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Sample records for ligand-assisted supercritical fluid

  1. 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

  2. Selective chelation-supercritical fluid extraction of metal ions from waste materials

    International Nuclear Information System (INIS)

    Wai, C.N.; Laintz, K.E.; Yonker, C.R.

    1993-01-01

    The removal of toxic organics, metals, and radioisotopes from solids or liquids is a major concern in the treatment of industrial and nuclear wastes. For this reason, developing methods for selective separation of toxic metals and radioactive materials from solutions of complex matrix is an important problem in environmental research. Recent developments indicate supercritical fluids are good solvents for organic compounds. Many gases become supercritical fluids under moderate temperatures and pressures. For example, the critical temperature and pressure of carbon dioxide are 31 degrees C and 73 atm, respectively. The high diffusivity, low viscosity, and T-P dependence of solvent strength are some attractive properties of supercritical fluid extraction (SFE). Since CO 2 offers the additional benefits of stability and non-toxicity, the SFE technique avoids generation of organic liquid waste and exposure of personnel to toxic solvents. While direct extraction of metal ions by supercritical fluids is highly inefficient, these ions when complexed with organic ligands become quite soluble in supercritical fluids. Specific ligands can be used to achieve selective extraction of metal ions in this process. After SFE, the fluid phase can be depressurized for precipitation of the metal chelates and recycled. The ligand can also be regenerated for repeated use. The success of this selective chelation-supercritical fluid extraction (SC-SFE) process depends on a number of factors including the efficiencies of the selective chelating agents, solubilities of metal chelates in supercritical fluids, rate of extraction, ease of regeneration of the ligands, etc. In this report, the authors present recent results on the studies of the solubilities of metal chelates in supercritical CO 2 , experimental ions from aqueous solution, and the development of selective chelating agents (ionizable crown ethers) for the extraction of lanthanides and actinides

  3. 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)

  4. 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.

  5. Materials processing using supercritical fluids

    Directory of Open Access Journals (Sweden)

    Orlović Aleksandar M.

    2005-01-01

    Full Text Available One of the most interesting areas of supercritical fluids applications is the processing of novel materials. These new materials are designed to meet specific requirements and to make possible new applications in Pharmaceuticals design, heterogeneous catalysis, micro- and nano-particles with unique structures, special insulating materials, super capacitors and other special technical materials. Two distinct possibilities to apply supercritical fluids in processing of materials: synthesis of materials in supercritical fluid environment and/or further processing of already obtained materials with the help of supercritical fluids. By adjusting synthesis parameters the properties of supercritical fluids can be significantly altered which further results in the materials with different structures. Unique materials can be also obtained by conducting synthesis in quite specific environments like reversed micelles. This paper is mainly devoted to processing of previously synthesized materials which are further processed using supercritical fluids. Several new methods have been developed to produce micro- and nano-particles with the use of supercritical fluids. The following methods: rapid expansion of supercritical solutions (RESS supercritical anti-solvent (SAS, materials synthesis under supercritical conditions and encapsulation and coating using supercritical fluids were recently developed.

  6. 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

  7. 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.

  8. 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)

  9. 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

  10. 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)

  11. 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.

  12. Supercritical fluids in ionic liquids

    NARCIS (Netherlands)

    Kroon, M.C.; Peters, C.J.; Plechkova, N.V.; Seddon, K.R.

    2014-01-01

    Ionic liquids and supercritical fluids are both alternative environmentally benign solvents, but their properties are very different. Ionic liquids are non-volatile but often considered highly polar compounds, whereas supercritical fluids are non-polar but highly volatile compounds. The combination

  13. 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

  14. Producing Polymer Fibers by Electrospinning in Supercritical Fluids

    Directory of Open Access Journals (Sweden)

    Lu Li

    2013-01-01

    Full Text Available Nanofibers have a wide range of applications, including filtration and biomedical engineering. Porous or hollow fibers with large surface-to-volume ratios are more popular in some fields than the common nanofibers. Porous nanofibers can be obtained through electrospinning with highly volatile solvents or through special treatment following electrospinning. A new process where electrospinning is conducted in supercritical or near-critical CO2 to produce porous or hollow nanofibers has been summarized. In addition, a process entailing compressed N2-assisted electrospinning was attempted to produce PVP nanofibers in this work, but it was proved to be unsuccessful. Since the fiber morphologies are dependent on the phase behavior of organic solvents in supercritical fluids, ASPEN PLUS 2006 was used to simulate the phase equilibrium of the solvent-supercritical fluid system to explain why porous or hollow fibers can be obtained in compressed CO2, but not in compressed N2.

  15. 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.

  16. PULSE RADIOLYSIS IN SUPERCRITICAL RARE GAS FLUIDS

    International Nuclear Information System (INIS)

    HOLROYD, R.

    2007-01-01

    Recently, supercritical fluids have become quite popular in chemical and semiconductor industries for applications in chemical synthesis, extraction, separation processes, and surface cleaning. These applications are based on: the high dissolving power due to density build-up around solute molecules, and the ability to tune the conditions of a supercritical fluid, such as density and temperature, that are most suitable for a particular reaction. The rare gases also possess these properties and have the added advantage of being supercritical at room temperature. Information about the density buildup around both charged and neutral species can be obtained from fundamental studies of volume changes in the reactions of charged species in supercritical fluids. Volume changes are much larger in supercritical fluids than in ordinary solvents because of their higher compressibility. Hopefully basic studies, such as discussed here, of the behavior of charged species in supercritical gases will provide information useful for the utilization of these solvents in industrial applications

  17. Supercritical fluid assisted production of chitosan oligomers micrometric powders.

    Science.gov (United States)

    Du, Zhe; Shen, Yu-Bin; Tang, Chuan; Guan, Yi-Xin; Yao, Shan-Jing; Zhu, Zi-Qiang

    2014-02-15

    Chitosan oligomers (O-chitosan) micrometric particles were produced from aqueous solution using a novel process, i.e. supercritical fluid assisted atomization introduced by hydrodynamic cavitation mixer (SAA-HCM). Hydrodynamic cavitation was introduced to enhance mass transfer and facilitate the mixing between SC-CO2 and liquid solution for fine particles formation. Well defined, separated and spherical microparticles were obtained, and the particles size could be well controlled with narrow distribution ranging from 0.5 μm to 3 μm. XRD patterns showed amorphous structure of O-chitosan microparticles. FTIR, TGA and DSC analyses confirmed that no change in molecular structure and thermal stability after SAA-HCM processing, while the water content was between 5.8% and 8.4%. Finally, tap densities were determined to be below 0.45 g/cm(3) indicating hollow or porous structures of microparticles. By tuning process parameters, theoretical mass median aerodynamic sizes lied inside respirable range of 1-2 μm, which presented the potential of the O-chitosan microparticles in application as inhaled dry powders. SAA-HCM was demonstrated to be very useful in particle size engineering. Copyright © 2013 Elsevier Ltd. All rights reserved.

  18. Supercritical fluid technologies for ceramic-processing applications

    International Nuclear Information System (INIS)

    Matson, D.W.; Smith, R.D.

    1989-01-01

    This paper reports on the applications of supercritical fluid technologies for ceramic processing. The physical and chemical properties of these densified gases are summarized and related to their use as solvents and processing media. Several areas are identified in which specific ceramic processes benefit from the unique properties of supercritical fluids. The rapid expansion of supercritical fluid solutions provides a technique for producing fine uniform powders and thin films of widely varying materials. Supercritical drying technologies allow the formation of highly porous aerogel products with potentially wide application. Hydrothermal processes leading to the formation of large single crystals and microcrystalline powders can also be extended into the supercritical regime of water. Additional applications and potential applications are identified in the areas of extraction of binders and other additives from ceramic compacts, densification of porous ceramics, the formation of powders in supercritical micro-emulsions, and in preceramic polymer processing

  19. 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.

  20. 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

  1. 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.

  2. 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)

  3. 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.

  4. 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) ...

  5. 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.”

  6. Supercritical fluid technology: concepts and pharmaceutical applications.

    Science.gov (United States)

    Deshpande, Praful Balavant; Kumar, G Aravind; Kumar, Averineni Ranjith; Shavi, Gopal Venkatesh; Karthik, Arumugam; Reddy, Meka Sreenivasa; Udupa, Nayanabhirama

    2011-01-01

    In light of environmental apprehension, supercritical fluid technology (SFT) exhibits excellent opportunities to accomplish key objectives in the drug delivery sector. Supercritical fluid extraction using carbon dioxide (CO(2)) has been recognized as a green technology. It is a clean and versatile solvent with gas-like diffusivity and liquid-like density in the supercritical phase, which has provided an excellent alternative to the use of chemical solvents. The present commentary provides an overview of different techniques using supercritical fluids and their future opportunity for the drug delivery industry. Some of the emerging applications of SFT in pharmaceuticals, such as particle design, drug solubilization, inclusion complex, polymer impregnation, polymorphism, drug extraction process, and analysis, are also covered in this review. The data collection methods are based on the recent literature related to drug delivery systems using SFT platforms. SFT has become a much more versatile and environmentally attractive technology that can handle a variety of complicated problems in pharmaceuticals. This cutting-edge technology is growing predominantly to surrogate conventional unit operations in relevance to the pharmaceutical production process. Supercritical fluid technology has recently drawn attention in the field of pharmaceuticals. It is a distinct conception that utilizes the solvent properties of supercritical fluids above their critical temperature and pressure, where they exhibit both liquid-like and gas-like properties, which can enable many pharmaceutical applications. For example, the liquid-like properties provide benefits in extraction processes of organic solvents or impurities, drug solubilization, and polymer plasticization, and the gas-like features facilitate mass transfer processes. It has become a much more versatile and environmentally attractive technology that can handle a variety of complicated problems in pharmaceuticals. This review is

  7. Electrochemistry in supercritical fluids

    Science.gov (United States)

    Branch, Jack A.; Bartlett, Philip N.

    2015-01-01

    A wide range of supercritical fluids (SCFs) have been studied as solvents for electrochemistry with carbon dioxide and hydrofluorocarbons (HFCs) being the most extensively studied. Recent advances have shown that it is possible to get well-resolved voltammetry in SCFs by suitable choice of the conditions and the electrolyte. In this review, we discuss the voltammetry obtained in these systems, studies of the double-layer capacitance, work on the electrodeposition of metals into high aspect ratio nanopores and the use of metallocenes as redox probes and standards in both supercritical carbon dioxide–acetonitrile and supercritical HFCs. PMID:26574527

  8. Bio-oil production from biomass via supercritical fluid extraction

    Energy Technology Data Exchange (ETDEWEB)

    Durak, Halil, E-mail: halildurak@yyu.edu.tr [Yuzuncu Yıl University, Vocational School of Health Services, 65080, Van (Turkey)

    2016-04-18

    Supercritical fluid extraction is used for producing bio-fuel from biomass. Supercritical fluid extraction process under supercritical conditions is the thermally disruption process of the lignocellulose or other organic materials at 250-400 °C temperature range under high pressure (4-5 MPa). Supercritical fluid extraction trials were performed in a cylindrical reactor (75 mL) in organic solvents (acetone, ethanol) under supercritical conditions with (calcium hydroxide, sodium carbonate) and without catalyst at the temperatures of 250, 275 and 300 °C. The produced liquids at 300 °C in supercritical liquefaction were analyzed and characterized by elemental, GC-MS and FT-IR. 36 and 37 different types of compounds were identified by GC-MS obtained in acetone and ethanol respectively.

  9. Bio-oil production from biomass via supercritical fluid extraction

    International Nuclear Information System (INIS)

    Durak, Halil

    2016-01-01

    Supercritical fluid extraction is used for producing bio-fuel from biomass. Supercritical fluid extraction process under supercritical conditions is the thermally disruption process of the lignocellulose or other organic materials at 250-400 °C temperature range under high pressure (4-5 MPa). Supercritical fluid extraction trials were performed in a cylindrical reactor (75 mL) in organic solvents (acetone, ethanol) under supercritical conditions with (calcium hydroxide, sodium carbonate) and without catalyst at the temperatures of 250, 275 and 300 °C. The produced liquids at 300 °C in supercritical liquefaction were analyzed and characterized by elemental, GC-MS and FT-IR. 36 and 37 different types of compounds were identified by GC-MS obtained in acetone and ethanol respectively.

  10. Technology with Supercritical Fluid. Part 2. Applications

    International Nuclear Information System (INIS)

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

    1998-01-01

    The present article is based on a bibliographical analysis of the main applications of the supercritical fluid in various fields, as: extraction from solid matrices, division of liquid charges, chromatography HPLC with supercritical eluent, chemical and biochemical reactions in supercritical solvents etc [it

  11. 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

  12. 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...

  13. Industrial applications and current trends in supercritical fluid technologies

    OpenAIRE

    Gamse Thomas

    2005-01-01

    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...

  14. 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.

  15. 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

  16. 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.

  17. 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

  18. Industrial applications and current trends in supercritical fluid technologies

    Directory of Open Access Journals (Sweden)

    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

  19. Supercritical fluid reverse micelle separation

    Science.gov (United States)

    Fulton, J.L.; Smith, R.D.

    1993-11-30

    A method of separating solute material from a polar fluid in a first polar fluid phase is provided. The method comprises combining a polar fluid, a second fluid that is a gas at standard temperature and pressure and has a critical density, and a surfactant. The solute material is dissolved in the polar fluid to define the first polar fluid phase. The combined polar and second fluids, surfactant, and solute material dissolved in the polar fluid is maintained under near critical or supercritical temperature and pressure conditions such that the density of the second fluid exceeds the critical density thereof. In this way, a reverse micelle system defining a reverse micelle solvent is formed which comprises a continuous phase in the second fluid and a plurality of reverse micelles dispersed in the continuous phase. The solute material is dissolved in the polar fluid and is in chemical equilibrium with the reverse micelles. The first polar fluid phase and the continuous phase are immiscible. The reverse micelles each comprise a dynamic aggregate of surfactant molecules surrounding a core of the polar fluid. The reverse micelle solvent has a polar fluid-to-surfactant molar ratio W, which can vary over a range having a maximum ratio W[sub o] that determines the maximum size of the reverse micelles. The maximum ratio W[sub o] of the reverse micelle solvent is then varied, and the solute material from the first polar fluid phase is transported into the reverse micelles in the continuous phase at an extraction efficiency determined by the critical or supercritical conditions. 27 figures.

  20. 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)

  1. 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.

  2. 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

  3. 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.

  4. 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.

  5. Optimization of microwave-assisted extraction and supercritical fluid extraction of carbamate pesticides in soil by experimental design methodology.

    Science.gov (United States)

    Sun, Lei; Lee, Hian Kee

    2003-10-03

    Orthogonal array design (OAD) was applied for the first time to optimize microwave-assisted extraction (MAE) and supercritical fluid extraction (SFE) conditions for the analysis of four carbamates (propoxur, propham, methiocarb, chlorpropham) from soil. The theory and methodology of a new OA16 (4(4)) matrix derived from a OA16 (2(15)) matrix were developed during the MAE optimization. An analysis of variance technique was employed as the data analysis strategy in this study. Determinations of analytes were completed using high-performance liquid chromatography (HPLC) with UV detection. Four carbamates were successfully extracted from soil with recoveries ranging from 85 to 105% with good reproducibility (approximately 4.9% RSD) under the optimum MAE conditions: 30 ml methanol, 80 degrees C extraction temperature, and 6-min microwave heating. An OA8 (2(7)) matrix was employed for the SFE optimization. The average recoveries and RSD of the analytes from spiked soil by SFE were 92 and 5.5%, respectively except for propham (66.3+/-7.9%), under the following conditions: heating for 30 min at 60 degrees C under supercritical CO2 at 300 kg/cm2 modified with 10% (v/v) methanol. The composition of the supercritical fluid was demonstrated to be a crucial factor in the extraction. The addition of a small volume (10%) of methanol to CO2 greatly enhanced the recoveries of carbamates. A comparison of MAE with SFE was also conducted. The results indicated that >85% average recoveries were obtained by both optimized extraction techniques, and slightly higher recoveries of three carbamates (propoxur, propham and methiocarb) were achieved using MAE. SFE showed slightly higher recovery for chlorpropham (93 vs. 87% for MAE). The effects of time-aged soil on the extraction of analytes were examined and the results obtained by both methods were also compared.

  6. 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 ...

  7. 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...

  8. 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.

  9. Lipidomics by Supercritical Fluid Chromatography

    Directory of Open Access Journals (Sweden)

    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.

  10. 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

  11. 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.

  12. Application of supercritical fluid extraction in analytical science

    International Nuclear Information System (INIS)

    Kumar, Pradeep

    2015-01-01

    In the recent years, supercritical fluid extraction (SFE) has emerged as a promising alternative to conventional solvent extraction process owing to its potential to minimize the generation of the liquid volume and simplification of the extraction process.This technology is some times referred to as 'green technology' and 'clean technology'. Supercritical fluid extraction process assumes significance as it exhibits practical advantages such as enhanced extraction rate due to rapid mass transfer in supercritical fluid medium and change of solvent properties such as density by tuning pressure/temperature conditions. Supercritical fluids (SCF) offer faster, cleaner and efficient extraction owing to low viscosity, high density, low surface tension and better diffusivity properties. Higher diffusivity than liquids facilitates rapid mass transfer and faster completion of reaction. Due to low viscosity and surface tension, SCF can penetrate deep inside the material, extracting the component of interest. Liquid like solvating characteristics of SCFs enable dissolution of compounds whereas gas like diffusion characteristics provide conditions for high degree of extraction in shorter time duration. CO 2 has been widely employed as supercritical fluid owing to its moderate critical constants (Pc= 72.9 atm, Tc =304.3 K, ñ c = 0.47 g mL -1 ) and attractive properties such as being easily available, recyclable, non-toxic, chemically inert, non inflammable and radio-chemically stable. SCF finds application in variety of fields. In nuclear industry for separation and purification of actinides from liquids and solid matrices. In food industry, Decaffeination of coffee is done by SCF. Pharmaceutical industry, organic compounds can be extracted from plants by SC CO 2 avoiding liquid solvent usage. SCF may also be utilised for the production of fine powders. In polymer and plastics industries, examples of applications include the impregnation of medical material

  13. 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.

  14. 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

  15. 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. 

  16. Evaluation of innovative stationary phase ligand chemistries and analytical conditions for the analysis of basic drugs by supercritical fluid chromatography.

    Science.gov (United States)

    Desfontaine, Vincent; Veuthey, Jean-Luc; Guillarme, Davy

    2016-03-18

    Similar to reversed phase liquid chromatography, basic compounds can be highly challenging to analyze by supercritical fluid chromatography (SFC), as they tend to exhibit poor peak shape, especially those with high pKa values. In this study, three new stationary phase ligand chemistries available in sub -2 μm particle sizes, namely 2-picolylamine (2-PIC), 1-aminoanthracene (1-AA) and diethylamine (DEA), were tested in SFC conditions for the analysis of basic drugs. Due to the basic properties of these ligands, it is expected that the repulsive forces may improve peak shape of basic substances, similarly to the widely used 2-ethypyridine (2-EP) phase. However, among the 38 tested basic drugs, less of 10% displayed Gaussian peaks (asymmetry between 0.8 and 1.4) using pure CO2/methanol on these phases. The addition of 10mM ammonium formate as mobile phase additive, drastically improved peak shapes and increased this proportion to 67% on 2-PIC. Introducing the additive in the injection solvent rather than in the organic modifier, gave acceptable results for 2-PIC only, with 31% of Gaussian peaks with an average asymmetry of 1.89 for the 38 selected basic drugs. These columns were also compared to hybrid silica (BEH), DIOL and 2-EP stationary phases, commonly employed in SFC. These phases commonly exhibit alternative retention and selectivity. In the end, the two most interesting ligands used as complementary columns were 2-PIC and BEH, as they provided suitable peak shapes for the basic drugs and almost orthogonal selectivities. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. 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.

  18. Studies on In-situ Chelation/Supercritical Fluid Extraction of Lanthanides and Actinides Using a Radiotracer Technique

    International Nuclear Information System (INIS)

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

    2001-01-01

    Radioisotope tracer techniques were used to study the process of in-situ chelation/supercritical fluid extraction(SFE) of La3+ and Lu3+ from solid matrix using mixed ligand hexafluoroacetylacetone (HFA) and tributylphosphate (TBP) as chelating agents. A lab-built SFE extactor was used in this study and the extractor design was optimized based on the experimental results. Quantitative recovery of La and Lu was achieved when the extrator design was optimized. Extraction of uranium from real world samples was also investigated to demonstrate the capability of this chelation/SFE technology for environmental remediation applications. A novel on-line back extraction technique for the recovery of metal ions and regeneration of ligands is also reported.

  19. The synergistic effect of complex ligands for radioactive metal salts decontamination in supercritical CO2

    International Nuclear Information System (INIS)

    Go, M. S.; Park, K. H.; Kim, H. W.; Kim, H. D.

    2004-01-01

    The organophosphorus and dithiocarbamate ligands were used to extract five metal ions (Cd 2+ , Co 2+ , Cu 2+ , Pb 2+ , Zn 2+ ) in supercritical CO 2 so as to decontaminate the radioactive contaminants. The experiments confirmed that the ligands mixed together in a variety of the mixing ratios efficiently extracted all metal ions by more than 90% due to its synergistic effect. The UV-Vis spectrometer installed in a high-pressurized cell showed that the NaDDC was decomposed in supercritical CO 2 containing the water. It also proved that the synergistic effect improved the deprotonation of the organophosphorus ligand when NaDDC was used together with. In addition, we mixed organophosphorus ligand together with diethylamine, the decomposed NaDDC, to obtain the same extraction result of more than 90% as with NaDDC. The enhanced extraction efficiency shows the synergistic effect that is produced by combining two ligands together

  20. 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.

  1. 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

  2. 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...

  3. 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.

  4. CO{sub 2}-based supercritical fluids as environmentally-friendly processing solvents

    Energy Technology Data Exchange (ETDEWEB)

    Rubin, J.B.; Davenhall, L.B.; Taylor, C.M.V.; Pierce, T. [Los Alamos National Lab., NM (United States). Physical Organic Chemistry Group; Tiefert, K. [Hewlett-Packard Co., Inc., Santa Clara, CA (United States)

    1999-03-01

    The production of integrated circuits involves a number of discrete steps that utilize hazardous or regulated solvents. Environmental, safety and health considerations associated with these chemicals have prompted a search for alternative, more environmentally benign, solvent systems. An emerging technology for conventional solvent replacement is the use of supercritical fluids based on carbon dioxide (CO{sub 2}). Supercritical CO{sub 2} (SCCO{sub 2}) is an excellent choice for IC manufacturing processes since it is non-toxic, non-flammable, inexpensive, and is compatible with all substrate and metallizations systems. Also, conditions of temperature and pressure needed to achieve the supercritical state are easily achievable with existing process equipment. The authors first describe the general properties of supercritical fluids, with particular emphasis on their application as alternative solvents. Next, they review some of the work which has been published involving the use of supercritical fluids, and particularly CO{sub 2}, as they may be applied to the various steps of IC manufacture, including wafer cleaning, thin film deposition, etching, photoresist stripping, and waste treatment. Next, they describe the research work conducted at Los Alamos, on behalf of Hewlett-Packard, on the use of SCCO{sub 2} in a specific step of the IC manufacturing process: the stripping of hard-baked photoresist.

  5. 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.

  6. 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.

  7. 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 ...

  8. 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.

  9. 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.

  10. 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.

  11. Fluid dynamic effects on precision cleaning with supercritical fluids

    Energy Technology Data Exchange (ETDEWEB)

    Phelps, M.R.; Hogan, M.O.; Silva, L.J.

    1994-06-01

    Pacific Northwest Laboratory staff have assembled a small supercritical fluids parts cleaning test stand to characterize how system dynamics affect the efficacy of precision cleaning with supercritical carbon dioxide. A soiled stainless steel coupon, loaded into a ``Berty`` autoclave, was used to investigate how changes in system turbulence and solvent temperature influenced the removal of test dopants. A pulsed laser beam through a fiber optic was used to investigate real-time contaminant removal. Test data show that cleaning efficiency is a function of system agitation, solvent density, and temperature. These data also show that high levels of cleaning efficiency can generally be achieved with high levels of system agitation at relatively low solvent densities and temperatures. Agitation levels, temperatures, and densities needed for optimal cleaning are largely contaminant dependent. Using proper system conditions, the levels of cleanliness achieved with supercritical carbon dioxide compare favorably with conventional precision cleaning methods. Additional research is currently being conducted to generalize the relationship between cleaning performance and parameters such as contaminant solubilities, mass transfer rates, and solvent agitation. These correlations can be used to optimize cleaning performance, system design, and time and energy consumption for particular parts cleaning applications.

  12. 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.

  13. Supercritical fluid extraction of uranium and thorium from nitric acid medium using organophosphorous compounds

    Energy Technology Data Exchange (ETDEWEB)

    Pitchaiah, K.C.; Sujatha, K.; Rao, C.V.S. Brahmmananda; Subramaniam, S.; Sivaraman, N.; Rao, P.R. Vasudeva [Indira Gandhi Centre for Atomic Research, Kalpakkam (India). Chemistry Group

    2015-06-01

    In recent years, Supercritical Fluid Extraction (SFE) technique has been widely used for the extraction of metal ions. In the present study, extraction of uranium from nitric acid medium was investigated using supercritical carbon dioxide (Sc-CO{sub 2}) containing various organophosphorous compounds such as trialkyl phosphates e.g. tri-iso-amyl phosphate (TiAP), tri-sec-butyl phosphate (TsBP) and tri-n-butyl phosphate (TBP), dialkylalkyl phosphonates, e.g. diamylamyl phosphonate (DAAP) and dibutyl butyl phosphonate (DBBP), dialkyl hydrogen phosphonates, e.g. dioctyl hydrogen phosphonate (DOHP), dioctylphosphineoxide (DOPO), trioctyl phosphine oxide (TOPO), n-octylphenyl N,N-diisobutyl carbamoylmethylphosphine oxide (CMPO) and di-2-ethyl-hexyl phosphoric acid (HDEHP). Some of these ligands have been investigated for the first time in the supercritical phase for the extraction of uranium. The extraction efficiency of uranium was studied with TiAP, DAAP and DBBP as a function of nitric acid concentration; the kinetics of the equilibration period (static extraction) and transportation of the metal complex (dynamic extraction) was investigated. The influence of pressure and temperature on the extraction behaviour of uranium with DAAP was studied from 4 N HNO{sub 3}. The extraction efficiency of uranium from 4 N nitric acid medium was found to increase in the order of phosphates < phosphonates < HDEHP < TOPO < CMPO. In the case of phosphates and phosphonates, the maximum extraction of uranium was found to be from 4 N HNO{sub 3} medium. The acidic extractants, HDEHP and DOHP showed relatively higher extraction at lower acidities. The relative extraction of uranium and thorium from their mixture was also examined using Sc-CO{sub 2} containing phosphates, phosphonates and TOPO. The ligand, TsBP provided better fractionation between uranium and thorium compared to trialkyl phosphates, dialkyl alkyl phosphonates and TOPO.

