The objective of this study was to investigate the possibility of the classification and triboelectrostatic separation of unburned carbon from coal fly ash for fly ash recycling. By examining the physical properties of unburned carbon and fly ash, several separation schedules were developed. A special type of cyclone with guide vanes was designed to purify the fly ash by size separation. Swirling motion of particles inside the cyclone provides tribocharging of particles, in turn, recleaning of the fine stream could by realized by subjecting the cyclone overflow to an electric field. Also, a better separation was obtained by incorporating the electric force inside the cyclone. Separately, a triboelectrostatic system was tested to evaluate the operating variables for collecting information required for scale-up to a commercial unit.