Studies were performed to compare the physical and chemical characteristics and the in vitro macrophage cytotoxicity of oil and coal fly ash. Sampling methodology was developed to collect size-fractionated particulate matter from the smokestack of either a coal-fired or an oil-fired power plant. Morphological studies demonstrated particle heterogeneity, although most coal fly ash particles appeared to be spherical. Oil fly ash contained two major morphologies; nonopaque amorphous particles and opaque amorphous particles. Elemental analysis indicates that the coal ash is predominantly composed of aluminosilicate particles, while the oil ash is predominantly inorganic sulfates and carbonaceous particles. In vitro macrophage assays demonstrate that the finest coal fly ash particles are the most cytotoxic; the cytotoxicity is significantly less than that of alpha-quartz, the positive control particle. In contrast, the oil fly ash particles are more cytotoxic than quartz. The cytotoxicity of oil fly ash is due to soluble components, possibly vanadium salts.