WorldWideScience

Sample records for thermospray liquid-liquid extraction

  1. Determination of organophosphorus acids by thermo-spray liquid chromatography-mass spectrometry

    NARCIS (Netherlands)

    Wils, E.R.J.; Hulst, A.G.

    1988-01-01

    The determination of thirteen organophosphorus acids, hydrolysis products of nerve agents and pesticides, by a combination of ion-pair liquid chromatography on a reversed-phase C18 column and thermospray mass spectrometry was investigated. Ammonium acetate and three tetraalkylammonium salts with

  2. Determination of ten carbamate pesticides in aquatic and sediment samples by liquid chromatography-ionspray and thermospray mass spectrometry.

    NARCIS (Netherlands)

    Honing, M.; Riu, J.; Barceló, D.; van Baar, B.L.M.; Brinkman, U.A.T.

    1996-01-01

    Ten carbamate pesticides which exhibit large differences in polarity were determined simultaneously in various environmental samples, using both column liquid chromatography (LC)-thermospray (TSP) mass spectrometry (MS) and LC-ionspray (ISP) MS. For sample clean-up, column chromatography with three

  3. INTERLABORATORY STUDY OF A THERMOSPRAY-LIQUID CHROMATOGRAPHIC/MASS SPECTROMETRIC METHOD FOR SELECTED N-METHYL CARBAMATES, N-METHYL CARBAMOYLOXIMES, AND SUBSTITUTED UREA PESTICIDES

    Science.gov (United States)

    A thermospray-liquid chromatographic/mass spectrometric (TS-LC/MS) method was evaluated in an interlaboratory study for determining 3 N-methyl carbamates (bendiocarb, carbaryl, and carbofuran), 3-N-methyl carbamoyloximes (aldicarb, methomyl, and oxamyl), 2 substituted urea pestic...

  4. Determination of trimethoprim in tissues using liquid chromatography-thermospray mass spectrometry.

    Science.gov (United States)

    Cannavan, A; Hewitt, S A; Floyd, S D; Kennedy, D G

    1997-11-01

    A method is described for the determination of the antibacterial drug trimethoprim in tissues. Minced tissue is homogenised with chloroform-acetone (1 + 1 v/v), filtered, and the filtrate evaporated to an oily residue using a rotary evaporator. The residue is redissolved in methanol-water-acetic acid (50 + 48.7 + 1.3 v/v) and any fats present are partitioned into hexane. The aqueous phase is analysed by liquid chromatography-thermospray mass spectrometry in positive mode with the protonated molecular ion at m/z 291 being monitored. Recoveries ranged between 60% in liver and 79% in muscle. The limit of determination was 25 micrograms kg-1 and the limit of detection was approximately 4 micrograms kg-1. The method is suitable for monitoring tissues taken under national surveillance schemes for veterinary drug residues.

  5. LIQUID-LIQUID EXTRACTION COLUMNS

    Science.gov (United States)

    Thornton, J.D.

    1957-12-31

    This patent relates to liquid-liquid extraction columns having a means for pulsing the liquid in the column to give it an oscillatory up and down movement, and consists of a packed column, an inlet pipe for the dispersed liquid phase and an outlet pipe for the continuous liquid phase located in the direct communication with the liquid in the lower part of said column, an inlet pipe for the continuous liquid phase and an outlet pipe for the dispersed liquid phase located in direct communication with the liquid in the upper part of said column, a tube having one end communicating with liquid in the lower part of said column and having its upper end located above the level of said outlet pipe for the dispersed phase, and a piston and cylinder connected to the upper end of said tube for applying a pulsating pneumatic pressure to the surface of the liquid in said tube so that said surface rises and falls in said tube.

  6. Use of micro-emulsions in liquid-liquid extraction

    International Nuclear Information System (INIS)

    Komornicki, Jacques

    1982-01-01

    As liquid-liquid extraction of metallic cations is an important method of separation and concentration of metals present in diluted aqueous solutions, and as the extraction rate is limited by one or several steps of matter transfer at the liquid-liquid interface, the extraction kinetics can be improved by creating a wide surface interface and by allowing an increased reactivity between species. In this research thesis, the author aims at determining to which extent systems of interface with a wide surface obtained by using for example amphiphile molecules to create micro-emulsions, can be used as reaction media for physical-chemical processes of liquid-liquid extraction. He also aims at identifying their applicability limitations and problems which might arise with their application. The author notably focuses of the liquid-liquid extraction of metallic cations exhibiting particularly slow extraction kinetics

  7. Parallel artificial liquid membrane extraction

    DEFF Research Database (Denmark)

    Gjelstad, Astrid; Rasmussen, Knut Einar; Parmer, Marthe Petrine

    2013-01-01

    This paper reports development of a new approach towards analytical liquid-liquid-liquid membrane extraction termed parallel artificial liquid membrane extraction. A donor plate and acceptor plate create a sandwich, in which each sample (human plasma) and acceptor solution is separated by an arti......This paper reports development of a new approach towards analytical liquid-liquid-liquid membrane extraction termed parallel artificial liquid membrane extraction. A donor plate and acceptor plate create a sandwich, in which each sample (human plasma) and acceptor solution is separated...... by an artificial liquid membrane. Parallel artificial liquid membrane extraction is a modification of hollow-fiber liquid-phase microextraction, where the hollow fibers are replaced by flat membranes in a 96-well plate format....

  8. The use of ultrasonic instrumentation in liquid/liquid extraction plant

    International Nuclear Information System (INIS)

    Asher, R.C.; Bradshaw, L.; Tolchard, A.C.

    1984-01-01

    Ultrasonic instruments can be used to determine many of the parameters of interest in a liquid/liquid extraction plant, eg liquid levels, the position of interfaces between immiscible liquids and the concentration of solutions. The determinations can often be made non-invasively. A number of instruments developed for a liquid/liquid extraction plant used for nuclear fuel reprocessing is described. These instruments have a wider application in liquid/liquid extraction plant in general. (author)

  9. Salting-out homogenous extraction followed by ionic liquid/ionic liquid liquid-liquid micro-extraction for determination of sulfonamides in blood by high performance liquid chromatography.

    Science.gov (United States)

    Liu, Zhongling; Yu, Wei; Zhang, Hanqi; Gu, Fanbin; Jin, Xiangqun

    2016-12-01

    Salting-out homogenous extraction followed by ionic liquid/ionic liquid dispersive liquid-liquid micro-extraction system was developed and applied to the extraction of sulfonamides in blood. High-performance liquid chromatography was applied to the determination of the analytes. The blood sample was centrifuged to obtain the serum. After the proteins in the serum were removed in the presence of acetonitrile, ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate, dipotassium hydrogen phosphate, ionic liquid 1-Hexyl-3-methylimidazolium hexafluorophosphate were added into the resulting solution. After the resulting mixture was ultrasonically shaken and centrifuged, the precipitate was separated. The acetonitrile was added in the precipitate and the analytes were extracted into the acetonitrile phase. The parameters affecting the extraction efficiency, such as volume of ionic liquid, amount of dipotassium hydrogen phosphate, volume of dispersant, extraction time and temperature were investigated. The limits of detection of sulfamethizole (STZ), sulfachlorpyridazine (SCP), sulfamethoxazole (SMX) and Sulfisoxazole (SSZ) were 4.78, 3.99, 5.21 and 3.77μgL -1 , respectively. When the present method was applied to the analysis of real blood samples, the recoveries of analytes ranged from 90.0% to 113.0% and relative standard deviations were lower than 7.2%. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Liquid-Liquid Extraction in Systems Containing Butanol and Ionic Liquids – A Review

    OpenAIRE

    Kubiczek Artur; Kamiński Władysław

    2017-01-01

    Room-temperature ionic liquids (RTILs) are a moderately new class of liquid substances that are characterized by a great variety of possible anion-cation combinations giving each of them different properties. For this reason, they have been termed as designer solvents and, as such, they are particularly promising for liquid-liquid extraction, which has been quite intensely studied over the last decade. This paper concentrates on the recent liquid-liquid extraction studies involving ionic liqu...

  11. Liquid-liquid extraction of plutonium(IV) in monoamide - ammonium ionic liquid mixture

    International Nuclear Information System (INIS)

    Rout, Alok; Venkatesan, K.A.; Antony, M.P.

    2016-01-01

    Room temperature ionic liquid (RTIL) can be regarded as a sustainable alternative to the conventional molecular diluent, n-dodecane (n-DD), in solvent extraction process. Replacement of volatile organic solvents by RTILs in solvent extraction could lead to inherently safer processes. As far as the cation is concerned, most of the studies reported in literature are focused on imidazolium-based ionic liquids. In contrast to imiadazolium ionic liquids, quarternary ammonium ionic liquids like trioctylmethylammonium chloride (Aliquat 336), trioctylmethylammonium nitrate etc., do not exhibit any cation exchange with the metal ions from aqueous phase during extraction. However, there is no report available in literature that emphasizes the application of trioctylmethylammonium bis(trifluoromethane-sulfonyl)imide ((N_1_8_8_8)(NTf_2)) ionic liquid, for the extraction of Pu(IV). In this paper, we report the advantages of using the ionic liquid, trioctylmethylammonium bis(trifluoromethanesulfonyl)imide ((N_1_8_8_8)(NTf_2)), as diluent, for the extraction of plutonium(IV) in DHOA/(N_1_8_8_8)(NTf_2)

  12. Liquid-liquid extraction in flow analysis: A critical review

    Energy Technology Data Exchange (ETDEWEB)

    Silvestre, Cristina I.C.; Santos, Joao L.M. [REQUIMTE, Servico de Quimica-Fisica, Faculdade de Farmacia, Universidade do Porto, R. Anibal Cunha, 164, 4099-030 Porto (Portugal); Lima, Jose L.F.C., E-mail: limajlfc@ff.up.pt [REQUIMTE, Servico de Quimica-Fisica, Faculdade de Farmacia, Universidade do Porto, R. Anibal Cunha, 164, 4099-030 Porto (Portugal); Zagatto, Elias A.G. [Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo, P.O. Box 96, Piracicaba 13400-970 (Brazil)

    2009-10-12

    Liquid-liquid extractions (LLE) are a common sample pre-treatment in many analytical applications. This review aims at providing a critical overview of the distinct automated continuous flow-based approaches that were developed for liquid-liquid extraction with the purpose of pre-concentration and/or separation of multiple analytes, such as ultra-trace metal and metalloid species, phenolic compounds, surfactants, pharmaceuticals, etc., hyphenated with many detection technique such as UV/vis spectrophotometry, atomic spectrometric detection systems and luminescent detectors, including distinct extraction strategies and applications like single and multiple extraction schemes, wetting film extraction, supported liquid membrane extraction, back extraction, closed-loop systems and the utilisation of zone sampling, chromatomembranes and iterative reversal techniques. The analytical performance of the developed flow-based LLE methods and the influence of flow manifold components such as the segmenter, extraction coil and phase separator, is emphasised and object of discussion. An overall presentation of each system components, selectivity, advantages and shortcomings is carried out and exemplified with selected applications.

  13. Liquid-Liquid Extraction in Systems Containing Butanol and Ionic Liquids – A Review

    Directory of Open Access Journals (Sweden)

    Kubiczek Artur

    2017-03-01

    Full Text Available Room-temperature ionic liquids (RTILs are a moderately new class of liquid substances that are characterized by a great variety of possible anion-cation combinations giving each of them different properties. For this reason, they have been termed as designer solvents and, as such, they are particularly promising for liquid-liquid extraction, which has been quite intensely studied over the last decade. This paper concentrates on the recent liquid-liquid extraction studies involving ionic liquids, yet focusing strictly on the separation of n-butanol from model aqueous solutions. Such research is undertaken mainly with the intention of facilitating biological butanol production, which is usually carried out through the ABE fermentation process. So far, various sorts of RTILs have been tested for this purpose while mostly ternary liquid-liquid systems have been investigated. The industrial design of liquid-liquid extraction requires prior knowledge of the state of thermodynamic equilibrium and its relation to the process parameters. Such knowledge can be obtained by performing a series of extraction experiments and employing a certain mathematical model to approximate the equilibrium. There are at least a few models available but this paper concentrates primarily on the NRTL equation, which has proven to be one of the most accurate tools for correlating experimental equilibrium data. Thus, all the presented studies have been selected based on the accepted modeling method. The reader is also shown how the NRTL equation can be used to model liquid-liquid systems containing more than three components as it has been the authors’ recent area of expertise.

  14. Membrane assisted liquid-liquid extraction of cerium

    International Nuclear Information System (INIS)

    Soldenhoff, K.M.

    2000-02-01

    Membrane assisted liquid-liquid extraction of cerium was investigated, with emphasis placed on the study of the reaction chemistry and the kinetics of non-dispersive solvent extraction and stripping with microporous membranes. A bulk liquid membrane process was developed for the purification of cerium(IV) from sulfate solutions containing other rare earth elements. The cerium process was studied in both a flat sheet contained liquid membrane configuration and with hollow fibre contactors. Di-2-ethylhexyl phosphoric acid (DEHPA) was identified as a suitable extractant for cerium(IV) from sulfuric acid solution, with due consideration of factors such as extraction ability, resistance to degradation, solvent selectivity and potential for sulfate transfer into a strip solution. A detailed study of the extraction of cerium(IV) with DEHPA defined the extraction reaction chemistry. The Ce/DEHPA/sulfate system was also investigated with a flat sheet bulk liquid membrane configuration, using both sulfuric and hydrochloric acid as receiver solutions. These tests identified that hydrophobic membranes provide better mass transfer for extraction and hydrophilic membranes are better for stripping. The presence of an impurity, mono 2-ethylhexyl phosphoric acid (MEHPA), was found to have a dramatic accelerating effect on the rate of the chemical extraction reaction. This was attributed to its higher interfacial activity and population compared to DEHPA, and the fact that MEHPA was also found to be an active carrier for cerium(IV). The mass transfer rate of membrane assisted extraction and stripping of cerium, using hydrophobic and hydrophilic microporous membranes, respectively, was investigated using a modified Lewis-type cell. It was quantitatively demonstrated that the extraction process was mainly controlled by membrane diffusion and the stripping process was controlled by the chemical reaction rate, with membrane diffusion becoming important at low distribution coefficients

  15. SISAK liquid-liquid extraction experiments with preseparated {sup 257}Rf

    Energy Technology Data Exchange (ETDEWEB)

    Omtvedt, Jon Petter; Alstad, J.; Breivik, H. [University of Oslo, Department of Chemistry, Oslo (NO)] (and others)

    2002-06-01

    The SISAK liquid-liquid extraction system was used to extract 4.0-s {sup 257}Rf. The {sup 257}Rf was produced in the reaction {sup 208}Pb({sup 50}Ti, 1n){sup 257}Rf with 237-MeV beam energy on target, separated in the Berkeley Gas-filled Separator (BGS) and transferred to a gas jet using the Recoil Transfer Chamber (RTC). The activity delivered by the gas jet was dissolved in 6-M HNO{sub 3} and Rf was extracted into 0.25-M dibutyl-phosphoric acid in toluene. This was the first time a transactinide, i.e., an element with Z{>=}104, was extracted and unequivocally identified by the SISAK system. Thus, this pilot experiment demonstrates that the fast liquid-liquid extraction system SISAK, in combination with liquid-scintillation detectors, can be used for investigating the chemical properties of the transactinides. The extraction result is in accordance with the behaviour shown by the Rf group IV homologues Zr and Hf. (author)

  16. Separation of Asphaltenes by Polarity using Liquid-Liquid Extraction

    DEFF Research Database (Denmark)

    Andersen, Simon Ivar

    1997-01-01

    In order to investigate the nature of petroleum asphaltenes in terms of polarity a process was developed using initial liquid-liquid extraction of the oil phase followed by precipitation of the asphaltenes using n-heptane. The liquid-liquid extraction was performed using toluene-methanol mixtures...... phase. The asphaltenes were analysed using FTir, Elemental analysis, and HPLC-SEC with a diode array detector. With increasing content of toluene in the methanol the molecular weight distribution of the asphaltenes significantly move to higher molecular weights. The content of nitrogen and sulfur...

  17. SISAK liquid-liquid extraction experiments with preseparated 257Rf

    International Nuclear Information System (INIS)

    Omtvedt, Jon Petter; Alstad, J.; Breivik, H.; Dyve, J.E.; Eberhardt, K.; Folden III, C.M.; Ginter, T.; Gregorich, K.E.; Hult, E.A.; Johansson, M.; Kirbach, U.W.; Lee, D.M.; Mendel, M.; Nahler, A.; Ninov, V.; Omtvedt, L.A.; Patin, J.B.; Skarnemark, G.; Stavsetra, L.; Sudowe, R.; Wiehl, N.; Wierczinski, B.; Wilk, P.A.; Zielinski, P.M.; Kratz, J.V.; Trautmann, N.; Nitsche, H.; Hoffman, D.C.

    2002-01-01

    The SISAK liquid-liquid extraction system was used to extract 4.0-s 257Rf. The 257Rf was produced in the reaction 208Pb(50Ti, 1n)257Rf with 237-MeV beam energy on target, separated in the Berkeley Gas-filled Separator (BGS) and transferred to a gas jet using the Recoil Transfer Chamber (RTC). The activity delivered by the gas jet was dissolved in 6-M HNO3 and Rf was extracted into 0.25-M dibutyl-phosphoric acid in toluene. This was the first time a transactinide, i.e., an element with Z >= 104, was extracted and unequivocally identified by the SISAK system. Thus, this pilot experiment demonstrates that the fast liquid-liquid extraction system SISAK, in combination with liquidscintillation detectors, can be used for investigating the chemical properties of the transactinides. The extraction result is in accordance with the behaviour shown by the Rf group IV homologues Zr and Hf

  18. Ionizable polyethers as specific metal ion carriers in liquid-liquid extraction and liquid membrane separations

    International Nuclear Information System (INIS)

    Walkowiak, W.; Charewicz, W.A.; Bartsch, R.A.; Ndip, G.M.

    1988-01-01

    Consideration is given to results of investigations into competitive extraction and penetration through a liquid membrane of alkali and alkaline earth cations from aqueous solutions by a series of lipophilic and ionizable acyclic polyethers of various molecular structure. It is shown that specificity and selectiviy of cation carriers in liquid-liquid extraction and liquid membrane separation depend on molecular structure of acyclic polyethers

  19. Determination of Niacinamide in Lotions and Creams Using Liquid-Liquid Extraction and High-Performance Liquid Chromatography

    Science.gov (United States)

    Usher, Karyn M.; Simmons, Carolyn R.; Keating, Daniel W.; Rossi, Henry F., III

    2015-01-01

    Chemical separations are an important part of an undergraduate chemistry curriculum. Sophomore students often get experience with liquid-liquid extraction in organic chemistry classes, but liquid-liquid extraction is not as often introduced as a quantitative sample preparation method in honors general chemistry or quantitative analysis classes.…

  20. Transuranium element purification by liquid-liquid extraction

    International Nuclear Information System (INIS)

    Madic, C.; Koehly, G.

    1976-01-01

    In the transuranium element production, the liquid-liquid extraction purification is presented. The affinity of TBP and trilaurylammonium nitrate for these elements is given. Exemples of NP/Pu, Pu/Np, U/Pu, Am/Cm, Am and Cm/Ln separation are presented [fr

  1. An inkjet-printed microfluidic device for liquid-liquid extraction.

    Science.gov (United States)

    Watanabe, Masashi

    2011-04-07

    A microfluidic device for liquid-liquid extraction was quickly produced using an office inkjet printer. An advantage of this method is that normal end users, who are not familiar with microfabrication, can produce their original microfluidic devices by themselves. In this method, the printer draws a line on a hydrophobic and oil repellent surface using hydrophilic ink. This line directs a fluid, such as water or xylene, to form a microchannel along the printed line. Using such channels, liquid-liquid extraction was successfully performed under concurrent and countercurrent flow conditions. © The Royal Society of Chemistry 2011

  2. Plate performance in liquid-liquid extraction

    International Nuclear Information System (INIS)

    Wadkins, R.P.

    1984-01-01

    The relative effectiveness of perforated, nozzle, and burred plates from a capacity and extraction standpoint were studied in a pulsed liquid-liquid extraction system. The experiments were conducted in a 3.8 x 10 -2 m diameter column using a mixture of aluminum nitrate, nitric acid, and uranyl nitrate as the aqueous phase, and tributyl phosphate dissolved in AMSCO 125-90 W as the organic phase. The uranium was extracted from the aqueous phase to the organic phase. A standard cartridge was made for each type of plate and consisted of an assembly of plates spaced 5.08 x 10 -2 m apart. Each plate had 3.2 x 10 -3 m holes spaced on 6.1 x 10 -3 -m centers, and contained 23% free area. 16 references, 4 figures, 1 table

  3. Kinetics of glycoalkaloid hydrolysis and solanidine extraction in liquid-liquid systems

    Directory of Open Access Journals (Sweden)

    Stanković Mihajlo Z.

    2002-01-01

    Full Text Available The kinetics of glycoalkaloid hydrolysis and solanidine extraction in Analyzed in this study. obtained from dried and milled potato haulm to to which hydrochlotic acid was added is the first liquid phase, while chloroform trichloroethylene or carbon tetrachlondeisthe second organic, liquid phase. The purpose of this paper was to combine the processes of glycoalkaloid hydrolysis to solanidine and solanidine extraction into one step, and to find the optimal liquid-liquid system for such a process.

  4. Liquid-liquid extraction by reversed micelles in biotechnological processes

    Directory of Open Access Journals (Sweden)

    Kilikian B. V.

    2000-01-01

    Full Text Available In biotechnology there is a need for new purification and concentration processes for biologically active compounds such as proteins, enzymes, nucleic acids, or cells that combine a high selectivity and biocompatibility with an easy scale-up. A liquid-liquid extraction with a reversed micellar phase might serve these purposes owing to its capacity to solubilize specific biomolecules from dilute aqueous solutions such as fermentation and cell culture media. Reversed micelles are aggregates of surfactant molecules containing an inner core of water molecules, dispersed in a continuous organic solvent medium. These reversed micelles are capable of selectively solubilizing polar compounds in an apolar solvent. This review gives an overview of liquid-liquid extraction by reversed micelles for a better understanding of this process.

  5. Microsystems for liquid-liquid extraction of radionuclides in the analytical protocols

    International Nuclear Information System (INIS)

    Helle, Gwendolyne

    2014-01-01

    Radiochemical analyses are necessary to numerous steps for nuclear wastes management and for the control of the environment. An analytical protocol generally includes different steps of chemical separations which are lengthy, manual and complicated to implement because of their confinement in glove boxes and because of the hostile chemical and radiochemical media. Thus there is a huge importance to propose innovative and robust solutions to automate these steps but also to reduce the volumes of the radioactive and chemical wastes at the end of the analytical cycle. One solution consists in the miniaturization of the analyses through the use of lab-on-chip. The objective of this thesis work was to propose a rational approach to the conception of separative microsystems for the liquid-liquid extraction of radionuclides. To achieve this, the hydrodynamic behavior as well as the extraction performances have been investigated in one chip for three different chemical systems: Eu(III)-HNO 3 /DMDBTDMA, Eu(III)-AcO(H,Na)-HNO 3 /HDEHP and U(VI)-HCl/Aliquat336. A methodology has been developed for the implementation of the liquid-liquid extraction in micro-system for each chemical system. The influence of various geometric parameters such as channel length or specific interfacial area has been studied and the comparison of the liquid-liquid extraction performances has led to highlight the influence of the phases viscosities ratio on the flows. Thanks to the modeling of both hydrodynamics and mass transfer in micro-system, the criteria related to physical and kinetic properties of the chemical systems have been distinguished to propose a rational conception of tailor-made chips. Finally, several examples of the liquid-liquid extraction implementation in micro-system have been described for analytical applications in the nuclear field: U/Co separation by Aliquat336, Eu/Sm separation by DMDBTDMA or even the coupling between a liquid-liquid extraction chip and the system of

  6. The Influence of Extractant TOA, Stirring Time on the Extraction ProcessLiquid-liquid, and Liquid Membrane on the Liquid Wastes Containing Cd

    International Nuclear Information System (INIS)

    Prayitno; Djoko-Sardjono; Nurimaniwati; Adhe-Helmayani

    2000-01-01

    The influence of extractant and stirring time on the reduction componentcadmium on liquid wastes has been investigated. The method of experimentalused the extraction with liquid membrane emulsion. The parameters to beinvestigated were extractant amount tri-n octylamine (TOA), duration ofstirring time. In this investigated, extractant amount was varied from 5 to25 % (v/v) TOA, duration of stirring time varied from 5 to minutes. Theresult of experimental can be concluded that the best condition obtained forreducing cadmium component was on extractant amount 20 % (v/v) TOA, stirringtime 25 minutes. The best condition for reducing the cadmium component wasefficiency factor 98.35%. (author)

  7. Hydrogen extraction from liquid lithium-lead alloy by gas-liquid contact method

    International Nuclear Information System (INIS)

    Xie Bo; Weng Kuiping; Hou Jianping; Yang Guangling; Zeng Jun

    2013-01-01

    Hydrogen extraction experiment from liquid lithium-lead alloy by gas-liquid contact method has been carried out in own liquid lithium-lead bubbler (LLLB). Experimental results show that, He is more suitable than Ar as carrier gas in the filler tower. The higher temperature the tower is, the greater hydrogen content the tower exports. Influence of carrier gas flow rate on the hydrogen content in the export is jagged, no obvious rule. Although the difference between experimental results and literature data, but it is feasible that hydrogen isotopes extraction experiment from liquid lithium-lead by gas-liquid contact method, and the higher extraction efficiency increases with the growth of the residence time of the alloy in tower. (authors)

  8. Hybrid Multiphase CFD Solver for Coupled Dispersed/Segregated Flows in Liquid-Liquid Extraction

    Directory of Open Access Journals (Sweden)

    Kent E. Wardle

    2013-01-01

    Full Text Available The flows in stage-wise liquid-liquid extraction devices include both phase segregated and dispersed flow regimes. As a additional layer of complexity, for extraction equipment such as the annular centrifugal contactor, free-surface flows also play a critical role in both the mixing and separation regions of the device and cannot be neglected. Traditionally, computional fluid dynamics (CFD of multiphase systems is regime dependent—different methods are used for segregated and dispersed flows. A hybrid multiphase method based on the combination of an Eulerian multifluid solution framework (per-phase momentum equations and sharp interface capturing using Volume of Fluid (VOF on selected phase pairs has been developed using the open-source CFD toolkit OpenFOAM. Demonstration of the solver capability is presented through various examples relevant to liquid-liquid extraction device flows including three-phase, liquid-liquid-air simulations in which a sharp interface is maintained between each liquid and air, but dispersed phase modeling is used for the liquid-liquid interactions.

  9. EPA Method 8321B (SW-846): Solvent-Extractable Nonvolatile Compounds by High Performance Liquid Chromatography-Thermospray-Mass Spectrometry (HPLC-TS-MS) or Ultraviolet (UV) Detection

    Science.gov (United States)

    Method 8321B describes procedures for preparation and analysis of solid, aqueous liquid, drinking water and wipe samples using high performance liquid chromatography and mass spectrometry for extractable non-volatile compounds.

  10. Kinetic of liquid-liquid extraction for uranyl nitrate and actinides (III) and lanthanides (III) nitrates by amide extractants

    International Nuclear Information System (INIS)

    Toulemonde, V.; CEA Centre d'Etudes de la Vallee du Rhone, 30 -Marcoule

    1995-01-01

    The kinetics of liquid-liquid extraction by amide extractants have been investigated for uranyl nitrate (monoamide extractants), actinides (III) and lanthanides (III) nitrates (diamide extractants). The transfer of the metallic species from the aqueous phase to the organic phase was studied using two experimental devices: ARMOLLEX (Argonne Modified Lewis cell for Liquid Liquid Extraction) and RSC (Rotating Stabilized Cell). The main conclusions are: for the extraction of uranyl nitrate by DEHDMBA monoamide, the rate-controlling step is the complexation of the species at the interface of the two liquids. Thus, an absorption-desorption (according to Langmuir theory) reaction mechanism was proposed; for the extraction of actinides (III) and lanthanides (III) nitrates in nitric acid media by DMDBTDMA diamide, the kinetic is also limited by interfacial reactions. The behavior of Americium and Europium is very similar as fare as their reaction kinetics are concerned. (author)

  11. Analysis of penicillin G in milk by liquid chromatography.

    Science.gov (United States)

    Boison, J O; Keng, L J; MacNeil, J D

    1994-01-01

    A liquid chromatographic (LC) method that was previously developed for penicillin G residues in animal tissues has been adapted to milk and milk products. After protein precipitation with sodium tungstate, samples are applied to a C18 solid-phase extraction cartridge, from which penicillin is eluted, derivatized with 1,2,4-triazole-mercuric chloride solution, and analyzed by isocratic liquid chromatography (LC) on a C18 column with UV detection at 325 nm. Quantitation is done with reference to penicillin V as an internal standard. Penicillin G recoveries were determined to be > 70% on standards fortified at 3-60 ppb. Accuracy approached 100% using the penicillin V internal standard. The detection limit for penicillin G residues was 3 ppb in fluid milk. Samples may be confirmed by thermospray/LC at concentrations approaching the detection limit of the UV method.

  12. Ionic liquid based dispersive liquid-liquid microextraction for the extraction of pesticides from bananas.

    Science.gov (United States)

    Ravelo-Pérez, Lidia M; Hernández-Borges, Javier; Asensio-Ramos, María; Rodríguez-Delgado, Miguel Angel

    2009-10-23

    This paper describes a dispersive liquid-liquid microextraction (DLLME) procedure using room temperature ionic liquids (RTILs) coupled to high-performance liquid chromatography with diode array detection capable of quantifying trace amounts of eight pesticides (i.e. thiophanate-methyl, carbofuran, carbaryl, tebuconazole, iprodione, oxyfluorfen, hexythiazox and fenazaquin) in bananas. Fruit samples were first homogenized and extracted (1g) with acetonitrile and after suitable evaporation and reconstitution of the extract in 10 mL of water, a DLLME procedure using 1-hexyl-3-methylimidazolium hexafluorophosphate ([C(6)MIM][PF(6)]) as extraction solvent was used. Experimental conditions affecting the DLLME procedure (sample pH, sodium chloride percentage, ionic liquid amount and volume of disperser solvent) were optimized by means of an experimental design. In order to determine the presence of a matrix effect, calibration curves for standards and fortified banana extracts (matrix matched calibration) were studied. Mean recovery values of the extraction of the pesticides from banana samples were in the range of 69-97% (except for thiophanate-methyl and carbofuran, which were 53-63%) with a relative standard deviation lower than 8.7% in all cases. Limits of detection achieved (0.320-4.66 microg/kg) were below the harmonized maximum residue limits established by the European Union (EU). The proposed method, was also applied to the analysis of this group of pesticides in nine banana samples taken from the local markets of the Canary Islands (Spain). To the best of our knowledge, this is the first application of RTILs as extraction solvents for DLLME of pesticides from samples different than water.

  13. Kinetic of liquid-liquid extraction for uranyl nitrate and actinides (III) and lanthanides (III) nitrates by amide extractants; Cinetique d`extraction liquide-liquide du nitrate d`uranyle et des nitrates d`actinides (III) et de lanthanides (III) par des extractants a fonction amide

    Energy Technology Data Exchange (ETDEWEB)

    Toulemonde, V [CEA Centre d` Etudes Nucleaires de Saclay, 91 -Gif-sur-Yvette (France); [CEA Centre d` Etudes de la Vallee du Rhone, 30 -Marcoule (France). Dept. d` Exploitation du Retraitement et de Demantelement

    1995-12-20

    The kinetics of liquid-liquid extraction by amide extractants have been investigated for uranyl nitrate (monoamide extractants), actinides (III) and lanthanides (III) nitrates (diamide extractants). The transfer of the metallic species from the aqueous phase to the organic phase was studied using two experimental devices: ARMOLLEX (Argonne Modified Lewis cell for Liquid Liquid Extraction) and RSC (Rotating Stabilized Cell). The main conclusions are: for the extraction of uranyl nitrate by DEHDMBA monoamide, the rate-controlling step is the complexation of the species at the interface of the two liquids. Thus, an absorption-desorption (according to Langmuir theory) reaction mechanism was proposed; for the extraction of actinides (III) and lanthanides (III) nitrates in nitric acid media by DMDBTDMA diamide, the kinetic is also limited by interfacial reactions. The behavior of Americium and Europium is very similar as fare as their reaction kinetics are concerned. (author). 89 refs.

  14. Ionic Liquids as Extraction Media for Metal Ions

    Science.gov (United States)

    Hirayama, Naoki

    In solvent extraction separation of metal ions, recently, many researchers have investigated possible use of hydrophobic ionic liquids as extraction media instead of organic solvents. Ionic liquids are salts of liquid state around room temperature and can act not only as solvents but also as ion-exchangers. Therefore, the extraction mechanism of metal ions into ionic liquids is complicated. This review presents current overview and perspective on evaluation of nature of hydrophobic ionic liquids as extraction media for metal ions.

  15. Liquid-liquid extraction and separation studies of uranium(VI)

    International Nuclear Information System (INIS)

    Langade, A.D.; Shinde, V.M.

    1980-01-01

    Separation of uranium(VI) from iron(III), molybdenum(VI), vanadium(V), bismuth(III), zirconium(IV) and thorium(IV) is achieved by liquid-liquid extraction with 4-methyl-3-pentene-2-one (mesityl oxide; MeO) from sodium salicylate media (0.1M, pH 6.0). The extracted species is UO 2 (HO.C 6 H 4 COO) 2 .2MeO. A procedure for separating 50 μg of uranium from mg amounts of the other metals is described. (author)

  16. Alkylsulfate-based ionic liquids in the liquid–liquid extraction of aromatic hydrocarbons

    International Nuclear Information System (INIS)

    García, Silvia; Larriba, Marcos; García, Julián; Torrecilla, José S.; Rodríguez, Francisco

    2012-01-01

    Highlights: ► Values of α 2,1 for the four R-SO 4 ionic liquids are higher than those of sulfolane. ► Values of D 2 for all the ionic liquids are lower than those of sulfolane. ► Values of D 2 for [emim][C 2 H 5 SO 4 ] are the highest among the R-SO 4 ionic liquids. - Abstract: The (liquid + liquid) equilibrium data (LLE) for the extraction of toluene from heptane with different ionic liquids (ILs) based on the alkylsulfate anion (R-SO 4 ) was determined at T = 313.2 K and atmospheric pressure. The effect of more complex R-SO 4 anions on capacity of extraction and selectivity in the liquid–liquid extraction of toluene from heptane was studied. The ternary systems were formed by {heptane + toluene + 1,3-dimethylimidazolium methylsulfate ([mmim][CH 3 SO 4 ]), 1-ethyl-3-methylimidazolium hydrogensulfate ([emim][HSO 4 ]), 1-ethyl-3-methylimidazolium methylsulfate ([emim][CH 3 SO 4 ]), or 1-ethyl-3-methylimidazolium ethylsulfate ([emim][C 2 H 5 SO 4 ])}. The degree of quality of the experimental LLE data was ascertained by applying the Othmer–Tobias correlation. The phase diagrams for the ternary systems were plotted, and the tie lines correlated with the NRTL model compare satisfactorily with the experimental data.

  17. Uranium Extraction From Artificial Liquid Waste Using Continuous Extraction Liquid membrane Technique

    International Nuclear Information System (INIS)

    Rusdianasari; Buchari

    2002-01-01

    The continuous extraction of uranium from artificial liquid waste by emulsion liquid membrane was carried out using one stage mixer-settler. This emulsion liquid membrane containing di-2-ethylhexylphosphoric acid (D2EHPA) and tri-n-buthyl phosphate (TBP) as carrier were carried out using one stage mixer-settler. The optimum condition gave the ratio of emulsion velocity to the feed velocity 1:4 and steady state reached after five minutes. The optimum condition was obtained at the 90.91 % of uranium recovered from raffinate, using EDTA as the masking agent with concentration 5x10 - 2 M . The total concentration of carrier was 3% with ratio D2EHPA and TBP 3:1. The emulsion liquid membrane has high relative selectivity after steady state with separation factors were α U , N i= 115,43 and α U , Fe 328,55. The result of experiment showed that emulsion liquid membrane containing D2EHPA and TBP as carrier have good performance for continuous system

  18. Solid-Liquid Separation Properties of Thermoregulated Dicationic Ionic Liquid as Extractant of Dyes from Aqueous Solution

    Directory of Open Access Journals (Sweden)

    Rui Lv

    2018-01-01

    Full Text Available Two thermoregulated dicationic ionic liquids were synthesized and applied for effective extraction of the common dye malachite green oxalate (MG. The extraction parameters such as amount of ionic liquids, pH of water phase, extraction time, cooling time, and centrifugal time on the extraction efficiency were investigated systematically. It revealed that the dye has been successfully extracted into the ionic liquids, with high extraction efficiency higher than 98%, and recovery of 98.2%–100.8%, respectively. Furthermore, these ionic liquids can be recycled easily after elution. The reusable yields were 87.1% and 88.7%. The extraction of the dye into the thermoregulated ionic liquid provides a method of minimizing pollution of waste water potentially.

  19. Liquid-liquid extraction of actinides, lanthanides, and fission products by use of ionic liquids: from discovery to understanding.

    Science.gov (United States)

    Billard, Isabelle; Ouadi, Ali; Gaillard, Clotilde

    2011-06-01

    Liquid-liquid extraction of actinides and lanthanides by use of ionic liquids is reviewed, considering, first, phenomenological aspects, then looking more deeply at the various mechanisms. Future trends in this developing field are presented.

  20. Pesticide extraction from table grapes and plums using ionic liquid based dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Ravelo-Pérez, Lidia M; Hernández-Borges, Javier; Herrera-Herrera, Antonio V; Rodríguez-Delgado, Miguel Angel

    2009-12-01

    Room temperature ionic liquids (RTILs) have been used as extraction solvents in dispersive liquid-liquid microextraction (DLLME) for the determination of eight multi-class pesticides (i.e. thiophanate-methyl, carbofuran, carbaryl, tebuconazole, iprodione, oxyfluorfen, hexythiazox, and fenazaquin) in table grapes and plums. The developed method involves the combination of DLLME and high-performance liquid chromatography with diode array detection. Samples were first homogenized and extracted with acetonitrile. After evaporation and reconstitution of the extract in water containing sodium chloride, a quick DLLME procedure that used the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate ([C(6)MIM][PF(6)]) and methanol was developed. The RTIL dissolved in a very small volume of acetonitrile was directed injected in the chromatographic system. The comparison between the calibration curves obtained from standards and from spiked sample extracts (matrix-matched calibration) showed the existence of a strong matrix effect for most of the analyzed pesticides. A recovery study was also developed with five consecutive extractions of the two types of fruits spiked at three concentration levels. Mean recovery values were in the range of 72-100% for table grapes and 66-105% for plum samples (except for thiophanate-methyl and carbofuran, which were 64-75% and 58-66%, respectively). Limits of detection (LODs) were in the range 0.651-5.44 microg/kg for table grapes and 0.902-6.33 microg/kg for plums, representing LODs below the maximum residue limits (MRLs) established by the European Union in these fruits. The potential of the method was demonstrated by analyzing 12 commercial fruit samples (six of each type).

  1. Application of liquid-liquid extraction in uranium hydrometallurgy (Paper No. : V-1)

    Energy Technology Data Exchange (ETDEWEB)

    Murthy, T K.S.; Koppiker, K S

    1979-01-01

    Uranium recovery from the ores is carried out exclusively by hydrometallurgical techniques. The initial solubilisation of uranium is achieved by either sodium carbonate or sulphuric acid leaching, the latter being more common. Further purification and upgrading of uranium from the sulphate liquors is carried out by an ion-exchange process. Solid resin type anion exchangers or liquid ion-exchangers are employed. The processing of uranium liquors is, perhaps, the first major application of liquid-liquid extraction in metal recovery. Organophosphoric acids were initially used but later the long-chain aliphatic amines have superseded them. The amine extraction system has been widely studied and several variations are now known. Chloride, nitrate, carbonate or sulphate or acid stripping can be used for getting back the uranium into the aqueous phase. Combination of ion exchange (resin type) and solvent extraction processes called Eluex processes are developed for special applications. Studies have also been made of solvent extraction of uranium from leach pulps instead of clear liquors. Tributylphosphate has found wide application in the refining of uranium concentrates to meet the stringent needs of nuclear purity. liquid-liquid extraction is, perhaps, the only successful technique for the recovery of uranium, as by-product, from wet-process phosphoric acid. This has opened up a new source of uranium.

  2. Metal extraction by solid-liquid agglomerates

    International Nuclear Information System (INIS)

    Fuller, E.F.

    1980-01-01

    Dissolved metal values are extracted from a liquid e.g. uranium from phosphoric acid by contacting the liquid with agglomerates for a time to load the agglomerate with the metal value, separating the loaded agglomerates from the liquid phase and stripping the metal value from the loaded agglomerate. The agglomerate may be made by combining finely divided solid particles with a binding liquid to form a paste, adding a suspending liquid to form a mixture, the suspending liquid and binding liquid being immiscible in each other and the solid particles being insoluble in the suspending liquid and shearing the mixture to form the agglomerate. (author)

  3. Liquid-liquid extraction of actinides, lanthanides, and fission products by use of ionic liquids: from discovery to understanding

    International Nuclear Information System (INIS)

    Billard, Isabelle; Ouadi, Ali; Gaillard, Clotilde

    2011-01-01

    Liquid-liquid extraction of actinides and lanthanides by use of ionic liquids is reviewed, considering, first, phenomenological aspects, then looking more deeply at the various mechanisms. Future trends in this developing field are presented. (orig.)

  4. Separation of rare earths by liquid-liquid extraction

    International Nuclear Information System (INIS)

    Helgorsky, M.; Leveque, M.

    1978-01-01

    The elements of the rare earth family are characterised by very similar chemical properties connected with their special electronic structure. The purification of the rare earths sold by RHONE-POULENC is now done by the liquid-liquid extraction technique. The development of different extracting agents and also counter-current techniques have led to solvent extraction replacing the other fractionation techniques because of its efficiency and low cost. There are usually several possible solutions to the main problem of choosing the extracting agent and its mode of use. The difficulty is to find the most economical one taking account of the thermodynamic and hydrodynamic constraints of the solvent. It is shown how ideas about the separation have changed over the course of the development of the uses of the rare earths, ending finally in an integrated scheme that makes RHONE-POULENC a world leader of manufacturers of separated rare earths [fr

  5. AFM fluid delivery/liquid extraction surface sampling/electrostatic spray cantilever probe

    Science.gov (United States)

    Van Berkel, Gary J.

    2015-06-23

    An electrospray system comprises a liquid extraction surface sampling probe. The probe comprises a probe body having a liquid inlet and a liquid outlet, and having a liquid extraction tip. A solvent delivery conduit is provided for receiving solvent liquid from the liquid inlet and delivering the solvent liquid to the liquid extraction tip. An open liquid extraction channel extends across an exterior surface of the probe body from the liquid extraction tip to the liquid outlet. An electrospray emitter tip is in liquid communication with the liquid outlet of the liquid extraction surface sampling probe. A system for analyzing samples, a liquid junction surface sampling system, and a method of analyzing samples are also disclosed.

  6. Recycling of Metal Containing Waste by Liquid-Liquid Extraction

    International Nuclear Information System (INIS)

    Reinhardt, H.

    1999-01-01

    Through the years, a large number of liquid-liquid extraction have been proposed for metal waste recovery and recycling(1,2). However, few of them have achieved commercial application. In fact, relatively little information is available on practical operation and economic feasibility. This presentation will give complementary information by describing and comparing three processes, based on the Am MAR hydrometallurgical concept and representing three different modes of operation

  7. Determination of diflubenzuron and chlorbenzuron in fruits by combining acetonitrile-based extraction with dispersive liquid-liquid microextraction followed by high-performance liquid chromatography.

    Science.gov (United States)

    Ruan, Chunqiang; Zhao, Xiang; Liu, Chenglan

    2015-09-01

    In this study, a simple and low-organic-solvent-consuming method combining an acetonitrile-partitioning extraction procedure followed by "quick, easy, cheap, effective, rugged and safe" cleanup with ionic-liquid-based dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection was developed for the determination of diflubenzuron and chlorbenzuron in grapes and pears. Ionic-liquid-based dispersive liquid-liquid microextraction was performed using the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate as the extractive solvent and acetonitrile extract as the dispersive solvent. The main factors influencing the efficiency of the dispersive liquid-liquid microextraction were evaluated, including the extractive solvent type and volume and the dispersive solvent volume. The validation parameters indicated the suitability of the method for routine analyses of benzoylurea insecticides in a large number of samples. The relative recoveries at three spiked levels ranged between 98.6 and 109.3% with relative standard deviations of less than 5.2%. The limit of detection was 0.005 mg/kg for the two insecticides. The proposed method was successfully used for the rapid determination of diflubenzuron and chlorbenzuron residues in real fruit samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Extraction by means of emulsified liquid membranes; Extraction par membranes liquides emulsionnees (MLE)

    Energy Technology Data Exchange (ETDEWEB)

    Pareau, D.; Stambouli, M. [Ecole Centrale de Paris, 75 (France)

    2006-12-15

    It is an alternative of the liquid-liquid extraction process where extraction and stripping are simultaneously carried out. The stripping solution is dispersed in the solvent in micro-droplets. This emulsion, stabilised by a surface-active agent, is then dispersed in the liquid to be treated and, during that step, the metal is transferred to the stripping solution, moving through the solvent which operates as an organic membrane. The paper describes in detail the mechanism of the process, its advantages and its disadvantages. Its field of applications is wide, but only a few units are now industrially in operation, most of them exists only at the pilot scale. It is particularly adapted for the treatment of effluents with a very low content in metallic impurities. As examples, the paper describes the recovery of zinc from viscose plant effluents (Lenzing plant, Austria) and the removal of free cyanide ions and cyanide metallic complexes (pilot scale). (authors)

  9. Glycerol-based deep eutectic solvents as extractants for the separation of MEK and ethanol via liquid-liquid extraction

    NARCIS (Netherlands)

    Rodriguez, N.R.; Ferré Güell, J.; Kroon, M.C.

    2016-01-01

    Four different glycerol-based deep eutectic solvents (DESs) were tested as extracting agents for the separation of the azeotropic mixture {methyl ethyl ketone + ethanol} via liquid-liquid extraction. The selected DESs for this work were: glycerol/choline chloride with molar ratios (4:1) and (2:1),

  10. Determination of Organic Pollutants in Small Samples of Groundwaters by Liquid-Liquid Extraction and Capillary Gas Chromatography

    DEFF Research Database (Denmark)

    Harrison, I.; Leader, R.U.; Higgo, J.J.W.

    1994-01-01

    A method is presented for the determination of 22 organic compounds in polluted groundwaters. The method includes liquid-liquid extraction of the base/neutral organics from small, alkaline groundwater samples, followed by derivatisation and liquid-liquid extraction of phenolic compounds after neu...... neutralisation. The extracts were analysed by capillary gas chromatography. Dual detection by flame Ionisation and electron capture was used to reduce analysis time....

  11. Liquid-liquid extraction kinetics of uranyl nitrate and actinides (III)-lanthanides nitrates by extractants with amide function

    International Nuclear Information System (INIS)

    Toulemonde, V.

    1995-01-01

    Nowadays, the most important part of electric power is generated by fission energy. But spent fuels have then to be reprocessed. The production of these reprocessed materials separately and with a high purity level is done according to a liquid-liquid extraction process (Purex process) with the use of tributyl phosphate as solvent. Optimization studies concerning the extracting agent have been undertaken. This work gives the results obtained for the uranyl nitrate and the actinides (III)-lanthanides (III) nitrates extraction by extractants with amide function (monoamide for U(VI) and diamide for actinides (III) and lanthanides (III)). The extraction kinetics have been studied in the case of a metallic specie transfer from the aqueous phase towards the organic phase. The experiments show that the nitrates extraction kinetics is limited by the complexation chemical reaction of the species at the interface between the two liquids. An adsorption-desorption interfacial reactional mechanism (Langmuir theory) is proposed for the uranyl nitrate. (O.M.)

  12. One-step extraction of polar drugs from plasma by Parallel Artificial Liquid Membrane Extraction

    DEFF Research Database (Denmark)

    Pilařová, Veronika; Sultani, Mumtaz; Ask, Kristine Skoglund

    2017-01-01

    in the pores of a thin polymeric membrane, a well-known extraction principle also used in hollow fiber liquid-phase microextraction (HF-LPME). However, the new PALME technique offers a more user-friendly setup in which the supported liquid membrane is incorporated in a 96 well plate system. Thus, high......The new microextraction technique named parallel artificial liquid membrane extraction (PALME) was introduced as an alternative approach to liquid-liquid extraction of charged analytes from aqueous samples. The concept is based on extraction of analytes across a supported liquid membrane sustained...... for extraction of polar basic drugs was developed in the present work. The basic drugs hydralazine, ephedrine, metaraminol, salbutamol, and cimetidine were used as model analytes, and were extracted from alkalized human plasma into an aqueous solution via the supported liquid membrane. The extraction...

