A program was undertaken to develop reliable methods for measuring trace elements in emission streams. This program concerns a sampling and analysis method for arsenic, cadmium, chromium, cobalt, manganese, nickel, lead, selenium, and vanaduim. Based upon a review of the literature, atomic absorption spectrophotometry was selected as the analysis method for all metals. To approximate a stationary source, a simulation system consisting of a fuel oil combustion chamber and stack with sampling ports was constructed. Known amounts of metals were introduced to the system as organometallic additives to the fuel. Flue gas sampling was carried out simultaneously with two trains, permitting a direct comparison of changes in configuration, impinger solutions and sample recovery procedures. Based upon relicate experiments, precisions of 7 to 11 percent were obtained for all elements except As (15 percent) and Se (21 percent). Accuracies of Co, Ni, Mn, Cd, Cr and V were within 15 percent at the 100mg level, with Pb being 31 percent high and As and Se being low by 32 and 48 percent, respectively.