Mass attenuation coefficient and linear attenuation coefficient of gamma rays of photons for Ni in the energy range 360- 1330 keV have been determined experimentally through photon–transmission measurement performed under narrow collimated beam counting geometry with scintillation spectrometer as a photon detector. The Mass attenuation coefficient and linear attenuation coefficient values reported in this work are found to be in good agreement with the values computed theoretically. These values represent a subject of considerable interest and importance, since it is required in solving various problems in a radiation physic and radiation dosimetry and of interest for industrial, biological, agriculture and medial studies.