Authors:
Christelle HermanTransfers, Interfaces and Processes Department, Chemical Engineering Unit, Université Libre de Bruxelles, 50 Avenue Franklin D-Roosevelt, CP 165/67, 1050, Brussels, Belgium

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Tom LeyssensInstitute of Condensed Matter and Nanosciences, Université Catholique de Louvain, 1 Place Louis Pasteur, 1348, Louvain-La-Neuve, Belgium

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Valérie VermylenUCB Pharma, 60 Allée de la Recherche, 1070, Braine l’Alleud (Brussels), Belgium

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Véronique HalloinTransfers, Interfaces and Processes Department, Chemical Engineering Unit, Université Libre de Bruxelles, 50 Avenue Franklin D-Roosevelt, CP 165/67, 1050, Brussels, Belgium

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Benoît HautTransfers, Interfaces and Processes Department, Chemical Engineering Unit, Université Libre de Bruxelles, 50 Avenue Franklin D-Roosevelt, CP 165/67, 1050, Brussels, Belgium

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Abstract

This article focuses on the development of an innovative method, based on thermodynamic considerations and with the use of Differential Scanning Calorimetry (DSC), for the estimation of the melting enthalpy of crystalline compounds which are metastable near their melting temperature. The curves obtained, at various heating rates, are analysed in two steps. In the first step, the area of a zone generated by the melting endothermic peak is calculated following a specific method. In the second step, the melting enthalpy is extracted from this area through an enthalpy balance. This method is applied to both identified crystallographic forms, named form I and form II, respectively, of Etiracetam (UCB Pharma). The results show that the melting enthalpy of the stable form II compare well with the ones obtained using conventional methods. The curves of the metastable form I present thermal instabilities (partial solid–solid polymorphic transition and beta-recrystallization) near the form I melting peak leading to difficulties for a direct determination of the melting enthalpy by conventional methods. The proposed method is therefore very useful for the estimation of the form I melting enthalpy.

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Journal of Thermal Analysis and Calorimetry
Language English
Size A4
Year of
Foundation
1969
Volumes
per Year
1
Issues
per Year
24
Founder Akadémiai Kiadó
Founder's
Address
H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
Publisher Akadémiai Kiadó
Springer Nature Switzerland AG
Publisher's
Address
H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
CH-6330 Cham, Switzerland Gewerbestrasse 11.
Responsible
Publisher
Chief Executive Officer, Akadémiai Kiadó
ISSN 1388-6150 (Print)
ISSN 1588-2926 (Online)

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Author:
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