The concentration of antimony in nail and hair was determined by thermal neutron activation analysis. Samples were collected from the workers of an antimony refinery, inhabitants near the refinery, and residents in control area. They were irradiated by Kyoto University 5 000 kW Reactor for 1 h, and cooled for 30 to 100 days. After cooling, the concentration of Sb in nail and hair was estimated by measuring the intensity of gamma-ray from 124Sb of the samples, then the samples were washed by 0.1% aqueous solution of nonionic surface active agent in an ultrasonic cleaner. The gamma-ray spectrometry was done again (after washing). The concentration of Sb in nail before washing was 730 ppm for the workers, 2.46 ppm for habitants near the refinery, and 0.19 ppm for the control; after washing, it became 230 ppm for the workers, 0.63 ppm for habitants, and 0.09 ppm for the control. The concentration of Sb in hair before and after washing was 222 ppm and 196 ppm for the workers, and 0.21 ppm and 0.15 ppm for the control, respectively.