A new calorimeter for simultaneous measurement of isotherms and heats of adsorption

A new calorimeter designed for simultaneous measurements of heats and isotherms of gas adsorption and desorption systems is presented. It consists of a volumetric/manometric gas adsorption instrument, the adsorption vessel of which is placed within a second vessel filled with inert gas. This gas acts as a sensor, as not only its temperature but also its pressure is increased if heat is released from the adsorption vessel via the sensor gas to its thermostated surroundings. Indeed, the time integral of the sensor gas pressure signal turned out to be strongly related to the total heat released from the adsorption vessel. A basic theoretical equation of the measurement procedure is given. Results of numerous calibration measurements are presented. The question of what type and amount of sensor gas should be used to achieve high sensitivity of the instrument is discussed. Two examples of measurements of heats of adsorption and adsorption isotherms are given, namely adsorption of N2 on alumina oxide (CRM-BAM-PM-104) at 77 K and CO2 on zeolite Na13X and wessalite DAY both at 298 K.