Conversion of a deasphalting unit for use in the process of supercritical solvent recovery

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Waintraub S.

2000-01-01

Full Text Available In order to reduce energy consumption and to increase deasphalted oil yield, an old PETROBRAS deasphalting unit was converted for use in the process of supercritical solvent recovery. In-plant and pilot tests were performed to determine the ideal solvent-to-oil ratio. The optimum conditions for separation of the supercritical solvent from the solvent-plus-oil liquid mixture were determined by experimental tests in PVT cells. These tests also allowed measurement of the dew and bubble points, determination of the retrograde region, observation of supercritical fluid compressibility and as a result construction of a phase equilibrium diagram.

Impacts of Extraction Methods in the Rapid Determination of Atrazine Residues in Foods using Supercritical Fluid Chromatography and Enzyme-Linked Immunosorbent Assay: Microwave Solvent vs. Supercritical Fluid Extractions

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Mohamed H. El-Saeid

2005-01-01

Full Text Available It is an accepted fact that many food products that we eat today have the possibility of being contaminated by various chemicals used from planting to processing. These chemicals have been shown to cause illnesses for which some concerned government agencies have instituted regulatory mechanisms to minimize the risks and the effects on humans. It is for these concerns that reliable and accurate rapid determination techniques are needed to effect proper regulatory standards for the protection of people's nutritional health. This paper, therefore, reports the comparative evaluation of the extraction methods in the determination of atrazine (commonly used in agricultural as a herbicide residues in foods using supercritical fluid chromatography (SFC and enzyme-linked immunosorbent assay (ELISA techniques. Supercritical fluid extraction (SFE and microwave solvent extraction (MSE methods were used to test samples of frozen vegetables, fruit juice, and jam from local food markets in Houston. Results showed a high recovery percentage of atrazine residues using supercritical fluid coupled with ELISA and SFC than with MSE. Comparatively, however, atrazine was detected 90.9 and 54.5% using SFC and ELISA techniques, respectively. ELISA technique was, however, less time consuming, lower in cost, and more sensitive with low detection limit of atrazine residues than SFC technique.

Supercritical fluid extraction of uranium

International Nuclear Information System (INIS)

Kumar, Pradeep

2017-01-01

Uranium being strategic material, its separation and purification is of utmost importance in nuclear industry, for which solvent extraction is being employed. During solvent extraction significant quantity of radioactive liquid waste gets generated which is of environmental concern. In recent decades supercritical fluid extraction (SFE) has emerged as promising alternative to solvent extraction owing to its inherent advantage of reduction in liquid waste generation and simplification of process. In this paper a brief overview of research work carried out so far on SFE of uranium by BARC has been given

Supercritical fluid carbon dioxide extraction of actinides

International Nuclear Information System (INIS)

Rao, Ankita; Tomar, B.S.

2016-01-01

Supercritical fluid extraction (SFE) is a process akin to liquid-liquid or solvent extraction where a Supercritical fluid (SCF) is contacted with a solid/ liquid matrix for the purpose of separating the component of interest from the original matrix. Carbon dioxide is a preferred choice as supercritical fluid (SCF) owing to its moderate critical parameter (P c = 7.38 MPa and T c = 304.1K) coupled with radiation and chemical stability, non toxic nature and low cost. Despite widespread applications for extraction of organic compounds and associated advantages especially liquid waste minimization, the SFE of metal ions was left unexplored for quite some time, as direct metal ion extraction is inefficient due charge neutralization requirement and weak solute-solvent interaction. Neutral SCF soluble metal-ligand complexation is imperative and SFE of actinides was reported only in 1994. Several studies have been carried out on SFE of uranium, thorium and plutonium from nitric acid medium employing different sets of ligands (organophosphorus, diketones, amides). Especially attractive is the possibility of direct dissolution and extraction of actinides employing ligand-acid adducts (like TBP.HNO 3 adduct) from solid matrices of different stages of nuclear fuel cycle viz. ores, spent nuclear fuels and radioactive wastes. Also, partitioning of actinides from fission products has been explored in spent nuclear fuel. These studies on supercritical fluid extraction of actinides indicate a more efficient and environmentally sustainable technology. (author)

Industrial applications and current trends in supercritical fluid technologies

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Gamse Thomas

2005-01-01

Full Text Available Supercritical fluids have a great potential for wide fields of processes Although CO2 is still one of the most used supercritical gases, for special purposes propane or even fluorinated-chlorinated fluids have also been tested. The specific characteristics of supercritical fluids behaviour were analyzed such as for example the solubilities of different components and the phase equilibria between the solute and solvent. The application at industrial scale (decaffeinating of tea and coffee, hop extraction or removal of pesticides from rice, activity in supercritical extraction producing total extract from the raw material or different fractions by using the fractionated separation of beverages (rum, cognac, whisky, wine, beer cider, of citrus oils and of lipids (fish oils, tall oil were also discussed. The main interest is still for the extraction of natural raw materials producing food ingredients, nutraceuticals and phytopharmaceuticals but also cleaning purposes were tested such as the decontamination of soils the removal of residual solvents from pharmaceutical products, the extraction of flame retardants from electronic waste or precision degreasing and cleaning of mechanical and electronic parts. An increasing interest obviously exists for impregnation purposes based on supercritical fluids behaviour, as well as for the dying of fibres and textiles. The production of fine particles in the micron and submicron range, mainly for pharmaceutical products is another important application of supercritical fluids. Completely new products can be produced which is not possible under normal conditions. Supercritical fluid technology has always had to compete with the widespread opinion that these processes are very expensive due to very high investment costs in comparison with classical low-pressure equipment. Thus the opinion is that these processes should be restricted to high-added value products. A cost estimation for different plant sizes and

Triticonazole enantiomers: Separation by supercritical fluid chromatography and the effect of the chromatographic conditions.

Science.gov (United States)

He, Jianfeng; Fan, Jun; Yan, Yilun; Chen, Xiaodong; Wang, Tai; Zhang, Yaomou; Zhang, Weiguang

2016-11-01

Enantiomeric pairs of triticonazole have been successfully separated by supercritical fluid chromatography coupled with a tris(3,5-dimethylphenylcarbamoyl) cellulose-coated chiral stationary phase in this work. The effects of co-solvent, dissolution solvent, flow rate, backpressure, and column temperature have been studied in detail with respect to retention, selectivity, and resolution of triticonazole. As indicated, the co-solvents mostly affected the retention factors and resolution, due to the different molecular structure and polarity. In addition, the dissolution solvents, namely, chloromethanes and alcohols, have been also important for enantioseparation because of the different interaction with stationary phase. Higher flow rate and backpressure led to faster elution of the triticonazole molecules, and the change of column temperature showed slight effect on the resolution of triticonazole racemate. Moreover, a comparative separation experiment between supercritical fluid chromatography and high performance liquid chromatography revealed that chiral supercritical fluid chromatography gave the 3.5 times value of R s /t R2 than high performance liquid chromatography, which demonstrated that supercritical fluid chromatography had much higher separation efficiency. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

MEASUREMENT OF PYRETHROID RESIDUES IN ENVIRONMENTAL AND FOOD SAMPLES BY ENHANCED SOLVENT EXTRACTION/SUPERCRITICAL FLUID EXTRACTION COUPLED WITH GAS CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

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The abstract summarizes pyrethorid methods development research. It provides a summary of sample preparation and analytical techniques such as supercritical fluid extraction, enhance solvent extraction, gas chromatography and tandem mass spectrometry.

Extraction of pesticides in soil using supercritical carbon dioxide co-solvents

International Nuclear Information System (INIS)

Forero, Jose R; Castro, Henry I; Guerrero, Jairo A.

2009-01-01

In this study, three organic solvents (ethyl acetate, methanol and acetone) were used as co solvent in supercritical fluid extraction (SFE) of a mixture of pesticides with different physical and chemical properties present in soil. These pesticides were determined by gas chromatography with electronic micro capture detector μECD and nitrogen-phosphorus detector (NPD), coupled in parallel. The extractions were performed on spiked soil samples using supercritical carbon dioxide (CO 2 SC) as the extracting phase to 35 celsius degrade and 14 MPa, using 10 mL of each co solvent and it was found that methanol offers the greatest efficiency in the extraction process obtaining recovery values between 51.24 and 123.50%.

Applications of supercritical fluid extraction (SFE) of palm oil and oil from natural sources.

Science.gov (United States)

Akanda, Mohammed Jahurul Haque; Sarker, Mohammed Zaidul Islam; Ferdosh, Sahena; Manap, Mohd Yazid Abdul; Ab Rahman, Nik Norulaini Nik; Ab Kadir, Mohd Omar

2012-02-10

Supercritical fluid extraction (SFE), which has received much interest in its use and further development for industrial applications, is a method that offers some advantages over conventional methods, especially for the palm oil industry. SC-CO₂ refers to supercritical fluid extraction (SFE) that uses carbon dioxide (CO₂) as a solvent which is a nontoxic, inexpensive, nonflammable, and nonpolluting supercritical fluid solvent for the extraction of natural products. Almost 100% oil can be extracted and it is regarded as safe, with organic solvent-free extracts having superior organoleptic profiles. The palm oil industry is one of the major industries in Malaysia that provides a major contribution to the national income. Malaysia is the second largest palm oil and palm kernel oil producer in the World. This paper reviews advances in applications of supercritical carbon dioxide (SC-CO₂) extraction of oils from natural sources, in particular palm oil, minor constituents in palm oil, producing fractionated, refined, bleached, and deodorized palm oil, palm kernel oil and purified fatty acid fractions commendable for downstream uses as in toiletries and confectionaries.

Applications of Supercritical Fluid Extraction (SFE of Palm Oil and Oil from Natural Sources

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Mohd Omar Ab Kadir

2012-02-01

Full Text Available Supercritical fluid extraction (SFE, which has received much interest in its use and further development for industrial applications, is a method that offers some advantages over conventional methods, especially for the palm oil industry. SC-CO2 refers to supercritical fluid extraction (SFE that uses carbon dioxide (CO2 as a solvent which is a nontoxic, inexpensive, nonflammable, and nonpolluting supercritical fluid solvent for the extraction of natural products. Almost 100% oil can be extracted and it is regarded as safe, with organic solvent-free extracts having superior organoleptic profiles. The palm oil industry is one of the major industries in Malaysia that provides a major contribution to the national income. Malaysia is the second largest palm oil and palm kernel oil producer in the World. This paper reviews advances in applications of supercritical carbon dioxide (SC-CO2 extraction of oils from natural sources, in particular palm oil, minor constituents in palm oil, producing fractionated, refined, bleached, and deodorized palm oil, palm kernel oil and purified fatty acid fractions commendable for downstream uses as in toiletries and confectionaries.

Supercritical fluid extraction of positron-emitting radioisotopes from solid target matrices

International Nuclear Information System (INIS)

Schlyer, D.

2000-01-01

Supercritical fluids are attractive as media for both chemical reactions, as well as process extraction, since their physical properties can be manipulated by small changes in pressure and temperature near the critical point of the fluid. Such changes can result in drastic effects on density-dependent properties such as solubility, refractive index, dielectric constant, viscosity and diffusivity of the fluid. This suggests that pressure tuning of a pure supercritical fluid may be a useful means to manipulate chemical reactions on the basis of a thermodynamic solvent effect. It also means that the solvation properties of the fluid can be precisely controlled to enable selective component extraction from a matrix. In recent years there has been a growing interest in applying supercritical fluid extraction to the selective removal of trace metals from solid samples. Much of the work has been done on simple systems comprised of inert matrices such as silica or cellulose. Recently, this process as been expanded to environmental samples as well. However, very little is understood about the exact mechanism of the extraction process. Of course, the widespread application of this technology is highly dependent on the ability of scientists to model and predict accurate phase equilibria in complex systems. In this project, we plan to explore the feasibility of utilizing supercritical fluids as solvents for reaction and extraction of radioisotopes produced from solid enriched targets. The reason for this work is that many of these enriched target materials used for radioisotope production are expensive

Lipidomics by Supercritical Fluid Chromatography

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Laurent Laboureur

2015-06-01

Full Text Available This review enlightens the role of supercritical fluid chromatography (SFC in the field of lipid analysis. SFC has been popular in the late 1980s and 1990s before almost disappearing due to the commercial success of liquid chromatography (LC. It is only 20 years later that a regain of interest appeared when new commercial instruments were introduced. As SFC is fully compatible with the injection of extracts in pure organic solvent, this technique is perfectly suitable for lipid analysis and can be coupled with either highly universal (UV or evaporative light scattering or highly specific (mass spectrometry detection methods. A short history of the use of supercritical fluids as mobile phase for the separation oflipids will be introduced first. Then, the advantages and drawbacks of SFC are discussed for each class of lipids (fatty acyls, glycerolipids, glycerophospholipids, sphingolipids, sterols, prenols, polyketides defined by the LIPID MAPS consortium.

Lipidomics by Supercritical Fluid Chromatography

Science.gov (United States)

Laboureur, Laurent; Ollero, Mario; Touboul, David

2015-01-01

This review enlightens the role of supercritical fluid chromatography (SFC) in the field of lipid analysis. SFC has been popular in the late 1980s and 1990s before almost disappearing due to the commercial success of liquid chromatography (LC). It is only 20 years later that a regain of interest appeared when new commercial instruments were introduced. As SFC is fully compatible with the injection of extracts in pure organic solvent, this technique is perfectly suitable for lipid analysis and can be coupled with either highly universal (UV or evaporative light scattering) or highly specific (mass spectrometry) detection methods. A short history of the use of supercritical fluids as mobile phase for the separation oflipids will be introduced first. Then, the advantages and drawbacks of SFC are discussed for each class of lipids (fatty acyls, glycerolipids, glycerophospholipids, sphingolipids, sterols, prenols, polyketides) defined by the LIPID MAPS consortium. PMID:26090714

Molecular simulation of CO chemisorption on Co(0001) in presence of supercritical fluid solvent: A potential of mean force study

Energy Technology Data Exchange (ETDEWEB)

Asiaee, Alireza; Benjamin, Kenneth M., E-mail: kenneth.benjamin@sdsmt.edu [Department of Chemical and Biological Engineering, South Dakota School of Mines and Technology, 501 E. Saint Joseph St., Rapid City, South Dakota 57701 (United States)

2016-08-28

For several decades, heterogeneous catalytic processes have been improved through utilizing supercritical fluids (SCFs) as solvents. While numerous experimental studies have been established across a range of chemistries, such as oxidation, pyrolysis, amination, and Fischer-Tropsch synthesis, still there is little fundamental, molecular-level information regarding the role of the SCF on elementary heterogeneous catalytic steps. In this study, the influence of hexane solvent on the adsorption of carbon monoxide on Co(0001), as the first step in the reaction mechanism of many processes involving syngas conversion, is probed. Simulations are performed at various bulk hexane densities, ranging from ideal gas conditions (no SCF hexane) to various near- and super-critical hexane densities. For this purpose, both density functional theory and molecular dynamics simulations are employed to determine the adsorption energy and free energy change during CO chemisorption. Potential of mean force calculations, utilizing umbrella sampling and the weighted histogram analysis method, provide the first commentary on SCF solvent effects on the energetic aspects of the chemisorption process. Simulation results indicate an enhanced stability of CO adsorption on the catalyst surface in the presence of supercritical hexane within the reduced pressure range of 1.0–1.5 at a constant temperature of 523 K. Furthermore, it is shown that the maximum stability of CO in the adsorbed state as a function of supercritical hexane density at 523 K nearly coincides with the maximum isothermal compressibility of bulk hexane at this temperature.

Chemical deposition methods using supercritical fluid solutions

Science.gov (United States)

Sievers, Robert E.; Hansen, Brian N.

1990-01-01

A method for depositing a film of a desired material on a substrate comprises dissolving at least one reagent in a supercritical fluid comprising at least one solvent. Either the reagent is capable of reacting with or is a precursor of a compound capable of reacting with the solvent to form the desired product, or at least one additional reagent is included in the supercritical solution and is capable of reacting with or is a precursor of a compound capable of reacting with the first reagent or with a compound derived from the first reagent to form the desired material. The supercritical solution is expanded to produce a vapor or aerosol and a chemical reaction is induced in the vapor or aerosol so that a film of the desired material resulting from the chemical reaction is deposited on the substrate surface. In an alternate embodiment, the supercritical solution containing at least one reagent is expanded to produce a vapor or aerosol which is then mixed with a gas containing at least one additional reagent. A chemical reaction is induced in the resulting mixture so that a film of the desired material is deposited.

Extraction of metals and/or metalloids from acidic media using supercritical fluids and salts

International Nuclear Information System (INIS)

Wai, C.M.; Smart, N.G.; Lin, Y.

1998-01-01

A method is described for extracting metalloid and metal species from a solid or liquid material by exposing the material to a fluid solvent, particularly supercritical carbon dioxide, containing a chelating agent. The chelating agent forms chelates that are soluble in the fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent comprises a trialkyl phosphate, a triaryl phosphate, a trialkylphosphine oxide, a triarylphosphine oxide, or mixtures thereof. The method provides an environmentally benign process for removing contaminants from industrial waste. The method is particularly useful for extracting actinides from acidic solutions, and the process can be aided by the addition of nitrate salts. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process. 7 figs

Extraction of metals and/or metalloids from acidic media using supercritical fluids and salts

Science.gov (United States)

Wai, Chien M.; Smart, Neil G.; Lin, Yuehe

1998-01-01

A method of extracting metalloid and metal species from a solid or liquid material by exposing the material to a fluid solvent, particularly supercritical carbon dioxide, containing a chelating agent is described. The chelating agent forms chelates that are soluble in the fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent comprises a trialkyl phosphate, a triaryl phosphate, a trialkylphosphine oxide, a triarylphosphine oxide, or mixtures thereof. The method provides an environmentally benign process for removing contaminants from industrial waste. The method is particularly useful for extracting actinides from acidic solutions, and the process can be aided by the addition of nitrate salts. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process.

Small angle X-ray scattering study on the conformation of polystyrene in the anti-solvent process of supercritical fluids

International Nuclear Information System (INIS)

Liu Yi; Wang Hongli; Zhao Xin; Chen Na; Li Dan; Liu Zhimin; Han Buxing; Rong Lixia; Zhao Hui; Wang Jun; Dong Baozhong

2003-01-01

The conformation of polystyrene in the anti-solvent process of supercritical fluids (compressed CO 2 + polystyrene + tetrahydrofuran) is studied by synchrotron radiation X-ray small angle scattering (SAXS). Coil-to-globule transform of polystyrene chain is observed with increasing the concentration of CO 2 . It is found that polystyrene coils at the pressure lower than cloud point pressure (p c ) and changes into globule with uniform density at the pressure higher than p c

Use and practice of achiral and chiral supercritical fluid chromatography in pharmaceutical analysis and purification.

Science.gov (United States)

Lemasson, Elise; Bertin, Sophie; West, Caroline

2016-01-01

The interest of pharmaceutical companies for complementary high-performance chromatographic tools to assess a product's purity or enhance this purity is on the rise. The high-throughput capability and economic benefits of supercritical fluid chromatography, but also the "green" aspect of CO2 as the principal solvent, render supercritical fluid chromatography very attractive for a wide range of pharmaceutical applications. The recent reintroduction of new robust instruments dedicated to supercritical fluid chromatography and the progress in stationary phase technology have also greatly benefited supercritical fluid chromatography. Additionally, it was shown several times that supercritical fluid chromatography could be orthogonal to reversed-phase high-performance liquid chromatography and could efficiently compete with it. Supercritical fluid chromatography is an adequate tool for small molecules of pharmaceutical interest: synthetic intermediates, active pharmaceutical ingredients, impurities, or degradation products. In this review, we first discuss about general chromatographic conditions for supercritical fluid chromatography analysis to better suit compounds of pharmaceutical interest. We also discuss about the use of achiral and chiral supercritical fluid chromatography for analytical purposes and the recent applications in these areas. The use of preparative supercritical fluid chromatography by pharmaceutical companies is also covered. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fast infrared spectroscopy in supercritical fluids

International Nuclear Information System (INIS)

Sun, X.

2000-05-01

Chapter 1: Introduction. A brief introduction to supercritical fluids is given, illustrating why supercritical fluids are unique solvents and why there is a wide application of supercritical fluids in industry and laboratories. Potential ways for solvation in supercritical fluids to affect reactivity are briefly reviewed. A general introduction to the photochemistry of organometallic complexes is also given. Chapter 2: Time resolved vibrational spectroscopy. Time resolved resonance Raman is introduced and compared with Time-resolved infrared spectroscopy (TRIR). The different approaches of TRIR, including microsecond, nanosecond, and ultrafast (picosecond and femtosecond) systems are discussed. The advantages and disadvantages of these systems are also compared. The TRIR apparatus using an IR diode laser used for work in this thesis are described in detail. Experimental procedures for supercritical fluid TRIR experiments are described with emphasis on handling the IR cell for supercritical fluids and preparation of supercritical fluid solutions. Chapter 3: Photochemistry of group VIB hexacarbonyl compounds in supercritical noble gases and CO 2 solutions. A systematic TRIR study of the photolysis of M(CO) 6 in supercritical Ar, Kr, Xe, and CO 2 and the observation of M(CO) 5 L (M = Cr, Mo, and W; L = Ar (W only), Kr, Xe, and CO 2 ) is described. The second-order rate constants for the reaction of M(CO) 5 L with CO have been evaluated and the reactivity for each metal is Kr > Xe ∼ CO 2 . For M(CO) 5 Kr, M(CO) 5 Xe, or M(CO) 5 (CO 2 ), the reactivity is Cr ∼ Mo > W. In supercritical Kr doped with either Xe or CO 2 , the M(CO) 5 moiety interacts with Xe or CO 2 in preference to Kr. The effect of solvent density on the rate of the reaction of W(CO) 5 (CO 2 ) with CO has been investigated. The reaction of W(CO) 5 (CO 2 ) with CO in scCO 2 is predominantly a dissociative process. The activation energies for the reaction of W(CO) 5 Xe and W(CO) 5 (CO 2 ) with CO and

Hydrogenation of diesel aromatic compounds in supercritical solvent environment

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E.P. Martins

2000-09-01

Full Text Available Reactions under supercritical conditions have been employed in many processes. Furthermore, an increasing number of commercial reactions have been conducted under supercritical or near critical conditions. These reaction conditions offer several advantages when compared to conditions in conventional catalytic processes in liquid-phase, gas-liquid interface, or even some gas-phase reactions. Basically, a supercritical solvent can diminish the reactant’s transport resistance from the bulk region to the catalyst surface due to enhancement of liquid diffusivity values and better solubility than those in different phases. Another advantage is that supercritical solvents permit prompt and easy changes in intermolecular properties in order to modify reaction parameters, such as conversion or selectivity, or even proceed with the separation of reaction products. Diesel fractions from petroleum frequently have larger than desirable quantities of aromatic compounds. Diesel hydrogenation is intended to decrease these quantities, i.e., to increase the quantity of paraffin present in this petroleum fraction. In this work, the hydrogenation of tetralin was studied as a model reaction for the aromatic hydrogenation process. A conventional gas-liquid-solid catalytic process was compared with that of supercritical carbon dioxide substrate under similar conditions. Additionally, an equilibrium conversion diagram was calculated for this reaction in a wide range of temperature and reactant ratios, so as to optimize the operational conditions and improve the results of subsequent experiments. An increase in the rate of reaction at 493 K in supercritical fluid, as compared to that in the conventional process, was observed.

Novel micronisation β-carotene using rapid expansion supercritical solution with co-solvent

Science.gov (United States)

Kien, Le Anh

2017-09-01

Rapid expansion of supercritical solution (RESS) is the most common approach of pharmaceutical pacticle forming methods using supercritical fluids. The RESS method is a technology producing a small solid product with a very narrow particle size distribution, organic solvent-free particles. This process is also simple and easy to control the operating parameters in comparision with other ways based on supercritical techniques. In this study, β-carotene, a strongly colored red-orange pigment abundant in plants and fruits, has been forming by RESS. In addition, the size and morphology effect of four different RESS parameters including co-solvent, extraction temperature, and extraction pressure and expansion nozzle temperature has surveyed. The particle size distribution has been determined by using laser diffraction experiment. SEM has conducted to analyze the surface structure, DSC and FTIR for thermal and chemical structure analysis.

Supercritical solvent extraction of oil sand bitumen

Science.gov (United States)

Imanbayev, Ye. I.; Ongarbayev, Ye. K.; Tileuberdi, Ye.; Mansurov, Z. A.; Golovko, A. K.; Rudyk, S.

2017-08-01

The supercritical solvent extraction of bitumen from oil sand studied with organic solvents. The experiments were performed in autoclave reactor at temperature above 255 °C and pressure 29 atm with stirring for 6 h. The reaction resulted in the formation of coke products with mineral part of oil sands. The remaining products separated into SARA fractions. The properties of the obtained products were studied. The supercritical solvent extraction significantly upgraded extracted natural bitumen.

Solid catalyzed isoparaffin alkylation at supercritical fluid and near-supercritical fluid conditions

Science.gov (United States)

Ginosar, Daniel M.; Fox, Robert V.; Kong, Peter C.

2000-01-01

This invention relates to an improved method for the alkylation reaction of isoparaffins with olefins over solid catalysts including contacting a mixture of an isoparaffin, an olefin and a phase-modifying material with a solid acid catalyst member under alkylation conversion conditions at either supercritical fluid, or near-supercritical fluid conditions, at a temperature and a pressure relative to the critical temperature(T.sub.c) and the critical pressure(P.sub.c) of the reaction mixture. The phase-modifying phase-modifying material is employed to promote the reaction's achievement of either a supercritical fluid state or a near-supercritical state while simultaneously allowing for decreased reaction temperature and longer catalyst life.

Method and apparatus for dissociating metals from metal compounds extracted into supercritical fluids

Science.gov (United States)

Wai, Chien M.; Hunt, Fred H.; Smart, Neil G.; Lin, Yuehe

2000-01-01

A method for dissociating metal-ligand complexes in a supercritical fluid by treating the metal-ligand complex with heat and/or reducing or oxidizing agents is described. Once the metal-ligand complex is dissociated, the resulting metal and/or metal oxide form fine particles of substantially uniform size. In preferred embodiments, the solvent is supercritical carbon dioxide and the ligand is a .beta.-diketone such as hexafluoroacetylacetone or dibutyldiacetate. In other preferred embodiments, the metals in the metal-ligand complex are copper, silver, gold, tungsten, titanium, tantalum, tin, or mixtures thereof. In preferred embodiments, the reducing agent is hydrogen. The method provides an efficient process for dissociating metal-ligand complexes and produces easily-collected metal particles free from hydrocarbon solvent impurities. The ligand and the supercritical fluid can be regenerated to provide an economic, efficient process.

Extraction of Stevia rebaudiana bertoni sweetener glycosides by supercritical fluid methods.

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Juan José Hinojosa-González

2017-05-01

Full Text Available Aim. The aim was to evaluate the supercritical carbon dioxide extraction method with and without the addition of co-solvent to the system (mixture water: ethanol to obtain the glycosides from leaves of Stevia rebaudiana Bertoni. Methods. A SFT-150 SFE / SFR model with CO2 as a fluid was used for the supercritical extraction. The variables studied were temperature, pressure, extraction time and the presence or absence of the co-solvent (water-ethanol mixture in a concentration of 70:30 v/v, incorporated in different proportions to determine the effect on yield. The amount of glycoside sweeteners was analyzed by High Performance Liquid Chromatography (HPLC. Results. The pressure was the factor that favored the extraction, which was selective in obtaining Rebaudioside A with yields no greater than 2%. The inclusion of the co-solvent achieved an increase in yield to values of 2.9% Conclusion. Supercritical CO2 individually and mixed with ethanol-water as a co-solvent was not efficient to extract Stevia rebaudiana stevioside sweeteners

Removal of common organic solvents from aqueous waste streams via supercritical C02 extraction: a potential green approach to sustainable waste management in the pharmaceutical industry.

Science.gov (United States)

Leazer, Johnnie L; Gant, Sean; Houck, Anthony; Leonard, William; Welch, Christopher J

2009-03-15

Supercritical CO2 extraction of aqueous streams is a convenient and effective method to remove commonly used solvents of varying polarities from aqueous waste streams. The resulting aqueous layers can potentially be sewered; whereas the organic layer can be recovered for potential reuse. Supercritical fluid extraction (SFE) is a technology that is increasingly being used in commercial processes (1). Supercritical fluids are well suited for extraction of a variety of media, including solids, natural products, and liquid products. Many supercritical fluids have low critical temperatures, allowing for extractions to be done at modestly low temperatures, thus avoiding any potential thermal decomposition of the solutes under study (2). Furthermore, the CO2 solvent strength is easily tuned by adjusting the density of the supercritical fluid (The density is proportional to the pressure of the extraction process). Since many supercritical fluids are gases at ambient temperature, the extract can be concentrated by simply venting the reaction mixture to a cyclone collection vessel, using appropriate safety protocols.

Birch Bark Dry Extract by Supercritical Fluid Technology: Extract Characterisation and Use for Stabilisation of Semisolid Systems

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Markus Armbruster

2017-03-01

Full Text Available Triterpene compounds like betulin, betulinic acid, erythrodiol, oleanolic acid and lupeol are known for many pharmacological effects. All these substances are found in the outer bark of birch. Apart from its pharmacological effects, birch bark extract can be used to stabilise semisolid systems. Normally, birch bark extract is produced for this purpose by extraction with organic solvents. Employing supercritical fluid technology, our aim was to develop a birch bark dry extract suitable for stabilisation of lipophilic gels with improved properties while avoiding the use of toxic solvents. With supercritical carbon dioxide, three different particle formation methods from supercritical solutions have been tested. First, particle deposition was performed from a supercritical solution in an expansion chamber. Second, the Rapid Expansion of Supercritical Solutions (RESS method was used for particle generation. Third, a modified RESS-procedure, forming the particles directly into the thereby gelated liquid, was developed. All three methods gave yields from 1% to 5.8%, depending on the techniques employed. The triterpene composition of the three extracts was comparable: all three gave more stable oleogels compared to the use of an extract obtained by organic solvent extraction. Characterizing the rheological behaviour of these gels, a faster gelling effect was seen together with a lower concentration of the extract required for the gel formation with the supercritical fluid (SCF-extracts. This confirms the superiority of the supercritical fluid produced extracts with regard to the oleogel forming properties.

Supercritical fluid chromatography approach for a sustainable manufacture of new stereoisomeric anticancer agent.

Science.gov (United States)

Ghinet, Alina; Zehani, Yasmine; Lipka, Emmanuelle

2017-10-25

Two routes aimed at the manufacture of unprecedented stereoisomeric combretastatin A-4 analogue were described: flash chromatography vs supercritical fluid chromatography. The latter has many advantages over liquid chromatography and was therefore chosen for the small scale separation of methyl 1-[(3-hydroxy-4-methoxyphenyl) (3,4,5-trimethoxyphenyl)methyl]-5-oxo-l-prolinate 5, with potential antitumoral activity. After a screening of six different polysaccharide based chiral stationary phases and four co-solvents, the percentage of co-solvent, the flow-rate and the outlet pressure were optimized through a design of experiments (DoE). The preparation of 50mg of each stereoisomer was achieved successfully on a Chiralpak AD-H with isopropanol as a co-solvent. Productivity (kkd), solvent usage and environmental factor (E Factor) were calculated. Flash chromatography and supercritical fluid chromatography approaches were compared in terms of yield and purity of each stereoisomer manufactured. Copyright © 2017 Elsevier B.V. All rights reserved.

Supercritical Fluid Extraction of Plutonium and Americium from Soil

International Nuclear Information System (INIS)

Fox, R.V.; Mincher, B.J.

2002-01-01

Supercritical fluid extraction (SFE) of plutonium and americium from soil was successfully demonstrated using supercritical fluid carbon dioxide solvent augmented with organophosphorus and beta-diketone complexants. Spiked Idaho soils were chemically and radiologically characterized, then extracted with supercritical fluid carbon dioxide at 2,900 psi and 65 C containing varying concentrations of tributyl phosphate (TBP) and thenoyltrifluoroacetone (TTA). A single 45 minute SFE with 2.7 mol% TBP and 3.2 mol% TTA provided as much as 88% ± 6.0 extraction of americium and 69% ± 5.0 extraction of plutonium. Use of 5.3 mol% TBP with 6.8 mol% of the more acidic beta-diketone hexafluoroacetylacetone (HFA) provided 95% ± 3.0 extraction of americium and 83% ± 5.0 extraction of plutonium in a single 45 minute SFE at 3,750 psi and 95 C. Sequential chemical extraction techniques were used to chemically characterize soil partitioning of plutonium and americium in pre-SFE soil samples. Sequential chemical extraction techniques demonstrated that spiked plutonium resides primarily (76.6%) in the sesquioxide fraction with minor amounts being absorbed by the oxidizable fraction (10.6%) and residual fractions (12.8%). Post-SFE soils subjected to sequential chemical extraction characterization demonstrated that 97% of the oxidizable, 78% of the sesquioxide and 80% of the residual plutonium could be removed using SFE. These preliminary results show that SFE may be an effective solvent extraction technique for removal of actinide contaminants from soil

Supercritical Fluid Extraction of Lovastatin from the Wheat Bran Obtained after Solid-State Fermentation

Directory of Open Access Journals (Sweden)

Ruchir C. Pansuriya

2009-01-01

Full Text Available The objective of the present work is to extract lovastatin with minimum impurity by using supercritical carbon dioxide (SC-CO2. A strain of Aspergillus terreus UV 1617 was used to produce lovastatin by solid-state fermentation (SSF on wheat bran as a solid substrate. Extraction of lovastatin and its hydroxy acid form was initially carried out using organic solvents. Among the different screened solvents, acetonitrile was found to be the most efficient. SC-CO2 was used for extraction of lovastatin from the dry fermented matter. The effect of supercritical extraction parameters such as the amount of an in situ pretreatment solvent, temperature, pressure, flow rate and contact time were investigated. The maximum recovery of lovastatin was obtained with 5 mL of methanol as an in situ pretreatment solvent for 1.5 g of solid matrix, flow rate of the supercritical solvent 2 L/min, temperature 50 °C, and contact time 155 min at a pressure 300 bar. The lovastatin extract obtained after optimizing the conditions of supercritical fluid extraction was found to have 5-fold more HPLC purity than the organic solvent extract.

Comparative analysis of essential oil composition of Iranian and Indian Nigella sativa L. extracted using supercritical fluid extraction and solvent extraction

Directory of Open Access Journals (Sweden)

Ghahramanloo KH

2017-07-01

Full Text Available Kourosh Hasanzadeh Ghahramanloo,1 Behnam Kamalidehghan,2 Hamid Akbari Javar,3 Riyanto Teguh Widodo,1 Keivan Majidzadeh,4 Mohamed Ibrahim Noordin1 1Department of Pharmacy, Faculty of Medicine, University of Malaya, Kuala Lumpur, Malaysia; 2Medical Genetics Department, National Institute of Genetic Engineering and Biotechnology (NIGEB, 3Department of Pharmaceutics, Faculty of Pharmacy, Tehran University of Medical Sciences (TUMS, 4Breast Cancer Research Center (BCRC Academic Center for Education, Culture and Research, Tehran, Iran Abstract: The objective of this study was to compare the oil extraction yield and essential oil composition of Indian and Iranian Nigella sativa L. extracted by using Supercritical Fluid Extraction (SFE and solvent extraction methods. In this study, a gas chromatography equipped with a mass spectrophotometer detector was employed for qualitative analysis of the essential oil composition of Indian and Iranian N. sativa L. The results indicated that the main fatty acid composition identified in the essential oils extracted by using SFE and solvent extraction were linoleic acid (22.4%–61.85% and oleic acid (1.64%–18.97%. Thymoquinone (0.72%–21.03% was found to be the major volatile compound in the extracted N. sativa oil. It was observed that the oil extraction efficiency obtained from SFE was significantly (P<0.05 higher than that achieved by the solvent extraction technique. The present study showed that SFE can be used as a more efficient technique for extraction of N. Sativa L. essential oil, which is composed of higher linoleic acid and thymoquinone contents compared to the essential oil obtained by the solvent extraction technique. Keywords: Nigella sativa L., essential oil extraction, supercritical fluid extraction, solvent extraction, fatty acid composition, thymoquinone, linoleic acid

Supercritical fluids processing: emerging opportunities

International Nuclear Information System (INIS)

Kovaly, K.A.

1985-01-01

This publication on the emerging opportunities of supercritical fluids processing reveals the latest research findings and development trends in this field. These findings and development trends are highlighted, and the results of applications of technology to the business of supercritical fluids are reported. Applications of supercritical fluids to chemical intermediates, environmental applications, chemical reactions, food and biochemistry processing, and fuels processing are discussed in some detail

Supercritical fluid chromatography in drug analysis: a literature survey.

Science.gov (United States)

Salvador, A; Jaime, M A; Becerra, G; Guardia, M de L

1996-08-01

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, diameter, particle film thickness, stationary phase), detectors, type of restrictors, and also some analytical features of the methods developed (such as retention time, resolution, sensitivity, limit of detection and relative standard deviation).

On the use of semiempirical models of (solid + supercritical fluid) systems to determine solid sublimation properties

International Nuclear Information System (INIS)

Tabernero, Antonio; Martin del Valle, Eva M.; Galan, Miguel A.

2011-01-01

Research highlights: → We propose a method to determine sublimation properties of solids. → Low deviations were produced calculating sublimation enthalpies and pressures. → It is a required step to determine the vaporization enthalpy of the solid. → It is possible to determine solid properties using semiempirical models solid-SCF. - Abstract: Experimental solubility data of solid-supercritical fluids have significantly increased in the last few years, and semiempirical models are emerging as one of the best choices to fit this type of data. This work establishes a methodology to calculate sublimation pressures using this type of equations. It requires the use of Bartle's equation to model equilibria data solid-supercritical fluids with the aim of determining the vaporization enthalpy of the compound. Using this method, low deviations were obtained by calculating sublimation pressures and sublimation enthalpies. The values of the sublimation pressures were subsequently used to successfully model different multiphasic equilibria, as solid-supercritical fluids and solid-solvent-supercritical fluids with the Peng-Robinson equation of state (without considering the sublimation pressure as an adjustable parameter). On the other hand, the sublimation pressures were also used to calculate solid sublimation properties and acetaminophen solvation properties in some solvents. Also, solubility data solid-supercritical fluids from 62 pharmaceuticals were fitted with different semiempirical equations (Chrastil, Kumar-Johnston and Bartle models) in order to present the values of solvation enthalpies in sc-CO 2 and vaporization enthalpies for these compounds. All of these results highlight that semiempirical models can be used for any other purpose as well as modeling (solid + supercritical fluids) equilibria.

Supercritical CO2 extraction of Schinus molle L with co-solvents: mathematical modeling and antimicrobial applications

Directory of Open Access Journals (Sweden)

Rodrigo Scopel

2013-06-01

Full Text Available This work investigates the antimicrobial activity of the Schinus molle L. leaves extracts obtained under supercritical conditions using carbon dioxide and co-solvents. Antimicrobial qualitative evaluation was carried out through the bioautography technique and the microorganisms studied were Staphylococcus aureus, Pseudomonas aeruginosas, Escherichia coli, Micrococcus luteus, and Salmonella choleraesuis. The supercritical fluid extraction was carried out in a pilot scale equipment using carbon dioxide modified by the addition of co-solvents, such as ethanol and water at 150 bar and 333 K. A mathematical modeling of the process was also performed.

Optimization of co-solvent addition in supercritical fluid extraction of fat with carbon dioxide

Directory of Open Access Journals (Sweden)

Ivanov Dušica S.

2011-01-01

Full Text Available This investigation is concerned with supercritical fluid extraction (SFE using CO2, as an analytical technique for total fat extraction from food and feed samples. Its most significant advantages are safety, cleanness, and shorter extraction time. The main limitation of this technique includes the difficulty of extracting polar lipids due to the non-polar character of the solvent (CO2 used for the extraction. The influence of ethanol as a co-solvent on the SFE of mash pig feed was investigated in this paper. Total fat content was determined by SFE and Soxhlet method for ten commercially available mesh pig feeds. Yields of the fat extracted by both methods were plotted one against the other and compared. Statistically significant difference (p ≤ 0.05 has been found only between the total fat obtained by the Soxhlet extraction and SFE by pure CO2. Based on the mathematical model, maximum yield of the extracted fat is achieved at an ethanol addition of 0.67 ml/g of sample, when the other parameters are the same as recommended by the producer’s procedure.

Sustainable extraction of molecules for potable alcohol, cosmetics and pharmaceuticals: extraction in supercritical fluids

International Nuclear Information System (INIS)

Leone, Gian Paolo; Ferri, Donatella

2015-01-01

Since many years the Laboratory of Agro-Industrial Innovation (UTAGRI-INN) ENEA proposed research and development of extraction processes with supercritical fluids (SFE, Supercritical Fluid Extraction), aiming on the sustainability of the process characteristics. The technique, in fact, makes no use of organic solvents, It has reduced energy consumption and requires a number of process step lower than the extractions traditional. The process also responds to the requirements required by the regulations for food use, cosmetics and pharmaceutical extracts. [it

Supercritical fluid extraction: spectroscopic study of interactions comparison to solvent extraction

Energy Technology Data Exchange (ETDEWEB)

Rustenholtz Farawila, A

2005-06-15

Supercritical fluid carbon dioxide (SF-CO{sub 2}) was chosen to study Supercritical Fluid Extraction (SFE) of cesium and uranium. At first, crown ethers were considered as chelating agents for the SFE of cesium. The role of water and its interaction with crown ethers were especially studied using Fourier-Transform Infra-Red (FT-IR) spectroscopy in SF-CO{sub 2}. A sandwich configuration between two crown ethers and a water molecule was observed in the SF-CO{sub 2} phase for the first time. The equilibrium between the single and the bridge configurations was defined. The enthalpy of the hydrogen bond formation was also calculated. These results were then compared to the one in different mixtures of chloroform and carbon tetra-chloride using Nuclear Magnetic Resonance (NMR). To conclude this first part and in order to understand the whole picture of the recovery of cesium, I studied the role of water in the equilibrium between the cesium and the di-cyclo-hexano18-crown-6.In a second part, the supercritical fluid extraction of uranium was studied in SF-CO{sub 2}. For this purpose, different complexes of Tributyl Phosphate (TBP), nitric acid and water were used as chelating and oxidizing agents. I first used FT-IR to study the TBP-water interaction in SF-CO{sub 2}. These results were then compared to the one obtained with NMR in chloroform. NMR spectroscopy was also used to understand the TBP-nitric acid-water interaction first alone and then in chloroform. To conclude my research work, I succeeded to improve the efficiency of uranium extraction and stripping into water for a pilot-plant where enriched uranium is extracted from incinerated waste coming from nuclear fuel fabrication. TBP-nitric acid complexes were used in SF-CO{sub 2} for the extraction of uranium from ash. (author)

Supercritical fluid extraction: spectroscopic study of interactions comparison to solvent extraction

International Nuclear Information System (INIS)

Rustenholtz Farawila, A.

2005-06-01

Supercritical fluid carbon dioxide (SF-CO 2 ) was chosen to study Supercritical Fluid Extraction (SFE) of cesium and uranium. At first, crown ethers were considered as chelating agents for the SFE of cesium. The role of water and its interaction with crown ethers were especially studied using Fourier-Transform Infra-Red (FT-IR) spectroscopy in SF-CO 2 . A sandwich configuration between two crown ethers and a water molecule was observed in the SF-CO 2 phase for the first time. The equilibrium between the single and the bridge configurations was defined. The enthalpy of the hydrogen bond formation was also calculated. These results were then compared to the one in different mixtures of chloroform and carbon tetra-chloride using Nuclear Magnetic Resonance (NMR). To conclude this first part and in order to understand the whole picture of the recovery of cesium, I studied the role of water in the equilibrium between the cesium and the di-cyclo-hexano18-crown-6.In a second part, the supercritical fluid extraction of uranium was studied in SF-CO 2 . For this purpose, different complexes of Tributyl Phosphate (TBP), nitric acid and water were used as chelating and oxidizing agents. I first used FT-IR to study the TBP-water interaction in SF-CO 2 . These results were then compared to the one obtained with NMR in chloroform. NMR spectroscopy was also used to understand the TBP-nitric acid-water interaction first alone and then in chloroform. To conclude my research work, I succeeded to improve the efficiency of uranium extraction and stripping into water for a pilot-plant where enriched uranium is extracted from incinerated waste coming from nuclear fuel fabrication. TBP-nitric acid complexes were used in SF-CO 2 for the extraction of uranium from ash. (author)

Sustainable extraction of molecules for human food, cosmetic and pharmaceutical products: extraction in supercritical fluids

International Nuclear Information System (INIS)

Leone, GianPaolo; Ferri, Donatella

2015-01-01

Since several years, the ENEA Innovation Laboratory for Agro-Industrial, proposed activities of research and development of extraction processes with supercritical fluids (SFE, Supercritical Fluid Extraction), focusing on sustainability characteristics of the process. The technique, in fact, makes no use of organic solvents, has a low energy consumption and requires a lower number of process steps compared to conventional extractions. The process also responds to the requirements imposed by the legislation for human food, cosmetic and pharmaceutical extracts. [it

Supercritical fluid chromatography

Science.gov (United States)

Vigdergauz, M. S.; Lobachev, A. L.; Lobacheva, I. V.; Platonov, I. A.

1992-03-01

The characteristic features of supercritical fluid chromatography (SCFC) are examined and there is a brief historical note concerning the development of the method. Information concerning the use of supercritical fluid chromatography in the analysis of objects of different nature is presented in the form of a table. The roles of the mobile and stationary phases in the separation process and the characteristic features of the apparatus and of the use of the method in physicochemical research are discussed. The bibliography includes 364 references.

Effect of solvent type and ratio on betacyanins and antioxidant activity of extracts from Hylocereus polyrhizus flesh and peel by supercritical fluid extraction and solvent extraction.

Science.gov (United States)

Fathordoobady, Farahnaz; Mirhosseini, Hamed; Selamat, Jinap; Manap, Mohd Yazid Abd

2016-07-01

The main objective of the present study was to investigate the effect of solvent type and ratio as well as the extraction techniques (i.e. supercritical fluid extraction (SFE) and conventional solvent extraction) on betacyanins and antioxidant activity of the peel and fresh extract from the red pitaya (Hylocereus polyrhizus). The peel and flesh extracts obtained by SFE at 25MPa pressure and 10% EtOH/water (v/v) mixture as a co-solvent contained 24.58 and 91.27mg/100ml total betacyanin, respectively; while the most desirable solvent extraction process resulted in a relatively higher total betacyanin in the peel and flesh extracts (28.44 and 120.28mg/100ml, respectively). The major betacyanins identified in the pitaya peel and flesh extracts were betanin, isobetanin, phyllocactin, butyrylbetanin, isophyllocactin and iso-butyrylbetanin. The flesh extract had the stronger antioxidant activity than the peel extract when the higher proportion of ethanol to water (E/W) was applied for the extraction. Copyright © 2016 Elsevier Ltd. All rights reserved.

Efficient separation of curcumin, demethoxycurcumin, and bisdemethoxycurcumin from turmeric using supercritical fluid chromatography: From analytical to preparative scale.

Science.gov (United States)

Song, Wei; Qiao, Xue; Liang, Wen-fei; Ji, Shuai; Yang, Lu; Wang, Yuan; Xu, Yong-wei; Yang, Ying; Guo, De-an; Ye, Min

2015-10-01

Curcumin is the major constituent of turmeric (Curcuma longa L.). It has attracted widespread attention for its anticancer and anti-inflammatory activities. The separation of curcumin and its two close analogs, demethoxycurcumin and bisdemethoxycurcumin, has been challenging by conventional techniques. In this study, an environmentally friendly method based on supercritical fluid chromatography was established for the rapid and facile separation of the three curcuminoids directly from the methanol extract of turmeric. The method was first developed and optimized by ultra performance convergence chromatography, and was then scaled up to preparative supercritical fluid chromatography. Eluted with supercritical fluid CO2 containing 8-15% methanol (containing 10 mM oxalic acid) at a flow rate of 80 mL/min, curcumin, demethoxycurcumin and bisdemethoxycurcumin could be well separated on a Viridis BEH OBD column (Waters, 250 mm × 19 mm, 5 μm) within 6.5 min. As a result, 20.8 mg of curcumin (97.9% purity), 7.0 mg of demethoxycurcumin (91.1%), and 4.6 mg of bisdemethoxycurcumin (94.8%) were obtained after a single step of supercritical fluid chromatography separation with a mean recovery of 76.6%. Showing obvious advantages in low solvent consumption, large sample loading, and easy solvent removal, supercritical fluid chromatography was proved to be a superior technique for the efficient separation of natural products. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Supercritical Fluid Extraction (SFE) of uranium and thorium nitrates using carbon dioxide modified with phosphonates

International Nuclear Information System (INIS)

Pitchaiah, K.C.; Sujatha, K.; Brahmananda Rao, C.V.S.; Sivaraman, N.; Vasudeva Rao, P.R.

2014-01-01

Supercritical Fluid Extraction (SFE) has emerged as a powerful technique for the extraction of metal ions.The liquid like densities and gas like physical properties of supercritical fluids make them unique to act as special solvents. SFE based procedures were developed and demonstrated in our laboratory for the recovery of actinides from various matrices. In the present study, we have examined for the first time, the use of dialkylalkylphosphonates in supercritical carbon dioxide (Sc-CO 2 ) medium to study the extraction behavior of uranium and thorium nitrates. A series of phosphonates were synthesised by Michaelis-Becker reaction in our laboratory and employed for the SFE

Correlation of supercritical-fluid extraction recoveries with supercritical-fluid chromatographic retention data: A fundamental study

NARCIS (Netherlands)

Lou, X.W.; Janssen, J.G.M.; Cramers, C.A.M.G.

1995-01-01

The possibility of using supercritical-fluid chromatographic retention data for examining the effects of operational parameters, such as pressure and flow rate, on the extraction characteristics in supercritical-fluid extraction (SFE) was investigated. A model was derived for calculating the

Research activities on supercritical fluid science in food biotechnology.

Science.gov (United States)

Khosravi-Darani, Kianoush

2010-06-01

This article serves as an overview, introducing the currently popular area of supercritical fluids and their uses in food biotechnology. Within each application, and wherever possible, the basic principles of the technique, as well as a description of the history, instrumentation, methodology, uses, problems encountered, and advantages over the traditional, non-supercritical methods are given. Most current commercial application of the supercritical extraction involve biologically-produced materials; the technique may be particularly relevant to the extraction of biological compounds in cases where there is a requirement for low-temperature processing, high mass-transfer rates, and negligible carrying over of the solvent into the final product. Special applications to food processing include the decaffeination of green coffee beans, the production of hops extracts, the recovery of aromas and flavors from herbs and spices, the extraction and fractionation of edible oils, and the removal of contaminants, among others. New advances, in which the extraction is combined with reaction or crystallization steps, may further increase the attractiveness of supercritical fluids in the bioprocess industries. To develop and establish a novel and effective alternative to heating treatment, the lethal action of high hydrostatic pressure CO(2) on microorganisms, with none or only a minimal heating process, has recently received a great deal of attention.

Evaluation of supercritical fluid extraction/gas chromatography/matrix isolation-infrared spectrometry for analysis of organic compounds

International Nuclear Information System (INIS)

Bopari, A.S.; Bierma, D.R.; Applegate, D.V.

1991-01-01

Analysis of soil samples for organic compounds typically first requires Soxhlet extraction or sonication. These processes are time consuming and generate large amounts of waste solvent. Supercritical fluid extraction (SFE), which uses a supercritical fluid such as carbon dioxide, has recently been shown to extract organic compounds from soil samples in good yields. Moreover, SFE does not generate waste solvent and can be performed rapidly. Gas Chromatography/Matrix Isolation-Infrared Spectrometry (GC/MI-IR) has been used in our laboratories for determining organic compounds present in extracts from various matrices. The authors have interfaced an SFE extraction apparatus to GC/MI-IR instruments. In this paper the utility of SPE/GC/MI-IR instrumentation is discussed

Studies on supercritical fluid extraction of uranium and thorium from liquid and solid matrix

International Nuclear Information System (INIS)

Kumar, Pradeep; Pal, Ankita; Saxena, M.K.; Ramakumar, K.L.

2006-05-01

Supercritical fluid extraction (SFE) is being widely used in pharmaceutical and food industry. Because of its simplicity, ease of operation and more importantly the reduction in the analytical waste generation, this technique is being viewed as a potential application technique in nuclear industry also. CO 2 is employed as supercritical fluid (SCF) as it is easily recyclable, non-toxic, chemically inert, radiochemically stable and inexpensive. Radioanalytical chemistry section (Radiochemistry and Isotope group) has recently procured a supercritical fluid extraction/chromatography system. The present report describes the work carried out on the system. Detailed study on uranium and thorium extraction from highly acidic medium and tissue paper matrix has been carried out. Direct dissolution and extraction of uranium compounds employing SCF has been carried out. CO 2 was employed as supercritical fluid along with very small amount of Tri n-butyl phosphate (TBP) and Tri n-octyl phosphine oxide (TOPO) as co-solvents. The effect of various operating parameters like CO 2 flow rate, co-solvent percentage, temperature and pressure on extraction was investigated and parameters for maximum extraction were optimized. For comparison, the modes of extraction viz. static and dynamic and modes of complexation viz. in-situ and online were studied. Uranium extraction of ∼98% has been achieved from nitric acid medium employing TBP as co-solvent in 30 minutes extraction time, whereas with TOPO ∼99% uranium extraction could be achieved. Uranium from tissue paper matrix could be extracted upto the extent of 98% with TOPO as co-solvent whereas with TBP extraction of (66.83± 9.80)% was achievable. Direct dissolution of UO 2 , U 3 O 8 , U metal, U-Al alloy solids into SCF CO 2 was carried out employing TBP-HNO 3 complex and SFE of uranium was performed using TBP as co-solvent. UO 2 and U 3 O 8 solids could be dissolved within 20 minutes and extraction of ∼98% was achieved. For U

Mass transfer in supercritical fluids instancing selected fluids in supercritical carbon dioxide

Science.gov (United States)

Hu, Miao; Benning, Rainer; Delgado, Antonio; Ertunc, Oezguer

The research interests lie in a deeper understanding of the mechanisms of diffusion and nucle-ation of organic solutes in near-and supercritical state of a solvent, which count as important means of mass transfer in the process engineering industry. The use of supercritical fluids in industrial processes, such as extraction and particle handling, has become a more and more popular method. Take a closer look at the two processes one would find that there are obviously two sub-processes involved in each of the process, namely the diffusion/nucleation as well as a phase transition procedure. Because of the operational limitations in the practice, this phase transition can-not be neglected. So it is also included in the theoretical approach. Classically to deduce conclusions from experiment results, mathematical/physical models outlining property changes and summarizing characteristics of the two processes are expected. In order to become an insight of these phenomena from the origin, and also to serve as a fundamental attribute for the numerical simulation later, the theories of statistical thermodynamics are adopted here as a proper means to describe the behaviors of the two processes. As the diffusion coefficients of the samples in our case are only of an order of approx. 10-8m2s-1, it can be assumed that the processes are in equilibrium (local changes are neglectably small), a model can be built on a general macroscopic approach for equilibrium systems, namely the Boltzmann-Gibbs distri-bution. And some rather general methods e.g. linear response theory can be applied. But as the transfer phenomena are genuinely not equilibrium systems, from this aspect a model can also be built based on the microscopic description -the kinetic theory of the behaviors of the particles of this non-equilibrium system. The characteristics under compensated gravity are also to be considered in the models. The differences and constraints between the models are to be compared and

Geothermal energy production with supercritical fluids

Science.gov (United States)

Brown, Donald W.

2003-12-30

There has been invented a method for producing geothermal energy using supercritical fluids for creation of the underground reservoir, production of the geothermal energy, and for heat transport. Underground reservoirs are created by pumping a supercritical fluid such as carbon dioxide into a formation to fracture the rock. Once the reservoir is formed, the same supercritical fluid is allowed to heat up and expand, then is pumped out of the reservoir to transfer the heat to a surface power generating plant or other application.

Solid-state flurbiprofen and methyl-β-cyclodextrin inclusion complexes prepared using a single-step, organic solvent-free supercritical fluid process.

Science.gov (United States)

Rudrangi, Shashi Ravi Suman; Kaialy, Waseem; Ghori, Muhammad U; Trivedi, Vivek; Snowden, Martin J; Alexander, Bruce David

2016-07-01

The aim of this study was to enhance the apparent solubility and dissolution properties of flurbiprofen through inclusion complexation with cyclodextrins. Especially, the efficacy of supercritical fluid technology as a preparative technique for the preparation of flurbiprofen-methyl-β-cyclodextrin inclusion complexes was evaluated. The complexes were prepared by supercritical carbon dioxide processing and were evaluated by solubility, differential scanning calorimetry, X-ray powder diffraction, scanning electron microscopy, practical yield, drug content estimation and in vitro dissolution studies. Computational molecular docking studies were conducted to study the possibility of molecular arrangement of inclusion complexes between flurbiprofen and methyl-β-cyclodextrin. The studies support the formation of stable molecular inclusion complexes between the drug and cyclodextrin in a 1:1 stoichiometry. In vitro dissolution studies showed that the dissolution properties of flurbiprofen were significantly enhanced by the binary mixtures prepared by supercritical carbon dioxide processing. The amount of flurbiprofen dissolved into solution alone was very low with 1.11±0.09% dissolving at the end of 60min, while the binary mixtures processed by supercritical carbon dioxide at 45°C and 200bar released 99.39±2.34% of the drug at the end of 30min. All the binary mixtures processed by supercritical carbon dioxide at 45°C exhibited a drug release of more than 80% within the first 10min irrespective of the pressure employed. The study demonstrated the single step, organic solvent-free supercritical carbon dioxide process as a promising approach for the preparation of inclusion complexes between flurbiprofen and methyl-β-cyclodextrin in solid-state. Copyright © 2016 Elsevier B.V. All rights reserved.

