Trace analysis methods have been developed for determining thallium, lead and bismuth. Proton or deuteron activation is used followed by a radiochemical separation of the reaction products:203Pb from thallium,206Bi from lead, and207Po from bismuth. Activation curves are presented for different nuclear reactions occuring on the elements studied. Determinations have been carried out on high purity samples containing varying amounts of thallium, lead, and bismuth. Based on experimental data, the detection limits are estimated at 0.01 ppm for lead, and 0.001 ppm for thallium and bismuth, respectively.