Carbon beds are increasingly used as a mode for suppression of volatile organic vapors from process streams for environmental control. Many incidents of spontaneous combustion of such beds have been reported. This is primarily due to operation under conditions where heat gains from oxidation of the adsorbed material on the high surface area carbon out pace any heat losses via conductive or convective mechanisms. In this paper we will discuss calorimetric methods for quantitation of the oxidation heats as well as heat loss and balance calculations to aid in developing safe operating discipline for successful use of this valuable technology for pollution control.