Comparative analysis of essential oil composition of Iranian and Indian Nigella sativa L. extracted using supercritical fluid extraction and solvent extraction.

Science.gov (United States)

Ghahramanloo, Kourosh Hasanzadeh; Kamalidehghan, Behnam; Akbari Javar, Hamid; Teguh Widodo, Riyanto; Majidzadeh, Keivan; Noordin, Mohamed Ibrahim

2017-01-01

The objective of this study was to compare the oil extraction yield and essential oil composition of Indian and Iranian Nigella sativa L. extracted by using Supercritical Fluid Extraction (SFE) and solvent extraction methods. In this study, a gas chromatography equipped with a mass spectrophotometer detector was employed for qualitative analysis of the essential oil composition of Indian and Iranian N. sativa L. The results indicated that the main fatty acid composition identified in the essential oils extracted by using SFE and solvent extraction were linoleic acid (22.4%-61.85%) and oleic acid (1.64%-18.97%). Thymoquinone (0.72%-21.03%) was found to be the major volatile compound in the extracted N. sativa oil. It was observed that the oil extraction efficiency obtained from SFE was significantly ( P essential oil, which is composed of higher linoleic acid and thymoquinone contents compared to the essential oil obtained by the solvent extraction technique.

Recovery of environmental analytes from clays and soils by supercritical fluid extracting/gas chromatography

International Nuclear Information System (INIS)

Emery, A.P.; Chesler, S.N.; MacCrehan, W.A.

1992-01-01

This paper reports on Supercritical Fluid Extraction (SFE) which promises to provide rapid extractions of organic analytes from environmental sample types without the use of hazardous solvents. In addition, SFE protocols using commercial instrumentation can be automated lowering analysis costs. Because of these benefits, we are investigating SFE as an alternative to the solvent extraction (eg. Soxhlet and sonication) techniques required in many EPA test procedures. SFE, using non-polar carbon dioxide as well as more polar supercritical fluids, was used to determine n-alkane hydrocarbons and polynuclear aromatic hydrocarbons (PAHs) in solid samples. The extraction behavior of these analyte classes from environmentally-contaminated soil matrices and model soil and clay matrices was investigated using a SFE apparatus in which the extracted analytes were collected on a solid phase trap and then selectively eluted with a solvent. The SFE conditions for quantitative recovery of n-alkane hydrocarbons in diesel fuel from a series of clays and soils were determined using materials prepared at the 0.02% level with diesel fuel oil in order to simplify analyte collection and analysis after extraction. The effect of extraction parameters including temperature, fluid flow rate and modifier addition were investigated by monitoring the amount of diesel fuel extracted as a function of time

Radiolytic and electron-transfer reactions in supercritical CO2

International Nuclear Information System (INIS)

Bartels, D. M.; Dimitrijevic, N. M.; Jonah, C. D.; Takahashi, K.

2000-01-01

Using supercritical fluids as solvents is useful for both practical and theoretical reasons. It has been proposed to use supercritical CO 2 as a solvent for synthesis because it eliminates the air pollution arising from other solvents. The properties of supercritical fluids can be easily varied with only modest changes in temperature and density, so they provide a way of testing theories of chemical reactions. It has also been proposed to use supercritical fluids for the treatment of hazardous mixed waste. For these reasons the authors have studied the production of radiolytic species in supercritical CO 2 and have measured their reactivity as a function of density. They have shown that the C 2 O 4 + is formed. They also have shown that the electron transfer reactions of dimethylaniline to C 2 O 4 + and CO 2 (e - ) to benzoquinone are diffusion controlled over a considerable density range

Supercritical Fluid Chromatographic Separation of Dimethylpolysiloxane Polymer

Energy Technology Data Exchange (ETDEWEB)

Pyo, Dong Jin; Lim, Chang Hyun [Kangwon National University, Chuncheon (Korea, Republic of)

2005-02-15

Water was used as a polar modifier and a μ-porasil column as a saturator column. The μ-porasil column was inserted between the pump outlet and the injection valve. During the passage of the supercritical fluid mobile phase through the silica column, a polar modifier (water) can be dissolved in the pressurized supercritical fluid. Dimethylpolysiloxane polymer has been known as more polar polymer than polystyrene polymer. Dimethylpolysiloxane polymer has never been separated using water modified mobile phase. In this paper, using a μ-porasil column as a saturator column, excellent supercritical fluid chromatograms of dimethylpolysiloxane oligomers were obtained. The use of compressed (dense) gases and supercritical fluids as chromatographic mobile phases in conjunction with liquid chromatographic (LC)-type packed columns was first reported by Klesper et al. in 1962. During its relatively short history, supercritical fluid chromatography (SFC) has become an attractive alternative to GC and LC in certain industrially important applications. SFC gives the advantage of high efficiency and allows the analysis of nonvolatile or thermally labile mixtures.

Supercritical Fluid Chromatographic Separation of Dimethylpolysiloxane Polymer

International Nuclear Information System (INIS)

Pyo, Dong Jin; Lim, Chang Hyun

2005-01-01

Water was used as a polar modifier and a μ-porasil column as a saturator column. The μ-porasil column was inserted between the pump outlet and the injection valve. During the passage of the supercritical fluid mobile phase through the silica column, a polar modifier (water) can be dissolved in the pressurized supercritical fluid. Dimethylpolysiloxane polymer has been known as more polar polymer than polystyrene polymer. Dimethylpolysiloxane polymer has never been separated using water modified mobile phase. In this paper, using a μ-porasil column as a saturator column, excellent supercritical fluid chromatograms of dimethylpolysiloxane oligomers were obtained. The use of compressed (dense) gases and supercritical fluids as chromatographic mobile phases in conjunction with liquid chromatographic (LC)-type packed columns was first reported by Klesper et al. in 1962. During its relatively short history, supercritical fluid chromatography (SFC) has become an attractive alternative to GC and LC in certain industrially important applications. SFC gives the advantage of high efficiency and allows the analysis of nonvolatile or thermally labile mixtures

Supercritical fluid extraction (SFE) and gas chromatographic (GC) analysis of products from irradiated foods containing fat

International Nuclear Information System (INIS)

Adam, S.T.

1993-01-01

Official analytical methods specify the use of organic liquid solvents which may be hazardous to human health. Non-toxic chlorinated fluorocarbons (CFC) which are still recommended for extracting soil samples are known to be detrimental to the stratospheric ozone layer and therefore subject to the ''FCKW-Halon-Verbots-Verordnung''. Therefore, alternative extraction methods using solvents in the supercritical state are currently being developed (Supercritical Fluid Extraction (SFE)). Their low viscosity and the high diffusivity of solutes in the fluids allow selective, efficient and timesaving extractions. Carbon dioxide (CO 2 ) is the fluid of choice in many applications because its critical parameters permit mild operating conditions. CO 2 of high purity is available at low cost, it is neither inflammable nor explosive, physiologically harmless and part of natural cycle processes. Furthermore, it is simply removed from the matrix without any residues left. The combination of SFE and sorptive collection of the extracted substances has been found to lead to high enrichment factors for the analytes. Distillative concentration and solid phase elution steps, required in the classical solvent extraction procedure, are no longer necessary. Loss of analytes occurring in cryogenic or solvent traps is completeley avoided. Plugging of the restrictor as a consequence of the Joule Thomson effect was not observed in the presented method. (orig./vhe)

Isolation of oxidative degradation products of atorvastatin with supercritical fluid chromatography.

Science.gov (United States)

Klobčar, Slavko; Prosen, Helena

2015-12-01

The isolation of four oxidative degradation products of atorvastatin using preparative high-performance liquid chromatography applying at least two chromatographic steps is known from the literature. In this paper it is shown that the same four impurities could be isolated from similarly prepared mixtures in only one step using supercritical fluid chromatography. The methods for separation were developed and optimized. The preparation of the mixtures was altered in such a way as to enhance the concentration of desired impurities. Appropriate solvents were applied for collection of separated impurities in order to prevent degradation. The structures of the isolated impurities were confirmed and their purity determined. The preparative supercritical fluid chromatography has proven to be superior to preparative HPLC regarding achieved purity of standards applying fewer chromatographic as well as isolation steps. Copyright © 2015 John Wiley & Sons, Ltd.

Effects of process parameters on peanut skins extract and CO2 diffusivity by supercritical fluid extraction

Science.gov (United States)

Putra, N. R.; Yian, L. N.; Nasir, H. M.; Idham, Z. Binti; Yunus, M. A. C.

2018-03-01

Peanut skins (Arachis hypogea) are an agricultural waste product which has received much attention because they contain high nutritional values and can be potentially utilized in difference industries. At present, only a few studies have been conducted to study the effects of parameters on the peanut skins oil extraction. Therefore, this study aimed to determine the best extraction condition in order to obtain the highest extract yield using supercritical carbon dioxide (SC-CO2) with co-solvent Ethanol as compared to Soxhlet extraction method. Diffusivity of carbon dioxide in supercritical fluid extraction was determined using Crank model. The mean particle size used in this study was 425 µm. The supercritical carbon dioxide was performed at temperature (40 – 70 °C), flow rate of co-solvent ethanol (0 - 7.5% Vethanol/Vtotal), and extraction pressure (10 – 30 MPa) were used in this studies. The results showed that the percentage of oil yields and effective diffusivity increase as the pressure, rate of co-solvent, and temperature increased.

Purification of radioactive waste oil by a supercritical fluid

International Nuclear Information System (INIS)

Yoo, Jaeryong; Sung, Jinhyun; Park, Kwangheon; Kim, Hongdoo; Kim, Hakwon; Lim, Taeyoon; Yim, Sanghak; Yoon, Weonseob

2006-01-01

The radioactive waste oil from the nuclear industry is potentially hazardous due to its possibility to contaminate soil and underwater. Pollutants in waste oil are generally radioactive heavy metals or organo-metals. Radioactive waste oils are highly viscous fluids that are similar to used-motor oils. Several processes have been developed to regenerated used motor oil, such as acid clay treatment, chemical addition, vacuum distillation, thermal cracking and hydrofinishing. However, these technologies are difficult to apply to separating radioactive nuclides from radioactive waste oils. In recent years, our laboratory developed a membrane method for the regeneration of used motor oils. We applied supercritical Co2 (scCO2) as a viscosity reducing additive to waste oils at a lower process temperature in order to improve membrane permeability and thus the energy saving. However, the membrane cannot filter the contaminants in radioactive waste oil that are not particles, such as radioactive ions in impurity water in the oil. In this paper, we suggest a method extracting clean oil from the radioactive waste oil rather than filtering by a supercritical fluid. We selected R22, a refrigerant, as a solvent for extraction. R22 has a mild critical point - 96.1 .deg. and 49.9bar. Regeneration of waste oils by extracting clean oil using a supercritical fluid such as R22 is easy to handle and reduce secondary wastes. In this paper, we examine the feasibility of R22 in extracting clean oil from radioactive waste oils

Comparison of the Behaviour of Polymers in Supercritical Fluids and Organic Solvents Via Small Angle Neutron Scattering

International Nuclear Information System (INIS)

Melnichenko, Y.B.; Kiran, E.; Heath, K.D.; Salaniwal, S.; Cochran, H.D.; Stamm, M.; Van Hook, W.A.; Wignall, G.D.

1999-01-01

Small-angle neutron scattering has been used to study the effect of temperature and pressure on the phase behavior of semidilute solutions of polymers dissolved in organic and supercritical solvents. Above the theta temperature (To), these systems exhibit a ''good solvent'' domain, where the molecules expand beyond the unperturbed dimensions in both organic solvents and in COZ. However, this transition can be made to occur at a critical ''theta pressure'' (PO) in CO2 and this represents a new concept in the physics of polymer-solvent systems. For T < To, and P < Po, the system enters the ''poor solvent'' domain where diverging concentration fluctuations prevent the chains from collapsing and allow them to maintain their unperturbed dimensions

Solvation in supercritical water

International Nuclear Information System (INIS)

Cochran, H.D.; Cummings, P.T.; Karaborni, S.

1991-01-01

The aim of this work is to determine the solvation structure in supercritical water composed with that in ambient water and in simple supercritical solvents. Molecular dynamics studies have been undertaken of systems that model ionic sodium and chloride, atomic argon, and molecular methanol in supercritical aqueous solutions using the simple point charge model of Berendsen for water. Because of the strong interactions between water and ions, ionic solutes are strongly attractive in supercritical water, forming large clusters of water molecules around each ion. Methanol is found to be a weakly-attractive solute in supercritical water. The cluster of excess water molecules surrounding a dissolved ion or polar molecule in supercritical aqueous solutions is comparable to the solvent clusters surrounding attractive solutes in simple supercritical fluids. Likewise, the deficit of water molecules surrounding a dissolved argon atom in supercritical aqueous solutions is comparable to that surrounding repulsive solutes in simple supercritical fluids. The number of hydrogen bonds per water molecule in supercritical water was found to be about one third the number in ambient water. The number of hydrogen bonds per water molecule surrounding a central particle in supercritical water was only mildly affected by the identify of the central particle--atom, molecule, or ion. These results should be helpful in developing a qualitative understanding of important processes that occur in supercritical water. 29 refs., 6 figs

Development of a test facility for analyzing supercritical fluid blowdown

International Nuclear Information System (INIS)

Roberto, Thiago D.; Alvim, Antonio C.M.

2015-01-01

The generation IV nuclear reactors under development mostly use supercritical fluids as the working fluid because higher temperatures improve the thermal efficiency. Supercritical fluids are used by modern nuclear power plants to achieve thermal efficiencies of around 45%. With water as the supercritical working fluid, these plants operate at a high temperature and pressure. However, experiments on supercritical water are limited by technical and financial difficulties. These difficulties can be overcome by using model fluids, which have more feasible supercritical conditions and exhibit a lower critical pressure and temperature. Experimental research is normally used to determine the conditions under which model fluids represent supercritical fluids under steady-state conditions. A fluid-to-fluid scaling approach has been proposed to determine model fluids that can represent supercritical fluids in a transient state. This paper presents an application of fractional scale analysis to determine the simulation parameters for a depressurization test facility. Carbon dioxide (CO 2 ) and R134a gas were considered as the model fluids because their critical point conditions are more feasible than those of water. The similarities of water (prototype), CO 2 (model) and R134a (model) for depressurization in a pressure vessel were analyzed. (author)

Method for removing impurities from an impurity-containing fluid stream

Science.gov (United States)

Ginosar, Daniel M.; Fox, Robert V.

2010-04-06

A method of removing at least one polar component from a fluid stream. The method comprises providing a fluid stream comprising at least one nonpolar component and at least one polar component. The fluid stream is contacted with a supercritical solvent to remove the at least one polar component. The at least one nonpolar component may be a fat or oil and the at least one polar component may be water, dirt, detergents, or mixtures thereof. The supercritical solvent may decrease solubility of the at least one polar component in the fluid stream. The supercritical solvent may function as a solvent or as a gas antisolvent. The supercritical solvent may dissolve the nonpolar components of the fluid stream, such as fats or oils, while the polar components may be substantially insoluble. Alternatively, the supercritical solvent may be used to increase the nonpolarity of the fluid stream.

Theoretical models for supercritical fluid extraction.

Science.gov (United States)

Huang, Zhen; Shi, Xiao-Han; Jiang, Wei-Juan

2012-08-10

For the proper design of supercritical fluid extraction processes, it is essential to have a sound knowledge of the mass transfer mechanism of the extraction process and the appropriate mathematical representation. In this paper, the advances and applications of kinetic models for describing supercritical fluid extraction from various solid matrices have been presented. The theoretical models overviewed here include the hot ball diffusion, broken and intact cell, shrinking core and some relatively simple models. Mathematical representations of these models have been in detail interpreted as well as their assumptions, parameter identifications and application examples. Extraction process of the analyte solute from the solid matrix by means of supercritical fluid includes the dissolution of the analyte from the solid, the analyte diffusion in the matrix and its transport to the bulk supercritical fluid. Mechanisms involved in a mass transfer model are discussed in terms of external mass transfer resistance, internal mass transfer resistance, solute-solid interactions and axial dispersion. The correlations of the external mass transfer coefficient and axial dispersion coefficient with certain dimensionless numbers are also discussed. Among these models, the broken and intact cell model seems to be the most relevant mathematical model as it is able to provide realistic description of the plant material structure for better understanding the mass-transfer kinetics and thus it has been widely employed for modeling supercritical fluid extraction of natural matters. Copyright © 2012 Elsevier B.V. All rights reserved.

Introduction to supercritical fluids a spreadsheet-based approach

CERN Document Server

Smith, Richard; Peters, Cor

2013-01-01

This text provides an introduction to supercritical fluids with easy-to-use Excel spreadsheets suitable for both specialized-discipline (chemistry or chemical engineering student) and mixed-discipline (engineering/economic student) classes. Each chapter contains worked examples, tip boxes and end-of-the-chapter problems and projects. Part I covers web-based chemical information resources, applications and simplified theory presented in a way that allows students of all disciplines to delve into the properties of supercritical fluids and to design energy, extraction and materials formation systems for real-world processes that use supercritical water or supercritical carbon dioxide. Part II takes a practical approach and addresses the thermodynamic framework, equations of state, fluid phase equilibria, heat and mass transfer, chemical equilibria and reaction kinetics of supercritical fluids. Spreadsheets are arranged as Visual Basic for Applications (VBA) functions and macros that are completely (source code) ...

Supercritical Fluids Processing of Biomass to Chemicals and Fuels

Energy Technology Data Exchange (ETDEWEB)

Olson, Norman K. [Iowa State Univ., Ames, IA (United States)

2011-09-28

The main objective of this project is to develop and/or enhance cost-effective methodologies for converting biomass into a wide variety of chemicals, fuels, and products using supercritical fluids. Supercritical fluids will be used both to perform reactions of biomass to chemicals and products as well as to perform extractions/separations of bio-based chemicals from non-homogeneous mixtures. This work supports the Biomass Program’s Thermochemical Platform Goals. Supercritical fluids are a thermochemical approach to processing biomass that, while aligned with the Biomass Program’s interests in gasification and pyrolysis, offer the potential for more precise and controllable reactions. Indeed, the literature with respect to the use of water as a supercritical fluid frequently refers to “supercritical water gasification” or “supercritical water pyrolysis.”

Use of supercritical carbon dioxide extraction

Energy Technology Data Exchange (ETDEWEB)

Taniguchi, Masayuki (Niigata Univ., Faculty of Engineering, Niigata, (Japan))

1989-09-25

Supercritical fluid extraction is a novel diffusion and separation technique which exploits simultaneously the increase of vapor pressure and the difference of chemical affinities of fluids near the critical point. A solvent which is used as the supercritical fluid has the following features: the critical point exists in the position of relatively ease of handling, the solvent is applicable to the extraction of a physiological active substance of thermal instability. Carbon dioxide as the solvent is non-flammable, non-corrosive, non-toxic, cheap, and readily available of high purity. The results of studies on the use of supercritical carbon dioxide (SC-CO{sub 2}) as a solvent for natural products in the fermentation and food industries, were collected. SC-CO{sub 2} extraction are used in many fields, examples for the application are as follows: removal of organic solvents from antibiotics; extraction of vegetable oils contained in wheat germ oil, high quality mustard seeds, rice bran and so on; brewing of sake using rice and rice-koji; use as a non-aqueous medium for the synthesis of precursors of the Aspartame; and use in sterilization. 66 refs., 17 figs., 21 tabs.

Kinetic models for supercritical CO2 extraction of oilseeds - a review

Directory of Open Access Journals (Sweden)

B. Nagy

2011-01-01

Full Text Available The supercritical fluid extraction of oilseeds is gaining increasing interest in commercial application for the last few decades, most particularly thanks to technical and environmental advantages of supercritical fluid extraction technology compared to current extraction methods with organic solvents. Furthermore, CO2 as a solvent is generally recognized as safe (GRAS. At present moment, supercritical fluid extractions on a commercial scale are limited to decaffeination, production of soluble hops extracts, sesame seed oil production and extraction of certain petroleum products. When considering industrial application, it is essential to test the applicability of the appropriate model for supercritical fluid extraction of oilseeds used for scale up of laboratory data to industrial design purposes. The aim of this paper is to review the most significant kinetic models reported in the literature for supercritical fluid extraction.

Supercritical fluid analytical methods

International Nuclear Information System (INIS)

Smith, R.D.; Kalinoski, H.T.; Wright, B.W.; Udseth, H.R.

1988-01-01

Supercritical fluids are providing the basis for new and improved methods across a range of analytical technologies. New methods are being developed to allow the detection and measurement of compounds that are incompatible with conventional analytical methodologies. Characterization of process and effluent streams for synfuel plants requires instruments capable of detecting and measuring high-molecular-weight compounds, polar compounds, or other materials that are generally difficult to analyze. The purpose of this program is to develop and apply new supercritical fluid techniques for extraction, separation, and analysis. These new technologies will be applied to previously intractable synfuel process materials and to complex mixtures resulting from their interaction with environmental and biological systems

Steps of Supercritical Fluid Extraction of Natural Products and Their Characteristic Times

OpenAIRE

Sovová, H. (Helena)

2012-01-01

Kinetics of supercritical fluid extraction (SFE) from plants is variable due to different micro-structure of plants and their parts, different properties of extracted substances and solvents, and different flow patterns in the extractor. Variety of published mathematical models for SFE of natural products corresponds to this diversification. This study presents simplified equations of extraction curves in terms of characteristic times of four single extraction steps: internal diffusion, exter...

Supercritical fluid technology for energy and environmental applications

CERN Document Server

Anikeev, Vladimir

2014-01-01

Supercritical Fluid Technology for Energy and Environmental Applications covers the fundamental principles involved in the preparation and characterization of supercritical fluids (SCFs) used in the energy production and other environmental applications. Energy production from diversified resources - including renewable materials - using clean processes can be accomplished using technologies like SCFs. This book is focused on critical issues scientists and engineers face in applying SCFs to energy production and environmental protection, the innovative solutions they have found, and the challenges they need to overcome. The book also covers the basics of sub- and supercritical fluids, like the thermodynamics of phase and chemical equilibria, mathematical modeling, and process calculations. A supercritical fluid is any substance at a temperature and pressure above its critical point where distinct liquid and gas phases do not exist. At this state the compound demonstrates unique properties, which can be "fine...

Supercritical fluid extraction of lanthanides and actinides from solid materials with a fluorinated β-diketone

International Nuclear Information System (INIS)

Lin, Y.; Brauer, R.D.; Laintz, K.E.; Wai, C.M.

1993-01-01

Direct extraction of metal ions by supercritical carbon dioxide is highly inefficient because of the charge neutralization requirement and the weak solute-solvent interactions. One suggested approach of extracting metal ions by supercritical carbon dioxide is to convert the charged species into metal chelates using a chelating agent in the fluid phase. This paper describes a method of extracting lanthanide and uranyl ions from a solid material by supercritical carbon dioxide containing a fluorinated beta-diketone, 2,2-dimethyl-6,6,7,7,8,8,8-heptafluoro-3,5-octanedione(FOD). Potential applications of this SFE method for separating the f-block elements from environmental samples are discussed. 13 refs., 2 tabs

Multivessel supercritical fluid extraction of food items in Total Diet Study.

Science.gov (United States)

Hopper, M L; King, J W; Johnson, J H; Serino, A A; Butler, R J

1995-01-01

An off-line, large capacity, multivessel supercritical fluid extractor (SFE) was designed and constructed for extraction of large samples. The extractor can simultaneously process 1-6 samples (15-25 g) by using supercritical carbon dioxide (SC-CO2), which is relatively nontoxic and nonflammable, as the solvent extraction medium. Lipid recoveries for the SFE system were comparable to those obtained by blending or Soxhlet extraction procedures. Extractions at 10,000 psi, 80 degrees C, expanded gaseous CO2 flow rates of 4-5 L/min (35 degrees C), and 1-3 h extraction times gave reproducible lipid recoveries for pork sausage (relative standard deviation [RSD], 1.32%), corn chips (RSD, 0.46%), cheddar cheese (RSD, 1.14%), and peanut butter (RSD, 0.44%). In addition, this SFE system gave reproducible recoveries (> 93%) for butter fortified with cis-chlordane and malathion at the 100 ppm and 0.1 ppm levels. Six portions each of cheddar cheese, saltine crackers, sandwich cookies, and ground hamburger also were simultaneously extracted with SC-CO2 and analyzed for incurred pesticide residues. Results obtained with this SFE system were reproducible and comparable with results from organic-solvent extraction procedures currently used in the Total Diet Study; therefore, use and disposal of large quantities of organic solvents can be eliminated.

Determination of major aromatic constituents in vanilla using an on-line supercritical fluid extraction coupled with supercritical fluid chromatography.

Science.gov (United States)

Liang, Yanshan; Liu, Jiaqi; Zhong, Qisheng; Shen, Lingling; Yao, Jinting; Huang, Taohong; Zhou, Ting

2018-04-01

An on-line supercritical fluid extraction coupled with supercritical fluid chromatography method was developed for the determination of four major aromatic constituents in vanilla. The parameters of supercritical fluid extraction were systematically investigated using single factor optimization experiments and response surface methodology by a Box-Behnken design. The modifier ratio, split ratio, and the extraction temperature and pressure were the major parameters which have significant effects on the extraction. While the static extraction time, dynamic extraction time, and recycle time had little influence on the compounds with low polarity. Under the optimized conditions, the relative extraction efficiencies of all the constituents reached 89.0-95.1%. The limits of quantification were in the range of 1.123-4.747 μg. The limits of detection were in the range of 0.3368-1.424 μg. The recoveries of the four analytes were in the range of 76.1-88.9%. The relative standard deviations of intra- and interday precision ranged from 4.2 to 7.6%. Compared with other off-line methods, the present method obtained higher extraction yields for all four aromatic constituents. Finally, this method has been applied to the analysis of vanilla from different sources. On the basis of the results, the on-line supercritical fluid extraction-supercritical fluid chromatography method shows great promise in the analysis of aromatic constituents in natural products. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Transport properties of supercritical carbon dioxide

NARCIS (Netherlands)

Lavanchy, F.; Fourcade, E.; de Koeijer, E.A.; Wijers, J.G.; Meyer, T.; Keurentjes, J.T.F.; Kemmere, M.F.; Meyer, T.

2005-01-01

Recently, supercritical fluids have emerged as more sustainable alternatives for the organic solvents often used in polymer processes. This is the first book emphasizing the potential of supercritical carbon dioxide for polymer processes from an engineering point of view. It develops a

Development of Nuclear Decontamination Technology Using Supercritical Fluid

Energy Technology Data Exchange (ETDEWEB)

Jung, Wonyoung; Park, Kwangheon; Park, Jihye; Lee, Donghee [Kyunghee Univ., Yongin (Korea, Republic of)

2014-05-15

Soil cleaning technologies that have been developed thus far increase treatment costs in contaminated soil recovery processes because they generate large amounts of secondary wastes. In this respect, this study is intended to develop soil decontamination methods using CO{sub 2}, which is a nontoxic, environmentally friendly substance, in order to fundamentally suppress the generation of secondary wastes from the decontamination process and to create high added values. In this study, to develop decontamination methods for uranium-contaminated soil using supercritical CO{sub 2}, a soil decontamination system using supercritical CO{sub 2} was constructed. In addition, the basic principle of supercritical CO{sub 2} decontamination using a TBP-HNO3 complex was explained. According to the results of the study, sea-sand samples having the same degree of contamination showed different results of decontamination according to the quantities of the TBP-HNO3 complex used as an extraction agent, which resulted in high extraction rates. Thus far, a most widely used method of extracting uranium has been the dissolving of uranium in acids. However, this method has the large adverse effect of generating strong acidic wastes that cannot be easily treated. On the other hand, supercritical CO{sub 2} requires critical conditions that are no more difficult to meet than those of other supercritical fluids, since its density can be changed from a very low state close to that of an ideal gas to a high state close to that of liquids. The critical gas conditions are a pressure of 71 bar and a temperature of 31 .deg. C, both of which are inexpensive to achieve. Moreover, CO{sub 2} is a solvent that is not harmful to the human body and few effects on environmental pollution. Therefore, nontoxic and environment friendly processes can be developed using supercritical CO{sub 2}. Supercritical CO{sub 2}'s advantages over prevailing methods suggest its potential for developing innovative

Development of Nuclear Decontamination Technology Using Supercritical Fluid

International Nuclear Information System (INIS)

Jung, Wonyoung; Park, Kwangheon; Park, Jihye; Lee, Donghee

2014-01-01

Soil cleaning technologies that have been developed thus far increase treatment costs in contaminated soil recovery processes because they generate large amounts of secondary wastes. In this respect, this study is intended to develop soil decontamination methods using CO 2 , which is a nontoxic, environmentally friendly substance, in order to fundamentally suppress the generation of secondary wastes from the decontamination process and to create high added values. In this study, to develop decontamination methods for uranium-contaminated soil using supercritical CO 2 , a soil decontamination system using supercritical CO 2 was constructed. In addition, the basic principle of supercritical CO 2 decontamination using a TBP-HNO3 complex was explained. According to the results of the study, sea-sand samples having the same degree of contamination showed different results of decontamination according to the quantities of the TBP-HNO3 complex used as an extraction agent, which resulted in high extraction rates. Thus far, a most widely used method of extracting uranium has been the dissolving of uranium in acids. However, this method has the large adverse effect of generating strong acidic wastes that cannot be easily treated. On the other hand, supercritical CO 2 requires critical conditions that are no more difficult to meet than those of other supercritical fluids, since its density can be changed from a very low state close to that of an ideal gas to a high state close to that of liquids. The critical gas conditions are a pressure of 71 bar and a temperature of 31 .deg. C, both of which are inexpensive to achieve. Moreover, CO 2 is a solvent that is not harmful to the human body and few effects on environmental pollution. Therefore, nontoxic and environment friendly processes can be developed using supercritical CO 2 . Supercritical CO 2 's advantages over prevailing methods suggest its potential for developing innovative decontamination methods, as demonstrated

Supercritical Fluid Extraction of Plant Flavors and Fragrances

Directory of Open Access Journals (Sweden)

Massimo E. Maffei

2013-06-01

Full Text Available Supercritical fluid extraction (SFE of plant material with solvents like CO2, propane, butane, or ethylene is a topic of growing interest. SFE allows the processing of plant material at low temperatures, hence limiting thermal degradation, and avoids the use of toxic solvents. Although today SFE is mainly used for decaffeination of coffee and tea as well as production of hop extracts on a large scale, there is also a growing interest in this extraction method for other industrial applications operating at different scales. In this review we update the literature data on SFE technology, with particular reference to flavors and fragrance, by comparing traditional extraction techniques of some industrial medicinal and aromatic crops with SFE. Moreover, we describe the biological activity of SFE extracts by describing their insecticidal, acaricidal, antimycotic, antimicrobial, cytotoxic and antioxidant properties. Finally, we discuss the process modelling, mass-transfer mechanisms, kinetics parameters and thermodynamic by giving an overview of SFE potential in the flavors and fragrances arena.

Supercritical fluid chromatography for lipid analysis in foodstuffs.

Science.gov (United States)

Donato, Paola; Inferrera, Veronica; Sciarrone, Danilo; Mondello, Luigi

2017-01-01

The task of lipid analysis has always challenged separation scientists, and new techniques in chromatography were often developed for the separation of lipids; however, no single technique or methodology is yet capable of affording a comprehensive screening of all lipid species and classes. This review acquaints the role of supercritical fluid chromatography within the field of lipid analysis, from the early developed capillary separations based on pure CO 2 , to the most recent techniques employing packed columns under subcritical conditions, including the niche multidimensional techniques using supercritical fluids in at least one of the separation dimensions. A short history of supercritical fluid chromatography will be introduced first, from its early popularity in the late 1980s, to the sudden fall and oblivion until the last decade, experiencing a regain of interest within the chromatographic community. Afterwards, the subject of lipid nomenclature and classification will be briefly dealt with, before discussing the main applications of supercritical fluid chromatography for food analysis, according to the specific class of lipids. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Supercritical fluid molecular spray film deposition and powder formation

Science.gov (United States)

Smith, Richard D.

1986-01-01

Solid films are deposited, or fine powders formed, by dissolving a solid material into a supercritical fluid solution at an elevated pressure and then rapidly expanding the solution through a short orifice into a region of relatively low pressure. This produces a molecular spray which is directed against a substrate to deposit a solid thin film thereon, or discharged into a collection chamber to collect a fine powder. Upon expansion and supersonic interaction with background gases in the low pressure region, any clusters of solvent are broken up and the solvent is vaporized and pumped away. Solute concentration in the solution is varied primarily by varying solution pressure to determine, together with flow rate, the rate of deposition and to control in part whether a film or powder is produced and the granularity of each. Solvent clustering and solute nucleation are controlled by manipulating the rate of expansion of the solution and the pressure of the lower pressure region. Solution and low pressure region temperatures are also controlled.

Optimization of conditions for supercritical fluid extraction of flavonoids from hops (Humulus lupulus L.)*

Science.gov (United States)

He, Guo-qing; Xiong, Hao-ping; Chen, Qi-he; Ruan, Hui; Wang, Zhao-yue; Traoré, Lonseny

2005-01-01

Waste hops are good sources of flavonoids. Extraction of flavonoids from waste hops (SC-CO2 extracted hops) using supercritical fluids technology was investigated. Various temperatures, pressures and concentrations of ethanol (modifier) and the ratio (w/w) of solvent to material were tested in this study. The results of single factor and orthogonal experiments showed that at 50 °C, 25 MPa, the ratio of solvent to material (50%), ethanol concentration (80%) resulted in maximum extraction yield flavonoids (7.8 mg/g). HPLC-MS analysis of the extracts indicated that flavonoids obtained were xanthohumol, the principal prenylflavonoid in hops. PMID:16187413

Measurement of polychlorinated biphenyls in solid waste such as transformer insulation paper by supercritical fluid extraction and gas chromatography electron capture detection.

Science.gov (United States)

Chikushi, Hiroaki; Fujii, Yuka; Toda, Kei

2012-09-21

In this work, a method for measuring polychlorinated biphenyls (PCBs) in contaminated solid waste was investigated. This waste includes paper that is used in electric transformers to insulate electric components. The PCBs in paper sample were extracted by supercritical fluid extraction and analyzed by gas chromatography-electron capture detection. The recoveries with this method (84-101%) were much higher than those with conventional water extraction (0.08-14%), and were comparable to those with conventional organic solvent extraction. Limit of detection was 0.0074 mg kg(-1) and measurable up to 2.5 mg kg(-1) for 0.5 g of paper sample. Data for real insulation paper by the proposed method agreed well with those by the conventional organic solvent extraction. Extraction from wood and concrete was also investigated and good performance was obtained as well as for paper samples. The supercritical fluid extraction is simpler, faster, and greener than conventional organic solvent extraction. Copyright © 2012 Elsevier B.V. All rights reserved.

The Effect of Pressure and Solvent on the Supercritical Fluid Chromatography Separation of Tocol Analogs in Palm Oil

Directory of Open Access Journals (Sweden)

Mei Han Ng

2017-08-01

Full Text Available There are six tocol analogs present in palm oil, namely α-tocopherol (α-T, α-tocomonoenol (α-T1, α-tocotrienol (α-T3, γ-tocotrienol (γ-T3, β-tocotrioenol (β-T3 and δ-tocotrienol (δ-T3. These analogs were difficult to separate chromatographically due to their similar structures, physical and chemical properties. This paper reports on the effect of pressure and injection solvent on the separation of the tocol analogs in palm oil. Supercritical CO2 modified with ethanol was used as the mobile phase. Both total elution time and resolution of the tocol analogs decreased with increased pressure. Ethanol as an injection solvent resulted in peak broadening of the analogs within the entire pressure range studied. Solvents with an eluent strength of 3.4 or less were more suitable for use as injecting solvents.

Heat Transfer Phenomena of Supercritical Fluids

Energy Technology Data Exchange (ETDEWEB)

Krau, Carmen Isabella; Kuhn, Dietmar; Schulenberg, Thomas [Forschungszentrum Karlsruhe, Institute for Nuclear and Energy Technologies, 76021 Karlsruhe (Germany)

2008-07-01

In concepts for supercritical water cooled reactors, the reactor core is cooled and moderated by water at supercritical pressures. The significant temperature dependence of the fluid properties of water requires an exact knowledge of the heat transfer mechanism to avoid fuel pin damages. Near the pseudo-critical point a deterioration of heat transfer might happen. Processes, that take place in this case, are not fully understood and are due to be examined systematically. In this paper a general overview on the properties of supercritical water is given, experimental observations of different authors will be reviewed in order to identify heat transfer phenomena and onset of occurrence. The conceptional design of a test rig to investigate heat transfer in the boundary layer will be discussed. Both, water and carbon dioxide, may serve as operating fluids. The loop, including instrumentation and safety devices, is shown and suitable measuring methods are described. (authors)

Driving Forces Controlling Host-Guest Recognition in Supercritical Carbon Dioxide Solvent.

Science.gov (United States)

Ingrosso, Francesca; Altarsha, Muhannad; Dumarçay, Florence; Kevern, Gwendal; Barth, Danielle; Marsura, Alain; Ruiz-López, Manuel F

2016-02-24

The formation of supramolecular host-guest complexes is a very useful and widely employed tool in chemistry. However, supramolecular chemistry in non-conventional solvents such as supercritical carbon dioxide (scCO2 ), one of the most promising sustainable solvents, is still in its infancy. In this work, we explored a successful route to the development of green processes in supercritical CO2 by combining a theoretical approach with experiments. We were able to synthesize and characterize an inclusion complex between a polar aromatic molecule (benzoic acid) and peracetylated-β-cyclodextrin, which is soluble in the supercritical medium. This finding opens the way to wide, environmental friendly, applications of scCO2 in many areas of chemistry, including supramolecular synthesis, reactivity and catalysis, micro and nano-particle formation, molecular recognition, as well as enhanced extraction processes with increased selectivity. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Particle Formation by Supercritical Fluid Extraction and Expansion Process

Directory of Open Access Journals (Sweden)

Sujuan Pan

2013-01-01

Full Text Available Supercritical fluid extraction and expansion (SFEE patented technology combines the advantages of both supercritical fluid extraction (SFE and rapid expansion of supercritical solution (RESS with on-line coupling, which makes the nanoparticle formation feasible directly from matrix such as Chinese herbal medicine. Supercritical fluid extraction is a green separation technology, which has been developed for decades and widely applied in traditional Chinese medicines or natural active components. In this paper, a SFEE patented instrument was firstly built up and controlled by LABVIEW work stations. Stearic acid was used to verify the SFEE process at optimized condition; via adjusting the preexpansion pressure and temperature one can get different sizes of particles. Furthermore, stearic acid was purified during the SFEE process with HPLC-ELSD detecting device; purity of stearic acid increased by 19%, and the device can purify stearic acid.

Squalene Extraction by Supercritical Fluids from Traditionally Puffed Amaranthus hypochondriacus Seeds

Directory of Open Access Journals (Sweden)

Teresa Rosales-García

2017-01-01

Full Text Available Extraction of squalene, a potent natural antioxidant, from puffed A. hypochondriacus seeds was performed by supercritical fluid extraction (SCFE; besides, to have a blank for comparison, extraction was performed also by Soxhlet method using organic solvents (hexane. Chemical proximal composition and seed morphology were determined in raw, puffed, and SCFE-extracted seeds. Extracts were obtained with a 500 mL capacity commercial supercritical extractor and performed between 10 and 30 MPa at 313, 323, and 333 K under constant CO2 flow of 0.18 kg CO2/h during 8 h. The squalene content was determined and the fatty acids present in the extracts were identified by GC-MS. The extract obtained by SCFE from puffed amaranth seeds reached 460 ± 28.1 g/kg squalene in oily extract at 313 K/20 MPa.

Supercritical fluid extraction of uranium and thorium employing dialkyl amides

International Nuclear Information System (INIS)

Rao, Ankita; Kumar, Pradeep

2014-01-01

Extraction and purification of actinides from different matrices is of utmost importance to the nuclear industry. In recent decades, supercritical fluid extraction (SFE) has emerged as a promising alternative to solvent extraction owing to its inherent potential of minimization of liquid waste generation. N,N-dialkyl aliphatic amides have been proposed to be an alternative to TBP in the reprocessing of spent nuclear fuel due to several attractive features like innocuous nature of degradation products (mainly carboxylic acids/ amines), possibility of complete incineration of the used extractant leading to reduction in volume of secondary waste. Also, physico-chemical properties of this class of extractants can be tuned by the judicious choice of alkyl groups. In the present work, N,N-dialkyl aliphatic amides with varying alkyl groups viz. N,N-dibutyl-2-ethylhexanamide (DBEHA), N,N-dibutyl-3,3-dimethylbutanamide (DBDMBA), N,N-dihexyloctanamide (DHOA), N,N-disecbutylpentamide (DBPA), N,N-dibutyloctanamide (DBOA), have been evaluated for supercritical fluid extraction (SFE) of uranium and thorium from nitric acid medium as well as tissue paper matrix. Amides were obtained from Department of Chemistry, Delhi University and were used as such. This fact could be exploited for separation of thorium and uranium

A field-portable supercritical fluid extractor for characterizing sources of waterborne organic compounds

International Nuclear Information System (INIS)

Fruchter, J.S.; Wright, B.W.

1992-01-01

Supercritical fluid extraction (SFE) is a viable alternative to current methods of liquid extraction for analyzing semivolatile organic compounds in contaminated solid matrices, such as soil and sediment. Because the SFE method is rapid (less than 30 min), large quantities of glassware and large volumes of solvent are not required, and there are fewer sample-handling and sample-preparation steps than in conventional liquid extraction methods, SFE lends itself to in-the-field extraction of solid samples. Laboratory-scale and portable SFE instruments were designed and tested both in the laboratory and in the field. The SFE method was validated through two recovery studies using individual polycyclic aromatic hydrocarbon (PAH) standards ranging from two to six rings in size and through two Soxhlet extraction comparison studies. Supercritical fluid extraction followed by gas chromatography was applied to 20 coal-tar-contaminated soil samples from three locations, 10 petroleum-oil-tar-contaminated soil samples, and 20 polychlorinated-biphenyl-contaminated soil samples. The SFE apparatus was transported and used in the field at four locations across the United States. Carbon dioxide was used as the extraction fluid

Structural behavior of supercritical fluids under confinement

Science.gov (United States)

Ghosh, Kanka; Krishnamurthy, C. V.

2018-01-01

The existence of the Frenkel line in the supercritical regime of a Lennard-Jones (LJ) fluid shown through molecular dynamics (MD) simulations initially and later corroborated by experiments on argon opens up possibilities of understanding the structure and dynamics of supercritical fluids in general and of the Frenkel line in particular. The location of the Frenkel line, which demarcates two distinct physical states, liquidlike and gaslike within the supercritical regime, has been established through MD simulations of the velocity autocorrelation (VACF) and radial distribution function (RDF). We, in this article, explore the changes in the structural features of supercritical LJ fluid under partial confinement using atomistic walls. The study is carried out across the Frenkel line through a series of MD simulations considering a set of thermodynamics states in the supercritical regime (P =5000 bar, 240 K ≤T ≤1500 K ) of argon well above the critical point. Confinement is partial, with atomistic walls located normal to z and extending to "infinity" along the x and y directions. In the "liquidlike" regime of the supercritical phase, particles are found to be distributed in distinct layers along the z axis with layer spacing less than one atomic diameter and the lateral RDF showing amorphous-like structure for specific spacings (packing frustration) and non-amorphous-like structure for other spacings. Increasing the rigidity of the atomistic walls is found to lead to stronger layering and increased structural order. For confinement with reflective walls, layers are found to form with one atomic diameter spacing and the lateral RDF showing close-packed structure for the smaller confinements. Translational order parameter and excess entropy assessment confirms the ordering taking place for atomistic wall and reflective wall confinements. In the "gaslike" regime of the supercritical phase, particle distribution along the spacing and the lateral RDF exhibit features

High Density Thermal Energy Storage with Supercritical Fluids

Science.gov (United States)

Ganapathi, Gani B.; Wirz, Richard

2012-01-01

A novel approach to storing thermal energy with supercritical fluids is being investigated, which if successful, promises to transform the way thermal energy is captured and utilized. The use of supercritical fluids allows cost-affordable high-density storage with a combination of latent heat and sensible heat in the two-phase as well as the supercritical state. This technology will enhance penetration of several thermal power generation applications and high temperature water for commercial use if the overall cost of the technology can be demonstrated to be lower than the current state-of-the-art molten salt using sodium nitrate and potassium nitrate eutectic mixtures.

Studies on supercritical fluid extraction of uranium from sodium diuranate

International Nuclear Information System (INIS)

Prabhat, Parimal; Vithal, G.K.; Rao, Ankita; Kumar, Pradeep; Tomar, B.S.

2014-01-01

Crude sodium diuranate (SDU) produced from phosphoric acid by solvent extraction process with di-2-ethyl hexyl phosphoric acid (D2EHPA) and tri-n-butyl phosphate(TBP) contains iron and other rare earth impurities along with uranium. For further use of this uranium for fuel fabrication and its subsequent use in nuclear reactors, it has to be purified up to nuclear grade ammonium diuranate (ADU) specifications. Conventionally crude SDU is being purified by dissolving it in nitric acid followed by solvent extraction process using TBP in diluent. Use of large amount of acid and organic solvents for industrial processes is an environmental concern. Nowadays there are efforts to minimize use of acid and organic solvents in industrial processes. Supercritical Fluid Extraction (SFE) of uranium from different matrices (solid as well as liquid) has been reported by several authors in recent years. Near complete extraction of uranium from UO 2 (powder, green pellet and sintered pellet) using TBP-HNO 3 adduct by SFE has been reported. We attempted to explore possibility to purify crude SDU to nuclear grade by SFE of uranium from crude SDU matrix and study the effect of different operational parameters, mode of extraction and complexation

Supercritical fluid chromatography-A Hybrid of GC and LC

Directory of Open Access Journals (Sweden)

Neha Sethi

2010-01-01

Full Text Available High performance specifications and unique functionality of chromatographic techniques is a demand of pharmaceutical industry and research. This leads to the origin of Supercritical Fluid Chromatography (SFC. It is a rapidly expanding analytical technique. The main feature that differentiates SFC from other chromatographic techniques is the replacement of either the liquid or gas mobile phase with a supercritical fluid mobile phase. It is considered a hybrid of GC and LC technique. High diffusion coefficient and low viscosity of supercritical fluids is responsible for high speed analysis, high efficiency and high sensitivity. Low mobile-phase flow rate, density programming and compatability with GC and LC detectors make SFC a versatile chromatographic technique in analytical re-search and development. It has a unique characteristic of analyzing thermo labile or non-volatile substances. This review highlights the role of supercritical fluid chromatography in the separation of polymers, thermally labile pesticides, fatty acids, metal chelates and organometallic compounds, chiral and achiral molecules, identification and analysis of polar samples, explosives, drugs of abuse and application of SFC in forensic science (fingerprint-ing.

Functionalization of silicon oxide using supercritical fluid deposition of 3,4-epoxybutyltrimethoxysilane for the immobilization of amino-modified oligonucleotide

Energy Technology Data Exchange (ETDEWEB)

Rull, Jordi [Université Grenoble Alpes, Grenoble F38000 (France); CEA, LETI, MINATEC Campus, Grenoble Cedex 9 F38054 (France); CEA, iRTSV, LCBM, Grenoble 38054 (France); CNRS, UMR 5249, Grenoble (France); Nonglaton, Guillaume, E-mail: guillaume.nonglaton@cea.fr [Université Grenoble Alpes, Grenoble F38000 (France); CEA, LETI, MINATEC Campus, Grenoble Cedex 9 F38054 (France); Costa, Guillaume; Fontelaye, Caroline [Université Grenoble Alpes, Grenoble F38000 (France); CEA, LETI, MINATEC Campus, Grenoble Cedex 9 F38054 (France); Marchi-Delapierre, Caroline; Ménage, Stéphane [Université Grenoble Alpes, Grenoble F38000 (France); CEA, iRTSV, LCBM, Grenoble 38054 (France); CNRS, UMR 5249, Grenoble (France); Marchand, Gilles [Université Grenoble Alpes, Grenoble F38000 (France); CEA, LETI, MINATEC Campus, Grenoble Cedex 9 F38054 (France)

2015-11-01

Graphical abstract: - Highlights: • First example of grafting of 3,4-epoxybutyltrimethoxysilane (EBTMOS) onto silicon oxide by supercritical fluid deposition. • Extraordinary efficiency of the supercritical fluid deposition for the grafting of the EBTMOS compared with the conventional solution or vapor phase methodologies. • Demonstration of the efficiency of this functionalization process for the immobilization of amino-modified oligonucleotides. - Abstract: The functionalization of silicon oxide based substrates using silanes is generally performed through liquid phase methodologies. These processes involve a huge quantity of potentially toxic solvents and present some important disadvantages for the functionalization of microdevices or porous materials, for example the low diffusion. To overcome this drawback, solvent-free methodologies like molecular vapor deposition (MVD) or supercritical fluid deposition (SFD) have been developed. In this paper, the deposition process of 3,4-epoxybutyltrimethoxysilane (EBTMOS) on silicon oxide using supercritical carbon dioxide (scCO{sub 2}) as a solvent is studied for the first time. The oxirane ring of epoxy silanes readily reacts with amine group and is of particular interest for the grafting of amino-modified oligonucleotides or antibodies for diagnostic application. Then the ability of this specific EBTMOS layer to react with amine functions has been evaluated using the immobilization of amino-modified oligonucleotide probes. The presence of the probes is revealed by fluorescence using hybridization with a fluorescent target oligonucleotide. The performances of SFD of EBTMOS have been optimized and then compared with the dip coating and molecular vapor deposition methods, evidencing a better grafting efficiency and homogeneity, a lower reaction time in addition to the eco-friendly properties of the supercritical carbon dioxide. The epoxysilane layers have been characterized by surface enhanced ellipsometric

Nanotechnology and supercritical fluids | Hamidreza | Journal of ...

African Journals Online (AJOL)

Supercritical fluid (SCF) technology has become an important tool of materials processing in the last two decades. Supercritical CO2 and H2O are extensively being used in the preparation of a great variety of nanomaterials. The interest in the preparation and application of nanometer size materials is increasing since they ...

Occurrence of turbulent flow conditions in supercritical fluid chromatography.

Science.gov (United States)

De Pauw, Ruben; Choikhet, Konstantin; Desmet, Gert; Broeckhoven, Ken

2014-09-26

Having similar densities as liquids but with viscosities up to 20 times lower (higher diffusion coefficients), supercritical CO2 is the ideal (co-)solvent for fast and/or highly efficient separations without mass-transfer limitations or excessive column pressure drops. Whereas in liquid chromatography the flow remains laminar in both the packed bed and tubing, except in extreme cases (e.g. in a 75 μm tubing, pure acetonitrile at 5 ml/min), a supercritical fluid can experience a transition from laminar to turbulent flow in more typical operation modes. Due to the significant lower viscosity, this transition for example already occurs at 1.3 ml/min for neat CO2 when using connection tubing with an ID of 127 μm. By calculating the Darcy friction factor, which can be plotted versus the Reynolds number in a so-called Moody chart, typically used in fluid dynamics, higher values are found for stainless steel than PEEK tubing, in agreement with their expected higher surface roughness. As a result turbulent effects are more pronounced when using stainless steel tubing. The higher than expected extra-column pressure drop limits the kinetic performance of supercritical fluid chromatography and complicates the optimization of tubing ID, which is based on a trade-off between extra-column band broadening and pressure drop. One of the most important practical consequences is the non-linear increase in extra-column pressure drop over the tubing downstream of the column which leads to an unexpected increase in average column pressure and mobile phase density, and thus decrease in retention. For close eluting components with a significantly different dependence of retention on density, the selectivity can significantly be affected by this increase in average pressure. In addition, the occurrence of turbulent flow is also observed in the detector cell and connection tubing. This results in a noise-increase by a factor of four when going from laminar to turbulent flow (e.g. going

Analysis of non-phthalates plasticizers on porous graphitic carbon by supercritical fluid chromatography using evaporative light scattering detection.

Science.gov (United States)

Vaccher, Claude; Decaudin, Bertrand; Sautou, Valérie; Lecoeur, Marie

2014-09-12

The analysis of several plasticizers, widely used in the production of medical devices, was investigated on porous graphitic carbon (PGC) stationary phase in supercritical fluid chromatography (SFC) with an evaporative light scattering detector (ELSD). Due to strong interaction of compounds with the PGC support, solvents of strong eluotropic strength were added to the CO2 supercritical fluid. The effect of alkyl chain (pentane, hexane, heptane) and chlorinated (CH2Cl2, CHCl3, CCl4) solvents was studied on the retention and on the ELSD detection of plasticizers. A co-solvent mixture composed of CHCl3/heptane, eluted under gradient mode, allowed a significant improvement of the ELSD response compared to the use of each solvent individually. Then, a central composite design (CCD) was implemented to optimize both the separation and the detection of plasticizers. The parameters involved were the outlet pressure, the gradient slope, the co-solvent composition and the drift tube temperature of the ELSD. After optimization, baseline separation of plasticizers was achieved in 7min and best signal-to-noise ratios were obtained with outlet pressure and drift tube temperature of ELSD set at 200bar and 31°C, respectively. The co-solvent mixture was also composed of CHCl3/heptane (35/65 v/v) and a gradient from 15 to 60% of co-solvent in 2.2min was employed. The results demonstrated that CCD is a powerful tool for the optimization of SFC/ELSD method and the response surface model analysis can provide statistical understandings of the significant factors required to achieve optimal separation and ELSD sensitivity. Copyright © 2014 Elsevier B.V. All rights reserved.

Operation and Performance of the Supercritical Fluids Reactor (SFR)

National Research Council Canada - National Science Library

Hanush, R

1996-01-01

The Supercritical Fluids Reactor (SFR) at Sandia National Laboratories, CA has been developed to examine and solve engineering, process, and fundamental chemistry issues regarding the development of supercritical water oxidation (SCWO...

The use of supercritical carbon dioxide for contaminant removal from solid waste

International Nuclear Information System (INIS)

Adkins, C.L.J.; Russick, E.M.; Smith, H.M.; Olson, R.B.

1994-01-01

Supercritical carbon dioxide is being explored as a waste minimization technique for separating oils, greases and solvents from solid waste. The containments are dissolved into the supercritical fluid and precipitated out upon depressurization. The carbon dioxide solvent can then be recycled for continued use. Definitions of the temperature, pressure, flowrate and potential co-solvents are required to establish the optimum conditions for hazardous contaminant removal. Excellent extractive capability for common manufacturing oils, greases, and solvents has been observed in both supercritical and liquid carbon dioxide. Solubility measurements are being used to better understand the extraction process, and to determine if the minimum solubility required by federal regulations is met

A comparative study of solvent and supercritical Co2 extraction of Simarouba gluaca seed oil

International Nuclear Information System (INIS)

Anjaneyulu, B.; Satyannarayana, S.; Kanjilal, S.; Siddaiah, V.; Prasanna Rani, K.N.

2017-01-01

In the present study, the supercritical carbon dioxide (Co2) extraction of oil from Simarouba gluaca seeds was carried out at varying conditions of pressure (300–500 bar), temperature (50–70 °C) and CO2 flow rate (10–30 g·min-1). The extraction condition for maximum oil yield was obtained at 500 bar pressure, 70 °C and at 30 g·min-1 flow rate of CO2. The extracted oil was analyzed thoroughly for physico-chemical properties and compared with those of conventional solvent extracted oil. An interesting observation is a significant reduction in the phosphorus content of the oil (8.4 mg·kg-1) extracted using supercritical CO2 compared to the phosphorous content of the solvent extracted oil (97 mg·kg-1). Moreover, the content of total tocopherols in supercritically extracted oil (135.6 mg·kg-1) was found to be higher than the solvent extracted oil (111 mg·kg-1). The rest of the physico-chemical properties of the two differently extracted oils matched well with each other. The results indicated the possible benefits of supercritical CO2 extraction over solvent extraction of Simarouba gluaca seed oil. [es

A comparative study of solvent and supercritical CO2 extraction of Simarouba gluaca seed oil

Directory of Open Access Journals (Sweden)

B. Anjaneyulu

2017-09-01

Full Text Available In the present study, the supercritical carbon dioxide (CO2 extraction of oil from Simarouba gluaca seeds was carried out at varying conditions of pressure (300–500 bar, temperature (50–70 °C and CO2 flow rate (10–30 g·min-1. The extraction condition for maximum oil yield was obtained at 500 bar pressure, 70 °C and at 30 g·min-1 flow rate of CO2. The extracted oil was analyzed thoroughly for physico-chemical properties and compared with those of conventional solvent extracted oil. An interesting observation is a significant reduction in the phosphorus content of the oil (8.4 mg·kg-1 extracted using supercritical CO2 compared to the phosphorous content of the solvent extracted oil (97 mg·kg-1. Moreover, the content of total tocopherols in supercritically extracted oil (135.6 mg·kg-1 was found to be higher than the solvent extracted oil (111 mg·kg-1. The rest of the physico-chemical properties of the two differently extracted oils matched well with each other. The results indicated the possible benefits of supercritical CO2 extraction over solvent extraction of Simarouba gluaca seed oil.

Supercritical fluids in separation science--the dreams, the reality and the future.

Science.gov (United States)

Smith, R M

1999-09-24

The last 20 years have seen an intense interest in the use of supercritical fluids in separation science. This started with the introduction of commercial instruments first for packed and then for capillary chromatography and it looked as if this would be a technique to rival gas-liquid chromatography and HPLC. The activity developed quite rapidly into packed column supercritical fluid separations then into supercritical fluid extraction. However, in recent years there has been a decline in publications. These later techniques continue to be used but are now principally applied to a limited group of applications where they offer significant advantages over alternative techniques. This review looks back over this period and analyses how these methods were developed and the fluids, detectors and applications that were examined. It suggests why many of the initial applications have vanished and why the initial apparent promise was not fulfilled. The rise and fall of supercritical fluids represents a lesson in the way analysts approach new techniques and how we might view other new separation developments at the end of this millennium. The review looks forward to the future of supercritical fluids and their role at the end of the first century of separation science. Probably the most important idea that supercritical fluids have brought to separation science is a recognition that there is unity in the separation methods and that a continuum exists from gases to liquids.

