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A Practical Method to Derive Sample Temperature during Nonisothermal Coupled Thermogravimetry Analysis and Differential Scanning Calorimetry Experiments
Author(s) -
Salvador S.,
Ferrasse J.H.
Publication year - 2006
Publication title -
chemical engineering and technology
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.403
H-Index - 81
eISSN - 1521-4125
pISSN - 0930-7516
DOI - 10.1002/ceat.200600022
Subject(s) - thermogravimetry , crucible (geodemography) , differential scanning calorimetry , thermodynamics , work (physics) , kinetic energy , heat flow , calorimetry , chemistry , atmospheric temperature range , analytical chemistry (journal) , materials science , thermal , physics , chromatography , inorganic chemistry , computational chemistry , quantum mechanics
Nonisothermal thermogravimetry differential scanning calorimetry (TG‐DSC) mounting is intensively used for the determination of kinetic parameters and reaction heat along the chemical transformation of a solid. Nevertheless, when tests are performed with heating rates as high as those encountered in industrial processes, e.g., several tens of K min –1 , there is great uncertainty in the knowledge of the exact sample temperature. In this work, a method to derive a simple mathematical expression is proposed and fully described in order to calculate the real sample temperature throughout a temperature‐ramped test on a commercial apparatus. The furnace temperature and the heat flow signals were used, together with the crucible specific heat and the heating rate. A number of validation tests were performed to derive similar reaction rates for a reference. First‐order kinetic reactions were presented and reconciled over a large range of heating rates from 3 to 50 K min –1 .