Neutron activation analysis (NAA) is an elemental analysis technique, which is based on the excitation of the atomic nucleus of an isotope of element with neutrons, and the emission of the specific gamma rays from the excited nucleus by decay. Due to the absence of a blank and less matrix contribution, NAA is therefore suitable for the analysis of biomedical materials, and has been successfully applied for trace element biomedical study and clinical analysis. A nuclear reactor is normally used as a neutron source for the determination of trace elements; the produced radionuclides are then measured by a gamma detector consisting of a germanium detector and a gamma spectrometry system. The theory, equipment and detailed methodology, and analytical quality assurance are discussed in this article. Some applications are also highlighted.