RED WINE EXTRACT OBTAINED BY MEMBRANE-BASED SUPERCRITICAL FLUID EXTRACTION: PRELIMINARY CHARACTERIZATION OF CHEMICAL PROPERTIES.

Directory of Open Access Journals (Sweden)

W. Silva

Full Text Available ABSTRACT This study aims to obtain an extract from red wine by using membrane-based supercritical fluid extraction. This technique involves the use of porous membranes as contactors during the dense gas extraction process from liquid matrices. In this work, a Cabernet Sauvignon wine extract was obtained from supercritical fluid extraction using pressurized carbon dioxide as solvent and a hollow fiber contactor as extraction setup. The process was continuously conducted at pressures between 12 and 18 MPa and temperatures ranged from 30 to 50ºC. Meanwhile, flow rates of feed wine and supercritical CO2 varied from 0.1 to 0.5 mL min-1 and from 60 to 80 mL min-1 (NCPT, respectively. From extraction assays, the highest extraction percentage value obtained from the total amount of phenolic compounds was 14% in only one extraction step at 18MPa and 35ºC. A summarized chemical characterization of the obtained extract is reported in this work; one of the main compounds in this extract could be a low molecular weight organic acid with aromatic structure and methyl and carboxyl groups. Finally, this preliminary characterization of this extract shows a remarkable ORAC value equal to 101737 ± 5324 µmol Trolox equivalents (TE per 100 g of extract.

Supercritical Fluid Chromatography/Fourier Transform Infrared Spectroscopy Of Food Components

Science.gov (United States)

Calvey, Elizabeth M.; Page, Samuel W.; Taylor, Larry T.

1989-12-01

Supercritical fluid (SF) technologies are being investigated extensively for applications in food processing. The number of SF-related patents issued testifies to the level of interest. Among the properties of materials at temperatures and pressures above their critical points (supercritical fluids) is density-dependent solvating power. Supercritical CO2 is of particular interest to the food industry because of its low critical temperature (31.3°C) and low toxicity. Many of the components in food matrices react or degrade at elevated temperatures and may be adversely affected by high temperature extractions. Likewise, these components may not be amenable to GC analyses. Our SF research has been in the development of methods employing supercritical fluid chromatography (SFC) and extraction (SFE) coupled to a Fourier transform infrared (FT-IR) spectrometer to investigate food composition. The effects of processing techniques on the isomeric fatty acid content of edible oils and the analysis of lipid oxidation products using SFC/FT-IR with a flow-cell interface are described.

Selective chelation and extraction of lanthanides and actinides with supercritical fluids

International Nuclear Information System (INIS)

Brauer, R.D.; Carleson, T.E.; Harrington, J.D.; Jean, F.; Jiang, H.; Lin, Y.; Wai, C.M.

1994-01-01

This report is made up of three independent papers: (1) Supercritical Fluid Extraction of Thorium and Uranium with Fluorinated Beta-Diketones and Tributyl Phosphate, (2) Supercritical Fluid Extraction of Lanthanides with Beta-Diketones and Mixed Ligands, and (3) A Group Contribution Method for Predicting the Solubility of Solid Organic Compounds in Supercritical Carbon Dioxide. Experimental data are presented demonstrating the successful extraction of thorium and uranium using fluorinated beta-diketones to form stable complexes that are extracted with supercritical carbon dioxide. The conditions for extracting the lanthanide ions from liquid and solid materials using supercritical carbon dioxide are presented. In addition, the Peng-Robison equation of state and thermodynamic equilibrium are used to predict the solubilities of organic solids in supercritical carbon dioxide from the sublimation pressure, critical properties, and a centric factor of the solid of interest

Supercritical fluids technology. Pt. 1 General topics

International Nuclear Information System (INIS)

Marongiu, B.; De Giorgi, M. R.; Porcedda, S.; Cadoni, E.

1998-01-01

Supercritical fluids technology is among the emerging 'clean' technologies, that allows the minimization in the use of chemical and thermic treatments and products irradiation, diminishing the quantity of liquid wastes to be treated. In this first article phase equilibria thermodynamics and fluid mechanics of transport phenomena are reviewed [it

Obtaining of the antioxidants by supercritical fluid extraction

Directory of Open Access Journals (Sweden)

Babović Nada V.

2011-01-01

Full Text Available One of the important trends in the food industry today is demand for natural antioxidants from plant material. Synthetic antioxidants such as butylated hydroxytoluene (BHT, and butylated hydroxyanisole (BHA are now being replaced by the natural antioxidants because of theirs possible toxicity and as they may act as promoters of carcinogens. The natural antioxidants may show equivalent or higher antioxidant activity than the endogenous or the synthetic antioxidants. Thus, great effort is being devoted to the search for alternative and cheap sources of natural antioxidants, as well as to the development of efficient and selective extraction techniques. The supercritical fluid extraction (SFE with carbon dioxide is considered to be the most suitable method for producing natural antioxidants for the use in food industry. The supercritical extract does not contain residual organic solvents as in conventional extraction processes, which makes these products suitable for use in food, cosmetic and pharmaceutical industry. The recovery of antioxidants from plant sources involves many problematic aspects: choice of an adequate source (in terms of availability, cost, difference in phenolic content with variety and season; selection of the optimal recovery procedure (in terms of yield, simplicity, industrial application, cost; chemical analysis of extracts (for optimization purposes a fast colorimetric method is more preferable than a chromatographic one; evaluation of the antioxidant power (preferably by the different assay methods. The paper presents information about different operational methods for SFE of bioactive compounds from natural sources. It also includes the various reports on the antioxidant activity of the supercritical extracts from Lamiaceae herbs, in comparison with the activity of the synthetic antioxidants and the extracts from Lamiaceae herbs obtained by the conventional methods.

Supercritical Fluid Chromatography- A Hybrid of GC and LC

Directory of Open Access Journals (Sweden)

Kaushal K Chandrul

2010-03-01

Full Text Available

High performance specifications and unique functionality of chromatographic techniques is a demand of pharmaceutical industry and research. This leads to the origin of Supercritical Fluid Chromatography (SFC. It is a rapidly expanding analytical technique. The main feature that differentiates SFC from other chromatographic techniques is the replacement of either the liquid or gas mobile phase with a supercritical fluid mobile phase. It is considered a hybrid of GC and LC technique. High diffusion coefficient and low viscosity of supercritical fluids is responsible for high speed analysis, high efficiency and high sensitivity. Low mobile-phase flow rate, density programming and compatability with GC and LC detectors make SFC a versatile chromatographic technique in analytical research and development. It has a unique characteristic of analyzing thermo labile or non-volatile substances. This review highlights the role of supercritical fluid chromatography in the separation of polymers, thermally labile pesticides, fatty acids, metal chelates and organometallic compounds, chiral and achiral molecules, identification and analysis of polar samples, explosives, drugs of abuse and application of SFC in forensic science (fingerprinting. 

Precipitation of fluticasone propionate microparticles using supercritical antisolvent

Directory of Open Access Journals (Sweden)

A Vatanara

2009-03-01

Full Text Available ABSTRACT Background: The ability of supercritical fluids (SCFs, such as carbon dioxide, to dissolve and expand or extract organic solvents and as result lower their solvation power, makes it possible the use of SCFs for the precipitation of solids from organic solutions. The process could be the injection of a solution of the substrate in an organic solvent into a vessel which is swept by a supercritical fluid. The aim of this study was to ascertain the feasibility of supercritical processing to prepare different particulate forms of fluticasone propionate (FP, and to evaluate the influence of different liquid solvents and precipitation temperatures on the morphology, size and crystal habit of particles. Method: The solution of FP in organic solvents, was precipitated by supercritical carbon dioxide (SCCO2 at two pressure and temperature levels. Effects of process parameters on the physicochemical characteristics of harvested microparticles were evaluated. Results: Particle formation was observed only at the lower selected pressure, whilst at the higher pressure, no precipitation of particles was occurred due to dissolution of FP in supercritical antisolvent. The micrographs of the produced particles showed different morphologies for FP obtained from different conditions. The results of thermal analysis of the resulted particles showed that changes in the processing conditions didn't influence thermal behavior of the precipitated particles. Evaluation of the effect of temperature on the size distribution of particles showed that increase in the temperature from 40 oC to 50 oC, resulted in reduction of the mean particle size from about 30 µm to about 12 μm. ‍Conclusion: From the results of this study it may be concluded that, processing of FP by supercritical antisolvent could be an approach for production of diverse forms of the drug and drastic changes in the physical characteristics of microparticles could be achieved by changing the

Supercritical Fluid Chromatography--Theoretical Background and Applications on Natural Products.

Science.gov (United States)

Hartmann, Anja; Ganzera, Markus

2015-11-01

The use of supercritical fluid chromatography for natural product analysis as well as underlying theoretical mechanisms and instrumental requirements are summarized in this review. A short introduction focusing on the historical development of this interesting separation technique is followed by remarks on the current instrumental design, also describing possible detection modes and useable stationary phases. The overview on relevant applications is grouped based on their basic intention, may it be (semi)preparative or purely analytical. They indicate that supercritical fluid chromatography is still primarily considered for the analysis of nonpolar analytes like carotenoids, fatty acids, or terpenes. The low polarity of supercritical carbon dioxide, which is used with modifiers almost exclusively as a mobile phase today, combined with high efficiency and fast separations might explain the popularity of supercritical fluid chromatography for the analysis of these compounds. Yet, it has been shown that more polar natural products (e.g., xanthones, flavonoids, alkaloids) are separable too, with the same (if not superior) selectivity and reproducibility than established approaches like HPLC or GC. Georg Thieme Verlag KG Stuttgart · New York.

Supercritical extraction of lycopene from tomato industrial wastes with ethane.

Science.gov (United States)

Nobre, Beatriz P; Gouveia, Luisa; Matos, Patricia G S; Cristino, Ana F; Palavra, António F; Mendes, Rui L

2012-07-11

Supercritical fluid extraction of all-E-lycopene from tomato industrial wastes (mixture of skins and seeds) was carried out in a semi-continuous flow apparatus using ethane as supercritical solvent. The effect of pressure, temperature, feed particle size, solvent superficial velocity and matrix initial composition was evaluated. Moreover, the yield of the extraction was compared with that obtained with other supercritical solvents (supercritical CO₂ and a near critical mixture of ethane and propane). The recovery of all-E-lycopene increased with pressure, decreased with the increase of the particle size in the initial stages of the extraction and was not practically affected by the solvent superficial velocity. The effect of the temperature was more complex. When the temperature increased from 40 to 60 °C the recovery of all-E-lycopene increased from 80 to 90%. However, for a further increase to 80 °C, the recovery remained almost the same, indicating that some E-Z isomerization could have occurred, as well as some degradation of lycopene. The recovery of all-E-lycopene was almost the same for feed samples with different all-E-lycopene content. Furthermore, when a batch with a higher all-E-lycopene content was used, supercritical ethane and a near critical mixture of ethane and propane showed to be better solvents than supercritical CO₂ leading to a faster extraction with a higher recovery of the carotenoid.

Comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones.

Science.gov (United States)

Carnes, Stephanie; O'Brien, Stacey; Szewczak, Angelica; Tremeau-Cayel, Lauriane; Rowe, Walter F; McCord, Bruce; Lurie, Ira S

2017-09-01

A comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones has been conducted. Nine different mixtures of bath salts were analyzed in this study. The three different chromatographic techniques were examined using a general set of controlled synthetic cathinones as well as a variety of other synthetic cathinones that exist as positional isomers. Overall 35 different synthetic cathinones were analyzed. A variety of column types and chromatographic modes were examined for developing each separation. For the ultra high performance supercritical fluid chromatography separations, analyses were performed using a series of Torus and Trefoil columns with either ammonium formate or ammonium hydroxide as additives, and methanol, ethanol or isopropanol organic solvents as modifiers. Ultra high performance liquid chromatographic separations were performed in both reversed phase and hydrophilic interaction chromatographic modes using SPP C18 and SPP HILIC columns. Gas chromatography separations were performed using an Elite-5MS capillary column. The orthogonality of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography was examined using principal component analysis. For the best overall separation of synthetic cathinones, the use of ultra high performance supercritical fluid chromatography in combination with gas chromatography is recommended. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Electrodeposition of germanium from supercritical fluids.

Science.gov (United States)

Ke, Jie; Bartlett, Philip N; Cook, David; Easun, Timothy L; George, Michael W; Levason, William; Reid, Gillian; Smith, David; Su, Wenta; Zhang, Wenjian

2012-01-28

Several Ge(II) and Ge(IV) compounds were investigated as possible reagents for the electrodeposition of Ge from liquid CH(3)CN and CH(2)F(2) and supercritical CO(2) containing as a co-solvent CH(3)CN (scCO(2)) and supercritical CH(2)F(2) (scCH(2)F(2)). For Ge(II) reagents the most promising results were obtained using [NBu(n)(4)][GeCl(3)]. However the reproducibility was poor and the reduction currents were significantly less than the estimated mass transport limited values. Deposition of Ge containing films was possible at high cathodic potential from [NBu(n)(4)][GeCl(3)] in liquid CH(3)CN and supercritical CO(2) containing CH(3)CN but in all cases they were heavily contaminated by C, O, F and Cl. Much more promising results were obtained using GeCl(4) in liquid CH(2)F(2) and supercritical CH(2)F(2). In this case the reduction currents were consistent with mass transport limited reduction and bulk electrodeposition produced amorphous films of Ge. Characterisation by XPS showed the presence of low levels of O, F and C, XPS confirmed the presence of Ge together with germanium oxides, and Raman spectroscopy showed that the as deposited amorphous Ge could be crystallised by the laser used in obtaining the Raman measurements.

Method of making supercritical fluid molecular spray films, powder and fibers

Science.gov (United States)

Smith, Richard D.

1988-01-01

Solid films are deposited, or fine powders formed, by dissolving a solid material into a supercritical fluid solution at an elevated pressure and then rapidly expanding the solution through a heated nozzle having a short orifice into a region of relatively low pressure. This produces a molecular spray which is directed against a substrate to deposit a solid thin film thereon, or discharged into a collection chamber to collect a fine powder. In another embodiment, the temperature of the solution and nozzle is elevated above the melting point of the solute, which is preferably a polymer, and the solution is maintained at a pressure such that, during expansion, the solute precipitates out of solution within the nozzle in a liquid state. Alternatively, a secondary solvent mutually soluble with the solute and primary solvent and having a higher critical temperature than that of primary solvent is used in a low concentration (<20%) to maintain the solute in a transient liquid state. The solute is discharged in the form of long, thin fibers. The fibers are collected at sufficient distance from the orifice to allow them to solidify in the low pressure/temperature region.

Modern supercritical fluid technology for food applications.

Science.gov (United States)

King, Jerry W

2014-01-01

This review provides an update on the use of supercritical fluid (SCF) technology as applied to food-based materials. It advocates the use of the solubility parameter theory (SPT) for rationalizing the results obtained when employing sub- and supercritical media to food and nutrient-bearing materials and for optimizing processing conditions. Total extraction and fractionation of foodstuffs employing SCFs are compared and are illustrated by using multiple fluids and unit processes to obtain the desired food product. Some of the additional prophylactic benefits of using carbon dioxide as the processing fluid are explained and illustrated with multiple examples of commercial products produced using SCF media. I emphasize the role of SCF technology in the context of environmentally benign and sustainable processing, as well as its integration into an overall biorefinery concept. Conclusions are drawn in terms of current trends in the field and future research that is needed to secure new applications of the SCF platform as applied in food science and technology.

Scalable organic solvent free supercritical fluid spray drying process for producing dry protein formulations.

Science.gov (United States)

Nuchuchua, O; Every, H A; Hofland, G W; Jiskoot, W

2014-11-01

In this study, we evaluated the influence of supercritical carbon dioxide (scCO2) spray drying conditions, in the absence of organic solvent, on the ability to produce dry protein/trehalose formulations at 1:10 and 1:4 (w/w) ratios. When using a 4L drying vessel, we found that decreasing the solution flow rate and solution volume, or increasing the scCO2 flow rate resulted in a significant reduction in the residual water content in dried products (Karl Fischer titration). The best conditions were then used to evaluate the ability to scale the scCO2 spray drying process from 4L to 10L chamber. The ratio of scCO2 and solution flow rate was kept constant. The products on both scales exhibited similar residual moisture contents, particle morphologies (SEM), and glass transition temperatures (DSC). After reconstitution, the lysozyme activity (enzymatic assay) and structure (circular dichroism, HP-SEC) were fully preserved, but the sub-visible particle content was slightly increased (flow imaging microscopy, nanoparticle tracking analysis). Furthermore, the drying condition was applicable to other proteins resulting in products of similar quality as the lysozyme formulations. In conclusion, we established scCO2 spray drying processing conditions for protein formulations without an organic solvent that holds promise for the industrial production of dry protein formulations. Copyright © 2014 Elsevier B.V. All rights reserved.

Supercritical fluid extraction of reed (thypa)

Energy Technology Data Exchange (ETDEWEB)

Kucuk, M.; Genel, Y. [YYU Educational Faculty, Van (Turkey); Demir, H. [YYU Science and Art Faculty, Van (Turkey)

2005-04-15

Reed (typha) mill was converted to liquid products by using organic solvents (methanol, ethanol and acetone) with catalysts (% 10 NaOH and ZnCl{sub 2}) and without catalyst in an autoclave at temperatures of 533, 553, and 573 K. The liquid products were extracted by liquid-liquid extraction [DSA1] (benzene and diethyl ether). The yields from supercritical methanol, ethanol and acetone conversions were 36.2, 24.5, and 55.1%, respectively, at 573 K. In the catalytic runs with methanol and ethanol extracts were 46.3 and 35.5% (for NaOH catalyst) and 51.8 and 38.5% (for ZnCl{sub 2} catalyst) respectively, at 573 K. The yields from supercritical methanol were increased from 38.2 to 52.4% as the temperature was increased from 533 to 573 K in the catalytic run. (Author)

Near-critical and supercritical fluid extraction of polycyclic aromatic hydrocarbons from town gas soil

International Nuclear Information System (INIS)

Kocher, B.S.; Azzam, F.O.; Cutright, T.J.; Lee, S.

1995-01-01

The contamination of soil by hazardous and toxic organic pollutants is an ever-growing problem facing the global community. One particular family of contaminants that are of major importance are polycyclic aromatic hydrocarbons (PAHs). PAHs are the result of coal gasification and high-temperature processes. Sludges from these town gas operations were generally disposed of into unlined pits and left there for eventual biodegradation. However, the high levels of PAH contained in the pits prevented the occurrence of biodegradation. PAH contaminated soil is now considered hazardous and must be cleaned to environmentally acceptable standards. One method for the remediation is extraction with supercritical water. Water in or about its critical region exhibits enhanced solvating power toward most organic compounds. Contaminated soil containing 4% by mass of hydrocarbons was ultra-cleaned in a 300-cm 3 semicontinuous system to an environmentally acceptable standard of less than 200 ppm residual hydrocarbon concentration. The effects of subcritical or supercritical extraction, solvent temperature, pressure, and density have been studied, and the discerning characteristics of this type of fluid have been identified. The efficiencies of subcritical and supercritical extraction have been discussed from a process engineering standpoint

Fluidos supercríticos em química analítica. I. Cromatografia com fluido supercrítico: conceitos termodinâmicos Supercritical fluid in analytical chemistry. I. Supercritical fluid chromatography: thermodynamic definitions

OpenAIRE

Emanuel Carrilho; Maria Cecília H. Tavares; Fernando M. Lanças

2001-01-01

Under the chromatographic point of view, the physico-chemical properties of a supercritical fluid are intermediate to those of the gases and liquids. Many times they approach the best features of each one, as for example, the solubilization power of liquids and low viscosity of gases. The thermodynamic definitions and main physico-chemical features of a supercritical fluid will be presented in this article. The use of supercritical fluids in analytical chemistry has been extremely modest in B...

Supercritical fluid regeneration of adsorbents

Science.gov (United States)

Defilippi, R. P.; Robey, R. J.

1983-05-01

The results of a program to perform studies supercritical (fluid) carbon dioxide (SCF CO2) regeneration of adsorbents, using samples of industrial wastewaters from manufacturing pesticides and synthetic solution, and to estimate the economics of the specific wastewater treatment regenerations, based on test data are given. Processing costs for regenerating granular activated carbon GAC) for treating industrial wastewaters depend on stream properties and regeneration throughput.

Effect of supercritical fluid density on nanoencapsulated drug particle size using the supercritical antisolvent method.

Science.gov (United States)

Kalani, Mahshid; Yunus, Robiah

2012-01-01

The reported work demonstrates and discusses the effect of supercritical fluid density (pressure and temperature of supercritical fluid carbon dioxide) on particle size and distribution using the supercritical antisolvent (SAS) method in the purpose of drug encapsulation. In this study, paracetamol was encapsulated inside L-polylactic acid, a semicrystalline polymer, with different process parameters, including pressure and temperature, using the SAS process. The morphology and particle size of the prepared nanoparticles were determined by scanning electron microscopy and transmission electron microscopy. The results revealed that increasing temperature enhanced mean particle size due to the plasticizing effect. Furthermore, increasing pressure enhanced molecular interaction and solubility; thus, particle size was reduced. Transmission electron microscopy images defined the internal structure of nanoparticles. Thermal characteristics of nanoparticles were also investigated via differential scanning calorimetry. Furthermore, X-ray diffraction pattern revealed the changes in crystallinity structure during the SAS process. In vitro drug release analysis determined the sustained release of paracetamol in over 4 weeks.

Optimization of metals extraction using cyanex series and NaDDC reagents in liquid/supercritical CO{sub 2}

Energy Technology Data Exchange (ETDEWEB)

Ko, M. S.; Kim, S. H.; Park, K. H.; Kim, H. D.; Kim, H. W. [Kyunghee Univ., Youngin (Korea, Republic of)

2002-05-01

In this research, extraction of small fraction of radioactive elements from mixed contaminated working dress has been conducted by organic solvent extraction, but use of organic solvents has created secondary wastes. In this study, liquid/supercritical fluid CO{sub 2}, an environmentally friendly solvent, was used to extract five metals(Co, Cu, Pb, Cd, Zn). Using five metals selective ligand Cyanex-272 and NaDDC, the most optimized extraction conditions were founded 20 .deg. C, 100atm and complexed ratio(Cyanex-272: 100mg, NaDDC:5mg). The results suggest the possibility of utilizing supercritical fluid technology for extraction of metals from contaminated working dress.

Forensic applications of supercritical fluid chromatography - mass spectrometry.

Science.gov (United States)

Pauk, Volodymyr; Lemr, Karel

2018-06-01

Achievements of supercritical fluid chromatography with mass spectrometric detection made in the field of forensic science during the last decade are reviewed. The main topics include analysis of traditional drugs of abuse (e.g. cannabis, methamphetamine) as well as new psychoactive substances (synthetic cannabinoids, cathinones and phenethylamines), doping agents (anabolic steroids, stimulants, diuretics, analgesics etc.) and chemical warfare agents. Control of food authenticity, detection of adulteration and identification of toxic substances in food are also pointed out. Main aspects of an analytical workflow, such as sample preparation, separation and detection are discussed. A special attention is paid to the performance characteristics and validation parameters of supercritical fluid chromatography-mass spectrometric methods in comparison with other separation techniques. Copyright © 2018 Elsevier B.V. All rights reserved.

SUPERCRITICAL FLUID EXTRACTION OF POLYCYCLIC AROMATIC HYDROCARBON MIXTURES FROM CONTAMINATED SOILS

Science.gov (United States)

Highly contaminated (with PAHs) topsoils were extracted with supercritical CO2 to determine the feasibility and mechanism of supercritical fluid extraction (SFE). Effect of SCF density, temperature, cosolvent type and amount, and of slurrying the soil with water were ...

PROSPECTS FOR USE OF CONDENSED GASES AND SUPERCRITICAL FLUIDS IN PHYTOCHEMICAL PRODUCTION

Directory of Open Access Journals (Sweden)

Demyanenko DV

2017-03-01

Full Text Available In the given review article analysis of the literature and patent sources concerning main methods for intensification of extraction processes of medicinal vegetative raw materials – use of condensed gases and supercritical fluids (SCF on more acceptable extractants has been carried out for last 20 years. Urgency of the specified technologies consists in need for replacement of traditional extraction methods on power- and time-saving ones, and also in use of nontoxic, fire-proof and low-boiling solvents because the most of routine organic solvents (ethanol, methanol, acetone, chloroform, ethylacetate, etc. are toxic and/or flammable or expansive and rather hard to evaporate out from extracts obtained. The abovementioned trends are the most universal for intensification of extraction processes and sometimes purification of final or intermediate products acceptable for commercial scale of manufacture. The main advantages and disadvantages of the given methods are compared for different plant species and groups of biologically active substances (BAS. It has been shown that in most cases supercritical СО2 (SC-СО2 are inferior in its dissolving ability to number of condensed gases and, besides, such technology is much more expensive. The range of BAS taken with SC-СО2 is limited to mainly lipophilic compounds because of zero electrical dipole moment of SC-СО2 and its low polarity. As extractants alternative to SC-СО2 with higher dissolving ability SC - ethane, nitrogen monoxide, freons - R134а, R23, R32, R408 and number of others can be used. Also to enlarge range of extractable BAS it is possible to add different cosolvents, mainly ethanol or methanol in quantity up to 20%. At the same time in phytochemical production prospective alternatives to liquid or supercritical СО2 are certain condensed gases with wider range of physico-chemical properties: fluorinated derivatives of hydrocarbons (freons, liquid ammonia, dimethyl ether (DME

Development and validation of spectroscopic methods for monitoring density changes in pressurized gaseous and supercritical fluid systems.

Science.gov (United States)

Blatchford, Marc A; Wallen, Scott L

2002-04-15

The further development of new processes utilizing liquid or supercritical CO2 as a solvent will benefit from the rational design of new CO2-philes. Understanding solvation structures and mechanisms of these molecules is an important part of this process. In such studies, determining the change in density as a function of the measured thermodynamic conditions (pressure and temperature) provides an excellent means of directly monitoring the solution conditions in the detection volume for a given technique. By integrating spectroscopic peaks, changes in area can be used to determine changes in analyte concentration in the detection volume, and thus, it should be possible to monitor the system density in situ. In the present study, we examine the utility of Raman and NMR spectroscopy as a means of following changes in solution density conditions and validate this approach in pure fluids and gases (N2 and CO2) and supercritical fluid mixtures (acetaldehyde vapor in N2). In addition, we present the design of a simple, inexpensive cell for conducting Raman and NMR measurements under moderate pressure conditions.

On-line supercritical fluid extraction-supercritical fluid chromatography-mass spectrometry of polycyclic aromatic hydrocarbons in soil.

Science.gov (United States)

Wicker, A Paige; Carlton, Doug D; Tanaka, Kenichiro; Nishimura, Masayuki; Chen, Vivian; Ogura, Tairo; Hedgepeth, William; Schug, Kevin A

2018-06-01

On-line supercritical fluid extraction - supercritical fluid chromatography - mass spectrometry (SFE-SFC-MS) has been applied for the determination of polycyclic aromatic hydrocarbons (PAHs) in soil. The purpose of this study was to develop and validate the first on-line SFE-SFC-MS method for the quantification of PAHs in various types of soil. By coupling the sample extraction on-line with chromatography and detection, sample preparation is minimized, diminishing sample loss and contamination, and significantly decreasing the required extraction time. Parameters for on-line extraction coupled to chromatographic analysis were optimized. The method was validated for concentrations of 10-1500 ng of PAHs per gram of soil in Certified Reference Material (CRM) sediment, clay, and sand with R 2  ≥ 0.99. Limits of detection (LOD) were found in the range of 0.001-5 ng/g, and limits of quantification (LOQ) in the range of 5-15 ng/g. The method developed in this study can be effectively applied to the study of PAHs in the environment, and may lay the foundation for further applications of on-line SFE-SFC-MS. Copyright © 2018 Elsevier B.V. All rights reserved.

Dynamics, thermodynamics and structure of liquids and supercritical fluids: crossover at the Frenkel line

Science.gov (United States)

Fomin, Yu D.; Ryzhov, V. N.; Tsiok, E. N.; Proctor, J. E.; Prescher, C.; Prakapenka, V. B.; Trachenko, K.; Brazhkin, V. V.

2018-04-01

We review recent work aimed at understanding dynamical and thermodynamic properties of liquids and supercritical fluids. The focus of our discussion is on solid-like transverse collective modes, whose evolution in the supercritical fluids enables one to discuss the main properties of the Frenkel line separating rigid liquid-like and non-rigid gas-like supercritical states. We subsequently present recent experimental evidence of the Frenkel line showing that structural and dynamical crossovers are seen at a pressure and temperature corresponding to the line as predicted by theory and modelling. Finally, we link dynamical and thermodynamic properties of liquids and supercritical fluids by the new calculation of liquid energy governed by the evolution of solid-like transverse modes. The disappearance of those modes at high temperature results in the observed decrease of heat capacity.

Comparison of liquid and supercritical fluid chromatography mobile phases for enantioselective separations on polysaccharide stationary phases.

Science.gov (United States)

Khater, Syame; Lozac'h, Marie-Anne; Adam, Isabelle; Francotte, Eric; West, Caroline

2016-10-07

Analysis and production of enantiomerically pure compounds is a major topic of interest when active pharmaceutical ingredients are concerned. Enantioselective chromatography has become a favourite both at the analytical and preparative scales. High-performance liquid chromatography (HPLC) and supercritical fluid chromatography (SFC) are dominating the scene and are often seen as complementary techniques. Nowadays, for economic and ecologic reasons, SFC may be preferred over normal-phase HPLC (NPLC) as it allows significant reductions in solvent consumption. However, the transfer of NPLC methods to SFC is not always straightforward. In this study, we compare the retention of achiral molecules and separation of enantiomers under supercritical fluid (carbon dioxide with ethanol or isopropanol) and liquid normal-phase (heptane with ethanol or isopropanol) elution modes with polysaccharide stationary phases in order to explore the differences between the retention and enantioseparation properties between the two modes. Chemometric methods (namely quantitative structure-retention relationships and discriminant analysis) are employed to compare the results obtained on a large set of analytes (171 achiral probes and 97 racemates) and gain some understanding on the retention and separation mechanisms. The results indicate that, contrary to popular belief, carbon dioxide - solvent SFC mobile phases are often weaker eluents than liquid mobile phases. It appears that SFC and NPLC elution modes provide different retention mechanisms. While some enantioseparations are unaffected, facilitating the transfer between the two elution modes, other enantioseparations may be drastically different due to different types and strength of interactions contributing to enantioselectivity. Copyright © 2016 Elsevier B.V. All rights reserved.

Environmentally Friendly Procedure Based on Supercritical Fluid Chromatography and Tandem Mass Spectrometry Molecular Networking for the Discovery of Potent Antiviral Compounds from Euphorbia semiperfoliata.

Science.gov (United States)

Nothias, Louis-Félix; Boutet-Mercey, Stéphanie; Cachet, Xavier; De La Torre, Erick; Laboureur, Laurent; Gallard, Jean-François; Retailleau, Pascal; Brunelle, Alain; Dorrestein, Pieter C; Costa, Jean; Bedoya, Luis M; Roussi, Fanny; Leyssen, Pieter; Alcami, José; Paolini, Julien; Litaudon, Marc; Touboul, David

2017-10-27

A supercritical fluid chromatography-based targeted purification procedure using tandem mass spectrometry and molecular networking was developed to analyze, annotate, and isolate secondary metabolites from complex plant extract mixture. This approach was applied for the targeted isolation of new antiviral diterpene esters from Euphorbia semiperfoliata whole plant extract. The analysis of bioactive fractions revealed that unknown diterpene esters, including jatrophane esters and phorbol esters, were present in the samples. The purification procedure using semipreparative supercritical fluid chromatography led to the isolation and identification of two new jatrophane esters (13 and 14) and one known (15) and three new 4-deoxyphorbol esters (16-18). The structure and absolute configuration of compound 16 were confirmed by X-ray crystallography. This compound was found to display antiviral activity against Chikungunya virus (EC 50 = 0.45 μM), while compound 15 proved to be a potent and selective inhibitor of HIV-1 replication in a recombinant virus assay (EC 50 = 13 nM). This study showed that a supercritical fluid chromatography-based protocol and molecular networking can facilitate and accelerate the discovery of bioactive small molecules by targeting molecules of interest, while minimizing the use of toxic solvents.

Supercritical fluid chromatography coupled with tandem mass spectrometry: A high-efficiency detection technique to quantify Taxane drugs in whole-blood samples.

Science.gov (United States)

Jin, Chan; Guan, Jibin; Zhang, Dong; Li, Bing; Liu, Hongzhuo; He, Zhonggui

2017-10-01

We present a technique to rapid determine taxane in blood samples by supercritical fluid chromatography together with mass spectrometry. The aim of this study was to develop a supercritical fluid chromatography with mass spectrometry method for the analysis of paclitaxel, cabazitaxel, and docetaxel in whole-blood samples of rats. Liquid-dry matrix spot extraction was selected in sample preparation procedure. Supercritical fluid chromatography separation of paclitaxel, cabazitaxel, docetaxel, and glyburide (internal standard) was accomplished within 3 min by using the gradient mobile phase consisted of methanol as the compensation solvent and carbon dioxide at a flow rate of 1.0 mL/min. The method was validated regarding specificity, the lower limit of quantification, repeatability, and reproducibility of quantification, extraction recovery, and matrix effects. The lower limit of quantification was found to be 10 ng/mL since it exhibited acceptable precision and accuracy at the corresponding level. All interday accuracies and precisions were within the accepted criteria of ±15% of the nominal value and within ±20% at the lower limit of quantification, implying that the method was reliable and reproducible. In conclusion, this method is a promising tool to support and improve preclinical or clinical pharmacokinetic studies with the taxanes anticancer drugs. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

US-UK Phase 3 Task 1 Oxidation in Supercritical Fluids

Energy Technology Data Exchange (ETDEWEB)

Holcomb, Gordon R. [National Energy Technology Lab. (NETL), Albany, OR (United States)

2017-03-20

A presentation of the US-UK Phase 3 Task 1 Oxidation in Supercritical Fluids. Includes slides on Supercritical Steam, sCO₂ Power Cycles – Indirect, sCO₂ Power Cycles – Direct, Experimental Exposures, Alloys, Why Si, Results—Ni-xCr Alloys (5-24Cr), Fatigue Crack Growth$-$Experiment, and Alloys and Samples, Fatigue Crack Growth—Results (H282).

A fully continuous supercritical fluid extraction system for contaminated soil

International Nuclear Information System (INIS)

Ryan, M.; Stiver, W.H.

2007-01-01

Brownfield sites are contaminated sites in an urban setting. There are hundreds of thousands of such sites, where contaminants migrate to the atmosphere, seep into groundwater, runoff into surface water and enter the food chain through plant uptake and soil ingestion. The Sydney Tar Ponds alone contain more than a million tonnes of contaminated soils and sediments. Soil vapour extraction, incineration, bioremediation, solvent extraction and land filling are among the remediation techniques that have been developed for brownfield sites over the years. However, no single technology is ideally suited to all cases because of the diversity of contaminants and diversity of site characterization. This paper focused on supercritical fluid extraction (SFE) which is well suited to sites contaminated with polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and heavy metal. A fully continuous laboratory-scale SFE process for a slurry-based system was designed and constructed to handle the supercritical carbon dioxide (SC-CO 2 ) and the soil slurry. The system continuously pumps carbon dioxide under supercritical conditions and soil slurry into a counter-current contacting column. The testing soil was Delhi loamy sand, spiked with 10 mg/g of naphthalene. The soil slurry ranged from 0.0028 g dry soil per g slurry to 0.072 g/g. The operating temperature was 43 degrees C and the operating pressure was 7.7 MPa. Near steady state, fully continuous flow was achieved with runs lasting up to 2 hours. The quantifiable recoveries of naphthalene from the soil slurry was demonstrated and the mass transfer coefficients for the system were quantified in order to provide the foundation to advance to a full-scale system and costing analysis. 14 refs., 1 tab., 3 figs

A fully continuous supercritical fluid extraction system for contaminated soil

Energy Technology Data Exchange (ETDEWEB)

Ryan, M.; Stiver, W.H. [Guelph Univ., ON (Canada). School of Engineering

2007-04-15

Brownfield sites are contaminated sites in an urban setting. There are hundreds of thousands of such sites, where contaminants migrate to the atmosphere, seep into groundwater, runoff into surface water and enter the food chain through plant uptake and soil ingestion. The Sydney Tar Ponds alone contain more than a million tonnes of contaminated soils and sediments. Soil vapour extraction, incineration, bioremediation, solvent extraction and land filling are among the remediation techniques that have been developed for brownfield sites over the years. However, no single technology is ideally suited to all cases because of the diversity of contaminants and diversity of site characterization. This paper focused on supercritical fluid extraction (SFE) which is well suited to sites contaminated with polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and heavy metal. A fully continuous laboratory-scale SFE process for a slurry-based system was designed and constructed to handle the supercritical carbon dioxide (SC-CO{sub 2}) and the soil slurry. The system continuously pumps carbon dioxide under supercritical conditions and soil slurry into a counter-current contacting column. The testing soil was Delhi loamy sand, spiked with 10 mg/g of naphthalene. The soil slurry ranged from 0.0028 g dry soil per g slurry to 0.072 g/g. The operating temperature was 43 degrees C and the operating pressure was 7.7 MPa. Near steady state, fully continuous flow was achieved with runs lasting up to 2 hours. The quantifiable recoveries of naphthalene from the soil slurry was demonstrated and the mass transfer coefficients for the system were quantified in order to provide the foundation to advance to a full-scale system and costing analysis. 14 refs., 1 tab., 3 figs.

A systematic investigation of sample diluents in modern supercritical fluid chromatography.

Science.gov (United States)

Desfontaine, Vincent; Tarafder, Abhijit; Hill, Jason; Fairchild, Jacob; Grand-Guillaume Perrenoud, Alexandre; Veuthey, Jean-Luc; Guillarme, Davy

2017-08-18

This paper focuses on the possibility to inject large volumes (up to 10μL) in ultra-high performance supercritical fluid chromatography (UHPSFC) under generic gradient conditions. Several injection and method parameters have been individually evaluated (i.e. analyte concentration, injection volume, initial percentage of co-solvent in the gradient, nature of the weak needle wash solvent, nature of the sample diluent, nature of the column and of the analyte). The most critical parameters were further investigated using in a multivariate approach. The overall results suggested that several aprotic solvents including methyl tert-butyl ether (MTBE), dichloromethane, acetonitrile or cyclopentyl methyl ether (CPME) were well adapted for the injection of large volume in UHPSFC, while MeOH was generally the worst alternative. However, the nature of the stationary phase also had a strong impact and some of these diluents did not perform equally on each column. This was due to the existence of a competition in the adsorption of the analyte and the diluent on the stationary phase. This observation introduced the idea that the sample diluent should not only be chosen according to the analyte but also to the column chemistry to limit the interactions between the diluent and the ligands. Other important characteristics of the "ideal" SFC sample diluent were finally highlighted. Aprotic solvents with low viscosity are preferable to avoid strong solvent effects and viscous fingering, respectively. In the end, the authors suggest that the choice of the sample diluent should be part of the method development, as a function of the analyte and the selected stationary phase. Copyright © 2017 Elsevier B.V. All rights reserved.

Discovering geothermal supercritical fluids: a new frontier for seismic exploration.

Science.gov (United States)

Piana Agostinetti, Nicola; Licciardi, Andrea; Piccinini, Davide; Mazzarini, Francesco; Musumeci, Giovanni; Saccorotti, Gilberto; Chiarabba, Claudio

2017-11-06

Exploiting supercritical geothermal resources represents a frontier for the next generation of geothermal electrical power plant, as the heat capacity of supercritical fluids (SCF),which directly impacts on energy production, is much higher than that of fluids at subcritical conditions. Reconnaissance and location of intensively permeable and productive horizons at depth is the present limit for the development of SCF geothermal plants. We use, for the first time, teleseismic converted waves (i.e. receiver function) for discovering those horizons in the crust. Thanks to the capability of receiver function to map buried anisotropic materials, the SCF-bearing horizon is seen as the 4km-depth abrupt termination of a shallow, thick, ultra-high (>30%) anisotropic rock volume, in the center of the Larderello geothermal field. The SCF-bearing horizon develops within the granites of the geothermal field, bounding at depth the vapor-filled heavily-fractured rock matrix that hosts the shallow steam-dominated geothermal reservoirs. The sharp termination at depth of the anisotropic behavior of granites, coinciding with a 2 km-thick stripe of seismicity and diffuse fracturing, points out the sudden change in compressibility of the fluid filling the fractures and is a key-evidence of deep fluids that locally traversed the supercritical conditions. The presence of SCF and fracture permeability in nominally ductile granitic rocks open new scenarios for the understanding of magmatic systems and for geothermal exploitation.

Rapid Determination of Two Triterpenoid Acids in Chaenomelis Fructus Using Supercritical Fluid Extraction On-line Coupled with Supercritical Fluid Chromatography.

Science.gov (United States)

Zhang, Xiaotian; Ji, Feng; Li, Yueqi; He, Tian; Han, Ya; Wang, Daidong; Lin, Zongtao; Chen, Shizhong

2018-01-01

In this study, an on-line supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC) method was developed for the rapid determination of oleanoic acid and ursolic acid in Chaenomelis Fructus. After optimization of the conditions, the two triterpenoid acids was obtained by SFE using 20% methanol as a modifier at 35°C in 8 min. They were resolved on a Shim-pack UC-X Diol column (4.6 × 150 mm, 3 μm) in 14 min (0 - 10 min, 5 - 10%; 10 - 14 min, 10% methanol in CO 2 ) with a backpressure of 15 MPa at 40°C. The on-line SFE-SFC method could be completed within 40 min (10.79 mg/g dry plant, R s = 2.36), while the ultrasound-assisted extraction and HPLC method required at least 90 min (3.55 mg/g dry plant, R s = 1.92). This on-line SFE-SFC method is powerful to simplify the pre-processing and quantitative analysis of natural products.

Ion mobility spectrometry after supercritical fluid chromatography

International Nuclear Information System (INIS)

Morrissey, M.A.

1988-01-01

In this work, a Fourier transform ion mobility spectrometer (FT-IMS) was constructed and evaluated as a detector for supercritical fluid chromatography (SFC). The FT-IMS provides both quantitative and qualitative data of a wide range of compounds, selective and nonselective modes of chromatographic detection, and it is compatible with a wide range of SFC mobile phases. Drift spectra are presented for a number of samples, including polymers, lipids, herbicides, antibiotics, and pharmaceuticals. The unique properties of supercritical fluids made it possible to introduce these compounds into the spectrometer. While the drift spectra presented are generally simple, showing only a quasi-molecular ion, a few are surprising complex. Examples of selective and non-selective detection demonstrate the usefulness of the detector. Examples are presented for fish oil concentrate, bacon grease extract, soil extract, and polymer mixtures. In the case of Triton X-100, a non-ionic surfactant, the FT-IMS was able to selectively detect individual oligomers in the polymer mixture. In the case of a polydimethylsilicone mixture the detector isolated a contaminant in the mixture

Supercritical Fluid Extraction of Eucalyptus globulus Bark—A Promising Approach for Triterpenoid Production

Science.gov (United States)

Domingues, Rui M. A.; Oliveira, Eduardo L. G.; Freire, Carmen S. R.; Couto, Ricardo M.; Simões, Pedro C.; Neto, Carlos P.; Silvestre, Armando J. D.; Silva, Carlos M.

2012-01-01

Eucalyptus bark contains significant amounts of triterpenoids with demonstrated bioactivity, namely triterpenic acids and their acetyl derivatives (ursolic, betulinic, oleanolic, betulonic, 3-acetylursolic, and 3-acetyloleanolic acids). In this work, the supercritical fluid extraction (SFE) of Eucalyptus globulus deciduous bark was carried out with pure and modified carbon dioxide to recover this fraction, and the results were compared with those obtained by Soxhlet extraction with dichloromethane. The effects of pressure (100–200 bar), co-solvent (ethanol) content (0, 5 and 8% wt), and multistep operation were studied in order to evaluate the applicability of SFE for their selective and efficient production. The individual extraction curves of the main families of compounds were measured, and the extracts analyzed by GC-MS. Results pointed out the influence of pressure and the important role played by the co-solvent. Ethanol can be used with advantage, since its effect is more important than increasing pressure by several tens of bar. At 160 bar and 40 °C, the introduction of 8% (wt) of ethanol greatly improves the yield of triterpenoids more than threefold. PMID:22837719

Remediation of flare pit soils using supercritical fluid extraction

Energy Technology Data Exchange (ETDEWEB)

Nagpal, V.; Guigard, S.E. [Alberta Univ., Edmonton, AB (Canada). Dept. of Civil Engineering

2005-09-01

A laboratory study was conducted to examine the ability of supercritical fluid extraction (SFE) to remove petroleum hydrocarbons (PHCs) from two flare pit soils in Alberta. SFE is a technology for remediation of contaminated soils. In order to determine the optimal extraction conditions and to understand the effects of pressure, temperature, supercritical carbon dioxide flow rate, soil type, and extraction time on the extraction efficiency of SFE, extractions were performed on two flare pit soils at various pressures and temperatures. Chemicals in the study included diesel oil, SAE 10-30W motor oil, n-decane, hexadecane, tetratriacontane and pentacontane. The best extraction conditions were defined as conditions that result in a treated soil with a PHC concentration that meets the regulatory guidelines of the Canadian Council of Ministers of the Environment in the Canada-wide standard for PHC is soil. The study results indicate that the efficiency of the SFE process is solvent-density dependent for the conditions studied. The highest extraction efficiency for both soils was obtained at conditions of 24.1 MPa and 40 degrees C. An increase in pressure at a fixed temperature led to an increase in the extraction efficiency while an increase in temperature at a fixed pressure led to a decrease in the extraction efficiency. The treated soils were observed to be lighter in colour, drier, and grainier than the soil prior to extraction. It was concluded that SFE is an effective method for remediating flare pit soils. 63 refs., 4 tabs., 5 figs.

Supercritical Fluid Extraction of Seed Oil from Chinese Licorice ...

African Journals Online (AJOL)

NJD

2005-12-17

Dec 17, 2005 ... a Key Laboratory of Forest Plant Ecology, Northeast Forestry University, Hexing Road 26, 150040, ... Carbon dioxide, the most commonly used supercritical fluid, has ... absorb the remaining water that the chloroform layer had.

Countercurrent flow of supercritical anti-solvent in the production of pure xanthophylls from Nannochloropsis oculata.

Science.gov (United States)

Cho, Yueh-Cheng; Wang, Yuan-Chuen; Shieh, Chwen-Jen; Lin, Justin Chun-Te; Chang, Chieh-Ming J; Han, Esther

2012-08-10

This study examined pilot scaled elution chromatography coupled with supercritical anti-solvent precipitation (using countercurrent flow) in generating zeaxanthin-rich particulates from a micro-algal species. Ultrasonic agitated acetone extract subjected to column fractionation successfully yielded a fraction containing 349.4 mg/g of zeaxanthin with a recovery of 85%. Subsequently, supercritical anti-solvent (SAS) precipitation of the column fraction at 150 bar and 343 K produced submicron-sized particulates with a concentration of 845.5mg/g of zeaxanthin with a recovery of 90%. Experimental results from a two-factor response surface method SAS precipitation indicated that purity, mean size and morphology of the precipitates were significantly affected by the flow type configuration, feed flow rate and injection time. Copyright © 2012 Elsevier B.V. All rights reserved.

Fluid extraction using carbon dioxide and organophosphorus chelating agents

Science.gov (United States)

Smart, Neil G.; Wai, Chien M.; Lin, Yuehe; Kwang, Yak Hwa

1998-01-01

Methods for extracting metalloid and metal species from a solid or liquid material by exposing the material to a fluid solvent, particularly supercritical CO.sub.2, and a chelating agent are described. The chelating agent forms a chelate with the species, the chelate being soluble in the fluid to allow removal of the species from the material. In preferred embodiments the extraction solvent is supercritical CO.sub.2 and the chelating agent comprises an organophosphorous chelating agent, particularly sulfur-containing organophosphorous chelating agents, including mixtures of chelating agents. Examples of chelating agents include monothiophosphinic acid, di-thiophosphinic acid, phosphine sulfite, phosphorothioic acid, and mixtures thereof. The method provides an environmentally benign process for removing metal and metalloids from industrial waste solutions, particularly acidic solutions. Both the chelate and the supercritical fluid can be regenerated and the contaminant species recovered to provide an economic, efficient process.

Supercritical fluid extraction of meat lipids: an alternative approach to the identification of irradiated meats

International Nuclear Information System (INIS)

Hampson, J.W.; Jones, K.C.; Foglia, T.A.; Kohout, K.M.

1996-01-01

Ionizing radiation is currently under study as an alternative method for extending the shelf life of meats and meat products. Accordingly, methods are needed to determine if a meat or meat product has been exposed to ionizing radiation. In this study, a method is described for the isolation and analysis of volatile hydrocarbons formed in meat lipids after exposure to ionizing radiation. The method is based on supercritical fluid extraction of the hydrocarbons from meat lipids and subsequent identification and quantitation of individual hydrocarbons by gas chromatography (GC) with a mass selection detector (MSD). Supercritical carbon dioxide at 175 bar and 40°C extracted the hydrocarbon fraction from total meat lipids within 20 min. The presence of radiolytic hydrocarbons, as determined by GC/MSD, was then correlated to the degree of irradiation of the meat from 0 to 10 kGy. Besides being faster, this method has the advantage of reduced solvent consumption when compared to current methods for determining if a meat or meat product has been irradiated

Multi-walled carbon nanotubes (MWCNTs) functionalized with amino groups by reacting with supercritical ammonia fluids

International Nuclear Information System (INIS)

Shao Lu; Bai Yongping; Huang Xu; Gao Zhangfei; Meng Linghui; Huang Yudong; Ma Jun

2009-01-01

For the first time, supercritical ammonia fluid was utilized to simply functionalize multi-walled carbon nanotube (MWCNT) with amino groups. The successful amino functionalization of MWCNTs was proven and the physicochemical properties of MWCNTs before and after supercritical ammonia fluids modifications were characterized using X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM), atomic force microscope (AFM) and Raman spectroscopy. The results also indicated that the supercritical ammonia fluids had the visible effects on the nanostructure of carbon nanotubes. Our novel modification approach provides an easy way to modify MWCNTs with amino groups, which is very useful for realizing 'carbon nanotube economy' in the near future.

Critical Casimir effect in a polymer chain in supercritical solvents.

Science.gov (United States)

Sumi, Tomonari; Imazaki, Nobuyuki; Sekino, Hideo

2009-03-01

Density fluctuation effects on the conformation of a polymer chain in a supercritical solvent were investigated by performing a multiscale simulation based on the density-functional theory. We found (a) a universal swelling of the polymer chain near the critical point, irrespective of whether the polymer chain is solvophilic or solvophobic, and (b) a characteristic collapse of the polymer chain having a strong solvophilicity at a temperature slightly higher than the critical point, where the isothermal compressibility becomes less than the ideal one.

Degradation of brominated flame retardant in computer housing plastic by supercritical fluids.

Science.gov (United States)

Wang, Yanmin; Zhang, Fu-Shen

2012-02-29

The degradation process of brominated flame retardant (BFR) and BFR-containing waste computer housing plastic in various supercritical fluids (water, methanol, isopropanol and acetone) was investigated. The results showed that the debromination and degradation efficiencies, final products were greatly affected by the solvent type. Among the four tested solvents, isopropanol was the most suitable solvent for the recovery of oil from BFR-containing plastic for its (1) excellent debromination effectiveness (debromination efficiency 95.7%), (2) high oil production (60.0%) and (3) mild temperature and pressure requirements. However, in this case, the removed bromine mostly existed in the oil. Introduction of KOH into the sc-isopropanol could capture almost all the inorganic bromine from the oil thus bromine-free oil could be obtained. Furthermore, KOH could enhance the depolymerization of the plastic. The obtained oil mainly consisted of single- and duplicate-ringed aromatic compounds in a carbon range of C9-C17, which had alkyl substituents or aliphatic bridges, such as butyl-benzene, (3-methylbutyl)-benzene, 1,1'-(1,3-propanediyl)bis benzene. Phenol, alkyl phenols and esters were the major oxygen-containing compounds in the oil. This study provides an efficient approach for debromination and simultaneous recovering valuable chemicals from BFR-containing plastic in e-waste. Copyright © 2011 Elsevier B.V. All rights reserved.

Advanced Materials Deposition for Semiconductor Nanostructures Using Supercritical Fluids

National Research Council Canada - National Science Library

Wai, Chien M

2007-01-01

... able to dissolve solutes like a liquid and transport dissolved materials like a gas. Metal and metal sulfide nanoparticles of controllable size can be synthesized in supercritical fluid carbon dioxide using water-in-CO2 microemulsion as template...

Hyphenation of supercritical fluid chromatography with tandem mass spectrometry for fast determination of four aflatoxins in edible oil.

Science.gov (United States)

Lei, Fang; Li, Chenglong; Zhou, Shuang; Wang, Dan; Zhao, Yunfeng; Wu, Yongning

2016-08-01

Aflatoxins (AFTs) are of great concern all over the world. Supercritical fluid chromatography (SFC) has the advantage of fast, high resolution and excellent compatibility with a broad range of organic solvents and samples, thus hyphenating SFC with tandem mass spectrometry (MS/MS) can be used for the easy and fast determination of AFTs in edible oils. Edible oil was spiked with isotope-labeled aflatoxin standards, diluted with hexane and extracted with acetonitrile. The extraction was directly loaded to an SFC apparatus and separated on a UPC(2) 2-EP column with CO2 -methanol gradient elution. A post-column make-up flow was introduced to facilitate mass spectrometry performance, and the mixture was analyzed by MS/MS with an electrospray ionization (ESI) source. The SFC conditions including separation column, modifier and sample solvent were optimized, and the four target aflatoxins were baseline separated. The ESI interface parameters were also investigated, implicating the make-up flow as a critical factor for sensitive determination by SFC-MS/MS. The LOQs for the AFTs were 0.05-0.12 μg L(-1) , while the RSDs were lower than 8.5%. Supercritical fluid chromatography was successfully coupled to tandem mass spectrometry to establish a simple, fast and sensitive method for the analysis of four aflatoxins in edible oil. This shows the combination of SFC-MS/MS has great potential in determination of trace contaminants in food. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Turbulent mixing of a slightly supercritical van der Waals fluid at low-Mach number

International Nuclear Information System (INIS)

Battista, F.; Casciola, C. M.; Picano, F.

2014-01-01

Supercritical fluids near the critical point are characterized by liquid-like densities and gas-like transport properties. These features are purposely exploited in different contexts ranging from natural products extraction/fractionation to aerospace propulsion. Large part of studies concerns this last context, focusing on the dynamics of supercritical fluids at high Mach number where compressibility and thermodynamics strictly interact. Despite the widespread use also at low Mach number, the turbulent mixing properties of slightly supercritical fluids have still not investigated in detail in this regime. This topic is addressed here by dealing with Direct Numerical Simulations of a coaxial jet of a slightly supercritical van der Waals fluid. Since acoustic effects are irrelevant in the low Mach number conditions found in many industrial applications, the numerical model is based on a suitable low-Mach number expansion of the governing equation. According to experimental observations, the weakly supercritical regime is characterized by the formation of finger-like structures – the so-called ligaments – in the shear layers separating the two streams. The mechanism of ligament formation at vanishing Mach number is extracted from the simulations and a detailed statistical characterization is provided. Ligaments always form whenever a high density contrast occurs, independently of real or perfect gas behaviors. The difference between real and perfect gas conditions is found in the ligament small-scale structure. More intense density gradients and thinner interfaces characterize the near critical fluid in comparison with the smoother behavior of the perfect gas. A phenomenological interpretation is here provided on the basis of the real gas thermodynamics properties

Turbulent mixing of a slightly supercritical van der Waals fluid at low-Mach number

Energy Technology Data Exchange (ETDEWEB)

Battista, F.; Casciola, C. M. [Department of Mechanical and Aerospace Engineering, Sapienza University, via Eudossiana 18, 00184 Rome (Italy); Picano, F. [Department of Industrial Engineering, University of Padova, via Venezia 1, 35131 Padova (Italy)

2014-05-15

Supercritical fluids near the critical point are characterized by liquid-like densities and gas-like transport properties. These features are purposely exploited in different contexts ranging from natural products extraction/fractionation to aerospace propulsion. Large part of studies concerns this last context, focusing on the dynamics of supercritical fluids at high Mach number where compressibility and thermodynamics strictly interact. Despite the widespread use also at low Mach number, the turbulent mixing properties of slightly supercritical fluids have still not investigated in detail in this regime. This topic is addressed here by dealing with Direct Numerical Simulations of a coaxial jet of a slightly supercritical van der Waals fluid. Since acoustic effects are irrelevant in the low Mach number conditions found in many industrial applications, the numerical model is based on a suitable low-Mach number expansion of the governing equation. According to experimental observations, the weakly supercritical regime is characterized by the formation of finger-like structures – the so-called ligaments – in the shear layers separating the two streams. The mechanism of ligament formation at vanishing Mach number is extracted from the simulations and a detailed statistical characterization is provided. Ligaments always form whenever a high density contrast occurs, independently of real or perfect gas behaviors. The difference between real and perfect gas conditions is found in the ligament small-scale structure. More intense density gradients and thinner interfaces characterize the near critical fluid in comparison with the smoother behavior of the perfect gas. A phenomenological interpretation is here provided on the basis of the real gas thermodynamics properties.

