Search results for "supercritical fluid"
showing 10 items of 166 documents
Supercritical fluid chromatography in drug analysis: A literature survey
1996
The applications of supercritical fluid chromatography to the analysis of drugs have been carefully revised from the literature compiled in the Analytical Abstracts until March 1994. Easy-to-read tables provide useful information about the state-of-the-art and possibilities offered by SFC in pharmaceutical analysis. The tables comprise extensive data about samples analyzed, pharmaceutical principles determined, solvents used and sample quantity injected, supercritical fluids and modifiers employed, injection system, instrumentation, experimental conditions for chromatographic separations (density, pressure, flow, temperature), characteristics of columns employed (type, support, length, diam…
Supercritical fluid extraction of resveratrol from grape skin of Vitis vinifera and determination by HPLC
2000
Supercritical fluid extraction of resveratrol from grape skin of Vitis vinifera was studied. Extraction variables such pressure, modifier concentration (ethanol), and extraction time were optimised. Final extraction conditions were: 40 degrees C, 150 bar, 7.5% ethanol and extraction time 15 min. Extraction recovery and precision (variation coefficient between 0.2 and 1.0%) were calculated. The resveratrol content in the ethanolic extract was determined by HPLC with UV detection at 306 nm. Acetic acid-methanol-water was used as the mobile phase, and C-18 and C-8 columns were tested, instrumental parameters were optimised, and analytical parameters were calculated (lineal interval 0-75 mg l(-…
Influence of the pH on the ZnO nanoparticle growth in supercritical water: Experimental and simulation approaches
2014
Abstract In order to improve the knowledge on the nucleation and the growth mechanisms of metal oxides nanoparticles produced in supercritical water domain, ZnO was used as a “model” material. A continuous process of hydrothermal synthesis was employed to synthesize ZnO nanopowders ( T = 410 °C and P = 305 bar) from Zn(NO 3 ) 2 and KOH solutions with different values of [KOH]/[Zn(II)] ratio from 0 to 8 in order to investigate the pH effect on the growth of ZnO nanocrystallite in terms of size and morphology. The samples were characterized by X-Ray Diffraction and Transmission Electronic Microscopy. ZnO crystal was considered as a cylindrical crystallite with a diameter D and height H . Es…
Analysis of Dissolved-Gas Atomization: Supercritical CO2 Dissolved in Water
2010
Supercritical dissolved-gas atomization is an atomization process in which carbon dioxide at temperature and pressure above its critical point is used as the atomizing gas. The spray characteristics in terms of droplets size and distribution have been experimentally studied using a laser diffraction method based on a Malvern apparatus. The main parameter that influences the droplets size is the gas-to-liquid mass ratio (GLR); the injection pressure in the range of 7.4-13 MPa has a minor effect. Upon variation of the GLR from 0.5 to 3, the droplet mean diameter changes from about 8.0 to 2.0 μm; very narrow droplet size distributions are also produced. From the point of view of the atomizatio…
Copolymerization of VDF and HFP in Supercritical Carbon Dioxide: A Robust Approach for Modeling Precipitation and Dispersion Kinetics
2012
A kinetic model is developed for the heterogeneous free-radical copolymerization of vinylidene fluoride and hexafluoropropylene in supercritical CO 2. The model accounts for polymerization in both the dispersed (polymer-rich) phase and in the continuous (polymer-free) supercritical phase, for radical interphase transport, diffusion limitations, and chain-length-dependent termination in the polymer-rich phase. A parameter evaluation strategy is developed and detailed to estimate most of the kinetic parameters a priori while minimizing their evaluation by direct fitting. The resulting model predictions compare favorably with the experimental results of conversion and MWD at varying monomer fe…
Copolymerization of vinylidene fluoride and acrylic acid in supercritical carbon dioxide
2009
The free-radical copolymerization of vinylidene fluoride (VDF) and acrylic acid (AA) was carried out in supercritical carbon dioxide using both precipitation and dispersion techniques in the presence of an ammonium carboxylate perfluoropolyether compound. Formation of a copolymer was confirmed by variable contact time CP MAS NMR spectroscopy. Macromolecular matrices were significantly enriched in AA with respect to the initial feed composition and we found that the nonfluorinated monomer has a much higher reactivity ratio with respect to VDF. The cumulative concentration, crystallinity, and water affinity of the synthesized copolymers could be modified changing the initial feed composition,…
Polymerization of methyl methacrylate through ionizing radiation in CO2-based dense systems
2000
Herein, we report the use of ionizing radiation to induce a dispersion polymerization reaction in dense CO2. As a model system, the polymerization of methyl methacrylate in the presence of poly(dimethylsiloxane) stabilizers was investigated. It was demonstrated that the dose plays the key role in the progress of the reaction and in the morphology of the resulting polymer. Dispersion polymerization carried out in the presence of mono- and bifunctionalized surfactants gave differently structured polymers. The polymers obtained have been characterized by scanning electron microscopy, solubility tests, and gel permeation chromatography, and the molecular structure has been related to dynamic me…
Polymer Synthesis in Supercritical Carbon Dioxide
2003
It is current opinion of most of the people involved in supercritical fluids (SCFs) technology that as the end of the twentieth century has been devoted to enlarge exploitation of compressed gases in separation processes the beginning of the twenty-first will be mainly aimed to improve their utilisation as solvents for reactions.
Continuous hydrothermal synthesis of inorganic nanopowders in supercritical water: towards a better control of the process
2009
International audience; A hydrothermal synthesis process working in supercritical conditions (T > 374 °C, P > 22 MPa) and in a continuous mode has been developed for inorganic nanopowder synthesis. This paper presents a review of the past 5 years of research conducted on this process. Numerous materials (oxides: ZrO2, TiO2, Fe2O3..., ferrites: Fe2CoO4..., or BaZrO3) were obtained with specific features. Some technical issues have been solved, that are presented here. Heat transfer was studied, leading to a more efficient design of the reactor. Future developments have been examined through process engineering, in which our group is engaged, especially through CFD modelling.
Experimental P-T-ro Measurements of Supercritical Mixtures of Carbon Dioxide, Carbon Monoxide, and Hydrogen and Semiquantitative Estimation of Their …
2007
The P-T-ρ behavior of the CO2-CO-H2 system was studied in the supercritical region under operative conditions close to those adopted to perform hydrogenation and hydroformylation reactions in dense CO 2, thus providing new interesting information on this fluid mixture. Experiments were performed in a fixed volume reactor in the temperature range from 298 K to 343 K changing the density and the composition of the fluid phase. The one-component (Hildebrand) solubility parameter of the mixture was estimated from experimentally measured P vs T profiles, and its dependence on the density and composition of the system was analyzed to study the antisolvent effect of the permanent gases. We have fo…