Base adsorption calorimetry for characterising surface acidity: a comparison between pulse flow and conventional “static” techniques

Abstract

A pulsed flow adsorption microcalorimeter (pulse-FMC) has been developed by modifying a Setaram 111. It is tested in comparison with a conventional pulsed static adsorption microcalorimeter (pulse-SMC) for characterising surface acidity of solid acid catalysts. Small pulses of 1% ammonia in helium are delivered to an activated catalyst sample and its surface acidity is differentially profiled in terms of the molar enthalpy of ammonia adsorption ( Δ H ads ° ) using a combination of differential scanning calorimeter (DSC) and a downstream thermal conductivity detector (TCD). The pulsing action and its sequences are controlled by in-house developed software and the TCD output also is logged into a PC. Thus, the pulse-FMC is fully automated. Two sulfonated polystyrene resin-type catalysts, Amberlyst 15 and Amberlyst 35, a zeolite of the type H +-ZSM-5 (CT 410) and an acid activated clay (Fulcat 220) are characterised at appropriate temperatures using both the new technique and the conventional static base adsorption method. Δ H ads ° versus surface coverage profiles of all the four catalysts obtained from both pulse-FMC and the conventional method are found to be comparable. Results are interpreted in terms of the extent to which NH 3 adsorption on the catalysts surface is under thermodynamic control in the two methods.