In this paper, present the results of the research on the determination and separation urani in gyps, hasinvestigated the optimal conditions for decomposition of 100 g gyps samples requiring 400 ml of H2SO430%. incubate sample for 150 min at temperature of 70 - 90oC, the neutralizing solution to precipitateis NH3 15%, the calcined precipitation temperature at 400oC reaches about 50% urani content, aftertreatment through urani ion exchange column, precipitate reached over 80% urani, same time build onthe extraction, handling and analysis urani content in gyps sample, urani content was 0.74 mg/g, withslight variability, below 5%.Keywords: urani, extraction, analysis, gyps