Triboelectrostatic separation has been investigated as a method for separating unburned carbon from coal combustion fly ash. It was found that when a fly ash is exposed to moisture before it undergoes separation, the charging properties of the components of the fly ash change significantly. The mineral and carbon components of the fly,ash appear to charge oppositely to how they were charged before exposure to moisture. A correlation was found between the degree of charge reversal and the relative amounts of leachable ions, especially calcium and sodium ions, present on the surface of the ash.