This study investigated the analytical data of metal components and leaching properties of petroleum fly ash from a U thermal power plant. Metal components in the crude oil differed according to the place of production, where it was concentrated as metal oxide type in fly ash containing V, Ni and so on. Valuable metal components of fly ash were treated as a second resource. From this point of view, our study carried out leaching, with hydrochloric acid and sulfuric acid of different concentrations in series being used as leachant. Leaching solution obtained a solid-liquid ratio of 1:5 at room temperature. Even though dilute acids and water were used as leachant, high concentration of various metal ions could be leached from fly ashes. The concentration of V and Ni in leaching solution was 40,000 ppm, and Ga content was 8,000 ppm. These basic data will be useful for any process for recovery and separation of rare metals in waste.