Carbon dioxide is one of the most important greenhouse gases causing global warming. It has been estimated that approximately 40 percent of carbon dioxide created by human activities is emitted from fossil fuel-fired power plants. To minimize the undesirable impact of carbon dioxide emissions on the environment, many new technologies are being developed to reduce its emissions from the use of fossil fuels. One of new technologies is the multi-cyclic carbonation and calcinations reaction (CCR) process, which utilizes a calcium-based sorbent in a high temperature reaction (carbonation) to capture the CO2 from the flue gas stream and releases a pure stream of CO2 in the subsequent calcination reaction that can be sequestered. A sub-pilot scale facility utilizing coal combustion at 20 pounds per hour has been established at Ohio State University for the purpose of demonstrating the CCR process. A number of calcium-based sorbents were tested at this facility. Several factors such as residence time and Ca/C ratio were investigated. Over 90% CO2 capture and near 100% SO2 capture has been achieved on a once-through basis.