The combined use of photon activation and γ-γ coincidence spectrometry is described for the useful and selective nondestructive determination of nickel in geological materials. This method is characterized by the utilization of the nuclide emitting β+ particles in its decay and γ-γ coincidence counting with two gates: one for the annihilation photopeak region and the other for the higher Compton plateau region. The practical detection limits by this method for nickel, arsenic, rubidium, sodium and scandium in silicate matrices could be set at 2.0, 1.2, 9.0, 110 and 1.4 μg, respectively.