to 12%. It was concluded that alpha spectrometric measurements of uranium isotopes preceded by efficient radiochemical separation using extraction chromatography is a fast and reliable technique for safeguard purposes.