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In the chemical and pharmaceutical industries, most processes are carried out in batch or semi-batch mode. The hazard potential and risk of chemical processes are related to reactivity and toxicity of chemicals involved and the process design itself. While the toxicity of the reagents cannot be influenced, the appropriate design of a process is essential to keep the reaction under control at any given time. As there is no steady-state in batch and semi-batch operation, the process dynamics becomes an important factor too and needs to be assessed carefully. Consequently, striving for an intrinsically safe chemical process is the goal of process development.
Calorimetry heat flow screening in a 100ml reaction vessel provides information not found in temperature measurements alone. Data from an exothermic oxidation reaction indicates that reactor temperature (Tr) measurements are not accurate indicators of reaction heat. The reactor temperature minus the jacket temperature (Tr-Tj) underestimates energy release and associated safety consequences. The reaction heat profile (Qr) from heat flow calorimetry tracks the quantitative heat release and is the best indication of future problems even before scaling to a 1 liter.