  14. Decontamination of Metal Ions in Soil by Supercritical CO{sub 2} Extraction with Catecholamine Ligand

    Energy Technology Data Exchange (ETDEWEB)

    Park, Jihye; Kim, Hakwon; Park, Kwangheon [Kyunghee University, Yongin (Korea, Republic of)

    2015-10-15

    The role of fuel cladding and reactor vessels is to help prevent the leakage of radioactive materials, including the fission products. However, if these shielding materials are damaged by a severe disaster such as the Fukushima Accident, radioactive materials could leak outside of a power plant site. Indeed, after the Fukushima Accident, radioactive materials have been detected in air and water samples. The air and water pollution lead to soil pollution, which is particularly difficult to decontaminate, as soil pollution has several types that vary according to the characteristics of a pollutant or its area. The existing decontamination methods generate a secondary waste owing to use of chemical toxicity solvents. It is also disadvantageous due to the additional cost of handling them. Therefore, new effective decontamination methods that reduce the use of toxicity solvents are necessary. For example, using supercritical CO{sub 2} has been studied as a new decontamination method. This study examines the method of decontaminating metallic ions inside of the soil using supercritical CO{sub 2} and a catecholamine compound. This study examined the effects of extracting metallic ions inside the soil using supercritical CO{sub 2} and catecholamine as the ligand. Based on these results, it is evident that when only the extraction agent was used, there was no extraction effect and that only when the ligand, co-ligand, and additive were used together was there an extraction effect. Following this, the optimal extraction-agent ratio was confirmed using varying amounts of extraction agents. The most effective extraction ratio of ligand to co-ligand was 1:2 in E-9 when 0.3 ml of H{sub 2}O were added.

  15. 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).

  16. 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).

  17. 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.

  18. 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

  19. 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.

  20. 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.

  1. 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

  2. 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.

  3. 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

  4. 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

  5. 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...

  6. 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.

  7. 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

  8. 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.

  9. 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

  10. Development of artificial neural network models for supercritical fluid solvency in presence of co-solvents

    Energy Technology Data Exchange (ETDEWEB)

    Shokir, Eissa Mohamed El-Moghawry; El-Midany, Ayman Abdel-Hamid [Cairo University, Giza (Egypt); Al-Homadhi, Emad Souliman; Al-Mahdy, Osama [King Saud University, Riyadh (Saudi Arabia)

    2014-08-15

    This paper presents the application of artificial neural networks (ANN) to develop new models of liquid solvent dissolution of supercritical fluids with solutes in the presence of cosolvents. The neural network model of the liquid solvent dissolution of CO{sub 2} was built as a function of pressure, temperature, and concentrations of the solutes and cosolvents. Different experimental measurements of liquid solvent dissolution of supercritical fluids (CO{sub 2}) with solutes in the presence of cosolvents were collected. The collected data are divided into two parts. The first part was used in building the models, and the second part was used to test and validate the developed models against the Peng- Robinson equation of state. The developed ANN models showed high accuracy, within the studied variables range, in predicting the solubility of the 2-naphthol, anthracene, and aspirin in the supercritical fluid in the presence and absence of co-solvents compared to (EoS). Therefore, the developed ANN models could be considered as a good tool in predicting the solubility of tested solutes in supercritical fluid.

  11. 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.

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

    Directory of Open Access Journals (Sweden)

    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.

  13. 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)

  14. 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

  15. 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.

  16. 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.

  17. 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)

  18. 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)

  19. 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.)

  20. 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.

  1. 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 ...

  2. 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

  3. 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

  4. 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

  5. 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

  6. 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

  7. 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

  8. 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

  9. 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

  10. 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

  11. 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

    Directory of Open Access Journals (Sweden)

    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.

  12. 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.

  13. 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

  14. 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.

  15. 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.

  16. 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...

  17. 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

  18. 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....

  19. 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.

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

    Directory of Open Access Journals (Sweden)

    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.

  1. 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.

  2. 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

    Full Text Available Le taux moyen de récupération par drainage naturel des gisements pétroliers atteint à peine 30 %. La récupération assistée désigne l'ensemble des procédés d'exploitation qui permettent d'accroître très sensiblement ce taux. Parmi ces procédés, l'injection de fluides supercritiques joue un rôle prometteur. Les principaux fluides actuellement utilisés sont : le méthane (ou plus généralement les gaz hydrocarbures dits pauvres , l'azote et enfin le gaz carbonique. Les domaines d'application et les mécanismes thermodynamiques mis en jeu sont brièvement exposés, les sources de fluides supercritiques disponibles au voisinage des gisements pétroliers sont rapidement répertoriées et certains problèmes d'exploitation évoqués. Outre leur application en récupération assistée, les fluides supercritiques sont également impliqués dans des procédés de raffinage et d'extraction divers. C'est le procédé de désasphaltage de fractions pétrolières lourdes qui, en 1956, a fait l'objet de la première application industrielle exploitant les fortes variations du pouvoir solvant d'un fluide au voisinage de son point critique. Ce procédé connaît, depuis une dizaine d'années, un regain d'intérêt du fait de l'économie d'énergie qu'il permet de réaliser. D'autre part, les schistes bitumineux, les sables asphaltiques et les charbons, sources d'hydrocarbures considérables pour l'avenir, constituent des domaines d'applications potentielles originales des fluides supercritiques. Les procédés spécifiques, pour la plupart en cours de développement au stade pilote, sont passés en revue. The average recovery by natural drainage from oil fields is barely 30%. Enhanced recovery includes all production processes which appreciably increase this rate. Among such processes, supercritical fluid flooding is quite promising. The main fluids now used are methane (or, more generally, so-called leangaseous hydrocarbons, nitrogen and carbon

  3. 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

  4. 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

  5. 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.

  6. 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

  7. 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.

  8. 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)

  9. 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.

  10. 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

  11. 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.

  12. 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

  13. 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.

  14. 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

  15. Solvent density inhomogeneities and solvation free energies in supercritical diatomic fluids: a density functional approach.

    Science.gov (United States)

    Husowitz, B; Talanquer, V

    2007-02-07

    Density functional theory is used to explore the solvation properties of a spherical solute immersed in a supercritical diatomic fluid. The solute is modeled as a hard core Yukawa particle surrounded by a diatomic Lennard-Jones fluid represented by two fused tangent spheres using an interaction site approximation. The authors' approach is particularly suitable for thoroughly exploring the effect of different interaction parameters, such as solute-solvent interaction strength and range, solvent-solvent long-range interactions, and particle size, on the local solvent structure and the solvation free energy under supercritical conditions. Their results indicate that the behavior of the local coordination number in homonuclear diatomic fluids follows trends similar to those reported in previous studies for monatomic fluids. The local density augmentation is particularly sensitive to changes in solute size and is affected to a lesser degree by variations in the solute-solvent interaction strength and range. The associated solvation free energies exhibit a nonmonotonous behavior as a function of density for systems with weak solute-solvent interactions. The authors' results suggest that solute-solvent interaction anisotropies have a major influence on the nature and extent of local solvent density inhomogeneities and on the value of the solvation free energies in supercritical solutions of heteronuclear molecules.

  16. 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

  17. 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.

  18. 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.

  19. 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.

  20. Supercritical fluid extraction of uranium and thorium using modifier free delivery of ligands

    International Nuclear Information System (INIS)

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

    2009-01-01

    The modifier free controlled delivery of octyl (phenyl)-N,N-diisobutylcarbamoylmethy phosphineoxide (CMPO) using supercritical carbon dioxide was established for the extraction of uranyl nitrate as well as uranyl nitrate sorbed on tissue paper matrix and the results were compared with modifier method. The preferential extraction of uranium over thorium was also demonstrated using di (2-ethylhexyl)isobutyramide (D2EHIBA). (author)

  1. 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

  2. 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

  3. 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

  4. 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

  5. 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)

  6. 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)

  7. 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

  8. 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)

  9. 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)

  10. Investigation of Thermal and Thermomechanical Properties of Biodegradable PLA/PBSA Composites Processed via Supercritical Fluid-Assisted Foam Injection Molding

    Directory of Open Access Journals (Sweden)

    Sai Aditya Pradeep

    2017-01-01

    Full Text Available Bio-based polymer foams have been gaining immense attention in recent years due to their positive contribution towards reducing the global carbon footprint, lightweighting, and enhancing sustainability. Currently, polylactic acid (PLA remains the most abundant commercially consumed biopolymer, but suffers from major drawbacks such as slow crystallization rate and poor melt processability. However, blending of PLA with a secondary polymer would enhance the crystallization rate and the thermal properties based on their compatibility. This study investigates the physical and compatibilized blends of PLA/poly (butylene succinate-co-adipate (PBSA processed via supercritical fluid-assisted (ScF injection molding technology using nitrogen (N2 as a facile physical blowing agent. Furthermore, this study aims at understanding the effect of blending and ScF foaming of PLA/PBSA on crystallinity, melting, and viscoelastic behavior. Results show that compatibilization, upon addition of triphenyl phosphite (TPP, led to an increase in molecular weight and a shift in melting temperature. Additionally, the glass transition temperature (Tg obtained from the tanδ curve was observed to be in agreement with the Tg value predicted by the Gordon–Taylor equation, further confirming the compatibility of PLA and PBSA. The compatibilization of ScF-foamed PLA–PBSA was found to have an increased crystallinity and storage modulus compared to their physically foamed counterparts.

  11. 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.

  12. 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

  13. 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

  14. 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.

  15. 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)

  16. 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)

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

    Directory of Open Access Journals (Sweden)

    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

  18. 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

  19. 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.

  20. 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

  1. 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...

  2. 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

  3. 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.

  4. 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

  5. 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

  6. 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.

  7. High-performance separation and supercritical extraction of lanthanides and actinides

    International Nuclear Information System (INIS)

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

    2010-01-01

    Extensive studies were carried out at Chemistry Group, IGCAR for the rapid separation of individual lanthanides and actinides using dynamic ion-exchange chromatographic technique. The atom percent fission was determined from the concentrations of the lanthanide fission products, uranium and plutonium contents of dissolver solution. These advantages were exploited to significantly reduce analysis time, liquid waste generation as well as dose to operator. Supercritical fluid extraction (SFE) of actinides from waste matrices was studied in detail at our laboratory using modified supercritical carbon dioxide (Sc-CO 2 ). Complete extraction and recovery of uranium, plutonium and americium from various matrices was achieved using Sc-CO 2 modified with suitable ligands. The technique was demonstrated for the recovery of plutonium from actual waste received from different laboratories. (author)

  8. 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

  9. 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.

  10. 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

  11. 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

  12. 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.

  13. 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.

  14. 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

  15. 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

  16. 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.

  17. Prediction of supercritical carbon dioxide drying of food products in packed beds

    NARCIS (Netherlands)

    Almeida-Rivera, C.; Khalloufi, S.; Bongers, P.M.M.

    2010-01-01

    Drying assisted by supercritical carbon dioxide is foreseen to become a promising technology for sensitive food products. In this contribution, a mathematical model is derived to describe the changes in water concentration in both a solid food matrix and a fluid carrier during drying. Finite

  18. 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.

  19. 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...

  20. 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.

  1. 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

  2. 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.

  3. 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.

  4. Microbial Inactivation by Ultrasound Assisted Supercritical Fluids

    Science.gov (United States)

    Benedito, Jose; Ortuño, Carmen; Castillo-Zamudio, Rosa Isela; Mulet, Antonio

    A method combining supercritical carbon dioxide (SC-CO2) and high power ultrasound (HPU) has been developed and tested for microbial/enzyme inactivation purposes, at different process conditions for both liquid and solid matrices. In culture media, using only SC-CO2, the inactivation rate of E. coli and S. cerevisiae increased with pressure and temperature; and the total inactivation (7-8 log-cycles) was attained after 25 and 140 min of SC-CO2 (350 bar, 36 °C) treatment, respectively. Using SC-CO2+HPU, the time for the total inactivation of both microorganisms was reduced to only 1-2 min, at any condition selected. The SC-CO2+HPU inactivation of both microorganisms was slower in juices (avg. 4.9 min) than in culture media (avg. 1.5 min). In solid samples (chicken, turkey ham and dry-cured pork cured ham) treated with SC-CO2 and SC-CO2+HPU, the inactivation rate of E. coli increased with temperature. The application of HPU to the SC-CO2 treatments accelerated the inactivation rate of E. coli and that effect was more pronounced in treatments with isotonic solution surrounding the solid food samples. The application of HPU enhanced the SC-CO2 inactivation mechanisms of microorganisms, generating a vigorous agitation that facilitated the CO2 solubilization and the mass transfer process. The cavitation generated by HPU could damage the cell walls accelerating the extraction of vital constituents and the microbial death. Thus, using the combined technique, reasonable industrial processing times and mild process conditions could be used which could result into a cost reduction and lead to the minimization in the food nutritional and organoleptic changes.

  5. 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.

  6. 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

  7. 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.

  8. 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)

  9. Extraction fatty acid as a source to produce biofuel in microalgae Chlorella sp. and Spirulina sp. using supercritical carbon dioxide

    Science.gov (United States)

    Tai, Do Chiem; Hai, Dam Thi Thanh; Vinh, Nguyen Hanh; Phung, Le Thi Kim

    2016-06-01

    In this research, the fatty acids of isolated microalgae were extracted by some technologies such as maceration, Soxhlet, ultrasonic-assisted extraction and supercritical fluid extraction; and analyzed for biodiesel production using GC-MS. This work deals with the extraction of microalgae oil from dry biomass by using supercritical fluid extraction method. A complete study at laboratory of the influence of some parameters on the extraction kinetics and yields and on the composition of the oil in terms of lipid classes and profiles is proposed. Two types of microalgae were studied: Chlorella sp. and Spirulina sp. For the extraction of oil from microalgae, supercritical CO2 (SC-CO2) is regarded with interest, being safer than n-hexane and offering a negligible environmental impact, a short extraction time and a high-quality final product. Whilst some experimental papers are available on the supercritical fluid extraction (SFE) of oil from microalgae, only limited information exists on the kinetics of the process. These results demonstrate that supercritical CO2 extraction is an efficient method for the complete recovery of the neutral lipid phase.

  10. 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.

  11. 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

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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

  18. 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

  19. 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

  20. 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

  1. 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.

  2. 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...

  3. 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.

  4. 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...

  5. 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

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. 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 ...

  12. 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.

  13. 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.

  14. 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)

  15. 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

  16. 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.

  17. 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

  18. 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.

  19. 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

  20. 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

  1. 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.

  2. 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

  3. 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.

  4. 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.

  5. 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

  6. Levels of soluble delta-like ligand 1 in the serum and cerebrospinal fluid of tuberculous meningitis patients

    Institute of Scientific and Technical Information of China (English)

    Jinghong Li; Jinyi Li; Yanjie Jia

    2012-01-01

    In this study, the levels of soluble delta-like ligand 1 in cerebrospinal fluid and serum of 50 patients with tuberculous meningitis, 30 patients with viral meningitis, 20 patients with purulent meningitis and 40 subjects without central nervous system disease were determined using an enzyme-linked immunosorbent assay. The mean levels of soluble delta-like ligand 1 in both cerebrospinal fluid and serum from patients with tuberculous meningitis were significantly higher compared with those from patients with viral meningitis or purulent meningitis or from subjects without central nervous system disease. Meanwhile, the level of soluble delta-like ligand 1 gradually decreased as tuberculous meningitis patients recovered. If patients deteriorated after treatment, the level of soluble delta-like ligand 1 in cerebrospinal fluid gradually increased. There was no correlation between the level of soluble delta-like ligand 1 and the protein level/cell number in cerebrospinal fluid. Our findings in-dicate that the levels of soluble delta-like ligand 1 in cerebrospinal fluid and serum are reliable markers for the diagnosis of tuberculous meningitis and for monitoring treatment progress. At the same time, this index is not influenced by protein levels or cell numbers in cerebrospinal fluid.

  7. 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

  8. 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.

  9. 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

  10. 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

  11. 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.

  12. Decontamination of Metal Ions in Soil by Supercritical CO2 Extraction with Crown Ether

    Energy Technology Data Exchange (ETDEWEB)

    Park, Jihe; Park, Kwangheon [Kyunghee University, Yongin (Korea, Republic of)

    2015-05-15

    Previous decontamination methods have shortcomings in that they produce additional waste due to the usage of solutions with chemical toxicity. Hence, demand is strong for new decontamination methods that can guarantee effective decontamination while decreasing the chemical solution. In particular, methods using supercritical CO2 as a means of decontamination are currently in progress. This study examines the method of decontaminating metallic ions inside soil using supercritical CO2. This paper examined the effects of extracting metallic ions inside soil using supercritical CO2 and crown ether as the ligand. It was confirmed that extraction effectiveness increases following greater usage of ligand and co-ligand, with a drastic increase in extraction effectiveness when using extracts over a certain dose. Moreover, it was shown that if the usage of ligand and additive decreases, the extraction ratio also decreases.

  13. Decontamination of Metal Ions in Soil by Supercritical CO2 Extraction with Crown Ether

    International Nuclear Information System (INIS)

    Park, Jihe; Park, Kwangheon

    2015-01-01

    Previous decontamination methods have shortcomings in that they produce additional waste due to the usage of solutions with chemical toxicity. Hence, demand is strong for new decontamination methods that can guarantee effective decontamination while decreasing the chemical solution. In particular, methods using supercritical CO2 as a means of decontamination are currently in progress. This study examines the method of decontaminating metallic ions inside soil using supercritical CO2. This paper examined the effects of extracting metallic ions inside soil using supercritical CO2 and crown ether as the ligand. It was confirmed that extraction effectiveness increases following greater usage of ligand and co-ligand, with a drastic increase in extraction effectiveness when using extracts over a certain dose. Moreover, it was shown that if the usage of ligand and additive decreases, the extraction ratio also decreases

  14. Preparation of rifampicin/poly(d,l-lactice) nanoparticles for sustained release by supercritical assisted atomization technique

    CSIR Research Space (South Africa)

    Labuschagne, Philip W

    2014-11-01

    Full Text Available In this work supercritical assisted atomization (SAA) process was used for the co-precipitation of poly(d,l-lactide) (PDLLA) and rifampicin (RIF) as nanoparticles for sustained release applications. The effect of the variation of PDLLA/RIF ratio...

  15. 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...

  16. 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.

  17. 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)

  18. 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.

  19. 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.

  20. Supercritical Carbon Dioxide and Its Potential as a Life-Sustaining Solvent in a Planetary Environment

    Directory of Open Access Journals (Sweden)

    Nediljko Budisa

    2014-08-01

    Full Text Available Supercritical fluids have different properties compared to regular fluids and could play a role as life-sustaining solvents on other worlds. Even on Earth, some bacterial species have been shown to be tolerant to supercritical fluids. The special properties of supercritical fluids, which include various types of selectivities (e.g., stereo-, regio-, and chemo-selectivity have recently been recognized in biotechnology and used to catalyze reactions that do not occur in water. One suitable example is enzymes when they are exposed to supercritical fluids such as supercritical carbon dioxide: enzymes become even more stable, because they are conformationally rigid in the dehydrated state. Furthermore, enzymes in anhydrous organic solvents exhibit a “molecular memory”, i.e., the capacity to “remember” a conformational or pH state from being exposed to a previous solvent. Planetary environments with supercritical fluids, particularly supercritical carbon dioxide, exist, even on Earth (below the ocean floor, on Venus, and likely on Super-Earth type exoplanets. These planetary environments may present a possible habitat for exotic life.

  1. 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

  2. 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.

  3. 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.

  4. 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.

  5. 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

  6. A Fluid Membrane-Based Soluble Ligand Display System for Live CellAssays

    Energy Technology Data Exchange (ETDEWEB)

    Nam, Jwa-Min; Nair, Pradeep N.; Neve, Richard M.; Gray, Joe W.; Groves, Jay T.

    2005-10-14

    Cell communication modulates numerous biological processes including proliferation, apoptosis, motility, invasion and differentiation. Correspondingly, there has been significant interest in the development of surface display strategies for the presentation of signaling molecules to living cells. This effort has primarily focused on naturally surface-bound ligands, such as extracellular matrix components and cell membranes. Soluble ligands (e.g. growth factors and cytokines) play an important role in intercellular communications, and their display in a surface-bound format would be of great utility in the design of array-based live cell assays. Recently, several cell microarray systems that display cDNA, RNAi, or small molecules in a surface array format were proven to be useful in accelerating high-throughput functional genetic studies and screening therapeutic agents. These surface display methods provide a flexible platform for the systematic, combinatorial investigation of genes and small molecules affecting cellular processes and phenotypes of interest. In an analogous sense, it would be an important advance if one could display soluble signaling ligands in a surface assay format that allows for systematic, patterned presentation of soluble ligands to live cells. Such a technique would make it possible to examine cellular phenotypes of interest in a parallel format with soluble signaling ligands as one of the display parameters. Herein we report a ligand-modified fluid supported lipid bilayer (SLB) assay system that can be used to functionally display soluble ligands to cells in situ (Figure 1A). By displaying soluble ligands on a SLB surface, both solution behavior (the ability to become locally enriched by reaction-diffusion processes) and solid behavior (the ability to control the spatial location of the ligands in an open system) could be combined. The method reported herein benefits from the naturally fluid state of the supported membrane, which allows

  7. 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

  8. 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

  9. 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)).

  10. Functionalization of whey proteins by reactive supercritical fluid extrusion

    Directory of Open Access Journals (Sweden)

    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.

  11. 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

    Directory of Open Access Journals (Sweden)

    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

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.)

  17. Optimization of supercritical fluid extraction and HPLC identification of wedelolactone from Wedelia calendulacea by orthogonal array design.

    Science.gov (United States)

    Patil, Ajit A; Sachin, Bhusari S; Wakte, Pravin S; Shinde, Devanand B

    2014-11-01

    The purpose of this work is to provide a complete study of the influence of operational parameters of the supercritical carbon dioxide assisted extraction (SC CO2E) on yield of wedelolactone from Wedelia calendulacea Less., and to find an optimal combination of factors that maximize the wedelolactone yield. In order to determine the optimal combination of the four factors viz. operating pressure, temperature, modifier concentration and extraction time, a Taguchi experimental design approach was used: four variables (three levels) in L9 orthogonal array. Wedelolactone content was determined using validated HPLC methodology. Optimum extraction conditions were found to be as follows: extraction pressure, 25 MPa; temperature, 40 °C; modifier concentration, 10% and extraction time, 90 min. Optimum extraction conditions demonstrated wedelolactone yield of 8.01 ± 0.34 mg/100 g W. calendulacea Less. Pressure, temperature and time showed significant (p yield. The supercritical carbon dioxide extraction showed higher selectivity than the conventional Soxhlet assisted extraction method.

  18. 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.

  19. 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.

  20. 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.

  1. 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)

  2. 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

  3. 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.

  4. 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)

  5. 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

  6. 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

  7. Systematic investigations of peak deformations due to co-solvent adsorption in preparative supercritical fluid chromatography.

    Science.gov (United States)

    Glenne, Emelie; Leek, Hanna; Klarqvist, Magnus; Samuelsson, Jörgen; Fornstedt, Torgny

    2017-05-05

    Strangely shaped overloaded bands were recently reported using a standard supercritical fluid chromatographic system comprising a diol column as the stationary phase and carbon dioxide with methanol as the mobile phase. Some of these overloaded elution profiles appeared strongly deformed and even had "anti-Langmuirian" shapes although their solute compounds had "Langmuirian" adsorption. To obtain a more complete understanding of the generality of these effects, the investigation was expanded to cover also other common co-solvents, such as ethanol, 2-propanol, and acetonitrile, as well as various stationary phase materials, such as silica, and 2-ethylpyridine. From this expanded study it could be confirmed that the effects of deformed overloaded solute band shapes, due to co-solvent adsorption, is general phenomena in supercritical fluid chromatographic. It could also be concluded that these effects as well as previously observed "solvent effects" or "plug effects" are entirely due to competition between the solute and solvent molecules for the adsorption sites on the stationary phase surface. Finally, guidelines were given for how to evaluate the risk of deformations occurring for a given solvent-column combination, based simply on testing retention times of solutes and co-solvent. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Supercritical CO₂assisted extraction and LC-MS identification of picroside I and picroside II from Picrorhiza kurroa.

    Science.gov (United States)

    Patil, Ajit A; Sachin, Bhusari S; Shinde, Devanand B; Wakte, Pravin S

    2013-02-01

    Picroside I and picroside II have been studied intensively because of their pharmacological actions and clinical applications. Numerous methods have been reported for extracting picroside I and picroside II from Picrorrhiza. kurroa rhizomes. This is the first report of picroside I and picroside II extraction using the supercritical carbon dioxide assisted extraction technique. To develop supercritical carbon dioxide assisted extraction and LC-MS identification of picroside I and picroside II from the Picrorrhiza kurroa Royle rhizomes. Surface response methodology based on 3³ fractional factorial design was used to extract picroside I and picroside II from P. kurroa rhizomes. The effects of various process factors, namely temperature (40-80°C), pressure (25-35 MPa) and co-solvent (methanol) concentration (0-10% v/v) on extraction yield of the two compounds were evaluated. The picroside I and picroside II contents were determined using validated LC-MS methodology. The maximum yield of picroside I (32.502 ± 1.131 mg/g) and picroside II (9.717 ± 0.382 mg/g) was obtained at the 10% v/v co-solvent concentration, 40°C temperature and 30 MPa pressure. The conventional Soxhlet assisted methanol extract of P. kurroa powder resulted in 36.743 ± 1.75 and 11.251 ± 0.54 mg/g yield of picroside I and picroside II, respectively. Variation of concentration and extraction time showed a significant effect on the picroside I and picroside II yield. Supercritical carbon dioxide assisted extraction using methanol as a co-solvent is an efficient and environmentally sustainable method for extracting picroside I and picroside II from P. kurroa rhizomes. Copyright © 2012 John Wiley & Sons, Ltd.

  9. 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....

  10. 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.

  11. 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...

  12. 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

  13. 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.

  14. 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

  15. 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.

  16. 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

  17. 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

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. Optimization of supercritical fluid extraction and HPLC identification of wedelolactone from Wedelia calendulacea by orthogonal array design

    Directory of Open Access Journals (Sweden)

    Ajit A. Patil

    2014-11-01

    Full Text Available The purpose of this work is to provide a complete study of the influence of operational parameters of the supercritical carbon dioxide assisted extraction (SC CO2E on yield of wedelolactone from Wedelia calendulacea Less., and to find an optimal combination of factors that maximize the wedelolactone yield. In order to determine the optimal combination of the four factors viz. operating pressure, temperature, modifier concentration and extraction time, a Taguchi experimental design approach was used: four variables (three levels in L9 orthogonal array. Wedelolactone content was determined using validated HPLC methodology. Optimum extraction conditions were found to be as follows: extraction pressure, 25 MPa; temperature, 40 °C; modifier concentration, 10% and extraction time, 90 min. Optimum extraction conditions demonstrated wedelolactone yield of 8.01 ± 0.34 mg/100 g W. calendulacea Less. Pressure, temperature and time showed significant (p < 0.05 effect on the wedelolactone yield. The supercritical carbon dioxide extraction showed higher selectivity than the conventional Soxhlet assisted extraction method.

  3. 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.

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

    Science.gov (United States)

    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.

  5. The coupling of supercritical fluid chromatography and field ionization time-of-flight high-resolution mass spectrometry for rapid and quantitative analysis of petroleum middle distillates.

    Science.gov (United States)

    Qian, Kuangnan; Diehl, John W; Dechert, Gary J; DiSanzo, Frank P

    2004-01-01

    We report the first coupling of supercritical fluid chromatography (SFC) with field ionization time-of-flight high-resolution mass spectrometry (FI-ToF HRMS), in parallel with ultraviolet (UV) detection and flame ionization detection (FID), for rapid and quantitative analysis of petroleum middle distillates. SFC separates petroleum middle distillates into saturates and 1- to 3-ring aromatics. FI generates molecular ions for hydrocarbon species eluted from the SFC. The high resolution and exact mass measurements by ToF mass spectrometry provide elemental compositions of the molecules in the petroleum product. The amounts of saturates and aromatic ring types were quantified using the parallel SFC-FID assisted by SFC-UV. With a proper carbon-number calibration, the detailed composition of the petroleum middle distillate was rapidly determined.

  6. 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.

  7. 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)

  8. 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

  9. 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

  10. 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.

  11. 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.

  12. 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.

