(13d) Comparison of the Results From Six Calorimeters In the Determination of the Thermokinetics of a Model Reaction

One of the cornerstones of risk assessment and managing reactive chemistry hazards is to have a thorough and complete understanding of the chemistry of the process under normal operating conditions but also in the case of all potential failures of the system, which was one of the conclusions of the CSB investigation of the T2 Laboratories explosion in December 2007. Other than basic physical and chemical properties, thermo-kinetic data are necessary for evaluating the risk of thermal runaway. This paper deals with the comparison of experimental results from several types of commercially available calorimeters: a screening calorimeter (DSC), a Calvet calorimeter (C80), a reaction calorimeter (RC1), and various pseudo-adiabatic calorimeters (VSP 2, ARSST, and Phi-Tec 1). One exothermic reaction was selected as a case study: the esterification of acetic anhydride by methanol, a system which has been well studied in the literature. This reaction is put to the test in the six calorimeters under similar operating conditions. The objective of this series of tests is to obtain the thermo-kinetics of the reaction with each apparatus and compare the results in terms of reproducibility, precision, userfriendlyness of the test procedure, time, ease of data interpretation, and relevance. The goal is to determine which calorimetric method can be used (or not be used) for what purpose with respect to the reactive chemistry hazard. This approach gives also the opportunity to illustrate and summarize the potential of the experimental tools used in a complete risk assessment of a particular chemical process. The result can also be used in the education field as a simple and complete model of a case study.