Numerical simulation of stress distribution in Inconel 718 components realized by metal injection molding during supercritical debinding

Science.gov (United States)

Agne, Aboubakry; Barrière, Thierry

2018-05-01

Metal injection molding (MIM) is a process combining advantages of thermoplastic injection molding and powder metallurgy process in order to manufacture components with complex and near net-shape geometries. The debinding of a green component can be performed in two steps, first by using solvent debinding in order to extract the organic part of the binder and then by thermal degradation of the rest of the binder. A shorter and innovative method for extracting an organic binder involves the use of supercritical fluid instead of a regular solvent. The debinding via a supercritical fluid was recently investigated to extract organic binders contained in components obtained by Metal Injection Molding. It consists to put the component in an enclosure subjected to high pressure and temperature. The supercritical fluid has various properties depending on these two conditions, e.g., density and viscosity. The high-pressure combined with the high temperature during the process affect the component structure. Three mechanisms contributing to the deformation of the component can been differentiated: thermal expansion, binder extraction and supercritical fluid effect on the outer surfaces of the component. If one supposes that, the deformation due to binder extraction is negligible, thermal expansion and the fluid effect are probably the main mechanisms that can produce several stress. A finite-element model, which couples fluid-structures interaction and structural mechanics, has been developed and performed on the Comsol Multiphysics® finite-element software platform allowed to estimate the stress distribution during the supercritical debinding of MIM component composed of Inconel 718 powders, polypropylene, polyethylene glycol and stearic acid as binder. The proposed numerical simulations allow the estimation of the stress distribution with respect to the processing parameters for MIM components during the supercritical debinding process using a stationary solver.

Supercritical fluid extraction of γ-Pyrones from Ammi visnaga L. fruits

Directory of Open Access Journals (Sweden)

Mokhtar Bishr

2018-06-01

Full Text Available Extraction with supercritical fluid technique has proved to be effective in many applications including extraction and separation of various active principals from medicinal plants. It was used due to its advantages especially safety, specificity, selectivity and ease of component recovery.Ammi visnaga, L. belongs to the family Apiaceae. The fruits are used specifically for the treatment of kidney stones depending on its γ-Pyrones (mainly khellin and visnagin [2]. The supercritical fluid extraction technique of khellin and visnagin was investigated and the operating conditions for their extraction were optimized. The effect of different pressure (150, 200, 300, 400 and 500 bars, temperature (35, 40, 45, 50 and 55 °C, and particle sizes of the raw material (0.5, 1, 1.4 mm and entire fruits on the extract yield was studied under dynamic conditions for extraction for a run time of 90 min. Optimum supercritical extraction condition was found to be 200 bars at 45 °C and optimum particle size was found to be 1.4 mm. The yield is yellowish white bitter powder and measures 1.74% w/w relative to the dried weight of the fruits containing 38.414% w/w average γ-Pyrones content of which 29.4%w/w khellin, and 9.014%w/w visnagin.The obtained extracts were analyzed by reversed phase HPLC. Keywords: Ammi visnaga fruits, γ-Pyrones (khellin and visnagin, Supercritical fluid extraction and HPLC

Ultrathin Hydrophobic Coatings Obtained on Polyethylene Terephthalate Materials in Supercritical Carbon Dioxide with Co-Solvents

Science.gov (United States)

Kumeeva, T. Yu.; Prorokova, N. P.

2018-02-01

The surface properties of ultradisperse polytetrafluoroethylene coatings on polyethylene terephthalate materials modified in a supercritical carbon dioxide medium with co-solvent additions (aliphatic alcohols) were analyzed. An atomic force microscopy study revealed the peculiarities of the morphology of the hydrophobic coatings formed in the presence of co-solvents. The contribution of the co-solvents to the formation of the surface layer with a low surface energy was evaluated from the surface energy components of the modified polyester material. The stability of the coatings against dry friction was analyzed.

A numerical study of a supercritical fluid jet

International Nuclear Information System (INIS)

Sierra-Pallares, J.; Garcia-Serna, J.; Cocero, M.J.; Parra-Santos, M.T.; Castro-Ruiz, F.

2009-01-01

This study affords the numerical solution of the mixing of a submerged turbulent jet under supercritical conditions and near-critical conditions. Turbulence plays a very important role in the behaviour of chemical engineering equipment. An accurate prediction of the turbulence at supercritical conditions with low computational cost is crucial in designing new processes such as reactions in supercritical media, high pressure separation processes, nanomaterials processing and heterogeneous catalysis. At high-pressure, the flow cannot be modelled accurately using the ideal-gas assumption. Therefore, the real gas models must be used in order to solve accurately the fluid flow and heat transfer problems where the working fluid behaviour deviate seriously from the ideal-gas assumption. The jet structure has three parts clearly distinguished: the injection, the transition and the fully developed jet. Once the flow is dominated by the turbulent eddies of the shear layer, the flow is fully developed and the radial profiles match a similarity profile. This work reports the state of the project that is not completed and is being processed now. This work is devoted to establish the distance downstream from the injector where the jet become self-preserving and the shape of the similarity profiles. This system is of interest in the design of supercritical reactor inlets, where two streams should be mixed in the shortest length, or mixing conditions strongly affect the behaviour of the processes. The numerical results have been validated with experimental measurements made in the jet mixing region. The radial profiles for average velocity, density and temperature are analyzed. The parameters of the profile that match better the numerical results are summarized in Table 1. The density requires a lower value of n than these for velocity and temperature, which reflect smoother profiles. These conclusions are in good agreement with the results from Oschwald and Schik. (author)

Extraction of functional ingredients from spinach (Spinacia oleracea L.) using liquid solvent and supercritical CO₂ extraction.

Science.gov (United States)

Jaime, Laura; Vázquez, Erika; Fornari, Tiziana; López-Hazas, María del Carmen; García-Risco, Mónica R; Santoyo, Susana; Reglero, Guillermo

2015-03-15

In this work three different techniques were applied to extract dry leaves of spinach (Spinacia oleracea): solid-liquid extraction (SLE), pressurised liquid extraction (PLE) and supercritical fluid extraction (SFE) to investigate the influence of extraction solvent and technique on extracts composition and antioxidant activity. Moreover, the influence of carotenoids and phenolic compounds on the antioxidant and anti-inflammatory activities of spinach extracts was also studied. The higher concentrations of carotenoids and the lower content of phenolic compounds were observed in the supercritical CO₂ extracts; whereas water and/or ethanol PLE extracts presented low amounts of carotenoids and the higher concentrations of phenolic compounds. PLE extract with the highest content of phenolic compounds showed the highest antioxidant activity, although SFE carotenoid rich extract also showed a high antioxidant activity. Moreover, both extracts presented an important anti-inflammatory activity. PLE seems to be a good technique for the extraction of antioxidant and anti-inflammatory compounds from spinach leaves. Moreover, spinach phenolic compounds and carotenoids present a high antioxidant activity, whereas spinach carotenoids seem to show a higher anti-inflammatory activity than phenolic compounds. It is worth noting that of our knowledge this is the first time the anti-inflammatory activity of lipophilic extracts from spinach leaves is reported. © 2014 Society of Chemical Industry.

Instrument for Solvent Extraction and Analysis (ISEE) of Organics from Regolith Simulant Using Supercritical Fluid Extraction and Chromatography

Science.gov (United States)

Franco, Carolina; Hintze, Paul E.

2017-01-01

ISEE is an instrument with the potential to perform extractions from regolith found on the surface of asteroids and planets, followed by characterization and quantitation of the extracts using supercritical fluid extraction (SFE) and chromatography (SFC). SFE is a developed technique proven to extract a wide range of organic compounds. SFC is similar to High Performance Liquid Chromatography (HPLC) but has the advantage of performing chiral separations without needing to derivatize the chiral compounds. CO2 will be the solvent for both stages as it is readily available in the Mars atmosphere. ISEE will capture CO2 from the environment, and use it for SFE and SFC. If successful, this would allow ISEE to perform analysis of organic compounds without using consumables. This paper will present results on a preliminary, proof-of-principle effort to use SFE and SFC to extract and analyze lunar regolith simulant spiked with organic compounds representing a range of organics that ISEE would expect to characterize. An optimization of variables for the extraction of the organics from the spiked regolith was successfully developed, using 138 bar pressure and 40 C temperature. The extraction flow rate was optimized at 2% SLPM with 30% methanol modifier. The extractions were successful with a value of 77.3+/- 0.9% of organics extracted. However, the recovery of organics after the extraction was very low with only 48.5+/-14.2%. Moreover, three columns were selected to analyze multiple samples at a time; two of them are Viridis HSS C18 SB and Torus DIOL, and the third column, specific for chiral separations, has not yet been selected yet.

Preparative supercritical fluid chromatography: A powerful tool for chiral separations.

Science.gov (United States)

Speybrouck, David; Lipka, Emmanuelle

2016-10-07

In 2012, the 4 biggest pharmaceutical blockbusters were pure enantiomers and separating racemic mixtures is now frequently a key step in the development of a new drug. For a long time, preparative liquid chromatography was the technique of choice for the separation of chiral compounds either during the drug discovery process to get up to a hundred grams of a pure enantiomer or during the clinical trial phases needing kilograms of material. However the advent of supercritical Fluid Chromatography (SFC) in the 1990s has changed things. Indeed, the use of carbon dioxide as the mobile phase in SFC offers many advantages including high flow rate, short equilibration time as well as low solvent consumption. Despite some initial teething troubles, SFC is becoming the primary method for preparative chiral chromatography. This article will cover recent developments in preparative SFC for the separation of enantiomers, reviewing several aspects such as instrumentation, chiral stationary phases, mobile phases or purely preparative considerations including overloading, productivity or large scale chromatography. Copyright © 2016 Elsevier B.V. All rights reserved.

Modeling heat transfer in supercritical fluid using the lattice Boltzmann method.

Science.gov (United States)

Házi, Gábor; Márkus, Attila

2008-02-01

A lattice Boltzmann model has been developed to simulate heat transfer in supercritical fluids. A supercritical viscous fluid layer between two plates heated from the bottom has been studied. It is demonstrated that the model can be used to study heat transfer near the critical point where the so-called piston effect speeds up the transfer of heat and results in homogeneous heating in the bulk of the layer. We have also studied the onset of convection in a Rayleigh-Bénard configuration. It is shown that our model can well predict qualitatively the onset of convection near the critical point, where there is a crossover between the Rayleigh and Schwarzschild criteria.

Differentiation of ring-substituted regioisomers of amphetamine and methamphetamine by supercritical fluid chromatography.

Science.gov (United States)

Segawa, Hiroki; T Iwata, Yuko; Yamamuro, Tadashi; Kuwayama, Kenji; Tsujikawa, Kenji; Kanamori, Tatsuyuki; Inoue, Hiroyuki

2017-03-01

Chromatographic differentiation of the ring-substituted regioisomers of amphetamine (AMP) and methamphetamine (MA) was performed by supercritical fluid chromatography (SFC). The behaviour of the retention against the changes of column temperature and co-solvent proportion was studied. The obtained information facilitated the optimization of the each regioisomer. As a result, 2-, 3-, and 4-ring-substituted analogues of AMP and MA with methyl, methoxy, fluoro, chloro, and bromo groups were separated, generally within 6 min. In addition, we found that the separation pattern of the examined regioisomers was classified into two, which depended on the electron donating/withdrawing effect of the substituent. Our results indicate that SFC could be used in forensic drug analysis for fast, reliable identification of structurally similar drugs of abuse. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Supercritical fluid extraction behaviour of polymer matrices

International Nuclear Information System (INIS)

Sujatha, K.; Kumar, R.; Sivaraman, N.; Srinivasan, T.G.; Vasudeva Rao, P.R.

2007-01-01

Organic compounds present in polymeric matrices such as neoprene, surgical gloves and PVC were co-extracted during the removal of uranium using supercritical fluid extraction (SFE) technique. Hence SFE studies of these matrices were carried out to establish the extracted species using HPLC, IR and mass spectrometry techniques. The initial study indicated that uranium present in the extract could be purified from the co-extracted organic species. (author)

Supercritical fluid molecular spray thin films and fine powders

Science.gov (United States)

Smith, Richard D.

1988-01-01

Solid films are deposited, or fine powders formed, by dissolving a solid material into a supercritical fluid solution at an elevated pressure and then rapidly expanding the solution through a short orifice into a region of relatively low pressure. This produces a molecular spray which is directed against a substrate to deposit a solid thin film thereon, or discharged into a collection chamber to collect a fine powder. The solvent is vaporized and pumped away. Solution pressure is varied to determine, together with flow rate, the rate of deposition and to control in part whether a film or powder is produced and the granularity of each. Solution temperature is varied in relation to formation of a two-phase system during expansion to control porosity of the film or powder. A wide variety of film textures and powder shapes are produced of both organic and inorganic compounds. Films are produced with regular textural feature dimensions of 1.0-2.0 .mu.m down to a range of 0.01 to 0.1 .mu.m. Powders are formed in very narrow size distributions, with average sizes in the range of 0.02 to 5 .mu.m.

SiC Coating Process Development Using H-PCS in Supercritical CO2

International Nuclear Information System (INIS)

Park, Kwangheon; Jung, Wonyoung

2013-01-01

We tried SiC coating using supercritical fluids. Supercritical fluids are the substance exists over critical temperature and critical pressure. It is hard to expect that there would be a big change as single-solvent as the fluid is incompressible and the space between the molecules is almost steady. But the fluid which is being supercritical can bring a great change when it is changed its pressure near its critical point, showing its successive change in the density, viscosity, diffusion coefficient and the polarity. We have tested the 'H-PCS into SiC' coating experiment with supercritical CO 2 which has the high penetration, low viscosity as well as the high density and the high solubility that shows the property of the fluid. This experiment is for SiC coating using H-PCS in supercritical CO 2 . It shows the clear difference that the penetration of H-PCS into the SiC between dip coating method and using the supercritical CO 2 If we can make a metal cladding with SiC composites as a protective layer, the use of the cladding will be very broad and diverse. Inherent safe nuclear fuels can be possible that can stand under severe accident conditions. SiC is known to be one of a few materials that maintain very corrosion-resistant properties under tough corrosive environments. The metal cladding with SiC composites as a protective layer will be a high-tech product that can be used in many applications including chemical, material, and nuclear engineering and etc

Supercritical fluid synthesis inthe preparation of β+-emitting labelled compounds

International Nuclear Information System (INIS)

Jacobson, G.; Markides, K.E.; Laangstroem, B.

1994-01-01

A system for synthesis in supercritical fluids has been developed for the microscale synthesis of pharmaceuticals labelled with 11 C. Supercritical ammonia was selected as the reaction medium and the following variables were studied in detail: trapping efficiency, cell design, substrate concentration, operation design, and temperature and pressure conditions. Alkylation of phenol by [ 11 C]methyl iodide to yield [methyl- 11 C]anisole was used as a model reaction for evaluation of the system. The results show an increased radiochemical yield in the highly compressible near-critical region. (au) (40 refs.)

Critical phenomena and their effect on thermal energy storage in supercritical fluids

International Nuclear Information System (INIS)

Hobold, Gustavo M.; Da Silva, Alexandre K.

2017-01-01

Highlights: •High power thermal energy storage using supercritical fluids. •Influence of property variation on energy and power density. •Multi-fluid analysis and generalization for several storage temperatures. •Cost, heat transfer and energy density evaluation for high temperature storage. -- Abstract: Large-scale implementation of concentrated solar power plants requires energy storage systems if fossil sources are to be fully replaced. While several candidates have appeared, most still face major issues such as cost, limited energy density and material compatibility. The present paper explores the influence of property variation in the proximity of the critical point on thermal energy storage using supercritical fluids (sTES) from thermodynamic and heat transfer standpoints. Influence of thermodynamic operational parameters on energy density of isobaric and isochoric sTES and their optima is discussed, showing that the energy density results from a competition between average specific heat and loaded density. Moreover, sTES is shown to be applicable to virtually any storage temperature, depending only on the fluid’s critical point. Finally, a heat transfer and energy density comparison to other existing storage mechanisms is presented and supercritical water is shown to be competitive for high temperature thermal energy storage.

Heat transfers and related effects in supercritical fluids

CERN Document Server

Zappoli, Bernard; Garrabos, Yves

2015-01-01

This book investigates the unique hydrodynamics and heat transfer problems that are encountered in the vicinity of the critical point of fluids. Emphasis is given on weightlessness conditions, gravity effects and thermovibrational phenomena. Near their critical point, fluids indeed obey universal behavior and become very compressible and expandable. Their comportment, when gravity effects are suppressed, becomes quite unusual. The problems that are treated in this book are of interest to students and researchers interested in the original behavior of near-critical fluids as well as to engineers that have to manage supercritical fluids. A special chapter is dedicated to the present knowledge of critical point phenomena. Specific data for many fluids are provided, ranging from cryogenics (hydrogen) to high temperature (water). Basic information in statistical mechanics, mathematics and measurement techniques is also included. The basic concepts of fluid mechanics are given for the non-specialists to be able to ...

Supercritical CO2 fluid radiochromatography system used to purify [11C]toluene for PET

International Nuclear Information System (INIS)

Muller, Ryan D.; Ferrieri, Richard A.; Gerasimov, Madina; Garza, Victor

2002-01-01

Abuse of inhalants in today's society has become such a widespread problem among today's adolescents that in many parts of the world their use exceeds that of many other illicit drugs or alcohol. Even so, little is known how such inhalants affect brain function to an extent that can lead to an abuse liability. While methodologies exist for radiolabeling certain inhalants of interest with short-lived positron emitting radioisotopes that would allow their investigation in human subjects using positron emission tomography (PET), the purification methodologies necessary to separate these volatile substances from the organic starting materials have not been developed. We've adapted supercritical fluid technology to this specific PET application by building a preparative-scale supercritical CO 2 fluid radiochromatograph, and applied it to the purification of [ 11 C]toluene. We've demonstrated that [ 11 C]toluene can be separated from the starting materials using a conventional C 18 HPLC column and pure supercritical CO 2 fluid as the mobile phase operating at 2000 psi and 40 deg. C. We've also shown that the purified radiotracer can be quantitatively captured on Tenax GR, a solid support material, as it exits the supercritical fluid stream, thus allowing for later desorption into a 1.5% cyclodextrin solution that is suitable for human injection, or into a breathing tube for direct inhalation

Hydroformylation of 1-octene in supercritical carbon dioxide and organic solvents using trifluoromethyl-substituted triphenylphosphine ligands

NARCIS (Netherlands)

Koeken, A.C.J.; Vliet, van M.C.A.; Broeke, van den L.J.P.; Deelman, B.J.; Keurentjes, J.T.F.

2006-01-01

Two different in situ prepared catalysts generated from Rh(CO)2acac and trifluoromethyl-substituted triphenylphosphine ligands have been evaluated for their activity and selectivity in the hydroformylation of 1-octene. The solvents used were supercritical carbon dioxide, hexane, toluene, and

Supercritical fluid extraction of uranium and neodymium nitrates

International Nuclear Information System (INIS)

Sujatha, K.; Sivaraman, N.; Srinivasan, T.G.; Vasudeva Rao, P.R.

2011-01-01

Supercritical fluid extraction (SFE) of uranyl nitrate and neodymium nitrate salts from a mixture was investigated in the present study using Sc-CO 2 modified with various ligands such as organophosphorous compounds, amides, and diketones. Preferential extraction of uranyl nitrate over neodymium nitrate was demonstrated using Sc-CO 2 modified with amide, di-(2ethylhexyl) isobutyramide (D2EHIBA). (author)

Supercritical fluid chromatography coupled with in-source atmospheric pressure ionization hydrogen/deuterium exchange mass spectrometry for compound speciation.

Science.gov (United States)

Cho, Yunju; Choi, Man-Ho; Kim, Byungjoo; Kim, Sunghwan

2016-04-29

An experimental setup for the speciation of compounds by hydrogen/deuterium exchange (HDX) with atmospheric pressure ionization while performing chromatographic separation is presented. The proposed experimental setup combines the high performance supercritical fluid chromatography (SFC) system that can be readily used as an inlet for mass spectrometry (MS) and atmospheric pressure photo ionization (APPI) or atmospheric pressure chemical ionization (APCI) HDX. This combination overcomes the limitation of an approach using conventional liquid chromatography (LC) by minimizing the amount of deuterium solvents used for separation. In the SFC separation, supercritical CO2 was used as a major component of the mobile phase, and methanol was used as a minor co-solvent. By using deuterated methanol (CH3OD), AP HDX was achieved during SFC separation. To prove the concept, thirty one nitrogen- and/or oxygen-containing standard compounds were analyzed by SFC-AP HDX MS. The compounds were successfully speciated from the obtained SFC-MS spectra. The exchange ions were observed with as low as 1% of CH3OD in the mobile phase, and separation could be performed within approximately 20min using approximately 0.24 mL of CH3OD. The results showed that SFC separation and APPI/APCI HDX could be successfully performed using the suggested method. Copyright © 2016 Elsevier B.V. All rights reserved.

Broken-and-Intact Cell Model for Supercritical Fluid Extraction: Its Origin and Limits.

Czech Academy of Sciences Publication Activity Database

Sovová, Helena

2017-01-01

Roč. 129, SI (2017), s. 3-8 ISSN 0896-8446. [Iberoamerican Conference on Supercritical Fluid s ProSCiba 2016 /4./. Vina del Mar, 28.03.2016-01.04.2016] Institutional support: RVO:67985858 Keywords : modelling * extraction kinetics * supercritical CO2 Subject RIV: CI - Industrial Chemistry, Chemical Engineering OBOR OECD: Chemical process engineering Impact factor: 2.991, year: 2016

Broken-and-Intact Cell Model for Supercritical Fluid Extraction: Its Origin and Limits.

Czech Academy of Sciences Publication Activity Database

Sovová, Helena

2017-01-01

Roč. 129, SI (2017), s. 3-8 ISSN 0896-8446. [Iberoamerican Conference on Supercritical Fluids ProSCiba 2016 /4./. Vina del Mar, 28.03.2016-01.04.2016] Institutional support: RVO:67985858 Keywords : modelling * extraction kinetics * supercritical CO2 Subject RIV: CI - Industrial Chemistry, Chemical Engineering OBOR OECD: Chemical process engineering Impact factor: 2.991, year: 2016

Determination of persistent organic pollutants in solid environmental samples using accelerated solvent extraction and supercritical fluid extraction. Exhaustive extraction and sorption/desorption studies of PCBs

Energy Technology Data Exchange (ETDEWEB)

Bjoerklund, E.

1998-10-01

Human activity is constantly causing environmental problems due to production and release of numerous chemicals. A group of compounds of special concern is persistent organic pollutants (POP). These toxic, lipophilic chemicals have a high chemical and biological stability, and tend to accumulate in the lipid phase of living organisms. A major sink for POPs are sediments, and consequently these are important for the distribution of POPs in the aquatic environment. Traditionally, determination of POPs relay on exhaustive extraction using liquid extraction techniques (e.g. Soxhlet extraction developed in the late 19th century) followed by gas chromatographic analysis. Since liquid-solid extraction normally requires large volumes of organic solvents in combination with long extraction times and extract clean-up, there has been an increasing demand for improved technology. This should result in reduced organic solvent consumption and sample preparation time, at the same time improving the environment and cutting costs for POP monitoring. In this thesis two modern techniques with capability of fulfilling at least one of these goals have been investigated: (1) Supercritical Fluid Extraction (SFE), and (2) Accelerated Solvent Extraction (ASE). Polychlorinated biphenyls (PCBs) were chosen as model compounds in all experiments performed on environmental matrices, since they cover a relatively large range of physiochemical parameters. Important parameters influencing the overall extraction efficiency in ASE and SFE, are discussed and illustrated for a large number of sediments. It was demonstrated that, by careful consideration of the experimental parameters, both techniques are capable of replacing old methods such as Soxhlet extraction. ASE is somewhat faster than SFE, but the extracts generated in SFE are much cleaner and can be analyzed without sample clean-up. Consequently the overall sample preparation time may be substantially lower using SFE. However, ASE is important

Thermophysical properties of supercritical fluids and fluid mixtures

International Nuclear Information System (INIS)

Sengers, J.V.

1991-07-01

This research is concerned with the development of a quantitative scientific description of the thermodynamic and transport properties of supercritical and subcritical fluids and fluid mixtures. It is known that the thermophysical properties of fluids and fluid mixtures asymptotically close to the critical point satisfy scaling laws with universal critical exponents and universal scaling functions. However, the range of validity of these asymptotic scaling laws is quite small. As a consequence, the impact of the modern theory of critical phenomena on chemical engineering has been limited. On the other hand, an a priori estimate of the range of temperatures and densities, where critical fluctuations become significant, can be made on the basis of the so-called Ginzburg criterion. A recent analysis of this criterion suggests that this range is actually quite large and for a fluid like carbon dioxide can easily extend to 100 degrees or so above the critical temperature. Hence, the use of traditional engineering equations like cubic equations is not scientifically justified in a very wide range of temperatures and densities around the critical point. We have therefore embarked on a scientific approach to deal with the global effects of critical fluctuations on the thermophysical properties of fluids and fluid mixtures. For this purpose it is not sufficient to consider the asymptotic critical fluctuations but we need to deal also with the nonasymptotic critical fluctuations. The goal is to develop scientifically based questions that account for the crossover of the thermophysical properties from their asymptotic singular behavior in the near vicinity of the critical point to their regular behavior very far away from the critical point

Optimization and characterization of condensation nucleation light scattering detection coupled with supercritical fluid chromatography

Science.gov (United States)

Yang, Shaoping

This dissertation is an investigation of two aspects of coupling condensation nucleation light scattering detection (CNLSD) with supercritical fluid chromatography (SFC). In the first part, it was demonstrated that CNLSD was compatible with packed column SFC using either pure CO2 or organic solvent modified CO2 as mobile phases. Factors which were expected to affect the interface between SFC and CNLSD were optimized for the detector to reach low detection limits. With SFC using pure CO2 as mobile phase, the detection limit of CNLSD with SFC was observed to be at low nanogram levels, which was at the same level of flame ionization detection (FID) coupled with SFC. For SFC using modified CO2 as mobile phase, detection limits at the picogram level were observed for CNLSD at optimal conditions, which were at least ten times lower than those reached by evaporative light scattering detection. In the second part, particle size distributions of aerosols produced from rapid expansion of supercritical solutions were measured with a scanning mobility particle sizer. The effect of the factors, which were investigated in the first part for their effects on signal intensities and signal to noise ratios (S/N), on particle size distributions (PSDs) of both analyte and background were investigated. Whenever possible, both particle sizes and particle number obtained from PSDs were used to explain the optimization results. In general, PSD data support the observations made in the first part. The detection limits of CNLSD obtained were much higher than predicted. PSDs did not provide direct explanation of this problem. The amount of analyte deposited in the transport tubing, evaporated to gas phase, and condensed to form particles was determined experimentally. Almost no analyte was found in the gas phase. Less than 3% was found in the particle forms. The vast majority of analyte was lost in the transport tubing, especially in the short distance after supercritical fluid expansion. A

Direct measurements of the enthalpy of solution of solid solute in supercritical fluids: study on the CO2-naphthalene system.

Science.gov (United States)

Zhang, X; Han, B; Zhang, J; Li, H; He, J; Yan, H

2001-10-01

A setup for a calorimeter for simultaneously measuring the solubility and the solution enthalpy of solid solutes in supercritical fluids (SCFs) has been established. The enthalpy of solution of naphthalene in supercritical CO2 was measured at 308.15 K in the pressure range from 8.0-11.0 MPa. It was found that the enthalpy of solution (deltaH) was negative in the pressure range from 8.0 to 9.5 MPa, and the absolute value decreased with increasing pressure. In this pressure range, the dissolution of the solute was enthalpy driven. However, the deltaH became positive at pressures higher than 9.5 MPa, and the dissolution was entropy driven. Monte Carlo simulation was performed to analyze the local structural environment of the solvated naphthalene molecules in supercritical CO2 under the experimental conditions for the calorimetric measurements. By combining the enthalpy data and the simulation results, it can be deduced that the energy level of CO2 in the high compressible region is higher than that at higher pressures, which results in the large negative enthalpy of solution and the larger degree of solvent-solute clustering in the high compressible region.

Removal of plutonium from real time waste using supercritical fluid extraction

International Nuclear Information System (INIS)

Sujatha, K.; Sivaraman, N.; Kumar, R.; Srinivasan, T.G.; Vasudeva Rao, P.R.

2010-01-01

Supercritical fluid extraction (SFE) technique was carried out for the recovery of plutonium from cellulose waste matrix using supercritical carbon dioxide (SC-CO 2 ) modified with suitable ligands such as octylphenyl N,N-diisobutyl carbamoylmethyl phosphine oxide (φCMPO), tri-n-butyl phosphate (TBP), acetyl acetone, trifluoro acetyl acetone and theonyltrifluoroacetyl acetone (TTA). The maximum plutonium recovery was found to be 99.8% when SC-CO 2 modified with CMPO was employed. About 15mg of plutonium was recovered from waste. (author)

Feasibility of ion-pair/supercritical fluid extraction of an ionic compound--pseudoephedrine hydrochloride.

Science.gov (United States)

Eckard, P R; Taylor, L T

1997-02-01

The supercritical fluid extraction (SFE) of an ionic compound, pseudoephedrine hydrochloride, from a spiked-sand surface was successfully demonstrated. The effect of carbon dioxide density (CO2), supercritical fluid composition (pure vs. methanol modified), and the addition of a commonly used reversed-phase liquid chromatographic ion-pairing reagent, 1-heptanesulfonic acid, sodium salt, on extraction efficiency was examined. The extraction recoveries of pseudoephedrine hydrochloride with the addition of the ion-pairing reagent from a spiked-sand surface were shown to be statistically greater than the extraction recoveries without the ion-pairing reagent with both pure and methanol-modified carbon dioxide.

Subchannel analysis with turbulent mixing rate of supercritical pressure fluid

International Nuclear Information System (INIS)

Wu, Jianhui; Oka, Yoshiaki

2015-01-01

Highlights: • Subchannel analysis with turbulent mixing rate law of supercritical pressure fluid (SPF) is carried out. • Turbulent mixing rate is enhanced, compared with that calculated by the law of pressurized water reactor (PWR). • Increase in maximum cladding surface temperature (MCST) is smaller comparing with PWR model. • The sensitivities of MCST on non-uniformity of subchannel area and power peaking are reduced by using SPF model. - Abstract: The subchannel analysis with turbulent mixing rate law of supercritical pressure fluid (SPF) is carried out for supercritical-pressurized light water cooled and moderated reactor (Super LWR). It is different from the turbulent mixing rate law of pressurized water reactor (PWR), which is widely adopted in Super LWR subchannel analysis study, the density difference between adjacent subchannels is taken into account for turbulent mixing rate law of SPF. MCSTs are evaluated on three kinds of fuel assemblies with different pin power distribution patterns, gap spacings and mass flow rates. Compared with that calculated by employing turbulent mixing rate law of PWR, the increase in MCST is smaller even when peaking factor is large and gap spacing is uneven. The sensitivities of MCST on non-uniformity of the subchannel area and power peaking are reduced

A flow-through column electrolytic cell for supercritical fluid chromatography.

Science.gov (United States)

Yamamoto, Kazuhiro; Ueki, Tatsuya; Higuchi, Naoyuki; Takahashi, Kouji; Kotani, Akira; Hakamata, Hideki

2017-10-01

A novel flow-through column electrolytic cell was proposed as a detector to obtain current signals for supercritical fluid chromatography. The electrochemical cell consisted of two electrodes and its holder, and a working and a counter electrode were fabricated from 192 carbon strings, which were composed of 400 carbon fibers of 10 μm in diameter filled into a heat-shrinkable tube. These electrodes were placed in the center of a holder made from polyether ether ketone blocks and they were separated by polytetrafluoroethylene membrane filters. To evaluate the sensitivity of this cell, a standard solution of ferrocene was injected into the supercritical fluid chromatography system connected to the electrolytic cell. The ferrocene was eluted through a silica gel column using a mixture of a mobile phase of supercritical CO 2 and a modifier of methanol containing ammonium acetate. The current peak area of ferrocene correlated to the ferrocene concentration in the range of 10-400 μmol/L (r = 0.999). Moreover, the limit of detection on the column estimated from a signal-to-noise ratio of 3 was 9.8  × 10 -13  mol. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Disintegration of fluids under supercritical conditions from mixing layer studies

Science.gov (United States)

Okong'o, N.; Bellan, J.

2003-01-01

Databases of transitional states obtained from Direct Numerical simulations (DNS) of temporal, supercritical mixing layers for two species systems, O2/H2 and C7H16/N2, are analyzed to elucidate species-specific turbulence aspects and features of fluid disintegration.

Supercritical fluid extraction of ginger (Zingiber Officinale Var. Amarum) : Global yield and composition study

Science.gov (United States)

Fitriady, Muhammad Arifuddin; Sulaswatty, Anny; Agustian, Egi; Salahuddin, Aditama, Deska Prayoga Fauzi

2017-11-01

An experiment to observe the effect of temperature and time process in ginger rhizome-Supercritical Fluid Extraction (SFE) using CO2 as the solvent has been conducted. The ginger rhizome (Zingiber Officinale Var. Amarum) was washed, drained, sliced, sun-dried, and then stored in a sealed bag prior to usage. The temperature and time process variables are each 35, 40, 45°C and 2, 4, 6 hours respectively with the pressure variable are 3500, 4000, and 4500 psi. It is found that the highest yield (2.9%) was achieved using temperature of 40°C and pressure of 4500 psiwith the process time of 4 hours. However, using the curve-fitting method, it is suggested to use 42°C as the temperature and 5 hours, 7 minutes, and 30 seconds (5.125 Hours) as the time process to obtain the highest yield. The temperature changes will affect both solvent and vapor pressure of diluted compounds of the ginger which will influence the global yield and the composition of the extract. The three major components of the extract are curcumene, zingiberene, and β - sesquipellandrene,

DIRECT-DEPOSITION INFRARED SPECTROMETRY WITH GAS AND SUPERCRITICAL FLUID CHROMATOGRAPHY

Science.gov (United States)

A direct-deposition Fourier transform infrared (FT-IR) system has been evaluated for applicability to gas chromatography (GC) and supercritical fluid chromatography (SFC) of environmental analytes. A 100-um i.d. fused-silica transfer line was used for GC, and a 50-um transfer lin...

Supercritical fluid chromatography of fish, shark and seal oils

DEFF Research Database (Denmark)

Borch-Jensen, Christina; Mollerup, Jørgen

1996-01-01

Various natural and treated fish, shark liver and seal oils have been analyzed by supercritical fluid chromatography (SFC) using a non-polar capillary column. The lipids are separated according to molecular mass. The lipid groups found included free fatty acids, cholesterol, squalene, vitamins, wax...... applications of SFC on fish, seal and shark liver oils are presented....

Extraction of Plutonium From Spiked INEEL Soil Samples Using the Ligand-Assisted Supercritical Fluid Extraction (LA-SFE) Technique

International Nuclear Information System (INIS)

Fox, R.V.; Mincher, B.J.; Holmes, R.G.G.

1999-01-01

In order to investigate the effectiveness of ligand-assisted supercritical fluid extraction for the removal of transuranic contaminations from soils an Idaho National Engineering and Environmental Laboratory (INEEL) silty-clay soil sample was obtained from near the Radioactive Waste Management Complex area and subjected to three different chemical preparations before being spiked with plutonium. The spiked INEEL soil samples were subjected to a sequential aqueous extraction procedure to determine radionuclide portioning in each sample. Results from those extractions demonstrate that plutonium consistently partitioned into the residual fraction across all three INEEL soil preparations whereas americium partitioned 73% into the iron/manganese fraction for soil preparation A, with the balance partitioning into the residual fraction. Plutonium and americium were extracted from the INEEL soil samples using a ligand-assisted supercritical fluid extraction technique. Initial supercritical fluid extraction runs produced plutonium extraction technique. Initial supercritical fluid extraction runs produced plutonium extraction efficiencies ranging from 14% to 19%. After a second round wherein the initial extraction parameters were changed, the plutonium extraction efficiencies increased to 60% and as high as 80% with the americium level in the post-extracted soil samples dropping near to the detection limits. The third round of experiments are currently underway. These results demonstrate that the ligand-assisted supercritical fluid extraction technique can effectively extract plutonium from the spiked INEEL soil preparations

Fast separation of triterpenoid saponins using supercritical fluid chromatography coupled with single quadrupole mass spectrometry.

Science.gov (United States)

Huang, Yang; Zhang, Tingting; Zhou, Haibo; Feng, Ying; Fan, Chunlin; Chen, Weijia; Crommen, Jacques; Jiang, Zhengjin

2016-03-20

Triterpenoid saponins (TSs) are the most important components of some traditional Chinese medicines (TCMs) and have exhibited valuable pharmacological properties. In this study, a rapid and efficient method was developed for the separation of kudinosides, stauntosides and ginsenosides using supercritical fluid chromatography coupled with single quadrupole mass spectrometry (SFC-MS). The separation conditions for the selected TSs were carefully optimized after the initial screening of eight stationary phases. The best compromise for all compounds in terms of chromatographic performance and MS sensitivity was obtained when water (5-10%) and formic acid (0.05%) were added to the supercritical carbon dioxide/MeOH mobile phase. Beside the composition of the mobile phase, the nature of the make-up solvent for interfacing SFC with MS was also evaluated. Compared to reversed phase liquid chromatography, the SFC approach showed higher resolution and shorter running time. The developed SFC-MS methods were successfully applied to the separation and identification of TSs present in Ilex latifolia Thunb., Panax quinquefolius L. and Panax ginseng C.A. Meyer. These results suggest that this SFC-MS approach could be employed as a useful tool for the quality assessment of natural products containing TSs as active components. Copyright © 2015 Elsevier B.V. All rights reserved.

Supercritical fluid technology in materials science and engineering: syntheses, properties, and applications

National Research Council Canada - National Science Library

Sun, Ya-Ping

2002-01-01

... and polymer preparations and as alternative solvent systems for materials processing. In fact, materials-related applications have emerged as a new frontier in the development of supercritical fluid technology. I hope that this book will be a timely contribution to this emerging research field by serving at least two purposes. One is to provide intere...

Flow rate control in pressure-programmed capillary supercritical fluid chromatography

NARCIS (Netherlands)

Janssen, J.G.M.; Rijks, J.A.; Cramers, C.A.M.G.

1990-01-01

A versatile and simple system is described that allows variation of the column flow rate in open-tubular capillary supercritical fluid chromatography using both on-column and postcolumn detection. The system is based on column-effluent splitting in a low-dead-volume T piece at the column exit just

Ionization mechanisms in capillary supercritical fluid chromatography-chemical ionization mass spectrometry

NARCIS (Netherlands)

Houben, R.J.; Leclercq, P.A.; Cramers, C.A.M.G.

1991-01-01

Ionization mechanisms have been studied for supercritical fluid chromatography (SFC) with mass spectrometric (MS) detection. One of the problems associated with SFC-MS is the interference of mobile phase constituents in the ionization process, which complicates the interpretation of the resulting

Extraction of Co ions from ion-exchange resin by supercritical carbon dioxide

International Nuclear Information System (INIS)

Ju, Min Su; Koh, Moon Sung; Yang, Sung Woo; Park, Kwang Heon; Kim, Hak Won; Kim, Hong Doo

2005-01-01

There are a number of liquid treatment processes for eliminating radioactive ionic contaminants in nuclear facilities. One of the most common treatment methods for aqueous streams is the use of ion exchange, which is a well-developed technique that has been employed for many years in the nuclear industry. More specifically speaking, systems that ion exchange method is applied to in nuclear power plants are liquid radioactive waste treatment system, chemical and volume control system, steam generator blowdown treatment system, and service water supply system. During the operation of nuclear power plants, radioactive contaminants such as Co-60, Mn-54, Fe-59 and Cs-137 are contained in liquid radioactive wastes. And the wastes containing small amount of uranium are generated in nuclear fuel cycle facilities. To treat the liquid radioactive waste, we usually install ion exchangers rather than evaporators due to their simplicity and effectiveness, and this trend is increasing. However, the ion exchange process produces large volume of spent organic resin, and has some problems of radiation damage and thermal instability. And the reuse of the resin is limited due to the degradation of ion-exchanging ability. For this reason, were should consider a better method to expand the lifetime of the resin or to reduce the volume of radioactive resin wastes by extracting radioactive contaminants located in the resin. Supercritical fluid CO 2 has many good points as a process solvent that include low viscosity, negligible surface tension, and variable selectivity. And supercritical fluids have physical properties of both liquid and gas such as good penetration with a high dissolution capability. Supercritical fluids have been widely used in extraction, purification, and recovery processes. A number of workers applied supercritical CO 2 solvent for cleaning of precision devices and waste treatments. Since supercritical CO 2 has its mild critical point at 31 and 73.8bar as .deg. C

High performance supercapacitor using N-doped graphene prepared via supercritical fluid processing with an oxime nitrogen source

International Nuclear Information System (INIS)

Balaji, S. Suresh; Elavarasan, A.; Sathish, M.

2016-01-01

Graphical abstract: N-doped graphene prepared via supercritical fluid processing with oxime nitrogen source (DMG) showed enhanced performance in electrochemical supercapacitor application. A maximum specific capacitance of 286 F g"−"1 at a current density of 0.5 A/g was achieved with a high specific capacity retention of 98% after 1000 cycles at 5 A/g. - Highlights: • N-functionalised graphene synthesized via supercritical fluid processing. • DMG, an oxime based nitrogen precursor. • Maximum specific capacitance of 286 F/g at 0.5 A/g in aqueous solution. • Pyridinic as well as quarternary nitrogen for enhanced capacitance. - Abstract: Heteroatom doped graphene has been proved for its promising applications in electrochemical energy storage systems. Here, nitrogen (N) doped graphene was prepared via two different techniques namely supercritical fluid assisted processing and hydrothermal heat treatment using dimethylglyoxime (DMG) as an oxime nitrogen precursor. The FT-IR and Raman spectra showed the N-containing functional group in the graphene. The XRD analysis revealed the complete reduction of graphene oxide during the supercritical fluid processing. The elemental analysis and X-ray photoelectron spectroscopy revealed the amount and nature of N-doping in the graphene, respectively. The surface morphology and physical nature of the samples were analyzed using scanning and transmission electron microscopic analysis. The electrochemical performance of prepared electrode materials was evaluated using cyclic voltammetry, galvanostatic charge-discharge analysis and electrochemical impedance spectroscopy. The N-doped graphene prepared via supercritical fluid assisted processing exhibit enhanced capacitive behaviour with a maximum specific capacitance of 286 F g"−"1 at a current density of 0.5 A/g. The cycling studies showed 98% specific capacity retention with 100% coulombic efficiency over 1000 cycles at 5 A/g. The enhanced specific capacitance of N

Supercritical fluid extraction of selected pharmaceuticals from water and serum.

Science.gov (United States)

Simmons, B R; Stewart, J T

1997-01-24

Selected drugs from benzodiazepine, anabolic agent and non-steroidal anti-inflammatory drug (NSAID) therapeutic classes were extracted from water and serum using a supercritical CO2 mobile phase. The samples were extracted at a pump pressure of 329 MPa, an extraction chamber temperature of 45 degrees C, and a restrictor temperature of 60 degrees C. The static extraction time for all samples was 2.5 min and the dynamic extraction time ranged from 5 to 20 min. The analytes were collected in appropriate solvent traps and assayed by modified literature HPLC procedures. Analyte recoveries were calculated based on peak height measurements of extracted vs. unextracted analyte. The recovery of the benzodiazepines ranged from 80 to 98% in water and from 75 to 94% in serum. Anabolic drug recoveries from water and serum ranged from 67 to 100% and 70 to 100%, respectively. The NSAIDs were recovered from water in the 76 to 97% range and in the 76 to 100% range from serum. Accuracy, precision and endogenous peak interference, if any, were determined for blank and spiked serum extractions and compared with classical sample preparation techniques of liquid-liquid and solid-phase extraction reported in the literature. For the benzodiazepines, accuracy and precision for supercritical fluid extraction (SFE) ranged from 1.95 to 3.31 and 0.57 to 1.25%, respectively (n = 3). The SFE accuracy and precision data for the anabolic agents ranged from 4.03 to 7.84 and 0.66 to 2.78%, respectively (n = 3). The accuracy and precision data reported for the SFE of the NSAIDs ranged from 2.79 to 3.79 and 0.33 to 1.27%, respectively (n = 3). The precision of the SFE method from serum was shown to be comparable to the precision obtained with other classical preparation techniques.

Inverse supercritical fluid extraction as a sample preparation method for the analysis of the nanoparticle content in sunscreen agents.

Science.gov (United States)

Müller, David; Cattaneo, Stefano; Meier, Florian; Welz, Roland; de Vries, Tjerk; Portugal-Cohen, Meital; Antonio, Diana C; Cascio, Claudia; Calzolai, Luigi; Gilliland, Douglas; de Mello, Andrew

2016-04-01

We demonstrate the use of inverse supercritical carbon dioxide (scCO2) extraction as a novel method of sample preparation for the analysis of complex nanoparticle-containing samples, in our case a model sunscreen agent with titanium dioxide nanoparticles. The sample was prepared for analysis in a simplified process using a lab scale supercritical fluid extraction system. The residual material was easily dispersed in an aqueous solution and analyzed by Asymmetrical Flow Field-Flow Fractionation (AF4) hyphenated with UV- and Multi-Angle Light Scattering detection. The obtained results allowed an unambiguous determination of the presence of nanoparticles within the sample, with almost no background from the matrix itself, and showed that the size distribution of the nanoparticles is essentially maintained. These results are especially relevant in view of recently introduced regulatory requirements concerning the labeling of nanoparticle-containing products. The novel sample preparation method is potentially applicable to commercial sunscreens or other emulsion-based cosmetic products and has important ecological advantages over currently used sample preparation techniques involving organic solvents. Copyright © 2016 Elsevier B.V. All rights reserved.

Screening of hydrocarbons as supercritical ORCs working fluids by thermal stability

International Nuclear Information System (INIS)

Dai, Xiaoye; Shi, Lin; An, Qingsong; Qian, Weizhong

2016-01-01

Highlights: • A rapid evaluation method for thermal stability of hydrocarbons for ORCs. • Methane and hydrogen are confirmed to be decomposition indicators. • The decomposition temperatures for some hydrocarbons using the rapid method. • Long carbon chain hydrocarbons are not suitable for supercritical ORCs. - Abstract: Organic Rankine Cycle (ORC) systems are widely used for industrial waste heat recovery and renewable energy utilization. The supercritical ORC is currently one of the main development directions due to its low exergy loss, high thermal efficiency and high work output. The thermal stability is the major limitation of organic working fluid selection with high temperature heat sources. This paper presents a rapid experimental method for assessing the thermal stability of hydrocarbons for ORCs. The fluids were tested in a high temperature reactor with methane and hydrogen theoretically and experimentally confirmed to be the indicators of thermal decomposition. The thermal decomposition temperatures were obtained for n-hexane, n-pentane, isopentane, cyclopentane, n-butane and isobutane using the rapid experimental method. The results show that cycloalkanes are not the good choices by thermal stability and long carbon chain hydrocarbons (longer than C6) are not suitable for supercritical ORCs due to the thermal stability limitation.

The use of solvent extractions and solubility theory to discern hydrocarbon associations in coal, with application to the coal-supercritical CO2 system

Science.gov (United States)

Kolak, Jonathan J.; Burruss, Robert A.

2014-01-01

Samples of three high volatile bituminous coals were subjected to parallel sets of extractions involving solvents dichloromethane (DCM), carbon disulfide (CS2), and supercritical carbon dioxide (CO2) (40 °C, 100 bar) to study processes affecting coal–solvent interactions. Recoveries of perdeuterated surrogate compounds, n-hexadecane-d34 and four polycyclic aromatic hydrocarbons (PAHs), added as a spike prior to extraction, provided further insight into these processes. Soxhlet-DCM and Soxhlet-CS2 extractions yielded similar amounts of extractable organic matter (EOM) and distributions of individual hydrocarbons. Supercritical CO2 extractions (40 °C, 100 bar) yielded approximately an order of magnitude less EOM. Hydrocarbon distributions in supercritical CO2 extracts generally mimicked distributions from the other solvent extracts, albeit at lower concentrations. This disparity increased with increasing molecular weight of target hydrocarbons. Five- and six-ring ring PAHs generally were not detected and no asphaltenes were recovered in supercritical CO2 extractions conducted at 40 °C and 100 bar. Supercritical CO2 extraction at elevated temperature (115 °C) enhanced recovery of four-ring and five-ring PAHs, dibenzothiophene (DBT), and perdeuterated PAH surrogate compounds. These results are only partially explained through comparison with previous measurements of hydrocarbon solubility in supercritical CO2. Similarly, an evaluation of extraction results in conjunction with solubility theory (Hildebrand and Hansen solubility parameters) does not fully account for the hydrocarbon distributions observed among the solvent extracts. Coal composition (maceral content) did not appear to affect surrogate recovery during CS2 and DCM extractions but might affect supercritical CO2 extractions, which revealed substantive uptake (partitioning) of PAH surrogates into the coal samples. This uptake was greatest in the sample (IN-1) with the highest vitrinite content. These

Supercritical fluid extraction from spent coffee grounds and coffee husks: antioxidant activity and effect of operational variables on extract composition.

Science.gov (United States)

Andrade, Kátia S; Gonçalvez, Ricardo T; Maraschin, Marcelo; Ribeiro-do-Valle, Rosa Maria; Martínez, Julian; Ferreira, Sandra R S

2012-01-15

The present study describes the chemical composition and the antioxidant activity of spent coffee grounds and coffee husks extracts, obtained by supercritical fluid extraction (SFE) with CO(2) and with CO(2) and co-solvent. In order to evaluate the high pressure method in terms of process yield, extract composition and antioxidant activity, low pressure methods, such as ultrasound (UE) and soxhlet (SOX) with different organic solvents, were also applied to obtain the extracts. The conditions for the SFE were: temperatures of 313.15K, 323.15K and 333.15K and pressures from 100 bar to 300 bar. The SFE kinetics and the mathematical modeling of the overall extraction curves (OEC) were also investigated. The extracts obtained by LPE (low pressure extraction) with ethanol showed the best results for the global extraction yield (X(0)) when compared to SFE results. The best extraction yield was 15±2% for spent coffee grounds with ethanol and 3.1±04% for coffee husks. The antioxidant potential was evaluated by DPPH method, ABTS method and Folin-Ciocalteau method. The best antioxidant activity was showed by coffee husk extracts obtained by LPE. The quantification and the identification of the extracts were accomplished using HPLC analysis. The main compounds identified were caffeine and chlorogenic acid for the supercritical extracts from coffee husks. Copyright © 2011 Elsevier B.V. All rights reserved.

Off-line supercritical fluid extraction-capillary GC applications in environmental analysis

NARCIS (Netherlands)

David, F.; Verschuere, M.; Sandra, P.J.F.

1992-01-01

The successful application of supercrit. fluid extn. for environmental samples requires that the extn. for environmental samples requires that the extn. conditions detd. for spiked samples must be optimized in order to overcome the solute-matrix interactions that are responsible for lower recoveries

Pushing the speed limit in enantioselective supercritical fluid chromatography.

Science.gov (United States)

Regalado, Erik L; Welch, Christopher J

2015-08-01

Chromatographic enantioseparations on the order of a few seconds can be achieved by supercritical fluid chromatography using short columns packed with chiral stationary phases. The evolution of 'world record' speeds for the chromatographic separation of enantiomers has steadily dropped from an industry standard of 20-40 min just two decades ago, to a current ability to perform many enantioseparations in well under a minute. Improvements in instrument and column technologies enabled this revolution, but the ability to predict optimal separation time from an initial method development screening assay using the t(min cc) predictor greatly simplifies the development and optimization of high-speed chiral chromatographic separations. In this study, we illustrate how the use of this simple tool in combination with the workhorse technique of supercritical fluid chromatography on customized short chiral columns (1-2 cm length) allows us to achieve ultrafast enantioseparations of pharmaceutically relevant compounds on the 5-20 s scale, bringing the technique of high-throughput enantiopurity analysis out of the specialist realm and into the laboratories of most researchers. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Supercritical fluid extraction of 2-alkylcyclobutanones formed from triglycerides by irradiation

International Nuclear Information System (INIS)

Horvatovich, P.; Farkas, J.; Hasselmann, C.; Marchioni, E.

1998-01-01

Complete text of publication follows. Radiation processing is employed to improve the microbiological safety of foodstuffs, and at the same time to suit the 'minimal processing' principle. However adequate information for consumers to enable their free choices requires specific detection methods of irradiation processes. For this purpose one of the most suitable methods is the detection of 2-alkylcyclobutanones which are formed - according to the present knowledge - only by irradiation from the fatty acid part of triglycerides. For detection of these compounds a European Norm (EN 1785) has been established. The method consists of Sohxlet extraction of fatty acids from the food sample, separation of 2-alkylcyclobutanones from other fatty components with liquid chromatography on Florisil TM , and the GC-MS analysis of the appropriate fraction with single ion monitoring (SIM) monitoring of 98 and 112 ions. But this method has a relatively high detection limit (∼1 kGy), it is time consuming and needs costly and sophisticated apparates. To improve the detection of 2-alkylcyclobutanones we replaced the Sohxlet extraction step with a supercritical fluid extraction. We optimised trapping and extraction parameters. It was found that supercritical fluid extraction is more selective than Sohxlet extraction used in the standard protocol. The extract obtained by supercritical fluid extraction contains less quantity and number of detection-disturbing components. This work is the first step towards decreasing the detection limit which will be the derivatization of 2-alkylcyclobutanones with halogen-containing reagent, and detection of derivatives with electron-capture detector (ECD)

TRUEX process solvent cleanup with solid sorbents

International Nuclear Information System (INIS)

Tse, Pui-Kwan; Reichley-Yinger, L.; Vandegrift, G.F.

1989-01-01

Solid sorbents, alumina, silica gel, and Amberlyst A-26 have been tested for the cleanup of degraded TRUEX-NPH solvent. A sodium carbonate scrub alone does not completely remove acidic degradation products from highly degraded solvent and cannot restore the stripping performance of the solvent. By following the carbonate scrub with either neutral alumina or Amberlyst A-26 anion exchange resin, the performance of the TRUEX-NPH is substantially restored. The degraded TRUEX-NPH was characterized before and after treatment by supercritical fluid chromatography. Its performance was evaluated by americium distribution ratios, phase-separation times, and lauric acid distribution coefficients. 17 refs., 2 figs., 5 tabs

Supercritical fluid processing: a new dry technique for photoresist developing

Science.gov (United States)

Gallagher-Wetmore, Paula M.; Wallraff, Gregory M.; Allen, Robert D.

1995-06-01

Supercritical fluid (SCF) technology is investigated as a dry technique for photoresist developing. Because of their unique combination of gaseous and liquid-like properties, these fluids offer comparative or improved efficiencies over liquid developers and, particularly carbon dioxide, would have tremendous beneficial impact on the environment and on worker safety. Additionally, SCF technology offers the potential for processing advanced resist systems which are currently under investigation as well as those that may have been abandoned due to problems associated with conventional developers. An investigation of various negative and positive photoresist systems is ongoing. Initially, supercritical carbon dioxide (SC CO2) as a developer for polysilane resists was explored because the exposure products, polysiloxanes, are generally soluble in this fluid. These initial studies demonstrated the viability of the SCF technique with both single layer and bilayer systems. Subsequently, the investigation focused on using SC CO2 to produce negative images with polymers that would typically be considered positive resists. Polymers such as styrenes and methacrylates were chemically modified by fluorination and/or copolymerization to render them soluble in SC CO2. Siloxane copolymers and siloxane-modified methacrylates were examined as well. The preliminary findings reported here indicate the feasibility of using SC CO2 for photoresist developing.

Modelling of heat transfer to fluids at a supercritical pressure

International Nuclear Information System (INIS)

Shuisheng, He

2014-01-01

A key feature of Supercritical Water-cooled Reactor (SCWR) is that, by raising the pressure of the reactor coolant fluid above the critical value, a phase change crisis is avoided. However, the changes in water density as it flows through the core of an SCWR are actually much higher than in the current water-cooled reactors. In a typical design, the ratio of the density of water at the core inlet to that at exit is as high as 7:1. Other fluid properties also vary significantly, especially around the pseudo-critical temperature (at which the specific heat capacity peaks). As a result, turbulent flow and heat transfer behaviour in the core is extremely complex and under certain conditions, significant heat transfer deterioration can potentially occur. Consequently, understanding and being able to predict flow and heat transfer phenomena under normal steady operation conditions and in start-up and hypothetical fault conditions are fundamental to the design of SCWR. There have been intensive studies on flow and heat transfer to fluids at supercritical pressure recently and several excellent review papers have been published. In the talk, we will focus on some turbulence modelling issues encountered in CFD simulations. The talk will first discuss some flow and heat transfer issues related to fluids at supercritical pressures and their potential implications in SCWR, and some recent developments in the understanding and modelling techniques of such problems, which will be followed by an outlook for some future developments.Factors which have a major influence on the flow and will be discussed are buoyancy and flow acceleration due to thermal expansion (both are due to density variations but involve different mechanisms) and the nonuniformity of other fluid properties. In addition, laminar-turbulent flow transition coupled with buoyancy and flow acceleration plays an important role in heat transfer effectiveness and wall temperature in the entrance region but such

Analysis of new psychoactive substances in human urine by ultra-high performance supercritical fluid and liquid chromatography: Validation and comparison.

