Abstract: The procedure for determination of ²³⁵U and ²³⁸U in soil by alpha spectrometry was developed. Several steps involved in this procedure are as follows: conversion of uranium associated with the matrix into acid-soluble form, radiochemical separation of uranium from the components of the sample and other radionuclides, purification of uranium and preparation of the source for measurement. The real separation and purification were preformed by selective anion exchange resin. The results show that the recoveries are relatively high and stable.