  13. Chiral separation of G-type chemical warfare nerve agents via analytical supercritical fluid chromatography.

    Science.gov (United States)

    Kasten, Shane A; Zulli, Steven; Jones, Jonathan L; Dephillipo, Thomas; Cerasoli, Douglas M

    2014-12-01

    Chemical warfare nerve agents (CWNAs) are extremely toxic organophosphorus compounds that contain a chiral phosphorus center. Undirected synthesis of G-type CWNAs produces stereoisomers of tabun, sarin, soman, and cyclosarin (GA, GB, GD, and GF, respectively). Analytical-scale methods were developed using a supercritical fluid chromatography (SFC) system in tandem with a mass spectrometer for the separation, quantitation, and isolation of individual stereoisomers of GA, GB, GD, and GF. Screening various chiral stationary phases (CSPs) for the capacity to provide full baseline separation of the CWNAs revealed that a Regis WhelkO1 (SS) column was capable of separating the enantiomers of GA, GB, and GF, with elution of the P(+) enantiomer preceding elution of the corresponding P(-) enantiomer; two WhelkO1 (SS) columns had to be connected in series to achieve complete baseline resolution. The four diastereomers of GD were also resolved using two tandem WhelkO1 (SS) columns, with complete baseline separation of the two P(+) epimers. A single WhelkO1 (RR) column with inverse stereochemistry resulted in baseline separation of the GD P(-) epimers. The analytical methods described can be scaled to allow isolation of individual stereoisomers to assist in screening and development of countermeasures to organophosphorus nerve agents. © 2014 The Authors. Chirality published by John Wiley Periodicals, Inc.

  14. 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.

  15. 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

  16. 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

  17. Enhancement of antioxidant activity of C-phycocyanin of Spirulina powder treated with supercritical fluid carbon dioxide

    Directory of Open Access Journals (Sweden)

    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

  18. 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

  19. 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.

  20. 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

  1. Sedative and hypnotic effects of supercritical carbon dioxide fluid extraction from Schisandra chinensis in mice

    Directory of Open Access Journals (Sweden)

    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.

  2. Integrated intelligent instruments using supercritical fluid technology for soil analysis

    International Nuclear Information System (INIS)

    Liebman, S.A.; Phillips, C.; Fitzgerald, W.; Levy, E.J.

    1994-01-01

    Contaminated soils pose a significant challenge for characterization and remediation programs that require rapid, accurate and comprehensive data in the field or laboratory. Environmental analyzers based on supercritical fluid (SF) technology have been designed and developed for meeting these global needs. The analyzers are designated the CHAMP Systems (Chemical Hazards Automated Multimedia Processors). The prototype instrumentation features SF extraction (SFE) and on-line capillary gas chromatographic (GC) analysis with chromatographic and/or spectral identification detectors, such as ultra-violet, Fourier transform infrared and mass spectrometers. Illustrations are given for a highly automated SFE-capillary GC/flame ionization (FID) configuration to provide validated screening analysis for total extractable hydrocarbons within ca. 5--10 min, as well as a full qualitative/quantitative analysis in 25--30 min. Data analysis using optional expert system and neural networks software is demonstrated for test gasoline and diesel oil mixtures in this integrated intelligent instrument approach to trace organic analysis of soils and sediments

  3. Visualization study for forced convection heat transfer of supercritical carbon dioxide near pseudo-boiling point

    International Nuclear Information System (INIS)

    Sakurai, K.; Ko, H.S.; Okamoto, K.; Madarame, H.

    2001-01-01

    For development of new reactor, supercritical water is expected to be used as coolant to improve thermal efficiency. However, the thermal characteristics of supercritical fluid is not revealed completely because its difficulty for experiment. Specific phenomena tend to occur near the pseudo-boiling point which is characterised by temperature corresponding to the saturation point in ordinary fluid. Around this point, the physic properties such as density, specific heat and thermal conductivity are drastically varying. Although there is no difference between gas and liquid phases in supercritical fluids, phenomena similar to boiling (with heat transfer deterioration) can be observed round the pseudo-boiling point. Experiments of heat transfer have been done for supercritical fluid in forced convective condition. However, these experiments were mainly realised inside stainless steel cylinder pipes, for which flow visualisation is difficult. Consequently, this work has been devoted to the development of method allowing the visualisation of supercritical flows. The experiment setup is composed of main loop and test section for the visualisation. Carbon dioxide is used as test fluid. Supercritical carbon dioxide flows upward in rectangular channel and heated by one-side wall to generate forced convection heat transfer. Through window at mid-height of the test section, shadowgraphy was applied to visualize density gradient distribution. The behavior of the density wave in the channel is visualized and examined through the variation of the heat transfer coefficient. (author)

  4. Comparison study of moisture content, colour properties and essential oil compounds extracted by hydrodistillation and supercritical fluid extraction between stem and leaves of lemongrass (Cymbopogun citratus)

    Science.gov (United States)

    Kamaruddin, Shazlin; Mustapha, Wan Aida Wan; Haiyee, Zaibunnisa Abdul

    2018-04-01

    The objectives of this study were to compare the properties of moisture content, colour and essential oil compounds between stem and leaves of lemongrass (Cymbopogun citratus). The essential oil was extracted using two different methods which are hydrodistillation and supercritical fluid extraction (SFE). There was no significant difference of moisture content between stem and leaves of lemongrass. The lightness (L) and yellowness (+b) values of the stems were significantly higher (pleaves. The highest yield of essential oil was obtained by extraction using supercritical fluid extraction (SFE) in leaves (˜ 0.7%) by treatment at 1700psi and 50°C. The main compound of extracted essential oil was citral (geranial and neral).

  5. Supercritical Carbon Dioxide-Soluble Ligands for Extracting Actinide Metal Ions from Porous Solids

    International Nuclear Information System (INIS)

    Dietz, Mark L.

    2001-01-01

    Numerous types of actinide-bearing waste materials are found throughout the DOE complex. Most of these wastes consist of large volumes of non-hazardous materials contaminated with relatively small quantities of actinide elements. Separation of these wastes into their inert and radioactive components would dramatically reduce the costs of stabilization and disposal. For example, the DOE is responsible for decontaminating concrete within 7000 surplus contaminated buildings. The best technology now available for removing surface contamination from concrete involves removing the surface layer by grit blasting, which produces a large volume of blasting residue containing a small amount of radioactive material. Disposal of this residue is expensive because of its large volume and fine particulate nature. Considerable cost savings would result from separation of the radioactive constituents and stabilization of the concrete dust. Similarly, gas diffusion plants for uranium enrichment contain valuable high-purity nickel in the form of diffusion barriers. Decontamination is complicated by the extremely fine pores in these barriers, which are not readily accessible by most cleaning techniques. A cost-effective method for the removal of radioactive contaminants would release this valuable material for salvage. The objective of this project is to develop novel, substituted diphosphonic acid ligands that can be used for supercritical carbon dioxide extraction of actinide ions from solid wastes. Specifically, selected diphosphonic acids, which are known to form extremely stable complexes with actinides in aqueous and organic solution, are to be rendered carbon dioxide-soluble by the introduction of appropriate alkyl- or silicon-containing substituents. The metal complexation chemistry of these new ligands in SC-CO2 will then be investigated and techniques for their use in actinide extraction from porous solids developed

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. Nitrate conversion and supercritical fluid extraction of UO{sub 2}-CeO{sub 2} solid solution prepared by an electrolytic reduction-coprecipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, L.Y. [Tsinghua Univ., Beijing (China). Inst. of Nuclear and New Energy Technology; China Institute of Atomic Energy, Beijing (China); Duan, W.H.; Wen, M.F.; Xu, J.M.; Zhu, Y.J. [Tsinghua Univ., Beijing (China). Inst. of Nuclear and New Energy Technology

    2014-04-01

    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{sub 2}O{sub 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{sub 2}-CeO{sub 2} solid solution was prepared as a surrogate for a UO{sub 2}-PuO{sub 2} solid solution, and the recovery of U and Ce from the UO{sub 2}-CeO{sub 2} solid solution with liquid N{sub 2}O{sub 4} and supercritical CO{sub 2} containing tri-n-butyl phosphate (TBP) was investigated. The UO{sub 2}-CeO{sub 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{sub 2}O{sub 4}. The XRD pattern of the nitrates was similar to that of UO{sub 2}(NO{sub 3}){sub 2} . 3H{sub 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{sub 2} containing TBP. The results suggest a promising potential technology for the reprocessing of SNF from HTGRs. (orig.)

  11. Enhanced oral bioavailability of silymarin using liposomes containing a bile salt: preparation by supercritical fluid technology and evaluation in vitro and in vivo

    Science.gov (United States)

    Yang, Gang; Zhao, Yaping; Zhang, Yongtai; Dang, Beilei; Liu, Ying; Feng, Nianping

    2015-01-01

    The aim of this investigation was to develop a procedure to improve the dissolution and bioavailability of silymarin (SM) by using bile salt-containing liposomes that were prepared by supercritical fluid technology (ie, solution-enhanced dispersion by supercritical fluids [SEDS]). The process for the preparation of SM-loaded liposomes containing a bile salt (SM-Lip-SEDS) was optimized using a central composite design of response surface methodology with the ratio of SM to phospholipids (w/w), flow rate of solution (mL/min), and pressure (MPa) as independent variables. Particle size, entrapment efficiency (EE), and drug loading (DL) were dependent variables for optimization of the process and formulation variables. The particle size, zeta potential, EE, and DL of the optimized SM-Lip-SEDS were 160.5 nm, −62.3 mV, 91.4%, and 4.73%, respectively. Two other methods to produce SM liposomes were compared to the SEDS method. The liposomes obtained by the SEDS method exhibited the highest EE and DL, smallest particle size, and best stability compared to liposomes produced by the thin-film dispersion and reversed-phase evaporation methods. Compared to the SM powder, SM-Lip-SEDS showed increased in vitro drug release. The in vivo AUC0−t of SM-Lip-SEDS was 4.8-fold higher than that of the SM powder. These results illustrate that liposomes containing a bile salt can be used to enhance the oral bioavailability of SM and that supercritical fluid technology is suitable for the preparation of liposomes. PMID:26543366

  12. Measurements of mixtures with carbon dioxide under supercritical conditions using commercial high pressure equipment

    Energy Technology Data Exchange (ETDEWEB)

    Andrade, Luciana L.P.R. de; Rutledge, Luis Augusto Medeiros; Moreno, Eesteban L.; Hovell, Ian; Rajagopal, Krishnaswamy [Universidade Federal do Rio de Janeiro (LATCA-EQ-UFRJ), RJ (Brazil). Escola de Quimica. Lab. de Termodinamica e Cinetica Aplicada

    2012-07-01

    There is a growing interest in studying physical properties of binary and multicomponent fluid mixtures with supercritical carbon dioxide (CO{sub 2}) over an extended range of temperature and pressure. The estimation of properties such as density, viscosity, saturation pressure, compressibility, solubility and surface tension of mixtures is important in design, operation and control as well as optimization of chemical processes especially in extractions, separations, catalytic and enzymatic reactions. The phase behaviour of binary and multicomponent mixtures with supercritical CO{sub 2} is also important in the production and refining of petroleum where mixtures of paraffin, naphthene and aromatics with supercritical fluids are often encountered. Petroleum fluids can present a complex phase behaviour in the presence of CO{sub 2}, where two-phase (VLE and LLE) and three phase regions (VLLE) might occur within ranges of supercritical conditions of temperature and pressure. The objective of this study is to develop an experimental methodology for measuring the phase behaviour of mixtures containing CO{sub 2} in supercritical regions, using commercial high-pressure equipment. (author)

  13. [Study on condition for extraction of arctiin from fruits of Arctium lappa using supercritical fluid extraction].

    Science.gov (United States)

    Dong, Wen-hong; Liu, Ben

    2006-08-01

    To study the feasibility of supercritical fluid extraction (SFE) for arctiin from the fruits of Arctium lappa. The extracts were analyzed by HPLC, optimum extraction conditions were studied by orthogonal tests. The optimal extraction conditions were: pressure 40 MPa, temperature 70 degrees C, using methanol as modifier carrier at the rate of 0.55 mL x min(-1), static extraction time 5 min, dynamic extraction 30 min, flow rate of CO2 2 L x min(-1). SFE has the superiority of adjustable polarity, and has the ability of extracting arctiin.

  14. 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.

  15. Simultaneous analysis for water- and fat-soluble vitamins by a novel single chromatography technique unifying supercritical fluid chromatography and liquid chromatography.

    Science.gov (United States)

    Taguchi, Kaori; Fukusaki, Eiichiro; Bamba, Takeshi

    2014-10-03

    Chromatography techniques usually use a single state in the mobile phase, such as liquid, gas, or supercritical fluid. Chromatographers manage one of these techniques for their purpose but are sometimes required to use multiple methods, or even worse, multiple techniques when the target compounds have a wide range of chemical properties. To overcome this challenge, we developed a single method covering a diverse compound range by means of a "unified" chromatography which completely bridges supercritical fluid chromatography and liquid chromatography. In our method, the phase state was continuously changed in the following order; supercritical, subcritical and liquid. Moreover, the gradient of the mobile phase starting at almost 100% CO2 was replaced with 100% methanol at the end completely. As a result, this approach achieved further extension of the polarity range of the mobile phase in a single run, and successfully enabled the simultaneous analysis of fat- and water-soluble vitamins with a wide logP range of -2.11 to 10.12. Furthermore, the 17 vitamins were exceptionally separated in 4min. Our results indicated that the use of dense CO2 and the replacement of CO2 by methanol are practical approaches in unified chromatography covering diverse compounds. Additionally, this is a first report to apply the novel approach to unified chromatography, and can open another door for diverse compound analysis in a single chromatographic technique with single injection, single column and single system. Copyright © 2014. Published by Elsevier B.V.

  16. Study of Variable Turbulent Prandtl Number Model for Heat Transfer to Supercritical Fluids in Vertical Tubes

    Science.gov (United States)

    Tian, Ran; Dai, Xiaoye; Wang, Dabiao; Shi, Lin

    2018-06-01

    In order to improve the prediction performance of the numerical simulations for heat transfer of supercritical pressure fluids, a variable turbulent Prandtl number (Prt) model for vertical upward flow at supercritical pressures was developed in this study. The effects of Prt on the numerical simulation were analyzed, especially for the heat transfer deterioration conditions. Based on the analyses, the turbulent Prandtl number was modeled as a function of the turbulent viscosity ratio and molecular Prandtl number. The model was evaluated using experimental heat transfer data of CO2, water and Freon. The wall temperatures, including the heat transfer deterioration cases, were more accurately predicted by this model than by traditional numerical calculations with a constant Prt. By analyzing the predicted results with and without the variable Prt model, it was found that the predicted velocity distribution and turbulent mixing characteristics with the variable Prt model are quite different from that predicted by a constant Prt. When heat transfer deterioration occurs, the radial velocity profile deviates from the log-law profile and the restrained turbulent mixing then leads to the deteriorated heat transfer.

  17. Supercritical fluid extraction of oregano (Origanum vulgare) essentials oils: anti-inflammatory properties based on cytokine response on THP-1 macrophages.

    Science.gov (United States)

    Ocaña-Fuentes, A; Arranz-Gutiérrez, E; Señorans, F J; Reglero, G

    2010-06-01

    Two fractions (S1 and S2) of an oregano (Origanum vulgare) extract obtained by supercritical fluid extraction have been used to test anti-inflammatory effects on activated human THP-1 cells. The main compounds present in the supercritical extract fractions of oregano were trans-sabinene hydrate, thymol and carvacrol. Fractions toxicity was assessed using the mitochondrial-respiration-dependent 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium (MTT) reduction method for several concentrations during 24 and 48 h of incubation. Concentrations higher than 30 microg/mL of both supercritical S1 and S2 oregano fractions caused a reduction in cell viability in a dose-dependent manner. Oxidized-LDLs (oxLDLs) activated THP-1 macrophages were used as cellular model of atherogenesis and the release/secretion of cytokines (TNT-alpha, IL-1beta, IL-6 and IL-10) and their respective mRNA expressions were quantified both in presence or absence of supercritical oregano extracts. The results showed a decrease in pro-inflammatory TNF-alpha, IL-1beta and IL-6 cytokines synthesis, as well as an increase in the production of anti-inflammatory cytokine IL-10. These results may suggest an anti-inflammatory effect of oregano extracts and their compounds in a cellular model of atherosclerosis. Copyright 2010 Elsevier Ltd. All rights reserved.

  18. Optimizing an advanced hybrid of solar-assisted supercritical CO2 Brayton cycle: A vital transition for low-carbon power generation industry

    International Nuclear Information System (INIS)

    Milani, Dia; Luu, Minh Tri; McNaughton, Robbie; Abbas, Ali

    2017-01-01

    Highlights: • The layout of 14 demonstrative supercritical CO 2 closed Brayton cycles are analysed. • The key parameters of the “combined” cycle are sensitized and optimized. • The effect of thermal efficiency vs HX area on techno-economic nexus is highlighted. • The design of a matching solar heliostat field in direct configuration is revealed. • The water demand for hybrid vs water-only cooling scenarios are assessed. - Abstract: Current worldwide infrastructure of electrical power generation would mostly continue to rely on fossil-fuel but require a modest transition for the ultimate goal of decarbonizing power generation industry. By relying on those already established and carefully managed centrepiece power plants (PPs), we aim at filling the deficits of the current electrical networks with smaller, cleaner, and also more efficient PPs. In this context, we present a unique model for a small-scale decentralized solar-assisted supercritical CO 2 closed Brayton cycle (sCO 2 -CBC). Our model is based on the optimized values of three key performance indicators (KPIs); thermal efficiency, concentrated solar power (CSP) compatibility, and water demand for cooling. For a case-study of 10 MW e CSP-assisted sCO 2 -CBC power plant, our dynamic model shows a 52.7% thermal efficiency and 25.9% solar penetration and up to 80% of water saving in heat-rejection units. These KPIs show significant promise of the solar-assisted supercritical CO 2 power cycle for an imperative transformation in the power industry towards future sustainable electricity generation.

  19. 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.

  20. Supercritical CO2 Extraction of Volatile Thymoquinone from Monarda didyma and M. fistulosa Herbs.

    Czech Academy of Sciences Publication Activity Database

    Sovová, Helena; Sajfrtová, Marie; Topiař, Martin

    2015-01-01

    Roč. 105, OCT (2015), s. 29-34 ISSN 0896-8446. [European Meeting on Supercritical Fluids /14./. Marseille, 18.05.2014-21.05.2014] R&D Projects: GA TA ČR TA01010578 Institutional support: RVO:67985858 Keywords : supercritical fluid extraction * kinetics * volatile oil Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 2.579, year: 2015

  1. Design of experimental system for supercritical CO2 fracturing under confining pressure conditions

    Science.gov (United States)

    Wang, H.; Lu, Q.; Li, X.; Yang, B.; Zheng, Y.; Shi, L.; Shi, X.

    2018-03-01

    Supercritical CO2 has the characteristics of low viscosity, high diffusion and zero surface tension, and it is considered as a new fluid for non-polluting and non-aqueous fracturing which can be used for shale gas development. Fracturing refers to a method of utilizing the high-pressure fluid to generate fractures in the rock formation so as to improve the oil and gas flow conditions and increase the oil and gas production. In this article, a new type of experimental system for supercritical CO2 fracturing under confining pressure conditions is designed, which is based on characteristics of supercritical CO2, shale reservoir and down-hole environment. The experimental system consists of three sub-systems, including supercritical CO2 generation system, supercritical CO2 fracturing system and data analysis system. It can be used to simulate supercritical CO2 fracturing under geo-stress conditions, thus to study the rock initiation pressure, the formation of the rock fractures, fractured surface morphology and so on. The experimental system has successfully carried out a series of supercritical CO2 fracturing experiments. The experimental results confirm the feasibility of the experimental system and the high efficiency of supercritical CO2 in fracturing tight rocks.

  2. Prediction of wall friction for fluids at supercritical pressure with CFD models

    International Nuclear Information System (INIS)

    Angelucci, M.; Ambrosini, W.; Forgione, N.

    2011-01-01

    In this paper, the STAR-CCM+ CFD code is used in the attempt to reproduce the values of friction factor observed in experimental data at supercritical pressures at various operating conditions. A short survey of available data and correlations for smooth pipe friction in circular pipes puts the basis for the discussion, reporting observed trends of friction factor in the liquid-like and the gas-like regions and within the transitional region around the pseudo-critical temperature. For smooth pipes, a general decrease of the friction factor in the transitional region is reported, constituting one of the relevant effects to be predicted by the computational fluid-dynamic models. A limited number of low-Reynolds number models is adopted, making use of refined near-wall discretisations as required by the constraint y + < 1 at the wall. In particular, the Lien k-ε and the SST k-ω models are considered. The values of the wall shear stress calculated by the code are then post-processed on the basis of bulk fluid properties to obtain the Fanning and then the Darcy-Weisbach friction factors, basing on their classical definitions. The obtained values are compared with those provided by experimental tests and correlations, finding a reasonable qualitative agreement. Expectedly, the agreement is better in the gas-like and liquid-like regions, where fluid property changes are moderate, than in the transitional region, where the trends provided by available correlations are reproduced only in a qualitative way. (author)

  3. Development of Decontamination Methods using Liquid/Supercritical CO2

    International Nuclear Information System (INIS)

    Park, Kwang Heon; Koh, Moon Sung; Yoon, Chung Hyun; Kim, Hong Doo; Kim, Hak Won

    1994-01-01

    A major problem of nuclear energy is the production of radioactive wastes. Needs for more environmentally favorable method to decontaminate radioactive contaminants make the use of liquid/supercritical CO2 as a solvent medium. In removing radioactive metallic contaminants under CO2 solvent, two methods - use of chelating ligands and that of water in CO2 emulsion - are possible. In the chelating ligand method, a combination of ligands that can make synergistic effects seems important. We discuss about the properties of microemulsion formed by F-AOT. By adding acid in water core, decontamination of metallic parts, soils were possible

  4. Supercritical heat transfer correlation for carbon dioxide flowing upward in a vertical tube

    International Nuclear Information System (INIS)

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

    2010-01-01

    The objective of the current study was to analyze heat-transfer at supercritical conditions using carbon dioxide as a modeling fluid, and to develop a heat-transfer correlation based on data published in open literature. Supercritical (SC) fluids have unique properties. Beyond the critical point (22.1 MPa and 374.1 deg.C for water and 7.38 MPa and 31.0 deg.C for carbon dioxide), the fluid resembles a dense gas. The transition from single-phase liquid to single-phase gas does not involve a distinct phase change under these conditions. Phenomena such as dryout (or critical heat flux) are therefore not relevant. However, at supercritical conditions, deteriorated heat-transfer regime, (i.e., lower Heat Transfer Coefficient (HTC) values, compared to those for the normal or regular heat-transfer regime) may exist. Experiments with Supercritical Water (SCW) are very expensive due to high critical parameters. Therefore, a number of experiments are performed in modeling fluids such as carbon dioxide or/and refrigerants. However, there is no common opinion if SC modeling fluids' correlations can be applied to SCW and vice versa. Thus, the objective of this work was to generalize SC carbon dioxide data with a new correlation, and also, to compare these data with SCW correlations The experimental data was analyzed, and a new correlation was developed as part of a larger project assessing the feasibility of Generation IV SCW reactor concepts. Results are given for supercritical heat-transfer for several combinations of wall and bulk-fluid temperatures that were below, at or above the pseudo critical temperature. Uncertainties of all primary parameters were estimated. Two modes of heat transfer at supercritical pressures have been identified: (I) Normal Heat Transfer (NHT), and (2) Deteriorated Heat Transfer (DHT) characterized by lower-than-expected HTCs (i.e., higher-than-expected wall temperatures) than in the normal heat-transfer regime. These heat-transfer data are

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

    OpenAIRE

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

    2012-01-01

    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 analysi...

  6. Optimisation of supercritical fluid extraction of polycyclic aromatic hydrocarbons and their nitrated derivatives adsorbed on highly sorptive diesel particulate matter

    International Nuclear Information System (INIS)

    Portet-Koltalo, F.; Oukebdane, K.; Dionnet, F.; Desbene, P.L.

    2009-01-01

    Supercritical fluid extraction (SFE) was performed to extract complex mixtures of polycyclic aromatic hydrocarbons (PAHs), nitrated derivatives (nitroPAHs) and heavy n-alkanes from spiked soot particulates that resulted from the incomplete combustion of diesel oils. This polluted material, resulting from combustion in a light diesel engine and collected at high temperature inside the particulate filter placed just after the engine, was particularly resistant to conventional extraction techniques, such as soxhlet extraction, and had an extraction behaviour that differed markedly from certified reference materials (SRM 1650). A factorial experimental design was performed, simultaneously modelling the influence of four SFE experimental factors on the recovery yields, i.e.: the temperature and the pressure of the supercritical fluid, the nature and the percentage of the organic modifier added to CO 2 (chloroform, tetrahydrofuran, methylene chloride), as a means to reach the optimal extraction yields for all the studied target pollutants. The results of modelling showed that the supercritical fluid pressure had to be kept at its maximum level (30 MPa) and the temperature had to be kept relatively low (75 o C). Under these operating conditions, adding 15% of methylene chloride to the CO 2 permitted quantitative extraction of not only light PAHs and their nitrated derivatives, but also heavy n-alkanes from the spiked soots. However, heavy polyaromatics were not quantitatively extracted from the refractory carbonaceous solid surface. As such, original organic modifiers were tested, including pyridine, which, as a strong electron donor cosolvent (15% into CO 2 ), was the most successful. The addition of diethylamine to pyridine, which enhanced the electron donor character of the cosolvent, even increased the extraction yields of the heaviest PAHs, leading to a quantitative extraction of all PAHs (more than 79%) from the diesel particulate matter, with detection limits

  7. 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.

  8. Online recovery of radiocesium from soil, tissue paper and plant samples by supercritical fluid extraction

    International Nuclear Information System (INIS)

    Kanekar, A.S.; Pathak, P.N.; Mohapatra, P.K.

    2014-01-01

    The feasibility of recovery of radio-cesium from soil, tissue papers, and plant samples has been evaluated by supercritical fluid extraction (SFE) route employing calix(4)arene-mono(crown-6) (CC) dissolved in acetonitrile. These studies showed that quantitative recovery of 137 Cs from soil samples was difficult under the conditions of these studies. However, experiments performed on tissue papers (cellulose matrix) showed quantitative recovery of 137 Cs. On the other hand, 137 Cs recovery from plant samples varied between ∼50 % (for stems) and ∼67.2 % (for leaves) employing 1x10 -3 M CC + 4 M HNO 3 dissolved in acetonitrile. (author)

  9. Flow Rates in Liquid Chromatography, Gas Chromatography and Supercritical Fluid Chromatography: A Tool for Optimization

    Directory of Open Access Journals (Sweden)

    Joris Meurs

    2016-08-01

    Full Text Available This paper aimed to develop a standalone application for optimizing flow rates in liquid chromatography (LC, gas chromatography (GC and supercritical fluid chromatography (SFC. To do so, Van Deemter’s equation, Knox’ equation and Golay’s equation were implemented in a MATLAB script and subsequently a graphical user interface (GUI was created. The application will show the optimal flow rate or linear velocity and the corresponding plate height for the set input parameters. Furthermore, a plot will be shown in which the plate height is plotted against the linear flow velocity. Hence, this application will give optimized flow rates for any set conditions with minimal effort.

  10. ENGINEERING BULLETIN: SUPERCRITICAL WATER OXIDATION

    Science.gov (United States)

    This engineering bulletin presents a description and status of supercritical water oxidation technology, a summary of recent performance tests, and the current applicability of this emerging technology. This information is provided to assist remedial project managers, contractors...

  11. 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

  12. 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.

  13. Evaluation of various Crown ethers for the supercritical fluid extraction of uranium from nitric acid medium

    International Nuclear Information System (INIS)

    Kumar, Pradeep; Rao, Ankita; Ramakumar, K.L.

