Development of In-House Thermoanalytical Tools and Testing Techniques

摘要

In many cases in order to develop safe operating envelopes for process scale-up,rnthermoanalytical information is required for which the corresponding technology doesrnnot exist. Over the years, the Operational Hazards Evaluation Group at Merck hasrndeveloped numerous in-house techniques to provide this required thermoanalyticalrninformation. The techniques, developed in-house, use commercially available technologyrnsuch as Differential Thermal Analysis and Reactive System Screening Tool. Theserntechniques include: a specially designed reusable closed testing cell to contain pressuresrnup to ~500 psi and eliminate corrosive interactions between test materials and the testrncell; small scale techniques to determine exothermic onset temperatures and heats ofrnreactions; a small scale adiabatic Dewar test system to determine the time to thermalrnrunaways; and a gas evolution test cell to determine rates of gas generation during thernstorage of waste solvents.rnThis paper will trace the development, calibration and use of these variousrnthermoanalytical testing techniques and evaluate the unique role they play in therndetermination of a safe operating envelope for Pilot Plant operations.