  13. Quaternary (liquid + liquid) equilibrium data for the extraction of toluene from alkanes using the ionic liquid [EMim][MSO4

    International Nuclear Information System (INIS)

    Corderí, Sandra; Calvar, Noelia; Gómez, Elena; Domínguez, Ángeles

    2014-01-01

    Highlights: • EMim[MSO 4 ] was proposed as solvent for the extraction of toluene from alkanes. • The quaternary system {heptane + cyclohexane + toluene + [EMim][MSO 4 ]} was evaluated. • The extraction of toluene would be facilitated in the presence of one alkane. • Experimental LLE data were successfully correlated with the NRTL model. - Abstract: (Liquid + liquid) equilibrium (LLE) studies for the extraction of aromatics from alkanes present in the petroleum fractions are important to develop theoretical/semiempirical (liquid + liquid) equilibrium models, which are used in the design of extraction processes. In this work, the ionic liquid 1-ethyl-3-methylimidazolium methylsulfate, [EMim][MSO 4 ], was evaluated as potential solvent for the separation of toluene from heptane and cyclohexane. The LLE data for the quaternary system {heptane (1) + cyclohexane (2) + toluene (3) + [EMim][MSO 4 ] (4)} were experimentally determined at T = 298.15 K and atmospheric pressure. Moreover, the LLE data for the ternary systems {heptane or cyclohexane (1) + toluene (2) + [EMim][MSO 4 ] (3)} were also determined. Solute distribution ratios and selectivities were calculated and analysed in order to evaluate the capability of the ionic liquid to accomplish the separation target. A comparison between the solute distribution ratios and selectivities for the quaternary and the ternary systems was also made. Finally, the experimental tie-line data were correlated with the NRTL model

  14. Ionic-liquid-impregnated resin for the microwave-assisted solid-liquid extraction of triazine herbicides in honey.

    Science.gov (United States)

    Wu, Lijie; Song, Ying; Hu, Mingzhu; Yu, Cui; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

    2015-09-01

    Microwave-assisted ionic-liquid-impregnated resin solid-liquid extraction was developed for the extraction of triazine herbicides, including cyanazine, metribuzin, desmetryn, secbumeton, terbumeton, terbuthylazine, dimethametryn, and dipropetryn in honey samples. The ionic-liquid-impregnated resin was prepared by immobilizing 1-hexyl-3-methylimidazolium hexafluorophosphate in the microspores of resin. The resin was used as the extraction adsorbent. The extraction and enrichment of analytes were performed in a single step. The extraction time can be shortened greatly with the help of microwave. The effects of experimental parameters including type of resin, type of ionic liquid, mass ratio of resin to ionic liquid, extraction time, amount of the impregnated resin, extraction temperature, salt concentration, and desorption conditions on the extraction efficiency, were investigated. A Box-Behnken design was applied to the selection of the experimental parameters. The recoveries were in the range of 80.1 to 103.4% and the relative standard deviations were lower than 6.8%. The present method was applied to the analysis of honey samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Primary metals extraction by liquid membranes

    International Nuclear Information System (INIS)

    Subramanian, K.N.

    1980-01-01

    The extraction of copper and uranium by liquid membranes is presented. The recovery of uranium from wet process phosphoric acid is described. The development of this process has progressed through three stages, firstly the chemistry of uranium extraction as it pertains to liquid membrane systems. This was followed by continuous extraction tests on fresh black acid and on aged acid. Results on a 1 litre/minute pilot plant demonstrated that the process could be operated with a minimum of feed pretreatment and about 90% of uranium could be extracted. The extraction of copper from copper leach liquors is also described. (U.K.)

  16. Haze Formation and Behavior in Liquid-Liquid Extraction Processes

    International Nuclear Information System (INIS)

    Arm, Stuart T.; Jenkins, J. A.

    2006-01-01

    Aqueous haze formation and behavior was studied in the liquid-liquid system tri-n-butyl phosphate in odorless kerosene and 3M nitric acid with uranyl nitrate and cesium nitrate representing the major solute and an impurity, respectively. A pulsed column, mixer-settler and centrifugal contactor were chosen to investigate the effect of different turbulence characteristics on the manifestation of haze since these contactors exhibit distinct mixing phenomena. The dispersive processes of drop coalescence and breakage, and water precipitation in the organic phase were observed to lead to the formation of haze drops of ∼1 um in diameter. The interaction between the haze and primary drops of the dispersion was critical to the separation efficiency of the liquid-liquid extraction equipment. Conditions of high power input and spatially homogeneous mixing enabled the haze drops to become rapidly assimilated within the dispersion to maximize the scrub performance and separation efficiency of the equipment

  17. Pre-concentration of uranium from water samples by dispersive liquid-liquid micro-extraction

    Energy Technology Data Exchange (ETDEWEB)

    Khajeh, Mostafa; Nemch, Tabandeh Karimi [Zabol Univ. (Iran, Islamic Republic of). Dept. of Chemistry

    2014-07-01

    In this study, a simple and rapid dispersive liquid-liquid microextraction (DLLME) was developed for the determination of uranium in water samples prior to high performance liquid chromatography with diode array detection. 1-(2-pyridylazo)-2-naphthol (PAN) was used as complexing agent. The effect of various parameters on the extraction step including type and volume of extraction and dispersive solvents, pH of solution, concentration of PAN, extraction time, sample volume and ionic strength were studied and optimized. Under the optimum conditions, the limit of detection (LOD) and preconcentration factor were 0.3 μg L{sup -1} and 194, respectively. Furthermore, the relative standard deviation of the ten replicate was <2.6%. The developed procedure was then applied to the extraction and determination of uranium in the water samples.

  18. Pre-concentration of uranium from water samples by dispersive liquid-liquid micro-extraction

    International Nuclear Information System (INIS)

    Khajeh, Mostafa; Nemch, Tabandeh Karimi

    2014-01-01

    In this study, a simple and rapid dispersive liquid-liquid microextraction (DLLME) was developed for the determination of uranium in water samples prior to high performance liquid chromatography with diode array detection. 1-(2-pyridylazo)-2-naphthol (PAN) was used as complexing agent. The effect of various parameters on the extraction step including type and volume of extraction and dispersive solvents, pH of solution, concentration of PAN, extraction time, sample volume and ionic strength were studied and optimized. Under the optimum conditions, the limit of detection (LOD) and preconcentration factor were 0.3 μg L -1 and 194, respectively. Furthermore, the relative standard deviation of the ten replicate was <2.6%. The developed procedure was then applied to the extraction and determination of uranium in the water samples.

  19. CONTRIBUTION TO THE DEVELOPMENT OF A SIMULATION SOFTWARE PERFORMANCE AND SHARING RATIO IN LIQUID-LIQUID EXTRACTION

    Directory of Open Access Journals (Sweden)

    A. Hadj Seyd

    2015-07-01

    Full Text Available The present work is to develop software to predict the value yield and the distribution coefficient in the process of liquid-liquid extraction of components of a mixture, from mathematical models expressing these entities, based on equations equilibrium between liquid-liquid phases, and predict the conditions under which the extraction operation is favorable, unfavorable or impossible to realize, by studying the variation of the entities cited, based on the parameters influencing the extraction, which are: initial concentrations, rate of solvent and pH, in the case of a simple extraction (extraction of neutral products or when it is reactive (extraction of complex acids or bases for one or more components.The programming language used is "Delphi" which is a very powerful oriented object programming under Windows.

  20. Synergistic extraction of europium(III) in ammonium ionic liquid

    International Nuclear Information System (INIS)

    Rout, Alok; Venkatesan, K.A.; Antony, M.P.

    2016-01-01

    Room temperature ionic liquids have been receiving increased attention for possible applications in the area of nuclear fuel reprocessing and waste management due to their fascinating properties such as good ionicity, high solvation capability, properties tunable etc. Most of the studies in the literature on the extraction of metal ions with molecular extractants dissolved in ionic liquid diluents are making use of the hydrophobic ionic liquids containing imidazolium cations such as the 1-alkyl-3-methylimidazolium ion. From an environmental point of view, such ionic liquids are not suitable as the primary mode of the metal extraction is by cation exchange mechanism wherein ionic liquid cation is lost to the aqueous phase leading to aqueous contamination and issue of recyclability of organic phase. However, there are some hydrophobic ionic liquids such as trioctylmethylammonium chloride ((N 1888 )(Cl)), and trihexyl(tetradecyl)phoshonium chloride (Cyphos IL 101) that exhibit no cation exchange in the aqueous phase during extraction. In this context, the extraction behavior of europium(III) using a neutral extractant, octyl, phenyl-N.N-diisobutylmethylcarbamoylphophinoxide (CMPO) and/or an acidic extractant bis(ethylhexyl)phosphoric acid (D2EHPA) dissolved in the ammonium ionic liquid diluent, trioctylmethylammonium bis(trifluoromethanesulfonyl)imide, (N 1888 )(NTf 2 ). The extraction behavior of CMPO (or D2EHPA)/(N 1888 )((Tf 2 ) system was investigated as a function of different extraction parameters such as feed acidity, extractant concentration, equilibration time etc.

  1. Removal of nitrogen compounds from Brazilian petroleum samples by oxidation followed by liquid-liquid extraction

    Energy Technology Data Exchange (ETDEWEB)

    Conceicao, L.; Pergher, S.B.C. [Universidade Regional Integrada do Alto Uruguai e das Misses (URI), Erechim, RS (Brazil). Dept. de Quimica], E-mail: pergher@uricer.edu.br; Oliveira, J.V. [Universidade Regional Integrada do Alto Uruguai e das Misses (URI), Erechim, RS (Brazil). Dept. de Engenharia dos Alimentos; Souza, W.F. [Petroleo Brasileiro S.A. (CENPES/PETROBRAS), Rio de Janeiro, RJ (Brazil). Centro de Pesquisas

    2009-10-15

    This work reports liquid-liquid extraction of nitrogen compounds from oxidized and non-oxidized Brazilian petroleum samples. The experiments were accomplished in a laboratory-scale liquid-liquid apparatus in the temperature range of 303 K-323 K, using methanol, n-methyl-2-pyrrolidone (NMP) and N,Ndimethylformamide (DMF), and their mixtures as extraction solvents, employing solvent to sample volume ratios of 1:2, 1:1 and 2:1, exploring up to three separation stages. Results show that an increase in temperature, solvent to oil ratio, and number of equilibrium stages greatly improves the nitrogen removal from the oxidized sample (from 2600 to 200 ppm). The employed oxidation scheme is thus demonstrated to be an essential and efficient step of sample preparation for the selective liquid-liquid removal of nitrogen compounds. It is shown that the use of mixtures of DMF and NMP as well their use as co-solvents with methanol did not prove to be useful for selective nitrogen extraction since great oil losses were observed in the final process. (author)

  2. Enhanced flavour extraction in continuous liquid-liquid extractors

    CSIR Research Space (South Africa)

    Apps, P

    2005-08-12

    Full Text Available stirrer that prevents channelling improves extraction efficiency by between 2.8 and 17.6 times. Use of the stir bar extends the application of CLLE to samples that are not free-running liquids, thereby reducing sample manipulations with their associated...

  3. Purification process for aqueous solutions of rare earths by liquid-liquid extraction

    International Nuclear Information System (INIS)

    Rollat, A.; Sabot, J.L.; Burgard, M.; Delloye, T.

    1986-01-01

    Alkaline earth metals are removed by liquid-liquid extraction between on aqueous nitric phase of impure rare earth compounds and an organic phase of polyether (crown ether). This process is particularly suited to removal of Ca, Ba and Ra contained in nitric solutions of rare earths [fr

  4. Evaluation of a contact device type ejector system for liquid-liquid extraction

    International Nuclear Information System (INIS)

    Schwamback, Niomedes

    2002-04-01

    The objective of the present work was to evaluate an ejector system, operated simultaneously with two immiscible liquid phases and a gas phase, as a contact device for liquid-liquid extraction processes. The ejector, made of perspex, has a variable geometry, although this feature was not explored in the thesis. Motivated by recent uses of liquid-liquid extraction processes for the removal of traces of heavy metal from waste waters, it was decided to carry out tests with synthetic effluents. This strategy, typical of experimental work under evaluation of technical feasibility, greatly simplifies experiments, since the nature of the chemical species involved and their feed concentrations are known exactly and do not fluctuate. The extractant used was DEHPA (diethyl hexyl phosphoric acid). The metal chosen for tests was iron with oxidation number +3, because of its high extraction coefficient towards DEHPA and also for its chemical behavior similar to americium and other heavy metals. In addition to that, iron forms soluble coloured complexes adequate to spectrophotometric determination analysis, a simple, quick and very reliable analytical technique. The effects of electrolytes of interest, namely NaCl, FeSO 4 and Al(NO 3 ) 3 , upon the extraction process were investigated. The effects resulting from the introduction of a gas phase, actually air (bubbles), in the ejector upon the extraction efficiency were studied. By coupling advanced digital photographic technique and image analysis with microcomputer, the bubble mean size was measured. It was then correlated with equipment's geometrical (characteristic diameters) and operational variables (phases' flow rates and gas hold-ups). To enable scale-up procedures, data were preferably correlated by means of dimensionless groups. For the systems and conditions investigated in this thesis and under the same operational conditions, the introduction of air bubbles by means of an ejector has greatly improved the process

  5. Feasibility of bio-based lactate esters as extractant for biobutanol recovery: (Liquid + liquid) equilibria

    International Nuclear Information System (INIS)

    Zheng, Shaohua; Cheng, Hongye; Chen, Lifang; Qi, Zhiwen

    2016-01-01

    Highlights: • Lactate esters were studied as solvent to remove butanol from aqueous media. • (Liquid + liquid) equilibrium data were measured at T = 298.15 K and 1 atm. • Selectivity and 1-butanol partition coefficient were calculated. • COSMO-based study of separation efficiency on solvent structure was conducted. - Abstract: As bio-based solvents, lactate esters can be used as extractant for removing 1-butanol from the aqueous fermentation broths. In order to evaluate the separation efficiency of butyl lactate and 2-ethylhexyl lactate for the extraction of 1-butanol from its mixture with water, the (liquid + liquid) equilibrium for the ternary systems {water (1) + 1-butanol (2) + lactate ester (3)} were measured at T = 298.15 K. The 1-butanol partition coefficient varied in the range of 4.46 to 10.29, and the solvent selectivity within 32.12 to 108.18. For the separation of low-concentration butanol from fermentation broths, butyl lactate exhibits higher partition coefficient and lower selectivity than 2-ethylhexyl lactate. The NRTL model was employed to correlate the experimental data, and the COSMO-RS theory was utilized to predict the (liquid + liquid) equilibria and to analyze the influence of lactate esters on extraction efficiency.

  6. Column liquid chromatography- mass spectrometry: selected techniques in environmental applications for polar pesticides and related compounds.

    NARCIS (Netherlands)

    Slobodnik, J.; van Baar, B.L.M.; Brinkman, U.A.T.

    1995-01-01

    A review covering the field of environmental applications of liquid chromatography-mass spectrometry (LC-MS) is presented. Recent developments and advances are discussed with emphasis on the presently popular thermospray, particle beam and atmospheric pressure ionisation interfaces. Each interface

  7. Pyridinium ionic liquid-based liquid-solid extraction of inorganic and organic iodine from Laminaria.

    Science.gov (United States)

    Peng, Li-Qing; Yu, Wen-Yan; Xu, Jing-Jing; Cao, Jun

    2018-01-15

    A simple, green and effective extraction method, namely, pyridinium ionic liquid- (IL) based liquid-solid extraction (LSE), was first designed to extract the main inorganic and organic iodine compounds (I - , monoiodo-tyrosine (MIT) and diiodo-tyrosine (DIT)). The optimal extraction conditions were as follows: ultrasonic intensity 100W, IL ([EPy]Br) concentration 200mM, extraction time 30min, liquid/solid ratio 10mL/g, and pH value 6.5. The morphologies of Laminaria were studied by scanning electron microscopy and transmission electron microscopy. The recovery values of I - , MIT and DIT from Laminaria were in the range of 88% to 94%, and limits of detection were in the range of 59.40 to 283.6ng/g. The proposed method was applied to the extraction and determination of iodine compounds in three Laminaria. The results showed that IL-based LSE could be a promising method for rapid extraction of bioactive iodine from complex food matrices. Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. Application of solid-liquid extraction separation in analytical chemistry: Pt. 1

    International Nuclear Information System (INIS)

    Xu Zulan; Dai Lixin

    1985-01-01

    Low m.p. waxes as solid solvents for solid-liquid extraction separation are advanced. Uranium in aqueous phase is extracted by homogeneous organic phase which is composed of waxes and various kinds of extractants. Various parameters of this extraction separation method are studied and compared with one of liquid-liquid extraction. The characteristic of wax as solvent, speciality and applicability of solid-liquid extraction separation method are evaluated

  9. Association of solvent extraction and liquid-liquid flotation processes for metal recovery

    International Nuclear Information System (INIS)

    Puget, Flavia P.; Mendonca, Luciano A. de; Massarani, Giulio

    2000-01-01

    From the batch solvent extraction process, in this work it has been carried out a preliminary study aiming the determination of the optimal operating conditions for zirconium recovery (10 ppm) using alamine 336 (tricaprylylamine) as extractor. The results have shown that the extraction takes place instantaneously (5s of manual agitation) and that at pH around 2.0 the extraction efficiency is up to 98-99% for an aqueous/organic phase volumetric ratio of 10. Based on these results, it is proposed to evaluate the possibility of using of a pioneering technology for metal recovery at low concentrations, using a experimental set-up that associates standard solvent extraction process with liquid-liquid flotation process. (author)

  10. PERFORMANCE OF A PACKED LIQUID-LIQUID EXTRACTION COLUMN

    Directory of Open Access Journals (Sweden)

    İ. Metin HASDEMİR

    1999-03-01

    Full Text Available The influence of feed ratios ((LE/LR on the performance of a packed liquid-liquid extraction column, with a diameter of 5.86 cm and a column height of 132 cm was investigated. The column is made of borosilicate glass and packed with 10 x 10 mm glass Raschig rings. In this study, a ternary system composed of water + propionic acid + trichloroethylene was used. The data used to triangular diagram were obtained experimentally. The overall mass transfer coefficients, the numbers of overall mass transfer units, the heights of mass transfer units, the numbers of theoretical stages and height equivalent to a theoretical stage (H. E. T. S. values were calculated and compared with each other.

  11. Liquid-liquid extraction from molten alkaline nitrates by using nitrogenous and organophosphorus derivatives

    International Nuclear Information System (INIS)

    Vittori, Olivier

    1971-01-01

    This research thesis reports the use of a system made of the LiNO 3 -KNO 3 eutectic at 160 deg. C and poly-phenyls in order to study the behaviour of phosphine and arsine oxides as extracting agents in a liquid-liquid process. In a first part, the author presents the studied system, its physical characteristics and its preparation, and the various analytical methods which have used. He discusses existing computation methods adapted to the separation of molten salts and organic phase, and proposes a specific method. Then, he reports the study of the behaviour of a phosphine oxide with Cobalt II and Nickel II, and discusses its application to the separation of this pair, Co II and Ni II. He highlights the different possibilities of three agents which are derivatives of phosphine and arsine in their ability to extract rare earths. A study of separation of rare earths is then addressed. The author reports the application of extraction equilibriums to the study of equilibriums in environments of molten salts with the Co II - chloride ions system. The author finally addresses the synergic phenomenon that pairs of neutral complexing agents of neighbouring structure or different donor central atom may display in liquid-liquid extraction

  12. Ionic liquids used in extraction and separation of metal ions

    International Nuclear Information System (INIS)

    Shen Xinghai; Xu Chao; Liu Xinqi; Chu Taiwei

    2006-01-01

    Ionic liquids as green solvents now have become a research hotspot in the field of separation of metal ions by solvent extraction. Experimental results of extraction of various metal ions with ionic liquids as solvents, including that of alkali metals, alkaline earths, transition metals rare earths and actinides are introduced. The extraction of uranium, plutonium and fission products that are involved in spent nuclear fuel reprocessing is also reviewed. The possible extraction mechanisms are discussed. Finally, the prospect of replacement of volatile and/or toxic organic solvents with environmentally benign ionic liquids for solvent extraction and the potency of applications of ionic liquids in solvent extraction are also commented. (authors)

  13. Liquid to liquid extraction and liquid chromatography-tandem mass spectrometry determination of hainanmycin in feed.

    Science.gov (United States)

    Wang, Ze Ping; Shen, Jian Zhong; Linhardt, Robert J; Jiang, Hui; Cheng, Lin Li

    2017-03-01

    Hainanmycin is a new veterinary polyether antibiotic and has few sensitive analytical method in present days. In this study, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) relying on multiple reaction monitoring (MRM) detection was developed for analysis of hainanmycin in animal feed. Feed samples were extracted with ethyl acetate and purified by two steps of liquid-liquid extraction (LLE) to get rid of water solvable matrix and lipids one by one. The final simple was analyzed by LC-MS/MS. The LC mobile phase was composed of 0.1% aqueous formic acid and 0.1% formic acidified acetonitrile by gradient elution. Average recoveries ranged from 74.22% to 87.85%, as determined by spiking with 2.0 (LOQ) ∼2500μgkg -1 of hainanmycin. The inter-day and intra-day coefficient of variation was 9.21% to 11.77% and 7.67% to 13.49%, respectively. The limit of detection (LOD) and the limit of quantitation (LOQ) were 0.36μgkg -1 and 2.0μgkg -1 , respectively. Copyright © 2016. Published by Elsevier B.V.

  14. Novel thiosalicylate-based ionic liquids for heavy metal extractions

    Energy Technology Data Exchange (ETDEWEB)

    Leyma, Raphlin; Platzer, Sonja [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, A-1090 Vienna (Austria); Jirsa, Franz [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, A-1090 Vienna (Austria); Department of Zoology, University of Johannesburg, PO Box 524, Auckland Park, 2006, Johannesburg (South Africa); Kandioller, Wolfgang, E-mail: wolfgang.kandioller@univie.ac.at [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, A-1090 Vienna (Austria); Krachler, Regina; Keppler, Bernhard K. [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, A-1090 Vienna (Austria)

    2016-08-15

    Highlights: • Six thiosalicylate-based ammonium and phosphonium ionic liquids (ILs) were newly synthesized. • ILs showed good extraction of cadmium, copper, and zinc. • Phosphonium ILs showed better extraction efficiencies than their ammonium counterparts. - Abstract: This study aims to develop novel ammonium and phosphonium ionic liquids (ILs) with thiosalicylate (TS) derivatives as anions and evaluate their extracting efficiencies towards heavy metals in aqueous solutions. Six ILs were synthesized, characterized, and investigated for their extracting efficacies for cadmium, copper, and zinc. Liquid-liquid extractions of Cu, Zn, or Cd with ILs after 1–24 h using model solutions (pH 7; 0.1 M CaCl{sub 2}) were assessed using flame atomic absorption spectroscopy (F-AAS). Phosphonium-based ILs trihexyltetradecylphosphonium 2-(propylthio)benzoate [P{sub 66614}][PTB] and 2-(benzylthio)benzoate [P{sub 66614}][BTB] showed best extraction efficiency for copper and cadmium, respectively and zinc was extracted to a high degree by [P{sub 66614}][BTB] exclusively.

  15. Extraction of toluene from aliphatic compounds using an ionic liquid as solvent: Influence of the alkane on the (liquid + liquid) equilibrium

    International Nuclear Information System (INIS)

    Gonzalez, Emilio J.; Calvar, Noelia; Dominguez, Irene; Dominguez, Angeles

    2011-01-01

    Research highlights: → An ionic liquid was analyzed as solvent for extraction of toluene from alkanes. → Liquid-liquid equilibrium data were measured at 298.15 K and atmospheric pressure. → Selectivity and solute distribution ratio were obtained and compared with literature. → The Othmer-Tobias equation was used to ascertain the experimental LLE data. → Experimental data were correlated using NRTL and UNIQUAC models. - Abstract: In this paper, the feasibility of using 1-ethyl-3-methylimidazolium ethylsulfate ionic liquid, [EMim][ESO 4 ], as solvent for the extraction of toluene from aliphatic compounds (hexane, heptane, octane, or nonane) was analyzed. (Liquid + liquid) equilibrium (LLE) data for the ternary systems {alkane (1) + toluene (2) + [EMim][ESO 4 ] (3)} were measured at T = 298.15 K and atmospheric pressure. Selectivity and solute distribution ratio were calculated from the experimental LLE data, and the obtained values were compared to those previously reported using other ionic liquids and sulfolane. The degree of consistency of the experimental LLE data was ascertained using the Othmer-Tobias equation. Finally, the experimental LLE data were satisfactorily correlated with NRTL and UNIQUAC models.

  16. Liquid-liquid extraction assisted by a carbon nanoparticles interface. Electrophoretic determination of atrazine in environmental samples.

    Science.gov (United States)

    Caballero-Díaz, Encarnación; Simonet, Bartolomé; Valcárcel, Miguel

    2013-10-21

    A novel method for the determination of atrazine, using liquid-liquid extraction assisted by a nanoparticles film formed in situ and composed of organic solvent stabilized-carbon nanoparticles, is described. The presence of nanoparticles located at the liquid-liquid interface reinforced the extraction of analyte from matrix prior to capillary electrophoresis (CE) analysis. Some influential experimental variables were optimized in order to enhance the extraction efficiency. The developed procedure confirmed that carbon nanoparticles, especially multi-walled carbon nanotubes, are suitable to be used in sample treatment processes introducing new mechanisms of interaction with the analyte. The application of the proposed preconcentration method followed by CE detection enabled the determination of atrazine in spiked river water providing acceptable RSD values (11.6%) and good recoveries (about 87.0-92.0%). Additionally, a similar extraction scheme was tested in soil matrices with a view to further applications in real soil samples.

  17. Homogeneous Liquid–Liquid Extraction of Rare Earths with the Betaine—Betainium Bis(trifluoromethylsulfonyl)imide Ionic Liquid System

    Science.gov (United States)

    Hoogerstraete, Tom Vander; Onghena, Bieke; Binnemans, Koen

    2013-01-01

    Several fundamental extraction parameters such as the kinetics and loading were studied for a new type of metal solvent extraction system with ionic liquids. The binary mixture of the ionic liquid betainium bis(trifluoromethylsulfonyl)imide and water shows thermomorphic behavior with an upper critical solution temperature (UCST), which can be used to avoid the slower mass transfer due to the generally higher viscosity of ionic liquids. A less viscous homogeneous phase and mixing on a molecular scale are obtained when the mixture is heated up above 55 °C. The influence of the temperature, the heating and cooling times, were studied for the extraction of neodymium(III) with betaine. A plausible and equal extraction mechanism is proposed in bis(trifluoromethylsulfonyl)imide, nitrate, and chloride media. After stripping of the metals from the ionic liquid phase, a higher recovery of the ionic liquid was obtained by salting-out of the ionic liquid fraction lost by dissolution in the aqueous phase. The change of the upper critical solution temperature by the addition of HCl or betaine was investigated. In addition, the viscosity was measured below and above the UCST as a function of the temperature. PMID:24169434

  18. Liquid-liquid reductive extraction in molten fluoride salt/liquid aluminium as a core of process for the An/Ln group separation

    International Nuclear Information System (INIS)

    Conocar, O.

    2007-06-01

    This report concerns a pyrochemical process based on liquid-liquid extraction in a molten fluoride/liquid aluminium system as a core process for actinide (An)/lanthanide (Ln) group separation, studied at CEA. The basic and demonstrative experiments have established the feasibility of the An/Ln group separation in the molten fluoride/liquid aluminium system (U, Pu, Np, Am, Cm traces from Nd, Ce, Eu, Sm, Eu, La - An/Ln separation factors over 1000 - An recovery yield over 98 % in one batch). The main experimental efforts must now be targeted on the recovery of actinides from the Al matrix. A thermodynamic and bibliographical survey has been done. It shows that back-extraction in a molten chloride melt could be a promising technique for this purpose

  19. Liquid-liquid reductive extraction in molten fluoride salt/liquid aluminium as a core of process for the An/Ln group separation

    Energy Technology Data Exchange (ETDEWEB)

    Conocar, O

    2007-06-15

    This report concerns a pyrochemical process based on liquid-liquid extraction in a molten fluoride/liquid aluminium system as a core process for actinide (An)/lanthanide (Ln) group separation, studied at CEA. The basic and demonstrative experiments have established the feasibility of the An/Ln group separation in the molten fluoride/liquid aluminium system (U, Pu, Np, Am, Cm traces from Nd, Ce, Eu, Sm, Eu, La - An/Ln separation factors over 1000 - An recovery yield over 98 % in one batch). The main experimental efforts must now be targeted on the recovery of actinides from the Al matrix. A thermodynamic and bibliographical survey has been done. It shows that back-extraction in a molten chloride melt could be a promising technique for this purpose.

  20. Advancing liquid/liquid extraction through a novel microfluidic device: Theory, instrumentation and applications in gas chromatography

    NARCIS (Netherlands)

    Peroni, D.; van Egmond, W.; Kok, W.T.; Janssen, J.G.M.

    2012-01-01

    A new chip-based liquid-liquid extraction technique for sample preparation of aqueous samples for GC was developed. Extraction is performed in a segmented flow system with additional mixing provided by an etched channel structure. The dimensions of the device are optimized to allow benefiting of the

  1. SYNTHESE D’EXTRACTANTS ACIDES HEXADECYL- ET DECYLAMINOBIMETHYLENEDIPHOSPHONIQUES APPLICATION A L’EXTRACTION LIQUIDE-LIQUIDE DE Ni (II

    Directory of Open Access Journals (Sweden)

    M.A DIDI

    2007-06-01

    Après purification puis caractérisation des produits, nous avons réalisé divers tests d’extraction liquide - liquide de Ni (II en milieu sulfaté. Le temps d’équilibre déterminé par étude cinétique a été fixé à 40 minutes. Les paramètres changeant tels la température ( T = 20°C, 30°C et 50°C, le rapport du nombre de moles (n extractant / n métal (Q =1 à 6 et le rapport des volumes (Vaq / Vorg= 1, 2, 3 et 4 ont permis de maximiser le rendement d’extraction qui est de 46% avec le HABMP et de 44% pour le DADMP et ceci pour des extractions à un seul plateau.

  2. Separation of phosphorous by liquid-liquid extraction for the measurement of 32P

    International Nuclear Information System (INIS)

    Lee, H.N.; Yang, S.D.

    2010-01-01

    Phosphorous containing radioisotope waste was separated and determined by liquid-liquid extraction method through liquid scintillation counter (LSC). In this process, ammonium phosphate was converted to phosphomolybdate (PMo) by the reaction of ammonium molybdate (Mo) in HCl solution (0.02 M) and maximum UV/VIS absorbance (λ max ) 218 nm was observed. The PMo solution was extracted with TOA (Tri-n-Octylamine)/xylene mixture and λ max 290 nm was found for this organic layer. Absorbance of aqueous and organic layer was linear through concentration. The impurities such as Co, Cr, Gd, etc. remain in aqueous layer by treating with Mo which was determined by ICP-AES and AAS. The quenching correction curve for 32 P was calculated using LSC results. No counting change was observed as the volume of quenchers increased. The recovery was 98% and 81% for the extraction and separation process from the test using H 3 32 PO 4 as standard tracer. (author)

  3. Counter current 'emulsion flow' extractor for continuous liquid-liquid extraction from suspended solutions

    International Nuclear Information System (INIS)

    Yanase, Nobuyuki; Naganawa, Hirochika; Nagano, Tetsushi; Noro, Junji

    2011-01-01

    A single current 'emulsion flow' liquid-liquid extraction apparatus has a head with a number of holes from which micrometer-sized droplets of an aqueous phase spout into an organic phase to mix the two liquid phases. For practical use, however, a fatal problem can occur when particulate components in the aqueous phase plug the holes. In the present study, we have succeeded in solving the problem by applying a counter current-type emulsion flow extractor where micrometer-sized droplets of the organic phase are generated. (author)

  4. Miniaturized preconcentration methods based on liquid-liquid extraction and their application in inorganic ultratrace analysis and speciation: A review

    International Nuclear Information System (INIS)

    Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

    2009-01-01

    Liquid-liquid extraction (LLE) is widely used as a pre-treatment technique for separation and preconcentration of both organic and inorganic analytes from aqueous samples. Nevertheless, it has several drawbacks, such as emulsion formation or the use of large volumes of solvents, which makes LLE expensive and labour intensive. Therefore, miniaturization of conventional liquid-liquid extraction is needed. The search for alternatives to the conventional LLE using negligible volumes of extractant and the minimum number of steps has driven the development of three new miniaturized methodologies, i.e. single-drop microextraction (SDME), hollow fibre liquid-phase microextraction (HF-LPME) and dispersive liquid-liquid microextraction (DLLME). The aim of this paper is to provide an overview of these novel preconcentration approaches and their potential use in analytical labs involved in inorganic (ultra)trace analysis and speciation. Relevant applications to the determination of metal ions, metalloids, organometals and non-metals are included

  5. Extractive behavior of U(VI) in the paraffin soluble ionic liquid

    International Nuclear Information System (INIS)

    Rama, R.; Kumaresan, R.; Venkatesan, K.A.; Antony, M.P.; Vasudeva Rao, P.R.

    2013-01-01

    An Aliquat-336 based ionic liquid namely, tri-n-octylmethylammonium bis(2-ethylhexyl)phosphate ((A3636) + (DEHP) - ) was prepared and studied for the extraction of U(VI) from nitric acid medium. Since the ionic liquid, (A336) + (DEHP) - , was miscible in n-dodecane (n-DD), the extraction of U(VI) in the solution of tri-n-butylphosphate (TBP) in n-DD, was investigated in the presence of small concentrations of ionic liquid. The distribution ratio of U(VI) in 0.3 M (A336) + (DEHP) - /n-DD decreased with increase in the concentration of nitric acid. The effect of concentration of TBP, ionic liquid nitric acid and nitrate ion on the extraction of U(VI) in ionic liquid medium was studied. The mechanistic aspect of extraction was investigated by the slope analysis of the extraction data. The studies indicated the feasibility of modifying the extractive properties of U(VI) in TBP/n-DD using ionic liquid. (author)

  6. Trace hydrogen extraction from liquid lithium tin alloy

    International Nuclear Information System (INIS)

    Xie Bo; Hu Rui; Xie Shuxian; Weng Kuiping

    2010-01-01

    In order to finish the design of tritium extraction system (TES) of fusion fission hybrid reactor (FFHR) tritium blanket, involving the dynamic mathematical model of liquid metal in contact with a gaseous atmosphere, approximate mathematical equation of tritium in lithium tin alloy was deduced. Moreover, carrying process used for trace hydrogen extraction from liquid lithium tin alloy was investigated with hydrogen being used to simulate tritium in the study. The study results indicate that carrying process is effective way for hydrogen extraction from liquid lithium tin alloy, and the best flow velocity of carrier gas is about 4 L/min under 1 kg alloy temperatures and carrying numbers are the main influencing factors of hydrogen number. Hydrogen extraction efficiency can reach 85% while the alloy sample is treated 6 times at 823 K. (authors)

  7. Rational approach to solvent system selection for liquid-liquid extraction-assisted sample pretreatment in counter-current chromatography.

    Science.gov (United States)

    Wang, Jiajia; Gu, Dongyu; Wang, Miao; Guo, Xinfeng; Li, Haoquan; Dong, Yue; Guo, Hong; Wang, Yi; Fan, Mengqi; Yang, Yi

    2017-05-15

    A rational liquid-liquid extraction approach was established to pre-treat samples for high-speed counter-current chromatography (HSCCC). n-Hexane-ethyl acetate-methanol-water (4:5:4:5, v/v) and (1:5:1:5, v/v) were selected as solvent systems for liquid-liquid extraction by systematically screening K of target compounds to remove low- and high-polarity impurities in the sample, respectively. After liquid-liquid extraction was performed, 1.4g of crude sample II was obtained from 18.5g of crude sample I which was extracted from the flowers of Robinia pseudoacacia L., and then separated with HSCCC by using a solvent system composed of n-hexane-ethyl acetate-methanol-water (1:2:1:2, v/v). As a result, 31mg of robinin and 37mg of kaempferol 7-O-α-l-rhamnopyranoside were isolated from 200mg of crude sample II in a single run of HSCCC. A scale-up separation was also performed, and 160mg of robinin with 95% purity and 188mg of kaempferol 7-O-α-l-rhamnopyranoside with 97% purity were produced from 1.2g of crude sample II. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Mixing-settling apparatus for liquid-liquid extraction

    International Nuclear Information System (INIS)

    Skolokin, L.I.; Leif, V.E.; Sednev, J.M.

    1989-01-01

    A mixing-settling apparatus for liquid-liquid extraction comprises a casing. A first partition is mounted along its longitudinal axis and above an overflow device. The mixing device is connected to a means of feeding at least one of the phases and is shaped as at least one hollow element mounted essentially perpendicularly to the longitudinal axis of the casing. The walls of the hollow element are provided with openings, the outlet cross-sections of which are directed to the first partition. The first partition is provided with a means for regulating the height of the layer of the mixed phases M in the mixing zone, said means being located in the partition at the point most distant from the means for feeding phases L, S in the longitudinal direction. A second transporting device is mounted in the settling zone. It is fixed on to the casing and is located after the overflow device in the direction of movement of the light phase l. (author) 10 figs

  9. Ionic-liquid-based dispersive liquid-liquid microextraction combined with magnetic solid-phase extraction for the determination of aflatoxins B1 , B2 , G1 , and G2 in animal feeds by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Zhao, Jiao; Zhu, Yan; Jiao, Yang; Ning, Jinyan; Yang, Yaling

    2016-10-01

    A novel two-step extraction technique combining ionic-liquid-based dispersive liquid-liquid microextraction with magnetic solid-phase extraction was developed for the preconcentration and separation of aflatoxins in animal feedstuffs before high-performance liquid chromatography coupled with fluorescence detection. In this work, ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate was used as the extractant in dispersive liquid-liquid microextraction, and hydrophobic pelargonic acid modified Fe 3 O 4 magnetic nanoparticles as an efficient adsorbent were applied to retrieve the aflatoxins-containing ionic liquid. Notably, the target of magnetic nanoparticles was the ionic liquid rather than the aflatoxins. Because of the rapid mass transfer associated with the dispersive liquid-liquid microextraction and magnetic solid phase steps, fast extraction could be achieved. The main parameters affecting the extraction recoveries of aflatoxins were investigated and optimized. Under the optimum conditions, vortexing at 2500 rpm for 1 min in the dispersive liquid-liquid microextraction and magnetic solid-phase extraction and then desorption by sonication for 2 min with acetonitrile as eluent. The recoveries were 90.3-103.7% with relative standard deviations of 3.2-6.4%. Good linearity was observed with correlation coefficients ranged from 0.9986 to 0.9995. The detection limits were 0.632, 0.087, 0.422 and 0.146 ng/mL for aflatoxins B 1 , B2, G1, and G2, respectively. The results were also compared with the pretreatment method carried out by conventional immunoaffinity columns. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Liquid-liquid extraction of plutonium and americium by cekanoic acid from alkaline medium

    International Nuclear Information System (INIS)

    Venugopal Chetty, K.; Sagar, V.; Swarup, R.

    2001-01-01

    Liquid-liquid extraction studies of plutonium and americium from aqueous carbonate medium using a high molecular weight carboxylic acid namely cekanoic acid in different diluents has been carried out. The distribution ratio (D) values for Pu(IV) and Am(III) under various parameters such as concentration of extractant, Na 2 CO 3 and initial pH were obtained. Results indicated that Pu(IV) and Am(III) could be satisfactorily extracted together or individually from aqueous carbonate medium using cekanoic acid in different diluents like carbon tetrachloride, cyclohexane, toluene, n-dodecane or solvesso-100. The D values for Pu(IV) and Am(III) also indicated the possibility of their mutual separation. The back extraction of Pu and Am with different reagents was also studied. (orig.)

  11. Literature Review: Crud Formation at the Liquid/Liquid Interface of TBP-Based Solvent-Extraction Processes

    Energy Technology Data Exchange (ETDEWEB)

    Delegard, Calvin H.; Casella, Amanda J.

    2016-09-30

    This report summarizes the literature reviewed on crud formation at the liquid:liquid interface of solvent extraction processes. The review is focused both on classic PUREX extraction for industrial reprocessing, especially as practiced at the Hanford Site, and for those steps specific to plutonium purification that were used at the Plutonium Reclamation Facility (PRF) within the Plutonium Finishing Plant (PFP) at the Hanford Site.

  12. Functionalized ionic liquids: new agents for the extraction of actinides/lanthanides

    International Nuclear Information System (INIS)

    Ouadi, A.; Hesemann, P.; Billard, I.; Gaillard, C.; Gadenne, B.; Moreau, Joel J.E; Moutiers, G.; Mariet, C.; Labet, A.

    2004-01-01

    The potentialities of hydrophobic ionic liquids BumimPF 6 and BumimTf 2 N for their use in the nuclear fuel cycle were investigated, in particular for the liquid liquid extraction. We demonstrate that the use of RTILs in replacement of the organic diluents for actinides partitioning is promising. In our contribution, we present the synthesis of several task-specific ionic liquids. Our results show that grafting metal complexing groups increases the affinity of metals to the IL phase and gives rise to suitable media for the liquid-liquid extraction of actinides. (authors)

  13. Development of a new extraction method based on counter current salting-out homogenous liquid-liquid extraction followed by dispersive liquid-liquid microextraction: Application for the extraction and preconcentration of widely used pesticides from fruit juices.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Feriduni, Behruz; Mogaddam, Mohammad Reza Afshar

    2016-01-01

    In this paper, a new extraction method based on counter current salting-out homogenous liquid-liquid extraction (CCSHLLE) followed by dispersive liquid-liquid microextraction (DLLME) has been developed for the extraction and preconcentration of widely used pesticides in fruit juice samples prior to their analysis by gas chromatography-flame ionization detection (GC-FID). In this method, initially, sodium chloride as a separation reagent is filled into a small column and a mixture of water (or fruit juice) and acetonitrile is passed through the column. By passing the mixture sodium chloride is dissolved and the fine droplets of acetonitrile are formed due to salting-out effect. The produced droplets go up through the remained mixture and collect as a separated layer. Then, the collected organic phase (acetonitrile) is removed with a syringe and mixed with 1,1,2,2-tetrachloroethane (extraction solvent at µL level). In the second step, for further enrichment of the analytes the above mixture is injected into 5 mL de-ionized water placed in a test tube with conical bottom in order to dissolve acetonitrile into water and to achieve a sedimented phase at µL-level volume containing the enriched analytes. Under the optimal extraction conditions (extraction solvent, 1.5 mL acetonitrile; pH, 7; flow rate, 0.5 mL min(-1); preconcentration solvent, 20 µL 1,1,2,2-tetrachloroethane; NaCl concentration; 5%, w/w; and centrifugation rate and time, 5000 rpm and 5 min, respectively), the extraction recoveries and enrichment factors ranged from 87% to 96% and 544 to 600, respectively. Repeatability of the proposed method, expressed as relative standard deviations, ranged from 2% to 6% for intra-day (n=6, C=250 or 500 µg L(-1)) and inter-days (n=4, C=250 or 500 µg L(-1)) precisions. Limits of detection are obtained between 2 and 12 µg L(-1). Finally, the proposed method is applied for the determination of the target pesticide residues in the juice samples. Copyright © 2015

  14. A validated solid-liquid extraction method for the HPLC determination of polyphenols in apple tissues Comparison with pressurised liquid extraction.

    Science.gov (United States)

    Alonso-Salces, Rosa M; Barranco, Alejandro; Corta, Edurne; Berrueta, Luis A; Gallo, Blanca; Vicente, Francisca

    2005-02-15

    A solid-liquid extraction procedure followed by reversed-phase high-performance liquid chromatography (RP-HPLC) coupled with a photodiode array detector (DAD) for the determination of polyphenols in freeze-dried apple peel and pulp is reported. The extraction step consists in sonicating 0.5g of freeze-dried apple tissue with 30mL of methanol-water-acetic acid (30:69:1, v/v/v) containing 2g of ascorbic acid/L, for 10min in an ultrasonic bath. The whole method was validated, concluding that it is a robust method that presents high extraction efficiencies (peel: >91%, pulp: >95%) and appropriate precisions (within day: R.S.D. (n = 5) <5%, and between days: R.S.D. (n = 5) <7%) at the different concentration levels of polyphenols that can be found in apple samples. The method was compared with one previously published, consisting in a pressurized liquid extraction (PLE) followed by RP-HPLC-DAD determination. The advantages and disadvantages of both methods are discussed.

  15. Selective extraction of emerging contaminants from water samples by dispersive liquid-liquid microextraction using functionalized ionic liquids.

    Science.gov (United States)

    Yao, Cong; Li, Tianhao; Twu, Pamela; Pitner, William R; Anderson, Jared L

    2011-03-25

    Functionalized ionic liquids containing the tris(pentafluoroethyl)trifluorophosphate (FAP) anion were used as extraction solvents in dispersive liquid-liquid microextraction (DLLME) for the extraction of 14 emerging contaminants from water samples. The extraction efficiencies and selectivities were compared to those of an in situ IL DLLME method which uses an in situ metathesis reaction to exchange 1-butyl-3-methylimidazolium chloride (BMIM-Cl) to 1-butyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide (BMIM-NTf(2)). Compounds containing tertiary amine functionality were extracted with high selectivity and sensitivity by the 1-(6-amino-hexyl)-1-methylpyrrolidinium tris(pentafluoroethyl)trifluorophosphate (HNH(2)MPL-FAP) IL compared to other FAP-based ILs and the BMIM-NTf(2) IL. On the other hand, polar or acidic compounds without amine groups exhibited higher enrichment factors using the BMIM-NTf(2) IL. The detection limits for the studied analytes varied from 0.1 to 55.1 μg/L using the traditional IL DLLME method with the HNH(2)MPL-FAP IL as extraction solvent, and from 0.1 to 55.8 μg/L using in situ IL DLLME method with BMIM-Cl+LiNTf(2) as extraction solvent. A 93-fold decrease in the detection limit of caffeine was observed when using the HNH(2)MPL-FAP IL compared to that obtained using in situ IL DLLME method. Real water samples including tap water and creek water were analyzed with both IL DLLME methods and yielded recoveries ranging from 91% to 110%. Copyright © 2011 Elsevier B.V. All rights reserved.

  16. Cone-shaped membrane liquid phase micro extraction

    International Nuclear Information System (INIS)

    Hong, Heng See; Sanagi, M.M.; Ibrahim, W.A.W.; Naim, A.A.

    2008-01-01

    A novel sample pre-treatment technique termed cone-shaped membrane liquid phase micro extraction (CSM-LPME) was developed and combined with micro-liquid chromatography (micro-LC) for the determination of selected pesticides in water samples. Several important extraction parameters such as types of extraction solvent, agitation rate, pH value, total exposure time and effect of salt and humic acids were investigated and optimized. Enrichment factors of >50 folds were easily achieved within 20 min of extraction. The new developed method demonstrated an excellent performance in terms of speed, cost effectiveness, reproducibility, as well as exceptional low detection limits. Current work provides a great interest to further investigate on the applicability of the CSM-LPME technique in analytical chemistry and explores the possibility of replacing conventional extraction techniques such as soxhlet, solid phase extraction (SPE) and solid phase micro extraction (SPME). (author)

  17. Combination of solvent extractants for dispersive liquid-liquid microextraction of fungicides from water and fruit samples by liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Pastor-Belda, Marta; Garrido, Isabel; Campillo, Natalia; Viñas, Pilar; Hellín, Pilar; Flores, Pilar; Fenoll, José

    2017-10-15

    A multiresidue method was developed to determine twenty-five fungicides belonging to three different chemical families, oxazoles, strobilurins and triazoles, in water and fruit samples, using dispersive liquid-liquid microextraction (DLLME) and liquid chromatography/tandem mass spectrometry (LC-MS 2 ). Solid-liquid extraction with acetonitrile was used for the analysis in fruits, the extract being used as dispersant solvent in DLLME. Since some of the analytes showed high affinity for chloroform and the others were more efficiently extracted with undecanol, a mixture of both solvents was used as extractant in DLLME. After evaporation of CHCl 3 , the enriched phase was analyzed. Enrichment factors in the 23-119 and 12-60 ranges were obtained for waters and fruits, respectively. The approach was most sensitive for metominostrobin with limits of quantification of 1ngL -1 and 5ngkg -1 in waters and fruits, respectively, while a similar sensitivity was attained for tebuconazole in fruits. Recoveries of the fungicides varied between 86 and 116%. Copyright © 2017 Elsevier Ltd. All rights reserved.

  18. The method for simultaneous extraction and back extraction in liquid three-phase system and equipment for simultaneous extraction and back extraction in liquid three-phase system

    International Nuclear Information System (INIS)

    Palyska, W.; Chmielewski, A.G.

    1992-01-01

    The method for simultaneous extraction and back extraction in liquid three-phase system has been worked out. The equipment designed for that process has been also subject of the patent. The interesting component is extracted first to intermediate phase consists of magnetic solvent keeping two extracting phases separately. The intermediate magnetic liquid has been kept in its position using a stable magnet maintained on the surface of the extraction vessel. Then the component pass from intermediate phase to the third phase as a result of back extraction. Mixing in the extraction and back extraction zones is organized by means of rotating shaft going along the whole apparatus. The extraction and back extraction processes occur simultaneously as a result of continuous flow of solvent in their zones. The single extraction back extraction facilities can be joined in larger batteries. 3 figs

  19. Predictive model for ionic liquid extraction solvents for rare earth elements

    International Nuclear Information System (INIS)

    Grabda, Mariusz; Oleszek, Sylwia; Panigrahi, Mrutyunjay; Kozak, Dmytro; Shibata, Etsuro; Nakamura, Takashi; Eckert, Franck

    2015-01-01

    The purpose of our study was to select the most effective ionic liquid extraction solvents for dysprosium (III) fluoride using a theoretical approach. Conductor-like Screening Model for Real Solvents (COSMO-RS), based on quantum chemistry and the statistical thermodynamics of predefined DyF 3 -ionic liquid systems, was applied to reach the target. Chemical potentials of the salt were predicted in 4,400 different ionic liquids. On the base of these predictions set of ionic liquids’ ions, manifesting significant decrease of the chemical potentials, were selected. Considering the calculated physicochemical properties (hydrophobicity, viscosity) of the ionic liquids containing these specific ions, the most effective extraction solvents for liquid-liquid extraction of DyF 3 were proposed. The obtained results indicate that the COSMO-RS approach can be applied to quickly screen the affinity of any rare earth element for a large number of ionic liquid systems, before extensive experimental tests

  20. Removal of actinide elements from liquid scintillation cocktail wastes using liquid-liquid extraction and demulsification techniques

    International Nuclear Information System (INIS)

    Foltz, K.; Landsberger, S.; Srinivasan, B.; Vandegrift, G.F.

    1994-01-01

    For many years liquid scintillation cocktail (LSC) wastes have been generated and stored at Argonne National Laboratory (ANL). These wastes are stored in thousands of 10--20 m scintillation vials, many of which contain elements with Z > 88. Because storage space is limited, disposal of this waste is pressing. These wastes could be commercially incinerated if the radionuclides with Z>88 are reduced to sufficiently low levels. However, there is currently no deminimus level for these radionuclides, and separation techniques are still being tested. The University of Illinois is conducting experiments to separate radionuclides with Z > 88 from simulated LSC wastes by using liquid-liquid extraction (LLX) and demulsification techniques. The actinide elements are removed from the LSC by extraction into an aqueous phase after the cocktail has been demulsified. The aqueous and organic phases are separated and the organic phase, now free from radionuclides with Z > 88, can be sent to a commercial incineration facility. The aqueous phase may be treated and disposed of using existing techniques. The LLX separation techniques used solutions of sodium oxalate, aluminum nitrate, and tetrasodium EDTA at varying concentrations. These extractants were mixed with the simulated waste in a 1:1 volume ratio. Using 1.0M Na 4 EDTA salt solutions, decontamination ratios as high as 230 were achieved

  1. Recovery of Steroidal Alkaloids from Potato Peels Using Pressurized Liquid Extraction

    Directory of Open Access Journals (Sweden)

    Mohammad B. Hossain

    2015-05-01

    Full Text Available A higher yield of glycoalkaloids was recovered from potato peels using pressurized liquid extraction (1.92 mg/g dried potato peels compared to conventional solid–liquid extraction (0.981 mg/g dried potato peels. Response surface methodology deduced the optimal temperature and extracting solvent (methanol for the pressurized liquid extraction (PLE of glycoalkaloids as 80 °C in 89% methanol. Using these two optimum PLE conditions, levels of individual steroidal alkaloids obtained were of 597, 873, 374 and 75 µg/g dried potato peel for α-solanine, α-chaconine, solanidine and demissidine respectively. Corresponding values for solid liquid extraction were 59%, 46%, 40% and 52% lower for α-solanine, α-chaconine, solanidine and demissidine respectively.