Science.gov (United States)

Borovcová, Lucie; Pauk, Volodymyr; Lemr, Karel

2018-05-01

New psychoactive substances represent serious social and health problem as tens of new compounds are detected in Europe annually. They often show structural proximity or even isomerism, which complicates their analysis. Two methods based on ultra high performance supercritical fluid chromatography and ultra high performance liquid chromatography with mass spectrometric detection were validated and compared. A simple dilute-filter-and-shoot protocol utilizing propan-2-ol or methanol for supercritical fluid or liquid chromatography, respectively, was proposed to detect and quantify 15 cathinones and phenethylamines in human urine. Both methods offered fast separation (chromatography. Limits of detection in urine ranged from 0.01 to 2.3 ng/mL, except for cathinone (5 ng/mL) in supercritical fluid chromatography. Nevertheless, this technique distinguished all analytes including four pairs of isomers, while liquid chromatography was unable to resolve fluoromethcathinone regioisomers. Concerning matrix effects and recoveries, supercritical fluid chromatography produced more uniform results for different compounds and at different concentration levels. This work demonstrates the performance and reliability of supercritical fluid chromatography and corroborates its applicability as an alternative tool for analysis of new psychoactive substances in biological matrixes. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Review on plasmas in extraordinary media: plasmas in cryogenic conditions and plasmas in supercritical fluids

Science.gov (United States)

Stauss, Sven; Muneoka, Hitoshi; Terashima, Kazuo

2018-02-01

Plasma science and technology has enabled advances in very diverse fields: micro- and nanotechnology, chemical synthesis, materials fabrication and, more recently, biotechnology and medicine. While many of the currently employed plasma tools and technologies are very advanced, the types of plasmas used in micro- and nanofabrication pose certain limits, for example, in treating heat-sensitive materials in plasma biotechnology and plasma medicine. Moreover, many physical properties of plasmas encountered in nature, and especially outer space, i.e. very-low-temperature plasmas or plasmas that occur in high-density media, are not very well understood. The present review gives a short account of laboratory plasmas generated under ’extreme’ conditions: at cryogenic temperatures and in supercritical fluids. The fundamental characteristics of these cryogenic plasmas and cryoplasmas, and plasmas in supercritical fluids, especially supercritical fluid plasmas, are presented with their main applications. The research on such exotic plasmas is expected to lead to further understanding of plasma physics and, at the same time, enable new applications in various technological fields.

Understanding the structural differences between spherical and rod-shaped human insulin nanoparticles produced by supercritical fluids precipitation.

Science.gov (United States)

Park, Yeonju; Seo, Yongil; Chae, Boknam; Pyo, Dongjin; Chung, Hoeil; Hwang, Hyonseok; Jung, Young Mee

2015-02-02

In this study, the thermal denaturation mechanism and secondary structures of two types of human insulin nanoparticles produced by a process of solution-enhanced dispersion by supercritical fluids using dimethyl sulfoxide (DMSO) and ethanol (EtOH) solutions of insulin are investigated using spectroscopic approaches and molecular dynamics calculations. First, the temperature-dependent IR spectra of spherical and rod-shaped insulin nanoparticles prepared from DMSO and EtOH solution, respectively, are analyzed using principal component analysis (PCA) and 2D correlation spectroscopy to obtain a deeper understanding of the molecular structures and thermal behavior of the two insulin particle shapes. All-atom molecular dynamics (AAMD) calculations are performed to investigate the influence of the solvent molecules on the production of the insulin nanoparticles and to elucidate the geometric differences between the two types of nanoparticles. The results of the PCA, the 2D correlation spectroscopic analysis, and the AAMD calculations clearly reveal that the thermal denaturation mechanisms and the degrees of hydrogen bonding in the spherical and rod-shaped insulin nanoparticles are different. The polarity of the solvent might not alter the structure or function of the insulin produced, but the solvent polarity does influence the synthesis of different shapes of insulin nanoparticles. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Modeling the Supercritical Fluid Extraction of Essential Oils from Plant Materials

Czech Academy of Sciences Publication Activity Database

Sovová, Helena

2012-01-01

Roč. 1250, SI (2012), s. 27-33 ISSN 0021-9673 R&D Projects: GA TA ČR TA01010578 Institutional support: RVO:67985858 Keywords : supercritical fluid extraction * essential oils * model for kinetics Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 4.612, year: 2012

Structural Characterisation of Acetogenins from Annona muricata by Supercritical Fluid Chromatography Coupled to High-Resolution Tandem Mass Spectrometry.

Science.gov (United States)

Laboureur, Laurent; Bonneau, Natacha; Champy, Pierre; Brunelle, Alain; Touboul, David

2017-11-01

Acetogenins are plant polyketides known to be cytotoxic and proposed as antitumor candidates. They are also suspected to be alimentary neurotoxins. Their occurrence as complex mixtures renders their dereplication and structural identification difficult using liquid chromatography coupled to tandem mass spectrometry and efforts are required to improve the methodology. To develop a supercritical fluid chromatography (SFC) high-resolution tandem mass spectrometry method, involving lithium post-column cationisation, for the structural characterisation of Annonaceous acetogenins in crude extracts. The seeds of Annona muricata L. were extracted with methanol. Supercritical fluid chromatography of the extract, using a 2-ethylpyridine stationary phase column, was monitored using a high-resolution quadrupole time-of-flight mass spectrometer. Lithium iodide was added post-column in the make-up solvent. For comparison, the same extract was analysed using high-pressure liquid chromatography coupled to the same mass spectrometer, with a column based on solid core particles. Sensitivity was similar for both HPLC and SFC approaches. Retention behaviour and fragmentation pathways of three different isomer groups are described. A previously unknown group of acetogenins was also evidenced for the first time. The use of SFC-MS/MS allows the reduction of the time of analysis, of environmental impact and an increase in the chromatographic resolution, compared to liquid chromatography. This new methodology enlightened a new group of acetogenins, isomers of montanacin-D. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Effects of modifiers in packed and open-tubular supercritical fluid chromatography

NARCIS (Netherlands)

Janssen, J.G.M.; Schoenmakers, P.J.; Cramers, C.A.M.G.

1991-01-01

The applicability of packed and open columns for supercritical fluid chromatography using pure carbon dioxide for the elution of a number of selected test components was investigated. It is showns that the number of solutes that can be eluted as symmetrical peaks is much larger in open-tubular

Supercritical CO{sub 2} fluid radiochromatography system used to purify [{sup 11}C]toluene for PET

Energy Technology Data Exchange (ETDEWEB)

Muller, Ryan D.; Ferrieri, Richard A. E-mail: rferrieri@bnl.gov; Gerasimov, Madina; Garza, Victor

2002-04-01

Abuse of inhalants in today's society has become such a widespread problem among today's adolescents that in many parts of the world their use exceeds that of many other illicit drugs or alcohol. Even so, little is known how such inhalants affect brain function to an extent that can lead to an abuse liability. While methodologies exist for radiolabeling certain inhalants of interest with short-lived positron emitting radioisotopes that would allow their investigation in human subjects using positron emission tomography (PET), the purification methodologies necessary to separate these volatile substances from the organic starting materials have not been developed. We've adapted supercritical fluid technology to this specific PET application by building a preparative-scale supercritical CO{sub 2} fluid radiochromatograph, and applied it to the purification of [{sup 11}C]toluene. We've demonstrated that [{sup 11}C]toluene can be separated from the starting materials using a conventional C{sub 18} HPLC column and pure supercritical CO{sub 2} fluid as the mobile phase operating at 2000 psi and 40 deg. C. We've also shown that the purified radiotracer can be quantitatively captured on Tenax GR, a solid support material, as it exits the supercritical fluid stream, thus allowing for later desorption into a 1.5% cyclodextrin solution that is suitable for human injection, or into a breathing tube for direct inhalation.

A comparative study of conventional and supercritical fluid extraction methods for the recovery of secondary metabolites from Syzygium campanulatum Korth#

Science.gov (United States)

Memon, Abdul Hakeem; Hamil, Mohammad Shahrul Ridzuan; Laghari, Madeeha; Rithwan, Fahim; Zhari, Salman; Saeed, Mohammed Ali Ahmed; Ismail, Zhari; Majid, Amin Malik Shah Abdul

2016-01-01

Syzygium campanulatum Korth is a plant, which is a rich source of secondary metabolites (especially flavanones, chalcone, and triterpenoids). In our present study, three conventional solvent extraction (CSE) techniques and supercritical fluid extraction (SFE) techniques were performed to achieve a maximum recovery of two flavanones, chalcone, and two triterpenoids from S. campanulatum leaves. Furthermore, a Box-Behnken design was constructed for the SFE technique using pressure, temperature, and particle size as independent variables, and yields of crude extract, individual and total secondary metabolites as the dependent variables. In the CSE procedure, twenty extracts were produced using ten different solvents and three techniques (maceration, soxhletion, and reflux). An enriched extract of five secondary metabolites was collected using n-hexane:methanol (1:1) soxhletion. Using food-grade ethanol as a modifier, the SFE methods produced a higher recovery (25.5%‒84.9%) of selected secondary metabolites as compared to the CSE techniques (0.92%‒66.00%). PMID:27604860

A comparative study of conventional and supercritical fluid extraction methods for the recovery of secondary metabolites from Syzygium campanulatum Korth.

Science.gov (United States)

Memon, Abdul Hakeem; Hamil, Mohammad Shahrul Ridzuan; Laghari, Madeeha; Rithwan, Fahim; Zhari, Salman; Saeed, Mohammed Ali Ahmed; Ismail, Zhari; Majid, Amin Malik Shah Abdul

2016-09-01

Syzygium campanulatum Korth is a plant, which is a rich source of secondary metabolites (especially flavanones, chalcone, and triterpenoids). In our present study, three conventional solvent extraction (CSE) techniques and supercritical fluid extraction (SFE) techniques were performed to achieve a maximum recovery of two flavanones, chalcone, and two triterpenoids from S. campanulatum leaves. Furthermore, a Box-Behnken design was constructed for the SFE technique using pressure, temperature, and particle size as independent variables, and yields of crude extract, individual and total secondary metabolites as the dependent variables. In the CSE procedure, twenty extracts were produced using ten different solvents and three techniques (maceration, soxhletion, and reflux). An enriched extract of five secondary metabolites was collected using n-hexane:methanol (1:1) soxhletion. Using food-grade ethanol as a modifier, the SFE methods produced a higher recovery (25.5%‒84.9%) of selected secondary metabolites as compared to the CSE techniques (0.92%‒66.00%).

Supercritical Fluid Extraction of Minor Components of Vegetable Oils: beta-Sitosterol

Czech Academy of Sciences Publication Activity Database

Sovová, Helena; Galushko, A.A.; Stateva, R.P.; Rochová, Kristina; Sajfrtová, Marie; Bártlová, Milena

2010-01-01

Roč. 101, č. 2 (2010), s. 201-209 ISSN 0260-8774 R&D Projects: GA MŠk 2B06024 Institutional research plan: CEZ:AV0Z40720504 Keywords : supercritical fluid extraction * sea buckthorn oil * beta-sitosterol Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 2.168, year: 2010

Performance optimization of low-temperature power generation by supercritical ORCs (organic Rankine cycles) using low GWP (global warming potential) working fluids

International Nuclear Information System (INIS)

Le, Van Long; Feidt, Michel; Kheiri, Abdelhamid; Pelloux-Prayer, Sandrine

2014-01-01

This paper presents the system efficiency optimization scenarios of basic and regenerative supercritical ORCs (organic Rankine cycles) using low-GWP (global warming potential) organic compounds as working fluid. A more common refrigerant, i.e. R134a, was also employed to make the comparison. A 150-°C, 5-bar-pressurized hot water is used to simulate the heat source medium. Power optimization was equally performed for the basic configuration of supercritical ORC. Thermodynamic performance comparison of supercritical ORCs using different working fluids was achieved by ranking method and exergy analysis method. The highest optimal efficiency of the system (η sys ) is always obtained with R152a in both basic (11.6%) and regenerative (13.1%) configurations. The highest value of optimum electrical power output (4.1 kW) is found with R1234ze. By using ranking method and considering low-GWP criterion, the best working fluids for system efficiency optimization of basic and regenerative cycles are R32 and R152a, respectively. The best working fluid for net electrical power optimization of basic cycle is R1234ze. Although CO 2 has many desirable environmental and safety properties (e.g. zero ODP (Ozone Depletion Potential), ultra low-GWP, non toxicity, non flammability, etc.), the worst thermodynamic performance is always found with the cycle using this compound as working fluid. - Highlights: • Performance optimizations were carried out for the supercritical ORCs using low-GWP working fluids. • Heat regeneration was used to improve the system efficiency of the supercritical ORC. • Thermodynamic performances of supercritical ORCs at the optima were evaluated by ranking method and exergy analysis

Effect temperature of supercritical CO2 fluid extraction on phytochemical analysis and antioxidant activity of Zingiber officinale Roscoe

Science.gov (United States)

Sondari, Dewi; Irawadi, Tun Tedja; Setyaningsih, Dwi; Tursiloadi, Silvester

2017-11-01

Supercritical fluid extraction of Zingiber officinale Roscoe has been carried out at a pressure of 16 MPa, with temperatures between 20-40 °C, during extraction time of 6 hours and the flow rate of CO2 fluid 5.5 ml/min. The result of supercritical method was compared with the extraction maceration using a mixture of water and ethanol (70% v/v) for 24 hours. The main content in ginger that has a main role as an antioxidant is a gingerol compound that can help neutralize the damaging effects caused by free radicals in the body, as anti-coagulant, and inhibit the occurrence of blood clots. This study aims to determine the effect of temperature on chemical components contained in rough extract of Zingiber officinale Roscoe and its antioxidant activity, total phenol and total flavonoid content. To determine the chemical components contained in the crude extract of Zingiber officinale Roscoe extracted by supercritical fluid and maceration extraction, GC-MS analysis was performed. Meanwhile, the antioxidant activity of the extract was evaluated based on a 2.2-diphenyl-1-picrylhydrazyl (DPPH) free radical damping method. The results of the analysis show that the result of ginger extract by using the supercritical CO2 extraction method has high antioxidant activity than by using maceration method. The highest total phenol content and total flavonoids were obtained on ginger extraction using supercritical CO2 fluid extraction, indicating that phenol and flavonoid compounds contribute to antioxidant activity. Chromatographic analysis showed that the chemical profile of ginger extract containing oxygenated monoterpenes, monoterpene hydrocarbons, sesquiterpene hydrocarbons, oxygenated monoterpene gingerol and esters. In supercritical fluid extraction, the compounds that can be identified at a temperature of 20-40 °C contain 27 compounds, and 11 compounds from the result of maceration extract. The main component of Zingiber officinale Roscoe extracted using supercritical fluid

Literature survey of heat transfer and hydraulic resistance of water, carbon dioxide, helium and other fluids at supercritical and near-critical pressures

Energy Technology Data Exchange (ETDEWEB)

Pioro, I.L.; Duffey, R.B

2003-04-01

This survey consists of 430 references, including 269 Russian publications and 161 Western publications devoted to the problems of heat transfer and hydraulic resistance of a fluid at near-critical and supercritical pressures. The objective of the literature survey is to compile and summarize findings in the area of heat transfer and hydraulic resistance at supercritical pressures for various fluids for the last fifty years published in the open Russian and Western literature. The analysis of the publications showed that the majority of the papers were devoted to the heat transfer of fluids at near-critical and supercritical pressures flowing inside a circular tube. Three major working fluids are involved: water, carbon dioxide, and helium. The main objective of these studies was the development and design of supercritical steam generators for power stations (utilizing water as a working fluid) in the 1950s, 1960s, and 1970s. Carbon dioxide was usually used as the modeling fluid due to lower values of the critical parameters. Helium, and sometimes carbon dioxide, were considered as possible working fluids in some special designs of nuclear reactors. (author)

Modifier free supercritical fluid extraction of uranium from sintered UO2, soil and ore samples

International Nuclear Information System (INIS)

Kanekar, A.S.; Pathak, P.N.; Acharya, R.; Mohapatra, P.K.; Manchanda, V.K.

2011-01-01

Direct extraction of uranium from different samples viz. sintered UO 2 , soil and ores was carried out by modifier free supercritical fluid using tri-n-butyl phosphate-nitric acid (TBP-HNO 3 ) adduct as extractant. These studies showed that pre-equilibration with more concentrated nitric acid helps in better dissolution and extraction of uranium from sintered UO 2 samples. Modifier free supercritical fluid extraction appears attractive with respect to minimization of secondary wastes. This method resulted 80-100% extraction of uranium from different soil/ore samples. The results were confirmed by performing neutron activation analysis of original (before extraction) and residue (after extraction) samples. (author)

Steps of Supercritical Fluid Extraction of Natural Products and Their Characteristic Times

Czech Academy of Sciences Publication Activity Database

Sovová, Helena

2012-01-01

Roč. 66, SI (2012), s. 73-79 ISSN 0896-8446 R&D Projects: GA MŠk 2B06049 Institutional support: RVO:67985858 Keywords : supercritical fluid extraction * vegetable oils * essential oils Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 2.732, year: 2012

Extraction of garlic with supercritical CO2 and conventional organic solvents

Directory of Open Access Journals (Sweden)

J. M. del Valle

2008-09-01

Full Text Available Garlic (Allium sativum L. and garlic extracts have therapeutical properties that stem from their sulfur-containing compounds, mainly allicin. The main objective of this work was to compare conventional and "premium" garlic extracts in terms of yield and quality, with the latter being obtained using supercritical carbon dioxide (SC-CO2 as the solvent. Yield ranged between 0.65 and 1.0% and increased with extraction pressure (150-400 bar at a constant temperature of 50°C. Extraction temperature (35-60°C, on the other hand, had little effect at a constant pressure of 300 bar. Based on yield and quality considerations, the best extraction conditions using SC-CO2 were 35-50°C and 300-400 bar. A yield of 5.5% was obtained by conventional extraction using ethanol as the solvent, but ethanol appeared to be less selective for valuable components than SC-CO2. The use of fresh garlic resulted in extracts that more closely resembled commercial products, possibly because of thermal and oxidative degradation of valuable microconstituents during drying.

Ionic Liquid and Supercritical Fluid Hyphenated Techniques for Dissolution and Separation of Lanthanides, Actinides, and Fission Products

International Nuclear Information System (INIS)

Wai, Chien M.; Mincher, Bruce

2012-01-01

This project is investigating techniques involving ionic liquids (IL) and supercritical (SC) fluids for dissolution and separation of lanthanides, actinides, and fission products. The research project consists of the following tasks: Study direct dissolution of lanthanide oxides, uranium dioxide and other actinide oxides in [bmin][Tf 2 N] with TBP(HNO 3 ) 1.8 (H 2 O) 0.6 and similar types of Lewis acid-Lewis base complexing agents; Measure distributions of dissolved metal species between the IL and the sc-CO 2 phases under various temperature and pressure conditions; Investigate the chemistry of the dissolved metal species in both IL and sc-CO 2 phases using spectroscopic and chemical methods; Evaluate potential applications of the new extraction techniques for nuclear waste management and for other projects. Supercritical carbon dioxide (sc-CO 2 ) and ionic liquids are considered green solvents for chemical reactions and separations. Above the critical point, CO 2 has both gas- and liquid-like properties, making it capable of penetrating small pores of solids and dissolving organic compounds in the solid matrix. One application of sc-CO 2 extraction technology is nuclear waste management. Ionic liquids are low-melting salts composed of an organic cation and an anion of various forms, with unique properties making them attractive replacements for the volatile organic solvents traditionally used in liquid-liquid extraction processes. One type of room temperature ionic liquid (RTIL) based on the 1-alkyl-3-methylimidazolium cation [bmin] with bis(trifluoromethylsulfonyl)imide anion [Tf 2 N] is of particular interest for extraction of metal ions due to its water stability, relative low viscosity, high conductivity, and good electrochemical and thermal stability. Recent studies indicate that a coupled IL sc-CO 2 extraction system can effectively transfer trivalent lanthanide and uranyl ions from nitric acid solutions. Advantages of this technique include operation at

Supercritical fluid extraction of peach (Prunus persica) almond oil: process yield and extract composition.

Science.gov (United States)

Mezzomo, Natália; Mileo, Bruna R; Friedrich, Maria T; Martínez, Julian; Ferreira, Sandra R S

2010-07-01

Peach kernels are industrial residues from the peach processing, contain oil with important therapeutic properties and attractive nutritional aspects because of the high concentration of oleic and linoleic acids. The extraction method used to obtain natural compounds from raw matter is critical for product quality definition. Thus, the aim of this work was to compare peach almond extraction yields obtained by different procedures: soxhlet extractions (Sox) with different solvents; hydrodistillation (HD); ethanolic maceration (Mac) followed by fractionation with various solvents, and supercritical fluid extraction (SFE) at 30, 40 and 50 degrees C and at 100, 200 and 300bar, performed with pure CO(2) and with a co-solvent. The extracts were evaluated with respect to fatty acid composition (FAC), fractionated chemical profile (FCP) and total phenolic content (TPC). The Sox total yields were generally higher than those obtained by SFE. The crossover pressure for SFE was between 260 and 280bar. The FAC results show oleic and linoleic acids as main components, especially for Sox and SFE extracts. The FCP for samples obtained by Sox and Mac indicated the presence of benzaldehyde and benzyl alcohol, components responsible for almond flavor and with important industrial uses, whereas the SFE extracts present a high content of a possible flavonoid. The higher TPC values were obtained by Sox and Mac with ethanol. In general, the maximum pressure in SFE produced the highest yield, TPC and oleic acid content. The use of ethanol at 5% as co-solvent in SFE did not result in a significant effect on any evaluated parameter. The production of peach almond oil through all techniques is substantially adequate and SFE presented advantages, with respect to the quality of the extracts due to the high oleic acid content, as presented by some Sox samples. Copyright (c) 2010 Elsevier Ltd. All rights reserved.

Batch production of micron size particles from poly(ethylene glycol) using supercritical CO2 as a processing solvent

NARCIS (Netherlands)

Nalawade, Sameer P.; Picchioni, Francesco; Janssen, L. P. B. M.

The major advantage of using supercritical carbon dioxide (CO2) as a solvent in polymer processing is an enhancement in the free volume of a polymer due to dissolved CO2, which causes a considerable reduction in the viscosity. This allows spraying the polymer melt at low temperatures to produce

Supercritical Fluid Extraction of Eucalyptus globulus Bark—A Promising Approach for Triterpenoid Production

Directory of Open Access Journals (Sweden)

Carlos M. Silva

2012-06-01

Full Text Available Eucalyptus bark contains significant amounts of triterpenoids with demonstrated bioactivity, namely triterpenic acids and their acetyl derivatives (ursolic, betulinic, oleanolic, betulonic, 3-acetylursolic, and 3-acetyloleanolic acids. In this work, the supercritical fluid extraction (SFE of Eucalyptus globulus deciduous bark was carried out with pure and modified carbon dioxide to recover this fraction, and the results were compared with those obtained by Soxhlet extraction with dichloromethane. The effects of pressure (100–200 bar, co-solvent (ethanol content (0, 5 and 8% wt, and multistep operation were studied in order to evaluate the applicability of SFE for their selective and efficient production. The individual extraction curves of the main families of compounds were measured, and the extracts analyzed by GC-MS. Results pointed out the influence of pressure and the important role played by the co-solvent. Ethanol can be used with advantage, since its effect is more important than increasing pressure by several tens of bar. At 160 bar and 40 °C, the introduction of 8% (wt of ethanol greatly improves the yield of triterpenoids more than threefold.

Effect of additives on eremomycin sorbent selectivity in separation of salbutamol enantiomers using supercritical fluid chromatography

Science.gov (United States)

Pokrovskiy, O. I.; Kayda, A. S.; Usovich, O. I.; Parenago, O. O.; Lunin, V. V.

2017-11-01

A regime is found in which chiral stationary phase based on macrocyclic glycopeptide eremomycin allows separation of salbutamol sulfate enantiomers in supercritical fluid chromatography. Enantioseparation occurs only when two dynamic modifiers are used simultaneously: isopropylamin + trifluoroacetic acid or isopropylamin + ammonium acetate. Amine molar concentration in mobile phase has to be higher than acid molar concentration, otherwise enantiomers coelute. We suppose that with amine excess a mechanism of enantiorecognition is realized which involves ionic sorbent-sorbate interactions. Such mechanism is well-known for glycopeptide chiral selectors in liquid chromatography, but for supercritical fluid chromatography it is reported for the first time.

Selective extraction of hydrocarbons, phosphonates and phosphonic acids from soils by successive supercritical fluid and pressurized liquid extractions.

Science.gov (United States)

Chaudot, X; Tambuté, A; Caude, M

2000-01-14

Hydrocarbons, dialkyl alkylphosphonates and alkyl alkylphosphonic acids are selectively extracted from spiked soils by successive implementation of supercritical carbon dioxide, supercritical methanol-modified carbon dioxide and pressurized water. More than 95% of hydrocarbons are extracted during the first step (pure supercritical carbon dioxide extraction) whereas no organophosphorus compound is evidenced in this first extract. A quantitative extraction of phosphonates is achieved during the second step (methanol-modified supercritical carbon dioxide extraction). Polar phosphonic acids are extracted during a third step (pressurized water extraction) and analyzed by gas chromatography under methylated derivatives (diazomethane derivatization). Global recoveries for these compounds are close to 80%, a loss of about 20% occurring during the derivatization process (co-evaporation with solvent). The developed selective extraction method was successfully applied to a soil sample during an international collaborative exercise.

Compressibility effects in packed and open tubular gas and supercritical fluid chromatography

NARCIS (Netherlands)

Janssen, J.G.M.; Snijders, H.M.J.; Cramers, C.A.; Schoenmakers, P.J.

1992-01-01

The influence of the pressure drop on the efficiency and speed of anal. in packed and open tubular supercrit. fluid chromatog. (SFC) is described: methods previously developed to describe the effects of mobile phase compressibility on the performance of open tubular columns in SFC have been extended

Decontamination of uranium-contaminated waste oil using supercritical fluid and nitric acid

International Nuclear Information System (INIS)

Sung, J.; Kim, J.; Lee, Y.; Seol, J.; Ryu, J.; Park, K.

2011-01-01

The waste oil used in nuclear fuel processing is contaminated with uranium because of its contact with materials or environments containing uranium. Under current law, waste oil that has been contaminated with uranium is very difficult to dispose of at a radioactive waste disposal site. To dispose of the uranium-contaminated waste oil, the uranium was separated from the contaminated waste oil. Supercritical R-22 is an excellent solvent for extracting clean oil from uranium-contaminated waste oil. The critical temperature of R-22 is 96.15 deg. C and the critical pressure is 49.9 bar. In this study, a process to remove uranium from the uranium-contaminated waste oil using supercritical R-22 was developed. The waste oil has a small amount of additives containing N, S or P, such as amines, dithiocarbamates and dialkyldithiophosphates. It seems that these organic additives form uranium-combined compounds. For this reason, dissolution of uranium from the uranium-combined compounds using nitric acid was needed. The efficiency of the removal of uranium from the uranium-contaminated waste oil using supercritical R-22 extraction and nitric acid treatment was determined. (authors)

Fiscal 1995 research investigation on chemical process technology using supercritical fluid; 1995 nendo chorinkai ryutai wo riyoshita kagaku process gijutsu ni kansuru chosa kenkyu

Energy Technology Data Exchange (ETDEWEB)

NONE

1996-03-01

With relation to the supercritical fluid utilization technology, conducted in fiscal 1995 were collection of basic data, extraction of R and D subjects and survey/analysis of application fields based on the literature survey and overseas field survey. From the research results, the following were selected as research subjects: as to the clean/recycling process technology, non-selection cascade treatment process of mixed waste plastics, hazardous waste treatment process, and radioactive waste treatment process. As to the unused resource utilization process technology, the supercritical submerged combustion power generation process, heavy hydrocarbon resource reutilization process, biomass synthetic utilization process, and carbon dioxide reutilization process. As to the next generation reaction process technology, the simple reaction process, de-organic solvent process, chemical materialization process for methane, and reaction separation combined process. As the innovative material process technology, the plastic forming process, high-functional materials, high-efficiency energy conversion materials, and heightening of function of solid wastes. 537 refs., 116 figs., 54 tabs.

Small scale separation of isoxazole structurally related analogues by chiral supercritical fluid chromatography.

Science.gov (United States)

Zehani, Yasmine; Lemaire, Lucas; Millet, Regis; Lipka, Emmanuelle

2017-07-07

Chromatographic preparative enantioseparation is now the preferred method to obtain milligram amounts of pure enantiomers in the first step of the development of a therapeutic molecule. Supercritical fluid chromatography has many advantages over liquid chromatography and was therefore chosen for the small scale enantioseparation of four original 3-carboxamido-5-aryl isoxazole molecules, ligands of the CB2 cannabinoid receptors. The preparation of about 10mg of each of the eight enantiomers was achieved successfully on a Chiralpak ® AD-H (tris-3,5-dimethylphenylcarbamate of amylose) polysaccharide based stationary phase with various percentages of ethanol as a co-solvent, through mixed-stream injections and touching-band approach. For the all compounds, no peak distortion is observed during the volume overloading, in spite of the injection mode. Production rate (mgmin -1 ), productivity (kilogram of racemate separated per kilogram of CSP per day (kkd)) and solvent usage were found higher and environmental factors (E Factor) were found lower for compounds 1 and 3. The yields of each purified enantiomer were comprised between 60 and 94%. In order to improve the limit of detection calculated with the diode array detector, the hyphenation with an evaporating light scattering detector was explored and a factor of ten was won. Lastely, the enantiomeric excess and achiral purity of each of the eight individual enantiomer generated was determined and found higher than 98%. Copyright © 2017 Elsevier B.V. All rights reserved.

Pressure drop effects on selectivity and resolution in packed-column supercritical fluid chromatography

NARCIS (Netherlands)

Lou, X.W.; Janssen, J.G.M.; Snijders, H.M.J.; Cramers, C.A.M.G.

1996-01-01

The influence of pressure drop on retention, selectivity, plate height and resolution was investigated systematically in packed supercritical fluid chromatography (SFC) using pure carbon dioxide as the mobile phase. Numerical methods developed previously which enabled the prediction of pressure

Enhancing power cycle efficiency for a supercritical Brayton cycle power system using tunable supercritical gas mixtures

Science.gov (United States)

Wright, Steven A.; Pickard, Paul S.; Vernon, Milton E.; Radel, Ross F.

2017-08-29

Various technologies pertaining to tuning composition of a fluid mixture in a supercritical Brayton cycle power generation system are described herein. Compounds, such as Alkanes, are selectively added or removed from an operating fluid of the supercritical Brayton cycle power generation system to cause the critical temperature of the fluid to move up or down, depending upon environmental conditions. As efficiency of the supercritical Brayton cycle power generation system is substantially optimized when heat is rejected near the critical temperature of the fluid, dynamically modifying the critical temperature of the fluid based upon sensed environmental conditions improves efficiency of such a system.

Control of optical transport parameters of 'porous medium – supercritical fluid' systems

Energy Technology Data Exchange (ETDEWEB)

Zimnyakov, D A; Ushakova, O V; Yuvchenko, S A [Yuri Gagarin State Technical University of Saratov, Saratov (Russian Federation); Bagratashvili, V N [M. V. Lomonosov Moscow State University, Moscow (Russian Federation)

2015-11-30

The possibility of controlling optical transport parameters (in particular, transport scattering coefficient) of porous systems based on polymer fibres, saturated with carbon dioxide in different phase states (gaseous, liquid and supercritical) has been experimentally studied. An increase in the pressure of the saturating medium leads to a rise of its refractive index and, correspondingly, the diffuse-transmission coefficient of the system due to the decrease in the transport scattering coefficient. It is shown that, in the case of subcritical saturating carbon dioxide, the small-angle diffuse transmission of probed porous layers at pressures close to the saturated vapour pressure is determined by the effect of capillary condensation in pores. The immersion effect in 'porous medium – supercritical fluid' systems, where the fluid pressure is used as a control parameter, is considered. The results of reconstructing the values of transport scattering coefficient of probed layers for different refractive indices of a saturating fluid are presented. (radiation scattering)

Investigation of R-134a as a modeling fluid for supercritical water

International Nuclear Information System (INIS)

Jouvin, J.C.; Pioro, I.

2014-01-01

The objective of this paper is to investigate the feasibility of using Refrigerant-134a (R-134a) as a potential modeling fluid by comparing the thermophysical properties with those of water. Operating conditions of SuperCritical Water-cooled Reactors (SCWRs) are scaled into those of R-134a, in order to provide proper SCWR-equivalent conditions. The thermophysical properties for R-134a are obtained from NIST REFPROP software. The results indicate that the thermophysical properties of R-134a undergo significant changes within the critical and pseudocritical regions similar to that of supercritical water. An investigation into the pseudocritical region of R-134a was also conducted. (author)

Solvent Effects on Cesium Complexation with Crown Ethers from Liquid to Supercritical Fluids

International Nuclear Information System (INIS)

Wai, Chien M.; Rustenholtz, Anne; Wang, Shaofen; Lee, Su-Chen; Herman, Jamie; Porter, Richard A.

2004-01-01

Nuclear magnetic resonance (NMR) techniques were used to study crown ether-water interactions in solvents of low dielectric constants such as chloroform and carbon tetrachloride. Water forms a 1:1 complex with a number of crown ethers including 12-crown-4, 15-crown-5, 18-crown-6, dicyclohexano-18=crown-6, dicyclohexano-24-crown 8, and dibenzl-24-crown-8 in chloroform. Among these crown ethers, the 18-crown-6-H2 complex has the largest equilibrium constant (K=545) and 97% of the crown is complexed to water in chloroform. Addition of carbon tetrachloride to chloroform lowers the equilibrium constants of the crown-water complexes. The partition coefficients of crown ethers (D=crown in water/crown in solvent) between water and organic solvent also vary with solvent composition

Ultra‐high performance supercritical fluid chromatography of lignin‐derived phenols from alkaline cupric oxide oxidation

Science.gov (United States)

Sun, Mingzhe; Lidén, Gunnar; Sandahl, Margareta

2016-01-01

Traditional chromatographic methods for the analysis of lignin‐derived phenolic compounds in environmental samples are generally time consuming. In this work, an ultra‐high performance supercritical fluid chromatography method with a diode array detector for the analysis of major lignin‐derived phenolic compounds produced by alkaline cupric oxide oxidation was developed. In an analysis of a collection of 11 representative monomeric lignin phenolic compounds, all compounds were clearly separated within 6 min with excellent peak shapes, with a limit of detection of 0.5–2.5 μM, a limit of quantification of 2.5–5.0 μM, and a dynamic range of 5.0–2.0 mM (R 2 > 0.997). The new ultra‐high performance supercritical fluid chromatography method was also applied for the qualitative and quantitative analysis of lignin‐derived phenolic compounds obtained upon alkaline cupric oxide oxidation of a commercial humic acid. Ten out of the previous eleven model compounds could be quantified in the oxidized humic acid sample. The high separation power and short analysis time obtained demonstrate for the first time that supercritical fluid chromatography is a fast and reliable technique for the analysis of lignin‐derived phenols in complex environmental samples. PMID:27452148

Supercritical fluid extraction and ultra performance liquid chromatography of respiratory quinones for microbial community analysis in environmental and biological samples.

Science.gov (United States)

Hanif, Muhammad; Atsuta, Yoichi; Fujie, Koichi; Daimon, Hiroyuki

2012-03-05

Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE) and ultra performance liquid chromatography (UPLC) method for the analysis of bacterial respiratory quinones (RQ) in environmental and biological samples. RQ profile analysis is one of the most widely used culture-independent tools for characterizing microbial community structure. A UPLC equipped with a photo diode array (PDA) detector was successfully applied to the simultaneous determination of ubiquinones (UQ) and menaquinones (MK) without tedious pretreatment. Supercritical carbon dioxide (scCO(2)) extraction with the solid-phase cartridge trap proved to be a more effective and rapid method for extracting respiratory quinones, compared to a conventional organic solvent extraction method. This methodology leads to a successful analytical procedure that involves a significant reduction in the complexity and sample preparation time. Application of the optimized methodology to characterize microbial communities based on the RQ profile was demonstrated for a variety of environmental samples (activated sludge, digested sludge, and compost) and biological samples (swine and Japanese quail feces).

Fiscal 1996 investigational research on the chemical process technology using supercritical fluids; 1996 nendo chorinkai ryutai wo riyoshita kagaku process gijutsu ni kansuru chosa kenkyu

Energy Technology Data Exchange (ETDEWEB)

NONE

1997-03-01

Importance was studied of making a research on the chemical process technology using the supercritical fluid. As for its effect on global warming, the amount of CO2 emission was compared during the operation between the conventional process and the process using the supercritical fluid, the CO2 reduction rate and amount were trially calculated, and a CO2 reduction of a several ten thousand ton scale in carbon conversion was predicted. As to hazardous materials and the reaction of waste retrieval, it was made clear that the process using the supercritical fluid was valid also for objects for which the chemical process used to be impossible, which indicates a possibility of the widening field of application. Concerning its effect on the energy conservation, energy reduction of several ten thousand tons in heavy oil conversion was predicted by replacing all the existing processes with supercritical fluids. Relating to the recycling, with the use of supercritical fluids, the process is possible which produces higher quality and yield and fewer unnecessary products such as char than the conventional process. 197 refs., 102 figs., 71 tabs.

Entropy generation in turbulent mixed convection heat transfer to highly variable property pipe flow of supercritical fluids

International Nuclear Information System (INIS)

Mohseni, Mahdi; Bazargan, Majid

2014-01-01

Highlights: • The entropy generation in supercritical fluid flows has been numerically investigated. • The mechanisms of entropy generation are different near and away from the walls. • In the near wall region, the energy dissipation is the deciding parameter. • Away from the wall, the heat transfer is the effective factor in entropy generation. • The bulk Be number is greater in the liquid-like region than in vapor-like region. - Abstract: In this study, a two dimensional CFD code has been developed to investigate entropy generation in turbulent mixed convection heat transfer flow of supercritical fluids. Since the fluid properties vary significantly under supercritical conditions, the changes of entropy generation are large. The contribution of each of the mechanisms of entropy production (heat transfer and energy dissipation) is compared in different regions of the flow. The results show that the mechanisms of entropy generation act differently in the near wall region within the viscous sub-layer and in the region away from the wall. The effects of the wall heat flux on the entropy generation are also investigated

SEPARATION OF T-MAZ ETHOXYLATED SORBITAN FATTY ACID ESTERS BY SUPERCRITICAL FLUID CHROMATOGRAPHY

Science.gov (United States)

The application of supercritical fluid chromatography (SFC) to the analysis of T-MAZ ethoxylated sorbitan fatty acid esters is described. FC separation methods utilize a density programming technique and a 50 um I.D. capillary column. his work demonstrates that capillary column S...

Preparative isolation and purification of hainanmurpanin, meranzin, and phebalosin from leaves of Murraya exotica L. using supercritical fluid extraction combined with consecutive high-speed countercurrent chromatography.

Science.gov (United States)

Yan, Rongwei; Shen, Jie; Liu, Xiaojing; Zou, Yong; Xu, Xinjun

2018-05-01

The objective of this study was to develop a consecutive preparation method for the isolation and purification of hainanmurpanin, meranzin, and phebalosin from leaves of Murraya exotica L. The process involved supercritical fluid extraction with CO 2 , solvent extraction, and two-step high-speed countercurrent chromatography. Pressure, temperature, and the volume of entrainer were optimized as 27 MPa, 52°C, and 60 mL by response surface methodology in supercritical fluid extraction with CO 2 , and the yield of the crude extracts was 7.91 g from 100 g of leaves. Subsequently, 80% methanol/water was used to extract and condense the three compounds from the crude extracts, and 4.23 g of methanol/water extracts was obtained. Then, a two-step high-speed countercurrent chromatography procedure was developed for the isolation of the three target compounds from methanol/water extracts, including conventional high-speed countercurrent chromatography for further enrichment and consecutive high-speed countercurrent chromatography for purification. The yield of concentrates from high-speed countercurrent chromatography was 2.50 g from 4.23 g of methanol/water extracts. Finally, the consecutive high-speed countercurrent chromatography produced 103.2 mg of hainanmurpanin, 244.7 mg of meranzin, and 255.4 mg of phebalosin with purities up to 97.66, 99.36, and 98.64%, respectively, from 900 mg of high-speed countercurrent chromatography concentrates in one run of three consecutive sample loadings without exchanging a solvent system. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Capillary supercritical fluid chromatography - Fourier transform infrared spectrometry

International Nuclear Information System (INIS)

Olesik, S.V.; French, S.B.; Movotny, M.

1984-01-01

One of the most demanding tasks asked of an analytical chemist today is to separate and identify the components of a nonvolatile complex mixture. An efficient separation technique combined with a universal detector that provides structural information, therefore, would be a great asset to analytical chemists. Capillary supercritical fluid chromatography (SFC) - Fourier transform infrared spectrometry (FTIR) shows great potential for being such a technique. SFC-FTIR shows great potential as a very powerful technique for separation and identification of thermally labile and nonvolatile compounds. Research is continuing in these labs to further optimize the technique. 2 refs

Extraction with supercritical gases

Energy Technology Data Exchange (ETDEWEB)

Schneider, G M; Wilke, G; Stahl, E

1980-01-01

The contents of this book derives from a symposium on the 5th and 6th of June 1978 in the ''Haus der Technik'' in Essen. Contributions were made to separation with supercritical gases, fluid extraction of hops, spices and tobacco, physicochemical principles of extraction, phase equilibria and critical curves of binary ammonia-hydrocarbon mixtures, a quick method for the microanalytical evaluation of the dissolving power of supercritical gases, chromatography with supercritical fluids, the separation of nonvolatile substances by means of compressed gases in countercurrent processes, large-scale industrial plant for extraction with supercritical gases, development and design of plant for high-pressure extraction of natural products.

Supercritical fluid extraction of bi & multi-layer graphene sheets from graphite by using exfoliation technique

Science.gov (United States)

Xavier, Gauravi; Dave, Bhoomi; Khanna, Sakshum

2018-05-01

In recent times, researchers have turned to explore the possibility of using Supercritical Fluid (SCFs) system to penetrate into the inert-gaping of graphite and exfoliate it into a number of layer graphene sheets. The supercritical fluid holds excellent wetting surfaces with low interfacial tension and high diffusion coefficients. Although SCFs exfoliation approach looks promising to developed large scale & low-cost graphene sheet but has not received much attention. To arouse interest and reflection on this approach, this review is organized to summarize the recent progress in graphene production by SCF technology. Here we present the simplest route to obtained layers of graphene sheets by intercalating and exfoliating graphite using supercritical CO2 processing. The layers graphene nano-sheets were collected in dichloromethane (DCM) solution which prevents the restocking of sheets. The obtained graphene sheets show the desired characteristics and thus can be used in physical, chemical and biological sciences. Thus this method provides an effortless and eco-friendly approach for the synthesis of layers of graphene sheets.

Integrating a post-column makeup pump into preparative supercritical fluid chromatography systems to address stability and recovery issues during purifications.

Science.gov (United States)

Bajpai, Lakshmikant; Naidu, Harshavardhan; Asokan, Kathiravan; Shaik, Khaja Mohiddin; Kaspady, Mahammed; Arunachalam, Piramanayagam; Wu, Dauh-Rurng; Mathur, Arvind; Sarabu, Ramakanth

2017-08-18

Purification of many pharmaceutical compounds by supercritical fluid chromatography (SFC) has always been challenging because of degradation of compound during the isolation step in the presence of acidic or basic modifiers in the mobile phase. Stability of such acid or base-sensitive compounds could be improved by post-column addition of a solvent containing base or acid modifier as counter ion through a make-up pump respectively to neutralize the compound fraction without affecting the resolution. One such case study has been presented in this work where the stability of a base-sensitive compound was addressed by the addition of acidic co-solvent through the make-up pump. Details of this setup and the investigation of degradation of the in-house base-sensitive compound are discussed in this paper. In addition, poor retentivity and low recovery of many non-polar compounds in SFC eluting under low co-solvent percentage is another major concern. Even though the desired separation could be achieved with low percentage of co-solvent, it's difficult to get the proper recovery after purification due to precipitation of the sample and significant aerosol formation inside the cyclone. We have demonstrated the first-time use of a post-column make-up pump on SFC 350 system to introduce additional solvent prior to cyclone to avoid the precipitation, reduce the aerosol formation and thus improve the recovery of non-polar compounds eluting under less than 10% of co-solvent. Copyright © 2017 Elsevier B.V. All rights reserved.

Critical fluid technology for the processing of lipid-related natural products

Energy Technology Data Exchange (ETDEWEB)

King, J.W. [Los Alamos National Lab., Supercritical Fluid Facility, Chemistry Div. NM (United States)

2004-07-01

In recent years, the technology envelope that embraces critical fluids can involve a wide range of conditions, different types of pure and modified fluids, as well as processing options involving extractions, fractionations or reactions. Technological development drivers continue to be environmentally and consumer-benign processing and/or products, however in recent years expansion of the use of sub- and supercritical fluids has been catalyzed by applications in such opportune fields as nutraceuticals, conversion of biomass (bio-refining), and the ability to modify natural products by reactions. The use of critical fluid technology is an important facet of any sustainable development program, particularly when utilized over a broad, interconnected application platform. In this overview presentation, concepts and applications of critical fluids from the author's research as well as the literature will be cited to support the above trends. A totally 'green' processing platform appears to be viable using carbon dioxide in the appropriate form, ethanol and water as intermediate co-solvents/reactants, and water from above its boiling point to supercritical conditions. These fluids can be combined in overall coupled unit processes, such as combining trans-esterification with hydrogenation, or glycero-lysis of lipid moieties with supercritical fluid fractionation. Such fluids also can exploited sequentially for bio-refining processes or the segregation of value-added products, but may require using coupled fluid or unit operations to obtain the targeted product composition or purity. Changing the reduced temperatures and/or pressures of critical fluids offers a plethora of opportunity, an excellent example being the relative critical fluid state of water. For example, sub-critical water slightly above its boiling point provides a unique medium that mimics polar organic solvents, and has been used even for the extraction of thermally labile solutes or

Supercritical Fluid Extraction of Bacterial and Archaeal Lipid Biomarkers from Anaerobically Digested Sludge

Directory of Open Access Journals (Sweden)

Koichi Fujie

2012-03-01

Full Text Available Supercritical fluid extraction (SFE was used in the analysis of bacterial respiratory quinone (RQ, bacterial phospholipid fatty acid (PLFA, and archaeal phospholipid ether lipid (PLEL from anaerobically digested sludge. Bacterial RQ were determined using ultra performance liquid chromatography (UPLC. Determination of bacterial PLFA and archaeal PLEL was simultaneously performed using gas chromatography-mass spectrometry (GC-MS. The effects of pressure, temperature, and modifier concentration on the total amounts of RQ, PLFA, and PLEL were investigated by 23 experiments with five settings chosen for each variable. The optimal extraction conditions that were obtained through a multiple-response optimization included a pressure of 23.6 MPa, temperature of 77.6 °C, and 10.6% (v/v of methanol as the modifier. Thirty nine components of microbial lipid biomarkers were identified in the anaerobically digested sludge. Overall, the SFE method proved to be more effective, rapid, and quantitative for simultaneously extracting bacterial and archaeal lipid biomarkers, compared to conventional organic solvent extraction. This work shows the potential application of SFE as a routine method for the comprehensive analysis of microbial community structures in environmental assessments using the lipid biomarkers profile.

Computational fluid dynamics study of viscous fingering in supercritical fluid chromatography.

Science.gov (United States)

Subraveti, Sai Gokul; Nikrityuk, Petr; Rajendran, Arvind

2018-01-26

Axi-symmetric numerical simulations are carried out to study the dynamics of a plug introduced through a mixed-stream injection in supercritical fluid chromatographic columns. The computational fluid dynamics model developed in this work takes into account both the hydrodynamics and adsorption equilibria to describe the phenomena of viscous fingering and plug effect that contribute to peak distortions in mixed-stream injections. The model was implemented into commercial computational fluid dynamics software using user-defined functions. The simulations describe the propagation of both the solute and modifier highlighting the interplay between the hydrodynamics and plug effect. The simulated peaks showed good agreement with experimental data published in the literature involving different injection volumes (5 μL, 50 μL, 1 mL and 2 mL) of flurbiprofen on Chiralpak AD-H column using a mobile phase of CO 2 and methanol. The study demonstrates that while viscous fingering is the main source of peak distortions for large-volume injections (1 mL and 2 mL) it has negligible impact on small-volume injections (5 μL and 50 μL). Band broadening in small-volume injections arise mainly due to the plug effect. Crown Copyright © 2017. Published by Elsevier B.V. All rights reserved.

Basil (Ocimum basilicum L. essential oil and extracts obtained by supercritical fluid extraction

Directory of Open Access Journals (Sweden)

Zeković Zoran P.

2015-01-01

Full Text Available The extracts obtained from sweet basil (Ocimum basilicum L. by hydrodistillation and supercritical fluid extraction (SFE were qualitative and quantitative analyzed by GC-MS and GC-FID. Essential oil (EO content of basil sample, determined by an official method, was 0.565% (V/w. The yields of basil obtained by SFE were from 0.719 to 1.483% (w/w, depending on the supercritical fluid (carbon dioxide density (from 0.378 to 0.929 g mL-1. The dominant compounds detected in all investigated samples (EO obtained by hydrodistillation and different SFE extracts were: linalool, as the major compound of basil EO (content from 10.14 to 49.79%, w/w, eugenol (from 3.74 to 9.78% and ä-cardinene (from 3.94 to 8.07%. The quantitative results of GC-MS from peak areas and by GC-FID using external standard method involving main standards, were compared and discussed. [Projekat Ministarstva nauke Republike Srbije, br. TR 31013

Substantial rate enhancements of the esterification reaction of phthalic anhydride with methanol at high pressure and using supercritical CO2 as a co-solvent in a glass microreactor

NARCIS (Netherlands)

Benito-Lopez, F.; Tiggelaar, Roald M.; Salblut, K.; Huskens, Jurriaan; Egberink, Richard J.M.; Reinhoudt, David; Gardeniers, Johannes G.E.; Verboom, Willem

2007-01-01

The esterification reaction of phthalic anhydride with methanol was performed at different temperatures in a continuous flow glass microreactor at pressures up to 110 bar and using supercritical CO2 as a co-solvent. The design is such that supercritical CO2 can be generated inside the microreactor.

Numerical Study on Heat Transfer Performance of PCHE With Supercritical CO2 as Working Fluid

International Nuclear Information System (INIS)

Jeon, Sang Woo; Ngo, Ich-long; Byon, Chan

2016-01-01

The printed circuit heat exchanger (PCHE) is regarded as a promising candidate for advanced heat exchangers for the next-generation supercritical CO 2 power generation owing to its high compactness and rigid structure. In this study, an innovative type of PCHE, in which the channel sizes for the heat source fluid and heat sink fluid are different, is considered for analysis. The thermal performance of the PCHE, with supercritical CO 2 as the working fluid, is numerically analyzed. The results have shown that the thermal performance of the PCHE decreases monotonically when the channel size of either the heat source channel or the heat sink channel, because of the decreased flow velocity. On the other hand, the thermal performance of the PCHE is found to be almost independent of the spacing between the channels. In addition, it was found that the channel cross sectional shape has little effect on the thermal performance when the hydraulic diameter of the channel remains constant.

Stability analysis of fluid at supercritical pressure in a heated channel

International Nuclear Information System (INIS)

Gallaway, T.; Podowski, M. Z.

2010-01-01

The Supercritical Water Reactor (SCWR) is one of several reactor design concepts included in the Generation IV International Advanced Reactor Design Program. This reactor design is based upon current light water reactors and supercritical fossil-fuel power plants. Water at supercritical pressures is used as the reactor coolant. At these conditions, there is no phase change in the coolant; however the fluid properties undergo significant variation, particularly in the pseudo-critical region. The fluid density may decrease by a factor of six with increasing temperature. It has been seen before that variations in fluid density can lead to density-wave oscillations in two-phase flow systems in general and boiling water reactors in particular. Such instabilities may cause many undesired problems for reactor operation and safety. Similar issues must be addressed in the design and safety analysis of SCWRs. The objective of the present work has been the development of a detailed one-dimensional model of instabilities in a heated channel corresponding to the geometry and flow conditions in the proposed typical SCWRs. The new model is capable of analyzing in detail transient effects of local property variations in parallel channels subject to a constant pressure drop boundary condition. In particular, such a model can be used to establish SCWR power limits imposed by the onset of instabilities in the hot channel of the reactor. Both time and frequency-domain methods of stability analysis have been developed. The latter method is particularly important since it is not associated with any numerical issues, is very accurate, and allows for establishing general stability boundaries in a computationally effective manner. Model testing has included a study of dependence of the proposed spatial discretization scheme on the accuracy of calculations. A parametric study has also been performed on the effect of channel operating conditions on flow oscillations. Finally, a stability map

Cellulose tris-(3,5-dimethylphenylcarbamate)-based chiral stationary phase for the enantioseparation of drugs in supercritical fluid chromatography: comparison with HPLC.

Science.gov (United States)

Kalíková, Květa; Martínková, Monika; Schmid, Martin G; Tesařová, Eva

2018-03-01

A cellulose tris-(3,5-dimethylphenylcarbamate)-based chiral stationary phase was studied as a tool for the enantioselective separation of 21 selected analytes with different pharmaceutical and physicochemical properties. The enantioseparations were performed using supercritical fluid chromatography. The effect of the mobile phase composition was studied. Four different additives (diethylamine, triethylamine, isopropylamine, and trifluoroacetic acid) and isopropylamine combined with trifluoroacetic acid were tested and their influence on enantioseparation was compared. The influence of two different mobile phase co-solvents (methanol and propan-2-ol) combined with all the additives was also evaluated. The best mobile phase compositions for the separation of the majority of enantiomers were CO 2 /methanol/isopropylamine 80:20:0.1 v/v/v or CO 2 /propan-2-ol/isopropylamine/trifluoroacetic acid 80:20:0.05:0.05 v/v/v/v. The best results were obtained from the group of basic β-blockers. A high-performance liquid chromatography separation system composed of the same stationary phase and mobile phase of similar properties prepared as a mixture of hexane/propan-2-ol/additive 80:20:0.1 v/v/v was considered for comparison. Supercritical fluid chromatography was found to yield better results, i.e. better enantioresolution for shorter analysis times than high-performance liquid chromatography. However, examples of enantiomers better resolved under the optimized conditions in high-performance liquid chromatography were also found. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ultra-high performance supercritical fluid chromatography of lignin-derived phenols from alkaline cupric oxide oxidation.

Science.gov (United States)

Sun, Mingzhe; Lidén, Gunnar; Sandahl, Margareta; Turner, Charlotta

2016-08-01

Traditional chromatographic methods for the analysis of lignin-derived phenolic compounds in environmental samples are generally time consuming. In this work, an ultra-high performance supercritical fluid chromatography method with a diode array detector for the analysis of major lignin-derived phenolic compounds produced by alkaline cupric oxide oxidation was developed. In an analysis of a collection of 11 representative monomeric lignin phenolic compounds, all compounds were clearly separated within 6 min with excellent peak shapes, with a limit of detection of 0.5-2.5 μM, a limit of quantification of 2.5-5.0 μM, and a dynamic range of 5.0-2.0 mM (R(2) > 0.997). The new ultra-high performance supercritical fluid chromatography method was also applied for the qualitative and quantitative analysis of lignin-derived phenolic compounds obtained upon alkaline cupric oxide oxidation of a commercial humic acid. Ten out of the previous eleven model compounds could be quantified in the oxidized humic acid sample. The high separation power and short analysis time obtained demonstrate for the first time that supercritical fluid chromatography is a fast and reliable technique for the analysis of lignin-derived phenols in complex environmental samples. © 2016 The Authors, Journal of Separation Science Published by WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Technical design issues for a field-portable supercritical fluid extractor

Energy Technology Data Exchange (ETDEWEB)

Wright, B.W.; Zemanian, T.S.; Robins, W.H.; Wright, C.W.

1995-01-01

Supercritical fluid extraction is gaining acceptance as an alternative sample preparation method for trace organic analysis. The development of SFE instrumentation optimized for field use requires taking several technical design issues including size and weight requirements, user-friendly operation, and technical performance capabilities into consideration. Parameters associated with a prototype SFE instrument under development for potential use in conducting on-site inspections of the Chemical Weapons Convention and its preliminary technical and operational performance are described.

Fiscal 1997 report on the results of the introductory R and D of the New Sunshine Project under a consignment from NEDO. Introductory R and D of the supercritical fluid use technology; 1997 nendo `New Sunshine keikaku` sendo kenkyu kaihatsu Shin Energy Sangyo Gijutsu Sogo Kaihatsu Kiko itaku. Chorinkai ryutai riyo gijutsu sendo kenkyu kaihatsu seika hokokusho

Energy Technology Data Exchange (ETDEWEB)

NONE

1998-03-01

The R and D of chemical reaction using supercritical fluids started in fiscal 1997. In the R and D of solvent reaction, as the research on polymer decomposition with supercritical water, studies were conducted of the mechanism of conversion reaction to chemical materials, cleavage mechanism of stable chemical bonds, and synthetic reaction in the supercritical state reaction field. In the research on oxidation reaction, as the study of complete oxidation in supercritical water for high efficiency energy recovery, studies of complete oxidation of liquid fuels, and complete oxidation of solid fuels. In the research on hydrogenation, studies of lightening of heavy oil in supercritical water, etc. In the R and D of the basic technology, studies of corrosion mechanism of metals in supercritical water, construction of the basic framework for technical database of supercritical fluids, etc. In the survey of technical trends and new research themes, the introductory R and D of element technology, etc. were conducted, and the results were described of the survey of technical trends and new research themes and the trend survey of overseas technology. 314 refs., 87 figs., 81 tabs.

Synthesis of biodiesel fuel additives from glycerol using green chemistry and supercritical fluids

Science.gov (United States)

For every 3 moles of fatty acid esters produced, 1 mole of glycerol remains, ~11% of the biodiesel volume. One new method of glycerol use could be as a biodiesel fuel additive/extender using eco-friendly heterogeneous catalysts and supercritical fluids (SFs). SFs have advantages such as greater diff...

