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Original Articles

Design, Calibration, and Testing of a New Tian-Calvet Heat-Flow Microcalorimeter for Measurement of Differential Heats of Adsorption

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Pages 455-475 | Received 15 Dec 2007, Accepted 02 May 2008, Published online: 29 Jul 2008
 

Abstract

A Tian-Calvet heat-flow microcalorimeter system is described for measurement of heats of adsorption and reaction on porous solids. Heat-flow signals are measured in transducer assemblies consisting of several hundred Seebeck-effect thermoelements connected in series and arranged in a square configuration. These transducers surround a stainless steel calorimeter cell connected to a high-vacuum volumetric adsorption system. The sensitivity of the calorimeter was calibrated by measurement of electric response and of heats of adsorption for known processes. Microcalorimetric measurements have been conducted at temperatures from 273 to 298 K. The calorimetric cell described here facilitates sample handling under controlled atmosphere conditions, allowing the study of freshly treated materials and samples that have been exposed to catalytic reaction conditions.

ACKNOWLEDGMENTS

The authors thank the Departments of Chemistry of Universidad Nacional de Colombia, Universidad de Los Andes (Colombia) and Universidad Nacional de San Luis (Argentina) and the Master Agreement established between these institutions. Special gratitude as extend Fondo Especial de Investigaciones de la Facultad de Ciencias de la Universidad de Los Andes (Colombia) for its partial financing.

Notes

∗Each reported value corresponds to the mean value of 20 measures and a certainty of 95%.

∗Each reported value corresponds to the mean value of 20 measures and a certainty of 95%.

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