    2009-01-01

    Various crowns have been evaluated for supercritical fluid extraction of uranium from nitric acid medium employing HPFOA as counter ion. Uranium extraction efficiency was found to be influenced by cavity size of crown ether and nature of substituents. Complexation tendency of UO 2 2+ increases with increasing cavity size of crown ether. Electron withdrawing substituents decreased the extraction efficiency which could be attributed to decrease in the basicity of four oxygen atoms and hence their bonding ability. Whereas electron donating substituents increased the efficiency due to increases in basicity of oxygen atoms and hence in increase in bonding ability. (author)

  14. Study on specifics of thermophysical properties of supercritical fluids in power engineering applications

    International Nuclear Information System (INIS)

    Mann, David; Pioro, Igor

    2015-01-01

    SuperCritical Pressures (SCPs) and SuperCritical Fluids (SFCs) are widely used in many industries worldwide. The largest application of SCPs is in the power industry in advanced coal-fired power plants. It is well-known that moving from subcritical-pressure power plants to SCP power plants increases gross thermal efficiency from 38-42% to about 50-55%. Despite all advances in thermal power-plants design and operation worldwide, they are still considered as not “environmentally friendly” due to significant carbon-dioxide emissions and air pollution as a result of the combustion process. In addition, coal-fired power-plants also produce virtual mountains of slag and ash, and other gas emissions that may contribute to acid rains. Therefore, the demand for clean, non-fossil-based electricity is growing. Due to this, nuclear power is considered as a basis for future electricity generation in the world. One of the major problems with current fleet of Nuclear Power Plants (NPPs) is their relatively low thermal efficiencies, especially, of water-cooled-reactor NPPs (the vast majority of NPPs) (30-36%), compared to those of advanced thermal power plants (55-62%). Based on that, next generation or Generation-IV reactors corresponding to those NPPs should definitely be more efficient. Higher level of thermal efficiencies can be reached only due to higher temperatures and, in some cases, higher pressures inside reactors and, especially, in power cycles of Generation-IV NPPs. Analysis of the six concepts of Generation-IV reactors and NPPs shows that three reactor concepts will use SCFs as reactor coolants (helium and water) and all concepts can be linked to SCFs as working fluids in power cycles (SC helium and /or carbon dioxide in the Brayton gas-turbine cycle, and SC water in the Rankine steam-turbine cycle). Therefore, the exact knowledge of specifics of thermophysical properties of SC helium, water and carbon dioxide is very important for any advances in these new

  15. Method and apparatus for waste destruction using supercritical water oxidation

    Science.gov (United States)

    Haroldsen, Brent Lowell; Wu, Benjamin Chiau-pin

    2000-01-01

    The invention relates to an improved apparatus and method for initiating and sustaining an oxidation reaction. A hazardous waste, is introduced into a reaction zone within a pressurized containment vessel. An oxidizer, preferably hydrogen peroxide, is mixed with a carrier fluid, preferably water, and the mixture is heated until the fluid achieves supercritical conditions of temperature and pressure. The heating means comprise cartridge heaters placed in closed-end tubes extending into the center region of the pressure vessel along the reactor longitudinal axis. A cooling jacket surrounds the pressure vessel to remove excess heat at the walls. Heating and cooling the fluid mixture in this manner creates a limited reaction zone near the center of the pressure vessel by establishing a steady state density gradient in the fluid mixture which gradually forces the fluid to circulate internally. This circulation allows the fluid mixture to oscillate between supercritical and subcritical states as it is heated and cooled.

  16. Computational Analysis of Supercritical Carbon Dioxide Gas Turbine for Liquid Metal Cooled Reactor

    Energy Technology Data Exchange (ETDEWEB)

    Jeong, Wi S.; Suh, Kune Y. [Seoul National University, Seoul (Korea, Republic of)

    2008-10-15

    Energy demands at a remote site are increased as the world energy requirement diversifies so that they should generate power on their own site. A Small Modular Reactor (SMR) becomes a viable option for these sites. Generally, the economic feasibility of a high power reactor is greater than that for SMR. As a result the supercritical fluid driven Brayton cycle is being considered for a power conversion system to increase economic competitiveness of SMR. The Brayton cycle efficiency is much higher than that for the Rankine cycle. Moreover, the components of the Brayton cycle are smaller than Rankine cycle's due to high heat capacity when a supercritical fluid is adopted. A lead (Pb) cooled SMR, BORIS, and a supercritical fluid driven Brayton cycle, MOBIS, are being developed at the Seoul National University (SNU). Dostal et al. have compared some advanced power cycles and proposed the use of a supercritical carbon dioxide (SCO{sub 2}) driven Brayton cycle. According to their suggestion SCO{sub 2} is adopted as a working fluid for MOBIS. The turbo machineries are most important components for the Brayton cycle. The turbo machineries of Brayton cycle consists of a turbine to convert kinetic energy of the fluid into mechanical energy of the shaft, and a compressor to recompress and recover the driving force of the working fluid. Therefore, turbine performance is one of the pivotal factors in increasing the cycle efficiency. In MOBIS a supercritical gas turbine is designed in the Gas Advanced Turbine Operation (GATO) and analyzed in the Turbine Integrated Numerical Analysis (TINA). A three-dimensional (3D) numerical analysis is employed for more detailed design to account for the partial flow which the one-dimensional (1D) analysis cannot consider.

  17. Computational Analysis of Supercritical Carbon Dioxide Gas Turbine for Liquid Metal Cooled Reactor

    International Nuclear Information System (INIS)

    Jeong, Wi S.; Suh, Kune Y.

    2008-01-01

    Energy demands at a remote site are increased as the world energy requirement diversifies so that they should generate power on their own site. A Small Modular Reactor (SMR) becomes a viable option for these sites. Generally, the economic feasibility of a high power reactor is greater than that for SMR. As a result the supercritical fluid driven Brayton cycle is being considered for a power conversion system to increase economic competitiveness of SMR. The Brayton cycle efficiency is much higher than that for the Rankine cycle. Moreover, the components of the Brayton cycle are smaller than Rankine cycle's due to high heat capacity when a supercritical fluid is adopted. A lead (Pb) cooled SMR, BORIS, and a supercritical fluid driven Brayton cycle, MOBIS, are being developed at the Seoul National University (SNU). Dostal et al. have compared some advanced power cycles and proposed the use of a supercritical carbon dioxide (SCO 2 ) driven Brayton cycle. According to their suggestion SCO 2 is adopted as a working fluid for MOBIS. The turbo machineries are most important components for the Brayton cycle. The turbo machineries of Brayton cycle consists of a turbine to convert kinetic energy of the fluid into mechanical energy of the shaft, and a compressor to recompress and recover the driving force of the working fluid. Therefore, turbine performance is one of the pivotal factors in increasing the cycle efficiency. In MOBIS a supercritical gas turbine is designed in the Gas Advanced Turbine Operation (GATO) and analyzed in the Turbine Integrated Numerical Analysis (TINA). A three-dimensional (3D) numerical analysis is employed for more detailed design to account for the partial flow which the one-dimensional (1D) analysis cannot consider

  18. Initial instability of round liquid jet at subcritical and supercritical environments

    International Nuclear Information System (INIS)

    Muthukumaran, C. K.; Vaidyanathan, Aravind

    2016-01-01

    In the present experimental work, the behavior of laminar liquid jet in its own vapor as well as supercritical fluid environment is conducted. Also the study of liquid jet injection into nitrogen (N_2) environment is carried out at supercritical conditions. It is expected that the injected liquid jet would undergo thermodynamic transition to the chamber condition and this would alter the behavior of the injected jet. Moreover at such conditions there is a strong dependence between thermodynamic and fluid dynamic processes. Thus the thermodynamic transition has its effect on the initial instability as well as the breakup nature of the injected liquid jet. In the present study, the interfacial disturbance wavelength, breakup characteristics, and mixing behavior are analysed for the fluoroketone liquid jet that is injected into N_2 environment as well as into its own vapor at subcritical to supercritical conditions. It is observed that at subcritical chamber conditions, the injected liquid jet exhibits classical liquid jet characteristics with Rayleigh breakup at lower Weber number and Taylor breakup at higher Weber number for both N_2 and its own environment. At supercritical chamber conditions with its own environment, the injected liquid jet undergoes sudden thermodynamic transition to chamber conditions and single phase mixing characteristics is observed. However, the supercritical chamber conditions with N_2 as ambient fluid does not have significant effect on the thermodynamic transition of the injected liquid jet.

  19. 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.

  20. FY 1998 'The New Sunshine Project' leading R and D. Report on the results of the leading R and D of supercritical fluid utilization technology; 1998 nendo 'New Sunshine Keikaku' sendo kenkyu kaihatsu. Chorinkai ryutai riyo gijutsu sendo kenkyu kaihatsu seika hokokusho

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1999-03-01

    The paper reported the FY 1998 achievement of the supercritical fluid utilization leading R and D which started in FY 1997 on a 3-year plan. In the R and D, solvolysis reaction, oxidation reaction and hydrogenation reaction were taken up in the chemical process using supercritical fluid. In the study of solvolysis reaction, the basic data were obtained on decomposition conditions of thermoplastic and thermosetting plastics in supercritical water. Further, concerning the synthesis of environmental friendly type carbonate using CO2, a conversion rate of almost 100% was obtained. About the oxidation reaction, conditions were found out for burning low grade coal in supercritical water without emitting acid gas. This is considered to lead to a possibility of the supercritical water power generation. Relating to the hydrogenation reaction, a study was made on lightening technology of heavy distillate using supercritical water, and the conditions for effective emission of methane and hydrogen were found out. As to the base technology, a study was made of metal materials with high corrosion resistance against supercritical water. (NEDO)

  1. Instrument modifications that produced reduced plate heights supercritical fluid chromatography.

    Science.gov (United States)

    Berger, Terry A

    2016-04-29

    The concept of peak fidelity was shown to be helpful in modeling tubing and detector cell dimensions. Connection tubing and flow cell variances were modeled to determine appropriate internal ID's, lengths, and volumes. A low dispersion plumbing configuration, based on these calculations, was assembled to replace the standard plumbing and produced the reported results. The modifications made were straightforward using commercially available parts. The full theoretical efficiency of a 3×100 mm column packed with 1.8 μm totally porous particles was achieved for the first time in supercritical fluid chromatography (SFC). Peak fidelity of >0.95 was maintained to below k=2. A reduced plate height as low as 1.87 was measured. Thus, true "ultra high performance" SFC was achieved, with the results a major improvement from all previous SFC reports. Since there were no efficiency losses, none could be attributed to thermal gradients caused by the expansion of the fluid over large pressure drops, under the conditions used. Similarly, changes in diffusion coefficients caused by significant decreases in density during expansion are apparently balanced by the increase in linear velocity, keeping the ratio between the diffusion coefficient and the linear velocity a constant. Changing modifier concentration to change retention was shown to not be a significant problem. All these issues have been a concern in the past. Diffusion coefficients, and viscosity data needs to be collected at high pressures before the actual limits of SFC can be discovered. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Specifics of forced-convective heat transfer in supercritical carbon dioxide

    Energy Technology Data Exchange (ETDEWEB)

    Saltanov, A.E.; Mann, B.D.; Harvel, C.G.; Pioro, D.I., E-mail: Eugene.saltanov@hotmail.com [University of Ontario Institute of Technology, Oshawa, ON (Canada)

    2015-07-01

    The appropriate description of heat-transfer to coolants at supercritical state is one of the main challenges in development of supercritical-fluids applications for the Generation-IV reactors. In this paper the basis for comparison of relatively recent experimental data on supercritical carbon dioxide (CO{sub 2}) obtained at facilities of the Korea Atomic Energy Research Institute (KAERI) and Chalk River Laboratories (CRL) of Atomic Energy of Canada Limited (AECL) is discussed, and a preliminary heat-transfer correlation for joint CRL and KAERI datasets is presented. (author)

  3. 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.

  4. Development of Nordic Standard for analysis of oil and fat in water based on supercritical fluid extraction. Preliminary study, part 2

    International Nuclear Information System (INIS)

    Jenssen, L.

    1994-06-01

    This report describes a preliminary study of a method of determining oil in water. The method is based on solid phase extraction and supercritical fluid extraction (SPE-SFE). The oil is extracted from the water by absorption to extraction disks from which it is then desorbed by supercritical carbon dioxide and detected by means of infrared spectrophotometry or gas chromatography. The results of the study will indicate if the method is suitable as a future substitute for the present Norwegian Standard, NS 9803 (Swedish Standard, SS 02 8145). The method has been validated using water samples with addition of real oil to 1-100 ppm. The accuracy is almost 70%, and the method has good repeatability and is linear in the 1-100 ppm range. 5 refs., 6 figs., 10 tabs

  5. Development and optimization of ultra-high performance supercritical fluid chromatography mass spectrometry method for high-throughput determination of tocopherols and tocotrienols in human serum

    Czech Academy of Sciences Publication Activity Database

    Pilařová, V.; Gottvald, T.; Svoboda, P.; Novák, Ondřej; Benešová, K.; Běláková, S.; Nováková, L.

    2016-01-01

    Roč. 934, AUG 31 (2016), s. 252-265 ISSN 0003-2670 R&D Projects: GA MŠk(CZ) LO1204 Institutional support: RVO:61389030 Keywords : Ultra-high performance supercritical fluid chromatography * Mass spectrometry * Liquid liquid extraction Subject RIV: EB - Genetics ; Molecular Biology Impact factor: 4.950, year: 2016

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

    OpenAIRE

    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 allows accurate quantitation in online SFE-split GC. The results obtained in online SFE-GC compare favorably with those from conventional GC with split injection. Discrimination is absent when wor...

  7. Consequences of transition from liquid chromatography to supercritical fluid chromatography on the overall performance of a chiral zwitterionic ion-exchanger.

    Science.gov (United States)

    Wolrab, Denise; Frühauf, Peter; Gerner, Christopher; Kohout, Michal; Lindner, Wolfgang

    2017-09-29

    Major differences in the chromatographic performance of a zwitterion ion-exchange type (ZWIX) chiral stationary phase (CSP) in supercritical fluid chromatography (SFC) and high-performance liquid chromatography (HPLC) have been observed. To explain these differences, transition from HPLC to SFC conditions has been performed. The amount of a protic organic modifier in supercritical carbon dioxide (scCO 2 ) was stepwise increased and the effect of this change studied using acidic, basic and ampholytic analytes. At the same time, the effect of various basic additives to the mobile phase and transient acidic buffer species, formed by the reaction of scCO 2 with the organic modifier and additives, was assessed. Evidence is provided that a transient acid together with the intrinsic counter-ions present in the ZWIX selector structure drive the elution of analytes even when no buffer is employed. We show that the tested analytes can be enantioseparated under both SFC and HPLC conditions; the best conditions for the resolution of ampholytes are in the so-called enhanced-fluidity mobile phase region. As a consequence, subcritical fluid and enhanced-fluidity mobile phase regions seem to be chromatographic modes with a high potential for operating ZWIX CSPs. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. 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

  9. 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.

  10. 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

  11. 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.

  12. Supercritical fluid extraction and chromatographic analysis (HRGC-FID and HRGC-MS of Lupinus spp. alkaloids

    Directory of Open Access Journals (Sweden)

    Nossack Ana C.

    2000-01-01

    Full Text Available The alkaloid extracts from Lupinus spp., obtained by conventional methods (maceration/sonication - solid phase extraction; maceration/sonication - liquid-liquid extraction and SFE (supercritical fluid extraction using CO2 and modified CO2 (CO2/MeOH, CO2/EtOH, CO2/iPrOH and CO2/H2O were analysed by HRGC-FID (high resolution gas chromatography - flame ionization detector and HRGC-MS (high resolution gas chromatography - mass spectrometry. The HRGC-FID quantitative analyses were performed with an internal standard method for quantification of lupanine, multiflorine and a spartein-like alkaloid. HRGC-MS allowed identification of the chemical constituents (alkaloids and other compounds from these extracts.

  13. High-Throughput Analysis of Sucrose Fatty Acid Esters by Supercritical Fluid Chromatography/Tandem Mass Spectrometry

    Science.gov (United States)

    Hori, Katsuhito; Tsumura, Kazunobu; Fukusaki, Eiichiro; Bamba, Takeshi

    2014-01-01

    Supercritical fluid chromatography (SFC) coupled with triple quadrupole mass spectrometry was applied to the profiling of sucrose fatty acid esters (SEs). The SFC conditions (column and modifier gradient) were optimized for the effective separation of SEs. In the column test, a silica gel reversed-phase column was selected. Then, the method was used for the detailed characterization of commercial SEs and the successful analysis of SEs containing different fatty acids. The present method allowed for fast and high-resolution separation of monoesters to tetra-esters within a shorter time (15 min) as compared to the conventional high-performance liquid chromatography. The applicability of our method for the analysis of SEs was thus demonstrated. PMID:26819875

  14. Application of response surface methodology to optimise supercritical carbon dioxide extraction of volatile compounds from Crocus sativus.

    Science.gov (United States)

    Shao, Qingsong; Huang, Yuqiu; Zhou, Aicun; Guo, Haipeng; Zhang, Ailian; Wang, Yong

    2014-05-01

    Crocus sativus has been used as a traditional Chinese medicine for a long time. The volatile compounds of C. sativus appear biologically active and may act as antioxidants as well as anticonvulsants, antidepressants and antitumour agents. In order to obtain the highest possible yield of essential oils from C. sativus, response surface methodology was employed to optimise the conditions of supercritical fluid carbon dioxide extraction of the volatile compounds from C. sativus. Four factorswere investigated: temperature, pressure, extraction time and carbon dioxide flow rate. Furthermore, the chemical compositions of the volatile compounds extracted by supercritical fluid extraction were compared with those obtained by hydro-distillation and Soxhlet extraction. The optimum extraction conditions were found to be: optimised temperature 44.9°C, pressure 34.9 MPa, extraction time 150.2 min and CO₂ flow rate 10.1 L h⁻¹. Under these conditions, the mean extraction yield was 10.94 g kg⁻¹. The volatile compounds extracted by supercritical fluid extraction and Soxhlet extraction contained a large amount of unsaturated fatty acids. Response surface methodology was successfully applied for supercritical fluid CO₂ extraction optimisation of the volatile compounds from C. sativus. The study showed that pressure and CO₂ flow rate had significant effect on volatile compounds yield produced by supercritical fluid extraction. This study is beneficial for the further research operating on a large scale. © 2013 Society of Chemical Industry.

  15. 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.

  16. Cytotoxic Activity of Kenaf Seed Oils from Supercritical Carbon Dioxide Fluid Extraction towards Human Colorectal Cancer (HT29) Cell Lines

    OpenAIRE

    Abd Ghafar, Siti Aisyah; Ismail, Maznah; Saiful Yazan, Latifah; Fakurazi, Sharida; Ismail, Norsharina; Chan, Kim Wei; Md Tahir, Paridah

    2013-01-01

    Kenaf (Hibiscus cannabinus) from the family Malvaceae, is a valuable fiber plant native to India and Africa and is currently planted as the fourth commercial crop in Malaysia. Kenaf seed oil contains alpha-linolenic acid, phytosterol such as ? -sitosterol, vitamin E, and other antioxidants with chemopreventive properties. Kenaf seeds oil (KSO) was from supercritical carbon dioxide extraction fluid (SFE) at 9 different permutations of parameters based on range of pressures from 200 to 600 bars...

  17. Variability of standard artificial soils: Physico-chemical properties and phenanthrene desorption measured by means of supercritical fluid extraction

    International Nuclear Information System (INIS)

    Bielská, Lucie; Hovorková, Ivana; Komprdová, Klára; Hofman, Jakub

    2012-01-01

    The study is focused on artificial soil which is supposed to be a standardized “soil like” medium. We compared physico-chemical properties and extractability of Phenanthrene from 25 artificial soils prepared according to OECD standardized procedures at different laboratories. A substantial range of soil properties was found, also for parameters which should be standardized because they have an important influence on the bioavailability of pollutants (e.g. total organic carbon ranged from 1.4 to 6.1%). The extractability of Phe was measured by supercritical fluid extraction (SFE) at harsh and mild conditions. Highly variable Phe extractability from different soils (3–89%) was observed. The extractability was strongly related (R 2 = 0.87) to total organic carbon content, 0.1–2 mm particle size, and humic/fulvic acid ratio in the following multiple regression model: SFE (%) = 1.35 * sand (%) − 0.77 * TOC (%)2 + 0.27 * HA/FA. - Highlights: ► We compared properties and extractability of Phe from 25 different artificial soils. ► Substantial range of soil properties was found, also for important parameters. ► Phe extractability was measured by supercritical fluid extraction (SFE) at 2 modes. ► Phe extractability was highly variable from different soils (3–89%). ► Extractability was strongly related to TOC, 0.1–2 mm particles, and HA/FA. - Significant variability in physico-chemical properties exists between artificial soils prepared at different laboratories and affects behavior of contaminants in these soils.

  18. 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.

  19. Cefuroxime axetil solid dispersions prepared using solution enhanced dispersion by supercritical fluids.

    Science.gov (United States)

    Jun, Seoung Wook; Kim, Min-Soo; Jo, Guk Hyun; Lee, Sibeum; Woo, Jong Soo; Park, Jeong-Sook; Hwang, Sung-Joo

    2005-12-01

    Cefuroxime axetil (CA) solid dispersions with HPMC 2910/PVP K-30 were prepared using solution enhanced dispersion by supercritical fluids (SEDS) in an effort to increase the dissolution rate of poorly water-soluble drugs. Their physicochemical properties in solid state were characterized by differential scanning calorimeter (DSC), powder X-ray diffraction (PXRD), Fourier transform infrared spectrometry (FT-IR) and scanning electron microscopy. No endothermic and characteristic diffraction peaks corresponding to CA were observed for the solid dispersions in DSC and PXRD. FTIR analysis demonstrated the presence of intermolecular hydrogen bonds between CA and HPMC 2910/PVP K-30 in solid dispersions, resulting in the formation of amorphous or non-crystalline CA. Dissolution studies indicated that the dissolution rates were remarkably increased in solid dispersions compared with those in the physical mixture and drug alone. In conclusion, an amorphous or non-crystalline CA solid dispersion prepared using SEDS could be very useful for the formulation of solid dosage forms.

  20. Determination of coumarins in the roots of Angelica dahurica by supercritical fluid chromatography.

    Science.gov (United States)

    Pfeifer, Isabella; Murauer, Adele; Ganzera, Markus

    2016-09-10

    The fact that supercritical fluid chromatography (SFC) offers many desirable features is known for a long time. Yet, the number of applications on natural products is still limited, because robust and user-friendly instrumentation became available just a few years ago. As coumarins hardly have been studied by this technique we developed the first SFC assay for their determination in crude plant material. After method optimization eight standard compounds, including simple coumarins, linear and angular furanocoumarins, could be baseline separated in 6min using an Acquity UPC(2) CSH Fluoro-Phenyl 1.7μm column with supercritical CO2, methanol and diethylamine as mobile phase. Method validation confirmed that the assay is linear (R(2)≥0.9995), precise (intra-day variation≤5.8%; inter-day variation≤4.4%) and accurate (recovery rates from 96.5 to 104.2%). Detection limits determined at 300nm were below 2ng on-column, and the method showed to be well suited for the analysis of coumarins in Angelica dahurica roots. It was observed that qualitative as well as quantitative composition vary significantly. In all samples Imperatorin (0.09-0.28%) was the major coumarin, followed either by Isoimperatorin or Oxypeucedanin; the total coumarin content ranged from 0.16 to 0.77%. The results were in good agreement to published data, so that because of its speed and green nature SFC is definitely an interesting alternative for the analysis of this important class of natural products. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. A Technique for Dynamic Corrosion Testing in Supercritical CO2

    International Nuclear Information System (INIS)

    Loewen, Eric P.; Davis, Cliff B.; Shropshire, David E.; Weaver, Kevan

    2004-01-01

    An experimental apparatus for the investigation of the flow-assisted corrosion of potential fuel cladding and structural materials to be used on a fast reactor cooled by supercritical carbon dioxide has been designed. This experimental project is part of a larger research at the Department of Energy being lead by the Idaho National Engineering and Environmental Laboratory (INEEL) to investigate the suitability of supercritical carbon dioxide for cooling a fast reactor designed to produce low-cost electricity as well as for actinide burning. The INEEL once-through corrosion apparatus consists of two syringe pumps, a pre-heat furnace, a 1.3 meter long heated corrosion test section, and a gas measuring system. The gas flow rates, heat input, and operating pressure can be adjusted so that a controlled coolant flow rate, temperature, and oxygen potential are created within each of six test sections. The corrosion cell will test tubing that is commercially available in the U.S. and specialty coupons to temperatures up to 600 deg. C and a pressure of 20 MPa. The ATHENA computer code was used to estimate the fluid conditions in each of the six test sections during normal operation. (authors)

  2. 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.

  3. An application of the modified turbulent model for analyzing supercritical heat transfer phenomena in a nuclear system

    International Nuclear Information System (INIS)

    Seo, Kyoung-Woo; Park, Cheon-Tae; Seo, Jae-Kwang; Kim, Moo-Hwan; Corradini, Michael L.

    2007-01-01

    For understanding the characteristic of a supercritical fluid heat transfer, we proposed a new parameter, a global Froude number (Fr), dependent on the heat and mass flux, to determine under what conditions the buoyancy effect is dominant and the reduction of the heat transfer rate. In the region of the global Fr>0.01, variable property effects, which may occur at a high heat flux, and buoyancy effects, which could occur at a low mass flux, make the existing standard turbulent model such as the standard wall function not suitably accurate to calculate the heat transfer in supercritical fluid, needed for a reactor thermal-hydraulics simulation and design. Therefore, the turbulence model, especially near the wall, the wall function for a momentum, applicable for a range of supercritical fluid conditions was modified. The modified models deal with a buoyancy, acceleration, and the variable property effect for supercritical conditions

  4. Supercritical Carbon Dioxide and Microwave-Assisted Extraction of Functional Lipophilic Compounds from Arthrospira platensis

    Directory of Open Access Journals (Sweden)

    Diego A. Esquivel-Hernández

    2016-05-01

    Full Text Available Arthrospira platensis biomass was used in order to obtain functional lipophilic compounds through green extraction technologies such as supercritical carbon dioxide fluid extraction (SFE and microwave-assisted extraction (MAE. The temperature (T factor was evaluated for MAE, while for SFE, pressure (P, temperature (T, and co-solvent (ethanol (CS were evaluated. The maximum extraction yield of the obtained oleoresin was (4.07% ± 0.14% and (4.27% ± 0.10% for SFE and MAE, respectively. Extracts were characterized by gas chromatography mass spectrometry (GC-MS and gas chromatography flame ionization detector (GC-FID. The maximum contents of functional lipophilic compounds in the SFE and MAE extracts were: for carotenoids 283 ± 0.10 μg/g and 629 ± 0.13 μg/g, respectively; for tocopherols 5.01 ± 0.05 μg/g and 2.46 ± 0.09 μg/g, respectively; and for fatty acids 34.76 ± 0.08 mg/g and 15.88 ± 0.06 mg/g, respectively. In conclusion, the SFE process at P 450 bar, T 60 °C and CS 53.33% of CO2 produced the highest yield of tocopherols, carotenoids and fatty acids. The MAE process at 400 W and 50 °C gives the best extracts in terms of tocopherols and carotenoids. For yield and fatty acids, the MAE process at 400 W and 70 °C produced the highest values. Both SFE and MAE showed to be suitable green extraction technologies for obtaining functional lipophilic compounds from Arthrospira platensis.

  5. COMPARISONS OF SOXHLET EXTRACTION, PRESSURIZED LIQUID EXTRACTION, SUPERCRITICAL FLUID EXTRACTION, AND SUBCRITICAL WATER EXTRACTION FOR ENVIRONMENTAL SOLIDS: RECOVERY, SELECTIVITY, AND EFFECTS ON SAMPLE MATRIX. (R825394)

    Science.gov (United States)

    Extractions of a polycyclic aromatic hydrocarbon (PAH)-contaminated soil from a former manufactured gas plant site were performed with a Soxhlet apparatus (18 h), by pressurized liquid extraction (PLE) (50 min at 100°C), supercritical fluid extraction (SFE) (1 h at 150°...

