The coal-fired electric utility generation industry has been identified as the largest anthropogenic source of mercury (Hg) emissions in the United States. One of the promising techniques for Hg removal from flue gas is activated carbon injection (ACI). The aim of this project was to liberate Hg bound to fly ash and activated carbon after ACI and provide high-quality coal combustion products for use in construction materials. Both bench- and pilot-scale tests were conducted to liberate Hg using a thermal desorption process. The results indicated that up to 90% of the Hg could beliberated from the fly ash or fly-ash-and-activated-carbon mixture using a pilot-scale apparatus (air slide) at 538 °C with a very short retention time (less than 1 min). Scanning electron microscope (SEM) evaluation indicated no significant change in fly ash carbon particle morphology following the thermal treatment. Fly ash particles collected in the baghouse of the pilot-scale apparatus were smaller in size than those collected at the exit of the air slide. A similar trend was observed in carbon particles separated from the fly ash using froth flotation. The results of this study suggest a means for power plants to reduce the level of Hg in coalcombustion products and potentially recycle activated carbon while maintaining the resale value of fly ash. This technology is in the process of being patented.