The accurate and rapid determination of radionuclides in soil is very important to monitor the radioactivity of radionuclides for reduction of hazardous effects to human health. Here, a sequential separation method with a fusion technique was developed to separate uranium and thorium isotopes from a soil sample using polymer resins (UTEVA (R) and TEVA (R)) packed columns. The radioactivity of separated U and Th was measured using alpha particle spectrometry. The developed method was evaluated by assessing the key validation parameters of the selectivity, radioactivity range of linearity, scores for quality control, accuracy, tracer recovery yield, and quantification of uncertainty. The method offered a fast analysis of U and Th isotopes of the soil samples with very high chemical recovery yield and the effective removal of interferences, and demonstrated a satisfactory quality level for the selected criteria of the performance for the method validation. The developed method might be promising for use in a determination of the radioactivity of solid samples containing various interferences. (C) 2016 Elsevier B.V. All rights reserved.