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See detailIn situ FTIR micro-spectroscopy to investigate polymeric fibers under supercritical carbon dioxide: CO2 sorption and swelling measurements
Champeau, Mathilde; Thomassin, Jean-Michel ULg; Jérôme, Christine ULg et al

in Journal of Supercritical Fluids (2014), 90

An original experimental set-up combining a FTIR (Fourier Transformed InfraRed) microscope with a high pressure cell has been built in order to analyze in situ and simultaneously the CO2 sorption and the ... [more ▼]

An original experimental set-up combining a FTIR (Fourier Transformed InfraRed) microscope with a high pressure cell has been built in order to analyze in situ and simultaneously the CO2 sorption and the polymer swelling of microscopic polymer samples, such as fibers, subjected to supercritical carbon dioxide. Thanks to this experimental set-up, we have determined as a function of the CO2 pressure (from 2 to 15 MPa) the CO2 sorption and the polymer swelling at T = 40 °C of four polymer samples, namely PEO (polyethylene oxide), PLLA (poly-l-lactide acid), PET (polyethylene terephtalate) and PP (polypropylene). The quantity of CO2 sorbed in all the studied polymers increases with pressure. PEO and PLLA display a significant level of CO2 sorption (20 and 25% respectively, at P = 15 MPa). However, we observe that a lower quantity of CO2 can be sorbed into PP and PET (7 and 8% respectively, at P = 15 MPa). Comparing their thermodynamic behaviors and their intrinsic properties, we emphasize that a high CO2 sorption can be reach if on one hand, the polymer is able to form specific interaction with CO2 in order to thermodynamically favor the presence of CO2 molecules inside the polymer and on the other, displays high chains mobility in the amorphous region. PLLA and PEO fulfilled these two requirements whereas only one property is fulfilled by PET (specific interaction with CO2) and PP (high chains mobility). Finally, we have found that for a given CO2 sorption, the resulting swelling of the polymer depends mainly on its crystallinity. [less ▲]

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See detail“One-pot” dispersion ATRP and alkyne-azide Huisgen’s 1,3-dipolar cycloaddition in supercritical carbon dioxide: towards the formation of functional microspheres
Grignard, Bruno ULg; Calberg, Cédric ULg; Jérôme, Christine ULg et al

in Journal of Supercritical Fluids (2010), 53(1-3), 151-155

Functional polymers were successfully prepared in scCO2 by combining alkyne-azide 1,3-dipolar Huisgen’s cycloaddition and dispersion ATRP in a “one pot” process using new perfluorinated polymeric amino ... [more ▼]

Functional polymers were successfully prepared in scCO2 by combining alkyne-azide 1,3-dipolar Huisgen’s cycloaddition and dispersion ATRP in a “one pot” process using new perfluorinated polymeric amino-based ligands that had a dual role, i.e. the complexation of the copper catalyst and the stabilization of growing particles. [less ▲]

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See detailThe supercritical micronization of solid dispersions by Particles from Gas Saturated Solutions using experimental design
Brion, Michaël ULg; Jaspart, Séverine ULg; Perrone, Leonardo et al

in Journal of Supercritical Fluids (2009), 51(1), 50-56

The Particle from Gas Saturated Solutions process was successfully used to micronize solid dispersions containing hydrophilic carriers and a new chemical entity, YNS3107. By means of experimental design ... [more ▼]

The Particle from Gas Saturated Solutions process was successfully used to micronize solid dispersions containing hydrophilic carriers and a new chemical entity, YNS3107. By means of experimental design, the effects of several experimental parameters on micronization were investigated. Within the chosen experimental conditions, the results showed that the autoclave temperature, autoclave pressure, drug loading, flow rate of carbon dioxide and air pressure were significant parameters. During the optimization step, the most relevant parameters of the screening were optimized using a central composite design meanwhile other factors were kept constant. Optimal conditions were used to produce microparticles with a volume weighted mean diameter of 30.4 µm. The closeness between the measured and predicted response, evaluated at 28.1 µm, demonstrated the validity of the statistical analyses. Finally, an enhancement of the rate of dissolution of YNS3107 in the solid dispersion microparticles was measured using USP II dissolution test apparatus. [less ▲]

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See detailOptimisation of SFE method on-line coupled to FT-IR spectroscopy for the real-time monitoring of the extraction of tagitinin C in T-diversifolia
Ziemons, Eric ULg; Mbakop, N. W.; Rozet, Eric ULg et al

in Journal of Supercritical Fluids (2007), 40(3), 368-375

The monitoring in real time of dynamic extractions of tagitinin C from Tithonia diversifolia leaves was carried out with a home made high-pressure fiber optic cell which coupled a supercritical fluid ... [more ▼]

The monitoring in real time of dynamic extractions of tagitinin C from Tithonia diversifolia leaves was carried out with a home made high-pressure fiber optic cell which coupled a supercritical fluid extractor with carbon dioxide as the extraction medium and a FT-IR spectrometer equipped with a mercury cadmium telluride detector (MCT). The shape of extraction curves obtained during the monitoring was used to decide when to stop the supercritical fluid extraction (SFE). No significant density dependence of the molar absorption coefficient or wavenumber of the C=O stretching vibration (v(C=O)) of tagitinin C at 1668 cm(-1) was noticed. The physical characteristics of SCCO2 governing the extraction yield of the active component from leaves were optimized by means of a central composite design (CCD). The studied variables were temperature (40, 60 and 80 degrees C) and pressure (8.0, 14.0 and 20.0 MPa) of the supercritical fluid. The composition profile of T diversifolia extracts obtained by SFE was investigated in the range from 3400 to 2600 cm-1 according to the pressure and temperature conditions of SCCO2. The qualitative approach of the extracts composition was accomplished through the CH stretching vibrations of components. [less ▲]

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See detailSupercritical carbon dioxide extraction of tagitinin C from Tithonia diversifolia
Ziemons, Eric ULg; Goffin, Eric ULg; Lejeune, Robert ULg et al

in Journal of Supercritical Fluids (2005), 33(1), 53-59

Different parameters as temperature, pressure, solvent mass and sample granulometry governing the extraction yield of tagitinin C from the aerial parts of Tithonia diversifolia were optimised. An ... [more ▼]

Different parameters as temperature, pressure, solvent mass and sample granulometry governing the extraction yield of tagitinin C from the aerial parts of Tithonia diversifolia were optimised. An experimental design was carried out to map the effects of pressure (at 20.3, 30.4 and 40.5 MPa) and temperature (at 40, 60 and 80degreesC) on the extraction yield of the active component and to determine the optimal conditions for the extraction of tagitinin C from T diversifolia. The best conditions are met for a pressure of 35.0 MPa and a temperature of 68degreesC. The effect of the particle size was studied under low pressure (13.7 MPa) and temperature (40degreesC) conditions, which failed to extract quantitatively the tagitinin C from leaves sieved to 250 mum size. The reduction of the particle size increased the extraction yield which became comparable to that of the optimised SFE for the particle in the range of 0-63 mum. From the analysis of extraction kinetic curves of 200 mg of plant with supercritical carbon dioxide (range of 5-30 g), it appears that 15 g of this supercritical fluid is never limiting. The optimised supercritical fluid extraction (SFE) was compared favourably to Soxhlet extraction with dichloromethane (S) and to maceration followed by lixiviation with diethyl ether (ML), which gave similar extraction yields but higher extract content of tagitinin C were found using SFE (15.6 and 30.7% w/w tagitinin C in S and ML extracts, respectively, versus 52.8% in SFE extract). [less ▲]

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