  6. Poly(butylene terephthalate) based novel achiral stationary phase investigated under supercritical fluid chromatography conditions.

    Science.gov (United States)

    Nagai, Kanji; Shibata, Tohru; Shinkura, Satoshi; Ohnishi, Atsushi

    2018-05-11

    Poly(butylene terephthalate) based novel stationary phase (SP), composed of planar aromatic phenyl group together with ester group monomer units, was designed for supercritical fluid chromatography (SFC) use. As expected from its structure, this phase shows planarity recognition of isomeric aromatics and closely similar compounds. Interestingly, for most analytes, the retention behavior of this SP is significantly distinct from that of the 2-ethylpyridine based SPs which is among the most well-known SFC dedicated phases. Although the poly(butylene terephthalate) is coated on silica gel, the performance of the column did not change by using extended range modifiers such as THF, dichloromethane or ethyl acetate and column robustness was confirmed by cycle durability testing. Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.

  7. Geological model of supercritical geothermal reservoir related to subduction system

    Science.gov (United States)

    Tsuchiya, Noriyoshi

    2017-04-01

    Following the Great East Japan Earthquake and the accident at the Fukushima Daiichi Nuclear power station on 3.11 (11th March) 2011, geothermal energy came to be considered one of the most promising sources of renewable energy for the future in Japan. The temperatures of geothermal fields operating in Japan range from 200 to 300 °C (average 250 °C), and the depths range from 1000 to 2000 m (average 1500 m). In conventional geothermal reservoirs, the mechanical behavior of the rocks is presumed to be brittle, and convection of the hydrothermal fluid through existing network is the main method of circulation in the reservoir. In order to minimize induced seismicity, a rock mass that is "beyond brittle" is one possible candidate, because the rock mechanics of "beyond brittle" material is one of plastic deformation rather than brittle failure. Supercritical geothermal resources could be evaluated in terms of present volcanic activities, thermal structure, dimension of hydrothermal circulation, properties of fracture system, depth of heat source, depth of brittle factures zone, dimension of geothermal reservoir. On the basis of the GIS, potential of supercritical geothermal resources could be characterized into the following four categories. 1. Promising: surface manifestation d shallow high temperature, 2 Probability: high geothermal gradient, 3 Possibility: Aseismic zone which indicates an existence of melt, 4 Potential : low velocity zone which indicates magma input. Base on geophysical data for geothermal reservoirs, we have propose adequate tectonic model of development of the supercritical geothermal reservoirs. To understand the geological model of a supercritical geothermal reservoir, granite-porphyry system, which had been formed in subduction zone, was investigated as a natural analog of the supercritical geothermal energy system. Quartz veins, hydrothermal breccia veins, and glassy veins are observed in a granitic body. The glassy veins formed at 500-550

  8. Preliminary Hazard Analysis of Supercritical Fluid Separation of Energetic Materials

    National Research Council Canada - National Science Library

    1997-01-01

    .... Army Research Laboratory (ARL) and elsewhere, particularly at the Phasex Corporation, Lawrence, MA, has demonstrated the feasibility of separating the energetic moieties by use of supercritical CO2...

  9. Characterization of Arachis hypogaea L. oil obtained from different extraction techniques and in vitro antioxidant potential of supercritical fluid extraction extract

    Directory of Open Access Journals (Sweden)

    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.

  10. FY 1998 'The New Sunshine Project' leading R and D. Report on the results of the leading R and D of supercritical fluid utilization technology; 1998 nendo 'New Sunshine Keikaku' sendo kenkyu kaihatsu. Chorinkai ryutai riyo gijutsu sendo kenkyu kaihatsu seika hokokusho

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1999-03-01

    The paper reported the FY 1998 achievement of the supercritical fluid utilization leading R and D which started in FY 1997 on a 3-year plan. In the R and D, solvolysis reaction, oxidation reaction and hydrogenation reaction were taken up in the chemical process using supercritical fluid. In the study of solvolysis reaction, the basic data were obtained on decomposition conditions of thermoplastic and thermosetting plastics in supercritical water. Further, concerning the synthesis of environmental friendly type carbonate using CO2, a conversion rate of almost 100% was obtained. About the oxidation reaction, conditions were found out for burning low grade coal in supercritical water without emitting acid gas. This is considered to lead to a possibility of the supercritical water power generation. Relating to the hydrogenation reaction, a study was made on lightening technology of heavy distillate using supercritical water, and the conditions for effective emission of methane and hydrogen were found out. As to the base technology, a study was made of metal materials with high corrosion resistance against supercritical water. (NEDO)

  11. Destruction of polyphasic systems in supercritical water reaction media

    International Nuclear Information System (INIS)

    Leybros, A.

    2009-12-01

    Spent ion exchange resins (IER) are, hence, radioactive process wastes for which there is no satisfactory industrial treatment. Supercritical water oxidation offers a viable alternative treatment to destroy the organic structure of resins by using supercritical water properties. The reactor used in Supercritical Fluids and Membranes Laboratory is a double shell stirred reactor. Total Organic Carbon reduction rates higher than 99% were obtained thanks to POSCEA2 experimental set-up when using a co-fuel, isopropyl alcohol. Influence of operating parameters was studied. A detailed reactional mechanism for cationic and anionic resins is created. For the solubilization of the particles in supercritical water, a mechanism has been created with the identified rate determining species and implemented into Fluent software through the EDC approach. Experimental temperature profiles are well represented by EDC model. Reaction rates are hence controlled by the chemical species mixing. (author)

  12. Method and apparatus for jet-assisted drilling or cutting

    Science.gov (United States)

    Summers, David Archibold; Woelk, Klaus Hubert; Oglesby, Kenneth Doyle; Galecki, Grzegorz

    2012-09-04

    An abrasive cutting or drilling system, apparatus and method, which includes an upstream supercritical fluid and/or liquid carrier fluid, abrasive particles, a nozzle and a gaseous or low-density supercritical fluid exhaust abrasive stream. The nozzle includes a throat section and, optionally, a converging inlet section, a divergent discharge section, and a feed section.

  13. Surface modification of chitin using ultrasound-assisted and supercritical CO{sub 2} technologies for cobalt adsorption

    Energy Technology Data Exchange (ETDEWEB)

    Dotto, Guilherme L., E-mail: guilherme_dotto@yahoo.com.br; Cunha, Jeanine M., E-mail: jeaninecunha@gmail.com; Calgaro, Camila O., E-mail: camila.itepjr@gmail.com; Tanabe, Eduardo H., E-mail: edutanabe@yahoo.com.br; Bertuol, Daniel A., E-mail: dbertuol@gmail.com

    2015-09-15

    Highlights: • Chitin was modified by ultrasound-assisted (UA) and supercritical (SCO{sub 2}) technologies. • Chitin, UA-chitin and SCO{sub 2}-chitin were used as adsorbents for Co(II). • UA and SCO{sub 2} treatments provided increase of 20 and 3 times in chitin surface area. • The Co(II) adsorption capacity increased until 67.8%, using UA-chitin. - Abstract: Ultrasound-assisted (UA) and supercritical CO{sub 2} technologies (SCO{sub 2}) were used to modify the chitin surface and, improve its adsorption characteristics regarding to cobalt. Chitin, before and after the treatments, was characterized by N{sub 2} adsorption isotherms (BET), infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and scanning electron microscopy (SEM). Unmodified and surface modified chitins were used as adsorbents to remove cobalt from aqueous solutions. The adsorption study was performed by equilibrium isotherms and kinetic curves. The chitin particle characteristics, such as, surface area, pore volume and porosity were improved by the UA and SCO{sub 2} treatments. The crystallinity index decreased after the UA and SCO{sub 2} treatments, and also, intense surface modifications were observed. Langmuir and Freundlich models were adequate to represent the adsorption equilibrium. The maximum adsorption capacities were 50.03, 83.94 and 63.08 mg g{sup −1} for unmodified chitin, UA surface modified chitin and SCO{sub 2} surface modified chitin. The adsorption kinetic curves were well represented by the pseudo-second order model. UA and SCO{sub 2} technologies are alternatives to modify the chitin surface and improve its adsorption characteristics.

  14. Production of solid lipid submicron particles for protein delivery using a novel supercritical gas-assisted melting atomization process.

    Science.gov (United States)

    Salmaso, Stefano; Elvassore, Nicola; Bertucco, Alberto; Caliceti, Paolo

    2009-02-01

    A supercritical carbon dioxide micronization technique based on gas-assisted melting atomization has been designed to prepare protein-loaded solid lipid submicron particles. The supercritical process was applied to homogeneous dispersions of insulin in lipid mixtures: (1) tristearin, Tween-80, phosphatidylcholine and 5 kDa PEG (1:0.1:0.9:1 and 1:0.1:0.9:2 weight ratio); and (2) tristearin, dioctyl sulfosuccinate and phosphatidylcholine (1:1:0.5 weight ratio). Optimized process conditions yielded dry nonagglomerated powders with high product recovery (70%, w/w). Dynamic light scattering and transmission electron microscopy showed that two size fractions of particles, with 80-120 and 200-400 nm diameters, were produced. In all final products, dimethylsulfoxide used to prepare the insulin/lipid mixture was below 20 ppm. Protein encapsulation efficiency increased up to 80% as the DMSO content in the insulin/lipid mixture increased. Compared to the particles without PEG, the polymer-containing particles dispersed rapidly in water, and the dispersions were more stable under centrifugation as less than 20% of suspended particles precipitated after extensive centrifugation. In vitro, the protein was slowly released from the formulation without PEG, while a burst and faster release were obtained from the formulations containing PEG. Subcutaneous injection to diabetic mice of insulin extracted from the particles showed that the supercritical process did not impair the protein hypoglycemic activity.

  15. Thermodynamic Analysis of a Supercritical Mercury Power Cycle

    Energy Technology Data Exchange (ETDEWEB)

    Roberts, Jr, A S

    1969-04-15

    An heat engine is considered which employs supercritical mercury as the working fluid and a magnetohydrodynamic (MHD) generator for thermal to electrical energy conversion. The main thrust of the paper is power cycle thermodynamics, where constraints are imposed by utilizing a MHD generator operating between supercritical, electrically conducting states of the working fluid; and, pump work is accomplished with liquid mercury. The temperature range is approximately 300 to 2200 K and system pressure is > 1,500 atm. Equilibrium and transport properties are carefully considered since these are known to vary radically in the vicinity of the critical point, which is found near the supercritical states of interest. A maximum gross plant efficiency is 20% with a regenerator effectiveness of 90% and greater, a cycle pressure ratio of two, and with highly efficient pump and generator. Certain specified cycle irreversibilities and others such as heat losses and heat exchanger pressure drops, which are not accounted for explicitly, reduce the gross plant efficiency to a few per cent. Experimental efforts aimed at practical application of the power cycle are discouraged by the marginal thermodynamic performance predicted by this study, unless such applications are insensitive to gross cycle efficiency.

  16. Thermodynamic Analysis of a Supercritical Mercury Power Cycle

    International Nuclear Information System (INIS)

    Roberts, A.S. Jr.

    1969-04-01

    An heat engine is considered which employs supercritical mercury as the working fluid and a magnetohydrodynamic (MHD) generator for thermal to electrical energy conversion. The main thrust of the paper is power cycle thermodynamics, where constraints are imposed by utilizing a MHD generator operating between supercritical, electrically conducting states of the working fluid; and, pump work is accomplished with liquid mercury. The temperature range is approximately 300 to 2200 K and system pressure is > 1,500 atm. Equilibrium and transport properties are carefully considered since these are known to vary radically in the vicinity of the critical point, which is found near the supercritical states of interest. A maximum gross plant efficiency is 20% with a regenerator effectiveness of 90% and greater, a cycle pressure ratio of two, and with highly efficient pump and generator. Certain specified cycle irreversibilities and others such as heat losses and heat exchanger pressure drops, which are not accounted for explicitly, reduce the gross plant efficiency to a few per cent. Experimental efforts aimed at practical application of the power cycle are discouraged by the marginal thermodynamic performance predicted by this study, unless such applications are insensitive to gross cycle efficiency

  17. 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.

  18. Extraction of curcumin from Curcuma longa L. using ultrasound assisted supercritical carbon dioxide

    Science.gov (United States)

    Kimthet, Chhouk; Wahyudiono, Kanda, Hideki; Goto, Motonobu

    2017-05-01

    Curcumin is one of phenolic compounds, which has been recently shown to have useful pharmacological properties such as anti-inflammatory, anti-bacterial, anti-carcinogenic, antifungal, and antimicrobial activities. The objective of this research is to extract the curcumin from Curcuma longa L. using ultrasound assisted supercritical carbon dioxide extraction (USC-CO2). The extraction was performed at 50°C, 25 MPa, CO2 flow rate of 3 mL/min with 10% cosolvent. The result of extraction, thermogravimetry (TG), Fourier transform infrared spectroscopy (FTIR) and scanning electron microscope (SEM) showed that ultrasound power could disrupt cell wall and release the target compounds from Curcuma longa L. USC-CO2 could provide higher curcumin content in the extracts and faster extraction compared to SC-CO2 extraction without ultrasound.

  19. Experimental study of elliptical jet from sub to supercritical conditions

    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)

    2014-04-15

    The jet mixing at supercritical conditions involves fluid dynamics as well as thermodynamic phenomena. All the jet mixing studies at critical conditions to the present date have focused only on axisymmetric jets. When the liquid jet is injected into supercritical environment, the thermodynamic transition could be well understood by considering one of the important fluid properties such as surface tension since it decides the existence of distinct boundary between the liquid and gaseous phase. It is well known that an elliptical liquid jet undergoes axis-switching phenomena under atmospheric conditions due to the presence of surface tension. The experimental investigations were carried out with low speed elliptical jet under supercritical condition. Investigation of the binary component system with fluoroketone jet and N{sub 2} gas as environment shows that the surface tension force dominates for a large downstream distance, indicating delayed thermodynamic transition. The increase in pressure to critical state at supercritical temperature is found to expedite the thermodynamic transition. The ligament like structures has been observed rather than droplets for supercritical pressures. However, for the single component system with fluoroketone jet and fluoroketone environment shows that the jet disintegrates into droplets as it is subjected to the chamber conditions even for the subcritical pressures and no axis switching phenomenon is observed. For a single component system, as the pressure is increased to critical state, the liquid jet exhibits gas-gas like mixing behavior and that too without exhibiting axis-switching behavior.

  20. Supercritical water decontamination of town gas soil

    International Nuclear Information System (INIS)

    Kocher, B.S.; Azzam, F.O.; Lee, S.

    1994-01-01

    Town gas sites represent a large environmental problem that exists in more than 2,000 sites across North America alone. The major contaminants in town gas sods are polycyclic aromatic hydrocarbons (PAHs). These are stable compounds that migrate deep into the soil and are traditionally very difficult to remove by conventional remediation processes. Supercritical fluids offer enhanced solvating properties along with reduced mass transfer resistances that make them ideal for removing compounds that are difficult or impossible to remove by conventional processes. Supercritical water is ideal for removing PAHs and other hydrocarbons from soil due to its high solvating power towards most hydrocarbon species. Supercritical water was investigated for its ability to remediate two different town gas sods containing from 3--20 wt% contamination. The sod was remediated in a 300-cc semi-continuous system to a more environmentally acceptable level

  1. 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.

  2. Temperature and pressure effects on solubility in supercritical carbon dioxide and retention in supercritical fluid chromatography

    NARCIS (Netherlands)

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

    1997-01-01

    Solubilities of some polycyclic aromatic hydrocarbons (PAHs) in supercritical carbon dioxide were measured with a procedure based on a direct on-line combination of a saturation cell to a flame ionization detector. Acenaphthene, anthrance and chrysene were selected as the test solutes. A method was

  3. Profiling of modified nucleosides from ribonucleic acid digestion by supercritical fluid chromatography coupled to high resolution mass spectrometry.

    Science.gov (United States)

    Laboureur, Laurent; Guérineau, Vincent; Auxilien, Sylvie; Yoshizawa, Satoko; Touboul, David

    2018-02-16

    A method based on supercritical fluid chromatography coupled to high resolution mass spectrometry for the profiling of canonical and modified nucleosides was optimized, and compared to classical reverse-phase liquid chromatography in terms of separation, number of detected modified nucleosides and sensitivity. Limits of detection and quantification were measured using statistical method and quantifications of twelve nucleosides of a tRNA digest from E. coli are in good agreement with previously reported data. Results highlight the complementarity of both separation techniques to cover the largest view of nucleoside modifications for forthcoming epigenetic studies. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. 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.

  5. Numerical comparison of thermal hydraulic aspects of supercritical carbon dioxide and subcritical water-based natural circulation loop

    Energy Technology Data Exchange (ETDEWEB)

    Sarkar, Milan Krishna Singhar; Basu, Dipankar Narayan [Dept. of Mechanical Engineering, Indian Institute of Technology Guwahati, Guwahati (India)

    2017-02-15

    Application of the supercritical condition in reactor core cooling needs to be properly justified based on the extreme level of parameters involved. Therefore, a numerical study is presented to compare the thermalhydraulic performance of supercritical and single-phase natural circulation loops under low-to-intermediate power levels. Carbon dioxide and water are selected as respective working fluids, operating under an identical set of conditions. Accordingly, a three-dimensional computational model was developed, and solved with an appropriate turbulence model and equations of state. Large asymmetry in velocity and temperature profiles was observed in a single cross section due to local buoyancy effect, which is more prominent for supercritical fluids. Mass flow rate in a supercritical loop increases with power until a maximum is reached, which subsequently corresponds to a rapid deterioration in heat transfer coefficient. That can be identified as the limit of operation for such loops to avoid a high temperature, and therefore, the use of a supercritical loop is suggested only until the appearance of such maxima. Flow-induced heat transfer deterioration can be delayed by increasing system pressure or lowering sink temperature. Bulk temperature level throughout the loop with water as working fluid is higher than supercritical carbon dioxide. This is until the heat transfer deterioration, and hence the use of a single-phase loop is prescribed beyond that limit.

  6. Field—Based Supercritical Fluid Extraction of Hydrocarbons at Industrially Contaminated Sites

    Directory of Open Access Journals (Sweden)

    Peggy Rigou

    2002-01-01

    Full Text Available Examination of organic pollutants in groundwaters should also consider the source of the pollution, which is often a solid matrix such as soil, landfill waste, or sediment. This premise should be viewed alongside the growing trend towards field-based characterisation of contaminated sites for reasons of speed and cost. Field-based methods for the extraction of organic compounds from solid samples are generally cumbersome, time consuming, or inefficient. This paper describes the development of a field-based supercritical fluid extraction (SFE system for the recovery of organic contaminants (benzene, toluene, ethylbenzene, and xylene and polynuclear aromatic hydrocarbons from soils. A simple, compact, and robust SFE system has been constructed and was found to offer the same extraction efficiency as a well-established laboratory SFE system. Extraction optimisation was statistically evaluated using a factorial analysis procedure. Under optimised conditions, the device yielded recovery efficiencies of >70% with RSD values of 4% against the standard EPA Soxhlet method, compared with a mean recovery efficiency of 48% for a commercially available field-extraction kit. The device will next be evaluated with real samples prior to field deployment.

  7. 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.

  8. 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

  9. 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

  10. 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.

  11. Numerical investigation on cryogenic liquid jet under transcritical and supercritical conditions

    Science.gov (United States)

    Li, Liang; Xie, Maozhao; Wei, Wu; Jia, Ming; Liu, Hongsheng

    2018-01-01

    Cryogenic fluid injection and mixing under transcritical and supercritical conditions is numerically investigated with emphasis on the difference of the mechanism and characteristics between the two injections. A new solver is developed which is capable of handling the nonideality of the equation of state and the anomalies in fluid transport properties and is incorporated into the CFD software OpenFOAM. The new solver has been validated against available experimental data and exhibits a good performance. Computational results indicates that the differences between transcritical and supercritical injections are mainly induced by the pseudo-boiling phenomenon, resulting in that the transcritical jet has a longer cold liquid core and an isothermal expansion occurs at the surface of the cold core. The thickness of the supercritical mixing layer and its increase value along the jet direction are greater than its transcritical counterpart. The high-temperature jet whose initial temperature is above the pseudo-boiling temperature has the ability of enhancing the mixing of the jet with the surrounding gas.

  12. Efficiency optimization potential in supercritical Organic Rankine Cycles

    Energy Technology Data Exchange (ETDEWEB)

    Schuster, A.; Aumann, R. [Technische Universitaet Muenchen Institute of Energy Systems Boltzmannstr. 15, 85748 Garching (Germany); Karellas, S. [National Technical University of Athens Laboratory of Steam Boilers and Thermal Plants Heroon Polytechniou 9, 15780 Athens (Greece)

    2010-02-15

    Nowadays, the use of Organic Rankine Cycle (ORC) in decentralised applications is linked with the fact that this process allows the use of low temperature heat sources and offers an advantageous efficiency in small-scale concepts. Many state-of-the-art and innovative applications can successfully use the ORC process. In this process, according to the heat source level, special attention must be drawn to the choice of the appropriate working fluid, which is a factor that affects the thermal and exergetic efficiency of the cycle. The investigation of supercritical parameters of various working fluids in ORC applications seems to bring promising results concerning the efficiency of the application. This paper presents the results from a simulation of the ORC and the optimization potential of the process when using supercritical parameters. In order to optimize the process, various working fluids are considered and compared concerning their thermal efficiency and the usable percentage of heat. The reduction of exergy losses is discussed based on the need of surplus heat exchanger surface. (author)

  13. Supercritical carbon dioxide extraction of pigments from Bixa orellana seeds (experiments and modeling

    Directory of Open Access Journals (Sweden)

    B. P. Nobre

    2006-06-01

    Full Text Available Supercritical CO2 extraction of the pigments from Bixa orellana seeds was carried out in a flow apparatus at a pressure of 200 bar and a temperature of 40 ºC at two fluid flow rates (0.67g/min and 1.12g/min. The efficiency of the extraction was low (only about 1% of the pigment was extracted. The increase in flow rate led to a decrease in pigment recovery. A large increase in recovery (from 1% to 45% was achieved using supercritical carbon dioxide with 5 mol % ethanol as extraction fluid at pressures of 200 and 300 bar and temperatures of 40 and 60 ºC. Although the increase in temperature and pressure led to an increase in recovery, the changes in flow rate did not seem to affect it. Furthermore, two plug flow models were applied to describe the supercritical extraction of the pigments from annatto seeds. Mass transfer coefficients were determined and compared well with those obtained by other researchers with similar models for the supercritical extraction of solutes from plant materials.

  14. Geological Model of Supercritical Geothermal Reservoir on the Top of the Magma Chamber

    Science.gov (United States)

    Tsuchiya, N.

    2017-12-01

    We are conducting supercritical geothermal project, and deep drilling project named as "JBBP: Japan Beyond Brittle Project" The temperatures of geothermal fields operating in Japan range from 200 to 300 °C (average 250 °C), and the depths range from 1000 to 2000 m (average 1500 m). In conventional geothermal reservoirs, the mechanical behavior of the rocks is presumed to be brittle, and convection of the hydrothermal fluid through existing network is the main method of circulation in the reservoir. In order to minimize induced seismicity, a rock mass that is "beyond brittle" is one possible candidate, because the rock mechanics of "beyond brittle" material is one of plastic deformation rather than brittle failure. To understand the geological model of a supercritical geothermal reservoir, granite-porphyry system, which had been formed in subduction zone, was investigated as a natural analog of the supercritical geothermal energy system. Quartz veins, hydrothermal breccia veins, and glassy veins are observed in a granitic body. The glassy veins formed at 500-550 °C under lithostatic pressures, and then pressures dropped drastically. The solubility of silica also dropped, resulting in formation of quartz veins under a hydrostatic pressure regime. Connections between the lithostatic and hydrostatic pressure regimes were key to the formation of the hydrothermal breccia veins, and the granite-porphyry system provides useful information for creation of fracture clouds in supercritical geothermal reservoirs. A granite-porphyry system, associated with hydrothermal activity and mineralization, provides a suitable natural analog for studying a deep-seated geothermal reservoir where stockwork fracture systems are created in the presence of supercritical geothermal fluids. I describe fracture networks and their formation mechanisms using petrology and fluid inclusion studies in order to understand this "beyond brittle" supercritical geothermal reservoir, and a geological

  15. Complete removal of uranyl nitrate from tissue matrix using supercritical fluid extraction

    International Nuclear Information System (INIS)

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

    2003-01-01

    The removal of uranyl nitrate from tissue matrix has been studied with supercritical carbon dioxide modified with methanol alone as well as complexing reagents dissolved in methanol. A systematic study of various complexing agents led to the development of an extraction procedure for the quantitative recovery of uranium from tissue matrix with supercritical carbon dioxide modified with methanol containing small quantities of acetylacetone. The drying time and temperature employed in loading of uranyl nitrate onto tissue paper were found to influence the extraction efficiency significantly

  16. Fluidos supercríticos em química analítica. III.: aplicações Supercritical fluids in analytical chemistry. III.: applications

    Directory of Open Access Journals (Sweden)

    Emanuel Carrilho

    2006-07-01

    Full Text Available The first two papers in this series described the basic theory involved in supercritical fluid chromatography (SFC, how the technique evolved from gas and liquid chromatography and how the instrumentation was developed. Over the last two years, a commercial, dedicated packed-column SFC/MS instrument appeared on the market. The SFC continues to grow in use, with fundamental developments, coupled with a steady rise in the number of industrial users and applications.

  17. Separation of furostanol saponins by supercritical fluid chromatography.

    Science.gov (United States)

    Yang, Jie; Zhu, Lingling; Zhao, Yang; Xu, Yongwei; Sun, Qinglong; Liu, Shuchen; Liu, Chao; Ma, Baiping

    2017-10-25

    Supercritical fluid chromatography (SFC) has good separation efficiency and is suitable for separating weakly polar compounds. Furostanol saponins, as an important kind of steroidal saponins, generally have two sugar chains, which are polar and hydrophilic. The hydroxyl group at the C-22 position of furostanol saponins is active and easily reacts with lower alcohols under appropriate conditions. The separation of hydrophilic furostanol saponins was tested by SFC in this study. The effects of chromatographic conditions on the separation of the mixed furostanol saponins and their hydroxyl derivatives at the C-22 position were studied. The conditions for SFC, which included different column polarity, modifier, additive, and column temperature, were tested. After optimization, the mixed 10 similar structures of furostanol saponins were separated in 22min on the Diol column at a temperature of 40°C. The mobile phase was CO 2 (mobile phase A) and methanol (containing 0.2% NH 3 ∙H 2 O and 3% H 2 O) (mobile phase B). The backpressure was maintained isobarically at 11.03MPa. SFC was found to be effective in separating the furostanol saponins that shared the same aglycone but varied in sugar chains. SFC was sensitive to the number and type of sugars. The resolution of furostanol saponin isomers was not ideal. The extract of Dioscorea zingiberensis C. H. Wright was profiled by SFC-quadrupole time-of-flight mass spectrometry. The main saponins of the extract were well separated. Therefore, SFC could be used for separating hydrophilic furostanol saponins and analyzing traditional Chinese medicines that mainly contained steroidal saponins. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Application of response surface methodology for the optimization of supercritical fluid extraction of essential oil from pomegranate (Punica granatum L.) peel.

