The procedure for determination of 238 U, 234 U, 232 Th, 230 Th and 228 Th nuclides by alpha spectroscopy was developed. Nuclides of uranium (U) and thorium (Th) were separated from the soil samples by chromatographic method. In the medium of 8 M nitric acid, U(VI) and Th(IV) were adsorbed on the Dowex 1 anion resin column. However, U(VI) was eluted from column by increasing the used volume of 8 M nitric acid. Th(IV) was eluted from the column with 50 ml HCl 9 M. In order to separate U from other elements in the same with the uranium fraction, the sample solution containing uranium and other elements (Fe, Al, Ca, Mg, Na, K) was dried and dissolved the residue by 10 ml HCl 9 M. The result solution was mounted on the anion exchanger