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J. SempereUniversitat Ramon Institut Químic de Sarrià Llull Via Augusta, 390 08017 Barcelona Spain Llull Via Augusta, 390 08017 Barcelona Spain

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R. NomenUniversitat Ramon Institut Químic de Sarrià Llull Via Augusta, 390 08017 Barcelona Spain Llull Via Augusta, 390 08017 Barcelona Spain

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E. SerraUniversitat Ramon Institut Químic de Sarrià Llull Via Augusta, 390 08017 Barcelona Spain Llull Via Augusta, 390 08017 Barcelona Spain

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J. SalesUniversitat Ramon Institut Químic de Sarrià Llull Via Augusta, 390 08017 Barcelona Spain Llull Via Augusta, 390 08017 Barcelona Spain

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Abstract  

A small scale (100 mL) calorimeter is developed. It includes a glass vessel submerged in a thermostatic bath, a compensation electrical heater, and a control system. The typical operation mode consists on introducing the solvents and part of the reactants into the vessel, to stabilise a temperature of the bath (T j) some degrees below the desired process temperature (T p) and to adjust the reaction mass temperature (T r) to T p using the electrical heater. An oscillating set point is established for Tr, which produces an oscillating response of the applied compensation power (Q c). Finally, the rest of reactants are dosed to the vessel. A small deviation of T r and T p is observed. Even though it can be avoided improving the tuning of the controller, it can be useful for enhancing the calculation of the heat capacity of the reaction mixture (C P). The signals of T r, Q c and T j are processed on-line using the FFT (Fast Fourier Transform) method as the mathematical tool used to analyse the data obtained, producing accurate values of the heat evolved (Q c) by the process, the heat transfer coefficient (UA), and the heat capacity of the reaction mixture (C P).

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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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