  2. Design of guanidinium ionic liquid based microwave-assisted extraction for the efficient extraction of Praeruptorin A from Radix peucedani.

    Science.gov (United States)

    Ding, Xueqin; Li, Li; Wang, Yuzhi; Chen, Jing; Huang, Yanhua; Xu, Kaijia

    2014-12-01

    A series of novel tetramethylguanidinium ionic liquids and hexaalkylguanidinium ionic liquids have been synthesized based on 1,1,3,3-tetramethylguanidine. The structures of the ionic liquids were confirmed by (1)H NMR spectroscopy and mass spectrometry. A green guanidinium ionic liquid based microwave-assisted extraction method has been developed with these guanidinium ionic liquids for the effective extraction of Praeruptorin A from Radix peucedani. After extraction, reversed-phase high-performance liquid chromatography with UV detection was employed for the analysis of Praeruptorin A. Several significant operating parameters were systematically optimized by single-factor and L9 (3(4)) orthogonal array experiments. The amount of Praeruptorin A extracted by [1,1,3,3-tetramethylguanidine]CH2CH(OH)COOH is the highest, reaching 11.05 ± 0.13 mg/g. Guanidinium ionic liquid based microwave-assisted extraction presents unique advantages in Praeruptorin A extraction compared with guanidinium ionic liquid based maceration extraction, guanidinium ionic liquid based heat reflux extraction and guanidinium ionic liquid based ultrasound-assisted extraction. The precision, stability, and repeatability of the process were investigated. The mechanisms of guanidinium ionic liquid based microwave-assisted extraction were researched by scanning electron microscopy and IR spectroscopy. All the results show that guanidinium ionic liquid based microwave-assisted extraction has a huge potential in the extraction of bioactive compounds from complex samples. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Determination of methylphenidate in Calliphorid larvae by liquid-liquid extraction and liquid chromatography mass spectrometry - Forensic entomotoxicology using an in vivo rat brain model

    DEFF Research Database (Denmark)

    Bushby, Sarah K.; Thomas, Nicky; Priemel, Petra A.

    2012-01-01

    and Calliphorid larvae) by liquid-liquid extraction with recovery of >80%, and quantified using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The LC-MS/MS assay was validated for entomotoxicological use and initially applied to male Sprague-Dawley rats (n=6) that were dosed with MPH (20mg/kg) ante...

  4. Determination of Gemfibrozil (Lipitor and Lopid in Water, Biological Fluids and Drug Matrix by Dispersive Liquid-Liquid micro Extraction (DLLME and Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Ghorbani A.

    2014-07-01

    Full Text Available In this study Dispersive liquid-liquid micro extraction (DLLME coupled with High performance liquid chromatography was applied for the determination of Gemfibrozil in water, drug`s matrix and biological liquids (human plasma and urine. In this method, the appropriate mixture of extraction solvent (200 μl chlorophorm and disperser solvent (1 ml methanol are injected rapidly into the aqueous sample (10.0 ml by syringe, cloudy solution is formed that consisted of fine particles of extraction solvent which is dispersed entirely into aqueous phase. The mixture was centrifuged and the extraction solvent is sedimented on the bottom of the conical test tube. 50 μl of the sedimented phase is puted in a vial and it`s solvent is evaporated. Then 1ml methanol injected to vial and 20 μL of it injected into the HPLC for separation and determination of Gemfibrozil. Some important parameters, such as kind of extraction and disperser solvent, volume of them, extraction time, pH and ionic strength of the aqueous feed solution were optimized. Under the optimum conditions, the enrichment factors and extraction recoveries were 10 and 93.64%. The linear range was (0.1-100.0 mgl-1, limit of detection was 12.3 mgl-1. The relative standard deviations (RSD for 2 mgl-1 of Gemfibrozil in water were 1.3%, (n=10.

  5. Hollow fiber-based liquid-liquid-liquid micro-extraction with osmosis: II. Application to quantification of endogenous gibberellins in rice plant.

    Science.gov (United States)

    Wu, Qian; Wu, Dapeng; Duan, Chunfeng; Shen, Zheng; Guan, Yafeng

    2012-11-23

    The phenomenon and benefits of osmosis in hollow fiber-based liquid-liquid-liquid micro-extraction (HF-LLLME) were theoretically discussed in part I of this study. In this work, HF-LLLME with osmosis was coupled with high performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-triple quadrupole MS/MS) to analyze eight gibberellins (gibberellin A(1), gibberellin A(3), gibberellin A(4), gibberellin A(7), gibberellin A(8), gibberellin A(9), gibberellin A(19) and gibberellin A(20)) in rice plant samples. According to the theory of HF-LLLME with osmosis, single factor experiments, orthogonal design experiments and mass transfer simulation of extraction process were carried out to select the optimal conditions. Cyclohexanol - n-octanol (1:3, v/v) was selected as organic membrane. Donor phase of 12 mL was adjusted to pH 2 and 20% NaCl (w/v) was added. Acceptor phase with an initial volume of 20 μL was the solution of 0.12 mol L(-1) Na(2)CO(3)-NaHCO(3) buffer (pH 9). Temperature was chosen to be 30 °C and extraction time was selected to be 90 min. Under optimized conditions, this method provided good linearity (r, 0.99552-0.99991) and low limits of detection (0.0016-0.061 ng mL(-1)). Finally, this method was applied to the analysis of endogenous gibberellins from plant extract which was obtained with traditional solvent extraction of rice plant tissues, and the relative recoveries were from 62% to 166%. Copyright © 2012 Elsevier B.V. All rights reserved.

  6. Evaluation of a novel task specific ionic liquid for actinide ion extraction

    International Nuclear Information System (INIS)

    Paramanik, M.; Ghosh, S.K.; Raut, D.R.; Mohapatra, P.K.

    2016-01-01

    Separation of U and Pu from nuclear waste is of great relevance for a sustainable closed fuel cycle point of view. Spent fuel reprocessing by the well known PUREX process is done world wide for the recovery of U and Pu using TBP as the extractant. Room temperature ionic liquids (RTILs) have shown significantly higher extraction of metal ions, particularly at lower acidity as compared to the molecular diluents. Functionalization of ionic liquids has resulted in highly efficient task specific ionic liquids (TSILs) with superior extraction properties than the analogous extractants dissolved in ionic liquids. The present paper reports the evaluation of a novel task specific ionic liquid (TSIL) containing >P=O functional group for the extraction of actinides like U(VI) and Pu(IV)

  7. Niobium, tantalum and titanium extraction from natural and technogenic raw materials of the Kola Peninsula by liquid-liquid extraction methods

    International Nuclear Information System (INIS)

    Kassikova, N.I.; Kassikov, A.G.; Balabanov, Yu.I.; Petrov, V.B.; Kalinnikov, V.T.

    2003-01-01

    Such rare metals as niobium and tantalum are important strategic materials underlying many of the modern advanced technologies. Since the extraction and processing of rare metal concentrates from own deposits has diminished abruptly in recent years, it is essential to look into the possibility of extracting these elements from various production wastes. This work discusses liquid-liquid extraction and purification of niobium, tantalum and titanium from process solutions of loparite, perovskite and sphene concentrate decomposition with sulphuric and hydrochloric acids; niobium from lithium niobate production wastes decomposed by hydrochloric acid; and tantalum from tantalum capacitor and heat-resistant alloy wastes. (Original)

  8. Selective solvent extraction of actinides associated to liquid scintillation measurements

    International Nuclear Information System (INIS)

    Ardois, C.; Musikas, C.

    1997-01-01

    The problems associated to radioactive waste disposal have acquired a special attention due, particularly, to the element instability and, consequently, to their lixiviation and to their peculiarities which are essential in the radioactivity penetration in the food chains; the other important parameters are the produced amounts and the noxiousnesses. New commercial liquid scintillation counters allow rapid α/β measurements. Associated with liquid-liquid extraction techniques, rapid and selective actinide analyses are possible. Among various actinide extractants, such as amines or organophosphorus compounds, we were particularly interested in tri-n-octyl-phosphine oxide (TOPO). Uranium, thorium and americium extractions with (TOPO) in toluene have been investigated. A systematic study of the counting parameters of a PACKARD 2550 TR/AB TM liquid scintillation analyzer is under completion

  9. Parallel artificial liquid membrane extraction of acidic drugs from human plasma

    DEFF Research Database (Denmark)

    Roldan-Pijuan, Mercedes; Pedersen-Bjergaard, Stig; Gjelstad, Astrid

    2015-01-01

    The new sample preparation concept “Parallel artificial liquid membrane extraction (PALME)” was evaluated for extraction of the acidic drugs ketoprofen, fenoprofen, diclofenac, flurbiprofen, ibuprofen, and gemfibrozil from human plasma samples. Plasma samples (250 μL) were loaded into individual......-performance liquid chromatography-ultraviolet detection of the individual acceptor solutions. Important PALME parameters including the chemical composition of the liquid membrane, extraction time, and sample pH were optimized, and the extraction performance was evaluated. Except for flurbiprofen, exhaustive...

  10. On-line control of a liquid-liquid extraction column by the modal control method

    International Nuclear Information System (INIS)

    Bonnefoi, P.; Poujol, A.; Zwingelstein, G.; Dargier, C.; Rouyer, H.

    1977-02-01

    The application of modal analysis to the on-line control of a liquid-liquid extraction column is presented. This process is used in reprocessing for U purification. U in the aqueous acid phase is extracted by a solvent flowing at counter-current. The process is described by 4 nonlinear equations and gives the U and acid concentrations in the two phases. An approximative model is established adapted to the control of the column. Some results of a numerical simulation are given when a single mode is controled. They show that a single sensor allows a good control [fr

  11. [Preparation and applications of a supported liquid-liquid extraction column with a composite diatomite material].

    Science.gov (United States)

    Bao, Jianmin; Ma, Zhishuang; Sun, Ying; Wang, Yongzun; Li, Youxin

    2012-08-01

    A rapid and special supported liquid-liquid extraction (SLE) column was developed with a composite diatomite material. The SLE column was evaluated by high performance liquid chromatography (HPLC) with acidic, neutral and alkaline compounds dissolved in water. Furthermore, some real complex samples were also analyzed by HPLC with the SLE method. The recoveries of benzoic acid (acidic), p-nitroaniline (alkaline) and 4-hydroxy-benzoic methyl ester (neutral) treated by the SLE column were 90.6%, 98.1% and 97.7%. However, the recoveries of the three compounds treated by traditional liquid-liquid extraction (LLE) method were 71.9%, 81.9% and 83.9%. The results showed that the SLE technique had higher recoveries than the traditional LLE method. The spiked recoveries of the complex samples, such as benzoic acid in Sprite and dexamethasone acetate, chlorphenamine maleate, indomethacin in bovine serum, were between 80% and 110% and the relative standard deviations (RSDs) were less than 15%. For biological specimen, the results could be accepted. Meantime, many disadvantages associated with traditional LLE method, such as emulsion formation, didn't occur using SLE column. The SLE column technique is a good sample preparation method with many advantages, such as rapid, simple, robust, easily automated, high recovery and high-throughput, which would be widely used in the future.

  12. Studies of extractant molecules in solution and at liquid-liquid interfaces: structural and mechanistic aspects of synergy effects

    International Nuclear Information System (INIS)

    Baaden, Marc

    2000-01-01

    Molecular dynamics simulations reported herein provide new important insights into cation recognition and complexation in solution as well as liquid-liquid extraction, with a particular focus on the microscopic events taking place at the interface between two immiscible liquids. Preliminary studies concerned the representation of the trivalent rare earth cations La 3+ , Eu 3+ and Yb 3+ in force field simulations, probing structural and energetic features on an experimentally characterized model system based on substituted pyridine dicarboxamide ligands. Complexation of such cations by a novel calixarene derivative was investigated showing unexpected features, such as the position of the cation in the complex. Independent experimental studies published subsequently support these findings. Another part of the work is related to industrial liquid-liquid extraction systems using tri-n-butyl phosphate (TBP) as co-solvent, extractant, surfactant and synergist. We investigate 1) concentration effects simulating up to 60 TBP at a water/chloroform interface, 2) acidity using a neutral and ionic model of HNO 3 and 3) synergistic aspects of mixed TBP/calixarene extraction systems. These simulations provide the first microscopic insights into such issues. We finally addressed the topic of solute transfer across the water/chloroform interface. The potential of mean force for such a process has been calculated by both standard methods and novel approaches [fr

  13. Ionic liquid pre-treatment of microalgae and extraction of biomolecules

    NARCIS (Netherlands)

    Desai, Rupali K.

    2016-01-01

    Liquid-liquid extraction (LLE) techniques are widely used in separation primarily due to ease of scale up. Conventional (LLE) systems based on organic solvents are not suitable for extraction of fragile molecules such as proteins as it would result in denaturation. On the other hand aqueous

  14. Solvent extraction of Sr2+ and Cs+ based on hydrophobic protic ionic liquids

    International Nuclear Information System (INIS)

    Luo, Huimin; Yu, Miao; Dai, Sheng

    2007-01-01

    A series of new hydrophobic and protic alkylammonium ionic liquids with bis(trifluoromethylsulfonyl) imide or bis(perfluoroethylsulfonyl)imide as conjugated anions was synthesized in a one-pot reaction with a high yield. In essence our synthesis method involves the combination of neutralization and metathesis reactions. Some of these hydrophobic and protic ionic liquids were liquids at room temperature and therefore investigated as new extraction media for separation of Sr 2+ and Cs + from aqueous solutions. An excellent extraction efficiency was found for some of these ionic liquids using dicyclohexano-18-crown-6 and calix[4]arene-bis(tert-octylbenzo-crown-6) as extractants. The observed enhancement in the extraction efficiency can be attributed to the greater hydrophilicity of the cations of the protic ionic liquids. The application of the protic ionic liquids as new solvent systems for solvent extraction opens up a new avenue in searching for simple and efficient ionic liquids for tailored separation processes. (orig.)

  15. Determination of sulfonamides in butter samples by ionic liquid magnetic bar liquid-phase microextraction high-performance liquid chromatography.

    Science.gov (United States)

    Wu, Lijie; Song, Ying; Hu, Mingzhu; Xu, Xu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

    2015-01-01

    A novel, simple, and environmentally friendly pretreatment method, ionic liquid magnetic bar liquid-phase microextraction, was developed for the determination of sulfonamides in butter samples by high-performance liquid chromatography. The ionic liquid magnetic bar was prepared by inserting a stainless steel wire into the hollow of a hollow fiber and immobilizing ionic liquid in the micropores of the hollow fiber. In the extraction process, the ionic liquid magnetic bars were used to stir the mixture of sample and extraction solvent and enrich the sulfonamides in the mixture. After extraction, the analyte-adsorbed ionic liquid magnetic bars were readily isolated with a magnet from the extraction system. It is notable that the present method was environmentally friendly since water and only several microliters of ionic liquid were used in the whole extraction process. Several parameters affecting the extraction efficiency were investigated and optimized, including the type of ionic liquid, sample-to-extraction solvent ratio, the number of ionic liquid magnetic bars, extraction temperature, extraction time, salt concentration, stirring speed, pH of the extraction solvent, and desorption conditions. The recoveries were in the range of 73.25-103.85 % and the relative standard deviations were lower than 6.84 %. The experiment results indicated that the present method was effective for the extraction of sulfonamides in high-fat content samples.

  16. Thermodynamic equilibrium model to predict the cobalt distribution coefficient in the CoCl2--HCl--H2O--TBP liquid--liquid extraction system

    International Nuclear Information System (INIS)

    Nevarez, M.; Bautista, R.G.

    1976-01-01

    The development of a thermodynamic equilibrium model to predict the cobalt distribution coefficient in the CoCl 2 -HCl-H 2 O-TBP system is described. The model makes use of the various aqueous phase cobaltous chloride complexes stoichiometric stability constants expressed as their degree of formation, their mechanism of extraction into the organic phase, and the equilibrium constant for the extraction reaction. The model was verified by the good agreement between the calculated cobalt distribution coefficients and those obtained experimentally both in the present study and published by other investigators. The optimum extraction of cobalt by the TBP occurred at an HCl equilibrium aqueous place concentration between 8.5 and 9.5M. The development of efficient procedures for the separation and concentration of important industrial metals from their aqueous solutions by liquid-liquid extraction has recently been given impetus by the realization of an impending shortage of energy and mineral resources. Liquid-liquid extraction is one of the few methods by which it is possible to quantitatively separate elements which are similar in properties. The use of liquid-liquid extraction to separate cobalt and nickel, which very frequently occur in nature together, is an important separation problem in nonferrous metallurgy. There is some fundamental information available in the chemical literature regarding the mechanism and equilibrium thermodynamic properties of selected liquid-liquid extraction systems. This research effort shows how this available information can be utilized to improve existing separation and concentration theory and technique. The development and application of a thermodynamic equilibrium model for describing the liquid-liquid extraction of cobaltous chloride from aqueous HCl solutions by tributyl phosphate (TBP) using experimental data obtained in this investigation and from the literature are presented

  17. Screening and quantitative determination of twelve acidic and neutral pharmaceuticals in whole blood by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Simonsen, Kirsten Wiese; Steentoft, Anni; Buck, Maike

    2010-01-01

    . The method was fully validated for salicylic acid, paracetamol, phenobarbital, carisoprodol, meprobamate, topiramate, etodolac, chlorzoxazone, furosemide, ibuprofen, warfarin, and salicylamide. The method also tentatively includes thiopental, theophylline, piroxicam, naproxen, diclophenac, and modafinil......We describe a multi-method for simultaneous identification and quantification of 12 acidic and neutral compounds in whole blood. The method involves a simple liquid-liquid extraction, and the identification and quantification are performed using liquid chromatography-tandem mass spectrometry...

  18. Liquid-liquid extraction to lithium isotope separation based on room-temperature ionic liquids containing 2,2'-binaphthyldiyl-17-crown-5

    International Nuclear Information System (INIS)

    Sun Xiaoli; Zhou Wen; Gu Lin; Qiu Dan; Ren Donghong; Gu Zhiguo; Li Zaijun

    2015-01-01

    A novel liquid-liquid extraction system was investigated for the selective separation of lithium isotopes using ionic liquids (ILs = C 8 mim + PF 6 - , C 8 mim + BF 4 - , and C 8 mim + NTf 2 - ) as extraction solvent and 2,2'-binaphthyldiyl-17-crown-5 (BN-17-5) as extractant. The effects of the concentration of lithium salt, counter anion of lithium salt, initial pH of aqueous phase, extraction temperature, and time on the lithium isotopes separation were discussed. Under optimized conditions, the maximum single-stage separation factor α of 6 Li/ 7 Li obtained in the present study was 1.046 ± 0.002, indicating the lighter isotope 6 Li was enriched in IL phase while the heavier isotope 7 Li was concentrated in the solution phase. The formation of 1:1 complex Li(BN-17-5) + in the IL phase was determined on the basis of slope analysis method. The large value of the free energy change (-ΔG° = 92.89 J mol -1 ) indicated the high separation capability of the Li isotopes by BN-17-5/IL system. Lithium in Li(BN-17-5) + complex was stripped by 1 mol L -1 HCl solution. The extraction system offers high efficiency, simplicity, and green application prospect to lithium isotope separation. (author)

  19. Determination of sedative hypnotics in sewage sludge by pressurized liquid extraction with high-performance liquid chromatography and tandem mass spectrometry.

    Science.gov (United States)

    Arbeláez, Paula; Granados, Judith; Borrull, Francesc; Marcé, Rosa Maria; Pocurull, Eva

    2014-12-01

    This paper describes a method for the determination of eight sedative hypnotics (benzodiazepines and barbiturates) in sewage sludge using pressurized liquid extraction and liquid chromatography with tandem mass spectrometry. Pressurized liquid extraction operating conditions were optimized and maximum recoveries were reached using methanol under the following operational conditions: 100ºC, 1500 psi, extraction time of 5 min, one extraction cycle, flush volume of 60% and purge time of 120 s. Pressurized liquid extraction recoveries were higher than 88% for all the compounds except for carbamazepine (55%). The repeatability and reproducibility between days, expressed as relative standard deviation (n = 5), were lower than 6 and 10%, respectively. The detection limits for all compounds were lower than 12.5 μg/kg of dry weight. The method was applied to determine benzodiazepines and barbiturates in sewage sludge from urban sewage treatment plants, and carbamazepine showed the highest concentration (7.9-18.9 μg/kg dry weight). © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Extraction Equilibrium of Acrylic Acid by Aqueous Two-Phase Systems Using Hydrophilic Ionic Liquids

    International Nuclear Information System (INIS)

    Lee, Yong Hwa; Lee, Woo Youn; Kim, Ki-Sub; Hong, Yeon Ki

    2014-01-01

    As an effective method for extraction of acrylic acid, aqueous two-phase systems based on morpholinium ionic liquids were used in this study. Effects of the alkyl chain length of cation in morpholinium ionic liquids on phase diagram and extraction efficiencies were investigated. Experimental results show that aqueous two phase systems can be formed by adding appropriate amount of morpholinium ionic liquids to aqueous K 2 HPO 4 solutions. It can be found that the ability of morpholinium ionic liquids for phase separation followed the order [HMMor][Br]>[OMMor][Br]>[BMMor][Br]>[EMMor][Br]. There was little difference between binodal curves of imidazolium ionic liquids and those of morpholinium ionic liquids. 50-90% of the extraction efficiency was observed for acrylic acid by aqueous two phase extraction of acrylic acid with morpholinium ionic liquids. It can be concluded that morpholinium ionic liquids/K 2 HPO 4 were effective for aqueous two phases extraction of acrylic acid comparing to imidazolium ionic liquids/K 2 HPO 4 systems because of their lower cost

  1. Separation of tungsten from molybdenum by liquid-liquid extraction and extraction chromatography using thiocyanate and a quarternary ammonium salt

    International Nuclear Information System (INIS)

    Yonezawa, C.; Onishi, H.

    1977-01-01

    Methods were developed for the separation of tungsten from molybdenum by liquid-liquid extraction and extraction chromatography using thiocyanate and a quaternary ammonium salt, Zephiramine. Tungsten was extracted into chloroform as an ion associate of tungsten(V)-thiocyanate complex and Zephiramine cation was retained on a column of Teflon powder coated with Zephiramine, but molybdenum(III) was neither extracted nor retained. The extraction chromatographic method was succesfully applied to the determination of trace amounts of tungsten in molybdenum by neutron activation analysis. The γ-ray spectrum, observed with the Ge(Li) detector, of tungsten fraction separated from irradiated molybdenum are shown. The peaks of 99 Mo, sup(99m)Tc, and sup(99m)Nb (produced by 92 Mo(n,p)sup(99m)Nb) were seen, but these nuclides did nit interfere with the determination of tungsten using a NaI(Tl) detector. The results of the neutron activation analysis of a sample of ammonium molybdate agreed quite well with that of the spectrophotometric determination after extraction chromatographic separation. (T.G.)

  2. Liquid-liquid extraction of uranium(VI) using Cyanex 272 in toluene from sodium salicylate medium

    International Nuclear Information System (INIS)

    Madane, Namdev S.; Nikam, Gurunath H.; Jadhav, Deepali V.; Mohite, Baburao S.

    2011-01-01

    Liquid-liquid extraction of U(VI) from sodium salicylate media using Cyanex 272 in toluene has been carried out. Uranium(VI) was quantitatively extracted from 1 x 10 -3 M sodium salicylate with 5 x 10 -4 M Cyanex 272 in toluene. It was stripped quantitatively from the organic phase with 1M HCl and determined spectrophotometrically with arsenazo(III) at 660 nm. The effect of concentrations of sodium salicylate, extractant, diluents, metal ion and strippants have been studied. Separation of uranium(VI) from other elements was achieved from binary as well as from multicomponent mixtures. The method was extended to determination of uranium(VI) in geological samples. The method is simple, rapid and selective with good reproducibility (approximately ± 2%). (author)

  3. Complex Formation in a Liquid-Liquid Extraction System Containing Cobalt(II), 4-(2-Pyridylazo)resorcinol, and Nitron

    OpenAIRE

    Racheva, Petya Vassileva; Gavazov, Kiril Blazhev; Lekova, Vanya Dimitrova; Dimitrov, Atanas Nikolov

    2013-01-01

    Complex formation and liquid-liquid extraction were studied in a system containing cobalt(II), 4-(2-pyridylazo)resorcinol (PAR), 1,4-diphenyl-3-(phenylamino)-1H-1,2,4-triazole (Nitron, Nt), water, and chloroform. The effect of some experimental parameters (pH, shaking time, concentration of PAR, and concentration of Nt) was systematically investigated, and the optimum conditions for cobalt extraction as an ion-association complex, (NtH+)[Co3+(PAR)2], were found. The following key equilibrium ...

  4. Liquid chromatography-tandem mass spectrometric assay for the quantitative determination of the tyrosine kinase inhibitor quizartinib in mouse plasma using salting-out liquid-liquid extraction

    NARCIS (Netherlands)

    Retmana, Irene A; Wang, Jing; Schinkel, Alfred H; Schellens, Jan H M; Beijnen, Jos H; Sparidans, Rolf W

    2017-01-01

    A bioanalytical assay for quizartinib -a potent, and selective FLT3 tyrosine kinase inhibitor- in mouse plasma was developed and validated. Salting-out assisted liquid-liquid extraction (SALLE), using acetonitrile and magnesium sulfate, was selected as sample pretreatment with deuterated quizartinib

  5. Liquid liquid extraction of Th(IV) and its complexation study by Calix(4)pyrole

    International Nuclear Information System (INIS)

    Rathod, N.V.; Kamble, J.H.; Malkhede, D.D.

    2015-01-01

    Due to increased demand for carbon-free energy, accelerated growth of nuclear power is foreseen in several countries, especially in China and India. This has made the sustainable use of fuel resources such as uranium and thorium very important. Today, uranium is the main-stay of the present generation of nuclear power plants. However, the anticipated growth in nuclear energy may require introducing thorium as a fuel in future. Meso-octamethyl calix(4)pyrole is known for anion receptor however the present study evaluate the effect of cation for complexation of thorium by liquid liquid extraction technique. Calix(4)pyrole was evaluated for extraction of Th(IV), and 97% extraction efficiency was obtained. Th(IV) was determine with arsenazo(III) at 655 nm. The effect of acid molarity of 0.1 M, 1:5 metal to ligand ratio found efficient for maximum extraction. The stoichiometry ratio 1:2 between metal to ligand is established

  6. Determination of Zinc Ions in Environmental Samples by Dispersive Liquid- Liquid Micro Extraction and Atomic Absorption Spectroscopy

    Directory of Open Access Journals (Sweden)

    F. Arabi

    2012-11-01

    Full Text Available In this work preconcentration of the Zn ions was investigated in water sample by Dispersive liquid- liquid micro extraction (DLLME using chloroform as an extraction solvent, methanol as a disperser solvent and 8-Hydroxyquinoline as a chelating agent. The determination of extracted ions was done by graphite furnace atomic absorption spectrometry. The influence of various analytical parameters including pH, extraction and disperser solvent type and volume and concentration of the chelating agent on the extraction efficiency of analyses was investigated. After extraction, the enrichment factor was 26 and the detection limit of the method was 0.0033 µg l-1 and the relative standard deviations (R.S.D for five determinations of 1 ng/ml Zn were 7.41%. 

  7. Selective extraction of copper, mercury, silver and palladium ionsfrom water using hydrophobic ionic liquids.

    Energy Technology Data Exchange (ETDEWEB)

    Papaiconomou, Nicolas; Lee, Jong-Min; Salminen, Justin; VonStosch, Moritz; Prausnitz, John M.

    2007-06-25

    Extraction of dilute metal ions from water was performed near room temperature with a variety of ionic liquids. Distribution coefficients are reported for fourteen metal ions extracted with ionic liquids containing cations 1-octyl-4-methylpyridinium [4MOPYR]{sup +}, 1-methyl-1-octylpyrrolidinium [MOPYRRO]{sup +} or 1-methyl-1-octylpiperidinium [MOPIP]{sup +}, and anions tetrafluoroborate [BF{sub 4}]{sup +}, trifluoromethyl sulfonate [TfO]{sup +} or nonafluorobutyl sulfonate [NfO]{sup +}. Ionic liquids containing octylpyridinium cations are very good for extracting mercury ions. However, other metal ions were not significantly extracted by any of these ionic liquids. Extractions were also performed with four new task-specific ionic liquids. Such liquids containing a disulfide functional group are efficient and selective for mercury and copper, whereas those containing a nitrile functional group are efficient and selective for silver and palladium.

  8. Extraction of lithium from salt lake brine using room temperature ionic liquid in tributyl phosphate

    International Nuclear Information System (INIS)

    Shi, Chenglong; Jia, Yongzhong; Zhang, Chao; Liu, Hong; Jing, Yan

    2015-01-01

    Highlights: • We proposed a new system for Li recovery from salt lake brine by extraction using an ionic liquid. • Cation exchange was proposed to be the mechanism of extraction followed in ionic liquid. • This ionic liquid system shown considerable extraction ability for lithium and the single extraction efficiency of lithium reached 87.28% under the optimal conditions. - Abstract: Lithium is known as the energy metal and it is a key raw material for preparing lithium isotopes which have important applications in nuclear energy source. In this work, a typical room temperature ionic liquid (RTILs), 1-butyl-3-methyl-imidazolium hexafluorophosphate ([C 4 mim][PF 6 ]), was used as an alternative solvent to study liquid/liquid extraction of lithium from salt lake brine. In this system, the ionic liquid, NaClO 4 and tributyl phosphate (TBP) were used as extraction medium, co-extraction reagent and extractant respectively. The effects of solution pH value, phase ratio, ClO 4 − amount and other factors on lithium extraction efficiency had been investigated. Optimal extraction conditions of this system include the ratio of TBP/IL at 4/1 (v/v), O/A at 2:1, n(ClO 4 − )/n(Li + ) at 2:1, the equilibration time of 10 min and unadjusted pH. Under the optimal conditions, the single extraction efficiency of lithium was 87.28% which was much higher than the conventional extraction system. Total extraction efficiency of 99.12% was obtained by triple-stage countercurrent extraction. Study on the mechanism revealed that the use of ionic liquid increased the extraction yield of lithium through cation exchange in this system. Preliminary results indicated that the use of [C 4 mim][PF 6 ] as an alternate solvent to replace traditional organic solvents (VOCs) in liquid/liquid extraction was very promising

  9. Liquid-liquid extraction of uranium (VI) using Cyanex 272 in kerosene from sodium salicylate medium

    International Nuclear Information System (INIS)

    Kamble, Pravin N.; Mohite, Baburao S.; Suryavanshi, Vishal J.; Salunkhe, Suresh T.

    2015-01-01

    Liquid-liquid extraction of uranium (VI) from sodium salicylate media using Cyanex 272 in kerosene has been carried out. Uranium (VI) was quantitatively extracted from 1x10 -4 M sodium salicylate with 5x10 -4 M Cyanex 272 in kerosene. It was stripped quantitatively from the organic phase with 4M HCl and determined spectrophotometrically with arsenazo(III) at 600 nm. The effects of concentrations of sodium salicylate, metal ions and strippants have been studied. Separation of uranium (VI) from other elements was achieved from binary as well as from multicomponent mixtures. The method is simple, rapid and selective with good reproducibility (approximately ±2%). (author)

  10. Comparison of salting-out and sugaring-out liquid-liquid extraction methods for the partition of 10-hydroxy-2-decenoic acid in royal jelly and their co-extracted protein content.

    Science.gov (United States)

    Tu, Xijuan; Sun, Fanyi; Wu, Siyuan; Liu, Weiyi; Gao, Zhaosheng; Huang, Shaokang; Chen, Wenbin

    2018-01-15

    Homogeneous liquid-liquid extraction (h-LLE) has been receiving considerable attention as a sample preparation method due to its simple and fast partition of compounds with a wide range of polarities. To better understand the differences between the two h-LLE extraction approaches, salting-out assisted liquid-liquid extraction (SALLE) and sugaring-out assisted liquid-liquid extraction (SULLE), have been compared for the partition of 10-hydroxy-2-decenoic acid (10-HDA) from royal jelly, and for the co-extraction of proteins. Effects of the amount of phase partition agents and the concentration of acetonitrile (ACN) on the h-LLE were discussed. Results showed that partition efficiency of 10-HDA depends on the phase ratio in both SALLE and SULLE. Though the partition triggered by NaCl and glucose is less efficient than MgSO 4 in the 50% (v/v) ACN-water mixture, their extraction yields can be improved to be similar with that in MgSO 4 SALLE by increasing the initial concentration of ACN in the ACN-water mixture. The content of co-extracted protein was correlated with water concentration in the obtained upper phase. MgSO 4 showed the largest protein co-extraction at the low concentration of salt. Glucose exhibited a large protein co-extraction in the high phase ratio condition. Furthermore, NaCl with high initial ACN concentration is recommended because it produced high extraction yield for 10-HDA and the lowest amount of co-extracted protein. These observations would be valuable for the sample preparation of royal jelly. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Fast and comprehensive analysis of secondary metabolites in cocoa products using ultra high-performance liquid chromatography directly after pressurized liquid extraction.

    Science.gov (United States)

    Damm, Irina; Enger, Eileen; Chrubasik-Hausmann, Sigrun; Schieber, Andreas; Zimmermann, Benno F

    2016-08-01

    Fast methods for the extraction and analysis of various secondary metabolites from cocoa products were developed and optimized regarding speed and separation efficiency. Extraction by pressurized liquid extraction is automated and the extracts are analyzed by rapid reversed-phase ultra high-performance liquid chromatography and normal-phase high-performance liquid chromatography methods. After extraction, no further sample treatment is required before chromatographic analysis. The analytes comprise monomeric and oligomeric flavanols, flavonols, methylxanthins, N-phenylpropenoyl amino acids, and phenolic acids. Polyphenols and N-phenylpropenoyl amino acids are separated in a single run of 33 min, procyanidins are analyzed by normal-phase high-performance liquid chromatography within 16 min, and methylxanthins require only 6 min total run time. A fourth method is suitable for phenolic acids, but only protocatechuic acid was found in relevant quantities. The optimized methods were validated and applied to 27 dark chocolates, one milk chocolate, two cocoa powders and two food supplements based on cocoa extract. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Molecular dynamics simulations of hydrophobous ions at the liquid-liquid interfaces: case of dicarbollide anions as synergy agents and of ionic liquids as extracting medium

    International Nuclear Information System (INIS)

    Chevrot, G.

    2008-01-01

    Based on molecular dynamics simulations, we first describe the distribution of dicarbollide salts (CCD - , Mn + ) in concentrated monophasic solutions (water, chloroform, octanol, nitrobenzene) and in the corresponding biphasic 'oil' - water solutions. We point to the importance of surface activity of the CCD - s and of their self-aggregation in water, with marked counterions effects, and we explain the synergistic effect of CCD - s in the Eu 3+ extraction by BTP ligands. In the second part of the thesis we report exploratory simulations on the extraction of Sr 2+ by 18-crown-6 to an hydrophobic ionic liquid ([BMI][PF6]), focusing on the liquid - liquid interface. Analogies and differences with a classical aqueous interface are outlined. (author)

  13. Liquid-liquid extraction of ion-association complexes of cobalt(II-4-(2-pyridylazoresorcinol with ditetrazolium salts

    Directory of Open Access Journals (Sweden)

    Divarova Vidka V.

    2015-01-01

    Full Text Available The formation and liquid-liquid extraction of ion-association complexes between Co(II-4-(2-Pyridylazoresorcinol (PAR anionic chelates and cations of three ditetrazolium chlorides were studied: Blue Tetrazolium chloride (BTC, Neotetrazolium chloride (NTC and Nitro Blue Tetrazolium chloride (NBT. The optimum conditions for the formation and solvent extraction of the ion-association comlpex chelates were determined. It has been found that in the systems of Co(II-PAR-DTS, the reactants are reacted in molar ratios 1:2:1 and the general formula of complexes was suggested. The extraction equilibria were investigated and quantitatively characterized by the equilibrium constants and the recovery factors. The analytical characteristics of the complexes were calculated.

  14. Determination of triazine herbicides in juice samples by microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography.

    Science.gov (United States)

    Su, Rui; Li, Dan; Wu, Lijie; Han, Jing; Lian, Wenhui; Wang, Keren; Yang, Hongmei

    2017-07-01

    A novel microextraction method, termed microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction, has been developed for the rapid enrichment and analysis of triazine herbicides in fruit juice samples by high-performance liquid chromatography. Instead of using hazardous organic solvents, two kinds of ionic liquids, a hydrophobic ionic liquid (1-hexyl-3-methylimidazolium hexafluorophosphate) and a hydrophilic ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate), were used as the extraction solvent and dispersion agent, respectively, in this method. The extraction procedure was induced by the formation of cloudy solution, which was composed of fine drops of 1-hexyl-3-methylimidazolium hexafluorophosphate dispersed entirely into sample solution with the help of 1-butyl-3-methylimidazolium tetrafluoroborate. In addition, an ion-pairing agent (NH 4 PF 6 ) was introduced to improve recoveries of the ionic liquid phase. Several experimental parameters that might affect the extraction efficiency were investigated. Under the optimum experimental conditions, the linearity for determining the analytes was in the range of 5.00-250.00 μg/L, with the correlation coefficients of 0.9982-0.9997. The practical application of this effective and green method is demonstrated by the successful analysis of triazine herbicides in four juice samples, with satisfactory recoveries (76.7-105.7%) and relative standard deviations (lower than 6.6%). In general, this method is fast, effective, and robust to determine triazine herbicides in juice samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Liquid-solid extraction of metallic cations by cationic amphiphiles

    International Nuclear Information System (INIS)

    Mueller, Wolfram; Sievers, Torsten K.; Zemb, Thomas; Diat, Olivier; Sievers, Torsten K.; Dejugnat, Christophe

    2012-01-01

    In the field of selective metal ion separation, liquid-liquid extraction is usually conducted through an emulsion mixing of hydrophobic complexants dispersed in an organic phase and acidic water containing the ionic species. Recently, it has been shown that amphiphilic complexants could influence strongly extraction efficiency by enhancing the interfacial interaction between the metal ion in the aqueous and the complexant in the organic phase. Moreover, these amphiphiles can also substitute the organic phase if an appropriate aliphatic chain is chosen. The dispersion of such amphiphilic complexants in an aqueous solution of salt mixtures is not only attractive for studying specific interactions but also to better the understanding of complex formation in aqueous solution of multivalent metal ions, such as lanthanides and actinides. This understanding is of potential interest for a broad range of industries including purification of rare earth metals and pollute treatment e.g. of fission byproducts. This principle can also be applied to liquid-solid extraction, where the final state of the separation is a solid phase containing the selectively extracted ions. Indeed, a novel solid-liquid extraction method exploits the selective precipitation of metal ions from an aqueous salt mixture using a cationic surfactant, below its Krafft point (temperature below which the long aliphatic chains of surfactant crystallize). This technique has been proven to be highly efficient for the separation of actinides and heavy metal using long chain ammonium or pyridinium amphiphiles. The most important point in this process is the recognition of cationic metal ions by cationic surfactants. By computing the free energy of the polar head group per micelle as a function of the different counter-anions, we have demonstrated for the first time that different interactions exist between the micellar surface and the ions. These interactions depend on the nature of the cation but also on

  16. Application of liquid metals for the extraction of solid metals

    International Nuclear Information System (INIS)

    Borgstedt, H.U.

    1996-01-01

    Liquid metals dissolve several solid metals in considerable amounts at moderate temperatures. The dissolution processes may be based upon simple physical solubility, formation of intermetallic phases. Even chemical reactions are often observed in which non-metallic elements might be involved. Thus, the capacity to dissolve metals and chemical properties of the liquid metals play a role in these processes. Besides the solubility also chemical properties and thermochemical data are of importance. The dissolution of metals in liquid metals can be applied to separate the solutes from other metals or non-metallic phases. Relatively noble metals can be chemically reduced by the liquid phases. Such solution processes can be applied in the extractive metallurgy, for instance to extract metals from metallic waste. The recycling of metals is of high economical and ecological importance. Examples of possible processes are discussed. (author)

  17. Task-specific thioglycolate ionic liquids for heavy metal extraction: Synthesis, extraction efficacies and recycling properties

    Energy Technology Data Exchange (ETDEWEB)

    Platzer, Sonja [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, 1090 Vienna (Austria); Kar, Mega [School of Chemistry, Monash University, Clayton, Victoria 3800 (Australia); Leyma, Raphlin; Chib, Sonia; Roller, Alexander [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, 1090 Vienna (Austria); Jirsa, Franz [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, 1090 Vienna (Austria); Department of Zoology, University of Johannesburg, PO Box 524, Auckland Park, 2006 Johannesburg (South Africa); Krachler, Regina [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, 1090 Vienna (Austria); MacFarlane, Douglas R. [School of Chemistry, Monash University, Clayton, Victoria 3800 (Australia); Kandioller, Wolfgang, E-mail: wolfgang.kandioller@univie.ac.at [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, 1090 Vienna (Austria); Keppler, Bernhard K. [Institute of Inorganic Chemistry, Faculty of Chemistry, University of Vienna, Waehringer Str. 42, 1090 Vienna (Austria)

    2017-02-15

    Highlights: • Thioglycolate-based ionic liquids have been synthesized and their physicochemical properties have been examined. • The developed ionic liquids can efficiently remove Cu(II) and Cd(II). • Loaded ionic liquids can be recycled by application of different stripping protocols. - Abstract: Eight novel task-specific ionic liquids (TSILs) based on the thioglycolate anion designed for heavy metal extraction have been prepared and characterized by {sup 1}H and {sup 13}C NMR, UV-Vis, infrared, ESI-MS, conductivity, viscosity, density and thermal properties. Evaluation of their time-resolved extraction abilities towards cadmium(II) and copper(II) in aqueous solutions have been investigated where distribution ratios up to 1200 were observed. For elucidation of the IL extraction mode, crystals were grown where Cd(II) was converted with an excess of S-butyl thioglycolate. It was found by X-ray diffraction analysis that cadmium is coordinated by five oxygen and one sulfur donor atoms provided by two thioglycolate molecules and one water molecule. Leaching behavior of the hydrophobic ionic liquids into aqueous systems was studied by TOC (total dissolved organic carbon) measurements. Additionally, the immobilization on polypropylene was elucidated and revealed slower metal extraction rates and similar leaching behavior. Finally, recovery processes for cadmium and copper after extraction were performed and recyclability was successfully proven for both metals.

  18. Molecular dynamics simulations of hydrophobous ions at the liquid-liquid interfaces: case of dicarbollide anions as synergy agents and of ionic liquids as extracting medium; Simulations par dynamique moleculaire d'ions hydrophobes aux interfaces liquide - liquide: le cas des anions dicarbollides comme agents de synergie et celui des liquides ioniques comme milieu extractant

    Energy Technology Data Exchange (ETDEWEB)

    Chevrot, G

    2008-01-15

    Based on molecular dynamics simulations, we first describe the distribution of dicarbollide salts (CCD{sup -}, Mn{sup +}) in concentrated monophasic solutions (water, chloroform, octanol, nitrobenzene) and in the corresponding biphasic 'oil' - water solutions. We point to the importance of surface activity of the CCD{sup -}s and of their self-aggregation in water, with marked counterions effects, and we explain the synergistic effect of CCD{sup -}s in the Eu{sup 3+} extraction by BTP ligands. In the second part of the thesis we report exploratory simulations on the extraction of Sr{sup 2+} by 18-crown-6 to an hydrophobic ionic liquid ([BMI][PF6]), focusing on the liquid - liquid interface. Analogies and differences with a classical aqueous interface are outlined. (author)

  19. Comparison of micellar extraction combined with ionic liquid based vortex-assisted liquid-liquid microextraction and modified quick, easy, cheap, effective, rugged, and safe method for the determination of difenoconazole in cowpea.

    Science.gov (United States)

    Chen, Xiaochu; Bian, Yanli; Liu, Fengmao; Teng, Peipei; Sun, Pan

    2017-10-06

    Two simple sample pretreatment for the determination of difenoconazole in cowpea was developed including micellar extraction combined with ionic liquid based vortex-assisted liquid-liquid microextraction (ME-IL-VALLME) prior to high performance liquid chromatography (HPLC), and modified quick, easy, cheap, effective, rugged, and safe method (QuEChERS) coupled with HPLC-MS/MS. In ME-IL-VALLME method, the target analyte was extracted by surfactant Tween 20 micellar solution, then the supernatant was diluted with 3mL water to decrease the solubility of micellar solution. Subsequently, the vortex-assisted liquid-liquid microextraction (VALLME) procedure was performed in the diluted extraction solution by using the ionic liquid of 1-hexyl-3-methylimidazolium hexafluorophosphate ([HMIM]PF 6 ) as the extraction solvent and Tween 20 as an emulsifier to enhance the dispersion of the water-immiscible ionic liquid into the aqueous phase. Parameters that affect the extraction have been investigated in both methods Under the optimum conditions, the limits of quantitation were 0.10 and 0.05mgkg -1 , respectively. And good linearity was achieved with the correlation coefficient higher than 0.9941. The relative recoveries ranged from 78.6 to 94.8% and 92.0 to 118.0% with the relative standard deviations (RSD) of 7.9-9.6% and 1.2-3.2%, respectively. Both methods were quick, simple and inexpensive. However, the ME-IL-VALLME method provides higher enrichment factor compared with conventional QuEChERS method. The ME-IL-VALLME method has a strong potential for the determination of difenoconazole in complex vegetable matrices with HPLC. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Extraction of tritium from liquid lithium by permeation

    International Nuclear Information System (INIS)

    Alire, R.M.

    1978-01-01

    This paper assesses a method for extracting tritium from liquid lithium for specific application to the conceptual laser fusion reactor that uses a continuous lithium ''waterfall.'' The tritium diffuses through a refractory metal that contains a getter and is then stored in a hydride-forming alloy. There are various uncertainties with this method including helium-4 extraction, unknown impurities that may accumulate in liquid lithium, the effects of these impurities on tritium separation, and the maintenance of tritium-contaminated equipment. Our study indicates that major tritium losses will occur during equipment maintenance rather than as a result of permeation losses through the primary vessel

  1. Extraction of lithium from salt lake brine using room temperature ionic liquid in tributyl phosphate

    Energy Technology Data Exchange (ETDEWEB)

    Shi, Chenglong [Key Laboratory of Salt Lake Resources and Chemistry, Qinghai Institute of Salt Lakes, Chinese Academy of Sciences, 810008 Xining (China); University of Chinese Academy of Sciences, 100049 Beijing (China); Jia, Yongzhong [Key Laboratory of Salt Lake Resources and Chemistry, Qinghai Institute of Salt Lakes, Chinese Academy of Sciences, 810008 Xining (China); Zhang, Chao [Key Laboratory of Salt Lake Resources and Chemistry, Qinghai Institute of Salt Lakes, Chinese Academy of Sciences, 810008 Xining (China); University of Chinese Academy of Sciences, 100049 Beijing (China); Liu, Hong [Qinghai Salt Chemical Products Supervision and Inspection Center, 816000 Golmud (China); Jing, Yan, E-mail: 1580707906@qq.com [Key Laboratory of Salt Lake Resources and Chemistry, Qinghai Institute of Salt Lakes, Chinese Academy of Sciences, 810008 Xining (China)

    2015-01-15

    Highlights: • We proposed a new system for Li recovery from salt lake brine by extraction using an ionic liquid. • Cation exchange was proposed to be the mechanism of extraction followed in ionic liquid. • This ionic liquid system shown considerable extraction ability for lithium and the single extraction efficiency of lithium reached 87.28% under the optimal conditions. - Abstract: Lithium is known as the energy metal and it is a key raw material for preparing lithium isotopes which have important applications in nuclear energy source. In this work, a typical room temperature ionic liquid (RTILs), 1-butyl-3-methyl-imidazolium hexafluorophosphate ([C{sub 4}mim][PF{sub 6}]), was used as an alternative solvent to study liquid/liquid extraction of lithium from salt lake brine. In this system, the ionic liquid, NaClO{sub 4} and tributyl phosphate (TBP) were used as extraction medium, co-extraction reagent and extractant respectively. The effects of solution pH value, phase ratio, ClO{sub 4}{sup −} amount and other factors on lithium extraction efficiency had been investigated. Optimal extraction conditions of this system include the ratio of TBP/IL at 4/1 (v/v), O/A at 2:1, n(ClO{sub 4}{sup −})/n(Li{sup +}) at 2:1, the equilibration time of 10 min and unadjusted pH. Under the optimal conditions, the single extraction efficiency of lithium was 87.28% which was much higher than the conventional extraction system. Total extraction efficiency of 99.12% was obtained by triple-stage countercurrent extraction. Study on the mechanism revealed that the use of ionic liquid increased the extraction yield of lithium through cation exchange in this system. Preliminary results indicated that the use of [C{sub 4}mim][PF{sub 6}] as an alternate solvent to replace traditional organic solvents (VOCs) in liquid/liquid extraction was very promising.

