Alpha spectrometry using pulse height analysis has been used for the determination of uranium concentrations in different environmental samples. The concentration of ²³⁸U was measured by both destructive and non-destructive techniques with a detection limit of less than 1.8 mBq/kg. However, because of the extremely low ²³⁴U concentrations in environmental samples, it was necessary to use a destructive technique to separate U from the sample matrices as well as remove interfering elements from the sample solution to determine ²³⁸U/²³⁴U ratio. In this study, the uranium was separated from the environmental samples using anion exchangers in (Dowex 1 × 8 Cl^? form) and purified via co-precipitation with Lanthanum fluorides (LaF₃) and the alpha source prepared by electrodeposition. The results obtained were validated using some certified reference samples.