A laboratory and field evaluation study was done to develop methodology for the measurement of cadmium in stationary source stack emissions. Field evaluations were performed at a municipal solid waste incinerator and a sewage sludge incinerator. The methodology was tested through the laboratory and field sampling validation phases to evaluate precision and accuracy of the proposed method. Colocated, quadruplicate flue gas samples of nominally 30 and 60 dscf in 1 and 2 hours sampling time were collected to assure an adequate cadmium content, a representative sample, and the production of data to validate the method in terms of between-train precision. The overall accuracy and precision of the analysis procedure were 89.2 percent and 1.7 percent, respectively. The detection limit of the atomic absorption instrument was 0.03 ug/mL. The methodology proved to be a reliable sampling approach to determine cadmium emissions from the stationary sources tested.