  2. Ionic liquid-based microwave-assisted extraction of rutin from Chinese medicinal plants.

    Science.gov (United States)

    Zeng, Huan; Wang, Yuzhi; Kong, Jinhuan; Nie, Chan; Yuan, Ya

    2010-12-15

    An ionic liquid-based microwave-assisted extraction (ILMAE) method has been developed for the effective extraction of rutin from Chinese medicinal plants including Saururus chinensis (Lour.) Bail. (S. chinensis) and Flos Sophorae. A series of 1-butyl-3-methylimidazolium ionic liquids with different anions were investigated. The results indicated that the characteristics of anions have remarkable effects on the extraction efficiency of rutin and among the investigated ionic liquids, 1-butyl-3-methylimidazolium bromide ([bmim]Br) aqueous solution was the best. In addition, the ILMAE procedures for the two kinds of medicinal herbs were also optimized by means of a series of single factor experiments and an L(9) (3(4)) orthogonal design. Compared with the optimal ionic liquid-based heating extraction (ILHE), marinated extraction (ILME), ultrasonic-assisted extraction (ILUAE), the optimized approach of ILMAE gained higher extraction efficiency which is 4.879 mg/g in S. chinensis with RSD 1.33% and 171.82 mg/g in Flos Sophorae with RSD 1.47% within the shortest extraction time. Reversed phase high performance liquid chromatography (RP-HPLC) with ultraviolet detection was employed for the analysis of rutin in Chinese medicinal plants. Under the optimum conditions, the average recoveries of rutin from S. chinensis and Flos Sophorae were 101.23% and 99.62% with RSD lower than 3%, respectively. The developed approach is linear at concentrations from 42 to 252 mg L(-1) of rutin solution, with the regression coefficient (r) at 0.99917. Moreover, the extraction mechanism of ILMAE and the microstructures and chemical structures of the two researched samples before and after extraction were also investigated. With the help of LC-MS, it was future demonstrated that the two researched herbs do contain active ingredient of rutin and ionic liquids would not influence the structure of rutin. Copyright © 2010 Elsevier B.V. All rights reserved.

  3. Use of water in aiding olefin/paraffin (liquid + liquid) extraction via complexation with a silver bis(trifluoromethylsulfonyl)imide salt

    International Nuclear Information System (INIS)

    Wang, Yu; Thompson, Jillian; Zhou, Jingjing; Goodrich, Peter; Atilhan, Mert; Pensado, Alfonso S.; Kirchner, Barbara; Rooney, David; Jacquemin, Johan; Khraisheh, Majeda

    2014-01-01

    Highlights: • Silver-based ILs used as olefin extracting agents for olefin/paraffin mixtures. • Each extraction process is based on the olefin complexation and solvation. • The presence of water influences positively each extraction process. • Each extraction process was evaluated by DFT calculations, NMR, IR and Raman. • LLE data were then correlated by using the UNIQUAC model. - Abstract: This paper describes the extraction of C 5 –C 8 linear α-olefins from olefin/paraffin mixtures of the same carbon number via a reversible complexation with a silver salt (silver bis(trifluoromethylsulfonyl)imide, Ag[Tf 2 N]) to form room temperature ionic liquids [Ag(olefin) x ][Tf 2 N]. From the experimental (liquid + liquid) equilibrium data for the olefin/paraffin mixtures and Ag[Tf 2 N], 1-pentene showed the best separation performance while C 7 and C 8 olefins could only be separated from the corresponding mixtures on addition of water which also improves the selectivity at lower carbon numbers like the C 5 and C 6 , for example. Using infrared and Raman spectroscopy of the complex and Ag[Tf 2 N] saturated by olefin, the mechanism of the extraction was found to be based on both chemical complexation and the physical solubility of the olefin in the ionic liquid ([Ag(olefin) x ][Tf 2 N]). These experiments further support the use of such extraction techniques for the separation of olefins from paraffins

  4. Liquid-liquid extraction of beryllium (II) using Cyanex 923 in kerosene from sodium acetate medium

    International Nuclear Information System (INIS)

    Kamble, Pravin N.; Madane, Namdev S.; Mohite, Baburao S.

    2013-01-01

    Liquid-liquid extraction of beryllium(II) from sodium acetate media using cyanex 923 in kerosene has been carried out. Beryllium(II) was quantitatively extracted from 1x10 -1 M sodium acetate with 1x10 -2 M cyanex 923 in kerosene. It was stripped quantitatively from the organic phase with 1M H 2 SO 4 and determined spectrophotometrically with eriochrome cyanine R at 525 nm. The effect of concentrations of sodium acetate, metal ions and strippants have been studied. Separation of beryllium(II) from other elements was achieved from binary as well as from multicomponent mixtures. The method is simple, rapid and selective with good reproducibility (approximately±2%). (author)

  5. Liquid-solid extraction of cationic metals by cationic amphiphiles

    International Nuclear Information System (INIS)

    Muller, W.

    2010-01-01

    In the field of selective separation for recycling of spent nuclear fuel, liquid-liquid extraction processes are widely used (PUREX, DIAMEX..) in industrial scale. In order to guarantee a sustainable nuclear energy for the forthcoming generations, alternative reprocessing techniques are under development. One of them bases on the studies from Heckmann et al in the 80's and consists in selectively precipitating actinides from aqueous waste solutions by cationic surfactants (liquid-solid extraction). This technique has some interesting advantages over liquid-liquid extraction techniques, because several steps are omitted like stripping or solvent washing. Moreover, the amount of waste is decreased considerably, since no contaminated organic solvent is produced. In this thesis, we have carried out a physico-chemical study to understand the specific interactions between the metallic cations with the cationic surfactant. First, we have analysed the specific effect of the different counter-ions (Cl - , NO 3 - , C 2 O 4 2- ) and then the effect of alkaline cations on the structural properties of the surfactant aggregation in varying thermodynamical conditions. Finally, different multivalent cations (Cu 2+ , Zn 2+ , UO 2 2+ , Fe 3+ , Nd 3+ , Eu 3+ , Th 4+ ) were considered; we have concluded that depending on the anionic complex of these metals formed in acidic media, we can observe either an adsorption at the micellar interface or not. This adsorption has a large influence of the surfactant aggregation properties and determines the limits of the application in term of ionic strength, temperature and surfactant concentration. (author) [fr

  6. Determination of carbohydrates in tobacco by pressurized liquid extraction combined with a novel ultrasound-assisted dispersive liquid-liquid microextraction method.

    Science.gov (United States)

    Cai, Kai; Hu, Deyu; Lei, Bo; Zhao, Huina; Pan, Wenjie; Song, Baoan

    2015-07-02

    A novel derivatization-ultrasonic assisted-dispersive liquid-liquid microextraction (UA-DLLME) method for the simultaneous determination of 11 main carbohydrates in tobacco has been developed. The combined method involves pressurized liquid extraction (PLE), derivatization, and UA-DLLME, followed by the analysis of the main carbohydrates with a gas chromatography-flame ionization detector (GC-FID). First, the PLE conditions were optimized using a univariate approach. Then, the derivatization methods were properly compared and optimized. The aldononitrile acetate method combined with the O-methoxyoxime-trimethylsilyl method was used for derivatization. Finally, the critical variables affecting the UA-DLLME extraction efficiency were searched using fractional factorial design (FFD) and further optimized using Doehlert design (DD) of the response surface methodology. The optimum conditions were found to be 44 μL for CHCl3, 2.3 mL for H2O, 11% w/v for NaCl, 5 min for the extraction time and 5 min for the centrifugation time. Under the optimized experimental conditions, the detection limit of the method (LODs) and linear correlation coefficient were found to be in the range of 0.06-0.90 μg mL(-1) and 0.9987-0.9999. The proposed method was successfully employed to analyze three flue-cured tobacco cultivars, among which the main carbohydrate concentrations were found to be very different. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Ionic Liquid-Based Ultrasonic/Microwave-Assisted Extraction of ...

    African Journals Online (AJOL)

    Conclusion: Compared with traditional methods, IL-UMAE method uses Ionic liquid-solvent which greatly shortens the extraction time. IL-UMAE as a simple, effective and environmentally friendly approach shows a broad prospect for active ingredient extraction. Keywords: Dioscorea zingiberensis Steroidal saponins, Ionic ...

  8. Separation of {sup 195(m,g),197m}Hg from bulk gold target by liquid-liquid extraction using hydrophobic ionic liquids

    Energy Technology Data Exchange (ETDEWEB)

    Ghosh, Kaustab; Lahiri, Susanta [Saha Institute of Nuclear Physics, Kolkata (India). Chemical Sciences Div.; Maiti, Moumita [Indian Institute of Technology Roorkee, Roorkee (India). Dept. of Physics

    2017-07-01

    The {sup 195(m,g),197m}Hg radionuclides were produced in accelerator when natural Au foil was irradiated with 23 MeV protons. The no-carrier-added (NCA) Hg radioisotopes were separated from the bulk Au target by liquid-liquid extraction (LLX) employing hydrophobic RTILs 1-butyl-3-methylimidazolium hexafluorophosphate([C{sub 4}mim][PF{sub 6}]) and 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide([bmim][Tf{sub 2}N]) as extractant with HNO{sub 3} and HCl. In each case, bulk Au was extracted into the RTIL phase leaving NCA Hg-radionuclides in the aqueous phase. The RTILs were recovered by washing with 1 M K{sub 2}S{sub 2}O{sub 5} and freshly prepared 1 M FeSO{sub 4}. The reported separation methods follow green chemistry approach as it does not involve any volatile reagents.

  9. Predictive thermodynamic models for liquid--liquid extraction of single, binary and ternary lanthanides and actinides

    International Nuclear Information System (INIS)

    Hoh, Y.C.

    1977-03-01

    Chemically based thermodynamic models to predict the distribution coefficients and the separation factors for the liquid--liquid extraction of lanthanides-organophosphorus compounds were developed by assuming that the quotient of the activity coefficients of each species varies slightly with its concentrations, by using aqueous lanthanide or actinide complexes stoichiometric stability constants expressed as its degrees of formation, by making use of the extraction mechanism and the equilibrium constant for the extraction reaction. For a single component system, the thermodynamic model equations which predict the distribution coefficients, are dependent on the free organic concentration, the equilibrated ligand and hydrogen ion concentrations, the degree of formation, and on the extraction mechanism. For a binary component system, the thermodynamic model equation which predicts the separation factors is the same for all cases. This model equation is dependent on the degrees of formation of each species in their binary system and can be used in a ternary component system to predict the separation factors for the solutes relative to each other

  10. Liquid–liquid extraction of Pu(IV), U(VI) and Am(III) using malonamide in room temperature ionic liquid as diluent

    International Nuclear Information System (INIS)

    Rout, Alok; Venkatesan, K.A.; Srinivasan, T.G.; Vasudeva Rao, P.R.

    2012-01-01

    Highlights: ► Extraction of actinides using malonamide in room temperature ionic liquid. ► High distribution ratios of actinides in room temperature ionic liquid. ► Ion exchange mechanism. ► Stoichiometry of extraction. ► High separation factors of U(VI) and Pu(IV) over Am(III) and fission products. - Abstract: The extraction behavior of U(VI), Pu(IV) and Am(III) from nitric acid medium by a solution of N,N-dimethyl-N,N-dioctyl-2-(2-hexyloxyethyl)malonamide (DMDOHEMA) in the room temperature ionic liquid, 1–butyl–3–methylimidazolium bis(trifluoromethanesulfonyl)imide (C 4 mimNTf 2 ), was studied. The distribution ratio of these actinides in DMDOHEMA/C 4 mimNTf 2 was measured as a function of various parameters such as the concentration of nitric acid, DMDOHEMA, NTf 2 − , alkyl chain length of ionic liquid. The extraction of actinides in the absence of DMDOHEMA was insignificant and the distribution ratio achieved in conjunction with C 4 mimNTf 2 , was remarkable. The separation factor of U(VI) and Pu(IV) achieved with the use of DMDOHEMA, ionic liquid was compared with Am(III) and other fission products. The stoichiometry of the metal-solvate was determined to be 1:2 for U(VI) and Pu(IV) and 1:3 for Am(III).

  11. Application of liquid-liquid extraction in separation of rare earths [Paper No. : V-6

    International Nuclear Information System (INIS)

    Deshpande, S.M.; Krishnan, N.P.K.; Murthy, T.K.S.; Swaminathan, T.V.

    1979-01-01

    The rare earths consist of fifteen elements which have very similar chemical properties and are difficult to separate from each other. Since they exist together in all naturally occurring minerals their separation is one of the important and difficult aspects of their technology. Liquid-liquid extraction has proved to be an efficient technique for their separation. The two important extraction systems that find practical and large scale application, the nitric acid + tri-n-butyl phosphate, and mineral acid (particularly hydrochloric acid) + organo phosphoric acid (like di-2-ethyl hexyl phosphoric acid), are briefly reviewed. The factors affecting the extraction and separation of rare earths in the two systems are discussed. On an industrial scale the extraction process is very often employed for an initial concentration of the desired rare earths from complex mixtures. The final purification is generally achieved by the ion exchange method. The utility of the solvent extraction process for the upgrading of selected rare earths-europium, samarium and gadolinium-from a mixed rare earth chloride, derived from monazite, is illustrated by the work carried out in this laboratory and pilot plant operation at the Alwaye plant of M/s. Indian Rare Earths Ltd. (author)

  12. Active liquid/liquid interfaces: contributions of non linear optics and tensiometry

    International Nuclear Information System (INIS)

    Gassin, P.M.

    2013-01-01

    Liquid-liquid extraction processes are widely used in the industrial fields of selective separation. Despite its numerous applications, the microscopic mechanisms which occur during a liquid-liquid extraction processes are really unknown specially at the liquid/liquid interface. Thus, this work deals on the understanding of the phenomena which drive the mass transfer across a liquid/liquid interface. Two experimental techniques were used in this work: dynamic interfacial tension measurement and non-linear optical experiments. Along with the use of this experimental approach, a numerical model describing the mass transfer dynamic has been developed. This model works under the assumption that both diffusion and a chemical step describing adsorption and desorption processes contribute to the global transfer kinetics. Model systems of surfactant molecules, chromophore molecules and complexing molecule were investigated at liquid/liquid and air/liquid interface. Interfacial phenomena like adsorption, surface aggregation and ion complexing were studied. Finally, the methodology developed in this work was applied to studied an extractant molecule with potential industrial application. (author) [fr

  13. Salting-out assisted liquid-liquid extraction coupled to ultra-high performance liquid chromatography-tandem mass spectrometry for the determination of tetracycline residues in infant foods.

    Science.gov (United States)

    Moreno-González, David; García-Campaña, Ana M

    2017-04-15

    The use of salting-out assisted liquid-liquid extraction (SALLE) combined with ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) has been evaluated for the determination of tetracyclines in infant foods based on meat and vegetables or in milk. To obtain satisfactory extraction efficiencies for the studied analytes, several parameters affecting the SALLE procedure were optimized. Analytical performances of the method were satisfactory, obtaining limits of quantification lower than 0.48μgkg -1 in all cases. The precision, expressed as relative standard deviation (%, RSD) was below 11.3%. The extraction efficiency for fortified samples ranged from 89.2 to 96.8%, with RSDs lower than 7.3%. Matrix effect was evaluated for all samples studied, being lower than |21|% in all cases. In relation to the low solvent consumption, the proposed methodology could be considered rapid, cheap and environmentally friendly. Its applicability has been successfully tested in a wide range of infant foods. Copyright © 2016 Elsevier Ltd. All rights reserved.

  14. Ternary liquid-liquid equilibria for mixtures of toluene + n-heptane + an ionic liquid

    NARCIS (Netherlands)

    Meindersma, G.W.; Podt, J.G.; de Haan, A.B.

    2006-01-01

    This research has been focused on a study of sulfolane and four ionic liquids as solvents in liquid–liquid extraction. Liquid–liquid equilibria data were obtained for mixtures of (sulfolane or 4-methyl-N-butylpyridinium tetrafluoroborate ([mebupy]BF4) or 1-ethyl-3-methylimidazolium ethylsulfate

  15. Task-specific ionic liquids for An and Ln extraction: unusual speciation and extraction mechanisms

    Energy Technology Data Exchange (ETDEWEB)

    Billard, Isabelle; Jobin, Emilie; Ouadi, Ali; Gaillard, Clotilde [IPHC-DRS, Chimie nucleaire, 23 rue du Loess, BP28, 67037 Strasbourg cedex 2 (France)

    2008-07-01

    Extraction mechanisms of uranium by TBP (tributylphosphate) diluted in an ionic liquid BumimTf{sub 2}N (1-butyl-3-methyl-imidazolium bis(tri-fluoro-methyl-sulfonyl)imide) and by Task-Specific Ionic Liquids (TSILs) bearing a phosphoryl group were investigated. Great differences between these mechanisms and the one in the industrial solvent, dodecane, have been put in evidence. While in dodecane, the neutral species, UO{sub 2}(NO{sub 3}){sub 2}(TBP){sub 2}, is the major extracted complex, in BumimTf{sub 2}N and TSILs, at least two species are extracted with more or less similar proportions. Moreover, no uranyl species with two nitrates could be observed in these ionic liquids. Finally, the mechanisms vary from TBP in BumimTf{sub 2}N to TSILs. These results led to a so-to-say new kind of actinide chemistry. (authors)

  16. Characterization of rhamnolipids by liquid chromatography/mass spectrometry after solid-phase extraction.

    Science.gov (United States)

    Behrens, Beate; Engelen, Jeannine; Tiso, Till; Blank, Lars Mathias; Hayen, Heiko

    2016-04-01

    Rhamnolipids are surface-active agents with a broad application potential that are produced in complex mixtures by bacteria of the genus Pseudomonas. Analysis from fermentation broth is often characterized by laborious sample preparation and requires hyphenated analytical techniques like liquid chromatography coupled to mass spectrometry (LC-MS) to obtain detailed information about sample composition. In this study, an analytical procedure based on chromatographic method development and characterization of rhamnolipid sample material by LC-MS as well as a comparison of two sample preparation methods, i.e., liquid-liquid extraction and solid-phase extraction, is presented. Efficient separation was achieved under reversed-phase conditions using a mixed propylphenyl and octadecylsilyl-modified silica gel stationary phase. LC-MS/MS analysis of a supernatant from Pseudomonas putida strain KT2440 pVLT33_rhlABC grown on glucose as sole carbon source and purified by solid-phase extraction revealed a total of 20 congeners of di-rhamnolipids, mono-rhamnolipids, and their biosynthetic precursors 3-(3-hydroxyalkanoyloxy)alkanoic acids (HAAs) with different carbon chain lengths from C8 to C14, including three rhamnolipids with uncommon C9 and C11 fatty acid residues. LC-MS and the orcinol assay were used to evaluate the developed solid-phase extraction method in comparison with the established liquid-liquid extraction. Solid-phase extraction exhibited higher yields and reproducibility as well as lower experimental effort.

  17. Proof of concept for continuous enantioselective liquid-liquid extraction in capillary microreactors using 1-octanol as a sustainable solvent

    NARCIS (Netherlands)

    Susanti, S.; Meinds, Tim G.; Pinxterhuis, Erik B.; Schuur, Boelo; De Vries, Johannes G.; Feringa, Ben L.; Winkelman, Jozef G.M.; Yue, Jun; Heeres, Hero J.

    2017-01-01

    The use of capillary microreactors for enantioselective liquid-liquid extraction (ELLE) was successfully demonstrated using a model system consisting of a buffered aqueous amino acid derivative (3,5-dinitrobenzoyl-(R,S)-leucine) solution (phosphate buffer, pH 6.58) and a chiral cinchona alkaloid

  18. Fast, simple and efficient salting-out assisted liquid-liquid extraction of naringenin from fruit juice samples prior to their enantioselective determination by liquid chromatography.

    Science.gov (United States)

    Magiera, Sylwia; Kwietniowska, Ewelina

    2016-11-15

    In this study, an easy, simple and efficient method for the determination of naringenin enantiomers in fruit juices after salting-out-assisted liquid-liquid extraction (SALLE) and high-performance liquid chromatography (HPLC) with diode-array detection (DAD) was developed. The sample treatment is based on the use of water-miscible acetonitrile as the extractant and acetonitrile phase separation under high-salt conditions. After extraction, juice samples were incubated with hydrochloric acid in order to achieve hydrolysis of naringin to naringenin. The hydrolysis parameters were optimized by using a half-fraction factorial central composite design (CCD). After sample preparation, chromatographic separation was obtained on a Chiralcel® OJ-RH column using the mobile phase consisting of 10mM aqueous ammonium acetate:methanol:acetonitrile (50:30:20; v/v/v) with detection at 288nm. The average recovery of the analyzed compounds ranged from 85.6 to 97.1%. The proposed method was satisfactorily used for the determination of naringenin enantiomers in various fruit juices samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. Aluminium sensitized spectrofluorimetric determination of fluoroquinolones in milk samples coupled with salting-out assisted liquid-liquid ultrasonic extraction

    Science.gov (United States)

    Xia, Qinghai; Yang, Yaling; Liu, Mousheng

    2012-10-01

    An aluminium sensitized spectrofluorimetric method coupled with salting-out assisted liquid-liquid ultrasonic extraction for the determination of four widely used fluoroquinolones (FQs) namely norfloxacin (NOR), ofloxacin (OFL), ciprofloxacin (CIP) and gatifloxacin (GAT) in bovine raw milk was described. The analytical procedure involves the fluorescence sensitization of aluminium (Al3+) by complexation with FQs, salting-out assisted liquid-liquid ultrasonic extraction (SALLUE), followed by spectrofluorometry. The influence of several parameters on the extraction (the salt species, the amount of salt, pH, temperature and phase volume ratio) was investigated. Under optimized experimental conditions, the detection limits of the method in milk varied from 0.009 μg/mL for NOR to 0.016 μg/mL for GAT (signal-to-noise ratio (S/N) = 3). The relative standard deviations (RSD) values were found to be relatively low (0.54-2.48% for four compounds). The calibration graph was linear from 0.015 to 2.25 μg/mL with coefficient of determinations not less than 0.9974. The methodology developed was applied to the determination of FQs in bovine raw milk samples. The main advantage of this method is simple, accurate and green. The method showed promising applications for analyzing polar analytes especially polar drugs in various sample matrices.

  20. Simultaneous Distillation Extraction of Some Volatile Flavor Components from Pu-erh Tea Samples—Comparison with Steam Distillation-Liquid/Liquid Extraction and Soxhlet Extraction

    Directory of Open Access Journals (Sweden)

    Xungang Gu

    2009-01-01

    Full Text Available A simutaneous distillation extraction (SDE combined GC method was constructed for determination of volatile flavor components in Pu-erh tea samples. Dichloromethane and ethyl decylate was employed as organic phase in SDE and internal standard in determination, respectively. Weakly polar DB-5 column was used to separate the volatile flavor components in GC, 10 of the components were quantitatively analyzed, and further confirmed by GC-MS. The recovery covered from 66.4%–109%, and repeatability expressed as RSD was in range of 1.44%–12.6%. SDE was most suitable for the extraction of the anlytes by comparing with steam distillation-liquid/liquid extraction and Soxhlet extraction. Commercially available Pu-erh tea samples, including Pu-erh raw tea and ripe tea, were analyzed by the constructed method. the high-volatile components, such as benzyl alcohol, linalool oxide, and linalool, were greatly rich in Pu-erh raw teas, while the contents of 1,2,3-Trimethoxylbenzene and 1,2,4-Trimethoxylbenzene were much high in Pu-erh ripe teas.

  1. Factors influencing the thermodynamic isotope effect of lithium in polyetherlithium liquid-liquid extraction systems

    International Nuclear Information System (INIS)

    Fu Lian; Fang Shengqiang; Yao Zhongqi; Gao Zhichang; Tan Ganzhu

    1989-01-01

    The published data up to now concerning polyether-lithium liquid-liquid extraction systems, can be summarized by the equation, ε p = (α-1)/[1 + 0.46(1-P)], where α denotes the isotope separation factor; P - the ratio of the lithium concentration in the organic phase to the initial concentration of crown ethers; ε p -the enrichment coefficient as P = 100%. Based on the changes in ε p , P, α and D(distribution ratio), the functions of factors such as polyether's structure, polyether's side group, polyether's concentration, organic solvent, negative ion of lithium salt and lithium salt's concentration, are discussed and reported

  2. The coupling of rapidly synergistic cloud point extraction with thermospray flame furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Wen, X.; Deng, Q.; Guo, J.; Zhao, X.; Zhao, Y.; Ji, S.

    2012-01-01

    Rapidly synergistic cloud point extraction (RS-CPE) was coupled with thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) to result in new CPE patterns and accelerated (1 min) protocols. It is demonstrated, for the case of copper (II) ion, that TS-FF-AAS improves the sampling efficiency and the sensitivity of FAAS determinations. Problems of nebulization associated with previous methods based on the coupling of FAAS and RS-CPE are overcome. TS-FF-AAS also improves sensitivity and gives a limit of detection for copper of 0.20 μg L -1 , which is better by a factor of 32. Compared to direct FAAS, the factor is 114. (author)

  3. Application of ionic liquids based enzyme-assisted extraction of chlorogenic acid from Eucommia ulmoides leaves

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Tingting; Sui, Xiaoyu, E-mail: suixiaoyu@outlook.com; Li, Li; Zhang, Jie; Liang, Xin; Li, Wenjing; Zhang, Honglian; Fu, Shuang

    2016-01-15

    A new approach for ionic liquid based enzyme-assisted extraction (ILEAE) of chlorogenic acid (CGA) from Eucommia ulmoides is presented in which enzyme pretreatment was used in ionic liquids aqueous media to enhance extraction yield. For this purpose, the solubility of CGA and the activity of cellulase were investigated in eight 1-alkyl-3-methylimidazolium ionic liquids. Cellulase in 0.5 M [C6mim]Br aqueous solution was found to provide better performance in extraction. The factors of ILEAE procedures including extraction time, extraction phase pH, extraction temperatures and enzyme concentrations were investigated. Moreover, the novel developed approach offered advantages in term of yield and efficiency compared with other conventional extraction techniques. Scanning electronic microscopy of plant samples indicated that cellulase treated cell wall in ionic liquid solution was subjected to extract, which led to more efficient extraction by reducing mass transfer barrier. The proposed ILEAE method would develope a continuous process for enzyme-assisted extraction including enzyme incubation and solvent extraction process. In this research, we propose a novel view for enzyme-assisted extraction of plant active component, besides concentrating on enzyme facilitated cell wall degradation, focusing on improvement of bad permeability of ionic liquids solutions. - Highlights: • An ionic liquid based enzyme-assisted extraction method of natural product was explored. • ILEAE utilizes enzymatic treatment to improve permeability of ionic liquids solution. • Enzyme incubation and solvent extraction process were ongoing simultaneously. • ILEAE process simplified operating process and suitable for more complete extraction.

  4. Application of ionic liquids based enzyme-assisted extraction of chlorogenic acid from Eucommia ulmoides leaves

    International Nuclear Information System (INIS)

    Liu, Tingting; Sui, Xiaoyu; Li, Li; Zhang, Jie; Liang, Xin; Li, Wenjing; Zhang, Honglian; Fu, Shuang

    2016-01-01

    A new approach for ionic liquid based enzyme-assisted extraction (ILEAE) of chlorogenic acid (CGA) from Eucommia ulmoides is presented in which enzyme pretreatment was used in ionic liquids aqueous media to enhance extraction yield. For this purpose, the solubility of CGA and the activity of cellulase were investigated in eight 1-alkyl-3-methylimidazolium ionic liquids. Cellulase in 0.5 M [C6mim]Br aqueous solution was found to provide better performance in extraction. The factors of ILEAE procedures including extraction time, extraction phase pH, extraction temperatures and enzyme concentrations were investigated. Moreover, the novel developed approach offered advantages in term of yield and efficiency compared with other conventional extraction techniques. Scanning electronic microscopy of plant samples indicated that cellulase treated cell wall in ionic liquid solution was subjected to extract, which led to more efficient extraction by reducing mass transfer barrier. The proposed ILEAE method would develope a continuous process for enzyme-assisted extraction including enzyme incubation and solvent extraction process. In this research, we propose a novel view for enzyme-assisted extraction of plant active component, besides concentrating on enzyme facilitated cell wall degradation, focusing on improvement of bad permeability of ionic liquids solutions. - Highlights: • An ionic liquid based enzyme-assisted extraction method of natural product was explored. • ILEAE utilizes enzymatic treatment to improve permeability of ionic liquids solution. • Enzyme incubation and solvent extraction process were ongoing simultaneously. • ILEAE process simplified operating process and suitable for more complete extraction.

  5. Ionic liquid foam floatation coupled with ionic liquid dispersive liquid-liquid microextraction for the separation and determination of estrogens in water samples by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Zhang, Rui; Wang, Chuanliu; Yue, Qiaohong; Zhou, Tiecheng; Li, Na; Zhang, Hanqi; Hao, Xiaoke

    2014-11-01

    An ionic liquid foam floatation coupled with ionic liquid dispersive liquid-liquid microextraction method was proposed for the extraction and concentration of 17-α-estradiol, 17-β-estradiol-benzoate, and quinestrol in environmental water samples by high-performance liquid chromatography with fluorescence detection. 1-Hexyl-3-methylimidazolium tetrafluoroborate was applied as foaming agent in the foam flotation process and dispersive solvent in microextraction. The introduction of the ion-pairing and salting-out agent NH4 PF6 was beneficial to the improvement of recoveries for the hydrophobic ionic liquid phase and analytes. Parameters of the proposed method including concentration of 1-hexyl-3-methylimidazolium tetrafluoroborate, flow rate of carrier gas, floatation time, types and concentration of ionic liquids, salt concentration in samples, extraction time, and centrifugation time were evaluated. The recoveries were between 98 and 105% with relative standard deviations lower than 7% for lake water and well water samples. The isolation of the target compounds from the water was found to be efficient, and the enrichment factors ranged from 4445 to 4632. This developing method is free of volatile organic solvents compared with regular extraction. Based on the unique properties of ionic liquids, the application of foam floatation, and dispersive liquid-liquid microextraction was widened. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Separation of uranium from aqueous solutions using calix[6]arenes in liquid-liquid extraction as well as solid phase extraction

    International Nuclear Information System (INIS)

    Schmeide, K.; Geipel, G.; Bernhard, G.

    2004-11-01

    The suitability of different calyx[n] arene types for uranyl extraction from liquid solutions was examined by means of liquid-liquid extraction using aqueous phases and organic solvents of varying compositions. It was found that COOH-derivatised calyx[6] arenes have good extraction properties and can even be used in the acid pH range. The use of calixarene-modified fleeces for the separation of uranyl from aqueous phases was examined in batch experiments with pH and uranyl concentration as variables and in the presence or absence of competing ions. The results showed that calixarene-modified fleeces can be used for uranium separation starting from pH 4. At pH 5, up to a maximum of 7.6 x 10 -7 mol uranium can be bound per 1 g of calixarene-modified fleece. The separation of uranyl from synthetic pit waters was examined as a means of testing the separation capacity of calixarene-modified fleeces in environmentally sensitive waters. Studies on the reversibility of uranium bonding to calixarene-treated polyester fleeces have shown that under environmentally realistic conditions (neutral pH range) the uranium is firmly bound to the calixarene-modified fleeces and cannot be mobilised. By contrast, in acidic environments calixarene-modified fleeces are capable of near-complete regeneration. Such regenerated textile filter materials can then be used for further uranium separation cycles [de

  7. Synergistic effect of dicarbollide anions in liquid-liquid extraction: a molecular dynamics study at the octanol-water interface.

    Science.gov (United States)

    Chevrot, G; Schurhammer, R; Wipff, G

    2007-04-28

    We report a molecular dynamics study of chlorinated cobalt bis(dicarbollide) anions [(B(9)C(2)H(8)Cl(3))(2)Co](-)"CCD(-)" in octanol and at the octanol-water interface, with the main aim to understand why these hydrophobic species act as strong synergists in assisted liquid-liquid cation extraction. Neat octanol is quite heterogeneous and is found to display dual solvation properties, allowing to well solubilize CCD(-), Cs(+) salts in the form of diluted pairs or oligomers, without displaying aggregation. At the aqueous interface, octanol behaves as an amphiphile, forming either monolayers or bilayers, depending on the initial state and confinement conditions. In biphasic octanol-water systems, CCD(-) anions are found to mainly partition to the organic phase, thus attracting Cs(+) or even more hydrophilic counterions like Eu(3+) into that phase. The remaining CCD(-) anions adsorb at the interface, but are less surface active than at the chloroform interface. Finally, we compare the interfacial behavior of the Eu(BTP)(3)(3+) complex in the absence and in the presence of CCD(-) anions and extractant molecules. It is found that when the CCD(-)'s are concentrated enough, the complex is extracted to the octanol phase. Otherwise, it is trapped at the interface, attracted by water. These results are compared to those obtained with chloroform as organic phase and discussed in the context of synergistic effect of CCD(-) in liquid-liquid extraction, pointing to the importance of dual solvation properties of octanol and of the hydrophobic character of CCD(-) for synergistic extraction of cations.

  8. A new dispersive liquid-liquid microextraction using ionic liquid based microemulsion coupled with cloud point extraction for determination of copper in serum and water samples.

    Science.gov (United States)

    Arain, Salma Aslam; Kazi, Tasneem Gul; Afridi, Hassan Imran; Arain, Mariam Shahzadi; Panhwar, Abdul Haleem; Khan, Naeemullah; Baig, Jameel Ahmed; Shah, Faheem

    2016-04-01

    A simple and rapid dispersive liquid-liquid microextraction procedure based on ionic liquid assisted microemulsion (IL-µE-DLLME) combined with cloud point extraction has been developed for preconcentration copper (Cu(2+)) in drinking water and serum samples of adolescent female hepatitits C (HCV) patients. In this method a ternary system was developed to form microemulsion (µE) by phase inversion method (PIM), using ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate ([C4mim][PF6]) and nonionic surfactant, TX-100 (as a stabilizer in aqueous media). The Ionic liquid microemulsion (IL-µE) was evaluated through visual assessment, optical light microscope and spectrophotometrically. The Cu(2+) in real water and aqueous acid digested serum samples were complexed with 8-hydroxyquinoline (oxine) and extracted into IL-µE medium. The phase separation of stable IL-µE was carried out by the micellar cloud point extraction approach. The influence of of different parameters such as pH, oxine concentration, centrifugation time and rate were investigated. At optimized experimental conditions, the limit of detection and enhancement factor were found to be 0.132 µg/L and 70 respectively, with relative standard deviation <5%. In order to validate the developed method, certified reference materials (SLRS-4 Riverine water) and human serum (Sero-M10181) were analyzed. The resulting data indicated a non-significant difference in obtained and certified values of Cu(2+). The developed procedure was successfully applied for the preconcentration and determination of trace levels of Cu(2+) in environmental and biological samples. Copyright © 2015 Elsevier Inc. All rights reserved.

  9. Solid-Phase Extraction Combined with High Performance Liquid ...

    African Journals Online (AJOL)

    Methods: Solid-phase extraction method was employed for the extraction of the estrogen from milk and high performance liquid chromatography-diode array detector (HPLC-DAD) was used for the determination of estrogen. Results: Optimal chromatographic conditions were achieved on an Eclipse XDB-C18 column at a ...

  10. Liquid-liquid extraction of U(VI), Np(V) et Th(IV) ions by two calix[4]arene carboxyls, and effect of Na+ and K+ alkaline ions

    International Nuclear Information System (INIS)

    Montavon, Gilles

    1996-01-01

    As the process mainly used for the reprocessing of nuclear wastes was the Purex process, this research thesis first presents this process and outlines that it allows the residual fissile matter to be recovered and reused for the fabrication of new fuel elements, but is neither efficient nor safe enough to separate fission and activation products. Thus, this thesis reports the study of extraction and selectivity properties of two compounds derived from the p-tert-butyl-calix[4]arene with respect to actinide ions such as Th(IV), U(VI) and Np(VI). The liquid-liquid extraction technique has been used with chloroform and 1,2-dichloroethane as solvents. After some generalities on actinides, calixarenes and the liquid-liquid extraction technique, and a presentation of the experimental method, the author reports and discusses the extractive properties of the studied calixarenes with respect to Na + and K + ions. Structural studies by proton NMR have been performed. He reports and discusses the liquid-liquid extraction on actinide ions when they are alone or in presence on Na + and K + alkaline ions [fr

  11. Determination of trace amount of lead in industrial and municipal effluent water samples based on dispersive liquid-liquid extraction

    International Nuclear Information System (INIS)

    Shirkhanloo, H.; Sedighi, K.; Mousavi, H. Z.

    2014-01-01

    In this study, a simple, sensitive and accurate method was developed for the determination of lead ion by combining ionic liquid dispersive liquid-liquid extraction (Il-DLL E) with flame atomic absorption spectrometry. Tetraethyl thiuram disulfide (Tetd), acetone and 1-octyl-3m ethylimidazolium hexafluorophosphate [(C 8 MIM) (PF 6 )] were used as the chelating agent, dispersive and extraction solvent, respectively. Under the optimal conditions, the calibration graph was linear in the range of 5-190 μg L -1 of lead and the detection limit was 0.8 μg L -1 with a sample volume of 200 ml. The proposed method was validated by the analysis of one certified reference material and applied successfully to the determination of lead in real water samples. (Author)

  12. A rapid method to estimate uranium using ionic liquid as extracting agent from basic aqueous media

    International Nuclear Information System (INIS)

    Prabhath Ravi, K.; Sathyapriya, R.S.; Rao, D.D.; Ghosh, S.K.

    2016-01-01

    Room temperature ionic liquids, as their name suggests are salts with a low melting point typically less than 100 °C and exist as liquid at room temperature. The common cationic parts of ionic liquids are imidazolium, pyridinium, pyrrolidinium, quaternary ammonium, or phosphonium ions, and common anionic parts are chloride, bromide, boron tetrafluorate, phosphorous hexafluorate, triflimide etc. The physical properties of ionic liquids can be tuned by choosing appropriate cations with differing alkyl chain lengths and anions. Application of ionic liquids in organic synthesis, liquid-liquid extractions, electrochemistry, catalysis, speciation studies, nuclear reprocessing is being studied extensively in recent times. In this paper a rapid method to estimate the uranium content in aqueous media by extraction with room temperature ionic liquid tricaprylammoniumthiosalicylate ((A- 336)(TS)) followed by liquid scintillation analysis is described. Re-extraction of uranium from ionic liquid phase to aqueous phase was also studied

  13. Microwave-assisted ionic liquid homogeneous liquid-liquid microextraction coupled with high performance liquid chromatography for the determination of anthraquinones in Rheum palmatum L.

    Science.gov (United States)

    Wang, Zhibing; Hu, Jianxue; Du, Hongxia; He, Shuang; Li, Qing; Zhang, Hanqi

    2016-06-05

    The microwave-assisted ionic liquid homogeneous liquid-liquid microextraction (MA-IL-HLLME) coupled with high performance liquid chromatography with diode array detection (HPLC-DAD) was developed for the determination of anthraquinones, including aloe-emodin, emodin, chrysophanol and physcion in root of Rheum palmatum L. Several experimental parameters influencing the extraction efficiency, including amount of sample, type and volume of ionic liquid, volume and pH value of extraction medium, microwave power and extraction time, concentration of NH4PF6 as well as centrifugal condition were optimized. When 140μL of ionic liquid ([C8MIM][BF4]) was used as an extraction solvent, target analytes can be extracted from sample matrix in one minute with the help of microwave irradiation. The MA-IL-HLLME is simple and quick. The calibration curves exhibited good linear relationship (r>0.9984). The limits of detection and quantification were in the range of 0.015-0.026 and 0.051-0.088μgmL(-1), respectively. The spiked recovery for each analyte was in the range of 81.13-93.07% with relative standard deviations lower than 6.89%. The present method is free of volatile organic solvents, and represents lower expenditures of sample, extraction time and solvent, compared with ultrasonic and heat reflux extraction. The results indicated that the present method can be successfully applied to the determination of anthraquinones in medicinal plant. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Liquid-Liquid Extraction and Determination of Trace Elements in Iron Minerals by Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    Taseska, Milena; Stafilov, Trajche; Makreski, Petre; Jacimovic, Radojko; Jovanovski, Gligor

    2006-01-01

    Various trace elements (cadmium, chromium, cobalt, nickel, manganese) in some iron minerals were determined by flame (FAAS) and electrothermal atomic absorption spectrometry (ETAAS). The studied minerals were chalcopyrite (CuFeS 2 ), hematite (Fe 2 O 3 ) and pyrite (FeS 2 ). To avoid the interference of iron, a method for liquid-liquid extraction of iron and determination of investigated elements in the inorganic phase was proposed. Iron was extracted by diisopropyl ether in hydrochloride acid solution and the extraction method was optimized. Some parameters were obtained to be significantly important: Fe mass in the sample should not exceed 0.3 g, the optimal concentration of HCI should be 7.8 mol 1 -1 and ratio of the inorganic and organic phase should be 1: 1. The procedure was verified by the method of standard additions and by its applications to reference standard samples. The investigated minerals originate from various mines in the Republic of Macedonia. (Author)

  15. The status of research on CFD-PBM simulation of liquid-liquid two-phase flow in extraction columns

    International Nuclear Information System (INIS)

    Li Shaowei; Jing Shan; Wu Qiulin; Zhang Qi

    2012-01-01

    Computational fluid dynamics (CFD) simulation has gained more and more interest in the chemical engineering researchers and is becoming a useful tool for the chemical engineering research. The research on liquid-liquid two-phase flow CFD simulation in extraction columns is now in its initial stage. There is much work to do for the developing of this research field. The purpose of this article is to review the CFD simulation methods for two-phase flow in extraction column. The population balance model (PBM) is detailedly described in this article because it is the main method used in the two-phase flow CFD simulation currently. Then some examples for the two-phase flow simulation in extraction columns are briefly introduced. The strategy for the research on CFD simulation of two-phase flow in extraction columns is suggested at last. (authors)

  16. Quantification of four ionophores in soil, sediment and manure using pressurised liquid extraction

    DEFF Research Database (Denmark)

    Bak, Søren Alex; Hansen, Martin; Pedersen, Kenneth Munk

    2013-01-01

    A multi-residue pressurised liquid extraction (PLE) methodology has been established for the determination of the four ionophores: lasalocid, monensin, salinomycin and narasin in solid environmental matrices. The PLE methodology is combined with solid phase extraction as clean-up using liquid...

  17. Extraction of plutonium(IV) by diglycolamide extractants in room temperature ionic liquids

    Energy Technology Data Exchange (ETDEWEB)

    Prabhu, Dattaprasad R.; Raut, Dhaval R.; Murali, Mallekav S.; Mohapatra, Prasanta K. [Bhabha Atomic Research Centre, Mumbai (India). Radiochemistry Div.

    2017-06-01

    Extraction of Pu(IV) was investigated using solutions of two diglycolamide extractants viz., N,N,N{sup '},N{sup '}-tetra-n-octyldiglycolamide (TODGA) and its branched homolog, N,N,N{sup '},N{sup '}-tetra(2-ethylhexyl) diglycolamide (T2EHDGA), dissolved in two imidazolium based room temperature ionic liquids viz., 1-butyl-3-methylimidazolium bis(trifluoromethanesulphonyl) imide ([C{sub 4}mim][NTf{sub 2}]) and 1-octyl-3-methylimidazolium bis(trifluoromethanesulphonyl) imide ([C{sub 8}mim][NTf{sub 2}]) from aqueous nitric acid medium. The extraction kinetics was found to be extremely slow which is reported for the first time for analogous extraction systems and took as long as 30 h to attain equilibrium D{sub Pu} values. In general, TODGA based solvents showed better extraction of Pu(IV) than the T2EHDGA based solvents, one order of magnitude higher, and though both the ionic liquids ultimately yielded comparable D{sub Pu} values, attainment of equilibrium was slower with [C{sub 4}mim][NTf{sub 2}]. The extracted species conformed to 1:1 for TODGA in both the ionic liquids while a mixture of 1:1 and 1:2 species was observed for T2EHDGA at 1 M HNO{sub 3} which changed to 1:1 species at 4 M HNO{sub 3}. The extracted species is proposed to be (Pu(L){sub x}{sup 4+}){sub IL} (where, L is the extractant and x=1 or 2) at lower acidities suggesting a cation exchange mechanism which changes over to (Pu(NO{sub 3}){sub 4} .L){sub IL} at 4 M HNO{sub 3} conforming to a solvation mechanism for all the systems except for T2EHDGA-[C{sub 8}mim][NTf{sub 2}]. UV-VIS spectroscopic studies were carried out to throw light on the nature of the extracted species.

  18. Liquid-liquid extraction of uranium from nitric acid solution using di-n-butylsulfoxide in petroleum ether as extractant

    Energy Technology Data Exchange (ETDEWEB)

    Khan, M.H.; Shahida, S. [Dept. of Chemistry, Univ. of Azad Jammu and Kashmir, Muzaffarabad (Pakistan); Ali, A. [Nuclear Chemistry Div., Pakistan Inst. of Nuclear Science and Technology, Nilore, Islamabad (Pakistan)

    2008-07-01

    A simple, efficient and economical liquid-liquid extraction method has been developed for quantitative extraction of uranium from 2 M HNO{sub 3} using di-n-butyl sulfoxide in petroleum ether. The dependence of the partition reaction of U(VI) on the concentration of HNO{sub 3}, extractant and temperature was studied. The reaction was found to be inversely dependent upon the temperature and the values for related thermodynamics functions ({delta}H, {delta}S, {delta}G) for extraction equilibrium were determined to be -33.6 kJ/mol, -1.29 kJ/mol/degree and -0.11 kJ/mol/degree, respectively. The effect of Al(NO{sub 3}){sub 3} as salting-out agent and diverse ions on the extraction was examined. The salting-out agent slightly enhanced the extraction. All cations studied have showed negligible effect on the extraction, whereas phosphate and fluoride interfered seriously. Among others, oxalate, citrate and sulphide ions affect the extraction to a lesser extent. Uranium was successfully extracted from a synthetic mixture of Ti{sup +4}, Zr{sup +4}, Hf{sup +4} and Th{sup +4} using EDTA as masking agent. Among strippants, deionized water was found most suitable, and the recovery of uranium was noted to be {>=} 96%. The stoichiometric composition of the extracted species was found to be UO{sub 2}(NO{sub 3}){sub 2} . 2DBSO. The extraction mechanism is discussed on the basis of the results obtained. The extractant has high loading as well as recycling capacity without any degradation. The method was also applied to the Standard Reference Material (NBL-49) and the measured value was found to be in agreement with the reported value within {+-}2% deviation. (orig.)

  19. Study on the extraction of rare earth elements in liquid bismuth

    International Nuclear Information System (INIS)

    Harada, M.; Adachi, M.; Kai, Y.; Koike, K.

    1987-01-01

    Three factors, which are important for the extraction of rare earth elements in liquid bismuth - molten salt system, were studied, i. e., the equilibrium distribution of neodymium, samarium and bismuth between molten LiCl - liquid Bi-Li alloys, the extraction rate of rare earths, and the characteristics of the extractor with drop dispersion. The rare earth elements were extracted through redox reactions. In high range of Li-mole fraction in the alloy phase, X Li , the distribution of neodymium and bismuth in the salt phase markedly increased as X Li increased. The anomalous increase is attributed to the formation of the compound comprised of Nd, Li, Bi and oxygen in the salt phase. The redox reaction processes were very fast and the extraction rates for rare earths are controlled by the diffusion processes of the solute and the metallic lithium. The process for the formation of liquid metal drops in the continuous phase is predictable from semiempirical correlations reported for aqueous solution - organic solvent systems. The height of droplet bed being accumulated on drop settling portion is predictable from the coalescence time of single drop to a flat metal interface. The coalescence of metal drop to clean interface was very fast. The extractor type of liquid metal dispersion in molten salt is suitable for the extraction process in the fuel reprocessing of MSR or MSBR. (author)

  20. Novel materials and methods for solid-phase extraction and liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Ambrose, Diana [Iowa State Univ., Ames, IA (United States)

    1997-06-24

    This report contains a general introduction which discusses solid-phase extraction and solid-phase micro-extraction as sample preparation techniques for high-performance liquid chromatography, which is also evaluated in the study. This report also contains the Conclusions section. Four sections have been removed and processed separately: silicalite as a sorbent for solid-phase extraction; a new, high-capacity carboxylic acid functionalized resin for solid-phase extraction; semi-micro solid-phase extraction of organic compounds from aqueous and biological samples; and the high-performance liquid chromatographic determination of drugs and metabolites in human serum and urine using direct injection and a unique molecular sieve.

  1. Hollow fibre supported liquid membrane extraction of ...

    African Journals Online (AJOL)

    A simple sample pre-treatment method utilizing hollow fibre supported liquid membrane (HFSLM) was carried out on pharmaceuticals samples comprising of cough syrups (CS1 and CS2) and an anti-inflammatory product (AI). The active ingredients targeted in the extraction process were diphenylhydramine (DPH), ...

  2. Simple and Rapid Dual-Dispersive Liquid-Liquid Microextraction as an Innovative Extraction Method for Uranium in Real Water Samples Prior to the Determination of Uranium by a Spectrophotometric Technique.

    Science.gov (United States)

    Khan, Naeemullah; Tuzen, Mustafa; Kazi, Tasneem Gul

    2017-11-01

    An innovative, rapid, and simple dual-dispersive liquid-liquid microextraction (DDLL-ME) approach was used to extract uranium from real samples for the first time. The main objective of this study was to disperse extraction solvent by using an air-agitated syringe system to overcome matrix effects and avoid dispersion of hazardous dispersive organic solvents by using heat. The DDLL-ME method consisted of two dispersive liquid-liquid extraction steps with chloroform as the extracting solvent. Uranium formed complexes with 4-(2-thiazolylazo) resorcinol in the aqueous phase and was extracted in extracting solvent (chloroform) after the first dispersive liquid-liquid process. Uranium was then back-extracted in the acidic aqueous phase in a second dispersive liquid-liquid process. Finally, uranium was determined by a spectrophotometric detection technique. The variables that played a key role in the proposed method were studied and optimized. The LOD and sensitivity enhancement factor for uranium were found to be 0.60 µg/L and 45, respectively, under optimized conditions. Calibration graphs were found to be linear in the range of 5.0-600 µg/L. The RSD was 2.5%. Reliability of the proposed method was verified by analyzing certified reference material TM-28.3.