    Science.gov (United States)

    Ara, Katayoun Mahdavi; Raofie, Farhad

    2016-07-01

    Essential oils and volatile components of pomegranate ( Punica granatum L.) peel of the Malas variety from Meybod, Iran, were extracted using supercritical fluid extraction (SFE) and hydro-distillation methods. The experimental parameters of SFE that is pressure, temperature, extraction time, and modifier (methanol) volume were optimized using a central composite design after a (2 4-1 ) fractional factorial design. Detailed chemical composition of the essential oils and volatile components obtained by hydro-distillation and optimum condition of the supercritical CO 2 extraction were analyzed by GC-MS, and seventy-three and forty-six compounds were identified according to their retention indices and mass spectra, respectively. The optimum SFE conditions were 350 atm pressure, 55 °C temperature, 30 min extraction time, and 150 µL methanol. Results showed that oleic acid, palmitic acid and (-)-Borneol were major compounds in both extracts. The optimum extraction yield was 1.18 % (w/w) for SFE and 0.21 % (v/w) for hydro-distillation.

  19. Effects of liquid post-column addition in electrospray ionization performance in supercritical fluid chromatography-mass spectrometry.

    Science.gov (United States)

    Akbal, Laura; Hopfgartner, Gérard

    2017-09-29

    In supercritical fluid chromatography coupled to atmospheric pressure ionization mass spectrometry (SFC-MS), the use of a make-up post-column is almost mandatory to avoid analyte precipitation, especially when using low percentage of modifier (supercritical conditions (1mL/min 40°C, 150bar) to gaseous state (room temperature, atmospheric pressure), the CO 2 expands around 430 times, contributing to almost 5% of the nebulizing process. In positive mode, the presence of ammonium ions either in the mobile phase or in the make-up did significantly increase the MS signal, even at basic apparent pH. The ionization performance of electrospray is influenced by the acidic buffer power of the carbon dioxide, and was found to be restricted in the apparent pH range of 3.8-7.2 in the various conditions investigated. This may challenge sensitive detection in negative mode, as illustrated for bosentan. The use of DMSO as make-up additive (up to 30%) showed a simplification of the full scan spectrum regarding the adducts. Finally, the optimization of make-up composition leads to an enhancement up to a factor of 69 on the electrospray MS response signal, for the SFC-SRM/MS analysis of HIV protease inhibitors in plasma extracted from Dried Plasma Spots. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Error analysis of supercritical water correlations using ATHLET system code under DHT conditions

    Energy Technology Data Exchange (ETDEWEB)

    Samuel, J., E-mail: jeffrey.samuel@uoit.ca [Univ. of Ontario Inst. of Tech., Oshawa, ON (Canada)

    2014-07-01

    The thermal-hydraulic computer code ATHLET (Analysis of THermal-hydraulics of LEaks and Transients) is used for analysis of anticipated and abnormal plant transients, including safety analysis of Light Water Reactors (LWRs) and Russian Graphite-Moderated High Power Channel-type Reactors (RBMKs). The range of applicability of ATHLET has been extended to supercritical water by updating the fluid-and transport-properties packages, thus enabling the code to the used in analysis of SuperCritical Water-cooled Reactors (SCWRs). Several well-known heat-transfer correlations for supercritical fluids were added to the ATHLET code and a numerical model was created to represent an experimental test section. In this work, the error in the Heat Transfer Coefficient (HTC) calculation by the ATHLET model is studied along with the ability of the various correlations to predict different heat transfer regimes. (author)

  1. Preparation of minute particle using supercritical fluid; Chorinkai ryutai wo mochiita biryushi no chosei

    Energy Technology Data Exchange (ETDEWEB)

    Ajiri, T [Tohoku University, Sendai (Japan). Faculty of Engineering

    1995-03-05

    The metal oxide minute particle synthesis method according to the water-heat reaction in supercritical water was described. Metal salt liquid solution was subjected to hydrolysis when heated to become metal hydroxide but dehydration reaction was generated at a high temperature to generate metal oxide minute particle. Metal salt aqueous solution was supplied to a circulation system unit to contact heated water and was rapidly heated to supercritical state and then was subjected to hydrolysis/dehydration reaction, thus continuously collecting metal oxide minute particles. The hydrolysis speed was in first order for the metal ion concentration and the reaction speed was accelerated by several tens of times when entering supercritical region from subcritical region. When the temperature was rapidly increased to the supercritical state, a radical hydrolysis was generated and a high saturation was instantly reached and minute particles tended to be generated easily since the dissolution force of supercritical water for a product was small. A minute particle with a crystallizability of 5 nm was obtained by synthesizing ceria super-minute particle which was the abrasive of an optical glass material. A single phase of a high magnetization characteristic was synthesized continuously and quickly (faster than a conventional method by two orders or more) in the continuous synthesis of Ba ferrite as a magnetic recording material. 12 refs., 3 figs., 1 tab.

  2. 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.

  3. The effect of low-concentration inorganic materials on the behaviour of supercritical water

    Energy Technology Data Exchange (ETDEWEB)

    Imre, A.R., E-mail: imre@aeki.kfki.h [KFKI Atomic Energy Research Institute, POB 49, Budapest (Hungary); Hazi, G.; Horvath, A.; Maraczy, Cs. [KFKI Atomic Energy Research Institute, POB 49, Budapest (Hungary); Mazur, V.; Artemenko, S. [Odessa State Academy of Refrigeration, 1/3 Dvoryanslaya Str., 65026, Odessa (Ukraine)

    2011-01-15

    Research highlights: Small amount of inorganic materials (like corrosion products) can be dissolved in the supercritical water. Pseudo-critical temperature and other properties will be changed. Thermal and hydraulic behaviours of the SCW with small amount of contaminants differ in great extent from the behaviour of pure SCW. - Abstract: Supercritical water is a promising working fluid in the new Generation IV nuclear power plants. Due to the presence of the pseudo-critical line, the thermo-hydraulics (thermal and flow properties) and the physical chemistry of the supercritical water differ significantly from the pressurized hot water used in pressurized water reactors. In this study we would like to analyse the effect of small amount of inorganic material on the thermo-hydraulics of the supercritical water cooled nuclear reactors and other, non-nuclear supercritical water loops.

  4. Development of correlations for combustion modelling with supercritical surrogate jet fuels

    Directory of Open Access Journals (Sweden)

    Raja Sekhar Dondapati

    2017-12-01

    Full Text Available Supercritical fluid technology finds its application in almost all engineering aspects in one or other way. Technology of clean jet fuel combustion is also seeing supercritical fluids as one of their contender in order to mitigate the challenges related to global warming and health issues occurred due to unwanted emissions which are found to be the by-products in conventional jet engine combustion. As jet fuel is a blend of hundred of hydrocarbons, thus estimation of chemical kinetics and emission characteristics while simulation become much complex. Advancement in supercritical jet fuel combustion technology demands reliable property statistics of jet fuel as a function temperature and pressure. Therefore, in the present work one jet fuel surrogate (n-dodecane which has been recognized as the constituent of real jet fuel is studied and thermophysical properties of each is evaluated in the supercritical regime. Correlation has been developed for two transport properties namely density and viscosity at the critical pressure and over a wide range of temperatures (TC + 100 K. Further, to endorse the reliability of the developed correlation, two arithmetical parameters have been evaluated which illustrates an outstanding agreement between the data obtained from online NIST Web-Book and the developed correlation.

  5. Thermal and hydrodynamic characteristics of supercritical CO2 natural circulation in closed loops

    International Nuclear Information System (INIS)

    Chen, Lin; Deng, Bi-Li; Jiang, Bin; Zhang, Xin-Rong

    2013-01-01

    Highlights: ► We model thermosyphon heat transfer and stability with super-/trans-critical turbulence model incorporated. ► Potentials of super-/trans-critical CO 2 thermosyphon are confirmed. ► Three characteristics found: flow instability; high flow rate with density wave; heat transfer discrepancies. ► Major laws of system stability factors are different compared with traditional fluids. ► Traditional thermosyphon flow correlation has its limitations and deserves further development. -- Abstract: Natural convective flow of supercritical fluids has become a hot topic in engineering applications. Natural circulation thermosyphon using supercritical/trans-critical CO 2 can be a potential choice for effectively transportation of heat and mass without pumping devices. This paper presents a series of numerical investigations into the fundamental features in a supercritical/trans-critical CO 2 based natural circulation loop. New heat transport model aiming at trans-critical thermosyphon heat transfer and stability is proposed with supercritical/trans-critical turbulence model incorporated. In this study, the fundamentals include the basic flow and heat transfer behavior of the above loop, the effect of heat source temperature on system stability, the effect of loop diameter on natural convection supercritical CO 2 loop and its coupling effect with heat source temperature and the effect of constant changing heat input condition and system behavior evolution during unsteady input or failure conditions. The fundamental potentials of supercritical/trans-critical CO 2 based natural convection system are confirmed. Basic supercritical CO 2 closed loop flow and heat transfer behaviors are clarified. During this study, the CO 2 loop stability map are also put forward and introduced as an important feature of supercritical CO 2 system. Stability factors of natural convective trans-critical CO 2 flow and its implications on real system control are also discussed in

  6. Thermal stability of biodiesel in supercritical methanol

    Energy Technology Data Exchange (ETDEWEB)

    Hiroaki Imahara; Eiji Minami; Shusaku Hari; Shiro Saka [Kyoto University, Kyoto (Japan). Department of Socio-Environmental Energy Science

    2008-01-15

    Non-catalytic biodiesel production technologies from oils/fats in plants and animals have been developed in our laboratory employing supercritical methanol. Due to conditions in high temperature and high pressure of the supercritical fluid, thermal stability of fatty acid methyl esters and actual biodiesel prepared from various plant oils was studied in supercritical methanol over a range of its condition between 270{sup o}C/17 MPa and 380{sup o}C/56 MPa. In addition, the effect of thermal degradation on cold flow properties was studied. As a result, it was found that all fatty acid methyl esters including poly-unsaturated ones were stable at 270{sup o}C/17 MPa, but at 350{sup o}C/43 MPa, they were partly decomposed to reduce the yield with isomerization from cis-type to trans-type. These behaviors were also observed for actual biodiesel prepared from linseed oil, safflower oil, which are high in poly-unsaturated fatty acids. Cold flow properties of actual biodiesel, however, remained almost unchanged after supercritical methanol exposure at 270{sup o}C/17 MPa and 350{sup o}C/43 MPa. For the latter condition, however, poly-unsaturated fatty acids were sacrificed to be decomposed and reduced in yield. From these results, it was clarified that reaction temperature in supercritical methanol process should be lower than 300{sup o}C, preferably 270{sup o}C with a supercritical pressure higher than 8.09 MPa, in terms of thermal stabilization for high-quality biodiesel production. 9 refs., 3 figs., 4 tabs.

  7. Gass-Assisted Displacement of Non-Newtonian Fluids

    DEFF Research Database (Denmark)

    Rasmussen, Henrik Koblitz; Eriksson, Torbjörn Gerhard

    2003-01-01

    in a circular cylinder. This is a simple model system used to investigate the gas-fluid displacement, as the problem is reduced to an axis-symmetric flow problem. The understanding of this process is relevant for the geometrically much more complex polymer processing operation Gas-assisted injection moulding...... (GAIM). This is a process, where a mould is filled partly with a polymer melt followed by the injection of inert gas into the core of the polymer melt. The numerical analysis of the fluid flow concerning the experimental observations data in these publications is all based on Newtonian or general...... equation of Boger fluids is the Oldroyd-B model. This model has, with success, been able to describe the complex flow behaviours of Boger fluid. Though, refinements in the flow analysis can be obtained using more complex constitutive models. To keep the flow analysis as simple as possible the Oldroyd...

  8. FY1995 generic supercritical water technology; 1995 nendo generic technology to shite no chorinkai riyo gijutsu

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1997-03-01

    For the establishment of the basis of supercritical fluid technology, we perform elucidation of the specific feature of the supercritical fluid as a reaction media and development of some new process. In this study, we first studied the fluid structure of SCF through in-situ spectroscopy and MD simulation. As a result, significant hydrogen bonding amongst water molecules and a solvation structure around the solute were observed in the supercritical state. This fluid structure has new features different from that of high temperature steam or liquid water. We found that this is closely related to the difference of bulk properties of SCF and local one around the solute. On the basis of these fundamental findings and with the better understanding of the specific features of SCF as a reaction media, development of some new process had been conducted more efficiently and successfully. The processes being developed in this study include 1) waste biomass and plastic conversion to recover chemicals, 2) hydrogenation of heavy oil for desulphurization through partial oxidation 1 and 3) hydrothermal synthesis of metal oxide fine particles. (NEDO)

  9. Supercritical Regeneration of an Activated Carbon Fiber Exhausted with Phenol

    OpenAIRE

    M. Jesus Sanchez-Montero; Jennifer Pelaz; Nicolas Martin-Sanchez; Carmen Izquierdo; Francisco Salvador

    2018-01-01

    The properties of supercritical CO2 (SCCO2) and supercritical water (SCW) turn them into fluids with a great ability to remove organic adsorbates retained on solids. These properties were used herein to regenerate an activated carbon fiber (ACF) saturated with a pollutant usually contained in wastewater and drinking water, phenol. Severe regeneration conditions, up to 225 bar and 400 °C, had to be employed in SCCO2 regeneration to break the strong interaction established between phenol and th...

  10. Development of a model system to study fuel autoxidation in supercritical media: decomposition kinetics of 2,2{prime}-azobis (isobutyronitrile) in supercritical carbon dioxide

    Energy Technology Data Exchange (ETDEWEB)

    Morris, R.E.; Mera, A.E.; Brady, R.F. Jr. [Naval Research Laboratory, Washington, DC (USA)

    2000-07-01

    A high pressure reactor has been constructed and used for in situ spectroscopic measurements of reaction kinetics in supercritical fluids. The thermal decomposition of 2,2{prime}-azobis(isobutyronitrile) (AIBN) in supercritical carbon dioxide (SC-CO{sub 2}) was studied as part of an effort to characterize free-radical autoxidation of hydrocarbon fuels under supercritical conditions. The findings show that AIBN decomposes both thermally and photochemically in SC-CO{sub 2} to form the 2-cyano-2-propyl free radical which dimerizes to form tetramethylsuccinic dinitrile and dimethyl-N-(2-cyano-2-propyl) ketenimine. Examination of the decomposition kinetics of the ketenimine revealed that it was photochemically stable in the kinetic reactor, but decomposed thermally to form the dinitrile. 21 refs., 4 figs., 1 tab.

  11. Thermophysical properties of supercritical fluids and fluid mixtures

    International Nuclear Information System (INIS)

    Sengers, J.V.

    1989-08-01

    The purpose of the research is to extend the theory of critical phenomena in fluids and fluid mixtures to obtain scientifically based equations that include the crossover from the asymptotic singular behavior of the thermophysical properties close to the critical point to the regular behavior of these properties far away from the critical point

  12. 179 Extraction of Coal-tar Pitch by Supercritical Carbon Dioxide ...

    African Journals Online (AJOL)

    Meyer

    Several extractions of coal-tar pitch were performed using supercritical fluid ..... pressure and temperature, unlike exhaustive extraction, which involves a change in ... mechanism that is operative on extracting coal-tar pitch components with.

  13. Phytochemical profile and anticholinesterase and antimicrobial activities of supercritical versus conventional extracts of Satureja montana.

    Science.gov (United States)

    Silva, Filipa V M; Martins, Alice; Salta, Joana; Neng, Nuno R; Nogueira, José M F; Mira, Delfina; Gaspar, Natália; Justino, Jorge; Grosso, Clara; Urieta, José S; Palavra, António M S; Rauter, Amélia P

    2009-12-23

    Winter savory Satureja montana is a medicinal herb used in traditional gastronomy for seasoning meats and salads. This study reports a comparison between conventional (hydrodistillation, HD, and Soxhlet extraction, SE) and alternative (supercritical fluid extraction, SFE) extraction methods to assess the best option to obtain bioactive compounds. Two different types of extracts were tested, the volatile (SFE-90 bar, second separator vs HD) and the nonvolatile fractions (SFE-250 bar, first and second separator vs SE). The inhibitory activity over acetyl- and butyrylcholinesterase by S. montana extracts was assessed as a potential indicator for the control of Alzheimer's disease. The supercritical nonvolatile fractions, which showed the highest content of (+)-catechin, chlorogenic, vanillic, and protocatechuic acids, also inhibited selectively and significantly butyrylcholinesterase, whereas the nonvolatile conventional extract did not affect this enzyme. Microbial susceptibility tests revealed the great potential of S. montana volatile supercritical fluid extract for the growth control and inactivation of Bacillus subtilis and Bacillus cereus, showing some activity against Botrytis spp. and Pyricularia oryzae. Although some studies were carried out on S. montana, the phytochemical analysis together with the biological properties, namely, the anticholinesterase and antimicrobial activities of the plant nonvolatile and volatile supercritical fluid extracts, are described herein for the first time.

  14. Antioxidant effects of supercritical fluid garlic extracts in canned artichokes.

    Science.gov (United States)

    Bravi, E; Marconi, O; Sileoni, V; Rollo, M R; Perretti, G

    2016-10-01

    The effects of adding supercritical carbon dioxide extracts of garlic (at two different concentrations of allicin) on select chemical indices in extra-virgin olive oil used to canned artichokes were studied. Tests were performed after processing and over a storage period of 1 year. A sensorial test was also conducted on the canned artichokes to establish the impact on flavor (in particular perceptions of rancidity and garlic flavor). Acidity, peroxide levels and p -anisidine values were measured as quality analytical parameters. Radical scavenging activity was also evaluated using the DPPH assay. The samples containing supercritical garlic extracts were compared with several other formulations, including control sample (prepared by mixing artichokes with powdered chili pepper and fresh garlic), artichokes with only garlic or only chili pepper, and artichokes treated with the synthetic antioxidant BHT. The results suggested that the allicin extract may be superior, or at least comparable, with BHT in preserving canned artichokes as demonstrated by its positive effects on oxidative stability and sensory profile.

  15. Supercritical fluid chromatography for GMP analysis in support of pharmaceutical development and manufacturing activities.

    Science.gov (United States)

    Hicks, Michael B; Regalado, Erik L; Tan, Feng; Gong, Xiaoyi; Welch, Christopher J

    2016-01-05

    Supercritical fluid chromatography (SFC) has long been a preferred method for enantiopurity analysis in support of pharmaceutical discovery and development, but implementation of the technique in regulated GMP laboratories has been somewhat slow, owing to limitations in instrument sensitivity, reproducibility, accuracy and robustness. In recent years, commercialization of next generation analytical SFC instrumentation has addressed previous shortcomings, making the technique better suited for GMP analysis. In this study we investigate the use of modern SFC for enantiopurity analysis of several pharmaceutical intermediates and compare the results with the conventional HPLC approaches historically used for analysis in a GMP setting. The findings clearly illustrate that modern SFC now exhibits improved precision, reproducibility, accuracy and robustness; also providing superior resolution and peak capacity compared to HPLC. Based on these findings, the use of modern chiral SFC is recommended for GMP studies of stereochemistry in pharmaceutical development and manufacturing. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Direct numerical simulation of heat transfer to CO2 at supercritical pressure in a vertical tube

    International Nuclear Information System (INIS)

    Bae, Joong-Hun; Yoo, Jung-Yul; Choi, Hae-Cheon

    2003-01-01

    In the present study, the turbulent heat transfer to CO 2 at supercritical pressure in a vertical tube is investigated using Direct Numerical Simulation (DNS), where no turbulence model is adopted. Heat transfer to the supercritical pressure fluids is characterized by rapid variation of thermodynamic/ thermo-physical properties in the fluids. This change in properties occurs within a very narrow range of temperature across the so-called pseudo-critical temperature, causing a peculiar behavior of heat transfer characteristics. The buoyancy effects associated with very large changes in density proved to play a major role in turbulent heat transfer to supercritical pressure fluids. Depending on the degree of buoyancy effects, turbulent heat transfer may increase or significantly decrease, resulting in a local hot spot along the wall. Based on the results of the present DNS study combined with theoretical considerations for turbulent mixed convection heat transfer, the basic mechanism of this local heat transfer deterioration is explained

  17. 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.

  18. Tuning the nanostructures and optical properties of undoped and N-doped ZnO by supercritical fluid treatment

    Science.gov (United States)

    Li, Yaping; Wang, Hui-Qiong; Chu, Tian-Jian; Li, Yu-Chiuan; Li, Xiaojun; Liao, Xiaxia; Wang, Xiaodan; Zhou, Hua; Kang, Junyong; Chang, Kuan-Chang; Chang, Ting-Chang; Tsai, Tsung-Ming; Zheng, Jin-Cheng

    2018-05-01

    Treatment of ZnO films in a supercritical fluid (SCF) has been reported to improve the performance of devices in which the treated ZnO films are incorporated; however, the mechanism of this improvement remains unclear. In this paper, we study the transformation of the surface morphologies and emission properties of ZnO films before and after SCF treatment, establishing the relationship between the treated and untreated structures and thereby enabling tuning of the catalytic or opto-electronic performance of ZnO films or ZnO-film-based devices. Both undoped and N-doped ZnO nanostructures generated by SCF treatment of films are investigated using techniques to characterize their surface morphology (scanning electron microscopy (SEM) and atomic force microscopy (AFM)) as well as room-temperature photoluminescence (RT-PL) spectroscopy. The water-mixed supercritical CO2 (W-SCCO2) technology was found to form nanostructures in ZnO films through a self-catalyzed process enabled by the Zn-rich conditions in the ZnO films. The W-SCCO2 was also found to promote the inhibition of defect luminescence by introducing -OH groups onto the films. Two models are proposed to explain the effects of the treatment with W-SCCO2. This work demonstrates that the W-SCCO2 technology can be used as an effective tool for the nanodesign and property enhancement of functional metal oxides.

  19. 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

  20. The effect of high concentration additive on chiral separations in supercritical fluid chromatography.

    Science.gov (United States)

    Speybrouck, David; Doublet, Charline; Cardinael, Pascal; Fiol-Petit, Catherine; Corens, David

    2017-08-11

    Supercritical Fluid Chromatography is frequently used to efficiently handle separations of enantiomers. The separation of basic analytes usually requires the addition of a basic additive in the mobile phase to improve the peak shape or even to elute the compounds. The effect of increasing the concentration of 2-propylamine as additive on the elution of a series of basic compounds on a Chiralpak-AD stationary phase was studied. In this study, unusual additive concentrations ranging from 0.3% to 10% of 2-propylamine 2-propylaminein the modifier were explored and the effect on retention, peak shape, selectivity and resolution was evaluated. The addition of a large quantity of additive allowed to drastically improve the selectivity and the resolution, and even enantiomers elution order reversal was observed by changing the concentration of basic additive. The role of the ratio additive/modifier appeared a key to tune the enantioselectivity. Finally, the impact of these drastic conditions on the column material was evaluated. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Supercritical Nonlinear Vibration of a Fluid-Conveying Pipe Subjected to a Strong External Excitation

    Directory of Open Access Journals (Sweden)

    Yan-Lei Zhang

    2016-01-01

    Full Text Available Nonlinear vibration of a fluid-conveying pipe subjected to a transverse external harmonic excitation is investigated in the case with two-to-one internal resonance. The excitation amplitude is in the same magnitude of the transverse displacement. The fluid in the pipes flows in the speed larger than the critical speed so that the straight configuration becomes an unstable equilibrium and two curved configurations bifurcate as stable equilibriums. The motion measured from each of curved equilibrium configurations is governed by a nonlinear integro-partial-differential equation with variable coefficients. The Galerkin method is employed to discretize the governing equation into a gyroscopic system consisting of a set of coupled nonlinear ordinary differential equations. The method of multiple scales is applied to analyze approximately the gyroscopic system. A set of first-order ordinary differential equations governing the modulations of the amplitude and the phase are derived via the method. In the supercritical regime, the subharmonic, superharmonic, and combination resonances are examined in the presence of the 2 : 1 internal resonance. The steady-state responses and their stabilities are determined. The various jump phenomena in the amplitude-frequency response curves are demonstrated. The effects of the viscosity, the excitation amplitude, the nonlinearity, and the flow speed are observed. The analytical results are supported by the numerical integration.

  2. 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)

  3. 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

  4. Rapid purification of diastereoisomers from Piper kadsura using supercritical fluid chromatography with chiral stationary phases.

    Science.gov (United States)

    Xin, Huaxia; Dai, Zhuoshun; Cai, Jianfeng; Ke, Yanxiong; Shi, Hui; Fu, Qing; Jin, Yu; Liang, Xinmiao

    2017-08-04

    Supercritical fluid chromatography (SFC) with chiral stationary phases (CSPs) is an advanced solution for the separation of achiral compounds in Piper kadsura. Analogues and stereoisomers are abundant in natural products, but there are obstacles in separation using conventional method. In this paper, four lignan diastereoisomers, (-)-Galbelgin, (-)-Ganschisandrin, Galgravin and (-)-Veraguensin, from Piper kadsura were separated and purified by chiral SFC. Purification strategy was designed, considering of the compound enrichment, sample purity and purification throughput. Two-step achiral purification method on chiral preparative columns with stacked automated injections was developed. Unconventional mobile phase modifier dichloromethane (DCM) was applied to improve the sample solubility. Four diastereoisomers was prepared at the respective weight of 103.1mg, 10.0mg, 152.3mg and 178.6mg from 710mg extract with the purity of greater than 98%. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Measurements of convective heat transfer to vertical upward flows of CO{sub 2} in circular tubes at near-critical and supercritical pressures

    Energy Technology Data Exchange (ETDEWEB)

    Zahlan, H., E-mail: hussamzahlan@gmail.com [Canadian Nuclear Laboratories, Chalk River, K0J 1J0 (Canada); Department of Mechanical Engineering, University of Ottawa, Ottawa, ON K1N 6N5 (Canada); Groeneveld, D. [Canadian Nuclear Laboratories, Chalk River, K0J 1J0 (Canada); Department of Mechanical Engineering, University of Ottawa, Ottawa, ON K1N 6N5 (Canada); Tavoularis, S. [Department of Mechanical Engineering, University of Ottawa, Ottawa, ON K1N 6N5 (Canada)

    2015-08-15

    Highlights: • We present and discuss results of thermal–hydraulic measurements in CO{sub 2} for the near critical and supercritical pressure region. • We report the full heat transfer and pressure drop database. - Abstract: An extensive experimental program of heat transfer measurements has been completed recently at the University of Ottawa's supercritical pressure test facility (SCUOL). Thermal–hydraulics tests were performed for vertical upflow of carbon dioxide in directly heated tubes with inner diameters of 8 and 22 mm, at high subcritical, near-critical and supercritical pressures. The test conditions, when converted to water-equivalent values, correspond to conditions of interest to current Super-Critical Water-Cooled Reactor designs, and include many measurements under conditions for which few data are available in the literature. These data significantly complement the existing experimental database and are being used for the derivation and validation of a new heat transfer prediction method in progress at the University of Ottawa. The same data are also suitable for the assessment of the accuracy of other heat transfer prediction methods and fluid-to-fluid scaling laws for near-critical and supercritical pressures. In addition, they permit further examination of previously suggested relationships describing the critical heat flux and post-dryout heat transfer coefficient at high subcritical pressures and the boundaries of the deteriorated/enhanced heat transfer regions for near-critical and supercritical pressures. The measurements reported in this paper cover several subcritical heat transfer modes, including single phase liquid heat transfer, nucleate boiling, critical heat flux, post-dryout heat transfer and superheated vapor heat transfer; they also cover several supercritical heat transfer modes, including heat transfer to liquid-like supercritical fluid and heat transfer to vapor-like supercritical fluid, which occurred in the

  6. Polymer-filled microcontainers for oral delivery loaded using supercritical impregnation

    DEFF Research Database (Denmark)

    Marizza, Paolo; Keller, Stephan Sylvest; Müllertz, Anette

    2014-01-01

    with a quasi-no-waste performance. Then ketoprofen is impregnated in the polymer matrix by using supercritical carbon dioxide (scCO2) as loading medium. The amount of polymer is controlled by the volume and the number of droplets of dispensed polymer and drug loading is tuned by varying the impregnation...... procedures. This work proposes an effective loading technique for a poorly soluble model drug in microcontainers, by combining inkjet printing and supercritical fluid impregnation. Well defined quantities of poly(vinyl pyrrolidone) (PVP) solutions are dispensed into microcontainers by inkjet printing...

