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Advanced Calorimetric Techniques in Polymer Engineering
Authors:Jean-Pierre E. Grolier  Florin Dan
Affiliation:1. Laboratory of Thermodynamics of Solutions and Polymers, Blaise Pascal University, 63177 Aubière, France;2. Analytical Sciences, The Dow Chemical Company, Midland, MI 48667, USA
Abstract:Summary: In polymer synthesis, reaction calorimetry (RC) is an appropriate technique for on-line process monitoring, since polymerization reactions are highly exothermic. Measurements are noninvasive, rapid, and straightforward. Nowadays RC is the technique recognized as the most powerful way to study such process in near-to-the- industrial conditions. Our approach was focused on temperature oscillation calorimetry (TOC). Two different reaction calorimeters were used, i.e. a isoperibolic calorimeter and a Calvet type high sensitivity differential calorimeter, respectively. A special attention was paid to the interpretation of the measured signals in order to obtain reliable calorimetric data. The evolution of heat transfer coefficient UA was followed by performing appropriate Joule effect calibrations, before and after the reaction. A convolution differential method of the measured heat flow by the generated one was used for determining the time constants and deconvoluting the measured heat flow.
Keywords:heat of reaction  heat transfer coefficient  polymerisation  reaction calorimetry  temperature oscillation
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