  3. Determination of trace amount of lead in industrial and municipal effluent water samples based on dispersive liquid-liquid extraction

    Energy Technology Data Exchange (ETDEWEB)

    Shirkhanloo, H. [Iranian Petroleum Industry Health Research Institute, Occupational and Environmental Health Research Center, Tehran (Iran, Islamic Republic of); Sedighi, K.; Mousavi, H. Z., E-mail: hzmousavi@semnan.ac.ir [Semnan University, College of Science, Department of Chemistry, Semnan (Iran, Islamic Republic of)

    2014-10-01

    In this study, a simple, sensitive and accurate method was developed for the determination of lead ion by combining ionic liquid dispersive liquid-liquid extraction (Il-DLL E) with flame atomic absorption spectrometry. Tetraethyl thiuram disulfide (Tetd), acetone and 1-octyl-3m ethylimidazolium hexafluorophosphate [(C{sub 8}MIM) (PF{sub 6})] were used as the chelating agent, dispersive and extraction solvent, respectively. Under the optimal conditions, the calibration graph was linear in the range of 5-190 μg L{sup -1} of lead and the detection limit was 0.8 μg L{sup -1} with a sample volume of 200 ml. The proposed method was validated by the analysis of one certified reference material and applied successfully to the determination of lead in real water samples. (Author)

  4. Metabolite Extraction from Saccharomyces cerevisiae for Liquid Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Rosebrock, Adam P; Caudy, Amy A

    2017-09-01

    Prior to mass spectrometric analysis, cellular small molecules must be extracted and separated from interfering components such as salts and culture medium. To ensure minimal perturbation of metabolism, yeast cells grown in liquid culture are rapidly harvested by filtration as described here. Simultaneous quenching of metabolism and extraction is afforded by immediate immersion in low-temperature organic solvent. Samples prepared using this method are suitable for a range of downstream liquid chromatography-mass spectrometry analyses and are stable in solvent for >1 yr at -80°C. © 2017 Cold Spring Harbor Laboratory Press.

  5. Uranium extraction process in a sulfuric medium by means of liquid emulsified membranes

    International Nuclear Information System (INIS)

    Monteillet, A.

    1985-02-01

    Uranium ore processing, after leaching by sulfuric acid, by liquid-liquid extraction is a rather heavy process, not suitable for small deposits. Extraction by emulsions was suggested. In this process the leachate is contacted with an oil in water type emulsion, a liquid organic membrane is formed by the continuous phase. Uranium complexes diffuse through the liquid membrane towards the dispersed aqueous phase of the emulsion (stripping solution). Uranium is recovered by breaking the emulsion. Are successively studied: development of stable emulsions, influence of emulsion composition on uranium transfer kinetics, transfer mechanisms through the membrane and modelling of kinetics data obtained in the experimental study [fr

  6. Application of ionic liquid for extraction and separation of bioactive compounds from plants.

    Science.gov (United States)

    Tang, Baokun; Bi, Wentao; Tian, Minglei; Row, Kyung Ho

    2012-09-01

    In recent years, ionic liquids (ILs), as green and designer solvents, have accelerated research in analytical chemistry. This review highlights some of the unique properties of ILs and provides an overview of the preparation and application of IL or IL-based materials to extract bioactive compounds in plants. IL or IL-based materials in conjunction with liquid-liquid extraction (LLE), ultrasonic-assisted extraction (UAE), microwave-assisted extraction (MAE), high performance liquid chromatography (HPLC) and solid-phase extraction (SPE) analytical technologies etc., have been applied successfully to the extraction or separation of bioactive compounds from plants. This paper reviews the available data and references to examine the advantages of IL and IL-based materials in these applications. In addition, the main target compounds reviewed in this paper are bioactive compounds with multiple therapeutic effects and pharmacological activities. Based on the importance of the targets, this paper reviews the applications of ILs, IL-based materials or co-working with analytical technologies. The exploitation of new applications of ILs on the extraction of bioactive compounds from plant samples is expected to increase. Copyright © 2012 Elsevier B.V. All rights reserved.

  7. CHEMOMETRICS IN BIOANALYTICAL SAMPLE PREPARATION - A FRACTIONATED COMBINED MIXTURE AND FACTORIAL DESIGN FOR THE MODELING OF THE RECOVERY OF 5 TRICYCLIC AMINES FROM PLASMA AFTER LIQUID-LIQUID-EXTRACTION PRIOR TO HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY

    NARCIS (Netherlands)

    WIELING, J; MENSINK, CK; JONKMAN, JHG; COENEGRACHT, PMJ; DUINEVELD, CAA; DOORNBOS, DA

    1993-01-01

    A general systematic approach is described for the chemometric modelling of liquid-liquid extraction data of drugs from biological fluids. Extraction solvents were selected from Snyder's solvent selectivity triangle: methyl tert.-butyl ether, methylene chloride and chloroform. The composition of a

  8. Liquid-liquid extraction and separation of VIII group elements, especially ruthenium, by synergic combinations or aromatic polyimines and micellar cationic exchangers

    International Nuclear Information System (INIS)

    Vitart, X.

    1991-01-01

    This thesis aims to characterize and to quantify the chemical equilibria involved in d-elements liquid-liquid extraction systems, especially elements belonging to the VIII group (Fe, Ni, Co, Ru, Rh, Pd, Pt). These systems are composed of synergic combination of aromatic polyimines and micellar cationic exchangers. Substitutions are first performed in aqueous acidic media by aromatic polyimines; then extractions are operated using micellic canionic exchangers. Chemical equilibria, selectivity effects, especially those due to ion-pair formations, kinetics, extractant behaviour are analysed and quantified [fr

  9. Quaternary ammonium based task specific ionic liquid for the efficient and selective extraction of neptunium

    Energy Technology Data Exchange (ETDEWEB)

    Gupta, Nishesh Kumar [National Institute of Technology, Odisha (India). Dept. of Chemistry; Sengupta, Arijit [Bhabha Atomic Research Centre, Mumbai (India). Radiochemistry Div.; Biswas, Sujoy [Bhabha Atomic Research Centre, Mumbai (India). Uranium Extraction Div.

    2017-07-01

    Liquid-liquid extraction of neptunium from aqueous acidic solution using quaternary ammonium based task specific ionic liquid (TSIL) was investigated. The extraction of Np was predominated by the 'cation exchange' mechanism via [NpO{sub 2}.Hpth]{sup +} species for NpO{sub 2}{sup 2+}, while NpO{sub 2}{sup +} was extracted in ionic liquid as [NpO{sub 2}.H.Hpth]{sup +}. The extraction process was thermodynamically spontaneous while kinetically slower. Na{sub 2}CO{sub 3} as strippant showed quantitative back extraction of neptunium ions from TSIL. TSIL showed excellent radiolytic stability upto 500 kGy gamma exposure. Finally, the TSIL was employed for the processing of simulated high level waste solutions revealing high selectivity of TSIL towards neptunium.

  10. The liquid membrane for extraction of Yttrium and Dysprosium from Acid Nitric

    International Nuclear Information System (INIS)

    Johny, W.S.; Raldi-Artono-Koestoer; Kris-Tri-Basuki; Sudibyo

    1996-01-01

    The determination of surfactant in liquid membrane has been done. The surfactant is span-80 (sorbitol-monooleate), the liquid membrane phase was the organic phase (O), the internal liquid phase (W) with ratio O/W = 1, and surfactant. The organic phase using D 2 EHPA in the kerosene and the internal liquid phase using aqua des or acid nitric. The determination of surfactant with variation of span-80 (0,25 - 2%) in the liquid membrane volume. The speed of stirrer was 3500 rpm in 20 minute. The ratio of liquid membrane phase form and external phase (aqua des or acid nitric) was 1, the speed of stirrer was 350 rpm in 10 minute (permeation process). The liquid phase and the liquid membrane phase was separated and then determinated the volume of liquid membrane, the result of percentage of span-80 was 0,25 % volume. The extraction of yttrium and dysprosium in 2 M HNO 3 was Kd y = 2.945 and Kd D y = 0.019

  11. Solvent Extraction: Structure of the Liquid-Liquid Interface Containing a Diamide Ligand

    Energy Technology Data Exchange (ETDEWEB)

    Scoppola, Ernesto [Institut Laue-Langevin, 38000 Grenoble France; Institut de Chimie Séparative de Marcoule, UMR 5257 CEA/CNRS/ENSCM/Université Montpellier, 30207 Bagnols-sur-Cèze France; Watkins, Erik B. [Institut Laue-Langevin, 38000 Grenoble France; Materials Synthesis and Integrated Devices, Los Alamos National Laboratory, Los Alamos NM 87545 USA; Campbell, Richard A. [Institut Laue-Langevin, 38000 Grenoble France; Konovalov, Oleg [European Synchrotron Radiation Facility, 38430 Grenoble France; Girard, Luc [Institut de Chimie Séparative de Marcoule, UMR 5257 CEA/CNRS/ENSCM/Université Montpellier, 30207 Bagnols-sur-Cèze France; Dufrêche, Jean-Francois [Institut de Chimie Séparative de Marcoule, UMR 5257 CEA/CNRS/ENSCM/Université Montpellier, 30207 Bagnols-sur-Cèze France; Ferru, Geoffroy [Argonne National Labororatory, Lemont IL 60439 USA; Fragneto, Giovanna [Institut Laue-Langevin, 38000 Grenoble France; Diat, Olivier [Institut de Chimie Séparative de Marcoule, UMR 5257 CEA/CNRS/ENSCM/Université Montpellier, 30207 Bagnols-sur-Cèze France

    2016-06-20

    Knowledge of the (supra)molecular structure of an interface that contains amphiphilic ligand molecules is necessary for a full understanding of ion transfer during solvent extraction. Even if molecular dynamics already yield some insight in the molecular configurations in solution, hardly any experimental data giving access to distributions of both extractant molecules and ions at the liquid–liquid interface exist. Here, the combined application of X-ray and neutron reflectivity measurements represents a key milestone in the deduction of the interfacial structure and potential with respect to two different lipophilic ligands. Indeed, we show for the first time that hard trivalent cations can be repelled or attracted by the extractant-enriched interface according to the nature of the ligand.

  12. Studies on the liquid-liquid phase distribution equilibria of selenium and its measurement in water using extraction plant with a pulsation column

    International Nuclear Information System (INIS)

    Iskanderani, F.; Sobhi, K.M.; Ejaz, M.

    1989-01-01

    Normal heptane, xylene and a 0.01 molar solution of 4-(5-nonyl)pyridine in toluene were investigated as extractants for selenium(IV) from nitric acid media in potassium iodide. Various parameters affecting the distribution of the element are investigated. Extraction at high aqueous to organic phase volume ratio was studied, using a liquid-liquid extraction plant with a pulsation column. The results were employed to measure selenium in spiked water samples. (author) 24 refs.; 8 figs

  13. Extraction efficiency of hydrophilic and lipophilic antioxidants from lyophilized foods using pressurized liquid extraction and manual extraction.

    Science.gov (United States)

    Watanabe, Jun; Oki, Tomoyuki; Takebayashi, Jun; Takano-Ishikawa, Yuko

    2014-09-01

    The efficient extraction of antioxidants from food samples is necessary in order to accurately measure their antioxidant capacities. α-Tocopherol and gallic acid were spiked into samples of 5 lyophilized and pulverized vegetables and fruits (onion, cabbage, Satsuma mandarin orange, pumpkin, and spinach). The lipophilic and hydrophilic antioxidants in the samples were sequentially extracted with a mixed solvent of n-hexane and dichloromethane, and then with acetic acid-acidified aqueous methanol. Duplicate samples were extracted: one set was extracted using an automated pressurized liquid extraction apparatus, and the other set was extracted manually. Spiked α-tocopherol and gallic acid were recovered almost quantitatively in the extracted lipophilic and hydrophilic fractions, respectively, especially when pressurized liquid extraction was used. The expected increase in lipophilic oxygen radical absorbance capacity (L-ORAC) due to spiking with α-tocopherol, and the expected increase in 2,2-diphenyl-1-picrylhydrazyl radical scavenging activities and total polyphenol content due to spiking with gallic acid, were all recovered in high yield. Relatively low recoveries, as reflected in the hydrophilic ORAC (H-ORAC) value, were obtained following spiking with gallic acid, suggesting an interaction between gallic acid and endogenous antioxidants. The H-ORAC values of gallic acid-spiked samples were almost the same as those of postadded (spiked) samples. These results clearly indicate that lipophilic and hydrophilic antioxidants are effectively extracted from lyophilized food, especially when pressurized liquid extraction is used. © 2014 Institute of Food Technologists®

  14. Extraction of lithium ion from alkaline aqueous media by a liquid surfactant membrane

    International Nuclear Information System (INIS)

    Kinugasa, Takumi; Ono, Yuri; Kawamura, Yuko; Watanabe, Kunio; Takeuchi, Hiroshi.

    1995-01-01

    Extraction of lithium ion from aqueous alkaline media by a liquid surfactant membrane was performed using a mixture of LIX54 and TOPO as the extractant. Stripping of lithium from the kerosene solution to the acid solution was suppressed with increasing content of polyamine (ECA) surfactant. The extraction rate of lithium by the liquid membrane could be interpreted taking account of an interfacial resistance due to ECA. It was confirmed that swelling of the (W/O) emulsion drops by water permeation through the liquid membrane is evaluated in terms of a change in osmotic pressure gradient between the external and internal aqueous phases during the lithium extraction. In the present operation, the extraction ratio of Li + from the external feed and the uptake into the internal phase reached as high as 95%. (author)

  15. Detection of Organophosphorus Pesticides in Wheat by Ionic Liquid-Based Dispersive Liquid-Liquid Microextraction Combined with HPLC

    Directory of Open Access Journals (Sweden)

    Wei Liu

    2018-01-01

    Full Text Available Food safety issues closely related to human health have always received widespread attention from the world society. As a basic food source, wheat is the fundamental support of human survival; therefore, the detection of pesticide residues in wheat is very necessary. In this work, the ultrasonic-assisted ionic liquid-dispersive liquid-liquid microextraction (DLLME method was firstly proposed, and the extraction and analysis of three organophosphorus pesticides were carried out by combining high-performance liquid chromatography (HPLC. The extraction efficiencies of three ionic liquids with bis(trifluoromethylsulfonylimide (Tf2N anion were compared by extracting organophosphorus in wheat samples. It was found that the use of 1-octyl-3-methylimidazolium bis(trifluoromethylsulfonylimide ([OMIM][Tf2N] had both high enrichment efficiency and appropriate extraction recovery. Finally, the method was used for the determination of three wheat samples, and the recoveries of them were 74.8–112.5%, 71.8–104.5%, and 83.8–115.5%, respectively. The results show that the method proposed is simple, fast, and efficient, which can be applied to the extraction of organic matters in wheat samples.

  16. CATION-EXCHANGE SOLID-PHASE AND LIQUID-LIQUID ...

    African Journals Online (AJOL)

    B. S. Chandravanshi

    An existing liquid-liquid extraction (LLE) method was improved in terms of ... clean-up of the alkaloids from khat leaves, prior to HPLC-DAD detection. Despite .... The limits of detection (LOD) and quantification (LOQ) were calculated using the.

  17. Ionic-Liquid-Mediated Extraction and Separation Processes for Bioactive Compounds: Past, Present, and Future Trends.

    Science.gov (United States)

    Ventura, Sónia P M; E Silva, Francisca A; Quental, Maria V; Mondal, Dibyendu; Freire, Mara G; Coutinho, João A P

    2017-05-24

    Ionic liquids (ILs) have been proposed as promising media for the extraction and separation of bioactive compounds from the most diverse origins. This critical review offers a compilation on the main results achieved by the use of ionic-liquid-based processes in the extraction and separation/purification of a large range of bioactive compounds (including small organic extractable compounds from biomass, lipids, and other hydrophobic compounds, proteins, amino acids, nucleic acids, and pharmaceuticals). ILs have been studied as solvents, cosolvents, cosurfactants, electrolytes, and adjuvants, as well as used in the creation of IL-supported materials for separation purposes. The IL-based processes hitherto reported, such as IL-based solid-liquid extractions, IL-based liquid-liquid extractions, IL-modified materials, and IL-based crystallization approaches, are here reviewed and compared in terms of extraction and separation performance. The key accomplishments and future challenges to the field are discussed, with particular emphasis on the major lacunas found within the IL community dedicated to separation processes and by suggesting some steps to overcome the current limitations.

  18. Identification of chemical compounds in a liquid-liquid extraction system

    International Nuclear Information System (INIS)

    Ramirez C, F de M de la.

    1980-01-01

    The objective of the present work is to identify the chemical compounds that are distributed in a liquid-liquid extraction system in which the third phase is observed; for this purpose the FeCl 3 (0.12M) - HCl (8.43M) - Diisopropilic ether - system was used, for the quantitative determination of the chemical compounds, FeCl 3 solutions labelled with 59 Fe or witH 38 Cl were used; the Karl Fischer method for the determination of the water concentration at the organic phases was used, the obtained data was used for the calculations of the H + distribution in each phase. The results are that when the distribution equilibrium is reached, the aqueous phase is a 7.5M HCl solution; the light organic phase contains 2 H[FeCl 4 ].6H 2 O and the dense organic phase contains 2 H[FeCl 4 ].6H 2 O.3HCl.12H 2 O. The differences between these compounds are due to a high concentration of water and the HCl in the organic solvent. This causes a heterogeneous physic field, and then the third phase formation. (author)

  19. Contribution to the study of liquid-liquid extraction dynamics in the case of fast transfers. Extractions of uranium, plutonium and neptunium in a laboratory centrifugal extractor

    International Nuclear Information System (INIS)

    Bergeonneau, Philippe

    1978-01-01

    The liquid-liquid extraction (also named solvent-based extraction) is a very important technique for the reprocessing of irradiated nuclear fuels. This research thesis is based on the use of a laboratory centrifugal extractor which allows interesting conditions to be achieved: fast transfer due to an intense solution mixing, very short duration of contact between solutions. Thus, after a report of a bibliographical study on chemical mechanisms of extraction, on the composition of extracted species, on extraction kinetics, and on centrifugal extractors, this thesis reports the design, fabrication and use of a centrifugal extractor: presentation of fundamental principles, description and characteristics (materials, hydrodynamic operation test and problems, prototype). It reports studies of fast transfer kinetics: mathematical processing, result interpretation, results and discussions of extraction kinetics for nitric acid, uranium VI and IV, plutonium IV, neptunium IV, and comparison of the different extraction kinetics

  20. Comparison of dispersive liquid-liquid microextraction and hollow fiber liquid-liquid-liquid microextraction for the determination of fentanyl, alfentanil, and sufentanil in water and biological fluids by high-performance liquid chromatography.

    Science.gov (United States)

    Saraji, Mohammad; Khalili Boroujeni, Malihe; Hajialiakbari Bidgoli, Ali Akbar

    2011-06-01

    Dispersive liquid-liquid microextraction (DLLME) and hollow fiber liquid-liquid-liquid microextraction (HF-LLLME) combined with HPLC-DAD have been applied for the determination of three narcotic drugs (alfentanil, fentanyl, and sufentanil) in biological samples (human plasma and urine). Different DLLME parameters influencing the extraction efficiency such as type and volume of the extraction solvent and the disperser solvent, concentration of NaOH, and salt addition were investigated. In the HF-LLLME, the effects of important parameters including organic solvent type, concentration of NaOH as donor solution, concentration of H(2)SO(4) as acceptor phase, salt addition, stirring rate, temperature, and extraction time were investigated and optimized. The results showed that both extraction methods exhibited good linearity, precision, enrichment factor, and detection limit. Under optimal condition, the limits of detection ranged from 0.4 to 1.9 μg/L and from 1.1 to 2.3 μg/L for DLLME and HF-LLLME, respectively. For DLLME, the intra- and inter-day precisions were 1.7-6.4% and 14.2-15.9%, respectively; and for HF-LLLME were 0.7-5.2% and 3.3-10.1%, respectively. The enrichment factors were from 275 to 325 and 190 to 237 for DLLME and HF-LLLME, respectively. The applicability of the proposed methods was investigated by analyzing biological samples. For analysis of human plasma and urine samples, HF-LLLME showed higher precision, more effective sample clean-up, higher extraction efficiency, lower organic solvent consumption than DLLME.

  1. Recent progress of task-specific ionic liquids in chiral resolution and extraction of biological samples and metal ions.

    Science.gov (United States)

    Wu, Datong; Cai, Pengfei; Zhao, Xiaoyong; Kong, Yong; Pan, Yuanjiang

    2018-01-01

    Ionic liquids have been functionalized for modern applications. The functional ionic liquids are also called task-specific ionic liquids. Various task-specific ionic liquids with certain groups have been constructed and exploited widely in the field of separation. To take advantage of their properties in separation science, task-specific ionic liquids are generally used in techniques such as liquid-liquid extraction, solid-phase extraction, gas chromatography, high-performance liquid chromatography, and capillary electrophoresis. This review mainly covers original research papers published in the last five years, and we will focus on task-specific ionic liquids as the chiral selectors in chiral resolution and as extractant or sensor for biological samples and metal ion purification. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Application of dispersive liquid-liquid microextraction and dispersive micro-solid-phase extraction for the determination of quinolones in swine muscle by high-performance liquid chromatography with diode-array detection

    International Nuclear Information System (INIS)

    Tsai, Wen-Hsien; Chuang, Hung-Yi; Chen, Ho-Hsien; Huang, Joh-Jong; Chen, Hwi-Chang; Cheng, Shou-Hsun; Huang, Tzou-Chi

    2009-01-01

    Dispersive liquid-liquid microextraction (DLLME) and dispersive micro-solid-phase extraction (DMSPE) are two simple and low-cost sample preparation methods for liquid samples. In this work, these two methods were applied to solid tissue sample for the determination of seven quinolones by high-performance liquid chromatography with diode-array detection (HPLC-DAD). After the homogenization of the swine muscle with acetonitrile and salt-promoted partitioning, small amounts of the extract were used for the DLLME and DMSPE methods. In the DLLME approach, the target analytes in the extraction solvent were rapidly extracted into a small volume of dichloromethane for drying and the residue was reconstituted for HPLC-DAD analysis. In the DMSPE approach, the target analytes in the extraction solvent were trapped by dispersive silica-based PSA (primary and secondary amine) sorbents and desorbed into a small amount of desorption solution for HPLC-DAD analysis. Under the optimal conditions, relative recoveries were determined for swine muscle spiked 50-200 μg kg -1 and quantification was achieved by matrix-matched calibration. The calibration curves of seven quinolones showed linearity with a correlation coefficient value above 0.998 for both approaches. Relative recoveries ranged from 93.0 to 104.7% and from 95.5 to 111.0% for DLLME and DMSPE, respectively. Limits of detection (LODs) ranged from 5.6 to 23.8 μg kg -1 and from 7.5 to 26.3 μg kg -1 for DLLME and DMSPE, respectively.

  3. A technical review of liquid/liquid and solid/liquid separation equipment in the field of nuclear-fuel reprocessing

    International Nuclear Information System (INIS)

    Vassallo, G.

    1981-01-01

    Liquid/liquid extraction is generally accepted as the preferred method in nuclear-fuel reprocessing. However, although many types of liquid/liquid contactors are available, only a few meet the stringent specifications set by the nuclear industry. This report discusses the criteria for contactor selection and then reviews the most important types, namely packed columns, pulsed columns, mixer-setters and centrifugal contactors. Finally, a short section concerned with solid/liquid separations is included because of the possible deleterious effects caused by solids in liquid/liquid contactors

  4. Aromatics extraction from pyrolytic sugars using ionic liquid to enhance sugar fermentability

    NARCIS (Netherlands)

    Li, X.; Luque-Moreno, L.C.; Oudenhoven, Stijn; Rehmann, L.; Kersten, Sascha R.A.; Schuur, Boelo

    2016-01-01

    Fermentative bioethanol production from pyrolytic sugars was improved via aromatics removal by liquid–liquid extraction. As solvents, the ionic liquid (IL) trihexyltetradecylphosphonium dicyanamide (P666,14[N(CN)2]) and ethyl acetate (EA) were compared. Two pyrolytic sugar solutions were created

  5. Determination of a metabolite of nifursol in foodstuffs of animal origin by liquid-liquid extraction and liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Wang, Chuanxian; Qu, Li; Liu, Xia; Zhao, Chaomin; Zhao, Fengjuan; Huang, Fuzhen; Zhu, Zhenou; Han, Chao

    2017-02-01

    An analytical method has been developed for the detection of a metabolite of nifursol, 3,5-dinitrosalicylic acid hydrazide, in foodstuffs of animal origin (chicken liver, pork liver, lobster, shrimp, eel, sausage, and honey). The method combines liquid chromatography and tandem mass spectrometry with liquid-liquid extraction. Samples were hydrolyzed with hydrochloric acid and derivatized with 2-nitrobenzaldehyde at 37°C for 16 h. The solutions of derivatives were adjusted to pH 7.0-7.5, and the metabolite was extracted with ethyl acetate. 3,5-Dinitrosalicylic acid hydrazide determination was performed in the negative electrospray ionization method. Both isotope-labeled internal standard and matrix-matched calibration solutions were used to correct the matrix effects. Limits of quantification were 0.5 μg/kg for all samples. The average recoveries, measured at three concentration levels (0.5, 2.0, and 10 μg/kg) were in the range of 75.8-108.4% with relative standard deviations below 9.8%. The developed method exhibits a high sensitivity and selectivity for the routine determination and confirmation of the presence of a metabolite of nifursol in foodstuffs of animal origin. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Liquid-liquid extraction. Choice, calculation and design of devices

    International Nuclear Information System (INIS)

    Leybros, J.

    2005-01-01

    The aim of this work is to study the problematic due to the choice of an equipment, to its size and to its industrial bringing into operation. Besides its efficiency to carry out a mass transfer, the economical interest of an industrial device will be proportional to its specific rate (volume treated by surface unit of the cross section of the extractor). Nevertheless, as it seems to be logic to maximize the three parameters which have an influence on it (transfer coefficient, interfacial surface and transfer potential), there exists no device which can modify separately any of these parameters. In order to satisfy these aims, a great diversity of devices have been put on the market. Indeed, it exists about twenty different industrial devices. This diversity leads the engineer, during the design of a solvent extraction device, to take difficult and subjective decisions without pilot experiment on the considered system. The main problem of an economical and optimized calculation of the liquid-liquid extractors from theoretical data has still not found totally satisfying solutions. Thus, except in some cases where we have empirical correlations, the recourse to prototype experiments is required and the most recent advances have resulted essentially to define more reliable rules for the extrapolation of these experiments for the size of industrial devices. (O.M.)

  7. In situ derivatization-liquid liquid extraction as a sample preparation strategy for the determination of urinary biomarker prolyl-4-hydroxyproline by liquid chromatography-tandem mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Cimlová, Jana; Kružberská, Pavla; Švagera, Z.; Hušek, Petr; Šimek, Petr

    2012-01-01

    Roč. 47, č. 3 (2012), s. 294-302 ISSN 1076-5174 R&D Projects: GA ČR GA203/09/2014; GA MZd NS9755; GA MŠk 7F09028 Institutional research plan: CEZ:AV0Z50070508 Keywords : alkyl chloroformate derivatization * liquid liquid extraction * urine Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.214, year: 2012 http://onlinelibrary.wiley.com/doi/10.1002/jms.2952/full

  8. Solid-phase extraction in combination with dispersive liquid-liquid microextraction and ultra-high performance liquid chromatography-tandem mass spectrometry analysis: the ultra-trace determination of 10 antibiotics in water samples.

    Science.gov (United States)

    Liang, Ning; Huang, Peiting; Hou, Xiaohong; Li, Zhen; Tao, Lei; Zhao, Longshan

    2016-02-01

    A novel method, solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME), was developed for ultra-preconcentration of 10 antibiotics in different environmental water samples prior to ultra-high performance liquid chromatography-tandem mass spectrometry detection. The optimized results were obtained as follows: after being adjusted to pH 4.0, the water sample was firstly passed through PEP-2 column at 10 mL min(-1), and then methanol was used to elute the target analytes for the following steps. Dichloromethane was selected as extraction solvent, and methanol/acetonitrile (1:1, v/v) as dispersive solvent. Under optimal conditions, the calibration curves were linear in the range of 1-1000 ng mL(-1) (sulfamethoxazole, cefuroxime axetil), 5-1000 ng mL(-1) (tinidazole), 10-1000 ng mL(-1) (chloramphenicol), 2-1000 ng mL(-1) (levofloxacin oxytetracycline, doxycycline, tetracycline, and ciprofloxacin) and 1-400 ng mL(-1) (sulfadiazine) with a good precision. The LOD and LOQ of the method were at very low levels, below 1.67 and 5.57 ng mL(-1), respectively. The relative recoveries of the target analytes were in the range from 64.16% to 99.80% with relative standard deviations between 0.7 and 8.4%. The matrix effect of this method showed a great decrease compared with solid-phase extraction and a significant value of enrichment factor (EF) compared with dispersive liquid-liquid microextraction. The developed method was successfully applied to the extraction and analysis of antibiotics in different water samples with satisfactory results.

  9. A generalized theory of chromatography and multistep liquid extraction

    Science.gov (United States)

    Chizhkov, V. P.; Boitsov, V. N.

    2017-03-01

    A generalized theory of chromatography and multistep liquid extraction is developed. The principles of highly efficient processes for fine preparative separation of binary mixture components on a fixed sorbent layer are discussed.

  10. Liquid-liquid extraction/separation of platinum(IV) and rhodium(III) from acidic chloride solutions using tri-iso-octylamine

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Jin-Young, E-mail: jinlee@kigam.re.kr [Metals Recovery Department, Minerals Resources Research Division, Korea Institute of Geoscience and Mineral Resources (KIGAM), 92 Gahangno, Yuesong-gu, Daejeon 305-350 (Korea, Republic of); Rajesh Kumar, J., E-mail: rajeshkumarphd@rediffmail.com [Metals Recovery Department, Minerals Resources Research Division, Korea Institute of Geoscience and Mineral Resources (KIGAM), 92 Gahangno, Yuesong-gu, Daejeon 305-350 (Korea, Republic of); Kim, Joon-Soo; Park, Hyung-Kyu; Yoon, Ho-Sung [Metals Recovery Department, Minerals Resources Research Division, Korea Institute of Geoscience and Mineral Resources (KIGAM), 92 Gahangno, Yuesong-gu, Daejeon 305-350 (Korea, Republic of)

    2009-08-30

    Liquid-liquid extraction/separation of platinum(IV) and rhodium(III) from acidic chloride solutions was carried out using tri-iso-octylamine (Alamine 308) as an extractant diluted in kerosene. The percentage extraction of platinum(IV) and rhodium(III) increased with increase in acid concentration up to 8 mol L{sup -1}. However, at 10 mol L{sup -1} HCl concentration, the extraction behavior was reversed, indicating the solvation type mechanism during extraction. The quantitative extraction of {approx}98% platinum(IV) and 36% rhodium(III) was achieved with 0.01 mol L{sup -1} Alamine 308. The highest separation factor (S.F. = 184.7) of platinum(IV) and rhodium(III) was achieved with 0.01 mol L{sup -1} Alamine 308 at 1.0 mol L{sup -1} of hydrochloric acid concentration. Alkaline metal salts like sodium chloride, sodium nitrate, sodium thiocyanate, lithium chloride, lithium nitrate, potassium chloride and potassium thiocyanate used for the salting-out effect. LiCl proved as best salt for the extraction of platinum(IV). Temperature effect demonstrates that the extraction process is exothermic. Hydrochloric acid and thiourea mixture proved to be better stripping reagents when compared with other mineral acids and bases.

  11. Dispersive liquid-liquid microextraction with solidification of floating organic droplets for simultaneous extraction of pesticides, pharmaceuticals and personal care products

    International Nuclear Information System (INIS)

    Marube, Liziane Cardoso; Caldas, Sergiane Souza; Soares, Karina Lotz; Primel, Ednei Gilberto

    2015-01-01

    Dispersive liquid-liquid microextraction based on solidification of floating organic droplets (DLLME-SFO) has been applied to the extraction of pharmaceutical and personal care products (PPCPs) and pesticides from water samples. The PPCPs included bisphenol A, sodium diclofenac, gemfibrozil, furosemide, glibenclamide, nifedipine, nimesulide, propylparaben and triclocarban. The pesticides included 2,4-D, atrazine, azoxystrobin, cyproconazole, clomazone, dichloran, difenoconazole, diuron, epoxiconazole, fenoxaprop-p-ethyl, fipronil, iprodione, irgarol, propanil, propiconazole, tebuconazole, and trifloxystrobin. The type and volume of extraction solvent, type and volume of disperser solvent, ionic strength and pH were optimized. All species were then quantified by liquid chromatography tandem mass spectrometry (LC-MS/MS). The limits of quantification (LOQs) ranged from 50 to 500 ng L −1 , and the linearity ranged from the LOQ of each compound up to 10,000 ng L −1 . Recoveries ranged from 63 to 120 %, with relative standard deviations lower than 14 %. It is making use of a low-toxicity and affordable extraction solvent (1-dodecanol) and was successfully applied to the analysis of surface water samples. (author)

  12. HPLC/Fluorometric Detection of Carvedilol in Real Human Plasma Samples Using Liquid-Liquid Extraction.

    Science.gov (United States)

    Yilmaz, Bilal; Arslan, Sakir

    2016-03-01

    A simple, rapid and sensitive high-performance liquid chromatography (HPLC) method has been developed to quantify carvedilol in human plasma using an isocratic system with fluorescence detection. The method included a single-step liquid-liquid extraction with diethylether and ethylacetate mixture (3 : 1, v/v). HPLC separation was carried out by reversed-phase chromatography with a mobile phase composed of 20 mM phosphate buffer (pH 7)-acetonitrile (65 : 35, v/v), pumped at a flow rate of 1.0 mL/min. Fluorescence detection was performed at 240 nm (excitation) and 330 nm (emission). The calibration curve for carvedilol was linear from 10 to 250 ng/mL. Intra- and interday precision values for carvedilol in human plasma were plasma averaged out to 91.8%. The limits of detection and quantification of carvedilol were 3.0 and 10 ng/mL, respectively. Also, the method was successfully applied to three patients with hypertension who had been given an oral tablet of 25 mg carvedilol. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  13. Complex Formation in a Liquid-Liquid Extraction System Containing Cobalt(II, 4-(2-Pyridylazoresorcinol, and Nitron

    Directory of Open Access Journals (Sweden)

    Petya Vassileva Racheva

    2013-01-01

    Full Text Available Complex formation and liquid-liquid extraction were studied in a system containing cobalt(II, 4-(2-pyridylazoresorcinol (PAR, 1,4-diphenyl-3-(phenylamino-1H-1,2,4-triazole (Nitron, Nt, water, and chloroform. The effect of some experimental parameters (pH, shaking time, concentration of PAR, and concentration of Nt was systematically investigated, and the optimum conditions for cobalt extraction as an ion-association complex, (NtH+[Co3+(PAR2], were found. The following key equilibrium constants were calculated: constant of association (Log β=4.77±0.06, constant of distribution (LogKD=1.34±0.01, and constant of extraction (LogKex=6.11±0.07. Beer’s law was obeyed for Co concentrations up to 1.7 μg mL−1 with a molar absorptivity of 6.0×104 L mol−1 cm−1 at λmax=520 nm. Some additional characteristics, such as limit of detection, limit of quantification, and Sandell’s sensitivity, were estimated as well.

  14. Ionic-liquid-based ultrasound-assisted extraction of isoflavones from Belamcanda chinensis and subsequent screening and isolation of potential α-glucosidase inhibitors by ultrafiltration and semipreparative high-performance liquid chromatography.

    Science.gov (United States)

    Li, Senlin; Li, Sainan; Huang, Yu; Liu, Chunming; Chen, Lina; Zhang, Yuchi

    2017-06-01

    The separation of a compound of interest from its structurally similar homologues to produce high-purity natural products is a challenging problem. This work proposes a novel method for the separation of iristectorigenin A from its structurally similar homologues by ionic-liquid-based ultrasound-assisted extraction and the subsequent screening and isolation of potential α-glucosidase inhibitors via ultrafiltration and semipreparative high-performance liquid chromatography. Ionic-liquid-based ultrasound-assisted extraction was successfully applied to the extraction of tectorigenin, iristectorigenin A, irigenin, and irisflorentin from Belamcanda chinensis. The optimum conditions for the efficient extraction of isoflavones were determined as 1.0 M 1-ethyl-3-methylimidazolium tetrafluoroborate with extraction time of 30 min and a solvent to solid ratio of 30 mL/g. Ultrafiltration with liquid chromatography and mass spectrometry was applied to screen and identify α-glucosidase inhibitors from B. chinensis, followed by the application of semipreparative high-performance liquid chromatography to separate and isolate the active constituents. Four major compounds including tectorigenin, iristectorigenin A, irigenin, and irisflorentin were screened and identified as α-glucosidase inhibitors, and then the four active compounds abovementioned were subsequently isolated by semipreparative high-performance liquid chromatography (99.89, 88.97, 99.79, and 99.97% purity, respectively). The results demonstrate that ionic liquid extraction can be successfully applied to the extraction of isoflavones from B. chinensis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Conceptual process design and economic analysis of a process based on liquid-liquid extraction for the recovery of glycols from aqueous streams

    NARCIS (Netherlands)

    Garcia Chavez, L.Y.; Schuur, Boelo; de Haan, A.B.

    2013-01-01

    The recovery of monoethylene glycol (MEG) and 1,2-propylene glycol (PG) from aqueous streams via liquid–liquid extraction (LLE) using a tailor-made ionic liquid [TOA MNaph] is evaluated as an alternative technology to conventional triple effect evaporation of water. In this paper, the conceptual

  16. Chiral separation of substituted phenylalanine analogues using chiral palladium phosphine complexes with enantioselective liquid-liquid extraction

    NARCIS (Netherlands)

    Verkuijl, B.J.V.; Schuur, B.; Minnaard, A.J.; Vries, de J.G.; Feringa, B.L.

    2010-01-01

    Chiral palladium phosphine complexes have been employed in the chiral separation of amino acids and phenylalanine analogues in particular. The use of (S)-xylyl-BINAP as a ligand for the palladium complex in enantioselective liquid–liquid extraction allowed the separation of the phenylalanine

  17. Screening of commercial and pecan shell-extracted liquid smoke agents as natural antimicrobials against foodborne pathogens.

    Science.gov (United States)

    Van Loo, Ellen J; Babu, D; Crandall, Philip G; Ricke, Steven C

    2012-06-01

    Liquid smoke extracts have traditionally been used as flavoring agents, are known to possess antioxidant properties, and serve as natural alternatives to conventional antimicrobials. The antimicrobial efficacies of commercial liquid smoke samples may vary depending on their source and composition and the methods used to extract and concentrate the smoke. We investigated the MICs of eight commercial liquid smoke samples against Salmonella Enteritidis, Staphylococcus aureus, and Escherichia coli . The commercial liquid smoke samples purchased were supplied by the manufacturer as water-based or concentrated extracts of smoke from different wood sources. The MICs of the commercial smokes to inhibit the growth of foodborne pathogens ranged from 0.5 to 6.0% for E. coli, 0.5 to 8.0% for Salmonella, and 0.38 to 6% for S. aureus. The MIC for each liquid smoke sample was similar in its effect on both E. coli and Salmonella. Solvent-extracted antimicrobials prepared using pecan shells displayed significant differences between their inhibitory concentrations depending on the type of solvent used for extraction. The results indicated that the liquid smoke samples tested in this study could serve as effective natural antimicrobials and that their inhibitory effects depended more on the solvents used for extraction than the wood source.

  18. Determination of chlorophenols in honey samples using in-situ ionic liquid-dispersive liquid-liquid microextraction as a pretreatment method followed by high-performance liquid chromatography.

    Science.gov (United States)

    Fan, Chen; Li, Nai; Cao, Xueli

    2015-05-01

    In-situ ionic liquid-dispersive liquid-liquid microextraction (IL-DLLME) method was developed as a pretreatment method for the detection of six chlorophenols (CPs) in honey samples. The hydrophobic ionic liquid [C4MIM][NTf2], formed in-situ by the hydrophilic ionic liquid [C4MIM][BF4] and the ion exchange reagent LiNTf2 was used as the microextractant solvent of CPs from honey sample. Then the enriched analytes were back-extracted into 40 μL of 0.14 M NaOH solution and finally subjected to analysis by high-performance liquid chromatography. The method showed low limit of detection of CPs, 0.8-3.2 μg/L and high enrichment factor, 34-65 with the recoveries range from 91.60% to 114.33%. The method is simple, rapid, environmentally friendly and with high extraction efficiency. Copyright © 2014 The Authors. Published by Elsevier Ltd.. All rights reserved.

  19. Surfactant-enhanced liquid-liquid microextraction coupled to micro-solid phase extraction onto highly hydrophobic magnetic nanoparticles

    International Nuclear Information System (INIS)

    Giannoulis, Kiriakos M.; Giokas, Dimosthenis L.; Tsogas, George Z.; Vlessidis, Athanasios G.; Zhu, Qing; Pan, Qinmin

    2013-01-01

    We are presenting a simplified alternative method for dispersive liquid-liquid microextraction (DLLME) by resorting to the use of surfactants as emulsifiers and micro solid-phase extraction (μ-SPE). In this combined procedure, DLLME of hydrophobic components is initially accomplished in a mixed micellar/microemulsion extractant phase that is prepared by rapidly mixing a non-ionic surfactant and 1-octanol in aqueous medium. Then, and in contrast to classic DLLME, the extractant phase is collected by highly hydrophobic polysiloxane-coated core-shell Fe 2 O 3 (at)C magnetic nanoparticles. Hence, the sample components are the target analyte in the DLLME which, in turn, becomes the target analyte of the μ-SPE step. This 2-step approach represents a new and simple DLLME procedure that lacks tedious steps such as centrifugation, thawing, or delicate collection of the extractant phase. As a result, the analytical process is accelerated and the volume of the collected phase does not depend on the volume of the extraction solvent. The method was applied to extract cadmium in the form of its pyrrolidine dithiocarbamate chelate from spiked water samples prior to its determination by FAAS. Detection limits were brought down to the low μg L −1 levels by preconcentrating 10 mL samples with satisfactory recoveries (96.0–108.0 %). (author)

  20. Ionic liquid performance in pilot plant contactors for aromatics extraction

    NARCIS (Netherlands)

    Onink, S.A.F.

    2011-01-01

    The main objectives of this study were an investigation into the applicability, in this case extraction capacity and equipment performance, of room temperature ionic liquids as solvent in the extraction of aromatics from aliphatics and a comparison of three types of contactors (a rotating disc

  1. Ionic liquids as alternative solvents for aromatics extraction

    NARCIS (Netherlands)

    Hansmeier, A.R.

    2010-01-01

    The objective of this thesis was the development of an extraction process for the removal of multiple aromatics from several petrochemical streams by means of an ionic liquid. Due to environmental legislation, the demand of ‘clean’ fuels is increasing and most likely will increase even more towards

  2. Deterpenation of eucalyptus essential oil by liquid + liquid extraction: Phase equilibrium and physical properties for model systems at T = 298.2 K

    International Nuclear Information System (INIS)

    Gonçalves, Daniel; Koshima, Cristina Chiyoda; Nakamoto, Karina Thiemi; Umeda, Thayla Karla; Aracava, Keila Kazue; Gonçalves, Cintia Bernardo; Rodrigues, Christianne Elisabete da Costa

    2014-01-01

    Highlights: • Fractionation of essential oil compounds. • Liquid + liquid equilibria of limonene, citronellal, ethanol and water were studied. • Distribution coefficients of limonene and citronellal were evaluated. • Densities and viscosities of the phases were experimentally determined. • Solvent selectivities and physical properties were dependent on citronellal and water mass fractions. -- Abstract: As the principal source in Brazil of eucalyptus essential oil extracts, Eucalyptus citriodora contains citronellal, an oxygenated compound responsible for the flavour characteristics. Deterpenation processes, consisting of the removal of terpenic hydrocarbons with the subsequent concentration of the oxygenated compounds, can be used to improve the aromatic characteristics of this essential oil. The purpose of this work was to perform a study of the technical feasibility of using a liquid + liquid extraction process to deterpenate eucalyptus essential oil. Model systems with various mixtures of limonene and citronellal (representing eucalyptus essential oil) as well as solvent (ethanol with various water mass fractions) were used to obtain liquid + liquid equilibrium data. The raffinate and extract phases were also analyzed to characterize the physical properties (density and viscosity). The equilibrium data were used to adjust the NRTL and UNIQUAC parameters. Two empirical models, the simple mixing rule and the Grunberg–Nissan model, were evaluated for use in the descriptions of the densities and viscosities, respectively, of the samples. Increasing the water content in the solvent resulted in decreases in the limonene and citronellal distribution coefficients, with consequential increases in the solvent selectivity values. Increasing values of the densities and viscosities, especially for the solvent-rich phases, were associated with systems using high amounts of hydrated ethanolic solvents

  3. Ionic liquid-modified materials for solid-phase extraction and separation: a review.

    Science.gov (United States)

    Vidal, Lorena; Riekkola, Marja-Liisa; Canals, Antonio

    2012-02-17

    In recent years, materials science has propelled to the research forefront. Ionic liquids with unique and fascinating properties have also left their footprints to the developments of materials science during the last years. In this review we highlight some of their recent advances and provide an overview at the current status of ionic liquid-modified materials applied in solid-phase extraction, liquid and gas chromatography and capillary electrochromatography with reference to recent applications. In addition, the potential of ionic liquids in the modification of capillary inner wall in capillary electrophoresis is demonstrated. The main target material modified with ionic liquids is silica, but polymers and monoliths have recently joined the studies. Although imidazolium is still clearly the most commonly used ionic liquid for the covalently modification of materials, the exploitation of pyridinium and phosphonium will most probably increase in the future. Copyright © 2011 Elsevier B.V. All rights reserved.

  4. High-throughput liquid-liquid extraction in 96-well format: Parallel artificial liquid membrane extraction

    DEFF Research Database (Denmark)

    Gjelstad, Astrid; Andresen, Alf Terje; Dahlgren, Anders

    2017-01-01

    , highly efficient sample cleanup, and direct compatibility with liquid chromatography–mass spectrometry (LC–MS). The consumption of hazardous organic solvents is also almost eliminated using PALME as the sample preparation technique. This article summarizes current experiences with PALME, based on work...

  5. Microwave-assisted liquid-liquid microextraction based on solidification of ionic liquid for the determination of sulfonamides in environmental water samples.

    Science.gov (United States)

    Song, Ying; Wu, Lijie; Lu, Chunmei; Li, Na; Hu, Mingzhu; Wang, Ziming

    2014-12-01

    An easy, quick, and green method, microwave-assisted liquid-liquid microextraction based on solidification of ionic liquid, was first developed and applied to the extraction of sulfonamides in environmental water samples. 1-Ethy-3-methylimidazolium hexafluorophosphate, which is a solid-state ionic liquid at room temperature, was used as extraction solvent in the present method. After microwave irradiation for 90 s, the solid-state ionic liquid was melted into liquid phase and used to finish the extraction of the analytes. The ionic liquid and sample matrix can be separated by freezing and centrifuging. Several experimental parameters, including amount of extraction solvent, microwave power and irradiation time, pH of sample solution, and ionic strength, were investigated and optimized. Under the optimum experimental conditions, good linearity was observed in the range of 2.00-400.00 μg/L with the correlation coefficients ranging from 0.9995 to 0.9999. The limits of detection for sulfathiazole, sulfachlorpyridazine, sulfamethoxazole, and sulfaphenazole were 0.39, 0.33, 0.62, and 0.85 μg/L, respectively. When the present method was applied to the analysis of environmental water samples, the recoveries of the analytes ranged from 75.09 to 115.78% and relative standard deviations were lower than 11.89%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Emulsion liquid membrane for selective extraction of bismuth from nitrate medium

    International Nuclear Information System (INIS)

    Mokhtari, Bahram; Pourabdollah, Kobra

    2013-01-01

    The novelty of this work is the selective extraction of bismuth ions from nitrate medium by emulsion liquid membrane. Di(2-ethylhexyl)phosphoric acid was used as extractant of bismuth ions from nitrate medium by emulsion liquid membrane, and Triton X-100 was used as the biodegradable surfactant in n-pentanol n-pentanol bulk membrane. The extraction of bismuth ions was evaluated by the yield of extraction. The experimental parameters were evaluated and were optimized. They included the ratio of di(2-ethylhexyl)phosphoric acid concentration to the concentration of /Triton X-100 concentration (1.0 : 0.5% w/w), nature of diluents (n-pentanol), nature and concentration of the stripping solution (sulfuric acid, 0.5M), stirring speed (1,800 rpm) and equilibrium time of extraction (20min), initial feed solution of bismuth (350 ppm) and the volume ratio of the internal stripping phase to the membrane phase (14 times). The experimental parameters of kinetic extraction revealed that the bismuth ions were extracted at 100% 97%

  7. Emulsion liquid membrane for selective extraction of bismuth from nitrate medium

    Energy Technology Data Exchange (ETDEWEB)

    Mokhtari, Bahram; Pourabdollah, Kobra [Islamic Azad University, Shahreza (Iran, Islamic Republic of)

    2013-07-15

    The novelty of this work is the selective extraction of bismuth ions from nitrate medium by emulsion liquid membrane. Di(2-ethylhexyl)phosphoric acid was used as extractant of bismuth ions from nitrate medium by emulsion liquid membrane, and Triton X-100 was used as the biodegradable surfactant in n-pentanol n-pentanol bulk membrane. The extraction of bismuth ions was evaluated by the yield of extraction. The experimental parameters were evaluated and were optimized. They included the ratio of di(2-ethylhexyl)phosphoric acid concentration to the concentration of /Triton X-100 concentration (1.0 : 0.5% w/w), nature of diluents (n-pentanol), nature and concentration of the stripping solution (sulfuric acid, 0.5M), stirring speed (1,800 rpm) and equilibrium time of extraction (20min), initial feed solution of bismuth (350 ppm) and the volume ratio of the internal stripping phase to the membrane phase (14 times). The experimental parameters of kinetic extraction revealed that the bismuth ions were extracted at 100% 97%.

  8. Parallel artificial liquid membrane extraction of new psychoactive substances in plasma and whole blood

    DEFF Research Database (Denmark)

    Vårdal, Linda; Askildsen, Hilde-Merete; Gjelstad, Astrid

    2017-01-01

    Parallel artificial liquid membrane extraction (PALME) was combined with ultra-high performance liquid chromatography-mass spectrometry (UHPLC–MS) and the potential for screening of new psychoactive substances (NPS) was investigated for the first time. PALME was performed in 96-well format...... comprising a donor plate, a supported liquid membrane (SLM), and an acceptor plate. Uncharged NPS were extracted from plasma or whole blood, across an organic SLM, and into an aqueous acceptor solution, facilitated by a pH gradient. MDAI (5,6-methylenedioxy-2-aminoindane), methylone, PFA (para...

  9. A green deep eutectic solvent dispersive liquid-liquid micro-extraction (DES-DLLME) for the UHPLC-PDA determination of oxyprenylated phenylpropanoids in olive, soy, peanuts, corn, and sunflower oil.

