Different analytical methods for different environmental samples (rock, soil, sediment, plant, waste water, ground water and tap water) which have low activity concentrations are developed for the determination of uranium isotopes to be assured of no contamination or pollution of the environment. Using of non-destructive method based on gamma spectrometer and destructive analysis based on alpha spectrometer. Choice of an accurate and precise technique to get better performance and quality is essential for the results assessment and improvement. A set of different matrices of IAEA reference certified samples were used for method verification. Two separation techniques for 238U, 234U and 235U were used; i) UTEVA extraction chromatography which achieved recoveries higher than 50 %, ranged between 59 and 79 % and ii) TOPO solvent extraction which achieved a chemical recovery lower than that obtained by UTEVA for the same matrices ranged from 26 % and 55 %. From the obtained results a significance difference were shown between UTEVA and TOPO techniques.