Recrystallization of andrographolide using the supercritical fluid antisolvent process

Science.gov (United States)

Chen, Kexun; Zhang, Xingyuan; Pan, Jian; Yin, Wenhong

2005-01-01

The supercritical antisolvent (SAS) process was used to modify the solid-state properties of andrographolide. Ethanol was employed as solvents for the pharmaceutical compound and carbon dioxide was used as an antisolvent. The effect of process parameters on the precipitate crystals such as pressure, organic solution flow rate, and concentration of the andrographolide solution were investigated. The crystal habit is column-like and its size changed from longer and thicker to shorter and thinner when pressure increased and when the solution flow rate increased, the size of the crystal decreased. The X-ray diffraction (XRD) patterns revealed variations of crystallinity and crystal orientation depending on pressure, where the degree of crystallinity increased when pressure increased. The differential scanning calorimetry patterns also showed the same results as XRD.

Solvent Removal and Spore Inactivation Directly in Dispensing Vials with Supercritical Carbon Dioxide and Sterilant

OpenAIRE

Howell, Jahna; Niu, Fengui; McCabe, Shannon E.; Zhou, Wei; Decedue, Charles J.

2012-01-01

A process is described using supercritical carbon dioxide to extract organic solvents from drug solutions contained in 30-mL serum vials. We report drying times of less than 1 h with quantitative recovery of sterile drug. A six-log reduction of three spore types used as biological indicators is achieved with direct addition of peracetic acid to a final concentration of approximately 5 mM (~0.04 %) to the drug solution in the vial. Analysis of two drugs, acetaminophen and paclitaxel, indicated...

Advanced Thermal Storage for Central Receivers with Supercritical Coolants

Energy Technology Data Exchange (ETDEWEB)

Kelly, Bruce D.

2010-06-15

The principal objective of the study is to determine if supercritical heat transport fluids in a central receiver power plant, in combination with ceramic thermocline storage systems, offer a reduction in levelized energy cost over a baseline nitrate salt concept. The baseline concept uses a nitrate salt receiver, two-tank (hot and cold) nitrate salt thermal storage, and a subcritical Rankine cycle. A total of 6 plant designs were analyzed, as follows: Plant Designation Receiver Fluid Thermal Storage Rankine Cycle Subcritical nitrate salt Nitrate salt Two tank nitrate salt Subcritical Supercritical nitrate salt Nitrate salt Two tank nitrate salt Supercritical Low temperature H2O Supercritical H2O Two tank nitrate salt Supercritical High temperature H2O Supercritical H2O Packed bed thermocline Supercritical Low temperature CO2 Supercritical CO2 Two tank nitrate salt Supercritical High temperature CO2 Supercritical CO2 Packed bed thermocline Supercritical Several conclusions have been drawn from the results of the study, as follows: 1) The use of supercritical H2O as the heat transport fluid in a packed bed thermocline is likely not a practical approach. The specific heat of the fluid is a strong function of the temperatures at values near 400 °C, and the temperature profile in the bed during a charging cycle is markedly different than the profile during a discharging cycle. 2) The use of supercritical CO2 as the heat transport fluid in a packed bed thermocline is judged to be technically feasible. Nonetheless, the high operating pressures for the supercritical fluid require the use of pressure vessels to contain the storage inventory. The unit cost of the two-tank nitrate salt system is approximately $24/kWht, while the unit cost of the high pressure thermocline system is nominally 10 times as high. 3) For the supercritical fluids, the outer crown temperatures of the receiver tubes are in the range of 700 to 800 °C. At temperatures of 700 °C and above

Development of a sensitive and rapid method for rifampicin impurity analysis using supercritical fluid chromatography.

Science.gov (United States)

Li, Wei; Wang, Jun; Yan, Zheng-Yu

2015-10-10

A novel simple, fast and efficient supercritical fluid chromatography (SFC) method was developed and compared with RPLC method for the separation and determination of impurities in rifampicin. The separation was performed using a packed diol column and a mobile phase B (modifier) consisting of methanol with 0.1% ammonium formate (w/v) and 2% water (v/v). Overall satisfactory resolutions and peak shapes for rifampicin quinone (RQ), rifampicin (RF), rifamycin SV (RSV), rifampicin N-oxide (RNO) and 3-formylrifamycinSV (3-FR) were obtained by optimization of the chromatography system. With gradient elution of mobile phase, all of the impurities and the active were separated within 4 min. Taking full advantage of features of SFC (such as particular selectivity, non-sloping baseline in gradient elution, and without injection solvent effects), the method was successfully used for determination of impurities in rifampicin, with more impurity peaks detected, better resolution achieved and much less analysis time needed compared with conventional reversed-phase liquid chromatography (RPLC) methods. Copyright © 2015 Elsevier B.V. All rights reserved.

Supercritical Fluid Extraction of Quinones from Compost for Microbial Community Analysis

Directory of Open Access Journals (Sweden)

Ni Luh Gede Ratna Juliasih

2015-01-01

Full Text Available Supercritical fluid extraction (SFE was used to extract quinones from compost to monitor the microbial community dynamics during composting. The 0.3 g of dried compost was extracted using 3 mL min−1 of carbon dioxide (90% and methanol (10% at 45°C and 25 MPa for a 30 min extraction time. The extracted quinones were analysed using ultra performance liquid chromatography (UPLC with 0.3 mL min−1 of methanol mobile phase for a 50 min chromatographic run time. A comparable detected amount of quinones was obtained using the developed method and an organic solvent extraction method, being 36.06 μmol kg−1 and 34.54 μmol kg−1, respectively. Significantly low value of dissimilarity index (D between the two methods (0.05 indicated that the quinone profile obtained by both methods was considered identical. The developed method was then applied to determine the maturity of the compost by monitoring the change of quinone during composting. The UQ-9 and MK-7 were predominant quinones in the initial stage of composting. The diversity of quinone became more complex during the cooling and maturation stages. This study showed that SFE had successfully extracted quinones from a complex matrix with simplification and rapidity of the analysis that is beneficial for routine analysis.

Fingerprints of flower absolutes using supercritical fluid chromatography hyphenated with high resolution mass spectrometry.

Science.gov (United States)

Santerre, Cyrille; Vallet, Nadine; Touboul, David

2018-06-02

Supercritical fluid chromatography hyphenated with high resolution mass spectrometry (SFC-HRMS) was developed for fingerprint analysis of different flower absolutes commonly used in cosmetics field, especially in perfumes. Supercritical fluid chromatography-atmospheric pressure photoionization-high resolution mass spectrometry (SFC-APPI-HRMS) technique was employed to identify the components of the fingerprint. The samples were separated with a porous graphitic carbon (PGC) Hypercarb™ column (100 mm × 2.1 mm, 3 μm) by gradient elution using supercritical CO 2 and ethanol (0.0-20.0 min (2-30% B), 20.0-25.0 min (30% B), 25.0-26.0 min (30-2% B) and 26.0-30.0 min (2% B)) as mobile phase at a flow rate of 1.5 mL/min. In order to compare the SFC fingerprints between five different flower absolutes: Jasminum grandiflorum absolutes, Jasminum sambac absolutes, Narcissus jonquilla absolutes, Narcissus poeticus absolutes, Lavandula angustifolia absolutes from different suppliers and batches, the chemometric procedure including principal component analysis (PCA) was applied to classify the samples according to their genus and their species. Consistent results were obtained to show that samples could be successfully discriminated. Copyright © 2018 Elsevier B.V. All rights reserved.

Isolation, Fractionation, and Identification of Sucrose Esters from Various Oriental Tobaccos Employing Supercritical Fluids

Directory of Open Access Journals (Sweden)

Ashraf-Khorassani M

2014-12-01

Full Text Available Isolation, fractionation, and identification of sucrose esters from aged oriental tobacco employing supercritical fluids have been completed. Underivatized sucrose ester-rich extracts were obtained using supercritical CO2 at densities greater than 0.73 g/mL. Lower density CO2 provided extracts with notable amounts of tobacco derived material; yet, no detectable sucrose ester content. Preparative supercritical fluid chromatography (SFC provided for an additional purification of the sucrose ester-enriched fraction after column optimization. Structural assignments of the SFC fractions were facilitated using gas chromatography/mass spectrometry (GC/MS accompanied by N, O-bis(trimethylsilyltrifluoroacetamide-dimethylformamide (BSTFA-DMF derivatization of the free hydroxyl groups and high performance-liquid chromatography/mass spectrometry (HPLC/MS. From a relative quantitative perspective regardless of tobacco type, sucrose esters having an acetyl group on C6 of the glucose function (Group III were in higher concentration compared to both the concentration observed for sucrose ester of Group I (acetyl group on C3 of fructose and sucrose ester of Group II (no acetyl group on either glucose or fructose. Saturated fatty acid constituents were found to range from a maximum total of 18 carbons to a minimum total of 13 carbons. Unsaturated and isomeric fatty acid homologues were detected within the Group II sucrose ester.

Monodisperse microbeads of hypercrosslinked polystyrene for liquid and supercritical fluid chromatography

Science.gov (United States)

Tsyurupa, M. P.; Blinnikova, Z. K.; Il'in, M. M.; Davankov, V. A.; Parenago, O. O.; Pokrovskii, O. I.; Usovich, O. I.

2015-11-01

Monodisperse styrene-divinylbenzene (1 wt %) copolymer microbeads are obtained via the elaborate method of high-productivity precipitation polymerization. The crosslinking of this copolymer with chloromethyl methyl ether in the presence of Friedel-Crafts catalyst yields porous hypercrosslinked polymers with degrees of crosslinking that range from 200 to 500%. Microbead sorbents are shown to be suited for selective stationary phases for high-performance liquid chromatography and supercritical fluid chromatography.

The use of supercritical fluid extraction as a sample preparation technique for soils

International Nuclear Information System (INIS)

Levy, J.M.; Dolata, L.A.; Rosselli, A.C.; Ravey, R.M.

1994-01-01

Using off-line supercritical fluid extraction (SFE), polynuclear aromatic hydrocarbons (PAHs) were extracted at different levels from various soil and sediment matrices. Based upon GC/MS measurements a number of SFE operational parameters including pressure, temperature and flow rate, were optimized to yield the highest efficiencies with the best precision

using Supercritical Fluid Extraction

African Journals Online (AJOL)

Methods: Supercritical CO2 extraction technology was adopted in this experiment to study the process of extraction of volatile oil from Polygonatum odoratum while gas chromatograph-mass spectrometer ..... Saponin rich fractions from.

Supercritical fluid extraction of silicone oil from uranate microspheres prepared by sol-gel process

International Nuclear Information System (INIS)

Kumar, R.; Venkatakrishnan, R.; Sivaraman, N.; Srinivasan, T.G.; Vasudeva Rao, P.R.

2005-01-01

Supercritical fluid extraction of silicone oil from urania microspheres prepared through sol-gel route was investigated. The influence of pressure, temperature, and flow rate on the extraction efficiency was studied. Experimental conditions were optimised for the complete removal of silicone oil from urania microspheres. (author)

Volatile and Nonvolatile Constituents and Antioxidant Capacity of Oleoresins in Three Taiwan Citrus Varieties as Determined by Supercritical Fluid Extraction

Directory of Open Access Journals (Sweden)

Min-Hung Chen

2016-12-01

Full Text Available As local varieties of citrus fruit in Taiwan, Ponkan (Citrus reticulata Blanco, Tankan (C. tankan Hayata, and Murcott (C. reticulate × C. sinensis face substantial competition on the market. In this study, we used carbon dioxide supercritical technology to extract oleoresin from the peels of the three citrus varieties, adding alcohol as a solvent assistant to enhance the extraction rate. The supercritical fluid extraction was fractionated with lower terpene compounds in order to improve the oxygenated amounts of the volatile resins. The contents of oleoresin from the three varieties of citrus peels were then analyzed with GC/MS in order to identify 33 volatile compounds. In addition, the analysis results indicated that the non-volatile oleoresin extracted from the samples contains polymethoxyflavones (86.2~259.5 mg/g, limonoids (111.7~406.2 mg/g, and phytosterols (686.1~1316.4 μg/g. The DPPH (1,1-Diphenyl-2-picrylhydrazyl, ABTS [2,2′-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid] scavenging and inhibition of lipid oxidation, which test the oleoresin from the three kinds of citrus, exhibited significant antioxidant capacity. The component polymethoxyflavones contributed the greatest share of the overall antioxidant capacity, while the limonoid and phytosterol components effectively coordinated with its effects.

Supercritical Fluid Extraction and Ultra Performance Liquid Chromatography of Respiratory Quinones for Microbial Community Analysis in Environmental and Biological Samples

Directory of Open Access Journals (Sweden)

Koichi Fujie

2012-03-01

Full Text Available Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE and ultra performance liquid chromatography (UPLC method for the analysis of bacterial respiratory quinones (RQ in environmental and biological samples. RQ profile analysis is one of the most widely used culture-independent tools for characterizing microbial community structure. A UPLC equipped with a photo diode array (PDA detector was successfully applied to the simultaneous determination of ubiquinones (UQ and menaquinones (MK without tedious pretreatment. Supercritical carbon dioxide (scCO2 extraction with the solid-phase cartridge trap proved to be a more effective and rapid method for extracting respiratory quinones, compared to a conventional organic solvent extraction method. This methodology leads to a successful analytical procedure that involves a significant reduction in the complexity and sample preparation time. Application of the optimized methodology to characterize microbial communities based on the RQ profile was demonstrated for a variety of environmental samples (activated sludge, digested sludge, and compost and biological samples (swine and Japanese quail feces.

Solvent removal and spore inactivation directly in dispensing vials with supercritical carbon dioxide and sterilant.

Science.gov (United States)

Howell, Jahna; Niu, Fengui; McCabe, Shannon E; Zhou, Wei; Decedue, Charles J

2012-06-01

A process is described using supercritical carbon dioxide to extract organic solvents from drug solutions contained in 30-mL serum vials. We report drying times of less than 1 h with quantitative recovery of sterile drug. A six-log reduction of three spore types used as biological indicators is achieved with direct addition of peracetic acid to a final concentration of approximately 5 mM (~0.04 %) to the drug solution in the vial. Analysis of two drugs, acetaminophen and paclitaxel, indicated no drug degradation as a result of the treatment. Furthermore, analysis of the processed drug substance showed that no residual peracetic acid could be detected in the final product. We have demonstrated an effective means to simultaneously dry and sterilize active pharmaceutical ingredients from organic solvents directly in a dispensing container.

Numerical Study on Heat Transfer Performance of PCHE With Supercritical CO{sub 2} as Working Fluid

Energy Technology Data Exchange (ETDEWEB)

Jeon, Sang Woo; Ngo, Ich-long; Byon, Chan [Yeungnam Univ., Gyeongsan (Korea, Republic of)

2016-11-15

The printed circuit heat exchanger (PCHE) is regarded as a promising candidate for advanced heat exchangers for the next-generation supercritical CO{sub 2} power generation owing to its high compactness and rigid structure. In this study, an innovative type of PCHE, in which the channel sizes for the heat source fluid and heat sink fluid are different, is considered for analysis. The thermal performance of the PCHE, with supercritical CO{sub 2} as the working fluid, is numerically analyzed. The results have shown that the thermal performance of the PCHE decreases monotonically when the channel size of either the heat source channel or the heat sink channel, because of the decreased flow velocity. On the other hand, the thermal performance of the PCHE is found to be almost independent of the spacing between the channels. In addition, it was found that the channel cross sectional shape has little effect on the thermal performance when the hydraulic diameter of the channel remains constant.

Advanced Supercritical Carbon Dioxide Brayton Cycle Development

Energy Technology Data Exchange (ETDEWEB)

Anderson, Mark [Univ. of Wisconsin, Madison, WI (United States); Sienicki, James [Argonne National Lab. (ANL), Argonne, IL (United States); Moisseytsev, Anton [Argonne National Lab. (ANL), Argonne, IL (United States); Nellis, Gregory [Univ. of Wisconsin, Madison, WI (United States); Klein, Sanford [Univ. of Wisconsin, Madison, WI (United States)

2015-10-21

Fluids operating in the supercritical state have promising characteristics for future high efficiency power cycles. In order to develop power cycles using supercritical fluids, it is necessary to understand the flow characteristics of fluids under both supercritical and two-phase conditions. In this study, a Computational Fluid Dynamic (CFD) methodology was developed for supercritical fluids flowing through complex geometries. A real fluid property module was implemented to provide properties for different supercritical fluids. However, in each simulation case, there is only one species of fluid. As a result, the fluid property module provides properties for either supercritical CO₂ (S-CO₂) or supercritical water (SCW). The Homogeneous Equilibrium Model (HEM) was employed to model the two-phase flow. HEM assumes two phases have same velocity, pressure, and temperature, making it only applicable for the dilute dispersed two-phase flow situation. Three example geometries, including orifices, labyrinth seals, and valves, were used to validate this methodology with experimental data. For the first geometry, S-CO₂ and SCW flowing through orifices were simulated and compared with experimental data. The maximum difference between the mass flow rate predictions and experimental measurements is less than 5%. This is a significant improvement as previous works can only guarantee 10% error. In this research, several efforts were made to help this improvement. First, an accurate real fluid module was used to provide properties. Second, the upstream condition was determined by pressure and density, which determines supercritical states more precise than using pressure and temperature. For the second geometry, the flow through labyrinth seals was studied. After a successful validation, parametric studies were performed to study geometric effects on the leakage rate. Based on these parametric studies, an optimum design strategy for the see

Immunomodulatory effects of supercritical fluid CO2 extracts from freeze-dried powder of Tenebrio molitor larvae (yellow mealworm

Directory of Open Access Journals (Sweden)

QingFeng TANG

2016-01-01

Full Text Available Abstract In order to take full advantage of Tenebrio molitor larvae (yellow mealworm resources, the supercritical CO2 fluid freeze-dried powder of T. molitor larvae (fdTML extraction on the immune systems of mice was carried out. The results about the effects of supercritical CO2 fluid fdTML extraction on carbon expurgation and phagocytosis of peritoneal macrophages experiments of mice indicated that the fdTML extraction enhanced observably carbon expurgatory index, phagocytic rate and phagocytic index. The fdTML extraction could stimulate response of delayed hypersensitivity. The proliferation of ConA-induced mitogenic reponse for spleen lymphocyte was also increased. The amount of hemolytic antibody in mice serum increased compared with those of the control group mice. The half of hemolysis values in serum of treated mice increased compared to the control group. Furthermore, serum NO content in all treatment groups was higher than that of the control group whereas acid phosphatase and alkaline phosphatase activity was only significantly higher relative to the control group. Our findings suggest that supercritical CO2 fluid the fdTML extraction has potential as a health food supplement.

Preheating of fluid in a supercritical Brayton cycle power generation system at cold startup

Science.gov (United States)

Wright, Steven A.; Fuller, Robert L.

2016-07-12

Various technologies pertaining to causing fluid in a supercritical Brayton cycle power generation system to flow in a desired direction at cold startup of the system are described herein. A sensor is positioned at an inlet of a turbine, wherein the sensor is configured to output sensed temperatures of fluid at the inlet of the turbine. If the sensed temperature surpasses a predefined threshold, at least one operating parameter of the power generation system is altered.

Influence of Solvent-Solvent and Solute-Solvent Interaction Properties on Solvent-Mediated Potential

International Nuclear Information System (INIS)

Zhou Shiqi

2005-01-01

A recently proposed universal calculational recipe for solvent-mediated potential is applied to calculate excess potential of mean force between two large Lennard-Jones (LJ) or hard core attractive Yukawa particles immersed in small LJ solvent bath at supercritical state. Comparison between the present prediction with a hypernetted chain approximation adopted for solute-solute correlation at infinitely dilute limit and existing simulation data shows high accuracy for the region with large separation, and qualitative reliability for the solute particle contact region. The calculational simplicity of the present recipe allows for a detailed investigation on the effect of the solute-solvent and solvent-solvent interaction details on the excess potential of mean force. The resultant conclusion is that gathering of solvent particles near a solute particle leads to repulsive excess PMF, while depletion of solvent particles away from the solute particle leads to attractive excess PMF, and minor change of the solvent-solvent interaction range has large influence on the excess PMF.

Extraction and isotopic analysis of medium molecular weight hydrocarbons from Murchison using supercritical carbon dioxide

Science.gov (United States)

Gilmour, Iain; Pillinger, Colin

1993-03-01

The large variety of organic compounds present in carbonaceous chondrites poses particular problems in their analysis not the least of which is terrestrial contamination. Conventional analytical approaches employ simple chromatographic techniques to fractionate the extractable compounds into broad classes of similar chemical structure. However, the use of organic solvents and their subsequent removal by evaporation results in the depletion or loss of semi-volatile compounds as well as requiring considerable preparative work to assure solvent purity. Supercritical fluids have been shown to provide a powerful alternative to conventional liquid organic solvents used for analytical extractions. A sample of Murchison from the Field Museum was analyzed. Two interior fragments were used; the first (2.85 g) was crushed in an agate pestel and mortar to a grain size of ca. 50-100 micron, the second (1.80 g) was broken into chips 3-8 mm in size. Each sample was loaded into a stainless steel bomb and placed in the extraction chamber of an Isco supercritical fluid extractor maintained at 35 C. High purity (99.9995 percent) carbon dioxide was used and was pressurized using an Isco syringe pump. The samples were extracted dynamically by flowing CO2 under pressure through the bomb and venting via a 50 micron fused filica capillary into 5 mls of hexane used as a collection solvent. The hexane was maintained at a temperature of 0.5 C. A series of extractions were done on each sample using CO2 of increasing density. The principal components extracted in each fraction are summarized.

Investigation of parameters affecting the online combination of supercritical fluid extraction with capillary gas chromatography

NARCIS (Netherlands)

Lou, X.W.; Janssen, J.G.M.; Cramers, C.A.M.G.

1996-01-01

Two different injectors, a split/splitless injector and a programmed temperature vaporizer (PTV) injector were investigated as the interface in on-line supercritical fluid extraction (SFE)-capillary gas chromatography (cGC). The parameters affecting the chromatographic peak shapes as well as the

Evolution of supercritical fluid in deeply subducted continental crust: a case study of composite granite-quartz veins in the Sulu belt, China

Science.gov (United States)

Wang, S.; Wang, L.; Brown, M.

2016-12-01

Although fluid plays a key role in element transport and rock strength during subduction to and exhumation from ultrahigh pressure (UHP) metamorphic conditions, the source of supercritical fluid at P above the second critical endpoints (SCE) and the subsequent evolution are not well constrained. To provide insight into the evolution of supercritical fluid in continental subduction zones, we undertook an integrated study of composite granite-quartz veins in retrogressed and migmatitic UHP eclogite at General's Hill, N of Qingdao, in the central Sulu belt. The composite veins are irregularly distributed in the eclogite, which occurs as blocks within gneiss. The granite component is enriched in large ion lithophile elements and light rare earth elements but depleted in high field strength elements and heavy rare earth elements, indicating crystallization from a melt phase of crustal origin. Additionally, the granite contains high modal phengite (22-30 vol%) and clinozoisite/epidote (3-10 vol%), implying precipitation from a H2O-rich silicate melt. By contrast, the quartz component is dominated by SiO2 (99.10 wt%), and contains low total rare earth elements (ΣREE = 0.46 ppm), indicating precipitation from an aqueous fluid. The crystallization age of the composite veins is 221 ± 2 Ma, which is younger than the UHP metamorphism in the Sulu belt at ca 230 Ma, consistent with formation during exhumation. Initial 176Hf/177Hf ratios and δ18O values of metamorphic zircons from the composite veins, and Sr-Nd isotope compositions of the granites all lie between values for eclogite and gneiss, indicating a mixed source. Accordingly, we propose that a supercritical fluid generated from the gneiss and the included blocks of eclogite at P-T conditions above the SCE for both compositions became trapped in the eclogite during exhumation. At P below the SCE for the hydrous granite system, the mixed supercritical fluid separated into immiscible aqueous melt and aqueous fluid and

Extraction and isolation of dictamnine, obacunone and fraxinellone from Dictamnus dasycarpus Turcz. by supercritical fluid extraction and high-speed counter-current chromatography

International Nuclear Information System (INIS)

Wang, Daijie; Lin, Yunliang; Lin, Xiaojing; Geng, Yanling; Wang, Xiao; Zhang, Jinjie; Qiu, Jiying

2012-01-01

Supercritical fluid extraction was used to extract active compounds from the Chinese traditional medicinal D. dasycarpus under the pressure of 30 MPa and temperature of 45 degree C. Further separation and purification was established by high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (1:0.8:1.3:0.9, volume ratio). The separation yielded a total of 47 mg of dictamnine, 24 mg of obacunone and 83 mg of fraxinellone from 1.0 g of the crude extract in one step separation with the purity of 99.2, 98.4 and 99.0%, respectively, as determined by HPLC. The chemical structures of these compounds were identified by ESI-MS, IR, 1H-NMR and 13 C-NMR. (author)

Extraction and isolation of dictamnine, obacunone and fraxinellone from Dictamnus dasycarpus Turcz. by supercritical fluid extraction and high-speed counter-current chromatography

Energy Technology Data Exchange (ETDEWEB)

Wang, Daijie; Lin, Yunliang; Lin, Xiaojing; Geng, Yanling; Wang, Xiao, E-mail: wxjn1998@126.com [Process Control Research Center of TCM. Shandong Academy of Sciences. Shandong Analysis and Test Center (China); Zhang, Jinjie [College of Biosystems Engineering and Food Science, Zhejiang University (China); Qiu, Jiying [Institute of Agro-Food Science and Technology, Shandong Academy of Agricultural Science, Shandong (China)

2012-07-01

Supercritical fluid extraction was used to extract active compounds from the Chinese traditional medicinal D. dasycarpus under the pressure of 30 MPa and temperature of 45 degree C. Further separation and purification was established by high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (1:0.8:1.3:0.9, volume ratio). The separation yielded a total of 47 mg of dictamnine, 24 mg of obacunone and 83 mg of fraxinellone from 1.0 g of the crude extract in one step separation with the purity of 99.2, 98.4 and 99.0%, respectively, as determined by HPLC. The chemical structures of these compounds were identified by ESI-MS, IR, 1H-NMR and {sup 13}C-NMR. (author)

Extraction and isolation of dictamnine, obacunone and fraxinellone from Dictamnus dasycarpus Turcz. by supercritical fluid extraction and high-speed counter-current chromatography

Directory of Open Access Journals (Sweden)

Daijie Wang

2012-01-01

Full Text Available Supercritical fluid extraction was used to extract active compounds from the Chinese traditional medicinal D. dasycarpus under the pressure of 30 MPa and temperature of 45 ºC. Further separation and purification was established by high-speed counter-current chromatography (HSCCC with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (1:0.8:1.3:0.9, volume ratio. The separation yielded a total of 47 mg of dictamnine, 24 mg of obacunone and 83 mg of fraxinellone from 1.0 g of the crude extract in one step separation with the purity of 99.2, 98.4 and 99.0%, respectively, as determined by HPLC. The chemical structures of these compounds were identified by ESI-MS, IR, ¹H-NMR and 13C-NMR.

A Novel Model for Multicomponent Supercritical Fluid Extraction and its Application to Ruta graveolens.

Czech Academy of Sciences Publication Activity Database

Sovová, Helena; Sajfrtová, Marie; Stateva, R.P.

2017-01-01

Roč. 120, Part 1 (2017), s. 102-112 ISSN 0896-8446 R&D Projects: GA MŠk 2B06049 Institutional support: RVO:67985858 Keywords : supercritical fluid extraction * multicomponent equilibrium * kinetics Subject RIV: CI - Industrial Chemistry, Chemical Engineering OBOR OECD: Chemical process engineering Impact factor: 2.991, year: 2016

Determination of fat- and water-soluble vitamins by supercritical fluid chromatography: A review.

Science.gov (United States)

Tyśkiewicz, Katarzyna; Dębczak, Agnieszka; Gieysztor, Roman; Szymczak, Tomasz; Rój, Edward

2018-01-01

Vitamins are compounds that take part in all basic functions of an organism but also are subject of number of studies performed by different researchers. Two groups of vitamins are distinguished taking into consideration their solubility. Chromatography with supercritical CO 2 has found application in the determination, separation, and quantitative analyses of both fat- and water-soluble vitamins. The methods of vitamins separation have developed and improved throughout the years. Both groups of compounds were separated using supercritical fluid chromatography with different detection on different stationary phases. The main aim of this review is to provide an overview of the studies of vitamins separation that have been determined so far. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Understanding and diminishing the extra-column band broadening effects in supercritical fluid chromatography.

Science.gov (United States)

De Pauw, Ruben; Shoykhet Choikhet, Konstantin; Desmet, Gert; Broeckhoven, Ken

2015-07-17

Supercritical fluid chromatography, where a low-viscosity mobile phase such as carbon dioxide is used, proves to be an excellent technique for fast and efficient separations, especially when sub-2μm particles are used. However, to achieve high velocities when using these small particles, and in order to stay within the flow rate range of current SFC-instruments, narrow columns (e.g. 2.1mm ID) must be used. Unfortunately, state-of-the-art instrumentation is limiting the full separation power of these narrower columns due to significant extra-column band broadening effects. The present work identifies and quantifies the different contributions to extra-column band broadening in SFC such as the influence of the sample solvent, injection volume, extra-column volumes and detector cell volume/design. When matching the sample solvent to the mobile phase in terms of elution strength and polarity (e.g. using hexane/ethanol/isopropanol 85/10/5vol%) and lowering the injection volume to 0.4μL, the plate count can be increased from 7600 to 21,300 for a low-retaining compound (k'=2.3) on a 2.1mm×150mm column (packed with 1.8μm particles). The application of a water/acetonitrile mixture as sample solvent was also investigated. It was found that when the volumetric ratio of water/acetonitrile was optimized, only a slightly lower plate count was measured compared to the hexane-based solvent when minimizing injection and extra-column volume. This confirms earlier results that water/acetonitrile can be used if water-soluble samples are considered or when a less volatile solvent is preferred. Minimizing the ID of the connection capillaries from 250 to 65μm, however, gives no further improvement in obtained efficiency for early-eluting compounds when a standard system configuration with optimized sample solvent was used. When switching to a state-of-the-art detector design with reduced (dispersion) volume (1.7-0.6μL), an increase in plate count is observed (from 11,000 to 14

Supercritical fluid extraction of triterpenes and aliphatic hydrocarbons from olive tree derivatives

Directory of Open Access Journals (Sweden)

Aimen Issaoui

2017-05-01

Full Text Available Olive leaves and tree bark were extracted through supercritical fluid extraction (SFE and the chemical composition of the extracted mixture was determined by Gas Chromatography–Mass Spectrometry (GC–MS. Both samples contain a great number of triterpenes as squalene, which were used since 1997 as a main constituent of the flu vaccine (FLUAD, and the alpha-tocopherol the most biologically active form of vitamin E. We also underline the presence of many aliphatic compounds such nonacosane and heptacosane in low concentrations. The extractions were carried out at 313 and 333 K, at a pressure varying from 90 to 250 bars and using pure carbon dioxide in its supercritical phase. Therefore, their solubilities at equilibrium were numerically optimized via two assumptions and compared with the experimental values. Indeed, a good agreement between several results was shown.

Impregnation of cinnamaldehyde into cassava starch biocomposite films using supercritical fluid technology for the development of food active packaging.

Science.gov (United States)

de Souza, Ana Cristina; Dias, Ana M A; Sousa, Hermínio C; Tadini, Carmen C

2014-02-15

In this work, supercritical solvent impregnation (SSI) has been tested for the incorporation of natural compounds into biocomposite materials for food packaging. Cinnamaldehyde, with proved antimicrobial activity against fungi commonly found in bread products, was successfully impregnated on biocomposite cassava starch based materials using supercritical carbon dioxide as solvent. Different process experimental conditions were tested (pressure, impregnation time and depressurization rate) at a fixed temperature (35 °C) in order to study their influence on the amount of impregnated cinnamaldehyde as well as on the morphology of the films. Results showed that all conditions permitted to impregnate antimicrobial active amounts superior to those previously obtained using conventional incorporation methods. Moreover, a significant decrease of the equilibrium water vapor sorption capacity and water vapor permeability of the films was observed after SSI processing which is a clear advantage of the process, considering the envisaged applications. Copyright © 2013 Elsevier Ltd. All rights reserved.

Study of high-pressure adsorption from supercritical fluids by the potential theory

DEFF Research Database (Denmark)

Monsalvo, Matias Alfonso; Shapiro, Alexander

2009-01-01

The multicomponent potential theory of adsorption (MPTA), which has been previously used to study low-pressure adsorption of subcritical fluids, is extended to adsorption equilibria from supercritical fluids up to high pressures. The MPTA describes an adsorbed phase as an inhomogeneous fluid...... the adsorbed and the gas phases. We have also evaluated the performance of the classical Soave-Redlich-Kwong (SRK) EoS. The fluid-solid interactions are described by simple Dubinin-Radushkevich-Astakhov (DRA) potentials. In addition, we test the performance of the 10-4-3 Steele potential. It is shown...... that application of sPC-SAFT slightly improves the performance of the MPTA and that in spite of its simplicity, the DRA model can be considered as an accurate potential, especially, for mixture adsorption. We show that, for the sets of experimental data considered in this work, the MPTA is capable of predicting...

Extraction of lapachol from Tabebuia avellanedae wood with supercritical CO2: an alternative to Soxhlet extraction?

Directory of Open Access Journals (Sweden)

Viana L.M.

2003-01-01

Full Text Available The solubility of lapachol in supercritical CO2 was determined at 40°C and pressures between 90 and 210 bar. Supercritical fluid extraction of lapachol and some related compounds by CO2 from Tabebuia avellanedae wood is compared to Soxhlet extraction with different solvents. A standard macroscale (100-200 g wood and a microscale (~10 mg wood experimental setup are described and their results are compared. The latter involved direct spectrophotometric quantification in a high-pressure autoclave with an integrated optical path and a magnetic stirrer, fitted directly into a commercial spectrophotometer. The relative amount of lapachol extracted by supercritical CO2 at 40°C and 200 bar was about 1.7%, which is similar to the results of Soxhlet extractions. Lower contents of alpha- and beta-lapachone as well as dehydro-alpha-lapachone are also reported.

Fiscal 1999 achievement report on regional consortium research and development project. Regional consortium on energy research in its 3rd year (Development of an environmentally-friendly industrial cleaning system using supercritical CO2 fluid); 1999 nendo chorinkai ryutai wo mochiita kankyo chowagata kogyo senjo sochi no kaihatsu seika hokokusho. 3

Energy Technology Data Exchange (ETDEWEB)

NONE

2000-03-01

In high-technology industries such as the semiconductor industry, cleaning operations are indispensable. In these industries, replacement of the current method with a new one has become an urgent matter, thanks to the new control imposed on pollutant CFC (chlorofluorocarbon). Using a supercritical fluid, whose density and other features may be regulated extensively and continuously by controlling temperature and pressure, various conditions may be set in detail for the cleaning element, such as the dissolving power, dispersion force, surface activity, and chemical reactivity. The fluid is environmentally friendly and free of pollution. Facilities for recovering, regenerating, and circulating the solvent are incorporated into a test cleaner built in the preceding fiscal year, and a new system is completed. The system is operated in a test run for performance assessment, and data are collected to specify cleaning conditions best for each kind of the target items. Studies are made to expand the scope of system application for use under supercritical conditions. An experiment is conducted using a pollutant model, and a method to analyze the degree of cleaning is studied using an effective diffusion coefficient. A self-cleaning method is studied for the filter for the regeneration of the supercritical cleaning solvent. A market research is carried out for the commercialization of the industrial cleaning system. (NEDO)

Extraction of aucubin from seeds of Eucommia ulmoides Oliv. using supercritical carbon dioxide.

Science.gov (United States)

Li, Hui; Hu, Jiangyu; Ouyang, Hui; Li, Yanan; Shi, Hui; Ma, Chengjin; Zhang, Yongkang

2009-01-01

Supercritical CO2 was used as solvent for the extraction of aucubin from the seeds of Eucommia ulmoides Oliv. The co-solvent composition was tested and extraction conditions were optimized. Results showed that the best co-solvent was a water-ethanol mixture (1 + 3, v/v), and the highest yield was obtained when the extraction was performed under 26 MPa at extraction and separation temperatures of 55 and 30 degrees C for 120 min, using 6 mL co-solvent/g material at a CO2 flow rate of 20 L/h. In a comparison of the supercritical CO2 and Soxhlet extraction methods, the Soxhlet method needed 3 h to extract 10 g material, whereas the supercritical CO2 extraction technique needed only 2 h to extract 100 g material, thus showing a high extraction capability. The supercritical CO2 extraction produced a higher yield, with a lower cost for the extraction. Owing to the advantages of low extraction temperature, high yield, and ease of separating the product from the solvent, supercritical CO2 extraction is likely to be developed into an ideal technique for the extraction of aucubin, a compound with thermal instability, from the seeds of this plant.

Instrumentation for analytical scale supercritical fluid chromatography.

Science.gov (United States)

Berger, Terry A

2015-11-20

Analytical scale supercritical fluid chromatography (SFC) is largely a sub-discipline of high performance liquid chromatography (HPLC), in that most of the hardware and software can be used for either technique. The aspects that separate the 2 techniques stem from the use of carbon dioxide (CO2) as the main component of the mobile phase in SFC. The high compressibility and low viscosity of CO2 mean that pumps, and autosamplers designed for HPLC either need to be modified or an alternate means of dealing with compressibility needs to be found. The inclusion of a back pressure regulator and a high pressure flow cell for any UV-Vis detector are also necessary. Details of the various approaches, problems and solutions are described. Characteristics, such as adiabatic vs. isothermal compressibility, thermal gradients, and refractive index issues are dealt with in detail. Copyright © 2015 Elsevier B.V. All rights reserved.

Design of preparative-supercritical fluid chromatography.

Science.gov (United States)

Rajendran, Arvind

2012-08-10

Preparative supercritical fluid chromatography (prep-SFC) is an important separation process in the chromatographers toolbox. Owing to the unique properties of the mobile phase, which is predominantly CO(2), the behavior of SFC is markedly different from high performance liquid chromatography (HPLC). This review article focuses on the scale-up of preparative chromatography. The basics of SFC, with particular focus on highlighting the key differences between SFC and HPLC, are introduced. Then, a framework for rational design of prep-SFC is proposed. This framework is based on obtaining basic system parameters from analytical scale equipment, i.e., with very small amount of material, and performing design and optimization in silico to evaluate process performance and to identify operating conditions for scale-up. The tools required to obtain the input parameters such as adsorption isotherms are discussed and the development of the design and optimization framework is elaborated. Examples from the literature which use this approach for successful scale-up are provided. Finally the design of multi-column SFC systems is discussed. Copyright © 2012 Elsevier B.V. All rights reserved.

Developing novel one-step processes for obtaining food-grade O/W emulsions from pressurized fluid extracts: processes description, state of the art and perspectives

Directory of Open Access Journals (Sweden)

Diego Tresinari SANTOS

2015-01-01

Full Text Available AbstractIn this work, a novel on-line process for production of food-grade emulsions containing oily extracts, i.e. oil-in-water (O/W emulsions, in only one step is presented. This process has been called ESFE, Emulsions from Supercritical Fluid Extraction. With this process, emulsions containing supercritical fluid extracts can be obtained directly from plant materials. The aim in the conception of this process is to propose a new rapid way to obtain emulsions from supercritical fluid extracts. Nowadays the conventional emulsion formulation method is a two-step procedure, i.e. first supercritical fluid extraction for obtaining an extract; secondly emulsion formulation using another device. Other variation of the process was tested and successfully validated originating a new acronymed process: EPFE (Emulsions from Pressurized Fluid Extractions. Both processes exploit the supercritical CO2-essential oils miscibility, in addition, EPFE process exploits the emulsification properties of saponin-rich pressurized aqueous plant extracts. The feasibility of this latter process was demonstrated using Pfaffia glomerata roots as source of saponin-rich extract, water as extracting solvent and clove essential oil, directly extracted using supercritical CO2, as a model dispersed phase. In addition, examples of pressurized fluid-based coupled processes applied for adding value to food bioactive compounds developed in the past five years are reviewed.

Supercritical fluid chromatography for separation and preparation of tautomeric 7-epimeric spiro oxindole alkaloids from Uncaria macrophylla.

Science.gov (United States)

Yang, Wenzhi; Zhang, Yibei; Pan, Huiqin; Yao, Changliang; Hou, Jinjun; Yao, Shuai; Cai, Luying; Feng, Ruihong; Wu, Wanying; Guo, Dean

2017-02-05

Increasing challenge arising from configurational interconversion in aqueous solvent renders it rather difficult to isolate high-purity tautomeric reference standards and thus largely hinders the holistic quality control of traditional Chinese medicine (TCM). Spiro oxindole alkaloids (SOAs), as the markers for the medicinal Uncaria herbs, can easily isomerize in polar or aqueous solvent via a retro-Mannich reaction. In the present study, supercritical fluid chromatography (SFC) is utilized to separate and isolate two pairs of 7-epimeric SOAs, including rhynchophylline (R) and isorhynchophylline (IR), corynoxine (C) and corynoxine B (CB), from Uncaria macrophylla. Initially, the solvent that can stabilize SOA epimers was systematically screened, and acetonitrile was used to dissolve and as the modifier in SFC. Then, key parameters of ultra-high performance SFC (ultra-performance convergence chromatography, UPC 2 ), comprising stationary phase, additive in modifier, column temperature, ABPR pressure, and flow rate, were optimized in sequence. Two isocratic UPC 2 methods were developed on the achiral Torus 1-AA and Torus Diol columns, suitable for UV and MS detection, respectively. MCI gel column chromatography fractionated the U. macrophylla extract into two mixtures (R/IR and C/CB). Preparative SFC, using a Viridis Prep Silica 2-EP OBD column and acetonitrile-0.2% diethylamine in CO 2 as the mobile phase, was finally employed for compound purification. As a result, the purity of four SOA compounds was all higher than 95%. Different from reversed-phase HPLC, SFC, by use of water-free mobile phase (inert CO 2 and aprotic modifier), provides a solution to rapid analysis and isolation of tautomeric reference standards for quality control of TCM. Copyright © 2016 Elsevier B.V. All rights reserved.

Feasibility of correlating separation of ternary mixtures of neutral analytes via thin layer chromatography with supercritical fluid chromatography in support of green flash separations.

Science.gov (United States)

Ashraf-Khorassani, M; Yan, Q; Akin, A; Riley, F; Aurigemma, C; Taylor, L T

2015-10-30

Method development for normal phase flash liquid chromatography traditionally employs preliminary screening using thin layer chromatography (TLC) with conventional solvents on bare silica. Extension to green flash chromatography via correlation of TLC migration results, with conventional polar/nonpolar liquid mixtures, and packed column supercritical fluid chromatography (SFC) retention times, via gradient elution on bare silica with a suite of carbon dioxide mobile phase modifiers, is reported. Feasibility of TLC/SFC correlation is individually described for eight ternary mixtures for a total of 24 neutral analytes. The experimental criteria for TLC/SFC correlation was assumed to be as follows: SFC/UV/MS retention (tR) increases among each of the three resolved mixture components; while, TLC migration (Rf) decreases among the same resolved mixture components. Successful correlation of TLC to SFC was observed for most of the polar organic solvents tested, with the best results observed via SFC on bare silica with methanol as the CO2 modifier and TLC on bare silica with a methanol/dichloromethane mixture. Copyright © 2015 Elsevier B.V. All rights reserved.

Fabrication of fluorographene nanosheets with high yield and good quality based on supercritical fluid-phase exfoliation

Energy Technology Data Exchange (ETDEWEB)

Chen, Qi; Ji, Yan; Zhang, Danying; Shi, Jia [Nanjing University of Science and Technology, Key Laboratory of Soft Chemistry and Functional Materials, College of Chemical Engineering (China); Xiao, Yinghong, E-mail: yhxiao@njnu.edu.cn [Nanjing Normal University, Jiangsu Collaborative Innovation Center of Biomedical Functional Materials, College of Chemistry and Materials Science (China); Che, Jianfei, E-mail: xiaoche@mail.njust.edu.cn [Nanjing University of Science and Technology, Key Laboratory of Soft Chemistry and Functional Materials, College of Chemical Engineering (China)

2016-07-15

This article presents a novel and simple method of supercritical fluid-phase exfoliation to fabricate fluorographene (FG) nanosheets with high yield and good quality. After soaking with supercritical CO{sub 2} and glycol at 10 MPa and 50 °C for 24 h, fluoride graphite powder was exfoliated by the intercalated CO{sub 2} and glycol molecules during an abrupt depressurization step. Here, supercritical CO{sub 2} acted as a penetrant and glycol acted as a “molecular wedge” to exfoliate fluoride graphite very well. The properties of FG nanosheets were detected by TEM, AFM, UV spectra, FTIR, XPS, Raman spectra, and XRD, which show the possibility of producing thickness-controlled FG nanosheets by varying numbers of supercritical CO{sub 2} process and the high yield of pure FG nanosheets of 32 wt%, four times higher than that of the sample treated only by the traditional method of sonication. Its simplicity, high productivity, low cost, and short processing time make this technique suitable for large-scale manufacturing of FG nanosheets.

Particle formation with supercritical fluids challenges and limitations

CERN Document Server

Türk, Michael

2014-01-01

Particle formation with supercritical fluids is a promising alternative to conventional precipitation processes as it allows the reduction of particle size and control of morphology and particle size distribution without degradation or contamination of the product. The book comprehensively examines the current status of research and development and provides perspectives and insights on promising future directions. The introduction to high pressure and high temperature phase equilibria and nucleation phenomena provides the basic principles of the underlying physical and chemical phenomena, allowing the reader an understanding of the relationship between process conditions and particle characteristics. Bridging the gap between theory and application, the book imparts the scientific and engineering fundamentals for innovative particle formation processes. The interdisciplinary "modus operandi" will encourage cooperation between scientists and researchers from different but complementary disciplines. Focuses on ...

Performance Analysis and Working Fluid Selection of a Supercritical Organic Rankine Cycle for Low Grade Waste Heat Recovery

Directory of Open Access Journals (Sweden)

Yourong Li

2012-08-01

Full Text Available The performance analysis of a supercritical organic Rankine cycle system driven by exhaust heat using 18 organic working fluids is presented. Several parameters, such as the net power output, exergy efficiency, expander size parameter (SP, and heat exchanger requirement of evaporator and the condenser, were used to evaluate the performance of this recovery cycle and screen the working fluids. The results reveal that in most cases, raising the expander inlet temperature is helpful to improve the net power output and the exergy efficiency. However, the effect of the expander inlet pressure on those parameters is related to the expander inlet temperature and working fluid used. Either lower expander inlet temperature and pressure, or higher expander inlet temperature and pressure, generally makes the net power output more. Lower expander inlet temperature results in larger total heat transfer requirement and expander size. According to the screening criteria of both the higher output and the lower investment, the following working fluids for the supercritical ORC system are recommended: R152a and R143a.

Generic supercritical water technology; Generic technology to shite no chorinkaisui riyo gijutsu

Energy Technology Data Exchange (ETDEWEB)

Arai, K; Ajiri, M; Inomata, H; Smith, R; Hakuta, Y [Tohoku University, Sendai (Japan). Faculty of Engineering; Yokoyama, C [Tohoku University, Sendai (Japan). The Institute forChemical Reaction Science; Chin, L [New Energy and Industrial Technology Development Organization, Tokyo, (Japan)

1997-02-01

This paper describes the measurement and analysis for clarifying solution structure of supercritical water and exhibition mechanism of solvent functions. It also describes the development of new processes using supercritical water as reaction solvent. The PVT measurements were conducted in the supercritical region using pure water and NaCl aqueous solution, to confirm the reduction of molar volume of the electrolyte solution. The hydration structure was examined in the supercritical aqueous solution by the molecular dynamic simulation. As a result, presence of hydrogen bond structure, where the contribution of two branching hydrogen bond can not be ignored, was suggested under the supercritical condition. Characteristics of supercritical aqueous solutions are analyzed through in-situ Raman and scattered X-ray spectral measurements. Moreover, this paper introduces developments of some processes in the supercritical water, such as decomposition of wasted polymers, recovery of chemical materials, reforming of heavy hydrocarbons by contact hydrogenation, and synthesis of fine powders of metal oxide by reaction crystallization.

Application of supercritical fluid chromatography coupled to mass spectrometry to the determination of fat-soluble vitamins in selected food products.

Science.gov (United States)

Oberson, Jean-Marie; Campos-Giménez, Esther; Rivière, Johann; Martin, Frédéric

2018-06-01

In the present manuscript, we describe a fully optimized and validated method suitable to analyse nine compounds (retinyl acetate, retinyl palmitate, retinol, α-tocopherol, α-tocopheryl acetate, cholecalciferol, ergocalciferol, phylloquinone, menaquinone-4) representing the major contributors to the fat-soluble vitamin activity of selected food products (infant formulas, adult nutritionals, infant cereals and mixed meals). Sample preparation involves direct solvent extraction using enzyme-assisted matrix disintegration and methanolic protein precipitation. Direct injection of the extract allows quantification of vitamins A, E and K in only 7 min, while vitamin D is determined after fast derivatization of the extract. Separation is achieved by supercritical fluid chromatography and detection performed by tandem mass spectrometry in positive Atmospheric Pressure Chemical Ionization mode. Results on a Standard Reference Material (SRM 1849a Infant/Adult Nutritional) were not statistically different from reference values. Full validation of the method showed excellent overall performance. Average recovery rate was between 90 and 110% for all vitamins and matrixes. The methodology shows enhanced safety and reduced cost as compared with previously published methods, together with potential for application to more complex matrixes. The full procedure can be easily applied in control laboratories dramatically increasing sample throughput and reducing solvent consumption. Copyright © 2018 Elsevier B.V. All rights reserved.

Studies on supercritical fluid extraction behaviour of uranium and thorium nitrates using amides

International Nuclear Information System (INIS)

Sujatha, K.; Kumar, R.; Sivaraman, N.; Srinivasan, T.G.; Vasudeva Rao, P.R.

2007-01-01

Supercritical fluid extraction studies of uranyl nitrate and thorium nitrate in mixture were carried out using various amides such as N,N-di(2-ethylhexyl) isobutyramide (D2EHIBA),N,N-dihexyl octanamide (DHOA) and Diisooctyl Butanamide (DiOBA). These studies established a preferential extraction of uranium over thorium. Among the various amides studied, D2EHIBA offered the best rate of preferential extraction of uranium over thorium. (author)

Ionic magnetic fluids in polar solvents with tuned counter-ions

Energy Technology Data Exchange (ETDEWEB)

Lopes Filomeno, C. [Sorbonne Universités, UPMC Univ Paris 06, CNRS, Lab. PHENIX, Paris (France); Grupo de Fluidos Complexos Inst. de Quimica, Univ. de Brasília, Brasília (DF) (Brazil); Kouyaté, M. [Sorbonne Universités, UPMC Univ Paris 06, CNRS, Lab. PHENIX, Paris (France); Cousin, F. [Lab. Léon Brillouin – CE-Saclay, Gif-sur-Yvette (France); Demouchy, G. [Sorbonne Universités, UPMC Univ Paris 06, CNRS, Lab. PHENIX, Paris (France); Dpt de physique, Univ. de Cergy Pontoise, Cergy-Pontoise (France); Dubois, E.; Michot, L.; Mériguet, G. [Sorbonne Universités, UPMC Univ Paris 06, CNRS, Lab. PHENIX, Paris (France); Perzynski, R., E-mail: regine.perzynski@upmc.fr [Sorbonne Universités, UPMC Univ Paris 06, CNRS, Lab. PHENIX, Paris (France); Peyre, V.; Sirieix-Plénet, J. [Sorbonne Universités, UPMC Univ Paris 06, CNRS, Lab. PHENIX, Paris (France); Tourinho, F.A. [Grupo de Fluidos Complexos Inst. de Quimica, Univ. de Brasília, Brasília (DF) (Brazil)

2017-06-01

The aim of the present study is to propose a new reproducible method for preparing colloidal dispersions of electrostatically charged nanoparticles (NPs) in polar solvents with different kinds of counter-ions. Maghemite NPs are here dispersed in solvents of different dielectric constant, namely water, dimethylsulfoxide (DMSO) and an ionic liquid, ethylammonium nitrate (EAN). If the existence of a NP superficial charge happens to be necessary for the colloidal stability of the dispersions in these three solvents, the standard DLVO theory cannot be used any more to describe the colloidal stability in EAN. The structure of the dispersions and the strength of the interparticle repulsion are investigated by small angle X-ray scattering measurements, in association with Ludwig–Soret coefficient determinations. Specificities, associated to the nature of the counter-ions are identified in this work on the colloidal stability, on the interparticle repulsion and on the Ludwig–Soret coefficient. - Highlights: • A controlled synthesis of ionic magnetic fluids in three polar solvents is proposed. • Colloidal repulsion in the magnetic fluids depends on the counter-ion nature. • Soret coefficient of citrate-coated maghemite nanoparticles is probed in water-pH7. • Thermophilicity of nanoparticles depends on the nature of their counter-ions. • Nanoparticles dressed with same counter-ions have solvent-dependent thermoproperties.

Modelling small angle neutron scattering data from polymers in supercritical fluids

International Nuclear Information System (INIS)

Triolo, F.; Triolo, A.; Lo Celso, F.; Donato, D. I.; Triolo, R.; Johnson, J. S. Jr.

2000-01-01

In this paper we report a SANS investigation of micelle formation by fluorocarbon-hydrocarbon block copolymers in supercritical CO 2 (scCO 2 ) at 313K. A sharp unimer-micelle transition is obtained due to the tuning of the solvating ability of scCO 2 by profiling pressure. At high pressure the copolymer is in a monomeric state with a random coil structure. By lowering the pressure aggregates are formed with the hydrocarbon segments forming the core and the fluorocarbon segments forming the corona of spherical aggregates. This aggregate-unimer transition is driven by the gradual penetration of CO 2 molecules toward the core of the aggregate and is critically related to the density of the solvent, thus suggesting the definition of a critical micellization density (CMD)

Comparison of supercritical fluid extraction and Soxhlet extraction for the determination of PCBs in seaweed samples.

Science.gov (United States)

Punín Crespo, M O; Lage Yusty, M A

2005-06-01

The efficiency of supercritical fluid extraction for the determination of 12 polychlorinated biphenyls from algae samples is compared to Soxhlet extraction. Analytical detection limits for the individual congeners ranged from 0.62 microgl(-1) to 19 microgl(-1). Recovery was tested for both methods using standard addition procedure. At maximum spike level of concentration, the mean recoveries were not significantly different (P>0.05) of all PCBs studied, with the exception of PCBs 28, 52, 77 and 169. Method precision for Soxhlet extraction (yield comparable results, SFE offers the advantage of detecting all PCBs studied at lower concentrations, reducing extraction time, and reducing the amount of solvents needed. The optimized methods were applied to the analysis of three real seaweed samples, except for PCB101 the concentrations of all PCBs were low or below the detection limits. The levels of PCB101 found in sample 1 were 6.6+/-0.54 ng g(-1) d.w., in sample 2 the levels were 8.2+/-0.86 ng g(-1) d.w. and in sample 3 they were 7.7+/-0.08 ng g(-1) d.w.

Drying of supercritical carbon dioxide with membrane processes

NARCIS (Netherlands)

Lohaus, Theresa; Scholz, Marco; Koziara, Beata; Benes, Nieck Edwin; Wessling, Matthias

2015-01-01

In supercritical extraction processes regenerating the supercritical fluid represents the main cost constraint. Membrane technology has potential for cost efficient regeneration of water-loaded supercritical carbon dioxide. In this study we have designed membrane-based processes to dehydrate

Method developments approaches in supercritical fluid chromatography applied to the analysis of cosmetics.

Science.gov (United States)

Lesellier, E; Mith, D; Dubrulle, I

2015-12-04

Analyses of complex samples of cosmetics, such as creams or lotions, are generally achieved by HPLC. These analyses are often multistep gradients, due to the presence of compounds with a large range of polarity. For instance, the bioactive compounds may be polar, while the matrix contains lipid components that are rather non-polar, thus cosmetic formulations are usually oil-water emulsions. Supercritical fluid chromatography (SFC) uses mobile phases composed of carbon dioxide and organic co-solvents, allowing for good solubility of both the active compounds and the matrix excipients. Moreover, the classical and well-known properties of these mobile phases yield fast analyses and ensure rapid method development. However, due to the large number of stationary phases available for SFC and to the varied additional parameters acting both on retention and separation factors (co-solvent nature and percentage, temperature, backpressure, flow rate, column dimensions and particle size), a simplified approach can be followed to ensure a fast method development. First, suited stationary phases should be carefully selected for an initial screening, and then the other operating parameters can be limited to the co-solvent nature and percentage, maintaining the oven temperature and back-pressure constant. To describe simple method development guidelines in SFC, three sample applications are discussed in this paper: UV-filters (sunscreens) in sunscreen cream, glyceryl caprylate in eye liner and caffeine in eye serum. Firstly, five stationary phases (ACQUITY UPC(2)) are screened with isocratic elution conditions (10% methanol in carbon dioxide). Complementary of the stationary phases is assessed based on our spider diagram classification which compares a large number of stationary phases based on five molecular interactions. Secondly, the one or two best stationary phases are retained for further optimization of mobile phase composition, with isocratic elution conditions or, when

Direct online extraction and determination by supercritical fluid extraction with chromatography and mass spectrometry of targeted carotenoids from red Habanero peppers (Capsicum chinense Jacq.).

Science.gov (United States)

Zoccali, Mariosimone; Giuffrida, Daniele; Dugo, Paola; Mondello, Luigi

2017-10-01

Recently, supercritical fluid chromatography coupled to mass spectrometry has gained attention as a fast and useful technology applied to the carotenoids analysis. However, no reports are available in the literature on the direct online extraction and determination by supercritical fluid extraction with chromatography and mass spectrometry. The aim of this research was the development of an online method coupling supercritical fluid extraction and supercritical fluid chromatography for a detailed targeted native carotenoids characterization in red habanero peppers. The online nature of the system, compared to offline approaches, improves run-to-run precision, enables the setting of batch-type applications, and reduces the risks of sample contamination. The extraction has been optimized using different temperatures, starting from 40°C up to 80°C. Multiple extractions, until depletion, were performed on the same sample to evaluate the extraction yield. The range of the first extraction yield, carried out at 80°C, which was the best extraction temperature, was 37.4-65.4%, with a %CV range of 2-12. Twenty-one targeted analytes were extracted and identified by the developed methodology in less than 17 min, including free, monoesters, and diesters carotenoids, in a very fast and efficient way. Quantification of the β-carotene was carried out by using the optimized conditions. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Computational fluid dynamic model for glycerol gasification in supercritical water in a tee junction shaped cylindrical reactor

NARCIS (Netherlands)

Yukananto, Riza; Pozarlik, Artur K.; Brem, Gerrit

2018-01-01

Gasification in supercritical water is a very promising technology to process wet biomass into a valuable gas. Providing insight of the process behavior is therefore very important. In this research a computational fluid dynamic model is developed to investigate glycerol gasification in

Supercritical transitiometry of polymers.