  7. Working regime identification for natural circulation loops by comparative thermalhydraulic analyses with three fluids under identical operating conditions

    International Nuclear Information System (INIS)

    Sarkar, Milan K.S.; Basu, Dipankar N.

    2015-01-01

    Highlights: • Thermalhydraulic analyses of NCL to justify the use of supercritical condition. • Mass flow rate of supercritical loop increases with heater power till a maxima. • Supercritical loop suffer from HTD beyond the maxima with jump in fluid temperature. • HTD is pronounced at higher sink temperatures and pressures just above critical. • Supercritical CO_2 is preferred fluid till the HTD and single-phase water afterwards. - Abstract: Computational investigation for comparative thermalhydraulic analyses of rectangular natural circulation loops is performed to propose a guideline for selecting the working fluid and nature of the loop, subcritical or supercritical, under identical levels of operating parameters like pressure, heating power and coolant temperature. A 3-d uniform-diameter loop geometry is developed with horizontal heating and cooling. Heating is provided in constant heat flux mode, whereas cooling is through a constant temperature sink. Due to favourable thermophysical properties and environmental conformity, water, CO_2 and R134a are selected as possible working fluids. Operational parameters are set so as to have sub- to supercritical condition for CO_2, supercritical for R134a and single-phase liquid for water. Mass flow rate for supercritical fluid rapidly increases with heater power, when the fluid is allowed to cross the pseudocritical point during its passage through the heater, and exhibits a maxima. Drastic fall in mass flow rate can be observed beyond the maxima, accompanied by a jump in maximum fluid temperature and a rapid decline in sink-side heat transfer coefficient. That can be identified as heat transfer deterioration in supercritical natural circulation loops, a highly undesirable situation from loop safety point of view. Allowable working range of heater power can be enhanced by increasing system pressure and decreasing sink temperature. For any specified set of operating conditions, CO_2-based supercritical loops

  8. Working regime identification for natural circulation loops by comparative thermalhydraulic analyses with three fluids under identical operating conditions

    Energy Technology Data Exchange (ETDEWEB)

    Sarkar, Milan K.S.; Basu, Dipankar N., E-mail: dipankar.n.basu@gmail.com

    2015-11-15

    Highlights: • Thermalhydraulic analyses of NCL to justify the use of supercritical condition. • Mass flow rate of supercritical loop increases with heater power till a maxima. • Supercritical loop suffer from HTD beyond the maxima with jump in fluid temperature. • HTD is pronounced at higher sink temperatures and pressures just above critical. • Supercritical CO{sub 2} is preferred fluid till the HTD and single-phase water afterwards. - Abstract: Computational investigation for comparative thermalhydraulic analyses of rectangular natural circulation loops is performed to propose a guideline for selecting the working fluid and nature of the loop, subcritical or supercritical, under identical levels of operating parameters like pressure, heating power and coolant temperature. A 3-d uniform-diameter loop geometry is developed with horizontal heating and cooling. Heating is provided in constant heat flux mode, whereas cooling is through a constant temperature sink. Due to favourable thermophysical properties and environmental conformity, water, CO{sub 2} and R134a are selected as possible working fluids. Operational parameters are set so as to have sub- to supercritical condition for CO{sub 2}, supercritical for R134a and single-phase liquid for water. Mass flow rate for supercritical fluid rapidly increases with heater power, when the fluid is allowed to cross the pseudocritical point during its passage through the heater, and exhibits a maxima. Drastic fall in mass flow rate can be observed beyond the maxima, accompanied by a jump in maximum fluid temperature and a rapid decline in sink-side heat transfer coefficient. That can be identified as heat transfer deterioration in supercritical natural circulation loops, a highly undesirable situation from loop safety point of view. Allowable working range of heater power can be enhanced by increasing system pressure and decreasing sink temperature. For any specified set of operating conditions, CO{sub 2}-based

  9. Novel Supercritical Carbon Dioxide Power Cycle Utilizing Pressured Oxy-combustion in Conjunction with Cryogenic Compression

    Energy Technology Data Exchange (ETDEWEB)

    Brun, Klaus; McClung, Aaron; Davis, John

    2014-03-31

    such as blade cooling. The overall technical readiness of the supercritical oxy-combustion cycle is TRL 2, Technology Concept, due to the maturity level of the supercritical oxy-combustor for solid fuels, and several critical supporting components, as identified in the Technical Gap Analysis. The supercritical oxycombustor for solid fuels operating at pressures near 100 atm is a unique component of the supercritical oxy-combustion cycle. In addition to the low TRL supercritical oxy-combustor, secondary systems were identified that would require adaptation for use with the supercritical oxycombustion cycle. These secondary systems include the high pressure pulverized coal feed, high temperature cyclone, removal of post-combustion particulates from the high pressure cyclone underflow stream, and micro-channel heat exchangers tolerant of particulate loading. Bench scale testing was utilized to measure coal combustion properties at elevated pressures in a CO{sub 2} environment. This testing included coal slurry preparation, visualization of coal injection into a high pressure fluid, and modification of existing test equipment to facilitate the combustion properties testing. Additional bench scale testing evaluated the effectiveness of a rotary atomizer for injecting a coal-water slurry into a fluid with similar densities, as opposed to the typical application where the high density fluid is injected into a low density fluid. The swirl type supercritical oxy-combustor was developed from initial concept to an advanced design stage through numerical simulation using FLUENT and Chemkin to model the flow through the combustor and provide initial assessment of the coal combustion reactions in the flow path. This effort enabled the initial combustor mechanical layout, initial pressure vessel design, and the conceptual layout of a pilot scale test loop. A pilot scale demonstration of the supercritical oxy-combustion cycle is proposed as the next step in the technology development

  10. Development and validation of ultra-high performance supercritical fluid chromatography method for determination of illegal dyes and comparison to ultra-high performance liquid chromatography method.

    Science.gov (United States)

    Khalikova, Maria A; Šatínský, Dalibor; Solich, Petr; Nováková, Lucie

    2015-05-18

    A novel simple, fast and efficient ultra-high performance supercritical fluid chromatography (UHPSFC) method was developed and validated for the separation and quantitative determination of eleven illegal dyes in chili-containing spices. The method involved a simple ultrasound-assisted liquid extraction of illegal compounds with tetrahydrofuran. The separation was performed using a supercritical fluid chromatography system and CSH Fluoro-Phenyl stationary phase at 70°C. The mobile phase was carbon dioxide and the mixture of methanol:acetonitrile (1:1, v/v) with 2.5% formic acid as an additive at the flow rate 2.0 mL min(-1). The UV-vis detection was accomplished at 500 nm for seven compounds and at 420 nm for Sudan Orange G, Butter Yellow, Fast Garnet GBC and Methyl Red due to their maximum of absorbance. All eleven compounds were separated in less than 5 min. The method was successfully validated and applied using three commercial samples of chili-containing spices - Chili sauce (Indonesia), Feferony sauce (Slovakia) and Mojo sauce (Spain). The linearity range of proposed method was 0.50-9.09 mg kg(-1) (r ≥ 0.995). The detection limits were determined as signal to noise ratio of 3 and were ranged from 0.15 mg kg(-1) to 0.60 mg kg(-1) (1.80 mg kg(-1) for Fast Garnet) for standard solution and from 0.25 mg kg(-1) to 1.00 mg kg(-1) (2.50 mg kg(-1) for Fast Garnet, 1.50 mg kg(-1) for Sudan Red 7B) for chili-containing samples. The recovery values were in the range of 73.5-107.2% and relative standard deviation ranging from 0.1% to 8.2% for within-day precision and from 0.5% to 8.8% for between-day precision. The method showed potential for being used to monitor forbidden dyes in food constituents. The developed UHPSFC method was compared to the UHPLC-UV method. The orthogonality of Sudan dyes separation by these two methods was demonstrated. Benefits and drawbacks were discussed showing the reliability of both methods for monitoring of studied illegal dyes in real

  11. 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).

  12. Supercritical Water Mixture (SCWM) Experiment

    Science.gov (United States)

    Hicks, Michael C.; Hegde, Uday G.

    2012-01-01

    The subject presentation, entitled, Supercritical Water Mixture (SCWM) Experiment, was presented at the International Space Station (ISS) Increment 33/34 Science Symposium. This presentation provides an overview of an international collaboration between NASA and CNES to study the behavior of a dilute aqueous solution of Na2SO4 (5% w) at near-critical conditions. The Supercritical Water Mixture (SCWM) investigation, serves as important precursor work for subsequent Supercritical Water Oxidation (SCWO) experiments. The SCWM investigation will be performed in DECLICs High Temperature Insert (HTI) for the purpose of studying critical fluid phenomena at high temperatures and pressures. The HTI includes a completely sealed and integrated test cell (i.e., Sample Cell Unit SCU) that will contain approximately 0.3 ml of the aqueous test solution. During the sequence of tests, scheduled to be performed in FY13, temperatures and pressures will be elevated to critical conditions (i.e., Tc = 374C and Pc = 22 MPa) in order to observe salt precipitation, precipitate agglomeration and precipitate transport in the presence of a temperature gradient without the influences of gravitational forces. This presentation provides an overview of the motivation for this work, a description of the DECLIC HTI hardware, the proposed test sequences, and a brief discussion of the scientific research objectives.

  13. Supercritical Fluid Extract of Spent Coffee Grounds Attenuates Melanogenesis through Downregulation of the PKA, PI3K/Akt, and MAPK Signaling Pathways

    Directory of Open Access Journals (Sweden)

    Huey-Chun Huang

    2016-01-01

    Full Text Available The mode of action of spent coffee grounds supercritical fluid CO2 extract (SFE in melanogenesis has never been reported. In the study, the spent coffee grounds were extracted by the supercritical fluid CO2 extraction method; the chemical constituents of the SFE were investigated by gas chromatography-mass spectrometry (GC-MS. The effects of the SFE and its major fatty acid components on melanogenesis were evaluated by mushroom tyrosinase activity assay and determination of intracellular tyrosinase activity and melanin content. The expression level of melanogenesis-related proteins was analyzed by western blotting assay. The results revealed that the SFE of spent coffee grounds (1–10 mg/mL and its major fatty acids such as linoleic acid and oleic acid (6.25–50 μM effectively suppressed melanogenesis in the B16F10 murine melanoma cells. Furthermore, the SFE decreased the expression of melanocortin 1 receptor (MC1R, microphthalmia-associated transcription factor (MITF, tyrosinase, tyrosinase-related protein-1 (TRP-1, and tyrosinase-related protein-2 (TRP-2. The SFE also decreased the protein expression levels of p-JNK, p-p38, p-ERK, and p-CREB. Our results revealed that the SFE of spent coffee grounds attenuated melanogenesis in B16F10 cells by downregulation of protein kinase A (PKA, phosphatidylinositol-3-kinase (PI3K/Akt, and mitogen-activated protein kinases (MAPK signaling pathways, which may be due to linoleic acid and oleic acid.

  14. Raman Scattering Study of Supercritical Bi-Component Mixtures Injected into a Subcritical Environment

    National Research Council Canada - National Science Library

    An, Young M

    2007-01-01

    .... Unique thermodynamic and transport properties of supercritical fluids along with phase transition phenomena during fuel injection process can significantly change combustion characteristics inside a scramjet combustor...

  15. 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.

  16. 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.

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

    Directory of Open Access Journals (Sweden)

    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.

  18. Phytosterols and their extraction from various plant matrices using supercritical carbon dioxide: a review.

    Science.gov (United States)

    Uddin, Md Salim; Sarker, Md Zaidul Islam; Ferdosh, Sahena; Akanda, Md Jahurul Haque; Easmin, Mst Sabina; Bt Shamsudin, Siti Hadijah; Bin Yunus, Kamaruzzaman

    2015-05-01

    Phytosterols provide important health benefits: in particular, the lowering of cholesterol. From environmental and commercial points of view, the most appropriate technique has been searched for extracting phytosterols from plant matrices. As a green technology, supercritical fluid extraction (SFE) using carbon dioxide (CO2) is widely used to extract bioactive compounds from different plant matrices. Several studies have been performed to extract phytosterols using supercritical CO2 (SC-CO2) and this technology has clearly offered potential advantages over conventional extraction methods. However, the efficiency of SFE technology fully relies on the processing parameters, chemistry of interest compounds, nature of the plant matrices and expertise of handling. This review covers SFE technology with particular reference to phytosterol extraction using SC-CO2. Moreover, the chemistry of phytosterols, properties of supercritical fluids (SFs) and the applied experimental designs have been discussed for better understanding of phytosterol solubility in SC-CO2. © 2014 Society of Chemical Industry.

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. Heat Transfer Behaviour and Thermohydraulics Code Testing for Supercritical Water Cooled Reactors (SCWRs)

    International Nuclear Information System (INIS)

    2014-08-01

    The supercritical water cooled reactor (SCWR) is an innovative water cooled reactor concept which uses water pressurized above its thermodynamic critical pressure as the reactor coolant. This concept offers high thermal efficiencies and a simplified reactor system, and is hence expected to help to improve economic competitiveness. Various kinds of SCWR concepts have been developed, with varying combinations of reactor type (pressure vessel or pressure tube) and core spectrum (thermal, fast or mixed). There is great interest in both developing and developed countries in the research and development (R&D) and conceptual design of SCWRs. Considering the high interest shown in a number of Member States, the IAEA established in 2008 the Coordinated Research Project (CRP) on Heat Transfer Behaviour and Thermo-hydraulics Code Testing for SCWRs. The aim was to foster international collaboration in the R&D of SCWRs in support of Member States’ efforts and under the auspices of the IAEA Nuclear Energy Department’s Technical Working Groups on Advanced Technologies for Light Water Reactors (TWG-LWR) and Heavy Water Reactors (TWG-HWR). The two key objectives of the CRP were to establish accurate databases on the thermohydraulics of supercritical pressure fluids and to test analysis methods for SCWR thermohydraulic behaviour to identify code development needs. In total, 16 institutes from nine Member States and two international organizations were involved in the CRP. The thermohydraulics phenomena investigated in the CRP included heat transfer and pressure loss characteristics of supercritical pressure fluids, development of new heat transfer prediction methods, critical flow during depressurization from supercritical conditions, flow stability and natural circulation in supercritical pressure systems. Two code testing benchmark exercises were performed for steady state heat transfer and flow stability in a heated channel. The CRP was completed with the planned outputs in

  4. Heat Transfer Behaviour and Thermohydraulics Code Testing for Supercritical Water Cooled Reactors (SCWRs)

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2014-08-15

    The supercritical water cooled reactor (SCWR) is an innovative water cooled reactor concept which uses water pressurized above its thermodynamic critical pressure as the reactor coolant. This concept offers high thermal efficiencies and a simplified reactor system, and is hence expected to help to improve economic competitiveness. Various kinds of SCWR concepts have been developed, with varying combinations of reactor type (pressure vessel or pressure tube) and core spectrum (thermal, fast or mixed). There is great interest in both developing and developed countries in the research and development (R&D) and conceptual design of SCWRs. Considering the high interest shown in a number of Member States, the IAEA established in 2008 the Coordinated Research Project (CRP) on Heat Transfer Behaviour and Thermo-hydraulics Code Testing for SCWRs. The aim was to foster international collaboration in the R&D of SCWRs in support of Member States’ efforts and under the auspices of the IAEA Nuclear Energy Department’s Technical Working Groups on Advanced Technologies for Light Water Reactors (TWG-LWR) and Heavy Water Reactors (TWG-HWR). The two key objectives of the CRP were to establish accurate databases on the thermohydraulics of supercritical pressure fluids and to test analysis methods for SCWR thermohydraulic behaviour to identify code development needs. In total, 16 institutes from nine Member States and two international organizations were involved in the CRP. The thermohydraulics phenomena investigated in the CRP included heat transfer and pressure loss characteristics of supercritical pressure fluids, development of new heat transfer prediction methods, critical flow during depressurization from supercritical conditions, flow stability and natural circulation in supercritical pressure systems. Two code testing benchmark exercises were performed for steady state heat transfer and flow stability in a heated channel. The CRP was completed with the planned outputs in

  5. Experimental analysis on a novel solar collector system achieved by supercritical CO2 natural convection

    International Nuclear Information System (INIS)

    Chen, Lin; Zhang, Xin-Rong

    2014-01-01

    Highlights: • Supercritical CO 2 flow is proposed for natural circulation solar water heater system. • Experimental system established and consists of supercritical fluid high pressure side and water side. • Stable supercritical CO 2 natural convective flow is well induced and water heating process achieved. • Seasonal solar collector system efficiency above 60% achieved and optimization discussed. - Abstract: Solar collector has become a hot topic both in scientific research and engineering applications. Among the various applications, the hot water supply demand accounts for a large part of social energy consumption and has become one promising field. The present study deals with a novel solar thermal conversion and water heater system achieved by supercritical CO 2 natural circulation. Experimental systems are established and tested in Zhejiang Province (around N 30.0°, E 120.6°) of southeast China. The current system is designed to operate in the supercritical region, thus the system can be compactly made and achieve smooth high rate natural convective flow. During the tests, supercritical CO 2 pipe flow with Reynolds number higher than 6700 is found. The CO 2 fluid temperature in the heat exchanger can be as high as 80 °C and a stable supply of hot water above 45 °C is achieved. In the seasonal tests, relative high collector efficiency generally above 60.0% is obtained. Thermal and performance analysis is carried out with the experiment data. Comparisons between the present system and previous solar water heaters are also made in this paper

  6. Hydrogenation of diesel aromatic compounds in supercritical solvent environment

    Directory of Open Access Journals (Sweden)

    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.

  7. Supercritical CO2 Extraction of Salvia officinalis L

    Czech Academy of Sciences Publication Activity Database

    Aleksovski, S.A.; Sovová, Helena

    2007-01-01

    Roč. 40, č. 2 (2007), s. 239-245 ISSN 0896-8446 R&D Projects: GA AV ČR(CZ) IAA4072102 Grant - others:GA_(MK) 40108601/0 Institutional research plan: CEZ:AV0Z40720504 Keywords : supercritical fluid extraction * essential oil * collection efficiency Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 2.189, year: 2007

  8. 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.

  9. Extraction of Thyme Oil: Comparison between Hydrodistillation and Supercritical CO2 Extraction

    Czech Academy of Sciences Publication Activity Database

    Aleksovski, S. A.; Sovová, Helena; Poposka, F. A.

    2001-01-01

    Roč. 51, č. 4 (2001), s. 305-310 ISSN 1330-0075 Institutional research plan: CEZ:AV0Z4072921 Keywords : thymus serpyllum * supercritical fluid extraction * assential oil Subject RIV: CI - Industrial Chemistry, Chemical Engineering

  10. 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.

  11. Evaluation of Supercritical Extracts of Algae as Biostimulants of Plant Growth in Field Trials

    OpenAIRE

    Michalak, Izabela; Chojnacka, Katarzyna; Dmytryk, Agnieszka; Wilk, Rados?aw; Gramza, Mateusz; R?j, Edward

    2016-01-01

    The aim of the field trials was to determine the influence of supercritical algal extracts on the growth and development of winter wheat (variety Akteur). As a raw material for the supercritical fluid extraction (SFE), the biomass of microalga Spirulina plantensis, brown seaweed – Ascophyllum nodosum and Baltic green macroalgae was used. Forthial and Asahi SL constituted the reference products. It was found that the tested biostimulants did not influence statistically significantly the plant...

  12. Supercritical synthesis and in situ deposition of PbS nanocrystals with oleic acid passivation for quantum dot solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Tavakoli, M.M. [Department of Materials Science and Engineering, Sharif University of Technology, 14588 Tehran (Iran, Islamic Republic of); Simchi, A., E-mail: simchi@sharif.edu [Department of Materials Science and Engineering, Sharif University of Technology, 14588 Tehran (Iran, Islamic Republic of); Institute for Nanoscience and Nanotechnology, Sharif University of Technology, 14588 Tehran (Iran, Islamic Republic of); Aashuri, H. [Department of Materials Science and Engineering, Sharif University of Technology, 14588 Tehran (Iran, Islamic Republic of)

    2015-04-15

    Colloidal quantum dot solar cells have recently attracted significant attention due to their low-processing cost and surging photovoltaic performance. In this paper, a novel, reproducible, and simple solution-based process based on supercritical fluid toluene is presented for in situ growth and deposition PbS nanocrystals with oleic-acid passivation. A lead precursor containing sulfur was mixed with oleic acid in toluene and processed in a supercritical fluid condition at different temperatures of 140, 270 and 330 °C for 20 min. The quantum dots were deposited on a fluorine-doped tin oxide glass substrate inside the supercritical reactor. Transmission electron microscopy, X-ray diffraction, absorption and dynamic light scattering showed that the nanocrystals processed at the supercritical condition (330 °C) are fully crystalline with a narrow size distribution of ∼3 nm with an absorption wavelength of 915 nm (bandgap of 1.3 eV). Fourier transform infrared spectroscopy indicated that the PbS quantum dots are passivated by oleic acid molecules during the growth. Photovoltaic characteristics of Schottky junction solar cells showed an improvement over devices prepared by spin-coating. - Highlights: • Supercritical fluid processing and in situ deposition of PbS QDs are presented. • The prepared nanocrystals are mono-dispersed with an optical bandgap of 1.3 eV. • Photovoltaic performance of the in situ deposited nanocrystals is reported. • An improved PV performance compared to spin coated Schottky solar cells is shown.

  13. The influence of different diffusion pattern to the sub- and super-critical fluid flow in brown coal

    Science.gov (United States)

    Peng, Peihuo

    2018-03-01

    Sub- and super-critical CO2 flowing in nanoscale pores are recently becoming of great interest due to that it is closely related to many engineering applications, such as geological burial and sequestration of carbon dioxide, Enhanced Coal Bed Methane recovery ( ECBM), super-critical CO2 fracturing and so on. Gas flow in nanopores cannot be described simply by the Darcy equation. Different diffusion pattern such as Fick diffusion, Knudsen diffusion, transitional diffusion and slip flow at the solid matrix separate the seepage behaviour from Darcy-type flow. According to the principle of different diffusion pattern, the flow of sub- and super-critical CO2 in brown coal was simulated by numerical method, and the results were compared with the experimental results to explore the contribution of different diffusion pattern and swelling effect in sub- and super-critical CO2 flow in nanoscale pores.

  14. Steady state and linear stability analysis of a supercritical water natural circulation loop

    International Nuclear Information System (INIS)

    Sharma, Manish; Pilkhwal, D.S.; Vijayan, P.K.; Saha, D.; Sinha, R.K.

    2010-01-01

    Supercritical water (SCW) has excellent heat transfer characteristics as a coolant for nuclear reactors. Besides it results in high thermal efficiency of the plant. However, the flow can experience instabilities in supercritical water reactors, as the density change is very large for the supercritical fluids. A computer code SUCLIN using supercritical water properties has been developed to carry out the steady state and linear stability analysis of a SCW natural circulation loop. The conservation equations of mass, momentum and energy have been linearized by imposing small perturbation in flow rate, enthalpy, pressure and specific volume. The equations have been solved analytically to generate the characteristic equation. The roots of the equation determine the stability of the system. The code has been qualitatively assessed with published results and has been extensively used for studying the effect of diameter, height, heater inlet temperature, pressure and local loss coefficients on steady state and stability behavior of a Supercritical Water Natural Circulation Loop (SCWNCL). The present paper describes the linear stability analysis model and the results obtained in detail.

  15. Features of supercritical carbon dioxide Brayton cycle coupled with reactor

    International Nuclear Information System (INIS)

    Duan Chengjie; Wang Jie; Yang Xiaoyong

    2010-01-01

    In order to obtain acceptable cycle efficiency, current helium gas turbine power cycle technology needs high cycle temperature which means that the cycle needs high core-out temperature. The technology has high requirements on reactor structure and fuel elements materials, and also on turbine manufacture. While utilizing CO 2 as cycle working fluid, it can guarantee to lower the cycle temperature and turbo machine Janume but achieve the same cycle efficiency, so as to enhance the safety and economy of reactor. According to the laws of thermodynamics, a calculation model of supercritical CO 2 power cycle was established to analyze the feature, and the decisive parameters of the cycle and also investigate the effect of each parameter on the cycle efficiency in detail were obtained. The results show that supercritical CO 2 power cycle can achieve quite satisfied efficiency at a lower cycle highest temperature than helium cycle, and CO 2 is a promising working fluid. (authors)

  16. Pesticide residues in canned foods, fruits, and vegetables: the application of Supercritical Fluid Extraction and chromatographic techniques in the analysis.

    Science.gov (United States)

    El-Saeid, Mohamed H

    2003-12-11

    Multiple pesticide residues have been observed in some samples of canned foods, frozen vegetables, and fruit jam, which put the health of the consumers at risk of adverse effects. It is quite apparent that such a state of affairs calls for the need of more accurate, cost-effective, and rapid analytical techniques capable of detecting the minimum concentrations of the multiple pesticide residues. The aims of this paper were first, to determine the effectiveness of the use of Supercritical Fluid Extraction (SFE) and Supercritical Fluid Chromatography (SFC) techniques in the analysis of the levels of pesticide residues in canned foods, vegetables, and fruits; and second, to contribute to the promotion of consumer safety by excluding pesticide residue contamination from markets. Fifteen different types of imported canned and frozen fruits and vegetables samples obtained from the Houston local food markets were investigated. The major types of pesticides tested were pyrethroids, herbicides, fungicides, and carbamates. By using these techniques, the overall data showed 60.82% of the food samples had no detection of any pesticide residues under this investigation. On the other hand, 39.15% different food samples were contaminated by four different pyrethroid residues +/- RSD% ranging from 0.03 +/- 0.005 to 0.05 +/- 0.03 ppm, of which most of the pyrethroid residues were detected in frozen vegetables and strawberry jam. Herbicide residues in test samples ranged from 0.03 +/- 0.005 to 0.8 +/- 0.01 ppm. Five different fungicides, ranging from 0.05 +/- 0.02 to 0.8 +/- 0.1 ppm, were found in five different frozen vegetable samples. Carbamate residues were not detected in 60% of investigated food samples. It was concluded that SFE and SFC techniques were accurate, reliable, less time consuming, and cost effective in the analysis of imported canned foods, fruits, and vegetables and are recommended for the monitoring of pesticide contaminations.

  17. Determination and theoretical analysis of supercritical fluid chromatographic retention of polycyclic aromatic hydrocarbons in a polymeric smectic phase

    International Nuclear Information System (INIS)

    Chao Yan; Martire, D.E.

    1992-01-01

    A mean-field lattice model is used to describe the partitioning of blocklike molecules between an isotropic mobile phase and an anisotropic stationary phase in chromatography by applying it to supercritical fluid retention of polycyclic aromatic hydrocarbons in a polymeric smectic phase. This concludes that the logarithm of the capacity factor (1) increases linearly with increasing reciprocal temperature, (2) decreases with increasing mobile phase density more rapidly for solute molecules with a relatively larger contact area with the mobile phase, and (3) is a linear function of the minimum area. The van't Hoff plot slope is also determined to be more negative for solute molecules with a relatively larger ratio of contact area with the stationary phase versus the mobile phase. 18 refs., 9 figs., 5 tabs

  18. Enhanced metal recovery through oxidation in liquid and/or supercritical carbon dioxide

    KAUST Repository

    Blanco, Mario; Buttner, Ulrich

    2017-01-01

    Process for enhanced metal recovery from, for example, metal-containing feedstock using liquid and/or supercritical fluid carbon dioxide and a source of oxidation. The oxidation agent can be free of complexing agent. The metal-containing feedstock

  19. Supercritical fluid extraction (SFE) of ketamine metabolites from dried urine and on-line quantification by supercritical fluid chromatography and single mass detection (on-line SFE-SFC-MS).