    Science.gov (United States)

    Ferrone, Vincenzo; Genovese, Salvatore; Carlucci, Maura; Tiecco, Matteo; Germani, Raimondo; Preziuso, Francesca; Epifano, Francesco; Carlucci, Giuseppe; Taddeo, Vito Alessandro

    2018-04-15

    A green dispersive liquid-liquid microextraction (DLLME) using deep eutectic solvent (DES) as the extracting solvent has been developed and applied for the simultaneous quantification of ferulic acid, umbelliferone, boropinic acid, 7-isopentenyloxycoumarin, 4'-geranyloxyferulic acid (GOFA), and auraptene in some vegetable oils using ultra high performance liquid chromatography (UHPLC) with photodiode array detection (PDA). All parameters in the extraction step, including selection and loading of both extracting and dispersing solvents, amount of both extractant and disperser solvent were investigated and optimized. PhAA/TMG DES achieved higher recovery and enrichment factor compared to other DESs. The validated method showed good linearity with correlation coefficients, r 2 >0.9990 for all the analytes. Furthermore, this is the first time that eco-friendly solvents are used for the extraction of oxyprenylated phenylpropanoids and the corresponding extract analyzed with ultra high performance liquid chromatography with photodiode array detection. Copyright © 2017 Elsevier Ltd. All rights reserved.

  10. Dispersive liquid-liquid microextraction coupled with magnetic nanoparticles for extraction of zearalenone in wheat samples

    Directory of Open Access Journals (Sweden)

    Mitra Amoli-Diva

    2017-01-01

    Full Text Available A new, sensitive and fast dispersive liquid-liquid microextraction (DLLME coupled with micro-solid phase extraction (μ-SPE was developed for determination of zearalenone (ZEN in wheat samples. The DLLME was performed using acetonitrile/water (80:20 v/v as the disperser solvent and 1-octanol as the extracting solvent.  The acetonitrile/water (80:20 v/v solvent was also used to extract ZEN from solid wheat matrix, and was directly applied as the disperser solvent for DLLME process. Additionally, hydrophobic oleic-acid-modified magnetic nanoparticles were used in μ-SPE approach to retrieve the analyte from the DLLME step. So, the method uses high surface area and strong magnetism properties of these nanoparticles to avoid time-consuming column-passing processes in traditional SPE. Main parameters affecting the extraction efficiency and signal enhancement were investigated and optimized. Under the optimum conditions, the calibration curve showed a good linearity in the range of 0.1-500 μg kg−1 (R2=0.9996 with low detection limit of 83 ng g−1. The intra-day and inter-day precisions (as RSD % in the range of 2.6-4.3 % and high recoveries ranging from 91.6 to 99.1 % were obtained. The pre-concentration factor was 3. The method is simple, inexpensive, accurate and remarkably free from interference effects.

  11. Liquid-liquid and solid-phase extractions of phenols from virgin olive oil and their separation by chromatographic and electrophoretic methods.

    Science.gov (United States)

    Bendini, Alessandra; Bonoli, Matteo; Cerretani, Lorenzo; Biguzzi, Barbara; Lercker, Giovanni; Toschi, Tullia Gallina

    2003-01-24

    The high oxidative stability of virgin olive oil is related to its high monounsaturated/polyunsaturated ratio and to the presence of antioxidant compounds, such as tocopherols and phenols. In this paper, the isolation of phenolic compounds from virgin olive oil, by different methods, was tested and discussed. Particularly liquid-liquid and solid-phase extraction methods were compared, assaying, for the latter, three stationary phases (C8, C18 and Diol) and several elution mixtures. Quantification of phenolic and o-diphenolic substances in the extracts was performed by the traditional Folin-Ciocalteau method and the sodium molybdate reaction, respectively. Furthermore, the quantification of phenolic compounds in the extracts and in a standard mixture was carried out both with diode array and mass spectrometric detection and capillary zone electrophoresis.

  12. RECOVERY OF CARBOXYLIC ACIDS FROM AQUEOUS SOLUTIONS BY LIQUID-LIQUID EXTRACTION WITH A TRIISOOCTYLAMINE DILUENT SYSTEM

    Directory of Open Access Journals (Sweden)

    G. Malmary

    2001-12-01

    Full Text Available Tertiary alkylamines in solution with organic diluents are attractive extractants for the recovery of carboxylic acids from dilute aqueous phases. The aim of this study was to investigate the mechanism for extraction of organic acids from water by a long-chain aliphatic tertiary amine. In order to attain this objective, we studied the liquid-liquid equilibria between the triisooctylamine + 1-octanol + n-heptane system as solvent and an aqueous solution of an individual carboxylic acid such as citric, lactic and malic acids. The experiments showed that the partition coefficient for a particular organic acid depends on the kind of solute, notably when the acid concentration in the aqueous phase is low. A mathematical model, where both chemical association and physical distribution are taken into consideration, is proposed. The model suggests that the various complexes obtained between amine and organic acids contribute to the distribution of the solute between the coexisting phases in equilibrium.

  13. Assessment of strobilurin fungicides' content in soya-based drinks by liquid micro-extraction and liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Campillo, Natalia; Iniesta, María Jesús; Viñas, Pilar; Hernández-Córdoba, Manuel

    2015-01-01

    Seven strobilurin fungicides were pre-concentrated from soya-based drinks using dispersive liquid-liquid micro-extraction (DLLME) with a prior protein precipitation step in acid medium. The enriched phase was analysed by liquid chromatography (LC) with dual detection, using diode array detection (DAD) and electrospray-ion trap tandem mass spectrometry (ESI-IT-MS/MS). After selecting 1-undecanol and methanol as the extractant and disperser solvents, respectively, for DLLME, the Taguchi experimental method, an orthogonal array design, was applied to select the optimal solvent volumes and salt concentration in the aqueous phase. The matrix effect was evaluated and quantification was carried out using external aqueous calibration for DAD and matrix-matched calibration method for MS/MS. Detection limits in the 4-130 and 0.8-4.5 ng g(-1) ranges were obtained for DAD and MS/MS, respectively. The DLLME-LC-DAD-MS method was applied to the analysis of 10 different samples, none of which was found to contain residues of the studied fungicides.

  14. Ionic liquid-based microwave-assisted extraction of flavonoids from Bauhinia championii (Benth.) Benth.

    Science.gov (United States)

    Xu, Wei; Chu, Kedan; Li, Huang; Zhang, Yuqin; Zheng, Haiyin; Chen, Ruilan; Chen, Lidian

    2012-12-03

    An ionic liquids (IL)-based microwave-assisted approach for extraction and determination of flavonoids from Bauhinia championii (Benth.) Benth. was proposed for the first time. Several ILs with different cations and anions and the microwave-assisted extraction (MAE) conditions, including sample particle size, extraction time and liquid-solid ratio, were investigated. Two M 1-butyl-3-methylimidazolium bromide ([bmim] Br) solution with 0.80 M HCl was selected as the optimal solvent. Meanwhile the optimized conditions a ratio of liquid to material of 30:1, and the extraction for 10 min at 70 °C. Compared with conventional heat-reflux extraction (CHRE) and the regular MAE, IL-MAE exhibited a higher extraction yield and shorter extraction time (from 1.5 h to 10 min). The optimized extraction samples were analysed by LC-MS/MS. IL extracts of Bauhinia championii (Benth.)Benth consisted mainly of flavonoids, among which myricetin, quercetin and kaempferol, β-sitosterol, triacontane and hexacontane were identified. The study indicated that IL-MAE was an efficient and rapid method with simple sample preparation. LC-MS/MS was also used to determine the chemical composition of the ethyl acetate/MAE extract of Bauhinia championii (Benth.) Benth, and it maybe become a rapid method to determine the composition of new plant extracts.

  15. Quantification of four ionophores in soil, sediment and manure using pressurised liquid extraction

    DEFF Research Database (Denmark)

    Bak, Søren Alex; Hansen, Martin; Pedersen, Kenneth Munk

    2013-01-01

    A multi-residue pressurised liquid extraction (PLE) methodology has been established for the determination of the four ionophores: lasalocid, monensin, salinomycin and narasin in solid environmental matrices. The PLE methodology is combined with solid phase extraction as clean-up using liquid...... chromatography coupled to tandem mass spectrometry applying electrospray ionisation for detection. The samples were freeze-dried prior to extraction. The absolute recoveries for soil and sediment ranged from 71 to 123% (relative standard deviation (RSDs) below 16%) and in the range 94-133% (RSDs 9...

  16. Optimisation of pressurized liquid extraction using a multivariate chemometric approach for the determination of anticancer drugs in sludge by ultra high performance liquid chromatography-tandem mass spectrometry

    OpenAIRE

    Seira , Jordan; Claparols , Catherine; Joannis-Cassan , Claire; Albasi , Claire; Montréjaud-Vignoles , Mireille; Sablayrolles , Caroline

    2013-01-01

    International audience; The present paper describes an analytical method for the determination of 2 widely administered anticancer drugs, ifosfamide and cyclophosphamide, contained in sewage sludge. The method relies on the extraction from the solid matrix by pressurized liquid extraction, sample purification by solid-phase extraction and analysis by ultra high performance liquid chromatography coupled with tandem mass spectrometry. The different parameters affecting the extraction efficiency...

  17. [Determination of fatty acid esters of chloropropanediols in diet samples by gas chromatography-mass spectrometry coupled with solid-supported liquid-liquid extraction].

    Science.gov (United States)

    Gao, Jie; Liu, Qing; Han, Feng; Miao, Hong; Zhao, Yunfeng; Wu, Yongning

    2014-05-01

    To establish a method for the determination of fatty acid esters of 3-monochloropropane-1, 2-diol (3-MCPD) and 2-monochloropropane-1, 3-diol (2-MCPD) in diet samples by gas chromatography-mass spectrometry (GC-MS) with solid-supported liquid-liquid extraction (SLE). Diet samples were ultrasonically extracted by hexane, followed by ester cleavage reaction with sodium methylate in methanol, and then purified by solid-supported liquid-liquid extraction. (SLE) using diatomaceous earth as the sorbent. After derivatization with heptafluorobutyrylimidazole, the analytes were detected by GC-MS and quantified by the deuterated internal standards. The limits of detection (LODs) of 3-MCPD esters and 2-MCPD esters in different diet samples were 0.002 - 0.005 mg/kg and 0.002 - 0.006 mg/kg. The average recoveries of 3-MCPD esters and 2-MCPD esters at the spiking levels of 0.05 and 0.1 mg/kg in the diet samples were in the range of 65.9% - 104.2% and 75.4% - 118.0%, respectively, with the relative standard deviations in the range of 2.2% - 14.2% and 0.8% - .13.9%. The method is simple, accurate and rugged for the determination of fatty acid esters of 3-MCPD and 2-MCPD in diet samples.

  18. Kinetic aspects of hollow fiber liquid-phase microextraction and electromembrane extraction

    DEFF Research Database (Denmark)

    Gjelstad, Astrid; Jensen, Henrik; Rasmussen, Knut Einar

    2012-01-01

    In this paper, extraction kinetics was investigated experimentally and theoretically in hollow fiber liquid-phase microextraction (HF-LPME) and electromembrane extraction (EME) with the basic drugs droperidol, haloperidol, nortriptyline, clomipramine, and clemastine as model analytes. In HF...

  19. Malonamide, phosphine oxide and calix[4]arene functionalized ionic liquids: synthesis and extraction of actinides and lanthanides

    International Nuclear Information System (INIS)

    Ternova, Dariia

    2014-01-01

    Radioactive waste treatment is a crucial problem nowadays. This work was dedicated to the development of the new extracting systems for radionuclides on the basis of 'green' solvents Ionic Liquids (Ils). For this purpose Ils were functionalized with various extracting patterns: phosphine oxide, carbamoyl phosphine oxide groups and malonamide fragment. Also the calix[4]arene platforms were used for the synthesis of functionalized ionic liquids (Fils) and their precursors. The Fils of both types cationic and anionic have been obtained. The synthesized Fils were tested for the liquid-liquid extraction of radionuclides. lt was found that extraction well occurs due to the extracting patterns, however a charge of a modified ion influences extraction.The various extracting experiments and mathematical modelling have been performed to determine the mechanisms of extraction. These studies showed that each extracting system is characterized by a different set of extracting equilibria, based mostly on cationic exchange. (author)

  20. Some studies on extractive liquid scintillation counting for Th-234/P-234m

    International Nuclear Information System (INIS)

    Grudpan, K.; Singjanusong, P.; Punyodom, W.

    1990-01-01

    A study on solvent extraction for Th-234/Pa-234m by liquid scintillation counting has not been reported. This paper will report an application of the technique on such a study. In a hydrochloric acid solution of an uranyl salt, Pa-234m which is one of the daughters of U-238 can be separated by extraction into isobutyl methyl ketone (IBMK). Cerenkov counting was applied for the extraction investigation. Solvent extraction of Th-234/Pa-234m from an aqueous nitric acid solution by TOPO/PPO in toluene by using liquid scintillation counting will be described

  1. Separation of toluene from n-heptane by liquid–liquid extraction using binary mixtures of [bpy][BF4] and [4bmpy][Tf2N] ionic liquids as solvent

    International Nuclear Information System (INIS)

    García, Silvia; Larriba, Marcos; García, Julián; Torrecilla, José S.; Rodríguez, Francisco

    2012-01-01

    Highlights: ► Binary mixtures of ionic liquids as extraction solvents of aromatics. ► [4bmpy][Tf 2 N] shows higher capacity but lower selectivity than sulfolane. ► [bpy][BF 4 ] shows lower capacity but higher selectivity than sulfolane. ► Mixed {[4bmpy][Tf 2 N] + [bpy][BF 4 ]} improves both extractive properties. - Abstract: The use of binary mixture of ionic liquids N-butylpyridinium tetrafluoroborate ([bpy][BF 4 ]), and 1-butyl-4-methylpyridinium bis(trifluoromethylsulfonyl)imide ([4bmpy][Tf 2 N]) in the liquid–liquid extraction of toluene from n-heptane has been investigated at 313.2 K and atmospheric pressure. The experimental capacity of extraction and selectivity for this binary mixture has proved to be intermediate to those corresponding to the pure ionic liquids, and they can be predicted using a logarithmic–linear model of solubility. Furthermore, the results showed that the use of binary mixture of {[bpy][BF 4 ] + [4bmpy][Tf 2 N]} at a mole solvent composition around 0.7 for [bpy][BF 4 ] improves both the capacity of extraction of toluene and the selectivity with respect to those of sulfolane, the organic solvent taken as a benchmark. Thus, this mixed ionic liquid could be likely to be used in the extraction of aromatic from aliphatic in replacement to sulfolane.

  2. Study on novel ionic liquids as extracting agent for priority metals from waste waters

    International Nuclear Information System (INIS)

    Fischer, L.; Falta, T.; Stingeder, G.; Koellensperger, G.; Hann, S.; Kogelnig, D.; Stojanovic, A.; Krachler, R.; Keppler, B.K.

    2009-01-01

    Full text: As the new EU Water Framework Directive (2000/60/EC) sets high environmental quality standards for priority substances in surface water, effective procedures for wastewater treatment are required. The characteristics of ionic liquids (IL) can be adjusted by modifying their ionic composition for liquid-liquid extraction of metals and metal containing compounds (Cd, Hg, Ni, Pb, tributyltin, cancerostatic platinum compounds) from the water phase. The potential of novel IL for selective removal of the above mentioned substances regarding extraction time, pH and matrix were determined by ICPSFMS, HPLC-ICPMS and GC-ICPMS measurements. (author)

  3. Caesium extraction from acidic high level liquid wastes with functionalized calixarenes

    International Nuclear Information System (INIS)

    Simon, N.; Eymard, S.; Tournois, B.; Dozol, J.F.

    2000-01-01

    In the framework of French law programme, studies are under way to selectively remove caesium from acidic high activity wastes. Calix[4]arene crown derivatives exhibit outstanding efficiency and selectivity for caesium. An optimisation of the formulation of a selective extractant system for Cs based on crown calixarenes and usable in a process which use liquid-liquid extraction is presented. A system involving a monoamide as a modifier is proposed. Besides these improvements, a reference solvent based on a standard 1,3-di-(n-octyl-oxy)2,4-calix(4)arene crown is studied. Flow-sheets related to this system are calculated and easily transferable to the optimised new system. (authors)

  4. Ionic liquid-based air-assisted liquid-liquid microextraction followed by high performance liquid chromatography for the determination of five fungicides in juice samples.

    Science.gov (United States)

    You, Xiangwei; Chen, Xiaochu; Liu, Fengmao; Hou, Fan; Li, Yiqiang

    2018-01-15

    A novel and simple ionic liquid-based air-assisted liquid-liquid microextraction technique combined with high performance liquid chromatography was developed to analyze five fungicides in juice samples. In this method, ionic liquid was used instead of a volatile organic solvent as the extraction solvent. The emulsion was formed by pulling in and pushing out the mixture of aqueous sample solution and extraction solvent repeatedly using a 10mL glass syringe. No organic dispersive solvent was required. Under the optimized conditions, the limits of detection (LODs) were 0.4-1.8μgL -1 at a signal-to-noise ratio of 3. The limits of quantification (LOQs) set as the lowest spiking levels with acceptable recovery in juices were 10μgL -1 , except for fludioxonil whose LOQ was 20μgL -1 . The proposed method was applied to determine the target fungicides in juice samples, and acceptable recoveries ranging from 74.9% to 115.4% were achieved. Copyright © 2017. Published by Elsevier Ltd.

  5. Oxidative desulfurization of dibenzothiophene from model oil using ionic liquids as extracting agent

    Science.gov (United States)

    Taha, Mohd F.; Atikah, N.; Chong, F. K.; Shaharun, Maizatul S.

    2012-09-01

    The oxidative desulfurization of dibenzothiophene (DBT) from model oil (in n-dodecane) was carried out using ionic liquid as the extractant and catalyst, and hydrogen peroxide (H2O2) in combination with acetic acid (CH3COOH) and sulphuric acid (H2SO4) as the oxidant. The ionic liquids used were 1-butyl-3-methylimidazolium octyl sulphate ([Bmim][OcSO4]) and 1-butyl-3-methylimidazolium acetate ([Bmim][Ac]). The effect of the amounts of H2O2 on oxidative desulphurization of model oil was first investigated without the usage of ionic liquids at room temperature. The results indicate that greater amount of H2O2 give higher desulfurization and the maximum desulfurization in this study, i.e. 34 %, was occurred when the molar ratio of H2O2 to sulfur was 5:1. With the usage of ionic liquid and the molar ratio of 5:1 (H2O2:sulfur), the efficiency of DBT removal from model oil was increased significantly in terms of percent removal and removal time. Ionic liquid of [Bmim][OcSO4] performed better than [Bmim][Ac] with 72 % DBT removal. When molar ratio of H2O2 to sulphur was 5:1, volume ratio of ionic liquid to model oil was 1:1 and mixing time was 60 min at room temperature. The results indicate the potential of ionic liquids as the extractant and catalyst for oxidative desulfurization of hydrocarbon fuels.

  6. Stability of Anthocyanins from Red Grape Skins under Pressurized Liquid Extraction and Ultrasound-Assisted Extraction Conditions

    Directory of Open Access Journals (Sweden)

    Ali Liazid

    2014-12-01

    Full Text Available The stability of anthocyanins from grape skins after applying different extraction techniques has been determined. The following compounds, previously extracted from real samples, were assessed: delphinidin 3-glucoside, cyanidin 3-glucoside, petunidin 3-glucoside, peonidin 3-glucoside, malvidin 3-glucoside, peonidin 3-acetylglucoside, malvidin 3-acetylglucoside, malvidin 3-caffeoylglucoside, petunidin 3-p-coumaroylglucoside and malvidin 3-p-coumaroylglucoside (trans. The techniques used were ultrasound-assisted extraction and pressurized liquid extraction. In ultrasound-assisted extraction, temperatures up to 75 °C can be applied without degradation of the aforementioned compounds. In pressurized liquid extraction the anthocyanins were found to be stable up to 100 °C. The relative stabilities of both the glycosidic and acylated forms were evaluated. Acylated derivatives were more stable than non-acylated forms. The differences between the two groups of compounds became more marked on working at higher temperatures and on using extraction techniques with higher levels of oxygen in the extraction media.

  7. Synthesis, characterization and application of 1-butyl-3-methylimidazolium tetrafluoroborate for extractive desulfurization of liquid fuel

    Directory of Open Access Journals (Sweden)

    Swapnil A. Dharaskar

    2016-07-01

    Full Text Available In the present paper the experimental data of extractive desulfurization of liquid fuel using 1-butyl-3-methylimidazolium tetrafluoroborate [BMIM]BF4 have been presented. The data of FTIR, 1H NMR and 13C NMR have been discussed for the molecular confirmation of synthesized [BMIM]BF4. Further, the thermal properties, conductivity, solubility, and viscosity analysis of the [BMIM]BF4 were carried out. The effects of reaction time, reaction temperature, sulfur compounds, and recycling of ionic liquid without regeneration on dibenzothiophene removal of liquid fuel were presented. In extractive desulfurization process, the removal of dibenzothiophene in n-dodecane was 73.02% for mass ratio of 1:1 in 30 min at 30 °C under the mild reaction conditions. The ionic liquids could be reused four times without a significant decrease in activity. Also, the desulfurizations of real fuels, multistage extraction were presented. The data and results provided in the present paper explore the significant insights of imidazoled ILs for extractive desulfurization of liquid fuels.

  8. A simple liquid extraction protocol for overcoming the ion suppression of triacylglycerols by phospholipids in liquid chromatography mass spectrometry studies.

    Science.gov (United States)

    Araujo, Pedro; Tilahun, Ephrem; Breivik, Joar Fjørtoft; Abdulkader, Bashir M; Frøyland, Livar; Zeng, Yingxu

    2016-02-01

    It is well-known that triacylglycerol (TAG) ions are suppressed by phospholipid (PL) ions in regiospecific analysis of TAG by mass spectrometry (MS). Hence, it is essential to remove the PL during sample preparation prior to MS analysis. The present article proposes a cost-effective liquid-liquid extraction (LLE) method to remove PL from TAG in different kinds of biological samples by using methanol, hexane and water. High performance thin layer chromatography confirmed the lack of PL in krill oil and salmon liver samples, submitted to the proposed LLE protocol, and liquid chromatography tandem MS confirmed that the identified TAG ions were highly enhanced after implementing the LLE procedure. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Ionic liquid-based microwave-assisted dispersive liquid-liquid microextraction and derivatization of sulfonamides in river water, honey, milk, and animal plasma.

    Science.gov (United States)

    Xu, Xu; Su, Rui; Zhao, Xin; Liu, Zhuang; Zhang, Yupu; Li, Dan; Li, Xueyuan; Zhang, Hanqi; Wang, Ziming

    2011-11-30

    The ionic liquid-based microwave-assisted dispersive liquid-liquid microextraction (IL-based MADLLME) and derivatization was applied for the pretreatment of six sulfonamides (SAs) prior to the determination by high-performance liquid chromatography (HPLC). By adding methanol (disperser), fluorescamine solution (derivatization reagent) and ionic liquid (extraction solvent) into sample, extraction, derivatization, and preconcentration were continuously performed. Several experimental parameters, such as the type and volume of extraction solvent, the type and volume of disperser, amount of derivatization reagent, microwave power, microwave irradiation time, pH of sample solution, and ionic strength were investigated and optimized. When the microwave power was 240 W, the analytes could be derivatized and extracted simultaneously within 90 s. The proposed method was applied to the analysis of river water, honey, milk, and pig plasma samples, and the recoveries of analytes obtained were in the range of 95.0-110.8, 95.4-106.3, 95.0-108.3, and 95.7-107.7, respectively. The relative standard deviations varied between 1.5% and 7.3% (n=5). The results showed that the proposed method was a rapid, convenient and feasible method for the determination of SAs in liquid samples. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. Injection molded lab-on-a-disc platform for screening of genetically modified E. coli using liquid-liquid extraction and surface enhanced Raman scattering

    DEFF Research Database (Denmark)

    Morelli, Lidia; Serioli, Laura; Centorbi, Francesca Alessandra

    2018-01-01

    We present the development of an automated centrifugal microfluidic platform with integrated sample pre-treatment (filtration and liquid-liquid extraction) and detection (SERS-based sensing). The platform consists of eight calibration and four assay modules, fabricated with polypropylene using...... injection molding and bonded with ultrasonic welding. The platform was used for detection of a secondary bacterial metabolite (p-coumaric acid) from bacterial supernatant. The obtained extraction efficiency was comparable to values obtained in batch experiments and the SERS-based sensing showed a good...

  11. Liquid membrane extraction techniques for trace metal analysis and speciation in environmental and biological matrices

    Energy Technology Data Exchange (ETDEWEB)

    Ndungu, Kuria

    1999-04-01

    In this thesis, liquid-membrane-based methods for the analysis of trace metal species in samples of environmental and biological origin were developed. By incorporating extracting reagents in the membrane liquid, trace metal ions were selectively separated from humic-rich natural waters and urine samples, prior to their determination using various instrumental techniques. The extractions were performed in closed flow systems thus allowing easy automation of both the sample clean-up and enrichment. An acidic organophosphorus reagent (DEHPA) and a basic tetraalkylammonium reagent (Aliquat-336) were used as extractants in the membrane liquid to selectively extract and enrich cationic and anionic metal species respectively. A speciation method for chromium species was developed that allowed the determination of cationic Cr(III) species and anionic CR(VI) species in natural water samples without the need of a chromatographic separation step prior to their detection. SLM was also coupled on-line to potentiometric stripping analysis providing a fast and sensitive method for analysis of Pb in urine samples. A microporous membrane liquid-liquid extraction (MMLLE) method was developed for the determination of organotin compounds in natural waters that reduced the number of manual steps involved in the LLE of organotin compounds prior to their CC separation. Clean extracts obtained after running unfiltered humic-rich river water samples through the MMLLE flow system allowed selective determination of all the organotin compounds in a single run using GC-MS in the selected ion monitoring mode (SIM) 171 refs, 9 figs, 4 tabs

  12. Magnetomotive room temperature dicationic ionic liquid: a new concept toward centrifuge-less dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Beiraghi, Asadollah; Shokri, Masood; Seidi, Shahram; Godajdar, Bijan Mombani

    2015-01-09

    A new centrifuge-less dispersive liquid-liquid microextraction technique based on application of magnetomotive room temperature dicationic ionic liquid followed by electrothermal atomic absorption spectrometry (ETAAS) was developed for preconcentration and determination of trace amount of gold and silver in water and ore samples, for the first time. Magnetic ionic liquids not only have the excellent properties of ionic liquids but also exhibit strong response to an external magnetic field. These properties provide more advantages and potential application prospects for magnetic ionic liquids than conventional ones in the fields of extraction processes. In this work, thio-Michler's ketone (TMK) was used as chelating agent to form Ag/Au-TMK complexes. Several important factors affecting extraction efficiency including extraction time, rate of vortex agitator, pH of sample solution, concentration of the chelating agent, volume of ionic liquid as well as effects of interfering species were investigated and optimized. Under the optimal conditions, the limits of detection (LOD) were 3.2 and 7.3ngL(-1) with the preconcentration factors of 245 and 240 for Au and Ag, respectively. The precision values (RSD%, n=7) were 5.3% and 5.8% at the concentration level of 0.05μgL(-1) for Au and Ag, respectively. The relative recoveries for the spiked samples were in the acceptable range of 96-104.5%. The results demonstrated that except Hg(2+), no remarkable interferences are created by other various ions in the determination of Au and Ag, so that the tolerance limits (WIon/WAu or Ag) of major cations and anions were in the range of 250-1000. The validated method was successfully applied for the analysis of Au and Ag in some water and ore samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Recovery of Acetic Acid from An Ethanol Fermentation Broth by Liquid-Liquid Extraction (LLE) Using Various Solvents

    International Nuclear Information System (INIS)

    Pham, Thi Thu Huong; Kim, Tae Hyun; Um, Byung Hwan

    2015-01-01

    Liquid-liquid extraction (LLE) using various solvents was studied for recovery of acetic acid from a synthetic ethanol fermentation broth. The microbial fermentation of sugars presented in hydrolyzate gives rise to acetic acid as a byproduct. In order to obtain pure ethanol for use as a biofuel, fermentation broth should be subjected to acetic acid removal step and the recovered acetic acid can be put to industrial use. Herein, batch LLE experiments were carried out at 25°C using a synthetic fermentation broth comprising 20.0 g l -1 acetic acid and 5.0 g l -1 ethanol. Ethyl acetate (EtOAc), tri-n-octylphosphine oxide (TOPO), tri-n-octylamine (TOA), and tri-n-alkylphosphine oxide (TAPO) were utilized as solvents, and the extraction potential of each solvent was evaluated by varying the organic phase-to-aqueous phase ratios as 0.2, 0.5, 1.0, 2.0, and 4.0. The highest acetic acid extraction yield was achieved with TAPO; however, the lowest ethanol-to-acetic acid extraction ratio was obtained using TOPO. In a single-stage batch extraction, 97.0 % and 92.4 % of acetic acid could be extracted using TAPO and TOPO when the ratio of organic-to-aqueous phases is 4:1 respectively. A higher solvent-to-feed ratio resulted in an increase in the ethanol-to-acetic acid ratio, which decreased both acetic acid purity and acetic acid extraction yield.

  14. Modified Dispersive Liquid-Liquid Micro Extraction Using Green Solvent for Determination of Polycyclic Aromatic Hydrocarbons (PAHs) in Vegetable Samples

    International Nuclear Information System (INIS)

    Kin, C.M.; Shing, W.L.

    2016-01-01

    According to International Agency for Research on Cancer (IARC), most of Polycyclic Aromatic Hydrocarbons (PAHs) known as genotoxic human carcinogen and mutagenic. PAHs represent as poorly degradable pollutants that exist in soils, sediments, surface water and atmosphere. A simple, rapid and sensitive extraction method termed modified Dispersive Liquid-Liquid Micro extraction (DLLME) using green solvent was developed to determine PAHs in vegetable samples namely radish, cabbage and cucumber prior to Gas Chromatography Flame Ionization Detection (GC-FID). The extraction method is based on replacing chlorinated organic extraction solvent in the conventional DLLME with low toxic solvent, 1-bromo-3-methylbutane without using dispersive solvent. Several experimental factors such as type and volume of extraction solvents, extraction time, confirmation of 12 PAHs by GC-MS, recovery percentages on vegetable samples and the comparative analysis with conventional DLLME were carried out. Both DLLME were successfully extracted 12 types of PAHs. In modified DLLME, the recoveries of the analytes obtained were in a range of 72.72 - 88.07 % with RSD value below 7.5 % which is comparable to the conventional DLLME. The use of microliter of low toxic extraction solvent without addition of dispersive solvent caused the method is economic and environmental friendly which is fulfill the current requirement, green chemistry based analytical method. (author)

  15. Lunar Oxygen Production and Metals Extraction Using Ionic Liquids

    Science.gov (United States)

    Marone, Matthew; Paley, Mark Steven; Donovan, David N.; Karr, Laurel J.

    2009-01-01

    Initial results indicate that ionic liquids are promising media for the extraction of oxygen from lunar regolith. IL acid systems can solubilize regolith and produce water with high efficiency. IL electrolytes are effective for water electrolysis, and the spent IL acid media are capable of regeneration.

  16. Hollow fiber liquid-phase microextraction of cadmium(II) using an ionic liquid as the extractant

    International Nuclear Information System (INIS)

    Chen, Hui; Wang, Yun; Hu, Yutao; Ni, Liang; Liu, Yingying; Kang, Wenbing; Liu, Yan; Han, Juan

    2014-01-01

    A method is presented for hollow fiber liquid-phase microextraction (HF-LPME) of cadmium(II), which is chelated with 1-(2-pyridylazo)-2-naphthol (PAN) to obtain a hydrophobic complex which then is extracted into a polypropylene hollow fiber containing an ionic liquid in its pores which acts as the membrane phase. EDTA is then injected into the lumen of the membrane as an acceptor phase to trap the analyte. The extraction time (20 min), agitation (400 rpm at 25 °C), pH value (10.0), and the concentrations of PAN (2.5 ng mL −1 ) and EDTA (250 ng mL −1 ) were optimized. With a sample volume of 50 mL and a stripping volume of 15 μL, the enrichment factor is 162. Cadmium(II) was then quantified by graphite furnace AAS. The limit of detection is 0.12 pg mL −1 , the relative standard deviation is 5.2 %, and the linear working range extends from 4 to 45 pg mL −1 . The method was successfully applied to the determination of Cd(II) in environmental and food samples. (author)

  17. Liquid-Liquid Extraction/Low-Temperature Purification (LLE/LTP Followed by Dispersive Solid-Phase Extraction (d-SPE Cleanup for Multiresidue Analysis in Palm Oil by LC-QTOF-MS

    Directory of Open Access Journals (Sweden)

    Elham Sobhanzadeh

    2013-01-01

    Full Text Available An evaluation of the extraction of multiresidue pesticides from palm oil by liquid-liquid extraction/low-temperature purification (LLE/LTP coupled with dispersive solid-phase extraction (d-SPE as the cleanup procedure with the determination by liquid chromatography mass spectrometry using electrospray as the ionization source (LC-ESI-MS was carried out. Optimization approaches were studied in terms of d-SPE to select efficiency of type and mass of adsorbents to obtain the highest recovery yield of pesticides and the lowest coextract fat residues in the final extract. The optimal conditions of d-SPE were obtained using 3 g of palm oil, 4 g anhydrous MgSO4, 150 mg of PSA, and 50 mg of GCB (PSA: GCB (3 : 1 w/w. Recovery study was performed at three concentration levels (25, 50, and 100 ng kg−1, yielding recovery rates between 71.8 and 112.4% except diuron with relative standard deviations of 3.2–15.1%. Detection and quantification limits were lower than 2.7 and 8.2 ng kg−1, respectively. The proposed method was successfully applied to the analysis of market-purchased palm oil samples from two different brands collected in Kuala Lumpur, showing its potential applicability and revealing the presence of some of the target species in the ng g−1 range.

  18. Removal of Radioactive Pollutants by Liquid Emulsion Membrane From Liquid Waste

    International Nuclear Information System (INIS)

    Yossef, Y.A.A.

    2013-01-01

    Radioactive liquid waste should be safely managed because it is potentially hazardous to human health and the environment. Several methods were used for treatment of liquid waste, such as liquid emulsion membrane (LEM). In this work, liquid emulsion membrane using Tri-butyl phosphate (TBP) plus Bis (2-ethylhexyl) phosphate (HDEHP) as mobile carriers, hydrochloric acid (HCl) as stripping agents and an emulsifying agent (span 80) was used for the extraction of uranium ions from radioactive liquid waste. Various parameters influencing the permeation of uranium ions through the membrane have been optimized to separate uranium ions from radioactive liquid waste such as: the effects of membrane material, carrier concentration, operating conditions, etc. were examined; moreover, the transport mechanism of this uranium was also studied. The internal mass transfer in the water/oil (W/O) emulsion drop, the external mass transfer around the drop, the rates of formation, and the decomposition of the complex at the external aqueous-organic interface were considered. The results show that, the liquid emulsion membrane which consists of (25% by volume HDEHP, 0.005 M + 75% by volume TBP, 0.01 M) as extractant (carrier), span 80, 4% (v/v) (sorbitan monooleate) as surfactant agent, hydrochloric acid (HCl), (1.0 M) as stripping agent. From the results, the maximum extraction percent of uranium ions (nearly about of 100%) occurred at the operating conditions: stirring speed =500 rpm, the ratio between LEM and feed phase (liquid waste) = 20 ml: 100 ml, the ratio between organic phase (membrane phase) to internal aqueous phase (stripping phase) = 1.0 and the ph value of the external aqueous phase equal to 5.0.

  19. The transfer of rare earth elements through liquid extraction membranes

    International Nuclear Information System (INIS)

    Kapranchik, V.P.; Proyaev, V.V.; Kopyrin, A.A.

    1988-01-01

    The transfer of rare earth elements through liquid extraction membranes, presenting Dacron nuclear filters, impregnated by extractants of different types (tributylphosphine oxide; di-2-ethylhexylphosphoric acid, HDEHP; trioctylamine, TOA) is investigated. It is ascertained that in systems with extractant-carriers TOA and HDEHP inversion of dependences of flow values and distribution coefficients on the element atomic number is observed. Mathematical model of transfer, permitting to establish relation between extractional and transport characteristics of the membrane, is suggested

  20. Isobaric vapor-liquid equilibria for the extractive distillation of 2-propanol + water mixtures using 1-ethyl-3-methylimidazolium dicyanamide ionic liquid

    International Nuclear Information System (INIS)

    Orchillés, A. Vicent; Miguel, Pablo J.; González-Alfaro, Vicenta; Llopis, Francisco J.; Vercher, Ernesto; Martínez-Andreu, Antoni

    2017-01-01

    Highlights: • VLE of binary and ternary systems of 2-propanol, water and [emim][DCA] at 100 kPa. • The e-NRTL model fits the VLE data of 2-propanol + water + [emim][DCA] system. • [emim][DCA] breaks the 2-propanol + water azeotrope at an IL mole fraction >0.085. - Abstract: Isobaric vapor–liquid equilibria for the binary systems 2-propanol + water, 2-propanol + 1-ethyl-3-methylimidazolium dicyanamide ([emim][DCA]), and water + [emim][DCA] as well as the vapor–liquid equilibria for the 2-propanol + water + [emim][DCA] ternary system have been obtained at 100 kPa using a recirculating still. The electrolyte nonrandom two-liquid (e-NRTL) model was used for fitting successfully the experimental data. The effect of [emim][DCA] on the 2-propanol + water system has been compared with that produced by other ionic liquids reported in the literature. From the results, [emim][DCA] appears as a good entrainer for the extractive distillation of this solvent mixture, causing the azeotrope to disappear at 100 kPa when the ionic liquid mole fraction is greater than 0.085.

  1. Feasibility of corona discharge ion mobility spectrometry for direct analysis of samples extracted by dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Jafari, Mohammad T; Riahi, Farhad

    2014-05-23

    The capability of corona discharge ionization ion mobility spectrometry (CD-IMS) for direct analysis of the samples extracted by dispersive liquid-liquid microextraction (DLLME) was investigated and evaluated, for the first time. To that end, an appropriate new injection port was designed and constructed, resulting in possibility of direct injection of the known sample volume, without tedious sample preparation steps (e.g. derivatization, solvent evaporation, and re-solving in another solvent…). Malathion as a test compound was extracted from different matrices by a rapid and convenient DLLME method. The positive ion mobility spectra of the extracted malathion were obtained after direct injection of carbon tetrachloride or methanol solutions. The analyte responses were compared and the statistical results revealed the feasibility of direct analysis of the extracted samples in carbon tetrachloride, resulting in a convenient methodology. The coupled method of DLLME-CD-IMS was exhaustively validated in terms of sensitivity, dynamic range, recovery, and enrichment factor. Finally, various real samples of apple, river and underground water were analyzed, all verifying the feasibility and success of the proposed method for the easy extraction of the analyte using DLLME separation before the direct analysis by CD-IMS. Copyright © 2014 Elsevier B.V. All rights reserved.

  2. Acid extraction by supported liquid membranes containing basic carriers

    International Nuclear Information System (INIS)

    Danesi, P.R.; Cianetti, C.; Horwitz, E.P.

    1983-01-01

    The extraction of HNO 3 (nitric acid) from aqueous solutions by permeation through a number of supported liquid membranes containing basic carriers dissolved in diethylbenzene has been studied. The results have shown that the best permeations are obtained with long chain aliphatic amines (TLA, Primene JM-T) followed by TOPO (trioctylphosphine oxide) and then by other monofunctional and bifunctional organophosphorous basic carriers. The influence of an aliphatic diluent on the permeability of HNO 3 through a supported liquid membrane containing TLA as carrier was also investigated. In this case the permeability to HNO 3 decreases as a result of the lower diffusion coefficient of the acid-carrier complex in the more vicous aliphatic solvent. 4 figures

  3. Extraction and preconcentration of trace Al and Cr from vegetable samples by vortex-assisted ionic liquid-based dispersive liquid-liquid microextraction prior to atomic absorption spectrometric determination.

    Science.gov (United States)

    Altunay, Nail; Yıldırım, Emre; Gürkan, Ramazan

    2018-04-15

    In the study, a simple, and efficient microextraction approach, which is termed as vortex-assisted ionic liquid-based dispersive liquid-liquid microextraction (VA-IL-DLLME), was developed for flame atomic absorption spectrometric analysis of aluminum (Al) and chromium (Cr) in vegetables. The method is based on the formation of anionic chelate complexes of Al(III) and Cr(VI) with o-hydroxy azo dye, at pH 6.5, and then extraction of the hydrophobic ternary complexes formed in presence of cetyltrimethylammonium bromide (CTAB) into a 125 μL volume of 1-butyl-3-methylimidazolium bis(trifluorosulfonyl)imide [C 4 mim][Tf 2 N]) as extraction solvent. Under optimum conditions, the detection limits were 0.02 µg L -1 in linear working range of 0.07-100 µg L -1 for Al(III), and 0.05 µg L -1 in linear working range of 0.2-80 µg L -1 for Cr(VI). After the validation by analysis of a certified reference material (CRM), the method was successfully applied to the determination of Al and Cr in vegetables using standard addition method. Copyright © 2017 Elsevier Ltd. All rights reserved.

  4. Multi-staging for extraction of cesium from nitric acid by a single liquid-liquid countercurrent centrifugal extractor with Taylor vortices

    International Nuclear Information System (INIS)

    Nakase, Masahiko; Kinuhata, Hiroshi; Takeshita, Kenji

    2013-01-01

    Fission products that emit considerable decay heat and radioactivity, such as 137 Cs, have a large impact on waste management. Small and high-performance extractor is desirable for separating such nuclei. In this study, we implemented the continuous extraction of Cs from nitric acid in a single liquid-liquid countercurrent centrifugal extractor with Taylor Vortices by calix arene-bis(t-octylbenzo-crown-6)(BOBCalixC6) as an extractant with trioctylamine(TOA) as a suppressant and with 1-(2,2,3,3-tetrafluoropropoxy)-3-(4-sec-butylphenoxy)-2-propanol (Cs-7SB) as a phase modifier. Because of slow extraction kinetics of this process, extraction with multiple theoretical stages by just replacing conventional extractors into the single centrifugal extractor is difficult. Hence, we improved the dispersion of organic phase by an inner rotor made of lipophilic epoxy resin and elevating the solution temperature to lower the viscosity. Higher temperature was not appropriate from the aspect of chemical equilibrium in this process, but extraction with multiple theoretical stages was found to be possible. (author)

  5. Determination of trace bisphenol A in environmental water by high-performance liquid chromatography using magnetic reduced graphene oxide based solid-phase extraction coupled with dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Li, Danping; Ma, Xiaoguo; Wang, Rui; Yu, Yumian

    2017-02-01

    Bisphenol A (BPA), an endocrine-disrupting chemical, has received much attention from researchers and the general public. In this paper, a novel method of determining BPA at trace levels was developed, using magnetic reduced graphene oxide (rGO-Fe 3 O 4 )-based solid-phase extraction coupled with dispersive liquid-liquid microextraction (DLLME), followed by high-performance liquid chromatographic determination. The rGO-Fe 3 O 4 was prepared and then characterized by Fourier transform infrared spectroscopy, transmission electron microscopy, and vibrating sample magnetometry. The greatest saturation magnetization of rGO-Fe 3 O 4 was up to 43.8 emu g -1 , which allowed rapid isolation of the rGO-Fe 3 O 4 from solutions upon applying an appropriate magnetic field. The effects of solution pH, adsorbent amount, type and volume of eluent and extraction solvent, extraction time, and salt concentration on the extraction efficiency of BPA were examined and optimized. Under the optimum conditions, an enrichment factor of 5217 and an LOD of 0.01 μg L -1 for BPA were obtained. The reusability of rGO-Fe 3 O 4 for at least 12 repeated cycles without any significant decrease in the extraction recovery of BPA was demonstrated. The proposed method was applied to the determination of BPA in different real water samples, with relative recoveries of 84.8-104.9 % and RSDs of 0.8-8.3 % in the spiked concentration range 1-10 μg L -1 .

  6. Liquid-Liquid Equilibrium data for mono ethylene glycol extraction from water with the new ionic liquid tetraoctyl ammonium 2-methyl-1-naphtoate as solvent

    NARCIS (Netherlands)

    Garcia Chavez, L.Y.; Schuur, Boelo; de Haan, A.B.

    2012-01-01

    Thermal recovery of mono ethylene glycol (MEG) from aqueous streams is one of the most energy demanding operations in industry, because of the large amount of water that needs to be evaporated. The use of alternative technologies such as liquid–liquid extraction could save energy. A new tailor made

  7. Liquid-liquid equilibrium data for mono ethylene glycol extraction from water with the new ionic liquid tetraoctyl ammonium 2-methyl-1-naphtoate as solvent

    NARCIS (Netherlands)

    Garcia Chavez, L.Y.; Schuur, B.; Haan, de A.B.

    2012-01-01

    Thermal recovery of mono ethylene glycol (MEG) from aqueous streams is one of the most energy demanding operations in industry, because of the large amount of water that needs to be evaporated. The use of alternative technologies such as liquid–liquid extraction could save energy. A new tailor made

  8. Determination of Fusarium toxins in functional vegetable milks applying salting-out-assisted liquid-liquid extraction combined with ultra-high-performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Hamed, Ahmed M; Arroyo-Manzanares, Natalia; García-Campaña, Ana M; Gámiz-Gracia, Laura

    2017-11-01

    Vegetable milks are considered as functional foods due to their physiological benefits. Although the consumption of these products has significantly increased, they have received little attention in legislation with regard to contaminants. However, they may contain mycotoxins resulting from the use of contaminated raw materials. In this work, ultra-high-performance liquid chromatography tandem mass spectrometry has been proposed for the determination of the most relevant Fusarium toxins (fumonisin B 1 and B 2 , HT-2 and T-2 toxins, zearalenone, deoxynivalenol and fusarenon-X) in different functional beverages based on cereals, legumes and seeds. Sample treatment consisted of a simple salting-out-assisted liquid-liquid extraction with no further clean-up. The method provided limits of quantification between 3.2 and 57.7 µg L -1 , recoveries above 80% and precision with RSD lower than 12%. The method was also applied for studying the occurrence of these mycotoxins in market samples of vegetable functional beverages and deoxynivalenol was found in three oat-based commercial drinks.

  9. Ultra-high performance liquid chromatography with fluorescence detection following salting-out assisted liquid-liquid extraction for the analysis of benzimidazole residues in farm fish samples.

    Science.gov (United States)

    Tejada-Casado, Carmen; Lara, Francisco J; García-Campaña, Ana M; Del Olmo-Iruela, Monsalud

    2018-03-30

    Ultra-high performance liquid chromatography (UHPLC) coupled with fluorescence detection (FL) has been proposed for the first time to determine thirteen benzimidazoles (BZs) in farmed fish samples. In order to optimize the chromatographic separation, parameters such as mobile phase composition and flow rate were carefully studied, establishing a gradient mode with a mobile phase consisted of water (solvent A) and acetonitrile (solvent B) at a flow rate of 0.4 mL/min. The separation was performed on a Zorbax Eclipse Plus RRHD C 18 column (50 × 2.1 mm, 1.8 μm), involving a total analysis time lower than 12 min. Salting-out assisted liquid-liquid extraction (SALLE) was applied as sample treatment to different types of farmed fish (trout, sea bream and sea bass). To obtain satisfactory extraction efficiencies for the studied analytes, several parameters affecting the SALLE procedure were optimized including the amount of sample, type and volume of the extraction solvent, and the nature and amount of the salt used. Characterization of the method in terms of performance characteristics was carried out, obtaining satisfactory results for the linearity (R 2  ≥ 0.997), repeatability (RSD ≤ 6.1%), reproducibility (RSD ≤ 10.8%) and recoveries (R ≥ 79%; RSD ≤ 7.8%). Detection limits between 0.04-29.9 μg kg -1 were obtained, demonstrating the applicability of this fast, simple and environmentally friendly method. Copyright © 2018 Elsevier B.V. All rights reserved.

  10. Separation of thorium and uranium by liquid-liquid extraction from mixed aqueous nitric acidic-methanolic solutions

    International Nuclear Information System (INIS)

    Schmid, E.R.; Kenndler, E.

    1976-01-01

    A method is described for the separation of Th and U from each other and from other elements, usually occuring in minerals, by liquid-liquid extraction with Aliquat Nitrate (tricaprylmethyl ammoniumnitrate, 6 vol%) in benzene from a mixed solution of 2.5 M HNO 3 and methanol (1:1 volume ratio). Permissible upper concentration ratios of interfering elements, such as Li, Na, K, Mg, Ca, Al, Cu, Co(II), Fe(III), Mn(II), Ti(IV), La(III), U(VI), Cl - , ClO 4 - , SO 4 2- , PO 4 3- , have been determined. Following the separation, Th has been determined by spectrophotometry using Thorin, and U by fluorometry. Results for yield under varying conditions, together with elemental concentrations in the ppm range for U and Th in minerals, are given. (B.T.)

  11. Solid-phase extraction assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet to determine sildenafil and its analogues in dietary supplements.

    Science.gov (United States)

    Li, Jing; Roh, Si Hun; Shaodong, Jia; Hong, Ji Yeon; Lee, Dong-Kyu; Shin, Byong-Kyu; Park, Jeong Hill; Lee, Jeongmi; Kwon, Sung Won

    2017-08-01

    A novel analytical method for the simultaneous determination of the concentration of sildenafil and its five analogues in dietary supplements using solid-phase extraction assisted reversed-phase dispersive liquid-liquid microextraction based on solidification of floating organic droplet combined with ion-pairing liquid chromatography with an ultraviolet detector was developed. Parameters that affect extraction efficiency were systematically investigated, including the type of solid-phase extraction cartridge, pH of the extraction environment, and the type and volume of extraction and dispersive solvent. The method linearity was in the range of 5.0-100 ng/mL for sildenafil, homosildenafil, udenafil, benzylsildenafil, and thiosildenafil and 10-100 ng/mL for acetildenafil. The coefficients of determination were ≥0.996 for all regression curves. The sensitivity values expressed as limit of detection were between 2.5 and 7.5 ng/mL. Furthermore, intraday and interday precisions expressed as relative standard deviations were less than 5.7 and 9.9%, respectively. The proposed method was successfully applied to the analysis of sildenafil and its five analogues in complex dietary supplements. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. The optimization of extraction of antioxidants from apple pomace by pressurized liquids.

