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Abstract  

Commercial humic acid (HA) was anchored onto silica gel (SiAPTS) previously modified with 3-aminopropyltrimethoxysilane (APTS). HA was anchored onto SiAPTS through two routes: adsorption and covalent chemical immobilization onto the surface. The adsorption occurred by adding SiAPTS to HA in an aqueous solution, producing SiHA1, while chemical immobilization was performed by reacting HA suspended in N,N-dimethylformamide with SiAPTS, to yield SiHA2. The infrared spectra confirm HA immobilization using both procedures and the termogravimetric results showed that the anchored compounds have significantly thermal stability increased. While natural HA presents a thermal stability up to 200C, the anchored compound presents a thermal stability near to 750C.

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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
Authors: R. Nomen, M. Bartra, J. Sempere, E. Serra, J. Sales, and X. Romero

Summary  

Estimation methods developed over years by S. W. Benson and co-workers for calculation the thermodynamic properties of organic compounds in the gas phase are applied to a pharmaceutical real process with all type of non-idealities. The different strategies used to calculate the reaction enthalpy of a chemical process, in the absence of data for complex molecules, using the Benson group additivity method are presented and also compared with the experimental value of reaction enthalpy obtained using reaction calorimetry (Mettler-Toledo, RC1). We demonstrate that there are some strategies that can be followed to obtain a good estimation of the reaction enthalpy in order to begin the safety assessment of a chemical reaction. This work is part of an industrial project [1] in which the main objective was the risk assessment of chemical real and complex processes using the commonly available tools for the SMEs (with limited resources).

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