Abstract: The experimental equipment of the neutron activation analysis is improved using MCNP code simulation,and ~(252)Cf neutron source is used as an irradiation source because of its high neutron yield.The nickel concentrates sample and standard samples are irradiated with ~(252)Cf neutron source,and the energy spectroscopes of these samples activated by neutrons are obtained with a HPGe detector.The components and contents of this sample are obtained with the relative measurement method by the energy spectroscopy process.It concluds that the neutron activation analysis method on line can commendably meet the demand of the industry by virtue of a ~(252)Cf neutron source.