There is an expanded interest for the determination of toxic elements such as arsenic, antimony and mercury in several materials. Many workers have determined these elements in biological materials by combined chemical separation and neutron activation analysis methods. It seems however that arsenic, antimony and mercury have been determined simultaneously only by Samsahl in biological materials and by Kiesel in meteorites. This article, based on previously reported extraction studies, describes a simple and rapid neutron activation analysis method for the simultaneous determination of arsenic, antimony and mercury in biological materials.