A method is described for the simultaneous determination of trace As and Hg in iron ores by microwave-assisted digestion-Chemical Vapor Generation-Atomic Fluorescence Spectrometry. This method gives a rapid simultaneous determination for both As and Hg which is based on methods of determination of As and Hg separately and reduces the detection limit of Hg. The low cost and easy operation of the method make it attractive for routine analysis of trace As and Hg in iron ores.