The physical and chemical properties of particles collected from the eruption fume of Kilauea, Mayon, and Arenal volcanoes were determined by colorimetric chemical techniques, neutron activation, atomic absorption, X‐ray diffraction, an electron microprobe, and electron microscopy. As in previous studies, more than 95% of the Kilauea particles were largely dilute sulfuric acid droplets plus some mainly needle‐like crystals, which previously had been tentatively identified as sulfur and calcium and ammonium sulfates. The wet chemical analysis demonstrated the presence of soluble calcium, ammonium, and magnesium sulfates. Each type of particle observed at Kilauea was also observed at Mayon, but most of the droplets from Mayon were much less acidic. Some Mayon particles were ‘ash’ or minute spheres; this type of particle was not observed at Kilauea. Particles in the fume from Arenal were more like the particles from Mayon than like those from Kilauea.