Science.gov (United States)

Randzio, S L; Grolier, J P

1998-06-01

Employing supercritical fluids (SCFs) during polymers processing allows the unusual properties of SCFs to be exploited for making polymer products that cannot be obtained by other means. A new supercritical transitiometer has been constructed to permit study of the interactions of SCFs with polymers during processing under well-defined conditions of temperature and pressure. The supercritical transitiometer allows pressure to be exerted by either a supercritical fluid or a neutral medium and enables simultaneous determination of four basic parameters of a transition, i.e., p, T, Δ(tr)H and Δ(tr)V. This permits determination of the SCF effect on modification of the polymer structure at a given pressure and temperature and defines conditions to allow reproducible preparation of new polymer structures. Study of a semicrystalline polyethylene by this method has defined conditions for preparation of new microfoamed phases with good mechanical properties. The low densities and microporous structures of the new materials may make them useful for applications in medicine, pharmacy, or the food industry, for example.

Molecular dynamics studies of transport properties and equation of state of supercritical fluids

Science.gov (United States)

Nwobi, Obika C.

Many chemical propulsion systems operate with one or more of the reactants above the critical point in order to enhance their performance. Most of the computational fluid dynamics (CFD) methods used to predict these flows require accurate information on the transport properties and equation of state at these supercritical conditions. This work involves the determination of transport coefficients and equation of state of supercritical fluids by equilibrium molecular dynamics (MD) simulations on parallel computers using the Green-Kubo formulae and the virial equation of state, respectively. MD involves the solution of equations of motion of a system of molecules that interact with each other through an intermolecular potential. Provided that an accurate potential can be found for the system of interest, MD can be used regardless of the phase and thermodynamic conditions of the substances involved. The MD program uses the effective Lennard-Jones potential, with system sizes of 1000-1200 molecules and, simulations of 2,000,000 time-steps for computing transport coefficients and 200,000 time-steps for pressures. The computer code also uses linked cell lists for efficient sorting of molecules, periodic boundary conditions, and a modified velocity Verlet algorithm for particle displacement. Particle decomposition is used for distributing the molecules to different processors of a parallel computer. Simulations have been carried out on pure argon, nitrogen, oxygen and ethylene at various supercritical conditions, with self-diffusion coefficients, shear viscosity coefficients, thermal conductivity coefficients and pressures computed for most of the conditions. Results compare well with experimental and the National Institute of Standards and Technology (NIST) values. The results show that the number of molecules and the potential cut-off radius have no significant effect on the computed coefficients, while long-time integration is necessary for accurate determination of the

Solute-matrix and Solute-Solute Interactions during Supercritical Fluid Extraction of Sea Buckthorn Leaves

Czech Academy of Sciences Publication Activity Database

Sajfrtová, Marie; Sovová, Helena

2012-01-01

Roč. 42, SI (2012), s. 1682-1691 E-ISSN 1877-7058. [International Congress of Chemical and Process Engineering CHISA 2012 and 15th Conference PRES 2012 /20./. Prague, 25.08.2012-29.08.2012] R&D Projects: GA TA ČR TA01010578 Institutional support: RVO:67985858 Keywords : supercritical fluid extraction * sea buckthom leaves * solute-solute interaction Subject RIV: CI - Industrial Chemistry, Chemical Engineering

Optical wave microphone measurements of laser ablation of copper in supercritical carbon dioxide

Energy Technology Data Exchange (ETDEWEB)

Mitsugi, Fumiaki, E-mail: mitsugi@cs.kumamoto-u.ac.jp [Graduate School of Science and Technology, Kumamoto University, 2-39-1 Kurokami, Kumamoto 860-8555 (Japan); Ikegami, Tomoaki [Graduate School of Science and Technology, Kumamoto University, 2-39-1 Kurokami, Kumamoto 860-8555 (Japan); Nakamiya, Toshiyuki; Sonoda, Yoshito [Graduate School of Industrial Engineering, Tokai University, 9-1-1 Toroku, Kumamoto 862-8652 (Japan)

2013-11-29

Laser ablation plasma in a supercritical fluid has attracted much attention recently due to its usefulness in forming nanoparticles. Observation of the dynamic behavior of the supercritical fluid after laser irradiation of a solid is necessary for real-time monitoring and control of laser ablation. In this study, we utilized an optical wave microphone to monitor pulsed laser irradiation of a solid in a supercritical fluid. The optical wave microphone works based on Fraunhofer diffraction of phase modulation of light by changes in refractive index. We hereby report on our measurements for pulsed laser irradiation of a Cu target in supercritical carbon dioxide using an optical wave microphone. Photothermal acoustic waves which generated after single pulsed laser irradiation of a Cu target were detectable in supercritical carbon dioxide. The speed of sound around the critical point of supercritical carbon dioxide was clearly slower than that in gas. The optical wave microphone detected a signal during laser ablation of Cu in supercritical carbon dioxide that was caused by shockwave degeneration. - Highlights: • Photothermal acoustic wave in supercritical fluid was observed. • Sound speed around the critical point was slower than that in gas. • Optical wave microphone detected degeneration of a shockwave. • Ablation threshold of a solid in supercritical fluid can be estimated. • Generation of the second shockwave in supercritical phase was suggested.

Supercritical fluid extraction of hops

Directory of Open Access Journals (Sweden)

ZORAN ZEKOVIC

2007-01-01

Full Text Available Five cultivars of hop were extracted by the method of supercritical fluid extraction using carbon dioxide (SFE–CO2 as extractant. The extraction (50 g of hop sample using a CO2 flow rate of 97.725 L/h was done in the two steps: 1. extraction at 150 bar and 40°C for 2.5 h (sample of series A was obtained and, after that, the same sample of hop was extracted in the second step: 2. extraction at 300 bar and 40 °C for 2.5 h (sample of series B was obtained. The Magnum cultivar was chosen for the investigation of the extraction kinetics. For the qualitative and quantitative analysis of the obtained hop extracts, the GC-MS method was used. Two of four themost common compounds of hop aroma (a-humulene and b-caryophyllene were detected in samples of series A. In addition, isomerized a-acids and a high content of b-acids were detected. The a-acids content in the samples of series B was the highest in the extract of the Magnum cultivar (it is a bitter variety of hop. The low contents of a-acids in all the other hop samples resulted in extracts with low a-acids content, i.e., that contents were under the prescribed a-acids content.

Preparation and Characterization of Tripterygium wilfordii Multi-Glycoside Nanoparticle Using Supercritical Anti-Solvent Process

Directory of Open Access Journals (Sweden)

Fengli Chen

2014-02-01

Full Text Available The aim of this study was to prepare nanosized Tripterygium wilfordii multi-glycoside (GTW powders by the supercritical antisolvent precipitation process (SAS, and to evaluate the anti-inflammatory effects. Ethanol was used as solvent and carbon dioxide was used as an antisolvent. The effects of process parameters such as precipitation pressure (15–35 MPa, precipitation temperature (45–65 °C, drug solution flow rates (3–7 mL/min and drug concentrations (10–30 mg/mL were investigated. The nanospheres obtained with mean diameters ranged from 77.5 to 131.8 nm. The processed and unprocessed GTW were characterized by scanning electron microscopy, X-ray diffraction, Fourier-transform infrared spectroscopy and thermal gravimetric analysis. The present study was designed to investigate the beneficial effect of the GTW nanoparticles on adjuvant-induced arthritis in albino rats. The processed and unprocessed GTW were tested against Freund’s complete adjuvant-induced arthritis in rats. Blood samples were collected for the estimation of interleukins (IL-1α, IL-1β and tumor necrosis factor-α (TNF-α. It was concluded that physicochemical properties and anti-inflammatory activity of GTW nanoparticles could be improved by physical modification, such as particle size reduction using supercritical antisolvent (SAS process. Further, SAS process was a powerful methodology for improving the physicochemical properties and anti-inflammatory activity of GTW.

Production of extracts from preserved olives using supercritical CO2 and preliminary evaluation of its polyphenol content

Directory of Open Access Journals (Sweden)

Maria João Cebola

2014-06-01

Full Text Available The supercritical fluid extraction (SFE technique was used to obtain extracts from a sample simulating an olive pomace, obtained from preserved olives. The objective was to achieve the extraction of polyphenolic components from this matrix which is considered a hazardous waste from the production of olive oil. The supercritical fluid used was carbon dioxide and the SFE studies were conducted in two stages, the first at a pressure of 200 bar and 40 ºC and the second stage at 300 bar, 45 ºC and using ethanol as co-solvent. In both cases the SFE was performed for 3 hours. The first stage was carried out to obtain a cleaner matrix and the second step was aimed at the components of interest. The overall mass yield obtained was 5.5 %. Preliminary HPLC screening of the samples obtained and also of the water in which the olives were preserved showed that the polyphenol compounds were mostly in the latter.

Investigations on the elution behaviour of TOPO complexes of uranium and thorium using supercritical fluid chromatography

International Nuclear Information System (INIS)

Kumar, R.; Sivaraman, N.; Srinivasan, T.G.; Vasudeva Rao, P.R.

2004-01-01

In summary uranium and thorium could be separated by supercritical fluid chromatography technique as their TOPO complexes. The elution profiles with pre-complexation of the metal nitrate indicate a better separation than the in-situ complexation. The technique can also be employed for the assay of uranium and thorium at low levels

Evaluation of an amide-based stationary phase for supercritical fluid chromatography

Science.gov (United States)

Borges-Muñoz, Amaris C.; Colón, Luis A.

2017-01-01

A relatively new stationary phase containing a polar group embedded in a hydrophobic backbone (i.e., ACE® C18-amide) was evaluated for use in supercritical fluid chromatography. The amide-based column was compared with columns packed with bare silica, C18 silica, and a terminal-amide silica phase. The system was held at supercritical pressure and temperature with a mobile phase composition of CO2 and methanol as cosolvent. The linear solvation energy relationship model was used to evaluate the behavior of these stationary phases, relating the retention factor of selected probes to specific chromatographic interactions. A five-component test mixture, consisting of a group of drug-like molecules was separated isocratically. The results show that the C18-amide stationary phase provided a combination of interactions contributing to the retention of the probe compounds. The hydrophobic interactions are favorable; however, the electron donating ability of the embedded amide group shows a large positive interaction. Under the chromatographic conditions used, the C18-amide column was able to provide baseline resolution of all the drug-like probe compounds in a text mixture, while the other columns tested did not. PMID:27396487

Injection of Fluids into Supercritical Environments

National Research Council Canada - National Science Library

Oschwald, M

2004-01-01

This paper summarizes and compares the results of systematic research programs at two independent laboratories regarding the injection of cryogenic liquids at subcritical and supercritical pressures...

Modeling of the Kinetics of Supercritical Fluid Extraction of Lipids from Microalgae with Emphasis on Extract Desorption

Directory of Open Access Journals (Sweden)

Helena Sovová

2016-05-01

Full Text Available Microalgae contain valuable biologically active lipophilic substances such as omega-3 fatty acids and carotenoids. In contrast to the recovery of vegetable oils from seeds, where the extraction with supercritical CO2 is used as a mild and selective method, economically viable application of this method on similarly soluble oils from microalgae requires, in most cases, much higher pressure. This paper presents and verifies hypothesis that this difference is caused by high adsorption capacity of microalgae. Under the pressures usually applied in supercritical fluid extraction from plants, microalgae bind a large fraction of the extracted oil, while under extremely high CO2 pressures their adsorption capacity diminishes and the extraction rate depends on oil solubility in supercritical CO2. A mathematical model for the extraction from microalgae was derived and applied to literature data on the extraction kinetics in order to determine model parameters.

Supercritical fluid extraction of uranium for its purification from various yellow cake matrices

International Nuclear Information System (INIS)

Prabhat, Parimal; Rao, Ankita; Tomar, B.S.; Kumar, Pradeep

2016-01-01

Uranium is produced from different uranium ores as crude yellow cake of different chemical composition such as sodium diuranate (SDU), ammonium diuranate (ADU), magnesium diuranate (MDU), high temperature uranium peroxide (HTUP) etc. This depends on nature of ores and ore processing methods, availability of required facilities at processing site and other economic as well as environmental factors. These yellow cakes are further processed to produce pure uranium suitable for fuel fabrication facility by conventional solvent extraction process. Supercritical Fluid Extraction (SFE) is being developed as an alternate method for separation in nuclear fields due to its inherent potential to minimize liquid waste generation and process simplification. In present study, SFE of uranium from various yellowcake of different chemical composition has been carried out. Chemical parameter such as effect of TBP amount on SFE of uranium has been carried out and optimized at 2 ml for 200 mg SDU. Instrumental parameter such as temperature and pressure on SFE of uranium has been optimized at 323 K and 15.2 MPa. Extraction efficiency (%) achieved at optimized condition is 91.45 ± 0.2, 97.01 ± 0.75 and 96.72 ± 0.27 for SDU, MDU and HTUP respectively. Purity of uranium before SFE and after has been compared. Further studies is in progress for better understanding of chemical composition of matrix on SFE of uranium and improving purity of uranium separated from this route. (author)

Recovery of cobalt from spent lithium-ion batteries using supercritical carbon dioxide extraction.

Science.gov (United States)

Bertuol, Daniel A; Machado, Caroline M; Silva, Mariana L; Calgaro, Camila O; Dotto, Guilherme L; Tanabe, Eduardo H

2016-05-01

Continuing technological development decreases the useful lifetime of electronic equipment, resulting in the generation of waste and the need for new and more efficient recycling processes. The objective of this work is to study the effectiveness of supercritical fluids for the leaching of cobalt contained in lithium-ion batteries (LIBs). For comparative purposes, leaching tests are performed with supercritical CO2 and co-solvents, as well as under conventional conditions. In both cases, sulfuric acid and H2O2 are used as reagents. The solution obtained from the supercritical leaching is processed using electrowinning in order to recover the cobalt. The results show that at atmospheric pressure, cobalt leaching is favored by increasing the amount of H2O2 (from 0 to 8% v/v). The use of supercritical conditions enable extraction of more than 95wt% of the cobalt, with reduction of the reaction time from 60min (the time employed in leaching at atmospheric pressure) to 5min, and a reduction in the concentration of H2O2 required from 8 to 4% (v/v). Electrowinning using a leach solution achieve a current efficiency of 96% and a deposit with cobalt concentration of 99.5wt%. Copyright © 2016 Elsevier Ltd. All rights reserved.

Nutritional Quality and Physicochemical Characteristics of Defatted Bovine Liver Treated by Supercritical Carbon Dioxide and Organic Solvent

Science.gov (United States)

Kang, Sung-Won; Kim, Hye-Min; Rahman, M. Shafiur; Kim, Ah-Na; Yang, Han-Sul

2017-01-01

Defatted bovine liver (DBL) is a potential source of protein and minerals. Supercritical carbon dioxide (SC-CO2) and a traditional organic solvent method were used to remove lipid from bovine liver, and the quality characteristics of a control bovine liver (CBL), bovine liver defatted by SC-CO2 (DBLSC-CO2) at different pressures, and bovine liver defatted by organic solvent (DBL-OS) were compared. The DBLSC-CO2 samples had significantly higher (pSC-CO2 than the organic solvent method. SDS-PAGE analysis demonstrated that the CBL and DBLSC-CO2 had protein bands of a similar intensity and area, whereas DBL-OS appeared extremely poor bands or no bands due to the degradation of proteins, particularly in the 50 to 75 kDa and 20 to 25 kDa molecular weight ranges. In addition, DBLSC-CO2 was shown to have superior functional properties in terms of total soluble content, water and oil absorption, and foaming and emulsification properties. Therefore, SC-CO2 treatment offers a nutritionally and environmentally friendly approach for the removal of lipid from high protein food sources. In addition, SC-CO2 may be a better substitute of traditional organic solvent extraction for producing more stable and high quality foods with high-protein, fat-free, and low calorie contents. PMID:28316468

MOLECULAR DESIGN OF COLLOIDS IN SUPERCRITICAL FLUIDS

Energy Technology Data Exchange (ETDEWEB)

Keith P. Johnston

2009-04-06

The environmentally benign, non-toxic, non-flammable fluids water and carbon dioxide (CO2) are the two most abundant and inexpensive solvents on earth. Emulsions of these fluids are of interest in many industrial processes, as well as CO2 sequestration and enhanced oil recovery. Until recently, formation of these emulsions required stabilization with fluorinated surfactants, which are expensive and often not environmentally friendly. In this work we overcame this severe limitation by developing a fundamental understanding of the properties of surfactants the CO2-water interface and using this knowledge to design and characterize emulsions stabilized with either hydrocarbon-based surfactants or nanoparticle stabilizers. We also discovered a new concept of electrostatic stabilization for CO2-based emulsions and colloids. Finally, we were able to translate our earlier work on the synthesis of silicon and germanium nanocrystals and nanowires from high temperatures and pressures to lower temperatures and ambient pressure to make the chemistry much more accessible.

Use of on-line supercritical fluid extraction-supercritical fluid chromatography/tandem mass spectrometry to analyze disease biomarkers in dried serum spots compared with serum analysis using liquid chromatography/tandem mass spectrometry.

Science.gov (United States)

Suzuki, Makoto; Nishiumi, Shin; Kobayashi, Takashi; Sakai, Arata; Iwata, Yosuke; Uchikata, Takato; Izumi, Yoshihiro; Azuma, Takeshi; Bamba, Takeshi; Yoshida, Masaru

2017-05-30

The analytical stability and throughput of biomarker assays based on dried serum spots (DSS) are strongly dependent on the extraction process and determination method. In the present study, an on-line system based on supercritical fluid extraction-supercritical fluid chromatography coupled with tandem mass spectrometry (SFE-SFC/MS/MS) was established for analyzing the levels of disease biomarkers in DSS. The chromatographic conditions were investigated using the ODS-EP, diol, and SIL-100A columns. Then, we optimized the SFE-SFC/MS/MS method using the diol column, focusing on candidate biomarkers of oral, colorectal, and pancreatic cancer that were identified using liquid chromatography (LC)/MS/MS. By using this system, four hydrophilic metabolites and 17 hydrophobic metabolites were simultaneously detected within 15 min. In an experiment involving clinical samples, PC 16:0-18:2/16:1-18:1 exhibited 93.8% sensitivity and 64.3% specificity, whereas PC 17:1-18:1/17:0-18:2 showed 81.3% sensitivity and 92.9% specificity for detecting oral cancer. In addition, assessments of the creatine levels demonstrated 92.3% sensitivity and 78.6% specificity for detecting colorectal cancer. The results of this study indicate that our method has great potential for clinical diagnosis and would be suitable for large-scale screening. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Simultaneous determination of inorganic anions and cations by supercritical fluid chromatography using evaporative light scattering detection.

Science.gov (United States)

Foulon, Catherine; Di Giulio, Pauline; Lecoeur, Marie

2018-01-26

Supercritical fluid chromatography (SFC) is commonly used for the analysis of non-polar compounds, but remains poorly explored for the separation of polar and ionized molecules. In this paper, SFC has been investigated for the separation of 14 inorganic ions sampled in aqueous solutions. Four polar stationary phases were first screened using CO 2 -methanol-based mobile phases containing water or different acidic or basic additives, in order to select the most efficient conditions for the simultaneous retention of inorganic cations and anions and to favor their detection using evaporative light scattering detector (ELSD). Orthogonal selectivity was obtained depending on the stationary phase used: whereas anions are less retained on HILIC stationary phase, 2-ethylpyridine (2-EP) stationary phase exhibits strong interaction for anions. Best results were obtained under gradient elution mode using a 2-EP stationary phase and by adding 0.2% triethylamine in the CO 2 -methanol-based mobile phase. The composition of the injection solvent was also investigated. The results showed that a methanolic sample containing a percentage of water not exceeding 20% does not affect the analytical performances obtained on 2-EP. Moreover, the presence of triethylamine in the injection solvent contributes to eliminate peaks shoulders. Among the 14 inorganic ions tested, three cations (Li + , Ca 2+ and Mg 2+ ) and five anions (Cl - , Br - , NO 3 - , I - , SCN - ) were totally resolved in 15 min. NO 3 - and NO 2 - still coeluted in the final optimized conditions. The other investigated ions were either strongly retained on the stationary phase or not detected by the ELSD. Copyright © 2017 Elsevier B.V. All rights reserved.

Supercritical Synthesis of Biodiesel

Directory of Open Access Journals (Sweden)

Michel Vaultier

2012-07-01

Full Text Available The synthesis of biodiesel fuel from lipids (vegetable oils and animal fats has gained in importance as a possible source of renewable non-fossil energy in an attempt to reduce our dependence on petroleum-based fuels. The catalytic processes commonly used for the production of biodiesel fuel present a series of limitations and drawbacks, among them the high energy consumption required for complex purification operations and undesirable side reactions. Supercritical fluid (SCF technologies offer an interesting alternative to conventional processes for preparing biodiesel. This review highlights the advances, advantages, drawbacks and new tendencies involved in the use of supercritical fluids (SCFs for biodiesel synthesis.

Supercritical heat transfer phenomena in nuclear system

International Nuclear Information System (INIS)

Seo, Kyoung Woo; Kim, Moo Hwan; Anderson, Mark H.; Corradini, Michael L.

2005-01-01

A supercritical water (SCW) power cycle has been considered as one of the viable candidates for advanced fission reactor designs. However, the dramatic variation of thermo-physical properties with a modest change of temperature near the pseudo-critical point make existing heat transfer correlations such as the Dittus-Boelter correlation not suitably accurate to calculate the heat transfer in supercritical fluid. Several other correlations have also been suggested but none of them are able to predict the heat transfer over a parameter range, needed for reactor thermal-hydraulics simulation and design. This has prompted additional research to understand the characteristic of supercritical fluid heat transfer

Hydrogenation of Anthracene in Supercritical Carbon Dioxide Solvent Using Ni Supported on Hβ-Zeolite Catalyst

Directory of Open Access Journals (Sweden)

Ashraf Aly Hassan

2012-01-01

Full Text Available Catalytic hydrogenation of anthracene was studied over Ni supported on Hβ-zeolite catalyst under supercritical carbon dioxide (sc-CO2 solvent. Hydrogenation of anthracene in sc-CO2 yielded 100% conversion at 100 °C, which is attributed to the reduced mass transfer limitations, and increased solubility of H2 and substrate in the reaction medium. The total pressure of 7 MPa was found to be optimum for high selectivity of octahydroanthracene (OHA. The conversion and selectivity for OHA increased with an increase in H2 partial pressure, which is attributed to higher concentration of hydrogen atoms at higher H2 pressures. The selectivity reduced the pressure below 7 MPa because of enhanced desorption of the tetrahydro-molecules and intermediates from Ni active sites, due to higher solubility of the surface species in sc-CO2. The selectivity of OHA increased with the increase in catalyst weight and reaction time. The rate of hydrogenation of anthracene was compared with that found for napthalene and phenanthrene. The use of acetonitrile as co-solvent or expanded liquid with CO2 decreased the catalytic activity.

Exploring a multi-scale method for molecular simulation in continuum solvent model: Explicit simulation of continuum solvent as an incompressible fluid.

Science.gov (United States)

Xiao, Li; Luo, Ray

2017-12-07

We explored a multi-scale algorithm for the Poisson-Boltzmann continuum solvent model for more robust simulations of biomolecules. In this method, the continuum solvent/solute interface is explicitly simulated with a numerical fluid dynamics procedure, which is tightly coupled to the solute molecular dynamics simulation. There are multiple benefits to adopt such a strategy as presented below. At this stage of the development, only nonelectrostatic interactions, i.e., van der Waals and hydrophobic interactions, are included in the algorithm to assess the quality of the solvent-solute interface generated by the new method. Nevertheless, numerical challenges exist in accurately interpolating the highly nonlinear van der Waals term when solving the finite-difference fluid dynamics equations. We were able to bypass the challenge rigorously by merging the van der Waals potential and pressure together when solving the fluid dynamics equations and by considering its contribution in the free-boundary condition analytically. The multi-scale simulation method was first validated by reproducing the solute-solvent interface of a single atom with analytical solution. Next, we performed the relaxation simulation of a restrained symmetrical monomer and observed a symmetrical solvent interface at equilibrium with detailed surface features resembling those found on the solvent excluded surface. Four typical small molecular complexes were then tested, both volume and force balancing analyses showing that these simple complexes can reach equilibrium within the simulation time window. Finally, we studied the quality of the multi-scale solute-solvent interfaces for the four tested dimer complexes and found that they agree well with the boundaries as sampled in the explicit water simulations.

Stability analysis of a heated channel cooled by supercritical water

International Nuclear Information System (INIS)

Magni, M. C.; Delmastro, D. F; Marcel, C. P

2009-01-01

A simple model to study thermal-hydraulic stability of a heated cannel under supercritical conditions is presented. Single cannel stability analysis for the SCWR (Supercritical Water Cooled Reactor) design was performed. The drastic change of fluid density in the reactor core of a SCWR may induce DWO (Density Wave Oscillations) similar to those observed in BWRs. Due to the similarities between subcritical and supercritical systems we may treat the supercritical fluid as a pseudo two-phase system. Thus, we may extend the modeling approach often used for boiling flow stability analysis to supercritical pressure operation conditions. The model developed in this work take into account three regions: a heavy fluid region, similar to an incompressible liquid; a zone where a heavy fluid and a light fluid coexist, similar to two-phase mixture; and a light fluid region which behaves like superheated steam. It was used the homogeneous equilibrium model (HEM) for the pseudo boiling zone, and the ideal gas model for the pseudo superheated steam zone. System stability maps were obtained using linear stability analysis in the frequency domain. Two possible instability mechanisms are observed: DWO and excursive Ledinegg instabilities. Also, a sensitivity analysis showed that frictions in pseudo superheated steam zone, together with acceleration effect, are the most destabilizing effects. On the other hand, frictions in pseudo liquid zone are the most important stabilizing effect. [es

Comparison of supercritical fluid and Soxhlet extractions for the quantification of hydrocarbons from Euphorbia macroclada.

Science.gov (United States)

Ozcan, Adnan; Ozcan, Asiye Safa

2004-10-08

This study compares conventional Soxhlet extraction and analytical scale supercritical fluid extraction (SFE) for their yields in extracting of hydrocarbons from arid-land plant Euphorbia macroclada. The plant material was firstly sequentially extracted with supercritical carbon dioxide, modified with 10% methanol (v/v) in the optimum conditions that is a pressure of 400atm and a temperature of 50 degrees C and then it was sonicated in methylene chloride for an additional 4h. E. macroclada was secondly extracted by using a Soxhlet apparatus at 30 degrees C for 8h in methylene chloride. The validated SFE was then compared to the extraction yield of E. macroclada with a Soxhlet extraction by using the Student's t-test at the 95% confidence level. All of extracts were fractionated with silica-gel in a glass column to get better hydrocarbon yields. Thus, the highest hydrocarbons yield from E. macroclada was achieved with SFE (5.8%) when it compared with Soxhlet extractions (1.1%). Gas chromatography (GC) analysis was performed to determine the quantitative hydrocarbons from plant material. The greatest quantitative hydrocarbon recovery from GC was obtained by supercritical carbon dioxide extract (0.6mgg(-1)).

Functionalization of whey proteins by reactive supercritical fluid extrusion

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Khanitta Ruttarattanamongkol

2012-09-01

Full Text Available Whey protein, a by-product from cheese-making, is often used in a variety of food formulations due to its unsurpassednutritional quality and inherent functional properties. However, the possibilities for the improvement and upgrading of wheyprotein utilization still need to be explored. Reactive supercritical fluid extrusion (SCFX is a novel technique that has beenrecently reported to successfully functionalize commercially available whey proteins into a product with enhanced functionalproperties. The specific goal of this review is to provide fundamental understanding of the reinforcement mechanism andprocessing of protein functionalization by reactive SCFX process. The superimposed extrusion variables and their interactionmechanism affect the physico-chemical properties of whey proteins. By understanding the structure, functional properties andprocessing relationships of such materials, the rational design criteria for novel functionalized proteins could be developedand effectively utilized in food systems.

Simultaneous analysis of nucleobases, nucleosides and ginsenosides in ginseng extracts using supercritical fluid chromatography coupled with single quadrupole mass spectrometry.

Science.gov (United States)

Huang, Yang; Zhang, Tingting; Zhao, Yumei; Zhou, Haibo; Tang, Guangyun; Fillet, Marianne; Crommen, Jacques; Jiang, Zhengjin

2017-09-10

Nucleobases, nucleosides and ginsenosides, which have a significant impact on the physiological activity of organisms, are reported to be the active components of ginseng, while they are less present in ginseng extracts. Few analytical methods have been developed so far to simultaneously analyze these three classes of compounds with different polarities present in ginseng extracts. In the present study, a simple and efficient analytical method was successfully developed for the simultaneous separation of 17 nucleobases, nucleosides and ginsenosides in ginseng extracts using supercritical fluid chromatography coupled with single quadrupole mass spectrometry (SFC-MS). The effect of various experimental factors on the separation performance, such as the column type, temperature and backpressure, the type of modifier and additive, and the concentration of make-up solvent were systematically investigated. Under the selected conditions, the developed method was successfully applied to the quality evaluation of 14 batches of ginseng extracts from different origins. The results obtained for the different batches indicate that this method could be employed for the quality assessment of ginseng extracts. Copyright © 2017 Elsevier B.V. All rights reserved.

Supercritical fluid chromatography applied to the highly selective isolation of urinary steroid hormones prior to GC/MS analysis.

Science.gov (United States)

Doué, Mickael; West, Caroline; Bichon, Emmanuelle; Le Bizec, Bruno; Lesellier, Eric

2018-06-01

To assess the presence of prohibited anabolic substances used to promote growth in livestock, calf urine is the most relevant matrix. However, the sample preparation methods (required to remove unwanted matrix components and fractionate isobaric species that may be unresolved by gas chromatography- mass spectrometry GC/MS) are long and complex. In this context, semi-preparative supercritical fluid chromatography (SFC) was considered to possibly simplify the sample preparation in reducing the number of procedures. Fifteen stationary phases were screened with SFC combined with UV and evaporative light-scattering detection (ELSD), among which two columns (Cosmosil π-NAP and Princeton DIOL) were retained for their ability to isolate steroid hormones from other matrix components and, for the second column, for the additional possibility to fractionate steroid hormones into different families (estrogens, mono-hydroxylated and di-hydroxylated androgens). The fractions were further analysed with GC/MS showing the benefit of class fractionation. The final method allows for significant time, solvent and money savings compared to the previously widely used method (solid-phase extraction combined with semi-preparative high-performance liquid chromatography). Copyright © 2018 Elsevier B.V. All rights reserved.

Thermodynamic Aspects of Supercritical Fluids Processing: Applications of Polymers and Wastes Treatment Aspects thermodynamiques des procédés mettant en oeuvre des fluides supercritiques : applications aux traitements des polymères et des déchets

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Beslin P.

2006-11-01

Full Text Available Supercritical fluid processes are of increasing interest for many fields : in supercritical fluid separation (petroleum-chemistry separation and purification, food industry and supercritical fluid chromatography (analytical and preparative separation, determination of physicochemical properties; as reaction media with continuously adjustable properties from gas to liquid (low-density polyethylene, waste destruction, polymer recycling; in geology and mineralogy (volcanoes, geothermal energy, hydrothermal synthesis; in particle, fibber and substrate formations (pharmaceuticals, explosives, coatings; in drying materials (gels. This paper presents the unusual physicochemical properties of supercritical fluids in relation to their engineering applications. After a short report of fundamental concepts of critical behavior in pure fluids, we develop in more details the tunable physicochemical properties of fluid in the supercritical domain. The second part of this paper describes the engineering applications of supercritical fluids relevant of chemical reactions and polymer processing. Each application presentation is divided in two parts : the first one recalls the basic concepts including general background, physicochemical properties and the second one develops the engineering applications relevant of the advocated domain. La mise en Suvre des fluides supercritiques est d'un intérêt croissant dans de nombreux domaines : pour la séparation (séparation et purification en pétrochimie, industrie alimentaire et la chromatographie par fluides supercritiques (séparation analytique et préparatoire, détermination des propriétés physicochimiques, comme milieux réactifs aux propriétés continûment ajustables allant du gaz au liquide (polyéthylène de faible densité, élimination des déchets, recyclage des polymères, en géologie et en minéralogie (volcanologie, énergie géothermique, synthèse hydrothermique, dans la formation des particules

Fluidos supercríticos em química analítica. II. Cromatografia com fluido supercrítico: instrumentação Supercritical fluid in analytical chemistry. II. Supercritical fluid chromatography: instrumentation

Directory of Open Access Journals (Sweden)

Emanuel Carrilho

2003-10-01

Full Text Available The first paper in this series discussed the basic theory involved in supercritical fluid chromatography (SFC and how the technique progressed from gas and liquid chromatography. The first SFC instruments were simple adaptations of the commercially available liquid chromatographs with packed columns followed by modifications in gas chromatographs using open tubular capillary columns. In this paper, the most important aspects regarding instrumentation are covered, including practical, simple, and the most important, inexpensive solutions to build a home-made SFC system.

Chiral separation of a diketopiperazine pheromone from marine diatoms using supercritical fluid chromatography.

Science.gov (United States)

Frenkel, Johannes; Wess, Carsten; Vyverman, Wim; Pohnert, Georg

2014-03-01

The proline derived diketopiperazine has been identified in plants, insects and fungi with unknown function and was recently also reported as the first pheromone from a diatom. Nevertheless the stereochemistry and enantiomeric excess of this natural product remained inaccessible using direct analytical methods. Here we introduce a chiral separation of this metabolite using supercritical fluid chromatography/mass spectrometry. Several chromatographic methods for chiral analysis of the diketopiperazine from the diatom Seminavis robusta and synthetic enantiomers have been evaluated but neither gas chromatography nor high performance liquid chromatography on different chiral cyclodextrin phases were successful in separating the enantiomers. In contrast, supercritical fluid chromatography achieved baseline separation within four minutes of run time using amylose tris(3,5-dimethylphenylcarbamate) as stationary phase and 2-propanol/CO2 as mobile phase. This very rapid chromatographic method in combination with ESI mass spectrometry allowed the direct analysis of the cyclic dipeptide out of the complex sea water matrix after SPE enrichment. The method could be used to determine the enantiomeric excess of freshly released pheromone and to follow the rapid degradation observed in diatom cultures. Initially only trace amounts of c(d-Pro-d-Pro) were found besides the dominant c(l-Pro-l-Pro) in the medium. However the enantiomeric excess decreased upon pheromone degradation within few hours indicating that a preferential conversion and thus inactivation of the l-proline derived natural product takes place. Copyright © 2014 Elsevier B.V. All rights reserved.

Nitrate conversion and supercritical fluid extraction of UO2-CeO2 solid solution prepared by an electrolytic reduction-coprecipitation method

International Nuclear Information System (INIS)

Zhu, L.Y.; Duan, W.H.; Wen, M.F.; Xu, J.M.; Zhu, Y.J.

2014-01-01

A low-waste technology for the reprocessing of spent nuclear fuel (SNF) has been developed recently, which involves the conversion of actinide and lanthanide oxides with liquid N 2 O 4 into their nitrates followed by supercritical fluid extraction of the nitrates. The possibility of the reprocessing of SNF from high-temperature gas-cooled reactors (HTGRs) with nitrate conversion and supercritical fluid extraction is a current area of research in China. Here, a UO 2 -CeO 2 solid solution was prepared as a surrogate for a UO 2 -PuO 2 solid solution, and the recovery of U and Ce from the UO 2 -CeO 2 solid solution with liquid N 2 O 4 and supercritical CO 2 containing tri-n-butyl phosphate (TBP) was investigated. The UO 2 -CeO 2 solid solution prepared by electrolytic reduction-coprecipitation method had square plate microstructures. The solid solution after heat treatment was completely converted into nitrates with liquid N 2 O 4 . The XRD pattern of the nitrates was similar to that of UO 2 (NO 3 ) 2 . 3H 2 O. After 120 min of online extraction at 25 MPa and 50 , 99.98% of the U and 98.74% of the Ce were recovered from the nitrates with supercritical CO 2 containing TBP. The results suggest a promising potential technology for the reprocessing of SNF from HTGRs. (orig.)

Phase behaviour of sterols and vitamins in supercritical CO2

Directory of Open Access Journals (Sweden)

Gerszt R.

2000-01-01

Full Text Available Extraction with supercritical solvents has been used in different areas, such as petroleum desasphaltation, descaffeination of coffee and tea and in the separation of other types of natural products. The supercritical solvent most frequently utilized in the extraction of natural products is carbon dioxide (CO2 due to its several advantages over other solvents such as low cost, atoxicity and volatility. The design, evaluation and optimization of a supercritical extraction that is based on phase equilibrium require phase equilibrium data. This type of data is very scarce for natural compounds like sterols and vitamins. These natural compounds are produced synthetically, but nowadays interest in their extraction from natural sources is increasing. Therefore, the objective of this work is to study the thermodynamic modelling equilibrium of systems containing vitamins A, D, E and K, using the predictive LCVM model. The sensitivity of critical properties in the calculation of the phase behavior was also studied. This study proved that the choice of a group contribution method to calculate thermodynamic properties is very important for obtaining good results in the phase equilibrium calculations.

Effects of Gravity on Supercritical Water Oxidation (SCWO) Processes

Science.gov (United States)

Hegde, Uday; Hicks, Michael

2013-01-01

The effects of gravity on the fluid mechanics of supercritical water jets are being studied at NASA to develop a better understanding of flow behaviors for purposes of advancing supercritical water oxidation (SCWO) technologies for applications in reduced gravity environments. These studies provide guidance for the development of future SCWO experiments in new experimental platforms that will extend the current operational range of the DECLIC (Device for the Study of Critical Liquids and Crystallization) Facility on board the International Space Station (ISS). The hydrodynamics of supercritical fluid jets is one of the basic unit processes of a SCWO reactor. These hydrodynamics are often complicated by significant changes in the thermo-physical properties that govern flow behavior (e.g., viscosity, thermal conductivity, specific heat, compressibility, etc), particularly when fluids transition from sub-critical to supercritical conditions. Experiments were conducted in a 150 ml reactor cell under constant pressure with water injections at various flow rates. Flow configurations included supercritical jets injected into either sub-critical or supercritical water. Profound gravitational influences were observed, particularly in the transition to turbulence, for the flow conditions under study. These results will be presented and the parameters of the flow that control jet behavior will be examined and discussed.

Processing of novel bioactive polymeric matrixes for tissue engineering using supercritical fluid technology

Energy Technology Data Exchange (ETDEWEB)

Duarte, Ana Rita C., E-mail: aduarte@dep.uminho.pt [3B' s Research Group, Biomaterials, Biodegradables and Biomimetics, University of Minho, Headquarters of the European Institute of Excellence on Tissue Engineering and Regenerative Medicine, AvePark, 4806-909 Taipas, Guimaraes (Portugal); IBB, Institute for Biotechnology and Bioengineering, PT Government Associated Laboratory, Guimaraes (Portugal); Caridade, Sofia G.; Mano, Joao F.; Reis, Rui L. [3B' s Research Group, Biomaterials, Biodegradables and Biomimetics, University of Minho, Headquarters of the European Institute of Excellence on Tissue Engineering and Regenerative Medicine, AvePark, 4806-909 Taipas, Guimaraes (Portugal); IBB, Institute for Biotechnology and Bioengineering, PT Government Associated Laboratory, Guimaraes (Portugal)

2009-08-31

The aim of this study was to develop a new process for the production of bioactive 3D scaffolds using a clean and environmentally friendly technology. The possibility of preparing composite scaffolds of Bioglass and a polymeric blend of starch and poly(L-lactic acid) (SPLA50) was evaluated. Supercritical phase-inversion technique was used to prepare inorganic particles loaded starch-based porous composite matrixes in a one-step process for bone tissue engineering purposes. Due to their osteoconductive properties some glasses and ceramics are interesting materials to be used for bone tissue engineering purposes; however their poor mechanical properties create the need of a polymeric support where the inorganic fraction can be dispersed. Samples impregnated with different concentrations of Bioglass (10 and 15% wt/wt polymer) were prepared at 200 bar and 55 deg. C. The presence of Bioglass did not affect the porosity or interconnectivity of the polymeric matrixes. Dynamic mechanical analysis has proven that the modulus of the SPLA50 scaffolds increases when glass particles are impregnated within the matrix. In vitro bioactivity studies were carried out using simulated body fluid and the results show that a calcium-phosphate layer started to be formed after only 1 day of immersion. Chemical analysis of the apatite layer formed on the surface of the scaffold was performed by different techniques, namely EDS and FTIR spectroscopy and X-ray diffraction (XRD). The ion concentration in the simulated body fluid was also carried out by ICP analysis. Results suggest that a bone-like apatite layer was formed. This study reports the feasibility of using supercritical fluid technology to process, in one step, a porous matrix loaded with a bioactive material for tissue engineering purposes.

Updated heat transfer correlations for supercritical water-cooled reactor applications

International Nuclear Information System (INIS)

Mokry, S.J.; Pioro, I.L.; Farah, A.; King, K.

2011-01-01

In support of the development of SuperCritical Water-cooled Reactors (SCWRs), research is currently being conducted for heat-transfer at supercritical conditions. Currently, there are no experimental datasets for heat transfer from power reactor fuel bundles to the fuel coolant (Water) available in open literature. Therefore, for preliminary calculations, heat-transfer correlations obtained with bare tube data can be used as a conservative approach. A large set of experimental data, for supercritical water was analyzed and an updated heat-transfer correlation for forced-convective heat-transfer, in the normal heat transfer regime, was developed. This experimental dataset was obtained within conditions similar to those for proposed SCWR concepts. Thus, this new correlation can be used for preliminary heat-transfer calculations in SCWR fuel channels. It has demonstrated a good fit for the analyzed dataset. Experiments with SuperCritical Water (SCW) are very expensive. Therefore, a number of experiments are performed in modeling fluids, such as carbon dioxide and refrigerants. However, there is no common opinion if SC modeling fluids' correlations can be applied to SCW and vice versa. Therefore, a correlation for supercritical carbon dioxide heat transfer was developed as a less expensive alternative to using supercritical water. The conducted analysis also meets the objective of improving our fundamental knowledge of the transport processes and handling of supercritical fluids. These correlations can be used for supercritical water heat exchangers linked to indirect-cycle concepts and the cogeneration of hydrogen, for future comparisons with other independent datasets, with bundle data, for the verification of computer codes for SCWR core thermalhydraulics and for the verification of scaling parameters between water and modeling fluids. (author)

A rapid supercritical fluid extraction method for the qualitative detection of 2-alkylcyclobutanones in gamma-irradiated fresh and sea water fish

International Nuclear Information System (INIS)

Tewfik, I.H.; Ismail, H.M.; Sumar, S.

1999-01-01

2-Alkylcyclobutanones are routinely used as chemical markers for irradiated foods containing lipids. However, current extraction procedures (soxhlet-Florisil chromatography) for the isolation of these markers involve a long and tedious clean-up regime prior to GC-MS identification. A simple and rapid method for the isolation of these markers using carbon dioxide as a super critical fluid is described for low lipid content fish samples (fresh and sea water) irradiated up to 8kGy. The presence of 2-dodecylcyclobutanone (2-DCB), a radiolytic marker, was confirmed in all irradiated fish samples at all doses. This was a clear indication that the fish samples had been irradiated and that both methods of isolation (florisil and supercritical fluid extraction) were capable of qualitatively extracting this marker. Supercritical fluid extraction is proposed as an alternative extraction procedure to the florisil chromatography method currently in use and has the added advantage of a considerably shorter extraction time

Reaction of phosphorus ylides with carbonyl compounds in supercritical carbon dioxide

International Nuclear Information System (INIS)

Jeong, Kyung Il; Kim, Hak Do; Shim, Jae Jin; Ra, Choon Sup

2004-01-01

The condensation reaction of (benzylene)triphenylphosphoranes with carbonyl compounds in supercritical carbon dioxide was examined. Reactions of (benzylene)phosphoranes (ca. 1 mmol) with several benzaldehydes in a supercritical carbon dioxide (80 .deg. C, 2,000 psi) containing THF entrainer (5%) in a 24 mL reactor proceed smoothly to yield olefination products in fairly good to excellent yields but slower, compared to reactions in a conventional THF solvent. Generally, phosphoranes that are not substituted with a nitro group show more (Z)-selective reactions with aromatic aldehydes under scCO 2 condition than in THF. The reaction of (benzylene)triphenylphosphosphoranes with 4-t-butylcyclohexanone gave the corresponding olefin compounds with a low conversion under both the supercritical carbon dioxide and the organic THF solvent. Our preliminary study showed the Wittig reaction carries out smoothly in supercritical carbon dioxide medium and also a possible tunability of this reaction pathway by adding a entrainer. The results would be useful for devising a novel process for the environmentally friendly Wittig reaction

Supercritical Algal Extracts: A Source of Biologically Active Compounds from Nature

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Izabela Michalak

2015-01-01

Full Text Available The paper discusses the potential applicability of the process of supercritical fluid extraction (SFE in the production of algal extracts with the consideration of the process conditions and yields. State of the art in the research on solvent-free isolation of biologically active compounds from the biomass of algae was presented. Various aspects related with the properties of useful compounds found in cells of microalgae and macroalgae were discussed, including their potential applications as the natural components of plant protection products (biostimulants and bioregulators, dietary feed and food supplements, and pharmaceuticals. Analytical methods of determination of the natural compounds derived from algae were discussed. Algal extracts produced by SFE process enable obtaining a solvent-free concentrate of biologically active compounds; however, detailed economic analysis, as well as elaboration of products standardization procedures, is required in order to implement the products in the market.

Preliminary Design and Computational Fluid Dynamics Analysis of Supercritical Carbon Dioxide Turbine Blade

International Nuclear Information System (INIS)

Jeong, Wi S.; Kim, Tae W.; Suh, Kune Y.

2007-01-01

The supercritical gas turbine Brayton cycle has been adopted in the secondary loop of the Generation IV Nuclear Energy Systems, and planned to be installed in power conversion cycles of the nuclear fusion reactors as well. The supercritical carbon dioxide (SCO 2 ) is one of widely considered fluids for this concept. The potential beneficiaries include the Secure Transportable Autonomous Reactor- Liquid Metal (STAR-LM), the Korea Advanced Liquid Metal Reactor (KALIMER) and Battery Omnibus Reactor Integral System (BORIS) which is being developed at the Seoul National University. The reason for these welcomed applications is that the SCO 2 Brayton cycle can achieve higher overall energy conversion efficiency than the steam turbine Rankine cycle. Seoul National University has recently been working on the SCO 2 based Modular Optimized Brayton Integral System (MOBIS). The MOBIS design power conversion efficiency is about 45%. Gas turbine design is crucial part in achieving this high efficiency. In this paper, the preliminary analysis on first stage of gas turbine was performed using CFX as a solver

Molecular theory of chromatography for blocklike solutes in isotropic stationary phases and its application to supercritical fluid chromatographic retention of PAHs

International Nuclear Information System (INIS)

Chao Yan; Martire, D.E.

1992-01-01

This report discusses a molecular theory of chromatography for blocklike solutes in isotropic stationary phases as an extension to the anisotopic phase approach. Its it applied to gas, liquid, and supercritical fluid chromatography

Quality Parameters of Curcuma Longa L. Extracts by Supercritical Fluid Extraction (SFE) and Ultrasonic Assisted Extraction (UAE)

International Nuclear Information System (INIS)

Zaibunnisa Abdul Haiyee; Siti Hafsah Mohd Shah; Khudzir Ismail; Nooraain Hashim; Wan Iryani Wan Ismail

2016-01-01

Turmeric is one of the prominently use herbal plants due to its diverse beneficial effects especially in Indian medicine. The rhizome part of the turmeric contains valuable compounds which have been said to owe its antimicrobial effects, anti-cancer, anti-inflammatory and enhance wound healing. Due to its short-life span and perishable properties, the conversion of the rhizome into turmeric extract is desirable. Several methods have been used for extraction such as Soxhlet extraction and pressurized liquid extraction (PLE). However, these techniques are tedious, laborious, time consuming and involves the usage of toxic organic solvent, of which safeness of the end product is doubtful. In this study, a rapid, reliable and green extraction method of supercritical fluid extraction (SFE) and ultrasonic assisted extraction (UAE) were used. SFE without modifier has resulted in 0.0006 mg/ 100 g of curcuminoids concentration and 5.62 % of yield (dry weight basis). UAE using ethanol was able to produce significantly the highest yield (6.40 %, dry weight basis) and the highest curcuminoids concentration (0.1020 mg/ 100 g). However, SFE was able to produce extract that contain significantly higher major volatile compounds; tumerone, ar-turmerone and curlone. Therefore, this study proves that both extraction methods were able to produce high quality turmeric extract. (author)

Plastic reactor suitable for high pressure and supercritical fluid electrochemistry

DEFF Research Database (Denmark)

Branch, Jack; Alibouri, Mehrdad; Cook, David A.

2017-01-01

The paper describes a reactor suitable for high pressure, particularly supercritical fluid, electrochemistry and electrodeposition at pressures up to 30 MPa at 115◦C. The reactor incorporates two key, new design concepts; a plastic reactor vessel and the use of o-ring sealed brittle electrodes...... by the deposition of Bi. The application of the reactor to the production of nanostructures is demonstrated by the electrodeposition of ∼80 nm diameter Te nanowires into an anodic alumina on silicon template. Key advantages of the new reactor design include reduction of the number of wetted materials, particularly...... glues used for insulating electrodes, compatability with reagents incompatible with steel, compatability with microfabricated planar multiple electrodes, small volume which brings safety advantages and reduced reagent useage, and a significant reduction in experimental time....

Krichevskii parameters of heavy n-alkanes in carbon dioxide: comparison of the results from solubility measurements and from supercritical fluid chromatography

Czech Academy of Sciences Publication Activity Database

Roth, Michal

2003-01-01

Roč. 212, 1-2 (2003), s. 1-9 ISSN 0378-3812 R&D Projects: GA ČR GA203/02/1093; GA ČR GA203/02/0023 Institutional research plan: CEZ:AV0Z4031919 Keywords : dilute solution in supercritical solvent * partial molar volume * cubic equation of state Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 1.165, year: 2003

Application des fluides supercritiques à la production d'hydrocarbures. Exploitation des gisements par récupération assistée et applications diverses : pétrole, sables, schistes, charbons Application of Supercritical Fluids to Hydrocarbon Production. Enhanced Oi Recovery and Miscellaneous Applications: Oil, Tar Sands, Shales, Coals

Directory of Open Access Journals (Sweden)

Behar E.

2006-11-01

dioxide. This article briefly describes the ranges of application and the thermodynamic mechanisms involved. Sources of available supercritical fluids in the vicinity of oil fields are quickly reviewed together with various operational problems. In addition to being used for enhanced recovery, supercritical fluids are also involved in various refining and extraction processes. The first industrial application was the process for deasphalting heavy petroleum fractions in 1956, making use of the great variations in the solvent power of a fluid in the vicinity of its critical point. This process has received revived interest in recent years because of the energy saving it entails. Likewise, oil shales, tar sands and coals, which are appreciable hydrocarbon sources for the future, are fields of potential applications for supercritical fluids. Specific processes are reviewed, most of which are undergoing pilot-plant development.

Supercritical CO2 extraction of raw propolis and its dry ethanolic extract

Directory of Open Access Journals (Sweden)

L. C. Paviani

2012-06-01

Full Text Available Three types of propolis extract were prepared and analyzed with respect to their global extraction yields and with respect to the concentration of the following markers: 3,5-diprenyl-4-hydroxycinnamic acid; 3-prenyl-4-hydroxycinnamic acid; 4-hydroxycinnamic acid and 4-methoxy-3,5,7-trihydroxyflavone. The extract EEP (ethanolic extract of propolis was obtained by the conventional method from raw propolis using ethanol as solvent. The extracts (SFE were obtained by supercritical solvent extraction from the raw propolis using supercritical carbon dioxide (sc-CO2, with and without the addition of ethanol as a co-solvent. The fractionated supercritical extracts (FSCE were obtained by fractionation (extract and raffinate of the dry EEP with sc-CO2. EEP yields of 39.5% were obtained and maximum global extraction yields were 7.3% for SFE with no co-solvent, 51% for SFE with 15% ethanol and 18% for the FSCE extract fraction. The concentrations of the markers in the different extracts differed as a function of the operational parameters, indicating that the addition of co-solvent and the selectivity of sc-CO2 could be manipulated so as to obtain extracts with the yields and concentrations of interest.

Formation of salbutamol sulphate microparticles using solution enhanced dispersion by supercritical carbon dioxide

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Abdolhossein Rouholamini Najafabadi

2005-01-01

Full Text Available Salbutamol sulphate (SS was precipitated by supercritical carbon dioxide (SC-CO2 using a homemade system at two different pressures. This process is characterized by spraying a methanolic solution of the drug into the supercritical fluid (SCF, extraction of the solvent by SC-CO2 and formation of drug particles. The morphology and size distribution of precipitated SS particles were characterized using scanning electron microscope and laser diffraction particle size analyzer respectively. FTIR spectra were used before and after processing to asses crystal modifications. Depending on the processing conditions, needle-like and flake-like particles with different size distributions were observed. The average size of the flake like particles was less than needle-like particles and the span parameter showed a narrower size distribution of the processed in comparison with the unprocessed materials. Analysis by FTIR showed that there was no significant effect on the structure of the drug under these processing conditions.

Modeling of mass transfer of Phospholipids in separation process with supercritical CO2 fluid by RBF artificial neural networks

Science.gov (United States)

An artificial Radial Basis Function (RBF) neural network model was developed for the prediction of mass transfer of the phospholipids from canola meal in supercritical CO2 fluid. The RBF kind of artificial neural networks (ANN) with orthogonal least squares (OLS) learning algorithm were used for mod...

Quantitative aspects of directly coupled supercritical fluid extraction-capillary gas chromatography with a conventional split/splitless injector as interface

NARCIS (Netherlands)

Lou, X.W.; Janssen, J.G.M.; Cramers, C.A.

1993-01-01

The quant. aspects of online supercrit. fluid extn.-capillary gas chromatog. (SFE-GC) with a split/splitless injector as interface were studied. Special attention was paid to the discrimination behavior and the reproducibility of the split/splitless interface. A simple exptl. set-up is proposed that

Remedial action of matrices contaminated by cobalt with supercritical CO_2: contribution to the understanding of the complex formation mechanisms and to the diphasic transfers

International Nuclear Information System (INIS)

Gervais, Florence

2001-01-01

Soils rehabilitation using supercritical CO_2 seems an interesting alternative way to existing techniques. No effluents are generated during the supercritical fluid extraction, which is the main advantage of this process. In order to be extracted by this techniques, metals or radionuclides have to be complexed by suitable chelating agents. Beta-diketones and dithiocarbamates (fluorinated or not) have been chosen. The first part of this work deals with chemical equilibria mechanisms study in an aqueous phase. Experiments show a very weak cobalt complexation kinetics with acetylacetone. Moreover, this complex exhibit a hydrophilic behaviour. On the other hand, cobalt and dithiocarbamate instantaneously from a chelate which is very hydrophobic. Mass transfer between extracting and aqueous phases (hexane and SC CO_2) are also investigated. Supercritical CO_2 seems to have a greater affinity towards fluorinated beta-diketones than hexane. This tendency is confirmed by in situ commercial chelates (fluorinates or not) solubility measurements using X-ray absorption spectroscopy. However, cobalt-beta-diketonates are hydrophilic because of their partial hydration. This kind of chelating agents is not suitable to cobalt supercritical fluid extraction from an aqueous phase. Inversely, distribution coefficients of hydrophobic dithiocarbamates are higher than beta-diketonates, whatever the extracting solvent is. Metals extraction from an aqueous matrix seems possible with these chelating agents. (author) [fr

HPLC/MS identification of the polyphenols present in an extract of Myrtus communis L. obtained by supercritical fluid extraction

Directory of Open Access Journals (Sweden)

Paula Pereira

2017-12-01

Full Text Available In this work, we studied an extract obtained by supercritical fluid extraction (SFE using a simpler method of cosolvent (ethanol addition. Instead of using a liquid pump, which is the most common process, the ethanol was directly introduced in the extraction cell, immediately after loading the cell with the plant sample. it was our intent to investigate if this change would have any effect in the composition of the extract obtained. The experimental conditions used were: temperature 48° C, pressure 10 MPa, supercritical fluid (SCF flow rate 130.71dm3h-1 (0.238 kgh-1 and an ethanol volume of 104 cm3. The composition of the extract obtained was different from previous tests, and the compounds identified by HPLC-MS were quinic acid, quinic acid 3,5-di-O-gallate, quinic acid 3,4,5-galloyl, myricetin-galactoside gallate, quercetin-galactoside gallate, quercetin, and myricetin-galactosiderhamnoside.

Supercritical fluid extraction-gas chromatography of volatile organic compounds (VOC) from Tenax devices. Final report, November 1985-September 1986

International Nuclear Information System (INIS)

Wright, B.W.; Kopriva, A.J.; Smith, R.D.

