ABSTRACT. Within the framework of radioecological studies, 90 Sr was determined in wheat grains, soil, and deposition samples. The radiochemical purification of 90 Y consisted of liquid-liquid extraction by tributyl phosphate (TBP), followed by hydroxide and oxalate precipitations and, if necessary, the removal of thorium by anion exchange chromatography. The procedure proved to be very robust and reliable, having yttrium yields of 92.7 ± 4.6% for 1-kg wheat samples, 90.9 ± 4.2% for 50-g soil samples, and 90.6 ± 3.2% for wet and dry deposition samples. 90 Y was determined by Cerenkov counting and proportional counting. By optimizing the Cerenkov counting window, a figure of merit (FOM) of 4750 could be reached using a Quantulus™ 1220 system. Minimum detectable activities were in the range of 10 mBq.