    Science.gov (United States)

    Wijngaard, Hilde; Brunton, Nigel

    2009-11-25

    Pressurized liquid extraction (PLE) is a green extraction technique that can enhance extraction rates of bioactive compounds. PLE was used to extract antioxidants and polyphenols from industrially generated apple pomace at two different temperature ranges: 160 to 193 degrees C and 75 to 125 degrees C. Antioxidant activity (DPPH radical scavenging test), total phenol content and three individual polyphenol groups were determined. Response surface methodology was used to optimize the five response values. Maximum antioxidant activity was obtained at a temperature of 200 degrees C, but unwanted compounds such as hydroxymethylfurfural were formed. Therefore a lower temperature range between 75 and 125 degrees C is recommended. Using this temperature range, a maximum antioxidant activity was determined at 60% ethanol and 102 degrees C. By using PLE the antioxidant activity was increased 2.4 times in comparison to traditional solid-liquid extraction, and the technique may be a promising alternative to conventional techniques for extracting antioxidants.

  13. Trace determination of five triazole fungicide residues in traditional Chinese medicine samples by dispersive solid-phase extraction combined with ultrasound-assisted dispersive liquid-liquid microextraction and UHPLC-MS/MS.

    Science.gov (United States)

    Ma, Shuping; Yuan, Xucan; Zhao, Pengfei; Sun, Hong; Ye, Xiu; Liang, Ning; Zhao, Longshan

    2017-08-01

    A novel and reliable method for determination of five triazole fungicide residues (triadimenol, tebuconazole, diniconazole, flutriafol, and hexaconazol) in traditional Chinese medicine samples was developed using dispersive solid-phase extraction combined with ultrasound-assisted dispersive liquid-liquid microextraction before ultra-high performance liquid chromatography with tandem mass spectrometry. The clean up of the extract was conducted using dispersive solid-phase extraction by directly adding sorbents into the extraction solution, followed by shaking and centrifugation. After that, a mixture of 400 μL trichloromethane (extraction solvent) and 0.5 mL of the above supernatant was injected rapidly into water for the dispersive liquid-liquid microextraction procedure. The factors affecting the extraction efficiency were optimized. Under the optimum conditions, the calibration curves showed good linearity in the range of 2.0-400 (tebuconazole, diniconazole, and hexaconazole) and 4.0-800 ng/g (triadimenol and flutriafol) with the regression coefficients higher than 0.9958. The limit of detection and limit of quantification for the present method were 0.5-1.1 and 1.8-4.0 ng/g, respectively. The recoveries of the target analytes ranged from 80.2 to 103.2%. The proposed method has been successfully applied to the analysis of five triazole fungicides in traditional Chinese medicine samples, and satisfactory results were obtained. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Ionic liquid-based microwave-assisted dispersive liquid-liquid microextraction and derivatization of sulfonamides in river water, honey, milk, and animal plasma

    Energy Technology Data Exchange (ETDEWEB)

    Xu Xu; Su Rui; Zhao Xin; Liu Zhuang; Zhang Yupu; Li Dan; Li Xueyuan; Zhang Hanqi [College of Chemistry, Jilin University, Changchun 130012 (China); Wang Ziming, E-mail: analchem@jlu.edu.cn [College of Chemistry, Jilin University, Changchun 130012 (China)

    2011-11-30

    Graphical abstract: The extraction and derivatization efficiency of SAs is dependent on type and volume of extraction solvent, type and volume of disperser, microwave power and irradiation time, volume of derivatization reagent, pH of sample solution as well as ionic strength. Highlights: Black-Right-Pointing-Pointer A new, rapid and sensitive method for determining sulfonamides (SAs) was proposed. Black-Right-Pointing-Pointer Derivatization, extraction and preconcentration of SAs were performed in one step. Black-Right-Pointing-Pointer IL-based MADLLME and derivatization were first applied for the determination of SAs. Black-Right-Pointing-Pointer Trace SAs in river water, honey, milk, and pig plasma were determined. - Abstract: The ionic liquid-based microwave-assisted dispersive liquid-liquid microextraction (IL-based MADLLME) and derivatization was applied for the pretreatment of six sulfonamides (SAs) prior to the determination by high-performance liquid chromatography (HPLC). By adding methanol (disperser), fluorescamine solution (derivatization reagent) and ionic liquid (extraction solvent) into sample, extraction, derivatization, and preconcentration were continuously performed. Several experimental parameters, such as the type and volume of extraction solvent, the type and volume of disperser, amount of derivatization reagent, microwave power, microwave irradiation time, pH of sample solution, and ionic strength were investigated and optimized. When the microwave power was 240 W, the analytes could be derivatized and extracted simultaneously within 90 s. The proposed method was applied to the analysis of river water, honey, milk, and pig plasma samples, and the recoveries of analytes obtained were in the range of 95.0-110.8, 95.4-106.3, 95.0-108.3, and 95.7-107.7, respectively. The relative standard deviations varied between 1.5% and 7.3% (n = 5). The results showed that the proposed method was a rapid, convenient and feasible method for the determination

  15. Extraction separation of toluene/cyclohexane with hollow fiber supported ionic liquid membrane

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Fan; Sun, Wei; Liu, Junteng; Zhang, Weidong; Ren, Zhongqi [Beijing University of Chemical Technology, Beijing (China)

    2014-06-15

    A supported liquid membrane with ionic liquid was used for the separation of toluene/cyclohexane. The interactions of ionic liquid with toluene and cyclohexane were calculated and experimentally studied by quantum chemical calculation and liquid-liquid extraction process. The results showed [BPy][BF{sub 4}] have stronger interaction with toluene than that with cyclohexane. The selectivity of SILM processes was larger than 10 at the temperature of 323 K and the flow rate of 13.5 mL·min{sup -1} on both shell side and lumen side. Due to the higher viscosity of IL, SILM process had good long-term stability. As the effects of mass transfer driving force of SILM process, the flux and removal efficiency increased with increase of initial toluene concentration, while the selectivity decreased because of the competitive transport. Base on the resistance in-series model and experimental results, the mass transfer resistance was mainly lay liquid membrane phase. The influence of flow rates on both sides was slight. The higher temperature could enhance the mass transfer performance significantly. The removal efficiency increased from 28.2% to 45.1% with the increasing of operation temperature from 298 K to 323 K.

  16. Non-porous membrane-assisted liquid-liquid extraction of UV filter compounds from water samples.

    Science.gov (United States)

    Rodil, Rosario; Schrader, Steffi; Moeder, Monika

    2009-06-12

    A method for the determination of nine UV filter compounds [benzophenone-3 (BP-3), isoamyl methoxycinnamate, 4-methylbenzylidene camphor, octocrylene (OC), butyl methoxydibenzoylmethane, ethylhexyl dimethyl p-aminobenzoate (OD-PABA), ethylhexyl methoxycinnamate (EHMC), ethylhexyl salicylate and homosalate] in water samples was developed and evaluated. The procedure includes non-porous membrane-assisted liquid-liquid extraction (MALLE) and LC-atmospheric pressure photoionization (APPI)-MS/MS. Membrane bags made of different polymeric materials were examined to enable a fast and simple extraction of the target analytes. Among the polymeric materials tested, low- and high-density polyethylene membranes proved to be well suited to adsorb the analytes from water samples. Finally, 2 cm length tailor-made membrane bags were prepared from low-density polyethylene in order to accommodate 100 microL of propanol. The fully optimised protocol provides recoveries from 76% to 101% and limits of detection (LOD) between 0.4 ng L(-1) (OD-PABA) and 16 ng L(-1) (EHMC). The interday repeatability of the whole protocol was below 18%. The effective separation of matrix molecules was proved by only marginal matrix influence during the APPI-MS analysis since no ion suppression effects were observed. During the extraction step, the influence of the matrix was only significant when non-treated wastewater was analysed. The analysis of lake water indicated the presence of seven UV filter compounds included in this study at concentrations between 40 ng L(-1) (BP-3) and 4381 ng L(-1) (OC). In non-treated wastewater several UV filters were also detected at concentration levels as high as 5322 ng L(-1) (OC).

  17. Comparison between different liquid-liquid and solid phase methods of extraction prior to the identification of the phenolic fraction present in olive oil washing wastewater from the two-phase olive oil extraction system

    Directory of Open Access Journals (Sweden)

    S. Jiménez-Herrera

    2017-09-01

    Full Text Available Phenolic compounds from olive mill wastewater (OMW, are characterized by a strong antioxidant activity. At the same time, they represent an environmental problem because they are difficult to degrade. The purpose of this work was to identify these biologically active compounds in the OMW from two-phase olive oil production in order to convert a polluting residue into a source of natural antioxidants. After optimizing the extraction process of phenolic compounds using liquid-liquid extraction (LLE and solid phase extraction (SPE methods, it was determined that the most appropriate sequence comprised a previous centrifugation to remove the lipid fraction, followed by liquid extraction with ethyl acetate or SPE. The most important compounds identified in olive oil washing wastewater (OOWW were tyrosol, hydroxytyrosol and succinic acid; whereas the ones in the wastewater derived from the washing of the olives (OWW were cresol, catechol, 4-methylcatechol, hydrocinnamic acid and p-hydroxy-hydrocinnamic acid.

  18. Comparison between different liquid-liquid and solid phase methods of extraction prior to the identification of the phenolic fraction present in olive oil washing wastewater from the two-phase olive oil extraction system

    International Nuclear Information System (INIS)

    Jiménez-Herrera, S.; Ochando-Pulido, J.M.; Martínez-Ferez, A.

    2017-01-01

    Phenolic compounds from olive mill wastewater (OMW), are characterized by a strong antioxidant activity. At the same time, they represent an environmental problem because they are difficult to degrade. The purpose of this work was to identify these biologically active compounds in the OMW from two-phase olive oil production in order to convert a polluting residue into a source of natural antioxidants. After optimizing the extraction process of phenolic compounds using liquid-liquid extraction (LLE) and solid phase extraction (SPE) methods, it was determined that the most appropriate sequence comprised a previous centrifugation to remove the lipid fraction, followed by liquid extraction with ethyl acetate or SPE. The most important compounds identified in olive oil washing wastewater (OOWW) were tyrosol, hydroxytyrosol and succinic acid; whereas the ones in the wastewater derived from the washing of the olives (OWW) were cresol, catechol, 4-methylcatechol, hydrocinnamic acid and p-hydroxy-hydrocinnamic acid. [es

  19. Evaluation and application of microwave-assisted extraction and dispersive liquid-liquid microextraction followed by high-performance liquid chromatography for the determination of polar heterocyclic aromatic amines in hamburger patties.

    Science.gov (United States)

    Aeenehvand, Saeed; Toudehrousta, Zahra; Kamankesh, Marzieh; Mashayekh, Morteza; Tavakoli, Hamid Reza; Mohammadi, Abdorreza

    2016-01-01

    This study developed an analytical method based on microwave-assisted extraction and dispersive liquid-liquid microextraction followed by high-performance liquid chromatography for the determination of three polar heterocyclic aromatic amines from hamburger patties. Effective parameters controlling the performance of the microextraction process, such as the type and volume of extraction and disperser solvents, microwave time, nature of alkaline aqueous solution, pH and salt amount, were optimized. The calibration graphs were linear in the range of 1-200 ng g(-1), with a coefficient of determination (R(2)) better than 0.9993. The relative standard deviations (RSD) for seven analyses were between 3.2% and 6.5%. The recoveries of those compounds in hamburger patties were from 90% to 105%. Detection limits were between 0.06 and 0.21 ng g(-1). A comparison of the proposed method with the existing literature demonstrates that it is a simple, rapid, highly selective and sensitive, and it gives good enrichment factors and detection limits for determining HAAs in real hamburger patties samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

  20. Effect of anions and cations on liquid extraction of TcO{sub 4} - in ionic liquids; Vplyv anionov a kationov na kvapalinovu extrakciu TcO4 - v ionovych kvapalinach

    Energy Technology Data Exchange (ETDEWEB)

    Suchanek, P.; Galambos, M.; Meciarova, M.; Rajec, P [Univerzita Komenskeho, Prirodovedecka fakulta, Katedra jadrovej chemie, 84215 Bratislava (Slovakia)

    2013-04-16

    An influence of monovalent and divalent cations and anions on an liquid extraction of pertechnetate anion from aqueous media using ionic liquids solubilized in various organic solvents has been studied. Suppression of extraction percentage was obtained with a divalent cations in a compare with monovalent cations showing almost no influence on extraction percentage. In a case of anions, perchlorate anion suppressed the extraction percentage in a highest degree. (authors)

  1. Liquid Membrane System for Extraction and Electrodeposition of Lead(II During Electrodialysis

    Directory of Open Access Journals (Sweden)

    Sadyrbaeva Tatiana

    2017-05-01

    Full Text Available A novel method for lead(II removal from aqueous acidic solutions is presented. The method involves electrodialysis through bulk liquid membranes accompanied by electrodeposition of metal from the cathodic solution. Solutions of di(2-ethylhexylphosphoric acid with admixtures of tri-n-octylamine in 1,2-dichloroethane were used as the liquid membranes. The effects of the main electrodialysis parameters as well as of the composition of the liquid membranes and aqueous solutions on the lead(II transport rate are studied. The optimal conditions are determined. A possibility of effective single-stage transfer of lead(II through the liquid membrane into dilute solutions of perchloric, nitric and acetic acids is demonstrated. Dense and adherent lead electrodeposits are obtained from perchloric acid solutions. Maximum extraction degree of 93 % and electrodeposition degree of ~60 % are obtained during 5 h of electrodialysis.

  2. The solid-liquid extraction separation of lithium isotopes by porous composite materials doped with ionic liquids and 2,2'-binaphthyldiyl-17-crown-5

    International Nuclear Information System (INIS)

    Xiao-Li Sun; Ling Gu; Dan Qiu; Dong-Hong Ren; Zaijun Li; Zhi-Guo Gu; Jiangnan University, Wuxi

    2015-01-01

    A green and efficient solid-liquid extraction method of lithium isotopes separation by porous composite materials doped with imidazolium ionic liquids and 2,2'-binaphthyldiyl-17-crown-5 has been reported in this paper. The composite materials of mesoporous silica and impregnated resin were synthesized by sol-gel and direct impregnation process, respectively. Various extraction parameters such as the concentration of lithium salt, anion of lithium salt, initial pH, time and temperature were investigated. Under optimized conditions, the maximum single-stage separation factor of 6 Li/ 7 Li was 1.048 ± 0.002, the maximum extraction efficiency was 15.86 %. The sorbents can be regenerated easily with HCl solution and reused repeatedly. (author)

  3. Ionic liquids based simultaneous ultrasonic and microwave assisted extraction of phenolic compounds from burdock leaves

    International Nuclear Information System (INIS)

    Lou Zaixiang; Wang Hongxin; Zhu Song; Chen Shangwei; Zhang Ming; Wang Zhouping

    2012-01-01

    The ionic liquids based simultaneous ultrasonic and microwave assisted extraction (IL-UMAE) technique was first proposed and applied to isolate compounds. The ionic liquids comprising a range of four anions, five 1-alkyl-3-methylimidazolium derivatives were designed and prepared. The results suggested that varying the anion and cation both had apparent effects on the extraction of phenolics. The results also showed that irradiation power, time and solid–liquid ratio significantly affected the yields. The yields of caffeic acid and quercetin obtained by IL-UMAE were higher than those by regular UMAE. Compared with conventional heat-reflux extraction (HRE), the proposed approach exhibited higher efficiency (8–17% enhanced) and shorter extraction time (from 5 h to 30 s). The results indicated ILUMAE to be a fast and efficient extraction technique. Moreover, the proposed method was validated by the reproducibility and recovery experiments. The ILUMAE method provided good recoveries (from 96.1% to 105.3%) with RSD lower than 5.2%, which indicated that the proposed method was credible. Based on the designable nature of ionic liquids, and the rapid and highly efficient performance of the proposed approach, ILUMAE provided a new alternative for preparation of various useful substances from solid samples.

  4. Reactive liquid/liquid extraction of heavy metals from landfill seepage waters. Its characterisation and application

    International Nuclear Information System (INIS)

    Woller, N.

    1994-06-01

    This study demonstrates the applicability of liquid-liquid extraction by means of the commercial complexers LIX26 R and LIX84 R to heavy metal removal from waste waters. The composition of this oil-soluble complex is MeR 2 , where Me denotes Hg 2+ , Cd 2+ , Zn 2+ , Cu 2+ , and Ni 2+ , and R denotes LIX84 R . This composition makes the complex electrically neutral, and all polar groups are located inside the molecule. The extraction efficiency of the complexer LIX84 R for the various metal ions is evident in the succession Cu 2+ , Ni 2+ >> Zn 2+ > Hg 2+ > Cd 2+ . These heavy metal ions are even readily extractable at chloride concentrations of up to 1 mol/l. As the structure of the complexer is that of an oil-soluble surfactant with complexing properties, it accumulates at the phase boundary between oil and water. Measurement of interfacial tension in various solvent systems showed that the polar solvent chloroform permits only a weak accumulation of the complexer (400 nmol/m 2 ), whereas the unpolar solvent kerosine permits greater accumulation specifically on the water side of the phase boundary (1958 nmol/m 2 ). Organic solvents solvate the complexer so well, that it is even removed from the air side of the phase boundary. The differing accumulation of the complexer at the water/oil phase boundary explains the differing increase of phase separation time for polar and unpolar solvents. (orig.) [de

  5. Solvent extraction in the treatment of acidic high-level liquid waste : where do we stand?

    International Nuclear Information System (INIS)

    Horwitz, E. P.; Schulz, W. W.

    1998-01-01

    During the last 15 years, a number of solvent extraction/recovery processes have been developed for the removal of the transuranic elements, 90 Sr and 137 Cs from acidic high-level liquid waste. These processes are based on the use of a variety of both acidic and neutral extractants. This chapter will present an overview and analysis of the various extractants and flowsheets developed to treat acidic high-level liquid waste streams. The advantages and disadvantages of each extractant along with comparisons of the individual systems are discussed

  6. U(VI) extraction by 8-hydroxyquinoline. A comparison study in ionic liquid and in dichloromethane

    Energy Technology Data Exchange (ETDEWEB)

    Yuan, Li-Yong; Shi, Wei-Qun [Chinese Academy of Sciences, Beijing (China). Lab. of Nuclear Energy Chemistry; Liao, Xiang-Hong [Chinese Academy of Sciences, Beijing (China). Lab. of Nuclear Energy Chemistry; East China Institute of Technology, Nanchang (China). School of Nuclear Engineering and Geophysics; Liu, Zhi-Rong [East China Institute of Technology, Nanchang (China). School of Nuclear Engineering and Geophysics; Chai, Zhi-Fang [Chinese Academy of Sciences, Beijing (China). Lab. of Nuclear Energy Chemistry; Soochow Univ., Suzhou (China). School of Radiological and Interdisciplinary Sciences and Collaborative Innovation Center of Radiation Medicine

    2017-08-01

    Room temperature ionic liquids (RTILs) represent a recent new class of solvents with potential application in liquid/liquid extraction based nuclear fuel reprocessing due to their unique physical and chemical properties. The work herein provides a comparison of U(VI) extraction by 8-hydroxyquinoline (HOX) in a commonly used RTIL, i.e. 1-butyl-3-methylimidazolium hexafluorophosphate ([C{sub 4}mim][PF{sub 6}]) and in conventional solvent, i.e. dichloromethane (CH{sub 2}Cl{sub 2}). The effect of HOX concentration, solution acidity and nitrate ions on the extraction were discussed in detail, and the speciation analyses of the extracted U(VI) were performed. One of the main emphasis of this work is the extraction mechanism of U(VI) extracted from aqueous phase into RTILs and conventional solvent. In CH{sub 2}Cl{sub 2}, the extraction occurs through a combination of ion change and neutral complexation, and the extracted complex is proposed as UO{sub 2}(OX){sub 2}HOX. In [C{sub 4}mim][PF{sub 6}], although a cation-change mechanism as previously reported for RTILs-based system was involved, the extracted complex of UO{sub 2}(OX){sub 1.5}(HOX){sub 1.5}(PF6){sub 0.5} gave a clear indication that the usage of HOX as an acidic extractant markedly inhibited the solubility loss of [C{sub 4}mim][PF{sub 6}] during the extraction by leaching H{sup +} to aqueous phase. Moreover, the extracted U(VI) in [C{sub 4}mim][PF{sub 6}] can be easily stripped by using 0.01 M nitric acid, which provides a simple way of the ionic liquid recycling.

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

    Science.gov (United States)

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

    2015-03-15

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

  8. Poisoning of liquid membrane carriers in extraction of metal ions

    International Nuclear Information System (INIS)

    Wang, Yuchun; Wang, Dexian

    1992-01-01

    As means of effective separation and preconcentration, emulsion liquid membranes (ELMs) have found application in many fields including biochemical separation, wastewater treatment, hydrometallurgy, and preconcentration in analytical chemistry. In the extraction of desired metal (scandium, mixed rare earths) ions using chelating extractants (TTA, HDEHP) as liquid membrane carriers, the carriers will become poisoned owing to the presence of even minute quantity of certain high ionic potential ions in the feed solution. The reason for the poisoning of carriers is that those ions have so much greater affinity than the desired ions for the membrane carrier that the ion-carrier coordination compound cannot be stripped at the interior interface of the membrane and gradually no more free carrier transports any metal ions across the membrane. The calculated results are in agreement with the experiments, and methods to avoid the poisoning are given in the paper

  9. Optimization and application of homogeneous liquid-liquid extraction in preconcentration of copper (II) in a ternary solvent system

    Energy Technology Data Exchange (ETDEWEB)

    Farajzadeh, Mir Ali [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)], E-mail: farajzade@yahoo.com; Bahram, Morteza [Department of Chemistry, Faculty of Science, Urmia University, Urmia (Iran, Islamic Republic of); Zorita, Saioa [Department of Analytical Chemistry, University of Lund, P.O. Box 124, 221 00 Lund (Sweden); Mehr, Behzad Ghorbani [Department of Chemistry, Faculty of Science, Urmia University, Urmia (Iran, Islamic Republic of)

    2009-01-30

    In this study a homogeneous liquid-liquid extraction based on the Ph-dependent phase-separation process was investigated using a ternary solvent system (water-acetic acid-chloroform) for the preconcentration of Cu{sup 2+} ions. 8-Hydroxy quinoline was used as the chelating agent prior to its extraction. Flame atomic absorption spectrophotometry using acetylene-air flame was used for the quantitation of analyte after preconcentration. The effect of various experimental parameters in extraction step was investigated using two optimization methods, one variable at a time and central composite design. The experimental design was done at five levels of operating parameters. Nearly the same optimized results were obtained using both methods: sample size, 5 mL; volume of NaOH 10 M, 2 mL; chloroform volume, 300 {mu}L; 8-hydroxy quinoline concentration more than 0.01 M and salt amount did not affect the extraction significantly. Under the optimum conditions the calibration graph was linear over the range 10-2000 {mu}g L{sup -1}. The relative standard deviation was 7.6% for six repeated determinations (C = 500 {mu}g L{sup -1}). Furthermore, the limit of detection (S/N = 3) and limit of quantification (S/N = 10) of the method were obtained as 1.74 and 6 {mu}g L{sup -1}, respectively.

  10. (Liquid + liquid) equilibria for the ternary mixtures (alkane + toluene + ionic liquid) at T = 298.15 K: Influence of the anion on the phase equilibria

    International Nuclear Information System (INIS)

    Seoane, Raquel G.; Gómez, Elena; González, Emilio J.; Domínguez, Ángeles

    2012-01-01

    Highlights: ► [BMpyr][NTF 2 ] and [BMpyr][TFO] were studied as solvents to extract aromatics from alkanes. ► (Liquid + liquid) equilibrium data were measured at 298.15 K for six ternary systems. ► Selectivity and solute distribution ratio were calculated and compared. ► The influence of the structure of anion of the ionic liquid was analyzed. ► Experimental data were satisfactorily correlated using NRTL model. - Abstract: (Liquid + liquid) equilibrium data for the ionic liquids 1-butyl-1-methylpyrrolidinium bis(trifluoromethylsulfonyl)imide, [BMpyr][NTf 2 ], and 1-butyl-1-methylpyrrolidinium trifluoromethanesulfonate, [BMpyr][TFO], with toluene, and heptane or cyclohexane were determined at T = 298.15 K and atmospheric pressure. In order to check if these ILs can be used as potential solvents for the extraction of toluene from aliphatic compounds, the ability of the ILs as solvents was evaluated in terms of selectivity and solute distribution ratio. The experimental data were correlated accurately with the Non Random Two-Liquid model.

  11. Extracting energy and structure properties of glass-forming liquids from structural relaxation time.

    Science.gov (United States)

    Wang, Lianwen

    2012-04-18

    A comprehensive examination of the kinetic liquid model (Wang et al 2010 J. Phys.: Condens. Matter 22 455104) is carried out by fitting the structural relaxation time of 26 different glass-forming liquids in a wide temperature range, including most of the well-studied materials. Careful analysis of the compiled reported data reveals that experimental inaccuracies should not be overlooked in any 'benchmark test' of relating theories or models (e.g. in Lunkenheimer et al 2010 Phys. Rev. E 81 051504). The procedure, accuracy, ability, and efficiency of the kinetic liquid model are discussed in detail and in comparison with other available fitting methods. In general, the kinetic liquid model could be verified by 17 of the 26 compiled data sets and can serve as a meaningful approximative method for analyzing these liquids. Nonetheless, further experimental examinations in a wide temperature range are needed and are called for. Through fitting, the microscopic details of these liquids are extracted, namely, the enthalpy, entropy, and cooperativity in structural relaxation, which may facilitate further quantitative analysis to both the liquidus and glassy states of these materials.

  12. Solid-Liquid Extraction Kinetics of Total Phenolic Compounds (TPC from Red Dates

    Directory of Open Access Journals (Sweden)

    Bee Lin Chua

    2018-01-01

    Full Text Available Red dates are one of the most famous herbal plants in making traditional Chinese medicine. They contain large amount of bioactive compounds. The objectives of this research were to optimise the crude extract yield and total phenolic compounds (TPC yield from red dates using response surface methodology (RSM and model the extraction kinetics of TPC yield from red dates. Date fruits were dried in an oven under temperatures 50°C, 60°C, 70°C and 80°C until a constant weight was obtained. The optimum drying temperature was 60°C as it gave the highest crude extract yield and TPC yield. Besides that, single factor experiments were used to determine the optimum range of four extraction parameters which were: liquid-solid ratio (10-30 ml/g; ultrasonic power (70-90%; extraction temperature (50-70°C; and extraction time (40-60min. The optimum range of the four parameters were further optimised using the Box-Behken Design (BBD of RSM. The extraction conditions that gave the highest crude extract yield and TPC yield were chosen. The optimum value for liquid-solid ratio, ultrasonic power, extraction temperature and extraction time were 30ml/g, 70%, 60°C and 60 min respectively. The two equations generated from RSM were reliable and can be used to predict the crude extract yield and TPC yield. The higher the extraction temperature, liquid-solid ratio, and extraction time and lower ultrasonic power, the higher the crude extract and TPC yield. Finally, the results of TPC yield versus time based on the optimum extraction parameters from RSM optimisation were fitted into three extraction kinetic models (Peleg’s model, Page’s model and Ponomaryov’s model. It was found that the most suitable kinetic model to represent the extraction process of TPC from red dates was Page’s model due to its coefficient of determination (R2 was the closest to unity, 0.9663 while its root mean square error (RMSE was the closest to zero, 0.001534.

  13. Analysis of aromatic amines in water samples by liquid-liquid-liquid microextraction with hollow fibers and high-performance liquid chromatography.

    Science.gov (United States)

    Zhao, Limian; Zhu, Lingyan; Lee, Hian Kee

    2002-07-19

    Liquid-liquid-liquid microextraction (LLLME) with hollow fibers in high-performance liquid chromatography (HPLC) has been applied as a rapid and sensitive quantitative method for the detection of four aromatic amines (3-nitroaniline, 4-chloroaniline, 4-bromoaniline and 3,4-dichloroaniline) in environmental water samples. The preconcentration procedure was induced by the pH difference inside and outside the hollow fiber. The target compounds were extracted from 4-ml aqueous sample (donor solution, pH approximately 13) through a microfilm of organic solvent (di-n-hexyl ether), immobilized in the pores of a hollow fiber (1.5 cm length x 0.6 mm I.D.), and finally into 4 microl of acid acceptor solution inside the fiber. After a prescribed period of time, the acceptor solution inside the fiber was withdrawn into the microsyringe and directly injected into the HPLC system for analysis. Factors relevant to the extraction procedure were studied. Up to 500-fold enrichment of analytes could be obtained under the optimized conditions (donor solution: 0.1 M sodium hydroxide solution with 20% sodium chloride and 2% acetone; organic phase: di-n-hexyl ether; acceptor solution: 0.5 M hydrochloric acid and 500 mM 18-crown-6 ether; extraction time of 30 min; stirring at 1,000 rev./min). The procedure also served as a sample clean-up step. The influence of humic acid on the extraction efficiency was also investigated, and more than 85% relative recoveries of the analytes at two different concentrations (20 and 100 microg/l) were achieved at various concentration of humic acid. This technique is a low cost, simple and fast approach to the analysis of polar compounds in aqueous samples.

  14. The removal of dinitrochlorobenzene from industrial residuals by liquid-liquid extraction with chemical reaction

    Directory of Open Access Journals (Sweden)

    G. C. M. Ferreira

    2007-09-01

    Full Text Available Nitrochlorobenzenes (NCBs are very important in the chemical industry since they have been used as raw material for the manufacture of crop protection products, as active ingredients in the pharmaceutical industry, as pigments and as antioxidants as well as for other uses. In industrial processes, NCBs are produced by monochlorobenzene (MCB nitration reactions and one of the main residuals formed is dinitrochlorobenzene (DNCB, which is mainly composed of the isomer 2,4DNCB. This subproduct, although of commercial interest when in its pure state, is generally incinerated due to the high costs of recovery treatment and purification. The objective of this study is to present an alternative to the treatment of industrial residuals containing DNCB. The technique consists of converting DNCB into sodium dinitrophenolate, which is very soluble in water and is also easy to reuse. For this purpose, liquid-liquid extraction with chemical reaction (alkaline hydrolysis with a rotating disc contactor (RDC is used. Experimental data on MCB nitration reactions as well as alkaline hydrolysis using a rotating disc contactor are presented.

  15. Molecular Dynamics Simulations on the solvation and interfacial behaviour of hydrophobic species. Applications to the TATB hypothesis and to the liquid/liquid extraction of cations to supercritical CO2

    International Nuclear Information System (INIS)

    Schurhammer, R.

    2001-12-01

    We report molecular dynamics studies on the solvation of charged hydrophobic molecules in pure liquids and at liquid / liquid interfaces. The first part of the thesis deals with the TATB hypothesis according to which the Asφ 4 + (TA + ) and Bφ 4 - (TB - ) ions have the same free energy of solvation in any solvent. The two ions are found to be solvated differently in pure liquids (water, chloroform, acetonitrile) as at a chloroform / water interface. These results are confirmed by free energy calculations and by simulations on iso-volume spherical S + and S - ions, which perfectly meet the TATB criteria. The many methodological tests performed show the importance of (i) the corrected treatment of 'long range interactions' (ii) the precise repartition of atomic charges (iii) the solvent models, especially for water, on the + / - charge discrimination by solvent. In the second part, in relation to the liquid / liquid extraction of cations from water to supercritical CO 2 , we report the behaviour of ions (Cs + , UO 2 2+ , Eu 3+ ), of un-complexed extractants molecules (tri-n-butylphosphate, calixarene), of their complexes with the cations and nitric acid at a preformed chloroform / water interface and during de-mixing simulations which started from a perfectly mixed CO 2 / water solutions. These studies demonstrate the importance of interfacial phenomena, of simulation conditions and acid and extractant concentrations, in assisted ion extraction to supercritical CO 2 . (author)

  16. Continuous process for selective metal extraction with an ionic liquid

    NARCIS (Netherlands)

    Parmentier, D.; Paradis, S.; Metz, S.J.; Wiedmer, S.K.; Kroon, M.C.

    2016-01-01

    This work describes for the first time a continuous process for selective metal extraction with an ionic liquid (IL) at room temperature. The hydrophobic fatty acid based IL tetraoctylphosphonium oleate ([P8888][oleate]) was specifically chosen for its low viscosity and high selectivity towards

  17. Selective extraction and recovery of rare earth metals from phosphor powders in waste fluorescent lamps using an ionic liquid system

    International Nuclear Information System (INIS)

    Yang, Fan; Kubota, Fukiko; Baba, Yuzo; Kamiya, Noriho; Goto, Masahiro

    2013-01-01

    Highlights: • Recycling of rare earth metals from fluorescent lamps was conducted by ionic liquid-mediated extraction. • Acid leaching from a waste phosphor powder was carried out using sulfuric and nitric acids. • An ionic liquid was used as extracting solvent for the rare earth metals. • Selective extraction of rare earth metals from leach solutions was attained. •The extracting ionic liquid phase was recyclable in the recovery process. -- Abstract: The recycling of rare earth metals from phosphor powders in waste fluorescent lamps by solvent extraction using ionic liquids was studied. Acid leaching of rare earth metals from the waste phosphor powder was examined first. Yttrium (Y) and europium (Eu) dissolved readily in the acid solution; however, the leaching of other rare earth metals required substantial energy input. Ionization of target rare earth metals from the waste phosphor powders into the leach solution was critical for their successful recovery. As a high temperature was required for the complete leaching of all rare earth metals, ionic liquids, for which vapor pressure is negligible, were used as an alternative extracting phase to the conventional organic diluent. An extractant, N, N-dioctyldiglycol amic acid (DODGAA), which was recently developed, showed a high affinity for rare earth metal ions in liquid–liquid extraction although a conventional commercial phosphonic extractant did not. An effective recovery of the rare earth metals, Y, Eu, La and Ce, from the metal impurities, Fe, Al and Zn, was achieved from the acidic leach solution of phosphor powders using an ionic liquid containing DODGAA as novel extractant system

  18. Selective extraction and recovery of rare earth metals from phosphor powders in waste fluorescent lamps using an ionic liquid system

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Fan; Kubota, Fukiko; Baba, Yuzo [Department of Applied Chemistry, Graduate School of Engineering, Kyushu University, 744 Motooka, Fukuoka 819-0395 (Japan); Kamiya, Noriho [Department of Applied Chemistry, Graduate School of Engineering, Kyushu University, 744 Motooka, Fukuoka 819-0395 (Japan); Center for Future Chemistry, Kyushu University, 744 Motooka, Fukuoka 819-0395 (Japan); Goto, Masahiro, E-mail: m-goto@mail.cstm.kyushu-u.ac.jp [Department of Applied Chemistry, Graduate School of Engineering, Kyushu University, 744 Motooka, Fukuoka 819-0395 (Japan); Center for Future Chemistry, Kyushu University, 744 Motooka, Fukuoka 819-0395 (Japan)

    2013-06-15

    Highlights: • Recycling of rare earth metals from fluorescent lamps was conducted by ionic liquid-mediated extraction. • Acid leaching from a waste phosphor powder was carried out using sulfuric and nitric acids. • An ionic liquid was used as extracting solvent for the rare earth metals. • Selective extraction of rare earth metals from leach solutions was attained. •The extracting ionic liquid phase was recyclable in the recovery process. -- Abstract: The recycling of rare earth metals from phosphor powders in waste fluorescent lamps by solvent extraction using ionic liquids was studied. Acid leaching of rare earth metals from the waste phosphor powder was examined first. Yttrium (Y) and europium (Eu) dissolved readily in the acid solution; however, the leaching of other rare earth metals required substantial energy input. Ionization of target rare earth metals from the waste phosphor powders into the leach solution was critical for their successful recovery. As a high temperature was required for the complete leaching of all rare earth metals, ionic liquids, for which vapor pressure is negligible, were used as an alternative extracting phase to the conventional organic diluent. An extractant, N, N-dioctyldiglycol amic acid (DODGAA), which was recently developed, showed a high affinity for rare earth metal ions in liquid–liquid extraction although a conventional commercial phosphonic extractant did not. An effective recovery of the rare earth metals, Y, Eu, La and Ce, from the metal impurities, Fe, Al and Zn, was achieved from the acidic leach solution of phosphor powders using an ionic liquid containing DODGAA as novel extractant system.

  19. Salting-Out Assisted Liquid-Liquid Extraction for Quantification of Febuxostat in Plasma Using RP-HPLC and Its Pharmacokinetic Application.

    Science.gov (United States)

    Tandel, Devang; Shah, Purvi; Patel, Kalpana; Thakkar, Vaishali; Patel, Kirti; Gandhi, Tejal

    2016-11-01

    A rapid and sensitive reversed-phase high-performance liquid chromatography (HPLC) method using novel salting-out assisted liquid-liquid extraction technique has been developed for the quantitative determination of febuxostat (FEB), used for the treatment of gout, in rat plasma. The method was validated according to US FDA guideline. Separation was achieved using a Phenomenex Luna-C 18 (250 × 4.60 mm, 5 µm) column and mobile phase composed of potassium dihydrogen orthophosphate buffer 25 mM, adjusted to pH 6.8 with triethylamine:methanol in a ratio of 35:65 (v/v) showing retention time 5.56 and 8.86 min for FEB and internal standard, respectively. The optimal salting-out parameters; 1 mL of acetonitrile and 200 µL of 2 M ammonium acetate salt showed extraction recovery >90% for FEB from plasma. This extraction procedure afforded clear samples resulting in convenient and cost-saving procedure and showed good linear relationship (r > 0.9997) between peak area ratio and concentration from 0.3 to 20 µg/mL. The results of pharmacokinetic study showed that absorption profile of spherical agglomerate of FEB compared to marketed formulation was higher indicating greater systemic absorption. In conclusion, the developed SALLE-HPLC method with simple ultraviolet detection offered a number of advantages including good quantitative ability, wide linear range, high recovery, short analysis time as well as low cost. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  20. Determination of three estrogens and bisphenol A by functional ionic liquid dispersive liquid-phase microextraction coupled with ultra-high performance liquid chromatography and ultraviolet detection.

    Science.gov (United States)

    Jiang, Yuehuang; Tang, Tingting; Cao, Zhen; Shi, Guoyue; Zhou, Tianshu

    2015-06-01

    A hydroxyl-functionalized ionic liquid, 1-hydroxyethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide, was employed in an improved dispersive liquid-phase microextraction method coupled with ultra high performance liquid chromatography for the enrichment and determination of three estrogens and bisphenol A in environmental water samples. The introduced hydroxyl group acted as the H-bond acceptor that dispersed the ionic liquid effectively in the aqueous phase without dispersive solvent or external force. Fourier transform infrared spectroscopy indicated that the hydroxyl group of the cation of the ionic liquid enhanced the combination of extractant and analytes through the formation of hydrogen bonds. The improvement of the extraction efficiency compared with that with the use of alkyl ionic liquid was proved by a comparison study. The main parameters including volume of extractant, temperature, pH, and extraction time were investigated. The calibration curves were linear in the range of 5.0-1000 μg/L for estrone, estradiol, and bisphenol A, and 10.0-1000 μg/L for estriol. The detection limits were in the range of 1.7-3.4 μg/L. The extraction efficiency was evaluated by enrichment factor that were between 85 and 129. The proposed method was proved to be simple, low cost, and environmentally friendly for the determination of the four endocrine disruptors in environmental water samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Possible applications of crown-ethers to metal extraction using liquid membrane technology - a literature survey

    International Nuclear Information System (INIS)

    Dozol, M.

    1990-01-01

    Ether-crowns, discovered in 1967 by J.C. PEDERSEN, exhibit attractive complexive and extractive properties, enhanced in various fields, such as analytical chemistry, chemical synthesis, field of biology, or extractive chemistry. The investigations carried out on these macrocyclic compounds are continually increasing, as show in international literature. Among the focus of interest, the applications to metal extraction are extensively studied with crown compounds present in liquid phase or impregnated on supports (membranes or resins). The goal of this paper is to describe the application of crown-ethers to metal extraction, using liquid membrane processes. 69 refs

  2. Extraction of zirconium from simulated acidic nitrate waste using liquid membrane in hollow fiber contactor

    International Nuclear Information System (INIS)

    Pandey, G.; Chinchale, R.; Renjith, A.U.; Dixit, S.; Mukhopadhyay, S.; Shenoy, K.T.; Ghosh, S.K.

    2015-01-01

    The acidic waste raffinate stream of zirconium (Zr) purification plant contains about 2 gpl of Zr in about 2M free nitric acid. TBP, which is the most commonly used solvent in the nuclear industry, is not suitable for the extraction of Zr from this lean solution as its distribution coefficient is less than one. In house synthesized Mixed Alkyl Phosphine Oxide (MAPO) is a potential extractant for Zr from this lean stream. Intensification of this process for recovery of Zr has been attempted through use of efficient contactor, namely, hollow fiber module and efficient process, namely, simultaneous extraction and stripping across liquid membrane containing MAPO. Based on batch equilibrium studies selection of suitable concentration of extractant, composition of diluent, selection and concentration of strippant for the proposed liquid membrane system was made. The selected organic and strippant concentration was used to study suitability of application of Dispersion Liquid Membrane (DLM) in hollow fiber contactor for recovery Zr from solution simulated to Zr plant raffinate. Challenges related to stable operation of the liquid membrane system like stability of the organic phase in the micropores of lumen and stability of the dispersion during the pertraction were addressed through pressure balance across the lumen and choice of adequate dispersion condition respectively. (author)

  3. Determination of organophosphorus pesticides by dispersive liquid-liquid micro extraction coupled with gas chromatography-electron capture detection

    International Nuclear Information System (INIS)

    Mohd Marsin Sanagi; Siti Umairah Mokhtar; Mazidatul Akmam Miskam; Wan Aini Wan Ibrahim

    2011-01-01

    A simple, rapid and sensitive method termed as dispersive liquid-liquid micro extraction (DLLME) combined with gas chromatography-electron capture detector (GC-ECD) was developed for the determination of selected organophosphorus pesticides (OPPs) namely chloropyrifos, dimethoate and diazinon in water sample. In this method, a mixture of carbon disulfide, CS 2 (extraction solvent) and methanol (disperser solvent) was rapidly injected using syringe into the 5.00 mL water sample to form a cloudy solution where the OPPs were extracted into the fine droplets of extraction solvent. Upon centrifugation for 3 min at 3500 rpm, the fine droplets were sedimented at the bottom of the centrifuge tube. Sedimented phase (1 μL) was injected into the GC-ECD for separation and determination of OPPs. Important extraction parameters, such as type of disperser solvent, volume of extraction solvent and volume of disperser solvent were investigated. The optimized conditions for DLLME of the selected OPPs were methanol as disperser solvent, 30 μL of extraction solvent (CS 2 ) and 1.0 mL of disperser solvent (methanol). Under the optimum extraction conditions, the method showed good linearity in the range of 0.1 to 1.0 μg/ mL with correlation coefficient (r 2 ), in the range of 0.9976 to 0.9994 and low limits of detection (LOD) between 0.047 and 0.201 μg/ mL. The proposed method provided acceptable recoveries (72.67- 144 %) with good RSDs ranging from 2.74 % to 7.48 %. This method was successfully applied to the determination of OPPs in water samples obtained from a golf course and chloropyrifos and diazinon were detected at concentration 0.18 μg/ mL and 0.07 μg/ mL, respectively. (author)

  4. Application of an efficient strategy based on liquid-liquid extraction, high-speed counter-current chromatography, and preparative HPLC for the rapid enrichment, separation, and purification of four anthraquinones from Rheum tanguticum.

    Science.gov (United States)

    Chen, Tao; Liu, Yongling; Zou, Denglang; Chen, Chen; You, Jinmao; Zhou, Guoying; Sun, Jing; Li, Yulin

    2014-01-01

    This study presents an efficient strategy based on liquid-liquid extraction, high-speed counter-current chromatography, and preparative HPLC for the rapid enrichment, separation, and purification of four anthraquinones from Rheum tanguticum. A new solvent system composed of petroleum ether/ethyl acetate/water (4:2:1, v/v/v) was developed for the liquid-liquid extraction of the crude extract from R. tanguticum. As a result, emodin, aloe-emodin, physcion, and chrysophanol were greatly enriched in the organic layer. In addition, an efficient method was successfully established to separate and purify the above anthraquinones by high-speed counter-current chromatography and preparative HPLC. This study supplies a new alternative method for the rapid enrichment, separation, and purification of emodin, aloe-emodin, physcione, and chrysophanol. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Vortex-assisted liquid-liquid microextraction for the rapid screening of short-chain chlorinated paraffins in water.

    Science.gov (United States)

    Chang, Chia-Yu; Chung, Wu-Hsun; Ding, Wang-Hsien

    2016-01-01

    The rapid screening of trace levels of short-chain chlorinated paraffins in various aqueous samples was performed by a simple and reliable procedure based on vortex-assisted liquid-liquid microextraction combined with gas chromatography and electron capture negative ionization mass spectrometry. The optimal vortex-assisted liquid-liquid microextraction conditions for 20 mL water sample were as follows: extractant 400 μL of dichloromethane; vortex extraction time of 1 min at 2500 × g; centrifugation of 3 min at 5000 × g; and no ionic strength adjustment. Under the optimum conditions, the limit of quantitation was 0.05 μg/L. Precision, as indicated by relative standard deviations, was less than 9% for both intra- and inter-day analysis. Accuracy, expressed as the mean extraction recovery, was above 91%. The vortex-assisted liquid-liquid microextraction with gas chromatography and electron capture negative ionization mass spectrometry method was successfully applied to quantitatively extract short-chain chlorinated paraffins from samples of river water and the effluent of a wastewater treatment plant, and the concentrations ranged from 0.8 to 1.6 μg/L. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Entropy feature extraction on flow pattern of gas/liquid two-phase flow based on cross-section measurement

    International Nuclear Information System (INIS)

    Han, J; Dong, F; Xu, Y Y

    2009-01-01

    This paper introduces the fundamental of cross-section measurement system based on Electrical Resistance Tomography (ERT). The measured data of four flow regimes of the gas/liquid two-phase flow in horizontal pipe flow are obtained by an ERT system. For the measured data, five entropies are extracted to analyze the experimental data according to the different flow regimes, and the analysis method is examined and compared in three different perspectives. The results indicate that three different perspectives of entropy-based feature extraction are sensitive to the flow pattern transition in gas/liquid two-phase flow. By analyzing the results of three different perspectives with the changes of gas/liquid two-phase flow parameters, the dynamic structures of gas/liquid two-phase flow is obtained, and they also provide an efficient supplementary to reveal the flow pattern transition mechanism of gas/liquid two-phase flow. Comparison of the three different methods of feature extraction shows that the appropriate entropy should be used for the identification and prediction of flow regimes.

  7. Maghemite nanoparticle-decorated hollow fiber electromembrane extraction combined with dispersive liquid-liquid microextraction for the determination of thymol from Carum copticum

    DEFF Research Database (Denmark)

    Khajeh, Mostafa; Pedersen-Bjergaard, Stig; Bohlooli, Mousa

    2017-01-01

    BACKGROUND A novel technique using maghemite nanoparticle-decorated hollow fibers to assist electromembrane extraction is proposed. Electromembrane extraction combined with dispersive liquid–liquid microextraction (EME-DLLME) was applied for the extraction of thymol from Carum copticum, followed...... by gas chromatography with flame ionization detection (GC-FID). RESULTS The use of maghemite nanoparticle-decorated hollow fibers was found to improve the extraction efficiency of thymol significantly. Important operational parameters, including pH of acceptor phase, extraction time, voltage...

  8. Preconcentration and determination of ceftazidime in real samples using dispersive liquid-liquid microextraction and high-performance liquid chromatography with the aid of experimental design.

    Science.gov (United States)

    Razmi, Rasoul; Shahpari, Behrouz; Pourbasheer, Eslam; Boustanifar, Mohammad Hasan; Azari, Zhila; Ebadi, Amin

    2016-11-01

    A rapid and simple method for the extraction and preconcentration of ceftazidime in aqueous samples has been developed using dispersive liquid-liquid microextraction followed by high-performance liquid chromatography analysis. The extraction parameters, such as the volume of extraction solvent and disperser solvent, salt effect, sample volume, centrifuge rate, centrifuge time, extraction time, and temperature in the dispersive liquid-liquid microextraction process, were studied and optimized with the experimental design methods. Firstly, for the preliminary screening of the parameters the taguchi design was used and then, the fractional factorial design was used for significant factors optimization. At the optimum conditions, the calibration curves for ceftazidime indicated good linearity over the range of 0.001-10 μg/mL with correlation coefficients higher than the 0.98, and the limits of detection were 0.13 and 0.17 ng/mL, for water and urine samples, respectively. The proposed method successfully employed to determine ceftazidime in water and urine samples and good agreement between the experimental data and predictive values has been achieved. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Stable isotope dilution quantification of mutagens in cooked foods by combined liquid chromatography-thermospray mass spectrometry

    International Nuclear Information System (INIS)

    Yamaizumi, Ziro; Kasai, Hiroshi; Nishimura, Susumu; Edmonds, C.G.; McCloskey, J.A.

    1986-01-01

    A method of general applicability for the detection and quantification of mutagens in cooked foods at the ppb level is presented. A minimal sample prefractionation is employed and [Me- 2 H 3 ]-labeled analogs of the compounds of interest are added for identification and quantification of mutagens by accurate measurement of chromatographic retention (K') in reverse-phase high-performance liquid chromatography (HPLC), and by measurement of the ratio of response of the protonated molecular ions of analyte and internal standard by directly coupled liquid chromatography-mass spectrometry (LC/MS). Initial application is demonstrated in the analysis of 2-amino-3-methylimidazo[4,5-f]quinoline (IQ) and 2-amino-3,4-dimethylimidazo[4,5-f]quinoline (MelQ) in broiled salmon. (Auth.)

  10. Ion-pair vortex assisted liquid-liquid microextraction with back extraction coupled with high performance liquid chromatography-UV for the determination of metformin in plasma.

