Abstract: The invention relates to a method of and apparatus for the regregation of radioactive iodine isotopes from fluid samples. The method consists in leading the degassed and in certain cases also otherwise prepared sample into a column filled with an amorphous solid medium for binding quantitatively the cations, fluoride anions and contaminations of colloidal state, then the effluent flow continuously through an energy-selective gamma detector and continuously recording the signals generated in the detector by the radioactive iodine isotopes. The proposed apparatus comprises a sampling unit (MV), a degassing vessel (G), fluid transfer pumps (P1, P2), pipings, cocks (CS), a bubble removing cell (BC), a column (K) with amorphous material filling, an energy-selective detector system (GD) for measuring gamma radiation, and a signal processing and recording unit (JR).