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A novel stirred microcalorimetric cell for DSC measurements applied to the study of ice slurries and clathrate hydrates

Torré, Jean-Philippe and Plantier, Frédéric and Marlin, Laurent and André, Rémi and Haillot, Didier A novel stirred microcalorimetric cell for DSC measurements applied to the study of ice slurries and clathrate hydrates. (2020) Chemical Engineering Research and Design, 160. 465-475. ISSN 0263-8762

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Official URL: https://doi.org/10.1016/j.cherd.2020.06.019


A novel prototype of a microcalorimetric cell with in-situ stirring has been developed to per-form DSC measurements under atmospheric or pressure conditions. After a brief technical description of the apparatus, preliminary tests are presented which analyzed the influ-ence of the stirrer rotation on the heat-flow signal. Experiments were then performed with complex fluids such as ice slurries and clathrate hydrates formed with cyclopentane and with carbon dioxide. They took place in stirred and non-stirred conditions and the results obtained were then compared. It was proven that the rotation of the microstirrer in the measuring cell does not disrupt the heat-flow signal during the analysis. As regards the prac-tical applications tested, the in-situ stirrer efficiently reduces crystallization metastability, increases the water-to-hydrate conversion, and reduces the amount of time needed for anal-ysis. The dissociation enthalpy of cyclopentane (CP) hydrates was measured at atmospheric pressure; it is effectively very difficult to analyze this system with non-stirred calorimetry techniques because the two liquid phases are immiscible. The experimental results, in good agreement with other data found in the literature, showed complete water-to-CP hydrate conversion within a short period of time using a simple protocol. Experiments were also performed under pressure to demonstrate that CO2 hydrate phase equilibrium data could be obtained rapidly and easily. It is therefore our opinion that the potential of this novel technology has been thoroughly demonstrated.

Item Type:Article
HAL Id:hal-02884590
Audience (journal):International peer-reviewed journal
Uncontrolled Keywords:
Institution:French research institutions > Centre National de la Recherche Scientifique - CNRS (FRANCE)
Other partners > Ecole de Technologie Supérieure - ETS (CANADA)
Université de Toulouse > Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE)
Other partners > KEP Technologies Lyon (FRANCE)
Other partners > Total (FRANCE)
Université de Toulouse > Université Toulouse III - Paul Sabatier - UT3 (FRANCE)
Other partners > Université de Pau et des Pays de l'Adour - UPPA (FRANCE)
Laboratory name:
Deposited On:03 Dec 2020 09:21

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