Abstract: In this paper,an analytical method based on microwave assisted sample digestion-vapor generation-atomic fluorescence spectrometry was proposed for the determination of arsenic and mercury in naphtha.Digestion parameters and working conditions were optimized.Interferences due to coexisting ions were studied,values of detection limit found were 0.11 μg·L-1 for arsenic and 0.045 μg·L-1 for mercury.Linearity of the calibration curves were in range of 1.0-100 μg·L-1 for arsenic and 0.5-50.0 μg·L-1 for mercury.Values of RSD′s of sample analysis were less than 4% for both arsenic and mercury.Values of recovery were in the ranges of 95.2%-97.2% for arsenic and 92.9%-95.2% for mercury.