Inductively coupled plasma mass spectrometry and thermal ionization mass spectrom - etry were used to measure concentration of uranium and thorium as well as isotopic composition of uranium respectively in soil samples collected around south Serbia. An analytical method was established for a routine sample preparation procedure for uranium and thorium. Uranium was chemically separated and purified from soil samples by anion exchange resin and UTEVA extraction chromatography and its isotopic composition was measured using a thermal ionization mass spectrometry. There was a little deviation of U/Th ratio from the average values in some soil samples. Presence of 236U as well as depleted uranium was observed in 235U/238U ratio measurement in the same soil sample.