A procedure for the simultaneous determination of tellurium and uranium is described. The procedure utilizes thermal neutron activation, followed by sample combustion and a gas phase separation of the volatile radionuclides of interest. This method is sensitive enough to permit the measurement of tellurium and uranium at their naturally occurring levels in materials of biological and environmental origin. The procedure has been successfully employed to determine the tellurium and uranium concentrations in three Standard Reference Materials (SRM's) currently being offered by the National Bureau of Standards, and in atmospheric particulate material collected in rural Maryland.