Microgram quantities of thallirum in meteorites, rocks, minerals, alloys and biological samples have been analyzed by rapid neutron activation analysis. A l0-minute radiochemical separation procedure coupled with a gas-flow proportional detector for 4.2-minute half life measurement and a gamma or beta scintillation detector placed in close proximity to the sample permitted detection of the 4.2-min Tl206. Samples were irradiated for 10-minutes at a thermal neutron flux of approximately $0.95{ imes}10^{11}$ neutron-$cm^{-2}-sec^{-1}.$ The low limits of detection was about $10^{-7}$ gm of thallium.