Sulphur isotopic compositions of pyrite, anhydrite and native sulphur in volcanic ashes discharged by the 1979 eruption of Ontake volcano, Nagano, Japan were determined. The isotopic data indicate that sulphate in anhydrite and a part of native sulphur were produced by the disproportionation reaction of sulphite formed by dissolution of SO₂ in volcanic gases into water which filled a mud reservoir probably located just below the crater zone. Some part of H₂S in volcanic gases was fixed as pyrite and some was oxidised to form native sulphur. Hydrothermal alteration of country rocks to form pyrite, anhydrite and clay minerals had proceeded in the mud reservoir before eruption at temperatures ranging from 110° to 185°C which were estimated by oxygen isotopic fractionation between anhydrite and water.