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2013, №1

сс. 3-13

Articles

Key words: PVT-properties, water, n-pentane, critical state, critical points

Thermal properties of the binary system n-pentane + water (1 : 4 by weight) re phase equilibria of hydrocarbon liquid—vapor and aqueous liquid—vapor have been studied in a wide temperature range 303—674 K under elevated pressures (up to 60 MPa) along 9 isochors. The phase equilibrium lines and critical points for the system were obtained and the phase diagrams are described.

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2013, №1

сс. 14-35

Articles

Preparative separation of psoralen methoxy-derivatives by supercritical fluid chromatography

O.I. Pokrovskiy, A.A. Krutikova, K.B. Ustinovich, O.O. Parenago, M.V. Moschnin, S.A. Gonchukov, V.V. Lunin.

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Key words: supercritical fluid chromatography, furocoumarin, methoxypsoralen, retention mechanisms

A method for separation of isomeric psoralen methoxy-derivatives, namely bergapten, xanthotoxin and isopimpinellin, is developed. The results of sorbent screening allow one to consider a normal phase elution regime as optimal for separation of these compounds in SFC. The analysis of methoxypsoralen (MOP) retention mechanisms showed that the same one is responsible for MOP’s separation on all tested silica sorbents containing polar groups, except 2-ethylpyridine and pentafluorophenyl. A possible explanation of the observed MOP’s retention phenomena is given. In the case of pentafluorophenyl sorbent π-electron intermolecular interactions play a key role in separation of closely related MOPs. It is likely that the same effects are responsible for a specific order of MOP’s elution observed when 2-ethylpyridine sorbent is used.

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2013, №1

сс. 36-45

Articles

Key words: supercritical carbon dioxide, biodegradable polymers, SCF micronization, poly-3-hydroxybutyrate, SAS

Micronization of poly-3-hydroxybutyrate (PHB) using SAS technique with supercritical carbon dioxide as an antisolvent is studied experimentally. The possibility of PHB particle fabrication with different morphology (including hollow spheres) and predetermined sizes varied from 100 nm to 20 μm is demonstrated. The effect of various mechanisms of the formation of solid phase during the SAS micronization process onto the size and morphology of poly-3-hydroxybutyrate particles is evaluated and discussed.

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2013, №1

сс. 46-56

Articles

Key words: supercritical carbon dioxide, aliphatic polyethers, matrixes for tissue engineering

A novel method for fabrication of highly porous bioresorbable polymer matrixes for tissue engineering is proposed and developed. It is shown that injection of polymer compositions plasticized in sub- or supercritical carbon dioxide at 20—40 °C through the nozzle of certain diameter to the moulds at atmospheric or elevated (up to 6 MPa) CO2 pressure enables to fabricate highly reproducible polymer matrixes with desirable structure and morphology and mean porosity up to 96 % without use of organic solvents. The effect of chemical composition and molecular weight of initial polymers, as well as, carbon dioxide temperature and pressure in reaction and receiver chambers onto the morphology and internal structure of fabricated matrixes is studied using a scanning electron microscopy.

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2013, №1

сс. 57-68

Articles

Key words: ESR, supercritical water, in situ spectroscopy, VO2+, VOSO4, clustering, heterogeneous catalyst, temperature gradient

Temperature variations of the EPR spectra of VO2+ ions in sub- and supercritical water, under isothermal and temperature gradient conditions are investigated using an in situ EPR. A broadening of the hyperfine structure at increasing temperature and appearance of an unresolved broad low intensity line (ΔHpp ≈ 300 Oe) in the supercritical state are observed in the absence of temperature gradients, indicating the increase of exchange interaction between VO2+ ions in supercritical water. Exchange-narrowed anisotropic absorption line is observed under the temperature gradient conditions in the subcritical water near the transition to supercritical state. The shape of this line is close to that observed in the solid salt VOSO4·3H2O. It is shown that in situ EPR allows us to investigate the effects of changing the local environment of paramagnetic ions, which is preceding a well-known process of clustering and formation of amorphous oxide particles in sub- and supercritical conditions.

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2013, №1

сс. 69-79

Articles

Subcritical water extraction of cichoric and caftaric acids from Echinacea purpurea L.

A.V. Lekar, S.N. Borisenko, O.V. Filonova, E.V. Vetrova, E.V. Maksimenko, N.I. Borisenko, V.I. Minkin.

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Key words: subcritical water, Echinacea purpurea L., caftaric acid, cichoric acid, HPLC

New method for extraction of caftaric acid and cichoric acid using subcritical water is developed. This method is environmentally benign and more efficient than traditional extraction methods based on the utilization of expensive and toxic organic solvents.

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2013, №1

сс. 80-86

Articles

Caprolactam and nitrobenzene desorption from polymeric sorbents by subcritical water

I.A. Platonov, E.A. Novikova, N.V. Nikitchenko, I.Yu. Rocshupkina.

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Key words: subcritical water, regeneration of sorbents, caprolactam, nitrobenzene, hyper-cross-linked polystyrene sorbents

Subcritical water is tested as an agent for caprolactam and nitrobenzene desorption from hyper-cross-linked polystyrene sorbents MN-202 and MN-270. The efficiencies of desorption of two mentioned compounds by subcritical water and by water solution of isopropanol are compared.

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2013, №1

сс. 87-97

Articles

Key words: supercritical fluids, pulse heating, heat transfer

A technique based on pulse heating of the wire probe (resistance thermometer) in the constant heating power mode is developed and applied for the studies of comparative heat transfer intensity in supercritical fluids (SCF) in the pressure and temperature ranges from 1рс to (4—6) рс and from 0,6Tс to 1,6Tс, respectively (рс and Tс — critical pressure and temperature). Characteristic parameters of the setup used are as follows: heating pulse length — 1—10 ms; density of the heat flux through the probe surface — 1—10 MW/m2; repeatability of the selected power value in a series of pulses — not worse than 0,1 %. A sharp decrease in the heat transfer intensity in SCF compared to that observed at subcritical temperatures is revealed.

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