    Science.gov (United States)

    Hofstetter, Robert; Fassauer, Georg M; Link, Andreas

    2018-02-15

    On-line solid-phase supercritical fluid extraction (SFE) and chromatography (SFC) coupled to mass spectrometry (MS) has been evaluated for its usefulness with respect to metabolic profiling and pharmacological investigations of ketamine in humans. The aim of this study was to develop and validate a rapid, highly selective and sensitive SFE-SFC-MS method for the quantification of ketamine and its metabolites in miniature amounts in human urine excluding liquid-liquid extraction (LLE). Several conditions were optimized systematically following the requirements of the European Medicines Agency: selectivity, carry-over, calibration curve parameters (LLOQ, range and linearity), within- and between-run accuracy and precision, dilution integrity, matrix effect, and stability. The method, which required a relatively small volume of human urine (20 μL per sample), was validated for pharmacologically and toxicologically relevant concentrations ranging from 25.0 to 1000 ng/mL (r 2  > 0.995). The lower limit of quantification (LLOQ) for all compounds was found to be as low as 0.5 ng. In addition, stability of analytes during removal of water from the urine samples using different conditions (filter paper or ISOLUTE® HM-N) was studied. In conclusion, the method developed in this study can be successfully applied to studies of ketamine metabolites in humans, and may pave the way for routine application of on-line SFE-SFC-MS in clinical investigations. Copyright © 2018 Elsevier B.V. All rights reserved.

  20. Extraction of uranium from simulated ore by the supercritical carbon dioxide fluid extraction method with nitric acid-TBP complex

    International Nuclear Information System (INIS)

    Dung, Le Thi Kim; Imai, Tomoki; Tomioka, Osamu; Nakashima, Mikio; Takahashi, Kuniaki; Meguro, Yoshihiro

    2006-01-01

    The supercritical fluid extraction (SFE) method using CO 2 as a medium with an extractant of HNO 3 -tri-n-butyl phosphate (TBP) complex was applied to extract uranium from several uranyl phosphate compounds and simulated uranium ores. An extraction method consisting of a static extraction process and a dynamic one was established, and the effects of the experimental conditions, such as pressure, temperature, and extraction time, on the extraction of uranium were ascertained. It was found that uranium could be efficiently extracted from both the uranyl phosphates and simulated ores by the SFE method using CO 2 . It was thus demonstrated that the SFE method using CO 2 is useful as a pretreatment method for the analysis of uranium in ores. (author)

  1. Final Report: Development of a Chemical Model to Predict the Interactions between Supercritical CO2, Fluid and Rock in EGS Reservoirs

    Energy Technology Data Exchange (ETDEWEB)

    McPherson, Brian J. [University of Utah; Pan, Feng [University of Utah

    2014-09-24

    This report summarizes development of a coupled-process reservoir model for simulating enhanced geothermal systems (EGS) that utilize supercritical carbon dioxide as a working fluid. Specifically, the project team developed an advanced chemical kinetic model for evaluating important processes in EGS reservoirs, such as mineral precipitation and dissolution at elevated temperature and pressure, and for evaluating potential impacts on EGS surface facilities by related chemical processes. We assembled a new database for better-calibrated simulation of water/brine/ rock/CO2 interactions in EGS reservoirs. This database utilizes existing kinetic and other chemical data, and we updated those data to reflect corrections for elevated temperature and pressure conditions of EGS reservoirs.

  2. Fundamental study of CO2-H2O-mineral interactions for carbon sequestration, with emphasis on the nature of the supercritical fluid-mineral interface.

    Energy Technology Data Exchange (ETDEWEB)

    Bryan, Charles R.; Dewers, Thomas A.; Heath, Jason E.; Wang, Yifeng; Matteo, Edward N.; Meserole, Stephen P.; Tallant, David Robert

    2013-09-01

    In the supercritical CO2-water-mineral systems relevant to subsurface CO2 sequestration, interfacial processes at the supercritical fluid-mineral interface will strongly affect core- and reservoir-scale hydrologic properties. Experimental and theoretical studies have shown that water films will form on mineral surfaces in supercritical CO2, but will be thinner than those that form in vadose zone environments at any given matric potential. The theoretical model presented here allows assessment of water saturation as a function of matric potential, a critical step for evaluating relative permeabilities the CO2 sequestration environment. The experimental water adsorption studies, using Quartz Crystal Microbalance and Fourier Transform Infrared Spectroscopy methods, confirm the major conclusions of the adsorption/condensation model. Additional data provided by the FTIR study is that CO2 intercalation into clays, if it occurs, does not involve carbonate or bicarbonate formation, or significant restriction of CO2 mobility. We have shown that the water film that forms in supercritical CO2 is reactive with common rock-forming minerals, including albite, orthoclase, labradorite, and muscovite. The experimental data indicate that reactivity is a function of water film thickness; at an activity of water of 0.9, the greatest extent of reaction in scCO2 occurred in areas (step edges, surface pits) where capillary condensation thickened the water films. This suggests that dissolution/precipitation reactions may occur preferentially in small pores and pore throats, where it may have a disproportionately large effect on rock hydrologic properties. Finally, a theoretical model is presented here that describes the formation and movement of CO2 ganglia in porous media, allowing assessment of the effect of pore size and structural heterogeneity on capillary trapping efficiency. The model results also suggest possible engineering approaches for optimizing trapping capacity and for

  3. Influence of various aspects of low Reynolds number k-ε turbulence models on predicting in-tube buoyancy affected heat transfer to supercritical pressure fluids

    International Nuclear Information System (INIS)

    Zhao, Chen-Ru; Zhang, Zhen; Jiang, Pei-Xue; Bo, Han-Liang

    2017-01-01

    Highlights: • Understanding of the mechanism of buoyancy effect on supercritical heat transfer. • Turbulence related parameters in upward and downward flows were compared. • Turbulent Prandtl number affected the prediction insignificantly. • Buoyancy production was insignificant compared with shear production. • Damping function had the greatest effect and is a priority for further modification. - Abstract: Heat transfer to supercritical pressure fluids was modeled for normal and buoyancy affected conditions using several low Reynolds number k-ε models, including the Launder and Sharma, Myong and Kasagi, and Abe, Kondoh and Nagano, with the predictions compared with experimental data. All three turbulence models accurately predicted the cases without heat transfer deterioration, but failed to accurately predict the cases with heat transfer deterioration although the general trends were captured, indicating that further improvements and modifications are needed for the low Reynolds number k-ε turbulence models to better predict buoyancy deteriorated heat transfer. Further investigations studied the influence of various aspects of the low Reynolds number k-ε turbulence models, including the turbulent Prandtl number, the buoyancy production of turbulent kinetic energy, and the damping function to provide guidelines for model development to more precisely predict buoyancy affected heat transfer. The results show that the turbulent Prandtl number and the buoyancy production of turbulent kinetic energy have little influence on the predictions for cases in this study, while new damping functions with carefully selected control parameters are needed in the low Reynolds number k-ε turbulence models to correctly predict the buoyancy effect for heat transfer simulations in various applications such as supercritical pressure steam generators (SPSGs) in the high temperature gas cooled reactor (HTR) and the supercritical pressure water reactor (SCWR).

  4. Influence of various aspects of low Reynolds number k-ε turbulence models on predicting in-tube buoyancy affected heat transfer to supercritical pressure fluids

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Chen-Ru; Zhang, Zhen [Institute of Nuclear and New Energy Technology of Tsinghua University, Advanced Nuclear Energy Technology Cooperation Innovation Centre, Key Laboratory of Advanced Nuclear Engineering and Safety, Ministry of Education, Beijing 100084 (China); Jiang, Pei-Xue, E-mail: jiangpx@tsinghua.edu.cn [Beijing Key Laboratory of CO_2 Utilization and Reduction Technology/Key Laboratory for Thermal Science and Power Engineering of Ministry of Education, Department of Thermal Engineering, Tsinghua University, Beijing 100084 (China); Bo, Han-Liang [Institute of Nuclear and New Energy Technology of Tsinghua University, Advanced Nuclear Energy Technology Cooperation Innovation Centre, Key Laboratory of Advanced Nuclear Engineering and Safety, Ministry of Education, Beijing 100084 (China)

    2017-03-15

    Highlights: • Understanding of the mechanism of buoyancy effect on supercritical heat transfer. • Turbulence related parameters in upward and downward flows were compared. • Turbulent Prandtl number affected the prediction insignificantly. • Buoyancy production was insignificant compared with shear production. • Damping function had the greatest effect and is a priority for further modification. - Abstract: Heat transfer to supercritical pressure fluids was modeled for normal and buoyancy affected conditions using several low Reynolds number k-ε models, including the Launder and Sharma, Myong and Kasagi, and Abe, Kondoh and Nagano, with the predictions compared with experimental data. All three turbulence models accurately predicted the cases without heat transfer deterioration, but failed to accurately predict the cases with heat transfer deterioration although the general trends were captured, indicating that further improvements and modifications are needed for the low Reynolds number k-ε turbulence models to better predict buoyancy deteriorated heat transfer. Further investigations studied the influence of various aspects of the low Reynolds number k-ε turbulence models, including the turbulent Prandtl number, the buoyancy production of turbulent kinetic energy, and the damping function to provide guidelines for model development to more precisely predict buoyancy affected heat transfer. The results show that the turbulent Prandtl number and the buoyancy production of turbulent kinetic energy have little influence on the predictions for cases in this study, while new damping functions with carefully selected control parameters are needed in the low Reynolds number k-ε turbulence models to correctly predict the buoyancy effect for heat transfer simulations in various applications such as supercritical pressure steam generators (SPSGs) in the high temperature gas cooled reactor (HTR) and the supercritical pressure water reactor (SCWR).

  5. 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.

  6. 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.

  7. Enantioselective potential of polysaccharide-based chiral stationary phases in supercritical fluid chromatography.

    Science.gov (United States)

    Kucerova, Gabriela; Kalikova, Kveta; Tesarova, Eva

    2017-06-01

    The enantioselective potential of two polysaccharide-based chiral stationary phases for analysis of chiral structurally diverse biologically active compounds was evaluated in supercritical fluid chromatography using a set of 52 analytes. The chiral selectors immobilized on 2.5 μm silica particles were tris-(3,5-dimethylphenylcarmabate) derivatives of cellulose or amylose. The influence of the polysaccharide backbone, different organic modifiers, and different mobile phase additives on retention and enantioseparation was monitored. Conditions for fast baseline enantioseparation were found for the majority of the compounds. The success rate of baseline and partial enantioseparation with cellulose-based chiral stationary phase was 51.9% and 15.4%, respectively. Using amylose-based chiral stationary phase we obtained 76.9% of baseline enantioseparations and 9.6% of partial enantioseparations of the tested compounds. The best results on cellulose-based chiral stationary phase were achieved particularly with propane-2-ol and a mixture of isopropylamine and trifluoroacetic acid as organic modifier and additive to CO 2 , respectively. Methanol and basic additive isopropylamine were preferred on amylose-based chiral stationary phase. The complementary enantioselectivity of the cellulose- and amylose-based chiral stationary phases allows separation of the majority of the tested structurally different compounds. Separation systems were found to be directly applicable for analyses of biologically active compounds of interest. © 2017 Wiley Periodicals, Inc.

  8. Quantitative determination of major alkaloids in Cinchona bark by Supercritical Fluid Chromatography.

    Science.gov (United States)

    Murauer, Adele; Ganzera, Markus

    2018-06-15

    Chinoline alkaloids found in Cinchona bark still play an important role in medicine, for example as antimalarial and antiarrhythmic drugs. For the first time Supercritical Fluid Chromatography has been utilized for their separation. Six respective derivatives (dihydroquinidine, dihydroquinine, quinidine, quinine, cinchonine and cinchonidine) could be resolved in less than 7 min, and three of them quantified in crude plant extracts. The optimum stationary phase showed to be an Acquity UPC 2 Torus DEA 1.7 μm column, the mobile phase comprised of CO 2 , acetonitrile, methanol and diethylamine. Method validation confirmed that the procedure is selective, accurate (recovery rates from 97.2% to 103.7%), precise (intra-day ≤2.2%, inter-day ≤3.0%) and linear (R 2  ≥ 0.999); at 275 nm the observed detection limits were always below 2.5 μg/ml. In all of the samples analyzed cinchonine dominated (1.87%-2.30%), followed by quinine and cinchonidine. Their total content ranged from 4.75% to 5.20%. These values are in good agreement with published data, so that due to unmatched speed and environmental friendly character SFC is definitely an excellent alternative for the analysis of these important natural products. Copyright © 2018 The Author(s). Published by Elsevier B.V. All rights reserved.

  9. Safety study of an experimental apparatus for extraction with supercritical CO2

    Directory of Open Access Journals (Sweden)

    V. B. Soares

    2012-09-01

    Full Text Available During the process of supercritical CO2 extraction it is necessary to use high pressures in the procedure. The explosion of a pressure vessel can be harmful to people and cause serious damage to the environment. The aim of this study is to investigate the probability of death and injury in a laboratory unit for supercritical fluid extraction in the case of an explosion of the extractor vessel. The procedure is explained via a case study involving fatty acid extraction from vegetable oils with carbon dioxide above its supercritical conditions and under optimum operating conditions. According to the results, more importance should be given to the use of a protective headset because the probability of eardrum injury is superior to the probability of death from lung injury.

  10. Partitioning behaviour of organic compounds between ionic liquids and supercritical fluids

    Czech Academy of Sciences Publication Activity Database

    Roth, Michal

    2009-01-01

    Roč. 1216, č. 10 (2009), s. 1861-1880 ISSN 0021-9673 R&D Projects: GA ČR GA203/08/1465; GA ČR GA203/08/1536 Institutional research plan: CEZ:AV0Z40310501 Keywords : ionic liquid * supercritical carbon dioxide * review Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.101, year: 2009

  11. Supercritical CO2-assisted preparation of ibuprofen loaded PEG-PVP complexes

    CSIR Research Space (South Africa)

    Labuschagne, Philip W

    2010-06-01

    Full Text Available Stoichiometric ratios of poly (ethylene glycol) (PEG, Mw = 400) with poly(vinylpyrrolidone) (PVP, Mw = ±3.1 x 104 & Mw = 1.25 x 106 Mw) were prepared from ethanol cast solutions and in supercritical CO2. The complex formation was studied via glass...

  12. Extraction of Botanical Pesticides from Pelargonium graveolens using Supercritical Carbon Dioxide

    Czech Academy of Sciences Publication Activity Database

    Machalová, Zdeňka; Sajfrtová, Marie; Pavela, R.; Topiař, Martin

    2015-01-01

    Roč. 67, MAY (2015), s. 310-317 ISSN 0926-6690 R&D Projects: GA TA ČR TA01010578 Institutional support: RVO:67985858 Keywords : botanical pesticides * geranium oil * supercritical fluid extraction Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 3.449, year: 2015

  13. Early pleural fluid dynamics following video-assisted thoracoscopic lobectomy has limited clinical value

    DEFF Research Database (Denmark)

    Holbek, Bo Laksáfoss; Petersen, René Horsleben; Kehlet, Henrik

    2017-01-01

    The objective of this study was to evaluate the potential of predicting the pleural fluid output in patients after video-assisted thoracoscopic lobectomy of the lung. Detailed measurements of continuous fluid output were obtained prospectively using an electronic thoracic drainage device (Thopaz...... and 48 hours. Assessment of initial fluid production may predict high 24-hour fluid output (≥500 mL) but seems to lack clinical value in drain removal criteria....

  14. 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.

  15. 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,

  16. 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.

  17. Size-selective separation of polydisperse gold nanoparticles in supercritical ethane.

    Science.gov (United States)

    Williams, Dylan P; Satherley, John

    2009-04-09

    The aim of this study was to use supercritical ethane to selectively disperse alkanethiol-stabilized gold nanoparticles of one size from a polydisperse sample in order to recover a monodisperse fraction of the nanoparticles. A disperse sample of metal nanoparticles with diameters in the range of 1-5 nm was prepared using established techniques then further purified by Soxhlet extraction. The purified sample was subjected to supercritical ethane at a temperature of 318 K in the pressure range 50-276 bar. Particles were characterized by UV-vis absorption spectroscopy, TEM, and MALDI-TOF mass spectroscopy. The results show that with increasing pressure the dispersibility of the nanoparticles increases, this effect is most pronounced for smaller nanoparticles. At the highest pressure investigated a sample of the particles was effectively stripped of all the smaller particles leaving a monodisperse sample. The relationship between dispersibility and supercritical fluid density for two different size samples of alkanethiol-stabilized gold nanoparticles was considered using the Chrastil chemical equilibrium model.

  18. Viability and adaptation potential of indigenous microorganisms from natural gas field fluids in high pressure incubations with supercritical CO2.

    Science.gov (United States)

    Frerichs, Janin; Rakoczy, Jana; Ostertag-Henning, Christian; Krüger, Martin

    2014-01-21

    Carbon Capture and Storage (CCS) is currently under debate as large-scale solution to globally reduce emissions of the greenhouse gas CO2. Depleted gas or oil reservoirs and saline aquifers are considered as suitable reservoirs providing sufficient storage capacity. We investigated the influence of high CO2 concentrations on the indigenous bacterial population in the saline formation fluids of a natural gas field. Bacterial community changes were closely examined at elevated CO2 concentrations under near in situ pressures and temperatures. Conditions in the high pressure reactor systems simulated reservoir fluids i) close to the CO2 injection point, i.e. saturated with CO2, and ii) at the outer boundaries of the CO2 dissolution gradient. During the incubations with CO2, total cell numbers remained relatively stable, but no microbial sulfate reduction activity was detected. After CO2 release and subsequent transfer of the fluids, an actively sulfate-respiring community was re-established. The predominance of spore-forming Clostridiales provided evidence for the resilience of this taxon against the bactericidal effects of supercritical (sc)CO2. To ensure the long-term safety and injectivity, the viability of fermentative and sulfate-reducing bacteria has to be considered in the selection, design, and operation of CCS sites.

  19. Development of an analytical method for polycyclic aromatic hydrocarbons in coffee beverages and dark beer using novel high-sensitivity technique of supercritical fluid chromatography/mass spectrometry.

    Science.gov (United States)

    Yoshioka, Toshiaki; Nagatomi, Yasushi; Harayama, Koichi; Bamba, Takeshi

    2018-07-01

    Polycyclic aromatic hydrocarbons (PAHs) are carcinogenic substances that are mainly generated during heating in food; therefore, the European Union (EU) has regulated the amount of benzo[a]pyrene and PAH4 in various types of food. In addition, the Scientific Committee on Food of the EU and the Joint Food and Agriculture Organization/World Health Organization Expert Committee on Food Additives have recommended that 16 PAHs should be monitored. Since coffee beverages and dark beer are roasted during manufacture, monitoring these 16 PAHs is of great importance. On the other hand, supercritical fluid chromatography (SFC) is a separation method that has garnered attention in recent years as a complement for liquid and gas chromatography. Therefore, we developed a rapid high-sensitivity analytical method for the above-mentioned 16 PAHs in coffee beverages and dark beer involving supercritical fluid chromatography/atmospheric pressure chemical ionization-mass spectrometry (SFC/APCI-MS) and simple sample preparation. In this study, we developed a novel analytical technique that increased the sensitivity of MS detection by varying the back-pressure in SFC depending on the elution of PAHs. In addition, analysis of commercially available coffee and dark beer samples in Japan showed that the risk of containing the 16 PAHs may be low. Copyright © 2018 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

  20. Rapid and Green Separation of Mono- and Diesters of Monochloropropanediols by Ultrahigh Performance Supercritical Fluid Chromatography-Mass Spectrometry Using Neat Carbon Dioxide as a Mobile Phase.

    Science.gov (United States)

    Jumaah, Firas; Jędrkiewicz, Renata; Gromadzka, Justyna; Namieśnik, Jacek; Essén, Sofia; Turner, Charlotta; Sandahl, Margareta

    2017-09-20

    This study demonstrates the effect of column selectivity and density of supercritical carbon dioxide (SC-CO 2 ) on the separation of monochloropropanediol (MCPD) esters, known as food toxicants, using SC-CO 2 without addition of cosolvent in ultrahigh performance supercritical fluid chromatography-mass spectrometry (UHPSFC-MS). This study shows that over 20 2-monochloropropanediol (2-MCPD) and 3-monochloropropanediol (3-MCPD) mono- and diesters are separated on a 2-picolylamine column in less than 12 min. The presence and position of a hydroxyl group in the structure, the number of unsaturated bonds, and the acyl chain length play a significant role in the separation of MCPD esters. The flow rate, backpressure, and column oven temperature, which affect the density of the mobile phase, were shown to have a substantial impact on retention, efficiency, and selectivity. The developed method was successfully applied for the determination of MCPD esters in refined oils and showed a close to excellent green analysis score using the Analytical Eco-Scale.

  1. Supercritical Fluid Extraction of Lignans and Cinnamic Acid from Schizandra chinensis.

    Czech Academy of Sciences Publication Activity Database

    Sovová, Helena; Opletal, L.; Bártlová, Milena; Sajfrtová, Marie; Křenková, M.

    2007-01-01

    Roč. 42, 1 (2007) , s. 88-95 ISSN 0896-8446 R&D Projects: GA ČR(CZ) GA203/01/0550; GA AV ČR IAA4072102; GA AV ČR KSK4040110 Institutional research plan: CEZ:AV0Z40720504 Keywords : supercritical extraction * solubility * lignans Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 2.189, year: 2007

  2. Characteristics of turbulent heat transfer in an annulus at supercritical pressure

    NARCIS (Netherlands)

    Peeters, J.W.R.; Pecnik, R.; Rohde, M.; van der Hagen, T.H.J.J.; Boersma, B.J.

    2017-01-01

    Heat transfer to fluids at supercritical pressure is different from heat transfer at lower pressures due to strong variations of the thermophysical properties with the temperature. We present and analyze results of direct numerical simulations of heat transfer to turbulent CO2 at 8 MPa in an

  3. Investigation of forced convection heat transfer of supercritical pressure water in a vertically upward internally ribbed tube

    International Nuclear Information System (INIS)

    Wang Jianguo; Li Huixiong; Guo Bin; Yu Shuiqing; Zhang Yuqian; Chen Tingkuan

    2009-01-01

    In the present paper, the forced convection heat transfer characteristics of water in a vertically upward internally ribbed tube at supercritical pressures were investigated experimentally. The six-head internally ribbed tube is made of SA-213T12 steel with an outer diameter of 31.8 mm and a wall thickness of 6 mm and the mean inside diameter of the tube is measured to be 17.6 mm. The experimental parameters were as follows. The pressure at the inlet of the test section varied from 25.0 to 29.0 MPa, and the mass flux was from 800 to 1200 kg/(m 2 s), and the inside wall heat flux ranged from 260 to 660 kW/m 2 . According to experimental data, the effects of heat flux and pressure on heat transfer of supercritical pressure water in the vertically upward internally ribbed tube were analyzed, and the characteristics and mechanisms of heat transfer enhancement, and also that of heat transfer deterioration, were also discussed in the so-called large specific heat region. The drastic changes in thermophysical properties near the pseudocritical points, especially the sudden rise in the specific heat of water at supercritical pressures, may result in the occurrence of the heat transfer enhancement, while the covering of the heat transfer surface by fluids lighter and hotter than the bulk fluid makes the heat transfer deteriorated eventually and explains how this lighter fluid layer forms. It was found that the heat transfer characteristics of water at supercritical pressures were greatly different from the single-phase convection heat transfer at subcritical pressures. There are three heat transfer modes of water at supercritical pressures: (1) normal heat transfer, (2) deteriorated heat transfer with low HTC but high wall temperatures in comparison to the normal heat transfer, and (3) enhanced heat transfer with high HTC and low wall temperatures in comparison to the normal heat transfer. It was also found that the heat transfer deterioration at supercritical pressures was

  4. 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

  5. Experiments and Numerical Simulation of Mixing under Supercritical Conditions (PREPRINT)

    Science.gov (United States)

    2011-02-08

    prescribed phase between them. The signals were then sent to two amplifiers (Krohn-Hite model 7500 and a Trek model PZD2000A), one for each piezo... NASA Ames/Stanford Univ., 1999. [61] C. Segal and SA Polikhov. Subcritical to supercritical mixing. Physics of Fluids, 20:052101, 2008. [62] L. Selle and

  6. Quantitative determination of salbutamol sulfate impurities using achiral supercritical fluid chromatography.

    Science.gov (United States)

    Dispas, Amandine; Desfontaine, Vincent; Andri, Bertyl; Lebrun, Pierre; Kotoni, Dorina; Clarke, Adrian; Guillarme, Davy; Hubert, Philippe

    2017-02-05

    In the last years, supercritical fluid chromatography has largely been acknowledged as a singular and performing technique in the field of separation sciences. Recent studies highlighted the interest of SFC for the quality control of pharmaceuticals, especially in the case of the determination of the active pharmaceutical ingredient (API). Nevertheless, quality control requires also the determination of impurities. The objectives of the present work were to (i) demonstrate the interest of SFC as a reference technique for the determination of impurities in salbutamol sulfate API and (ii) to propose an alternative to a reference HPLC method from the European Pharmacopeia (EP) involving ion-pairing reagent. Firstly, a screening was carried out to select the most adequate and selective stationary phase. Secondly, in the context of robust optimization strategy, the method was developed using design space methodology. The separation of salbutamol sulfate and related impurities was achieved in 7min, which is seven times faster than the LC-UV method proposed by European Pharmacopeia (total run time of 50min). Finally, full validation using accuracy profile approach was successfully achieved for the determination of impurities B, D, F and G in salbutamol sulfate raw material. The validated dosing range covered 50 to 150% of the targeted concentration (corresponding to 0.3% concentration level), LODs close to 0.5μg/mL were estimated. The SFC method proposed in this study could be presented as a suitable fast alternative to EP LC method for the quantitative determination of salbutamol impurities. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. 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.

  8. Supercritical CO2 Extracts and Volatile Oil of Basil (Ocimum basilicum L. Comparison with Conventional Methods

    Directory of Open Access Journals (Sweden)

    José Coelho

    2018-03-01

    Full Text Available Interest in new products from aromatic plants as medical and nutritional compounds is increasing. The aim of this work was to apply different extraction methods, including the use of supercritical carbon dioxide extraction, and to test the antioxidant activity of basil (Ocimum basilicum L. extracts. In vitro efficacy assessments were performed using enzymatic assays. Essential oil obtained by hydrodistillation and volatile oil obtained from supercritical fluid extraction were analyzed by gas chromatography to quantify components. The total phenolic content in the extracts ranged from 35.5 ± 2.9 to 85.3 ± 8.6 mg of gallic acid equivalents and the total flavonoid content ranged from 35.5 ± 2.9 to 93.3 ± 3.9 micromole catechin equivalents per gram of dry weight of extract. All the extracts showed an antioxidant activity with 2,2-diphenyl-1-picrylhydrazyl (DPPH, 2,2-azino-bis(3-ethylbenzthiazoline-6-sulfonic acid (ABTS, and the reducing power test. Extracts obtained from methanol had a higher antioxidant capacity per the DPPH test results (IC50 = 3.05 ± 0.36 mg/mL and the reducing power test assay 306.8 ± 21.8 μmol of trolox equivalents per gram of extract (TE/g compared with ethanolic or supercritical fluid extracts. However, using the ABTS assay, the extract obtained by supercritical fluid extraction had a higher antioxidant capacity with an IC50 of 1.74 ± 0.05 mg/mL. Finally, the examined extracts showed practically no acetylcholinesterase (AChE inhibitory capacity and a slight inhibitory activity against tyrosinase.

  9. 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.

  10. Study of simple super-critical fluids (CO2, C2D6) through neutron scattering, Raman spectroscopy and molecular dynamic simulations

    International Nuclear Information System (INIS)

    Longelin, St.

    2004-04-01

    Super-critical