1987-11-01

This report describes the development and evaluation of on-line supercritical-fluid extraction - gas-chromatography instrumentation and methodology for the analysis of volatile organic compounds (VOC) from adsorbent sampling devices. Supercritical fluid extraction offers potential advantages for the removal and transport of organic components from adsorbent matrices including rapid and efficient extraction at mild temperatures. Extraction at mild temperatures eliminates potential problems such as analyte decomposition that can be encountered with the high temperatures needed for thermal desorption analysis. Since a major objective of the study was to develop viable instrumentation and methodology, a relatively detailed description of the instrumentation design requirements and present limitations are discussed. The results of several series of methodology validation studies are also presented. These studies included recovery studies of model VOC spiked on three types of Tenax sampling devices including authentic actively pumped (VOST) and passive (EPA) devices. Replicate devices spiked in an exposure chamber were also subjected to parallel analyses using the new methodology and traditional thermal-desorption gas chromatography

Quantification of the neurotransmitters melatonin and N-acetyl-serotonin in human serum by supercritical fluid chromatography coupled with tandem mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Wolrab, Denise; Frühauf, Peter; Gerner, Christopher, E-mail: christopher.gerner@univie.ac.at

2016-09-21

The aim of this study was developing a supercritical fluid chromatography tandem mass spectrometry (SFC-MS/MS) method and an ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method, for the analysis of N-acetyl-serotonin (NAS) and melatonin (Mel) in human serum, and to compare the performance of these methods. Deuterated isotopologues of the neurotransmitters were synthesized and evaluated for suitability as internal standards in sample preparation. Liquid-liquid extraction was selected as sample preparation procedure. With chloroform, the best extraction solvent tested, an extraction yield of 48 ± 2% for N-acetyl-serotonin and 101 ± 10% for melatonin was achieved. SFC separation was accomplished within 3 min on a BEH stationary phase, employing isocratic elution with 90% carbon dioxide and 0.1% formic acid as well as 0.05% ammonium formate in methanol. For the 4 min UHPLC gradient separation with 0.1% formic acid in water and methanol, respectively, a Kinetex XB-C18 was used as stationary phase. Both chromatographic techniques were optimized regarding mobile phase composition, additives to the mobile phase and column temperature. Multiple reaction monitoring (MRM) analysis was used for quantification of the metabolites. Both methods were validated regarding retention time stability, LOD, LOQ, repeatability and reproducibility of quantification, process efficiency, extraction recovery and matrix effects. LOD and LOQ were 0.017 and 0.05 pg μL{sup −1} for NAS and 0.006 and 0.018 pg μL{sup −1} for Mel in SFC-MS/MS compared to 0.028 and 0.1 pg μL{sup −1} for NAS and 0.006 and 0.017 pg μL{sup −1} for Mel in UHPLC-MS/MS. - Highlights: • Use of supercritical fluid chromatography (SFC) hyphenated with MS/MS. • Separation of biological relevant polar metabolites with SFC. • Critical comparison of validation parameters obtained with UHPLC.

Tipping Point for Expansion of Layered Aluminosilicates in Weakly Polar Solvents: Supercritical CO ₂

Energy Technology Data Exchange (ETDEWEB)

Schaef, Herbert T.; Loganathan, Narasimhan; Bowers, Geoffrey M.; Kirkpatrick, Robert J.; Yazaydin, A. O.; Burton, Sarah D.; Hoyt, David W.; Thanthiriwatte, Sahan; Dixon, David A.; McGrail, Bernard P.; Rosso, Kevin M.; Ilton, Eugene S.; Loring, John S.

2017-10-11

Layered aluminosilicates play a dominant role in the mechanical and gas storage properties of the subsurface, are used in diverse industrial applications, and serve as model materials for understanding solvent-ion-support systems. Although expansion in the presence of H2O is well known to be systematically correlated with the hydration free energy of the interlayer cation, in environments dominated by non-polar solvents (i.e. CO2), uptake into the interlayer is not well-understood. Using novel high pressure capabilities, we investigated the interaction of super-critical CO2 with Na+-, NH4+-, and Cs+-saturated montmorillonite, comparing results with predictions from molecular dynamics simulations. Despite the known trend in H2O, and that cation solvation energies in CO2 suggest a stronger interaction with Na+, both the NH4+- and Cs+-clays readily absorbed CO2 and expanded while the Na+-clay did not. The apparent inertness of the Na+-clay was not due to kinetics, as experiments seeking a stable expanded state showed that none exists. Molecular dynamics simulations revealed a large endothermicity to CO2 intercalation in the Na+-clay, but little or no energy barrier for the NH4+- and Cs+-clays. Consequently, we have shown for the first time that in the presence of a low dielectric constant gas swelling depends more on the strength of the interaction between interlayer cation and aluminosilicate sheets and less on that with solvent. The finding suggests a distinct regime in layered aluminosilicates swelling behavior triggered by low solvent polarizability, with important implications in geomechanics, storage and retention of volatile gases, and across industrial uses in gelling, decoloring, heterogeneous catalysis, and semi-permeable reactive barriers.

Experimental study of elliptical jet from supercritical to subcritical conditions using planar laser induced fluorescence

Energy Technology Data Exchange (ETDEWEB)

Muthukumaran, C. K.; Vaidyanathan, Aravind, E-mail: aravind7@iist.ac.in [Department of Aerospace Engineering, Indian Institute of Space Science and Technology, Trivandrum, Kerala 695547 (India)

2015-03-15

The study of fluid jet dynamics at supercritical conditions involves strong coupling between fluid dynamic and thermodynamic phenomena. Beyond the critical point, the liquid-vapor coexistence ceases to exist, and the fluid exists as a single phase known as supercritical fluid with its properties that are entirely different from liquids and gases. At the critical point, the liquids do not possess surface tension and latent heat of evaporation. Around the critical point, the fluid undergoes large changes in density and possesses thermodynamic anomaly like enhancement in thermal conductivity and specific heat. In the present work, the transition of the supercritical and near-critical elliptical jet into subcritical as well as supercritical environment is investigated experimentally with nitrogen and helium as the surrounding environment. Under atmospheric condition, a liquid jet injected from the elliptical orifice exhibits axis switching phenomena. As the injection temperature increases, the axis switching length also increases. Beyond the critical temperature, the axis switching is not observed. The investigation also revealed that pressure plays a major role in determining the thermodynamic transition of the elliptical jet only for the case of supercritical jet injected into subcritical chamber conditions. At larger pressures, the supercritical jet undergoes disintegration and formation of droplets in the subcritical environment is observed. However, for supercritical jet injection into supercritical environment, the gas-gas like mixing behavior is observed.

Experimental study of elliptical jet from supercritical to subcritical conditions using planar laser induced fluorescence

International Nuclear Information System (INIS)

Muthukumaran, C. K.; Vaidyanathan, Aravind

2015-01-01

The study of fluid jet dynamics at supercritical conditions involves strong coupling between fluid dynamic and thermodynamic phenomena. Beyond the critical point, the liquid-vapor coexistence ceases to exist, and the fluid exists as a single phase known as supercritical fluid with its properties that are entirely different from liquids and gases. At the critical point, the liquids do not possess surface tension and latent heat of evaporation. Around the critical point, the fluid undergoes large changes in density and possesses thermodynamic anomaly like enhancement in thermal conductivity and specific heat. In the present work, the transition of the supercritical and near-critical elliptical jet into subcritical as well as supercritical environment is investigated experimentally with nitrogen and helium as the surrounding environment. Under atmospheric condition, a liquid jet injected from the elliptical orifice exhibits axis switching phenomena. As the injection temperature increases, the axis switching length also increases. Beyond the critical temperature, the axis switching is not observed. The investigation also revealed that pressure plays a major role in determining the thermodynamic transition of the elliptical jet only for the case of supercritical jet injected into subcritical chamber conditions. At larger pressures, the supercritical jet undergoes disintegration and formation of droplets in the subcritical environment is observed. However, for supercritical jet injection into supercritical environment, the gas-gas like mixing behavior is observed

Continuous Process for the Etching, Rinsing and Drying of MEMS Using Supercritical Carbon Dioxide

Energy Technology Data Exchange (ETDEWEB)

Min, Seon Ki; Han, Gap Su; You, Seong-sik [Korea University of Technology and Education, Cheonan (Korea, Republic of)

2015-10-15

The previous etching, rinsing and drying processes of wafers for MEMS (microelectromechanical system) using SC-CO{sub 2} (supercritical-CO{sub 2}) consists of two steps. Firstly, MEMS-wafers are etched by organic solvent in a separate etching equipment from the high pressure dryer and then moved to the high pressure dryer to rinse and dry them using SC-CO{sub 2}. We found that the previous two step process could be applied to etch and dry wafers for MEMS but could not confirm the reproducibility through several experiments. We thought the cause of that was the stiction of structures occurring due to vaporization of the etching solvent during moving MEMS wafer to high pressure dryer after etching it outside. In order to improve the structure stiction problem, we designed a continuous process for etching, rinsing and drying MEMS-wafers using SC-CO{sub 2} without moving them. And we also wanted to know relations of states of carbon dioxide (gas, liquid, supercritical fluid) to the structure stiction problem. In the case of using gas carbon dioxide (3 MPa, 25 .deg. C) as an etching solvent, we could obtain well-treated MEMS-wafers without stiction and confirm the reproducibility of experimental results. The quantity of rinsing solvent used could be also reduced compared with the previous technology. In the case of using liquid carbon dioxide (3 MPa, 5 .deg. C), we could not obtain well-treated MEMS-wafers without stiction due to the phase separation of between liquid carbon dioxide and etching co-solvent(acetone). In the case of using SC-CO{sub 2} (7.5 Mpa, 40 .deg. C), we had as good results as those of the case using gas-CO{sub 2}. Besides the processing time was shortened compared with that of the case of using gas-CO{sub 2}.

Application of ultra-high performance supercritical fluid chromatography for the determination of carotenoids in dietary supplements.

Science.gov (United States)

Li, Bing; Zhao, Haiyan; Liu, Jing; Liu, Wei; Fan, Sai; Wu, Guohua; Zhao, Rong

2015-12-18

A quick and simple ultra-high performance supercritical fluid chromatography-photodiode array detector method was developed and validated for the simultaneous determination of 9 carotenoids in dietary supplements. The influences of stationary phase, co-solvent, pressure, temperature and flow rate on the separation of carotenoids were evaluated. The separation of the carotenoids was carried out using an Acquity UPC(2) HSS C18 SB column (150mm×3.0mm, 1.8μm) by gradient elution with carbon dioxide and a 1:2 (v:v) methanol/ethanol mixture. The column temperature was set to 35°C and the backpressure was 15.2MPa. Under these conditions, 9 carotenoids and the internal standard, β-apo-8'-carotenal, were successfully separated within 10min. The correlation coefficients (R(2)) of the calibration curves were all above 0.997, the limits of detection for the 9 carotenoids were in the range of 0.33-1.08μg/mL, and the limits of quantification were in the range of 1.09-3.58μg/mL. The mean recoveries were from 93.4% to 109.5% at different spiking levels, and the relative standard deviations were between 0.8% and 6.0%. This method was successfully applied to the determination of 9 carotenoids in commercial dietary supplements. Copyright © 2015 Elsevier B.V. All rights reserved.

Impact of solvents and supercritical CO2 drying on the morphology and structure of polymer-based biofilms

Science.gov (United States)

Causa, Andrea; Salerno, Aurelio; Domingo, Concepción; Acierno, Domenico; Filippone, Giovanni

2014-05-01

In the present work, two-dimensional systems based on biodegradable polymers such as poly(ɛ-caprolactone) (PCL), poly(ethylene oxide) (PEO) and polylactic acid (PLA) are fabricated by means of a sustainable approach which consists in inducing phase separation in solutions of such polymers and "green" solvents, namely ethyl lactate (EL) and ethyl acetate (EA). The extraction of the solvent is promoted by a controlled drying process, which is performed in either air or supercritical CO2. The latter can indeed act as both an antisolvent, which favors the deposition of the polymer by forming a mixture with EL and EA, and a plasticizing agent, whose solvation and transport properties may considerably affect the microstructure and crystallinity of the polymer films. The morphological, topographical and crystalline properties of the films are tailored through a judicial selection of the materials and the processing conditions and assessed by means of thermal analyses, polarized optical microscopy, scanning electron microscopy and confocal interferometric microscopy. The results show that the morphological and crystalline properties of the films are strongly dependent on the choice of both the polymer/solvent system and the operating conditions during the drying step. In particular, the morphological, topographical and thermal properties of films prepared starting from highly crystalline polymers, namely PCL and PEO, are greatly affected by the crystallization of the material. Conversely, the less crystalline PLA forms almost completely amorphous films.

Purification of lignans from Fructus Arctii using off-line two-dimensional supercritical fluid chromatography/reversed-phase liquid chromatography.

Science.gov (United States)

Yang, Bichao; Xin, Huaxia; Wang, Feier; Cai, Jianfeng; Liu, Yanfang; Fu, Qing; Jin, Yu; Liang, Xinmiao

2017-08-01

As a common traditional Chinese medicine, Fructus Arctii has important clinical medical values. Its main components are lignans, which are difficult to separate and analyze because of the complex composition, similar chemical structures, and close properties. In this study, an off-line two-dimensional supercritical fluid chromatography/reversed-phase liquid chromatography method, as well as an effective sample pretreatment method based on hydrophilic interaction chromatography material, was developed to enrich the minor lignan fractions and obtain high-purity compounds. In total, 12 high-purity compounds were isolated from Fructus Arctii. Their structures were identified by using high-resolution mass spectrometry and nuclear magnetic resonance spectroscopy, which showed that all were lignans and that most of them were isomers. The results demonstrated the effective off-line two-dimensional supercritical fluid chromatography/reversed-phase liquid chromatography method for the purification of lignans from Fructus Arctii. The separation protocol established here will be beneficial for the separation of complex samples from other kinds of natural products. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Update on Area Production in Mixing of Supercritical Fluids

Science.gov (United States)

Okongo, Nora; Bellan, Josette

2003-01-01

The focus of this research is on supercritical C7H16/N2 and O2/H2 mixing layers undergoing transitions to turbulence. The C7H16/N2 system serves as a simplified model of hydrocarbon/air systems in gas-turbine and diesel engines; the O2/H2 system is representative of liquid rocket engines. One goal of this research is to identify ways of controlling area production to increase disintegration of fluids and enhance combustion in such engines. As used in this research, "area production" signifies the fractional rate of change of surface area oriented perpendicular to the mass-fraction gradient of a mixing layer. In the study, a database of transitional states obtained from direct numerical simulations of the aforementioned mixing layers was analyzed to investigate global layer characteristics, phenomena in regions of high density-gradient magnitude (HDGM), irreversible entropy production and its relationship to the HDGM regions, and mechanisms leading to area production.

High temperature solvent extraction of oil shale and bituminous coal using binary solvent mixtures

Energy Technology Data Exchange (ETDEWEB)

Goetz, G.K.E. [Lehrstuhl fuer Geologie, Geochemie und Lagerstaetten des Erdoels und der Kohle, RWTH Aachen (Germany)

1997-12-31

A high volatile bituminous coal from the Saar Basin and an oil shale from the Messel deposit, both Germany, were extracted with binary solvent mixtures using the Advanced Solvent Extraction method (ASE). Extraction temperature and pressure were kept at 100 C, respectively 150 C, and 20,7 MPa. After the heating phase (5 min) static extractions were performed with mixtures (v:v, 1:3) of methanol with toluene, respectively trichloromethane, for further 5 min. Extract yields were the same or on a higher level compared to those from classical soxhlet extractions (3 days) using the same solvents at 60 C. Comparing the results from ASE with those from supercritical fluid extraction (SFE) the extract yields were similar. Increasing the temperature in ASE releases more soluble organic matter from geological samples, because compounds with higher molecular weight and especially more polar substances were solubilized. But also an enhanced extraction efficiency resulted for aliphatic and aromatic hydrocarbons which are used as biomarkers in Organic Geochemistry. Application of thermochemolysis with tetraethylammonium hydroxide (TEAH) using pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS) on the extraction residues shows clearly that at higher extraction temperatures minor amounts of free fatty acids or their methyl esters (original or produced by ASE) were trapped inside the pore systems of the oil shale or the bituminous coal. ASE offers a rapid and very efficient extraction method for geological samples reducing analysis time and costs for solvents. (orig.)

A fast and sensitive method for the separation of carotenoids using ultra-high performance supercritical fluid chromatography-mass spectrometry.

Science.gov (United States)

Jumaah, Firas; Plaza, Merichel; Abrahamsson, Victor; Turner, Charlotta; Sandahl, Margareta

2016-08-01

In this study, a rapid and sensitive ultra-high performance supercritical fluid chromatography-mass spectrometry (UHPSFC-MS) method has been developed and partially validated for the separation of carotenoids within less than 6 min. Six columns of orthogonal selectivity were examined, and the best separation was obtained by using a 1-aminoanthracene (1-AA) column. The length of polyene chain as well as the number of hydroxyl groups in the structure of the studied carotenoids determines their differences in the physiochemical properties and thus the separation that is achieved on this column. All of the investigated carotenoids were baseline separated with resolution values greater than 1.5. The effects of gradient program, back pressure, and column temperature were studied with respect to chromatographic properties such as retention and selectivity. Electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) were compared in both positive and negative mode, using both direct infusion and hyphenated with UHPSFC. The ESI in positive mode provided the highest response. The coefficient of determination (R (2)) for all calibration curves were greater than 0.998. Limit of detection (LOD) was in the range of 2.6 and 25.2 ng/mL for α-carotene and astaxanthin, respectively, whereas limit of quantification (LOQ) was in the range of 7.8 and 58.0 ng/mL for α-carotene and astaxanthin, respectively. Repeatability and intermediate precision of the developed UHPSFC-MS method were determined and found to be RSD supercritical fluid extracts of microalgae and rosehip. Graphical Abstract Ultra-high performance supercritical fluid chromatography-a rapid separation method for the analysis of carotenoids in rosehip and microalgae samples.

Model validation and parametric study of fluid flows and heat transfer of aviation kerosene with endothermic pyrolysis at supercritical pressure

Directory of Open Access Journals (Sweden)

Keke Xu

2015-12-01

Full Text Available The regenerative cooling technology is a promising approach for effective thermal protection of propulsion and power-generation systems. A mathematical model has been used to examine fluid flows and heat transfer of the aviation kerosene RP-3 with endothermic fuel pyrolysis at a supercritical pressure of 5 MPa. A pyrolytic reaction mechanism, which consists of 18 species and 24 elementary reactions, is incorporated to account for fuel pyrolysis. Detailed model validations are conducted against a series of experimental data, including fluid temperature, fuel conversion rate, various product yields, and chemical heat sink, fully verifying the accuracy and reliability of the model. Effects of fuel pyrolysis and inlet flow velocity on flow dynamics and heat transfer characteristics of RP-3 are investigated. Results reveal that the endothermic fuel pyrolysis significantly improves the heat transfer process in the high fluid temperature region. During the supercritical-pressure heat transfer process, the flow velocity significantly increases, caused by the drastic variations of thermophysical properties. Under all the tested conditions, the Nusselt number initially increases, consistent with the increased flow velocity, and then slightly decreases in the high fluid temperature region, mainly owing to the decreased heat absorption rate from the endothermic pyrolytic chemical reactions.

Supercritical extraction of oleaginous: parametric sensitivity analysis

Directory of Open Access Journals (Sweden)

Santos M.M.

2000-01-01

Full Text Available The economy has become universal and competitive, thus the industries of vegetable oil extraction must advance in the sense of minimising production costs and, at the same time, generating products that obey more rigorous patterns of quality, including solutions that do not damage the environment. The conventional oilseed processing uses hexane as solvent. However, this solvent is toxic and highly flammable. Thus the search of substitutes for hexane in oleaginous extraction process has increased in the last years. The supercritical carbon dioxide is a potential substitute for hexane, but it is necessary more detailed studies to understand the phenomena taking place in such process. Thus, in this work a diffusive model for semi-continuous (batch for the solids and continuous for the solvent isothermal and isobaric extraction process using supercritical carbon dioxide is presented and submitted to a parametric sensitivity analysis by means of a factorial design in two levels. The model parameters were disturbed and their main effects analysed, so that it is possible to propose strategies for high performance operation.

Selective free radical reactions using supercritical carbon dioxide.

Science.gov (United States)

Cormier, Philip J; Clarke, Ryan M; McFadden, Ryan M L; Ghandi, Khashayar

2014-02-12

We report herein a means to modify the reactivity of alkenes, and particularly to modify their selectivity toward reactions with nonpolar reactants (e.g., nonpolar free radicals) in supercritical carbon dioxide near the critical point. Rate constants for free radical addition of the light hydrogen isotope muonium to ethylene, vinylidene fluoride, and vinylidene chloride in supercritical carbon dioxide are compared over a range of pressures and temperatures. Near carbon dioxide's critical point, the addition to ethylene exhibits critical speeding up, while the halogenated analogues display critical slowing. This suggests that supercritical carbon dioxide as a solvent may be used to tune alkene chemistry in near-critical conditions.

Preparative isolation and purification of capsaicin and dihydrocapsaicin from Capsici Fructus using supercritical fluid extraction combined with high speed countercurrent chromatography.

Science.gov (United States)

Yan, Rongwei; Zhao, Leilei; Tao, Junfei; Zou, Yong; Xu, Xinjun

2018-05-01

Supercritical fluid extraction with CO 2 (SFE-CO 2 ) was utilized for extraction of capsaicin (CA) and dihydrocapsaicin (DHCA) from Capsici Fructus, and then a two-step enrichment method for separating capsaicinoids from SFE-CO 2 extracts was developed. The process involved extraction with aqueous methanol and crystallization by alkali extraction and acid precipitation. Finally, a consecutive high-speed countercurrent chromatography (HSCCC) separation method was successfully applied in the purification of CA and DHCA from capsaicinoid crystal. The extraction pressure, extraction temperature and volume of co-solvent were optimized at 33 MPa, 41 °C and 75 mL, respectively, using response surface methodology; the extraction rates of CA and DHCA were about 93.18% and 93.49%, respectively. 407.43 mg capsaicinoid crystal was isolated from the SFE-CO 2 extracts obtained from 100 g capsicum powder by the two-step enrichment method. About 506 mg and 184 mg CA and DHCA with purities up to 98.31% and 96.68%, respectively, were obtained from 1 g capsaicinoid crystal in one HSCCC of three consecutive sample loadings without exchanging any solvent system. This method comprising SFE-CO 2 , a two-step enrichment and HSCCC was efficient, powerful and practical for the large-scale preparation of CA and DHCA from Capsici Fructus with high purity and high yield. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Reaction of phosphorus ylides with carbonyl compounds in supercritical carbon dioxide

Energy Technology Data Exchange (ETDEWEB)

Jeong, Kyung Il; Kim, Hak Do; Shim, Jae Jin; Ra, Choon Sup [Yeungnam Univ., Gyongsan (Korea, Republic of)

2004-02-15

The condensation reaction of (benzylene)triphenylphosphoranes with carbonyl compounds in supercritical carbon dioxide was examined. Reactions of (benzylene)phosphoranes (ca. 1 mmol) with several benzaldehydes in a supercritical carbon dioxide (80 .deg. C, 2,000 psi) containing THF entrainer (5%) in a 24 mL reactor proceed smoothly to yield olefination products in fairly good to excellent yields but slower, compared to reactions in a conventional THF solvent. Generally, phosphoranes that are not substituted with a nitro group show more (Z)-selective reactions with aromatic aldehydes under scCO{sub 2} condition than in THF. The reaction of (benzylene)triphenylphosphosphoranes with 4-t-butylcyclohexanone gave the corresponding olefin compounds with a low conversion under both the supercritical carbon dioxide and the organic THF solvent. Our preliminary study showed the Wittig reaction carries out smoothly in supercritical carbon dioxide medium and also a possible tunability of this reaction pathway by adding a entrainer. The results would be useful for devising a novel process for the environmentally friendly Wittig reaction.

Identification of Bioactivity, Volatile and Fatty Acid Profile in Supercritical Fluid Extracts of Mexican arnica

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J. Saúl García-Pérez

2016-09-01

Full Text Available Supercritical fluid extraction (SFE is a sustainable technique used for the extraction of lipophilic metabolites such as pigments and fatty acids. Arnica plant is considered a potential candidate material with high antioxidant and antimicrobial activities. Therefore, in this study, a locally available Heterotheca inuloides, also known as Mexican arnica, was analyzed for the extraction of high-value compounds. Based on different pressure (P, temperature (T, and co-solvent (CoS, four treatments (T were prepared. A maximum 7.13% yield was recovered from T2 (T = 60 °C, P = 10 MPa, CoS = 8 g/min, followed by 6.69% from T4 (T = 60 °C, P = 30 MPa, CoS = 4 g/min. Some bioactive sesquiterpenoids such as 7-hydroxycadalene, caryophyllene and δ-cadinene were identified in the extracts by GC/MS. The fatty acid profile revealed that the main components were palmitic acid (C16:0, followed by linoleic acid (C18:2ω6c, α-linolenic acid (C18:3ω3 and stearic acid (C18:0 differing in percent yield per treatment. Antibacterial activities were determined by the agar diffusion method, indicating that all the treatments exerted strong antibacterial activity against S. aureus, C. albicans, and E. coli strains. The antioxidant capacity of the extracts was also measured by three in vitro assays, DPPH, TEAC and FRAP, using Trolox as a standard. Results showed high antioxidant capacity enabling pharmaceutical applications of Mexican arnica.

Supercritical fluid extraction of volatile and non-volatile compounds from Schinus molle L.

Directory of Open Access Journals (Sweden)

M. S. T. Barroso

2011-06-01

Full Text Available Schinus molle L., also known as pepper tree, has been reported to have antimicrobial, antifungal, anti-inflammatory, antispasmodic, antipyretic, antitumoural and cicatrizing properties. This work studies supercritical fluid extraction (SFE to obtain volatile and non-volatile compounds from the aerial parts of Schinus molle L. and the influence of the process on the composition of the extracts. Experiments were performed in a pilot-scale extractor with a capacity of 1 L at pressures of 9, 10, 12, 15 and 20 MPa at 323.15 K. The volatile compounds were obtained by CO2 supercritical extraction with moderate pressure (9 MPa, whereas the non-volatile compounds were extracted at higher pressure (12 to 20 MPa. The analysis of the essential oil was carried out by GC-MS and the main compounds identified were sabinene, limonene, D-germacrene, bicyclogermacrene, and spathulenol. For the non-volatile extracts, the total phenolic content was determined by the Folin-Ciocalteau method. Moreover, one of the goals of this study was to compare the experimental data with the simulated yields predicted by a mathematical model based on mass transfer. The model used requires three adjustable parameters to predict the experimental extraction yield curves.

Characterization of Linum usitatissimum L. oil obtained from different extraction technique and in vitro antioxidant potential of supercritical fluid extract

Science.gov (United States)

Chauhan, Rishika; Chester, Karishma; Khan, Yasmeen; Tamboli, Ennus Tajuddin; Ahmad, Sayeed

2015-01-01

Aim: Present investigation was aimed to characterize the fixed oil of Linum usitatissimum L. using five different extraction methods: Supercritical fluid extraction (SFE), ultrasound-assistance, soxhlet extraction, solvent extraction, and three phase partitioning method. Materials and Methods: The SFE conditions (temperature, pressure, and volume of CO2) were optimized prior for better yield. The extracted oils were analyzed and compared for their physiochemical parameters, high performance thin layer chromatography (HPTLC), gas chromatography-mass spectrometry (GC-MS), and Fourier-transformed infrared spectroscopy (FT-IR) fingerprinting. Antioxidant activity was also determined using 1,1-diphenyl-2-picrylhydrazyl and superoxide scavenging method. Result: The main fatty acids were α-linolenic acid, linoleic acid, palmitic acid, and stearic acid as obtained by GC-MS. HPTLC analysis revealed the presence of similar major components in chromatograms. Similarly, the pattern of peaks, as obtained in FT-IR and GC-MS spectra of same oils by different extraction methods, were superimposable. Conclusion: Analysis reported that the fixed oil of L. usitatissimum L. is a good source of n-3 fatty acid with the significant antioxidant activity of oil obtained from SFE extraction method. PMID:26681884

Characterization of Linum usitatissimum L. oil obtained from different extraction technique and in vitro antioxidant potential of supercritical fluid extract

Directory of Open Access Journals (Sweden)

Rishika Chauhan

2015-01-01

Full Text Available Aim: Present investigation was aimed to characterize the fixed oil of Linum usitatissimum L. using five different extraction methods: Supercritical fluid extraction (SFE, ultrasound-assistance, soxhlet extraction, solvent extraction, and three phase partitioning method. Materials and Methods: The SFE conditions (temperature, pressure, and volume of CO2 were optimized prior for better yield. The extracted oils were analyzed and compared for their physiochemical parameters, high performance thin layer chromatography (HPTLC, gas chromatography-mass spectrometry (GC-MS, and Fourier-transformed infrared spectroscopy (FT-IR fingerprinting. Antioxidant activity was also determined using 1,1-diphenyl-2-picrylhydrazyl and superoxide scavenging method. Result: The main fatty acids were α-linolenic acid, linoleic acid, palmitic acid, and stearic acid as obtained by GC-MS. HPTLC analysis revealed the presence of similar major components in chromatograms. Similarly, the pattern of peaks, as obtained in FT-IR and GC-MS spectra of same oils by different extraction methods, were superimposable. Conclusion: Analysis reported that the fixed oil of L. usitatissimum L. is a good source of n-3 fatty acid with the significant antioxidant activity of oil obtained from SFE extraction method.

Enhancing the solubility and bioavailability of poorly water-soluble drugs using supercritical antisolvent (SAS) process.

Science.gov (United States)

Abuzar, Sharif Md; Hyun, Sang-Min; Kim, Jun-Hee; Park, Hee Jun; Kim, Min-Soo; Park, Jeong-Sook; Hwang, Sung-Joo

2018-03-01

Poor water solubility and poor bioavailability are problems with many pharmaceuticals. Increasing surface area by micronization is an effective strategy to overcome these problems, but conventional techniques often utilize solvents and harsh processing, which restricts their use. Newer, green technologies, such as supercritical fluid (SCF)-assisted particle formation, can produce solvent-free products under relatively mild conditions, offering many advantages over conventional methods. The antisolvent properties of the SCFs used for microparticle and nanoparticle formation have generated great interest in recent years, because the kinetics of the precipitation process and morphologies of the particles can be accurately controlled. The characteristics of the supercritical antisolvent (SAS) technique make it an ideal tool for enhancing the solubility and bioavailability of poorly water-soluble drugs. This review article focuses on SCFs and their properties, as well as the fundamentals of overcoming poorly water-soluble drug properties by micronization, crystal morphology control, and formation of composite solid dispersion nanoparticles with polymers and/or surfactants. This article also presents an overview of the main aspects of the SAS-assisted particle precipitation process, its mechanism, and parameters, as well as our own experiences, recent advances, and trends in development. Copyright © 2017 Elsevier B.V. All rights reserved.

Study on the possibility of supercritical fluid extraction for reprocessing of spent nuclear fuel from high temperature gas-cooled reactor

International Nuclear Information System (INIS)

Duan Wuhua; Zhu Liyang; Zhu Yongjun; Xu Jingming

2011-01-01

International interest in high temperature gas-cooled reactor (HTGR) has been increasing in recent years. It is important to study on reprocessing of spent nuclear fuel from HTGR for recovery of nuclear resource and reduction of nuclear waste. Treatment of UO 2 pellets for preparing fuel elements of the 10 MW high temperature gas-cooled reactor (HTR-10) using supercritical fluid extraction was investigated. UO 2 pellets are difficult to be directly dissolved and extracted with TBP-HNO 3 complex in supercritical CO 2 (SC-CO 2 ), and the extraction efficiency is only about 7% under experimental conditions. UO 2 pellets are also difficult to be converted completely into nitrate with N 2 O 4 . When UO 2 pellets break spontaneously into U 3 O 8 powders with particle size below 100 μm under O 2 flow and 600degc, the extraction efficiency of U 3 O 8 powders with TBP-HNO 3 complex in SC-CO 2 can reach more than 98%. U 3 O 8 powders are easy to be completely converted into nitrate with N 2 O 4 . The extraction efficiency of the nitrate product with TBP in SC-CO 2 can reach more than 99%. So it has a potential prospect that application of supercritical fluid extraction in reprocessing of spent nuclear fuel from HTGR. (author)

Experimental investigation and oral bioavailability enhancement of nano-sized curcumin by using supercritical anti-solvent process.

Science.gov (United States)

Anwar, Mohammed; Ahmad, Iqbal; Warsi, Musarrat H; Mohapatra, Sharmistha; Ahmad, Niyaz; Akhter, Sohail; Ali, Asgar; Ahmad, Farhan J

2015-10-01

The biomedical applications of curcumin (CUR) are limited due to its poor oral bioavailability. In this work, CUR nanoparticles were successfully prepared by combining the supercritical anti-solvent (SAS) process with Tween 80 as a solubilizing agent and permeation enhancer. Different processing parameters that can govern the mean particle size and size distribution of nanoparticles were well investigated by manipulating the types of solvents, mixing vessel pressure, mixing vessel temperature, CO2 flow rate, solution flow rate and solution concentration. Solid state characterization was done by Fourier Transform infrared spectroscopy, differential scanning calorimetry, dynamic light scattering, scanning electron microscopy, and powder X-ray diffraction study. Solubility and dissolution profile of SAS-processed CUR were found to be significantly increased in comparison with native CUR. Further, a validated ultra-performance liquid chromatographic method with quadrupole-time of flight-mass spectrometry was developed to investigate the pharmacokinetic parameters after a single oral dose (100mg/kg) administration of CUR (before/after SAS-processed) in male Wistar rats. From the plasma concentration vs. time profile graph, oral bioavailability of SAS-processed CUR was found to be increased approximately 11.6-fold (p<0.001) as compared to native CUR. Copyright © 2015 Elsevier B.V. All rights reserved.

Coiled tubing drilling with supercritical carbon dioxide

Science.gov (United States)

Kolle , Jack J.

2002-01-01

A method for increasing the efficiency of drilling operations by using a drilling fluid material that exists as supercritical fluid or a dense gas at temperature and pressure conditions existing at a drill site. The material can be used to reduce mechanical drilling forces, to remove cuttings, or to jet erode a substrate. In one embodiment, carbon dioxide (CO.sub.2) is used as the material for drilling within wells in the earth, where the normal temperature and pressure conditions cause CO.sub.2 to exist as a supercritical fluid. Supercritical carbon dioxide (SC--CO.sub.2) is preferably used with coiled tube (CT) drilling equipment. The very low viscosity SC--CO.sub.2 provides efficient cooling of the drill head, and efficient cuttings removal. Further, the diffusivity of SC--CO.sub.2 within the pores of petroleum formations is significantly higher than that of water, making jet erosion using SC--CO.sub.2 much more effective than water jet erosion. SC--CO.sub.2 jets can be used to assist mechanical drilling, for erosion drilling, or for scale removal. A choke manifold at the well head or mud cap drilling equipment can be used to control the pressure within the borehole, to ensure that the temperature and pressure conditions necessary for CO.sub.2 to exist as either a supercritical fluid or a dense gas occur at the drill site. Spent CO.sub.2 can be vented to the atmosphere, collected for reuse, or directed into the formation to aid in the recovery of petroleum.

Development of a test facility for analyzing transients in supercritical water-cooled reactors by fractional scaling analysis

Energy Technology Data Exchange (ETDEWEB)

Roberto, Thiago D., E-mail: thiagodbtr@gmail.com [Instituto de Engenharia Nuclear (IEN/CNEN—RJ), Rua Hélio de Almeida, 75 21941-972, Rio de Janeiro Caixa-Postal: 68550, RJ (Brazil); Silva, Mário A. B. da, E-mail: mabs500@gmail.com [Departamento de Energia Nuclear (CTG/UFPE), Av. Professor Luiz Freire, 1000, Recife 50740-540, PE (Brazil); Lapa, Celso M.F., E-mail: lapa@ien.gov.br [Instituto de Engenharia Nuclear (IEN/CNEN—RJ), Rua Hélio de Almeida, 75 21941-972, Rio de Janeiro Caixa-Postal: 68550, RJ (Brazil)

2016-01-15

The feasibility of performing experiments using water under supercritical conditions is limited by technical and financial difficulties. These difficulties can be overcome by using model fluids that are characterized by feasible supercritical conditions, that is, lower critical pressure and critical temperature. Experimental investigations are normally used to determine the conditions under which model fluids reliably represent supercritical fluids under steady-state conditions. A fluid-to-fluid scaling approach has been proposed to determine the model fluids that represent supercritical fluids in a transient state. Recently, a similar technique known as fractional scaling analysis was developed to establish the conditions under which experiments can be performed using models that represent transients in prototypes. This paper presents a fractional scaling analysis application to determine parameters for a test facility in which transient conditions in supercritical water-cooled reactors are simulated by using carbon dioxide as a model fluid, whose critical point conditions are more feasible than those of water. Similarity is obtained between water (prototype) and carbon dioxide (model) by depressurization in a simple vessel. The main parameters required for the construction of a future test facility are obtained using the proposed method.

Development of a test facility for analyzing transients in supercritical water-cooled reactors by fractional scaling analysis

International Nuclear Information System (INIS)

Roberto, Thiago D.; Silva, Mário A. B. da; Lapa, Celso M.F.

2016-01-01

The feasibility of performing experiments using water under supercritical conditions is limited by technical and financial difficulties. These difficulties can be overcome by using model fluids that are characterized by feasible supercritical conditions, that is, lower critical pressure and critical temperature. Experimental investigations are normally used to determine the conditions under which model fluids reliably represent supercritical fluids under steady-state conditions. A fluid-to-fluid scaling approach has been proposed to determine the model fluids that represent supercritical fluids in a transient state. Recently, a similar technique known as fractional scaling analysis was developed to establish the conditions under which experiments can be performed using models that represent transients in prototypes. This paper presents a fractional scaling analysis application to determine parameters for a test facility in which transient conditions in supercritical water-cooled reactors are simulated by using carbon dioxide as a model fluid, whose critical point conditions are more feasible than those of water. Similarity is obtained between water (prototype) and carbon dioxide (model) by depressurization in a simple vessel. The main parameters required for the construction of a future test facility are obtained using the proposed method.

Comparison of the Apoptotic Effects of Supercritical Fluid Extracts of Antrodia cinnamomea Mycelia on Hepatocellular Carcinoma Cells

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Hsiu-Man Lien

2014-06-01

Full Text Available Antrodia cinnamomea (AC has been widely used as a folk medicine in the prevention and treatment of liver diseases, such as hepatitis, hepatic fibrosis, and hepatocellular carcinoma. Previous studies have indicated that triterpenoids and benzenoids show selective cytotoxicity against human hepatoma cell lines. The aim of the study was to compare the triterpenoid content of extract and the extract-induced cytotoxicity in HepG2 cells from mycelia extracts of solid state cultured AC obtained by supercritical fluid extraction (SFE and the conventional solvent extraction method. SFE with CO2 mixed with a constant amount of ethanol co-solvent (10% of CO2 volume applied at different temperatures and pressures (40, 60 and 80 °C and, 20.7, 27.6 and 34.5 Mpa was also compared in the study. Although the extraction yield of triterpenoids (59.7 mg/g under the optimal extraction conditions of 34.5 MPa (5000 psi/60 °C (designated as sample S-5000-60 was equivalent to the extraction yield using conventional liquid solvent extraction with ethanol (ETOH-E at room temperature (60.33 mg/g, the cytotoxicity of the former against the proliferation of HepG2 cell line measured as the inhibition of 50% of cell growth activity (IC50 at dosages of 116.15, 57.82 and 43.96 µg/mL was superior to that of EtOH-E at 131.09, 80.04 and 48.30 µg/mL at 24, 48 and 72 h, respectively. Additionally, we further proved that the apoptotic effect of S-5000-60 presented a higher apoptosis ratio (21.5% than ETOH-E (10.5% according to annexin V-FITC and propidium iodide double staining assay results. The high affinity and selectivity of SFE on bioactive components resulted in a higher extraction efficiency than conventional solvent extraction. The chemical profile of the obtained extracts from solid state cultivated mycelium of AC was also determined by high-performance liquid chromatography electrospray ionization tandem mass spectrometry (LC-MS/MS, whereby three benzenoids and four

Impact of solvents and supercritical CO2 drying on the morphology and structure of polymer-based biofilms

International Nuclear Information System (INIS)

Causa, Andrea; Acierno, Domenico; Filippone, Giovanni; Salerno, Aurelio; Domingo, Concepción

2014-01-01

In the present work, two-dimensional systems based on biodegradable polymers such as poly(ε-caprolactone) (PCL), poly(ethylene oxide) (PEO) and polylactic acid (PLA) are fabricated by means of a sustainable approach which consists in inducing phase separation in solutions of such polymers and “green” solvents, namely ethyl lactate (EL) and ethyl acetate (EA). The extraction of the solvent is promoted by a controlled drying process, which is performed in either air or supercritical CO 2 . The latter can indeed act as both an antisolvent, which favors the deposition of the polymer by forming a mixture with EL and EA, and a plasticizing agent, whose solvation and transport properties may considerably affect the microstructure and crystallinity of the polymer films. The morphological, topographical and crystalline properties of the films are tailored through a judicial selection of the materials and the processing conditions and assessed by means of thermal analyses, polarized optical microscopy, scanning electron microscopy and confocal interferometric microscopy. The results show that the morphological and crystalline properties of the films are strongly dependent on the choice of both the polymer/solvent system and the operating conditions during the drying step. In particular, the morphological, topographical and thermal properties of films prepared starting from highly crystalline polymers, namely PCL and PEO, are greatly affected by the crystallization of the material. Conversely, the less crystalline PLA forms almost completely amorphous films

Application of supercritical and subcritical fluids for the extraction of hazardous materials from soil

Directory of Open Access Journals (Sweden)

Skorupan Dara

2002-01-01

Full Text Available Subcritical and supercritical extractions are novel, non destructive techniques which can be applied for the removal of hazardous compounds from contaminated soil without any changes of the soil composition and structure. The aim of the presented review paper is to give information on up-to day results of this method commonly applied by several institutions worldwide. Interest in the application of SC CO2 has been more expressed in the last two decades, which may be related to its favorable characteristics (non-toxic, non-flammable, increase diffusion into small pores, low viscosity under SC conditions, low price and others. However, interest in wet oxidation (WO and especially in SCWO (the application of water under supercritical conditions with air has also increased in the last few years. Interest in H2O as a SC fluid, as well as in extraction with water under subcritical conditions may also be related to specific characteristics and the enhanced rate of extraction. Moreover, the solubility of some specific compounds present in soil can be easily changed by adjusting the pressure and temperature of extraction. The high price of the units designed to operate safely at a pressure and temperature much higher than the a critical one of the applied fluids is the main reason why, at present, there is no more broader application of such techniques for the removal hazardous materials from contaminated soil. In the present paper, among many literature citations and their overall review, some specific details related to the development of specific analytical methods under SC conditions are also considered.

Degradation Characteristics of Wood Using Supercritical Alcohols

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Jeeban Poudel

2012-11-01

Full Text Available In this work, the characteristics of wood degradation using supercritical alcohols have been studied. Supercritical ethanol and supercritical methanol were used as solvents. The kinetics of wood degradation were analyzed using the nonisothermal weight loss technique with heating rates of 3.1, 9.8, and 14.5 °C/min for ethanol and 5.2, 11.3, and 16.3 °C/min for methanol. Three different kinetic analysis methods were implemented to obtain the apparent activation energy and the overall reaction order for wood degradation using supercritical alcohols. These were used to compare with previous data for supercritical methanol. From this work, the activation energies of wood degradation in supercritical ethanol were obtained as 78.0–86.0, 40.1–48.1, and 114 kJ/mol for the different kinetic analysis methods used in this work. The activation energies of wood degradation in supercritical ethanol were obtained as 78.0–86.0, 40.1–48.1, and 114 kJ/mol. This paper also includes the analysis of the liquid products obtained from this work. The characteristic analysis of liquid products on increasing reaction temperature and time has been performed by GC-MS. The liquid products were categorized according to carbon numbers and aromatic/aliphatic components. It was found that higher conversion in supercritical ethanol occurs at a lower temperature than that of supercritical methanol. The product analysis shows that the majority of products fall in the 2 to 15 carbon number range.

An oscillation free shock-capturing method for compressible van der Waals supercritical fluid flows

International Nuclear Information System (INIS)

Pantano, C.; Saurel, R.; Schmitt, T.

2017-01-01

Numerical solutions of the Euler equations using real gas equations of state (EOS) often exhibit serious inaccuracies. The focus here is the van der Waals EOS and its variants (often used in supercritical fluid computations). The problems are not related to a lack of convexity of the EOS since the EOS are considered in their domain of convexity at any mesh point and at any time. The difficulties appear as soon as a density discontinuity is present with the rest of the fluid in mechanical equilibrium and typically result in spurious pressure and velocity oscillations. This is reminiscent of well-known pressure oscillations occurring with ideal gas mixtures when a mass fraction discontinuity is present, which can be interpreted as a discontinuity in the EOS parameters. We are concerned with pressure oscillations that appear just for a single fluid each time a density discontinuity is present. As a result, the combination of density in a nonlinear fashion in the EOS with diffusion by the numerical method results in violation of mechanical equilibrium conditions which are not easy to eliminate, even under grid refinement.

Characterization of Arachis hypogaea L. oil obtained from different extraction techniques and in vitro antioxidant potential of supercritical fluid extraction extract

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Rishika Chauhan

2016-01-01

Full Text Available Aim: The present investigation was aimed to characterize the fixed oil of Arachis hypogaea L. using five different extraction methods: Supercritical fluid extraction (SFE, ultrasound assistance extraction, soxhlet extraction, solvent extraction, and three phase partitioning method. Materials and Methods: The SFE conditions (temperature, pressure, and volume of CO 2 were optimized prior for better yield. The extracted oils were analyzed and compared for their physiochemical parameters, high-performance thin layer chromatography (HPTLC, gas chromatography-mass spectrometry (GC-MS, and Fourier transform infrared spectrometry (FT-IR fingerprinting. Anti-oxidant activity was also determined using DPPH and superoxide scavenging method. Results: The main fatty acids were oleic, linoleic, palmitic, and stearic acids as obtained by GC-MS. HPTLC analysis revealed the presence of similar major components in chromatograms. Similarly, the pattern of peaks as obtained in FT-IR and GC-MS spectra of same oils by different extraction methods was superimposable. Conclusion: Analysis reported that the fixed oil of A. hypogaea L. is a good source of unsaturated fatty acid, mainly n-6 and n-9 fatty acid with a significant antioxidant activity of oil obtained from SFE extraction method.

Optimized process for recovery of glass- and carbon fibers with retained mechanical properties by means of near- and supercritical fluids

DEFF Research Database (Denmark)

Sokoli, Hülya U.; Beauson, Justine; Simonsen, Morten E.

2017-01-01

on the resin degradation efficiency and the quality of the recovered glass and carbon fibers. Supercritical acetone at 260 ºC, 60 bar and a c/s ratio up to 2.1 g/mL could achieve nearly complete degradation of the resin. The glass fibers were recovered with up to 89% retained tensile strength compared...... to the virgin glass fibers. The use of near-critical water reduced the tensile strength of the glass fibers by up to 65%, whereas the carbon fibers were recovered with retained tensile strength compared to the virgin carbon fibers using water or acetone.......Degradation of hybrid fiber composites using near-critical water or supercritical acetone has been investigated in this study. Process parameters such as temperature (T= 260-300 ºC), pressure (p = 60-300 bar) and composite/solvent (c/s = 0.29-2.1 g/mL) ratio were varied to determine the effect...

Diffusion of Supercritical Fluids through Single-Layer Nanoporous Solids: Theory and Molecular Simulations.

Science.gov (United States)

Oulebsir, Fouad; Vermorel, Romain; Galliero, Guillaume

2018-01-16

With the advent of graphene material, membranes based on single-layer nanoporous solids appear as promising devices for fluid separation, be it liquid or gaseous mixtures. The design of such architectured porous materials would greatly benefit from accurate models that can predict their transport and separation properties. More specifically, there is no universal understanding of how parameters such as temperature, fluid loading conditions, or the ratio of the pore size to the fluid molecular diameter influence the permeation process. In this study, we address the problem of pure supercritical fluids diffusing through simplified models of single-layer porous materials. Basically, we investigate a toy model that consists of a single-layer lattice of Lennard-Jones interaction sites with a slit gap of controllable width. We performed extensive equilibrium and biased molecular dynamics simulations to document the physical mechanisms involved at the molecular scale. We propose a general constitutive equation for the diffusional transport coefficient derived from classical statistical mechanics and kinetic theory, which can be further simplified in the ideal gas limit. This transport coefficient relates the molecular flux to the fluid density jump across the single-layer membrane. It is found to be proportional to the accessible surface porosity of the single-layer porous solid and to a thermodynamic factor accounting for the inhomogeneity of the fluid close to the pore entrance. Both quantities directly depend on the potential of mean force that results from molecular interactions between solid and fluid atoms. Comparisons with the simulations data show that the kinetic model captures how narrowing the pore size below the fluid molecular diameter lowers dramatically the value of the transport coefficient. Furthermore, we demonstrate that our general constitutive equation allows for a consistent interpretation of the intricate effects of temperature and fluid loading

Development of a split-flow system for high precision variable sample introduction in supercritical fluid chromatography.

Science.gov (United States)

Sakai, Miho; Hayakawa, Yoshihiro; Funada, Yasuhiro; Ando, Takashi; Fukusaki, Eiichiro; Bamba, Takeshi

2017-09-15

In this study, we propose a novel variable sample injection system based on full-loop injection, named the split-flow sample introduction system, for application in supercritical fluid chromatography (SFC). In this system, the mobile phase is split by the differential pressure between two back pressure regulators (BPRs) after full-loop injection suitable for SFC, and this differential pressure determines the introduction rate. Nine compounds with a wide range of characteristics were introduced with high reproducibility and universality, confirming that a robust variable sample injection system was achieved. We also investigated the control factors of our proposed system. Sample introduction was controlled by the ratio between the column-side pressure drops in splitless and split flow, ΔP columnsideinsplitless and ΔP columnsideinsplit , respectively, where ΔP columnsideinsplitless is related to the mobile phase flow rate and composition and the column resistance. When all other conditions are kept constant, increasing the make-up flow induces an additional pressure drop on the column side of the system, which leads to a reduced column-side flow rate, and hence decreased the amount of sample injected, even when the net pressure drop on the column side remains the same. Thus, sample introduction could be highly controlled at low sample introduction rate, regardless of the introduction conditions. This feature is advantageous because, as a control factor, the solvent in the make-up pump is independent of the column-side pressure drop. Copyright © 2017. Published by Elsevier B.V.

Enhancement of antioxidant activity of C-phycocyanin of Spirulina powder treated with supercritical fluid carbon dioxide

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Monchai Dejsungkranont

2017-10-01

Full Text Available The functionality and activity of proteins can be modified by supercritical fluid CO2 (SCFCO2. The objectives of this study were to investigate the possibility of enhanced antioxidant activity of C-phycocyanin (C-PC proteins from light-harvested Spirulina maxima powder using the SCFCO2 pretreatment and to optimize the SCFCO2 pretreatment conditions enhancing the antioxidant activity of C-PC. The Taguchi method was used to determine the optimum conditions for the SCFCO2 pretreatment. The experimental factors were the pretreatment temperature, pressure, pretreatment mode (static, dynamic and conjugated and duration. The optimal conditions of SCFCO2 pretreatment were: 60 °C, 24.13 MPa and 60 min in static batch mode. Using these pretreatment conditions, the maximum antioxidant activity of C-PC from the treated residual biomass was 410.1 μmole trolox/mg, which was 1.7-fold higher than the untreated biomass (control. The factor that most affected the antioxidant activity of C-PC was temperature (59%. A high pretreatment temperature could damage C-PC, but promoted antioxidant activity. Of note is that this work was the first to explore SCFCO2 treatment enhancing the antioxidant activity of C-PC in Spirulina sp. powder. Keywords: Antioxidant activity, C-phycocyanin, Spirulina sp., Supercritical fluid carbon dioxide pretreatment, Taguchi method

Discussion of heat transfer phenomena in fluids at supercritical pressure with the aid of CFD models

International Nuclear Information System (INIS)

Sharabi, Medhat; Ambrosini, Walter

2009-01-01

The paper discusses heat transfer enhancement and deterioration phenomena observed in experimental data for fluids at supercritical pressure. The results obtained by the application of various CFD turbulence models in the prediction of experimental data for water and carbon dioxide flowing in circular tubes are firstly described. On this basis, the capabilities of the addressed models in predicting the observed phenomena are shortly discussed. Then, the analysis focuses on further results obtained by a low-Reynolds number k - ε model addressing one of the considered experimental apparatuses by changing the operating conditions. In particular, the usual imposed heat flux boundary condition is changed to assigned wall temperature, in order to highlight effects otherwise impossible to point out. The obtained results, supported by considerations drawn from experimental information, allow comparing the trends observed for heat transfer deterioration at supercritical pressure with those typical of the thermal crisis in boiling systems, clarifying old concepts of similarity among them

A supercritical carbon dioxide plasma process for preparing tungsten oxide nanowires

International Nuclear Information System (INIS)

Kawashima, Ayato; Nomura, Shinfuku; Toyota, Hiromichi; Takemori, Toshihiko; Mukasa, Shinobu; Maehara, Tsunehiro

2007-01-01

A supercritical carbon dioxide (CO 2 ) plasma process for fabricating one-dimensional tungsten oxide nanowires coated with amorphous carbon is presented. High-frequency plasma was generated in supercritical carbon dioxide at 20 MPa by using tungsten electrodes mounted in a supercritical cell, and subsequently an organic solvent was introduced with supercritical carbon dioxide into the plasma. Electron microscopy and Raman spectroscopy investigations of the deposited materials showed the production of tungsten oxide nanowires with or without an outer layer. The nanowires with an outer layer exhibited a coaxial structure with an outer concentric layer of amorphous carbon and an inner layer of tungsten oxide with a thickness and diameter of 20-30 and 10-20 nm, respectively

A comparative study of solvent and supercritical Co2 extraction of Simarouba gluaca seed oil; Estudio comparativo de la extracción con solvente y CO2 supercrítico de aceites de semillas de Simarouba glauca.

Energy Technology Data Exchange (ETDEWEB)

Anjaneyulu, B.; Satyannarayana, S.; Kanjilal, S.; Siddaiah, V.; Prasanna Rani, K.N.

2017-07-01

In the present study, the supercritical carbon dioxide (Co2) extraction of oil from Simarouba gluaca seeds was carried out at varying conditions of pressure (300–500 bar), temperature (50–70 °C) and CO2 flow rate (10–30 g·min-1). The extraction condition for maximum oil yield was obtained at 500 bar pressure, 70 °C and at 30 g·min-1 flow rate of CO2. The extracted oil was analyzed thoroughly for physico-chemical properties and compared with those of conventional solvent extracted oil. An interesting observation is a significant reduction in the phosphorus content of the oil (8.4 mg·kg-1) extracted using supercritical CO2 compared to the phosphorous content of the solvent extracted oil (97 mg·kg-1). Moreover, the content of total tocopherols in supercritically extracted oil (135.6 mg·kg-1) was found to be higher than the solvent extracted oil (111 mg·kg-1). The rest of the physico-chemical properties of the two differently extracted oils matched well with each other. The results indicated the possible benefits of supercritical CO2 extraction over solvent extraction of Simarouba gluaca seed oil. [Spanish] En el presente estudio se llevó a cabo la extracción con dióxido de carbono supercrítico (CO2) de aceites de semillas de Simarouba gluaca en diversas condiciones de presión (300–500 bar), temperatura (50–70 °C) y el caudal de CO2 (10–30 g·min-1). La condición de extracción para obtener el máximo rendimiento de aceite se obtuvo a una presión de 500 bares, una temperatura de 70 °C y un caudal de CO2 de 30 g·min-1. Al aceite extraido se determinó sus propiedades fisicoquímicas y se comparó con las del aceite extraído con disolvente convencional. Una observación interesante es la reducción significativa del contenido de fósforo (8,4 mg·kg-1) del aceite extraído utilizando CO2 supercrítico en comparación con el del aceite extraído con disolvente (97 mg·kg-1). Además, el contenido de tocoferol total en el aceite extra

Sedative and hypnotic effects of supercritical carbon dioxide fluid extraction from Schisandra chinensis in mice

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Hongyan Zhu

2016-10-01

Full Text Available Schisandra chinensis is a traditional Chinese medicine that has been used for treating insomnia and neurasthenia for centuries. Lignans, which are considered to be the bioactive components, are apt to be extracted by supercritical carbon dioxide. This study was conducted to investigate the sedative and hypnotic activities of the supercritical carbon dioxide fluid extraction of S. chinensis (SFES in mice and the possible mechanisms. SFES exhibited an obvious sedative effect on shortening the locomotor activity in mice in a dose-dependent (10–200 mg/kg manner. SFES (50 mg/kg, 100 mg/kg, and 200 mg/kg, intragstrically showed a strong hypnotic effect in synergy with pentobarbital in mouse sleep, and reversal of insomnia induced by caffeine, p-chlorophenylalanine and flumazenil by decreasing sleep latency, sleep recovery, and increasing sleeping time. In addition, it produced a synergistic effect with 5-hydroxytryptophan (2.5 mg/kg, intraperitoneally. The behavioral pharmacological results suggest that SFES has significant sedative and hypnotic activities, and the mechanisms might be relevant to the serotonergic and γ-aminobutyric acid (GABAergic system.

超臨界二酸化炭素抽出の応用

OpenAIRE

谷口, 正之; MASAYUKI, TANIGUCHI; 新潟大学工学部化学工学科; Department of Chemical Engineering, Faculty of Engineering

1989-01-01

Supercritical fluid extraction is a novel separation technique which exploits the solvent properties of fluids near the critical point. The use of supercritical carbon dioxide (SC-CO_2) as a solvent for natural products in the fermentation and food indusries has advantages over other solvents because CO_2 is non-toxic, non-flammable, non-corrosive, cheap, and readily available in large quantities of high purity. In this paper, the following examples for the application of SC-CO_2 extraction a...