Abstract: A gamma-rays measurement method of radionucludes (iodine-131, cobalt-60, etc.) coexisting with radionuclides (nitrogen-13, fluorine-18, cobalt-58, etc.) each emitting a pair of annihilation gamma-rays, particularly in primary water of a nuclear reactor by the use of a gamma-ray spectrometric system which includes a primary detector for detecting the gamma-rays and the one annihilation gamma-rays as pulses, a secondary detector for detecting the other annihilation gamma-rays as pulses, and shield detector for detecting gamma-rays Compton-scattered and escaped from the primary to shield detectors as pulses. The method comprises counting the pulses of the secondary detector in anticoincidence with the pulses of the primary detector, thereby to reject the recording of the annihilation gamma-rays from the primary detector, thus minimizing the annihilation gamma-rays disturbing to the measurement, followed by determining count numbers of the gamma-rays.