Radionuclidic purity tests of (18)F radiopharmaceuticals (Na(18)F and fluorodeoxyglucose [(18)F]FDG) and radionuclide composition analysis of irradiated water [(18)O]H2O were performed. The measurements were conducted using a High-Purity Germanium (HPGe) detector and a liquid scintillation counter. Radionuclide identification and activity measurements were performed for samples from different stages of the production process. Most of the impurities were detected on QMA (quaternary methylammonium) anion exchange columns and in liquid wastes. Using liquid scintillation counting, the activity of (3)H resulting from the (18)O[p, (3)H](16)O reaction was determined. It was shown that all of the impurities were efficiently determined and eliminated in the radiopharmaceuticals synthesis process and that the final products meet the requirements set by relevant regulations.