Differential pulse polarography was employed for the determination of arsenic in bituminous coal from Figueiras, Parana, Brazil. The dried coal sample was crushed to -100 mesh, ashed, and treated with reducing reagents in acidic media. The arsine generated was collected and selectively oxidized to Al +3 using an absorbing solution of 0.1 mol.L -1 [tris(hydroxymethyl) aminomethane] ( TRIS) and 0. 002 mol.L -1 silver nitrate. A solution of TRIS and hydrochloric acid, pH -1, was used as supporting electrolyte for differential pulse polarographic determination of Al+3 in the concentration range 0.05 -0.60 μglmL. The average arsenic concentration found was 69.0 ± 2.6 mg.kg -1 and was in agreement with the spectrophotometric method using silver-diethyldithiocarbamate-pyridine.