Crystallization of carbon tetrachloride in confined geometries

Abstract

The thermal behaviour of carbon tetrachloride confined in silica gels of different porosities was studied by differential scanning calorimetry. Both the melting point and the low temperature phase transition were measured and found to be inextricably dependant on the degree of confinement. The amount of solvent was varied through two sets of experiments, sequential addition and original progressive evaporation allowing the measurement of DSC signals for the various transitions as a function of the amount of CCl₄. These experiments allowed the determination of the transition enthalpies in the confined state, which in turn allowed the determination of the exact quantities of solvent undergoing these transitions. A clear correlation was found between the amounts of solvent (both free and confined) undergoing the two transitions, demonstrating that the formation of the adsorbed layer t does not interfere with the second transition. The thickness of this layer and the porous volumes of the two silica samples were measured and found to be in very close agreement with the values determined by gas sorption.