    Science.gov (United States)

    Alshishani, Anas; Makahleh, Ahmad; Yap, Hui Fang; Gubartallah, Elbaleeq Adam; Salhimi, Salizawati Muhamad; Saad, Bahruddin

    2016-12-01

    A new sample preparation method, ion-pair vortex assisted liquid-liquid microextraction (VALLME-BE), for the determination of a highly polar anti-diabetic drug (metformin) in plasma sample was developed. The VALLME-BE was performed by diluting the plasma in borate buffer and extracted to 150µL 1-octanol containing 0.2M di-(2-ethylhexyl)phosphoric acid as intermediate phase. The drug was next back-extracted into 20µL of 0.075M HCl solution. The effects of pH, ion-pair concentration, type of organic solvent, volume of extraction phases, ionic strength, vortexing and centrifugation times on the extraction efficiency were investigated. The optimum conditions were at pH 9.3, 60s vortexing and 2min centrifugation. The microextract, contained metformin and buformin (internal standard), was directly injected into a HPLC unit using C1 column (250mm×4.6mm×10µm) and detected at 235nm. The method was validated and calibration curve was linear with r 2 >0.99 over the range of 20-2000µgL -1 . The limits of detection and quantitation were 1.4 and 4.1µgL -1 , respectively. The accuracy was within 94.8-108% of the nominal concentration. The relative standard deviation for inter- and intra-day precision was less than 10.8%. The method was conveniently applied for the determination of metformin in plasma samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Determination of caffeoylquinic acids in feed and related products by focused ultrasound solid-liquid extraction and ultra-high performance liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Tena, M T; Martínez-Moral, M P; Cardozo, P W

    2015-06-26

    A method to determine caffeoylquinic acids (CQAs) in three sources (herbal extract, feed additive and finished feed) using for the first time focused ultrasound solid-liquid extraction (FUSLE) followed by ultra-high performance liquid chromatography (UPLC) coupled to quadrupole-time of flight mass spectrometry is presented. Pressurized liquid extraction (PLE) was also tested as extraction technique but it was discarded because cynarin was not stable under temperature values used in PLE. The separation of the CQAs isomers was carried out in only seven minutes. FUSLE variables such as extraction solvent, power and time were optimized by a central composite design. Under optimal conditions, FUSLE extraction was performed with 8mL of an 83:17 methanol-water mixture for 30s at a power of 60%. Only two extraction steps were found necessary to recover analytes quantitatively. Sensitivity, linearity, accuracy and precision were established. Matrix effect was studied for each type of sample. It was not detected for mono-CQAs, whereas the cynarin signal was strongly decreased due to ionization suppression in presence of matrix components; so the quantification by standard addition was mandatory for the determination of di-caffeoylquinic acids. Finally, the method was applied to the analysis of herbal extracts, feed additives and finished feed. In all samples, chlorogenic acid was the predominant CQA, followed by criptochlorogenic acid, neochlorogenic acid and cynarin. The method allows an efficient determination of chlorogenic acid with good recovery rates. Therefore, it may be used for screening of raw material and for process and quality control in feed manufacture. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Analysis of chlorpheniramine in human urine samples using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Mehdi Maham

    2014-09-01

    Full Text Available A simple and environmentally friendly microextraction technique was used for determination of chlorpheniramine (CPM, an antihistamine drug, in human urine samples using dispersive liquid-liquid microextraction (DLLME followed by high performance liquid chromatography with diode array detection (HPLC-DAD. In this extraction technique, an appropriate mixture of acetonitrile (disperser solvent and carbon tetrachloride (extraction solvent was rapidly injected into the urine sample containing the target analyte. Tiny droplets of extractant were formed and dispersed into the sample solution and then sedimented at the bottom of the conical test tube by centrifugation. Under optimal conditions, the calibration curve was linear in the range of 0.055-5.5 µg mL-1, with a detection limit of 16.5 ng mL-1. This proposed method was successfully applied to the analysis of real urine samples. Low consumption of toxic organic solvents, simplicity of operation, low cost and acceptable figures of merit are the main advantages of the proposed technique.

  13. Magnetic silica nanomaterials for solid-phase extraction combined with dispersive liquid-liquid microextraction of ultra-trace quantities of plasticizers

    International Nuclear Information System (INIS)

    Yamini, Yadollah; Faraji, Mohammad; Adeli, Mahnaz

    2015-01-01

    We are presenting surface modified magnetic silica nanoparticles (m-Si-NPs) for use in solid-phase extraction combined with dispersive liquid-liquid microextraction (DLLME). The m-Si-NPs were surface-functionalized with octadecyl groups to give a material for the extraction of the plasticizers dibutyl phthalate, di(2-ethylhexyl) adipate and di(2-ethylhexyl) phthalate from water samples. The functionalized m-Si-NPs were characterized by scanning electron microscopy, FTIR spectroscopy, thermal gravimetric analysis, and vibrating sample magnetometry. The results showed that the m-Si-NPs were well functionalized with octadecyl groups. The effects of various experimental variables on the extraction efficiencies were investigated. The analytes were quantified by GC/FID. Under optimal conditions, the calibration plots are linear in the range from 0.01 to 100 μg∙L -1 , and very high enrichment factors (mean value ∼20,000) were obtained. As a result of the high enrichment factors, the detection limits are as low as 2–3 ng∙L -1 . The method was successfully employed to the extraction of the plasticizers from (spiked) water samples, and recoveries are in the order of 93.9 to 106.7 %. The method is low cost, fast, and very sensitive (author)

  14. Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction of herbicides in peanuts.

    Science.gov (United States)

    Li, Na; Wang, Zhibing; Zhang, Liyuan; Nian, Li; Lei, Lei; Yang, Xiao; Zhang, Hanqi; Yu, Aimin

    2014-10-01

    Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction was developed and applied to the extraction of pesticides in high fatty matrices. The herbicides were ultrasonically extracted from peanut using ethyl acetate as extraction solvent. The separation of the analytes from a large amount of co-extractive fat was achieved by dispersive solid-phase extraction using MIL-101(Cr) as sorbent. In this step, the analytes were adsorbed on MIL-101(Cr) and the fat remained in bulk. The herbicides were separated and determined by high-performance liquid chromatography. The experimental parameters, including type and volume of extraction solvent, ultrasonication time, volume of hexane and eluting solvent, amount of MIL-101(Cr) and dispersive solid phase extraction time, were optimized. The limits of detection for herbicides range from 0.98 to 1.9 μg/kg. The recoveries of the herbicides are in the range of 89.5-102.7% and relative standard deviations are equal or lower than 7.0%. The proposed method is simple, effective and suitable for treatment of the samples containing high content of fat. Copyright © 2014 Elsevier B.V. All rights reserved.

  15. Progress in liquid ion exchangers

    International Nuclear Information System (INIS)

    Nakagawa, Genkichi

    1974-01-01

    Review is made on the extraction with anion exchangers and the extraction with liquid cation exchangers. On the former, explanation is made on the extraction of acids, the relation between anion exchange and the extraction of metals, the composition of the metallic complexes that are extracted, and the application of the extraction with anion exchangers to analytical chemistry. On the latter, explanation is made on the extraction of metals and its application to analytical chemistry. The extraction with liquid ion exchangers is suitable for the operation in chromatography, because the distribution of extracting agents into aqueous phase is small, and extraction equilibrium is quickly reached, usually within 1 to several minutes. The separation by means of anion exchangers is usually made from hydrochloric acid solution. For example, Brinkman et al. determined Rf values for more than 50 elements by thin layer chromatography. Tables are given for showing the structure of the liquid ion exchangers and the polymerized state of various amines. (Mori, K.)

  16. Rapid pretreatment and determination of bisphenol A in water samples based on vortex-assisted liquid-liquid microextraction followed by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Yang, Xiao; Diao, Chun-Peng; Sun, Ai-Ling; Liu, Ren-Min

    2014-10-01

    A method for the rapid pretreatment and determination of bisphenol A in water samples based on vortex-assisted liquid-liquid microextraction followed by high-performance liquid chromatography with fluorescence detection was proposed in this paper. A simple apparatus consisting of a test tube and a cut-glass dropper was designed and applied to collect the floating extraction drop in liquid-liquid microextraction when low-density organic solvent was used as the extraction solvent. Solidification and melting steps that were tedious but necessary once the low-density organic solvent used as extraction solvent could be avoided by using this apparatus. Bisphenol A was selected as model pollutant and vortex-assisted liquid-liquid microextraction was employed to investigate the usefulness of the apparatus. High-performance liquid chromatography with fluorescence detection was selected as the analytical tool for the detection of bisphenol A. The linear dynamic range was from 0.10 to 100 μg/L for bisphenol A, with good squared regression coefficient (r(2) = 0.9990). The relative standard deviation (n = 7) was 4.7% and the limit of detection was 0.02 μg/L. The proposed method had been applied to the determination of bisphenol A in natural water samples and was shown to be economical, fast, and convenient. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Separation of aromatic precipitates from simulated high level radioactive waste by hydrolysis, evaporation and liquid-liquid extraction

    International Nuclear Information System (INIS)

    Young, S.R.; Shah, H.B.; Carter, J.T.

    1991-01-01

    The Defense Waste Processing Facility (DWPF) at the SRS will be the United States' first facility to process High Level radioactive Waste (HLW) into a borosilicate glass matrix. The removal of aromatic precipitates by hydrolysis, evaporation and liquid-liquid extraction will be a key step in the processing of the HLW. This step, titled the Precipitate Hydrolysis Process, has been demonstrated by the Savannah River Laboratory with the Precipitate Hydrolysis Experimental Facility (PHEF). The mission of the PHEF is to demonstrate processing of simulated high level radioactive waste which contains tetraphenylborate precipitates and nitrite. Reduction of nitrite by hydroxylamine nitrate and hydrolysis of the tetraphenylborate by formic acid is discussed. Gaseous production, which is primarily benzene, nitrous oxide and carbon dioxide, has been quantified. Production of high-boiling organic compounds and the accumulation of these organic compounds within the process are addressed

  18. Air-assisted liquid-liquid microextraction using floating organic droplet solidification for simultaneous extraction and spectrophotometric determination of some drugs in biological samples through chemometrics methods

    Science.gov (United States)

    Farahmand, Farnaz; Ghasemzadeh, Bahar; Naseri, Abdolhossein

    2018-01-01

    An air assisted liquid-liquid microextraction by applying the solidification of a floating organic droplet method (AALLME-SFOD) coupled with a multivariate calibration method, namely partial least squares (PLS), was introduced for the fast and easy determination of Atenolol (ATE), Propanolol (PRO) and Carvedilol (CAR) in biological samples via a spectrophotometric approach. The analytes would be extracted from neutral aqueous solution into 1-dodecanol as an organic solvent, using AALLME. In this approach a low-density solvent with a melting point close to room temperature was applied as the extraction solvent. The emulsion was immediately formed by repeatedly pulling in and pushing out the aqueous sample solution and extraction solvent mixture via a 10-mL glass syringe for ten times. After centrifugation, the extractant droplet could be simply collected from the aqueous samples by solidifying the emulsion at a lower than the melting point temperature. In the next step, analytes were back extracted simultaneously into the acidic aqueous solution. Derringer and Suich multi-response optimization were utilized for simultaneous optimizing the parameters of three analytes. This method incorporates the benefits of AALLME and dispersive liquid-liquid microextraction considering the solidification of floating organic droplets (DLLME-SFOD). Calibration graphs under optimized conditions were linear in the range of 0.30-6.00, 0.32-2.00 and 0.30-1.40 μg mL- 1 for ATE, CAR and PRO, respectively. Other analytical parameters were obtained as follows: enrichment factors (EFs) were found to be 11.24, 16.55 and 14.90, and limits of detection (LODs) were determined to be 0.09, 0.10 and 0.08 μg mL- 1 for ATE, CAR and PRO, respectively. The proposed method will require neither a highly toxic chlorinated solvent for extraction nor an organic dispersive solvent in the application process; hence, it is more environmentally friendly.

  19. Separation of uranium(VI) by liquid-solid extraction with tri-n-octylphosphine oxide diluted with naphthalene

    International Nuclear Information System (INIS)

    Shigetomi, Y.; Kojima, T.; Kamba, H.; Yamamoto, Y.

    1980-01-01

    Liquid-liquid distribution with tri-n-octylphosphine oxide (TOPO) and molten naphthalene has been investigated for the extraction of 20 metals from nitric acid and hydrochloric acid solutions. Uranium is quantitatively extracted from 1 M nitric acid or hydrochloric acid by using 100 mg of TOPO and 200 mg of naphthalene and shaking for 5 min at 80 0 C, and separated from transition metals, alkaline earth metals and rare earth metals (except scandium). Addition of naphthalene increases the extraction efficiency. (Auth.)

  20. Molecular Dynamics Simulations on the solvation and interfacial behaviour of hydrophobic species. Applications to the TATB hypothesis and to the liquid/liquid extraction of cations to supercritical CO{sub 2}; Simulations par dynamique moleculaire de la solvatation et du comportement interfacial d'especes hydrophobes: application a l'hypothese TATB et a l'extraction liquide/liquide de cations par le CO{sub 2} supercritique

    Energy Technology Data Exchange (ETDEWEB)

    Schurhammer, R

    2001-12-15

    We report molecular dynamics studies on the solvation of charged hydrophobic molecules in pure liquids and at liquid / liquid interfaces. The first part of the thesis deals with the TATB hypothesis according to which the As{phi}{sub 4}{sup +} (TA{sup +}) and B{phi}{sub 4}{sup -} (TB{sup -}) ions have the same free energy of solvation in any solvent. The two ions are found to be solvated differently in pure liquids (water, chloroform, acetonitrile) as at a chloroform / water interface. These results are confirmed by free energy calculations and by simulations on iso-volume spherical S{sup +} and S{sup -} ions, which perfectly meet the TATB criteria. The many methodological tests performed show the importance of (i) the corrected treatment of 'long range interactions' (ii) the precise repartition of atomic charges (iii) the solvent models, especially for water, on the + / - charge discrimination by solvent. In the second part, in relation to the liquid / liquid extraction of cations from water to supercritical CO{sub 2}, we report the behaviour of ions (Cs{sup +}, UO{sub 2}{sup 2+}, Eu{sup 3+}), of un-complexed extractants molecules (tri-n-butylphosphate, calixarene), of their complexes with the cations and nitric acid at a preformed chloroform / water interface and during de-mixing simulations which started from a perfectly mixed CO{sub 2} / water solutions. These studies demonstrate the importance of interfacial phenomena, of simulation conditions and acid and extractant concentrations, in assisted ion extraction to supercritical CO{sub 2}. (author)

  1. Determination of Np, Pu and Am in high level radioactive waste with extraction-liquid scintillation counting

    International Nuclear Information System (INIS)

    Yang Dazhu; Zhu Yongjun; Jiao Rongzhou

    1994-01-01

    A new method for the determination of transuranium elements, Np, Pu and Am with extraction-liquid scintillation counting has been studied systematically. Procedures for the separation of Pu and Am by HDEHP-TRPO extraction and for the separation of Np by TTA-TiOA extraction have been developed, by which the recovery of Np, Pu and Am is 97%, 99% and 99%, respectively, and the decontamination factors for the major fission products ( 90 Sr, 137 Cs etc.) are 10 4 -10 6 . Pulse shape discrimination (PSD) technique has been introduced to liquid scintillation counting, by which the counting efficiency of α-activity is >99% and the rejection of β-counts is >99.95%. This new method, combining extraction and pulse shape discrimination with liquid scintillation technique, has been successfully applied to the assay of Np, Pu and Am in high level radioactive waste. (author) 7 refs.; 7 figs.; 4 tabs

  2. Cortisol production rates measured by liquid chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Esteban, N.V.; Yergey, A.L.

    1990-01-01

    Cortisol production rates (FPRs) in physiologic and pathologic states in humans have been investigated over the past 30 years. However, there has been conflicting evidence concerning the validity of the currently accepted value of FPRs in humans (12 to 15 mg/m2/d) as determined by radiotracer methodology. The present study reviews previous methods proposed for the measurement of FPRs in humans and discusses the applications of the first method for the direct determination of 24-hour plasma FPRs during continuous administration of a stable isotope, using a thermospray high-pressure liquid chromatography-mass spectrometry technique. The technique is fast, sensitive, and, unlike gas chromatography-mass spectrometry methods, does not require derivatization, allowing on-line detection and quantification of plasma cortisol after a simple extraction procedure. The results of determination of plasma FPRs by stable tracer/mass spectrometry are directly in units of mass/time and, unlike radiotracer methods, are independent of any determination of volume of distribution or cortisol concentration. Our methodology offers distinct advantages over radiotracer techniques in simplicity and reliability since only single measurements of isotope ratios are required. The technique was validated in adrenalectomized patients. Circadian variations in daily FRPs were observed in normal volunteers, and, to date, results suggest a lower FRP in normal children and adults than previously believed. 88 references

  3. Determination of pharmaceuticals in environmental and biological matrices using pressurised liquid extraction--are we developing sound extraction methods?

    DEFF Research Database (Denmark)

    Runnqvist, Hannah; Bak, Søren Alex; Hansen, Martin

    2010-01-01

    Pressurised liquid extraction (PLE) is now a well established and extensively applied extraction technique in environmental analysis for pollutants such as persistent organic pollutants (POPs). During the past decade, an emerging group of environmentally interesting analytes are pharmaceuticals...

  4. Ultrasound-Assisted Extraction of Carnosic Acid and Rosmarinic Acid Using Ionic Liquid Solution from Rosmarinus officinalis

    Directory of Open Access Journals (Sweden)

    Chunjian Zhao

    2012-09-01

    Full Text Available Ionic liquid based, ultrasound-assisted extraction was successfully applied to the extraction of phenolcarboxylic acids, carnosic acid and rosmarinic acid, from Rosmarinus officinalis. Eight ionic liquids, with different cations and anions, were investigated in this work and [C8mim]Br was selected as the optimal solvent. Ultrasound extraction parameters, including soaking time, solid–liquid ratio, ultrasound power and time, and the number of extraction cycles, were discussed by single factor experiments and the main influence factors were optimized by response surface methodology. The proposed approach was demonstrated as having higher efficiency, shorter extraction time and as a new alternative for the extraction of carnosic acid and rosmarinic acid from R. officinalis compared with traditional reference extraction methods. Ionic liquids are considered to be green solvents, in the ultrasound-assisted extraction of key chemicals from medicinal plants, and show great potential.

  5. Dispersive solid-phase extraction followed by vortex-assisted dispersive liquid-liquid microextraction based on the solidification of a floating organic droplet for the determination of benzoylurea insecticides in soil and sewage sludge.

    Science.gov (United States)

    Peng, Guilong; He, Qiang; Mmereki, Daniel; Lu, Ying; Zhong, Zhihui; Liu, Hanyang; Pan, Weiliang; Zhou, Guangming; Chen, Junhua

    2016-04-01

    A novel dispersive solid-phase extraction combined with vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet was developed for the determination of eight benzoylurea insecticides in soil and sewage sludge samples before high-performance liquid chromatography with ultraviolet detection. The analytes were first extracted from the soil and sludge samples into acetone under optimized pretreatment conditions. Clean-up of the extract was conducted by dispersive solid-phase extraction using activated carbon as the sorbent. The vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet procedure was performed by using 1-undecanol with lower density than water as the extraction solvent, and the acetone contained in the solution also acted as dispersive solvent. Under the optimum conditions, the linearity of the method was in the range 2-500 ng/g with correlation coefficients (r) of 0.9993-0.9999. The limits of detection were in the range of 0.08-0.56 ng/g. The relative standard deviations varied from 2.16 to 6.26% (n = 5). The enrichment factors ranged from 104 to 118. The extraction recoveries ranged from 81.05 to 97.82% for all of the analytes. The good performance has demonstrated that the proposed methodology has a strong potential for application in the multiresidue analysis of complex matrices. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Separation and Recycling for Rare Earth Elements by Homogeneous Liquid-Liquid Extraction (HoLLE Using a pH-Responsive Fluorine-Based Surfactant

    Directory of Open Access Journals (Sweden)

    Shotaro Saito

    2015-08-01

    Full Text Available A selective separation and recycling system for metal ions was developed by homogeneous liquid-liquid extraction (HoLLE using a fluorosurfactant. Sixty-two different elemental ions (e.g., Ag, Al, As, Au, B, Ba, Be, Bi, Ca, Cd, Ce, Co, Cr, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Hg, Ho, In, Ir, La, Lu, Mg, Mn, Mo, Nb, Nd, Ni, Os, P, Pb, Pd, Pr, Pt, Re, Rh, Ru, Sb, Sc, Se, Si, Sm, Sn, Sr, Ta, Tb, Te, Ti, Tl, Tm, V, W, Y, Yb, Zn, and Zr were examined. By changing pH from a neutral or alkaline solution (pH ≥ 6.5 to that of an acidic solution (pH < 4.0, gallium, zirconium, palladium, silver, platinum, and rare earth elements were extracted at >90% efficiency into a sedimented Zonyl FSA® (CF3(CF2n(CH22S(CH22COOH, n = 6–8 liquid phase. Moreover, all rare earth elements were obtained with superior extraction and stripping percentages. In the recycling of rare earth elements, the sedimented phase was maintained using a filter along with a mixed solution of THF and 1 M sodium hydroxide aqueous solution. The Zonyl FSA® was filtrated and the rare earth elements were recovered on the filter as a hydroxide. Furthermore, the filtrated Zonyl FSA was reusable by conditioning the subject pH.

  7. Development of an on-line mixed-mode gel liquid chromatography×reversed phase liquid chromatography method for separation of water extract from Flos Carthami.

    Science.gov (United States)

    Wang, Yu-Qing; Tang, Xu; Li, Jia-Fu; Wu, Yun-Long; Sun, Yu-Ying; Fang, Mei-Juan; Wu, Zhen; Wang, Xiu-Min; Qiu, Ying-Kun

    2017-10-13

    A novel on-line comprehensive two-dimensional liquid chromatography (2D-LC) method by coupling mixed-mode gel liquid chromatography (MMG-LC) with reversed phase liquid chromatography (RPLC) was developed. A mixture of 17 reference compounds was used to study the separation mechanism. A crude water extract of Flos Carthami was applied to evaluate the performance of the novel 2D-LC system. In the first dimension, the extract was eluted with a gradient of water/methanol over a cross-linked dextran gel Sephadex LH-20 column. Meanwhile, the advantages of size exclusion, reversed phase partition and adsorption separation mechanism were exploited before further on-line reversed phase purification on the second dimension. This novel on-line mixed-mode Sephadex LH-20×RPLC method provided higher peak resolution, sample processing ability (2.5mg) and better orthogonality (72.9%) versus RPLC×RPLC and hydrophilic interaction liquid chromatography (HILIC)×RPLC. To the best of our knowledge, this is the first report of a mixed-mode Sephadex LH-20×RPLC separation method with successful applications in on-line mode, which might be beneficial for harvesting targets from complicated medicinal plants. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Liquids and liquid mixtures

    CERN Document Server

    Rowlinson, J S; Baldwin, J E; Buckingham, A D; Danishefsky, S

    2013-01-01

    Liquids and Liquid Mixtures, Third Edition explores the equilibrium properties of liquids and liquid mixtures and relates them to the properties of the constituent molecules using the methods of statistical thermodynamics. Topics covered include the critical state, fluid mixtures at high pressures, and the statistical thermodynamics of fluids and mixtures. This book consists of eight chapters and begins with an overview of the liquid state and the thermodynamic properties of liquids and liquid mixtures, including vapor pressure and heat capacities. The discussion then turns to the thermodynami

  9. Low Density Solvent-Based Dispersive Liquid-Liquid Microextraction for the Determination of Synthetic Antioxidants in Beverages by High-Performance Liquid Chromatography

    Science.gov (United States)

    Çabuk, Hasan; Köktürk, Mustafa

    2013-01-01

    A simple and efficient method was established for the determination of synthetic antioxidants in beverages by using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography with ultraviolet detection. Butylated hydroxy toluene, butylated hydroxy anisole, and tert-butylhydroquinone were the antioxidants evaluated. Experimental parameters including extraction solvent, dispersive solvent, pH of sample solution, salt concentration, and extraction time were optimized. Under optimal conditions, the extraction recoveries ranged from 53 to 96%. Good linearity was observed by the square of correlation coefficients ranging from 0.9975 to 0.9997. The relative standard deviations ranged from 1.0 to 5.2% for all of the analytes. Limits of detection ranged from 0.85 to 2.73 ng mL−1. The method was successfully applied for determination of synthetic antioxidants in undiluted beverage samples with satisfactory recoveries. PMID:23853535

  10. Low Density Solvent-Based Dispersive Liquid-Liquid Microextraction for the Determination of Synthetic Antioxidants in Beverages by High-Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Hasan Çabuk

    2013-01-01

    Full Text Available A simple and efficient method was established for the determination of synthetic antioxidants in beverages by using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography with ultraviolet detection. Butylated hydroxy toluene, butylated hydroxy anisole, and tert-butylhydroquinone were the antioxidants evaluated. Experimental parameters including extraction solvent, dispersive solvent, pH of sample solution, salt concentration, and extraction time were optimized. Under optimal conditions, the extraction recoveries ranged from 53 to 96%. Good linearity was observed by the square of correlation coefficients ranging from 0.9975 to 0.9997. The relative standard deviations ranged from 1.0 to 5.2% for all of the analytes. Limits of detection ranged from 0.85 to 2.73 ng mL−1. The method was successfully applied for determination of synthetic antioxidants in undiluted beverage samples with satisfactory recoveries.

  11. Extraction behaviour and mechanism of Pt(iv) and Pd(ii) by liquid-liquid extraction with an ionic liquid [HBBIm]Br.

    Science.gov (United States)

    Liu, Wenhui; Wang, Qi; Zheng, Yan; Wang, Shubin; Yan, Yan; Yang, Yanzhao

    2017-06-06

    In this study, a method of one-step separation and recycling of high purity Pd(ii) and Pt(iv) using an ionic liquid, 1-butyl-3-benzimidazolium bromate ([HBBIm]Br), was investigated. The effects of [HBBIm]Br concentration, initial metal concentration, and loading capacity of [HBBIm]Br were examined in detail. It was observed that [HBBIm]Br was a very effective extractant for selectively extracting Pd(ii) and precipitating Pt(iv). Through selectively extracting Pd(ii) and precipitating Pt(iv), each metal with high purity was separately obtained from mixed Pd(ii) and Pt(iv) multi-metal solution. The method of one-step separation of Pd(ii) and Pt(iv) is simple and convenient. The anion exchange mechanism between [HBBIm]Br and Pt(iv) was proven through Job's method and FTIR and 1 H NMR spectroscopies. The coordination mechanism between [HBBIm]Br and Pd(ii) was demonstrated via single X-ray diffraction and was found to be robust and distinct, as supported by the ab initio quantum-chemical studies. The crystals of the [PdBr 2 ·2BBIm] complex were formed first. Moreover, the influence of the concentrations of hydrochloric acid, sodium chloride, and sodium nitrate on the precipitation of Pt(iv) and extraction of Pd(ii) was studied herein. It was found that only the concentration of H + could inhibit the separation of Pt(iv) because H + could attract the anion PtCl 6 2- ; thus, the exchange (anion exchange mechanism) between the anions PtCl 6 2- and Br - was prevented. However, both the concentration of H + and Cl - can obviously inhibit the extraction of Pd(ii) because H + and Cl - are the reaction products and increasing their concentration can inhibit the progress of the reaction (coordination mechanism).

  12. (Liquid + liquid) equilibria for benzene + cyclohexane + N,N-dimethylformamide + sodium thiocyanate

    International Nuclear Information System (INIS)

    Dong, Hongxing; Yang, Xiaoguang; Yue, Guojun; Zhang, Wei; Zhang, Jin

    2013-01-01

    Graphical abstract: On the left, the figure was phase diagram about the LLE date. On the right, the figure was about the effects of mass fraction of benzene in the raffinate phase to the selectivity(S) coefficient under different salt concentration. ■, the NaSCN and DMF in ratio of 5/95; • , the NaSCN and DMF in ratio of 10/90; ▴, the NaSCN and DMF in ratio of 15/85; ★, the NaSCN and DMF in ratio of 20/80; ▾, the NaSCN and DMF in ratio of 23/77. ♦, only DMF was used extractant (the selectivity coefficient was calculated by literature 17). w 22 , refer to the mass fraction of benzene in the raffinate phase (cyclohexane-rich phase). Highlights: • (Liquid + liquid) equilibrium for quaternary system was measured. • The components include benzene, cyclohexane, N,N-dimethylformamide, sodium thiocyanate. • The (liquid + liquid) equilibrium data can be well correlated by the NRTL model. • Separation of benzene and cyclohexane by NaSCN + DMF was discussed. -- Abstract: (Liquid + liquid) equilibrium (LLE) data for benzene + cyclohexane + N,N-dimethylformamide (DMF) + sodium thiocyanate (NaSCN) were measured experimentally at atmospheric pressure and 303.15 K. The selectivity coefficients from these LLE data were calculated and compared to those previously reported in the literature for the systems (benzene + cyclohexane + DMF) and (benzene + cyclohexane + DMF + KSCN). The NRTL equation was used to correlate the experimental data. The agreement between the predicted and experimental results was good. It was found that the selectivity coefficients of DMF + NaSCN for benzene ranged from 2.45 to 11.99. Considering the relatively high extraction capacity and selectivity for benzene, DMF + NaSCN may be used as a potential extracting solvent for the separation of benzene from cyclohexane

  13. Extraction of Uranium from Aqueous Solutions Using Ionic Liquid and Supercritical Carbon Dioxide in Conjunction

    International Nuclear Information System (INIS)

    Wang, Joanna S.; Sheaff, Chrystal N.; Yoon, Byunghoon; Addleman, Raymond S.; Wai, Chien M.

    2009-01-01

    Uranyl ions (UO2)2+ in aqueous nitric acid solutions can be extracted into supercritical CO2 (sc-CO2) via an imidazolium-based ionic liquid using tri-n-butylphosphate (TBP) as a complexing agent. The transfer of uranium from the ionic liquid to the supercritical fluid phase was monitored by UV/Vis spectroscopy using a high-pressure fiberoptic cell. The form of the uranyl complex extracted into the supercritical CO2 phase was found to be UO2(NO3)2(TBP)2. The extraction results were confirmed by UV/Vis spectroscopy and by neutron activation analysis. This technique could potentially be used to extract other actinides for applications in the field of nuclear waste management.

  14. Rapid determination of some psychotropic drugs in complex matrices by tandem dispersive liquid-liquid microextraction followed by high performance liquid chromatography.

    Science.gov (United States)

    Asghari, Alireza; Fahimi, Ebrahim; Bazregar, Mohammad; Rajabi, Maryam; Boutorabi, Leila

    2017-05-01

    Simple and rapid determinations of some psychotropic drugs in some pharmaceutical wastewater and human plasma samples were successfully accomplished via the tandem dispersive liquid-liquid microextraction combined with high performance liquid chromatography-ultraviolet detection (TDLLME-HPLC-UV). TDLLME of the three psychotropic drugs clozapine, chlorpromazine, and thioridazine was easily performed through two consecutive dispersive liquid-liquid microextractions. By performing this convenient method, proper sample preconcentrations and clean-ups were achieved in just about 7min. In order to achieve the best extraction efficiency, the effective parameters involved were optimized. The optimal experimental conditions consisted of 100μL of CCl 4 (as the extraction organic solvent), and the pH values of 13 and 2 for the donor and acceptor phases, respectively. Under these optimum experimental conditions, the proposed TDLLME-HPLC-UV technique provided a good linearity in the range of 5-3000ngmL -1 for the three psychotropic drugs with the correlation of determinations (R 2 s) higher than 0.996. The limits of quantification (LOQs) and limits of detection (LODs) obtained were 5.0ngmL -1 and 1.0-1.5ngmL -1 , respectively. Also the proper enrichment factors (EFs) of 96, 99, and 88 for clozapine, chlorpromazine, and thioridazine, respectively, and good extraction repeatabilities (relative standard deviations below 9.3%, n=5) were obtained. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Ionic liquid solutions as extractive solvents for value-added compounds from biomass.

    Science.gov (United States)

    Passos, Helena; Freire, Mara G; Coutinho, João A P

    2014-12-01

    In the past few years, the number of studies regarding the application of ionic liquids (ILs) as alternative solvents to extract value-added compounds from biomass has been growing. Based on an extended compilation and analysis of the data hitherto reported, the main objective of this review is to provide an overview on the use of ILs and their mixtures with molecular solvents for the extraction of value-added compounds present in natural sources. The ILs (or IL solutions) investigated as solvents for the extraction of natural compounds, such as alkaloids, flavonoids, terpenoids, lipids, among others, are outlined. The extraction techniques employed, namely solid-liquid extraction, and microwave-assisted and ultrasound-assisted extractions, are emphasized and discussed in terms of extraction yields and purification factors. Furthermore, the evaluation of the IL chemical structure and the optimization of the process conditions (IL concentration, temperature, biomass-solvent ratio, etc.) are critically addressed. Major conclusions on the role of the ILs towards the extraction mechanisms and improved extraction yields are additionally provided. The isolation and recovery procedures of the value-added compounds are ascertained as well as some scattered strategies already reported for the IL solvent recovery and reusability. Finally, a critical analysis on the economic impact versus the extraction performance of IL-based methodologies was also carried out and is here presented and discussed.

  16. Simultaneous determination of four trace estrogens in feces, leachate, tap and groundwater using solid-liquid extraction/auto solid-phase extraction and high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Liu, Na; Shi, Yue-e; Li, Mengyan; Zhang, Ting-di; Gao, Song

    2015-10-01

    A simple and selective high-performance liquid chromatography method coupled with fluorescence detection was developed for the simultaneous measurement of trace levels of four estrogens (estrone, estradiol, estriol and 17α-ethynyl estradiol) in environmental matrices. For feces samples, solid-liquid extraction was applied with a 1:1 v/v mixture of acetonitrile and ethyl acetate as the extraction solvent. For liquid samples (e.g., leachate and groundwater), hydrophobic/lipophilic balanced automated solid-phase extraction disks were selected due to their high recoveries compared to conventional C18 disks. Chromatographic separations were performed on a reversed-phase C18 column gradient-eluted with a 45:55 v/v mixture of acetonitrile and water. The detection limits were down to 1.1 × 10(-2) (estrone), 4.11 × 10(-4) (estradiol), 5.2 × 10(-3) (estriol) and 7.18 × 10(-3) μg/L (17α-ethynyl estradiol) at excitation/emission wavelengths of 288/310 nm, with recoveries in the range of 96.9 ± 3.2-105.4 ± 3.2% (n = 3). The method was successfully applied to determine estrogens in feces and water samples collected at livestock farms and a major river in Northeast China. We observed relatively high abundance and widespread distribution of all four estrogens in our sample collections, implying the urgency for a comprehensive and intricate investigation of estrogenic fate and contamination in our researched area. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Genotoxicity, mutagenicity and cytotoxicity of carotenoids extracted from ionic liquid in multiples organs of Wistar rats.

    Science.gov (United States)

    Larangeira, Paula Martins; de Rosso, Veridiana Vera; da Silva, Victor Hugo Pereira; de Moura, Carolina Foot Gomes; Ribeiro, Daniel Araki

    2016-11-01

    The ionic liquid or melted salt 1-Butyl-3-methylimidazolium is an alternative process to extract natural pigments, such as carotenoids. Lycopene represents 80-90% of total of carotenoids presents in tomatoes and it has been widely studied due its potent antioxidant action. The aim of this study was to evaluate genotoxicity, mutagenicity and cytotoxicity of carotenoids extracted from ionic liquid using experimental model in vivo. For this purpose, a total of 20 male Wistar rats were distributed into four groups (n=5), as follows: control group; received a corresponding amount of corn oil for 7days by intragastric gavage (i.g.), ionic liquid group, received 10mgkg -1 body weight for 7days by gavage; 10mg carotenoids group, received 10mgkg -1 bw dissolved in corn oil for 7days by gavage and 500mg carotenoids group, received 500mgkg -1 bw dissolved in corn oil for 7days by gavage. Rat liver treated with ionic liquid exhibited moderate histopathological changes randomly distributed in the parenchyma, such as cytoplasmic eosinophilia, apoptotic bodies, inflammatory infiltrate and focal necrosis. DNA damage was found in peripheral blood and liver cells of rats treated with ionic liquid or carotenoids at 500mg. An increase of micronucleated cells and 8-OhDG immunopositive cells were also detected in rats treated with carotenoids at 500mg. In summary, our results demonstrate that recommended dose for human daily intake of carotenoids extracted by ionic liquid did not induce genotoxicity, mutagenicity and cytotoxicity in multiple organs of rats. Copyright © 2016 Elsevier GmbH. All rights reserved.

  18. chemical studies on the extraction of certain metal ions from aqueous solution by liquid emulsion membrane

    International Nuclear Information System (INIS)

    Kassem, A.T.

    2011-01-01

    In this thesis four systems are addressed related to the use of liquid emulsion membranes (ELM) based on Co(III)dicarbiolide and. The system was dedicated for permeation of cadmium , cobalt Nickel and lead for use of this system for preconcentration and separation of cadmium, cobalt, nickel and lead. The work carried out in this thesis is presented in three parts, namely; introduction, experimental and results and discussion.The first chapter is the introduction which includes aim of work, basic concepts of liquid membranes; liquid emulsion membranes; different models of emulsion permeation, literature survey of extraction chemistry of cadmium, cobalt, nickel and lead. Chapter two includes the experimental part. In this part detailed outlines on the chemicals and different elements used were given. Different instruments as well as analytical techniques were outlines. The preparation of liquid emulsion membrane and the permeation techniques were presented in details. The third chapter deals with the results and discussion. This chapter is divided into four main parts, the four parts is concerned with cadmium/Co(III) dicarbolide/NTA, EDTA, DPTA and DCTA systems. In this part the permeation of Cd(II) aqueous solution by the membrane used was experimented based on liquid-liquid extraction studies of cadmium from different sodium chloride molarities (from 0.01 to 0.1 M) by 0.01 M Cobalt(III) dicarbolides. It was found that the extraction of with cadmium is higher following in the first system, the permeation of the toxic elements, Cd(II) from HCl/sodium chloride medium was carried out using liquid emulsion membrane containing Co(III)dicarbiolide in xylene as carrier, Spain 80/ Spain 85(1:3) as surfactant and NTA, EDTA, DPTA and DCTA as a stripping solutions.

  19. Selective extraction and recovery of rare earth metals from phosphor powders in waste fluorescent lamps using an ionic liquid system.

    Science.gov (United States)

    Yang, Fan; Kubota, Fukiko; Baba, Yuzo; Kamiya, Noriho; Goto, Masahiro

    2013-06-15

    The recycling of rare earth metals from phosphor powders in waste fluorescent lamps by solvent extraction using ionic liquids was studied. Acid leaching of rare earth metals from the waste phosphor powder was examined first. Yttrium (Y) and europium (Eu) dissolved readily in the acid solution; however, the leaching of other rare earth metals required substantial energy input. Ionization of target rare earth metals from the waste phosphor powders into the leach solution was critical for their successful recovery. As a high temperature was required for the complete leaching of all rare earth metals, ionic liquids, for which vapor pressure is negligible, were used as an alternative extracting phase to the conventional organic diluent. An extractant, N, N-dioctyldiglycol amic acid (DODGAA), which was recently developed, showed a high affinity for rare earth metal ions in liquid-liquid extraction although a conventional commercial phosphonic extractant did not. An effective recovery of the rare earth metals, Y, Eu, La and Ce, from the metal impurities, Fe, Al and Zn, was achieved from the acidic leach solution of phosphor powders using an ionic liquid containing DODGAA as novel extractant system. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Liquid-liquid displacement in slippery liquid-infused membranes (SLIMs)

    OpenAIRE

    Bazyar, Hanieh; Lv, Pengyu; Wood, Jeffery A.; Porada, Slawomir; Lohse, Detlef; Lammertink, Rob G. H.

    2018-01-01

    Liquid-infused membranes inspired by slippery liquid-infused porous surfaces (SLIPS) have been recently introduced to membrane technology. The gating mechanism of these membranes is expected to give rise to anti-fouling properties and multi-phase transport capabilities. However, the long-term retention of the infusion liquid has not yet been explored. To address this issue, we investigate the retention of the infusion liquid in slippery liquid-infused membranes (SLIMs) via liquid-liquid displ...

  1. Binary Solvents Dispersive Liquid-Liquid Microextraction (BS-DLLME) Method for Determination of Tramadol in Urine Using High-Performance Liquid Chromatography.

    Science.gov (United States)

    Kiarostami, Vahid; Rouini, Mohamad-Reza; Mohammadian, Razieh; Lavasani, Hoda; Ghazaghi, Mehri

    2014-02-03

    Tramadol is an opioid, synthetic analog of codeine and has been used for the treatment of acute or chronic pain may be abused. In this work, a developed Dispersive liquid liquid microextraction (DLLME) as binary solvents-based dispersive liquid-liquid microextraction (BS-DLLME) combined with high performance liquid chromatography (HPLC) with fluorescence detection (FD) was employed for determination of tramadol in the urine samples. This procedure involves the use of an appropriate mixture of binary extraction solvents (70 μL CHCl3 and 30 μL ethyl acetate) and disperser solvent (600 μL acetone) for the formation of cloudy solution in 5 ml urine sample comprising tramadol and NaCl (7.5%, w/v). After centrifuging, the small droplets of extraction solvents were precipitated. In the final step, the HPLC with fluorescence detection was used for determination of tramadol in the precipitated phase. Various factors on the efficiency of the proposed procedure were investigated and optimized. The detection limit (S/N = 3) and quantification limit (S/N = 10) were found 0.2 and 0.9 μg/L, respectively. The relative standard deviations (RSD) for the extraction of 30 μg L of tramadol was found 4.1% (n = 6). The relative recoveries of tramadol from urine samples at spiking levels of 10, 30 and 60 μg/L were in the range of 95.6 - 99.6%. Compared with other methods, this method provides good figures of merit such as good repeatability, high extraction efficiency, short analysis time, simple procedure and can be used as microextraction technique for routine analysis in clinical laboratories.

  2. Micro-electromembrane extraction across free liquid membranes. Extractions of basic drugs from undiluted biological samples

    Czech Academy of Sciences Publication Activity Database

    Kubáň, Pavel; Boček, Petr

    2014-01-01

    Roč. 1337, Apr (2014), s. 32-39 ISSN 0021-9673 R&D Projects: GA ČR(CZ) GA13-05762S Institutional support: RVO:68081715 Keywords : micro-electromembrane extraction * free liquid membranes * biological samples Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.169, year: 2014

  3. Recent development of ionic liquid membranes

    OpenAIRE

    Wang, Junfeng; Luo, Jianquan; Feng, Shicao; Li, Haoran; Wan, Yinhua; Zhang, Xiangping

    2016-01-01

    The interest in ionic liquids (IL) is motivated by its unique properties, such as negligible vapor pressure, thermal stability, wide electrochemical stability window, and tunability of properties. ILs have been highlighted as solvents for liquidâliquid extraction and liquid membrane separation. To further expand its application in separation field, the ionic liquid membranes (ILMs) and its separation technology have been proposed and developed rapidly. This paper is to give a comprehensive ov...

  4. Separation of thiophene from heptane with ionic liquids

    International Nuclear Information System (INIS)

    Domańska, Urszula; Lukoshko, Elena Vadimovna; Królikowski, Marek

    2013-01-01

    Highlights: ► The ternary (liquid + liquid) equilibria in 1-butyl-1-methylpyrrolidinium-based ILs was measured. ► High selectivity and distribution ratio for the extraction of thiophene was found. ► [BMPYR][TCM] was proposed as entrainer for the separation process. ► Extraction of sulphur-compounds from alkanes was proposed. -- Abstract: Ionic liquids (ILs) are well known novel green solvents, which can be used for removing sulfur compounds from gasoline and diesel oils. Ternary (liquid + liquid) equilibrium data are presented for mixtures of {ionic liquid (1) + thiophene (2) + heptane (3)} at T = 298.15 K and ambient pressure to analyze the performance of the ionic liquid (IL) in the extraction of thiophene from the alkanes. Three pyrrolidinium-based ionic liquids have been studied: 1-butyl-1-methylpyrrolidinium tris(pentafluoroethyl)trifluorophosphate, ([BMPYR][FAP]), 1-butyl-1-methylpyrrolidinium tetracyanoborate, [BMPYR][TCB] and 1-butyl-1-methylpyrrolidinium tricyanomethanide, [BMPYR][TCM]. The results are discussed in terms of the selectivity and distribution ratio of separation of related systems. The immiscibility in the binary liquid systems of (thiophene + heptane) with all used ILs was observed. The [TCM] − anion in comparison with [TCB] − and [FAP] − anions shows much higher selectivity and slightly lower distribution ratio for extraction of thiophene. The non-random two liquid NRTL model was used successfully to correlate the experimental tie-lines and to calculate the phase composition error in mole fraction in the ternary systems. The average root mean square deviation (RMSD) of the phase composition was 0.047. The densities of [BMPYR][TCM] in temperature range from (298.15 to 348.15) K were measured. The data presented here show that the [BMPYR][TCM] ionic liquid can be used as an alternative solvent for the separation of thiophene from the hydrocarbon stream using solvent liquid–liquid extraction at ambient conditions

  5. Vacuum sieve tray for tritium extraction from liquid Pb-17Li

    Energy Technology Data Exchange (ETDEWEB)

    Okino, Fumito, E-mail: fumito.okino@iae.kyoto-u.ac.jp [Graduate School of Energy Science, Kyoto University, Uji, Kyoto 611-0011 (Japan); Noborio, Kazuyuki [Institute of Sustainability Science, Kyoto University, Uji, Kyoto 611-0011 (Japan); Yamamoto, Yasushi [Faculty of Engineering Science, Kansai University, 3-3-35 Suita-shi, Osaka 564-8680 (Japan); Konishi, Satoshi [Institute of Advanced Energy, Kyoto University, Uji, Kyoto 611-0011 (Japan)

    2012-08-15

    Formation of droplet of liquid Li-17Pb released from a nozzle into vacuum was studied for the evaluation of the feasibility as a tritium extraction process. Size of droplets formed from the nozzles was estimated by theoretical and experimental methods. For the theoretical estimation, the non-dimensional comparison of the physical bulk property of liquid Pb-17Li with water (H{sub 2}O) at ambient temperature was applied. It was found to be reasonable to apply the Plateau-Rayleigh-Instability theory for the droplet size formula of the fluid Pb-17Li for the nozzle diameter 0.4 mm-1.0 mm, temperature 400 Degree-Sign C-500 Degree-Sign C, at initial velocity of 3 m/s. The experimental results of the droplet size showed good agreement with the theory. This device was used for the parametric study of extraction of deuterium during their free fall in vacuum. The scaling of the device suggests the engineering feasibility of the process.

  6. Combination of solid phase extraction and dispersive liquid-liquid microextraction for separation/preconcentration of ultra trace amounts of uranium prior to its fiber optic-linear array spectrophotometry determination.

    Science.gov (United States)

    Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji; Shakerian, Farid; Shiralian Esfahani, Golnaz

    2013-12-15

    A simple and sensitive method for the separation and preconcentration of the ultra trace amounts of uranium and its determination by spectrophotometry was developed. The method is based on the combination of solid phase extraction and dispersive liquid-liquid microextraction. Thus, by passing the sample through the basic alumina column, the uranyl ion and some cations are separated from the sample matrix. The retained uranyl ion along with the cations are eluted with 5 mL of nitric acid (2 mol L(-1)) and after neutralization of the eluent, the extracted uranyl ion is converted to its anionic benzoate complex and is separated from other cations by extraction of its ion pair with malachite green into small volume of chloroform using dispersive liquid-liquid microextraction. The amount of uranium is then determined by the absorption measurement of the extracted ion pair at 621 nm using flow injection spectrophotometry. Under the optimum conditions, with 500 mL of the sample, a preconcentration factor of 1980, a detection limit of 40 ng L(-1), and a relative standard deviation of 4.1% (n=6) at 400 ng L(-1) were obtained. The method was successfully applied to the determination of uranium in mineral water, river water, well water, spring water and sea water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. A comparison of various modes of liquid-liquid based microextraction techniques: determination of picric acid.

    Science.gov (United States)

    Burdel, Martin; Šandrejová, Jana; Balogh, Ioseph S; Vishnikin, Andriy; Andruch, Vasil

    2013-03-01

    Three modes of liquid-liquid based microextraction techniques--namely auxiliary solvent-assisted dispersive liquid-liquid microextraction, auxiliary solvent-assisted dispersive liquid-liquid microextraction with low-solvent consumption, and ultrasound-assisted emulsification microextraction--were compared. Picric acid was used as the model analyte. The determination is based on the reaction of picric acid with Astra Phloxine reagent to produce an ion associate easily extractable by various organic solvents, followed by spectrophotometric detection at 558 nm. Each of the compared procedures has both advantages and disadvantages. The main benefit of ultrasound-assisted emulsification microextraction is that no hazardous chlorinated extraction solvents and no dispersive solvent are necessary. Therefore, this procedure was selected for validation. Under optimized experimental conditions (pH 3, 7 × 10(-5) mol/L of Astra Phloxine, and 100 μL of toluene), the calibration plot was linear in the range of 0.02-0.14 mg/L and the LOD was 7 μg/L of picric acid. The developed procedure was applied to the analysis of spiked water samples. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. A highly selective dispersive liquid-liquid microextraction approach based on the unique fluorous affinity for the extraction and detection of per- and polyfluoroalkyl substances coupled with high performance liquid chromatography tandem-mass spectrometry.

    Science.gov (United States)

    Wang, Juan; Shi, Yali; Cai, Yaqi

    2018-04-06

    In the present study, a highly selective fluorous affinity-based dispersive liquid-liquid microextraction (DLLME) technique was developed for the extraction and analysis of per- and polyfluoroalkyl substances (PFASs) followed by high performance liquid chromatography tandem-mass spectrometry. Perfluoro-tert-butanol with multiple C-F bonds was chosen as the extraction solvent, which was injected into the aqueous samples with a dispersive solvent (acetonitrile) in a 120:800 (μL, v/v) mixture for PFASs enrichment. The fluorous affinity-based extraction mechanism was confirmed by the significantly higher extraction recoveries for PFASs containing multiple fluorine atoms than those for compounds with fewer or no fluorine atoms. The extraction recoveries of medium and long-chain PFASs (CF 2  > 5) exceeded 70%, except perfluoroheptanoic acid, while those of short-chain PFASs were lower than 50%, implying that the proposed DLLME may not be suitable for their extraction due to weak fluorous affinity. This highly fluoroselective DLLME technique can greatly decrease the matrix effect that occurs in mass spectrometry detection when applied to the analysis of urine samples. Under the optimum conditions, the relative recoveries of PFASs with CF 2  > 5 ranged from 80.6-121.4% for tap water, river water and urine samples spiked with concentrations of 10, 50 and 100 ng/L. The method limits of quantification for PFASs in water and urine samples were in the range of 0.6-8.7 ng/L. Furthermore, comparable concentrations of PFASs were obtained via DLLME and solid-phase extraction, confirming that the developed DLLME technique is a promising method for the extraction of PFASs in real samples. Copyright © 2018 Elsevier B.V. All rights reserved.

  9. Combination of electromembrane extraction and liquid-phase microextraction in a single step: Simultaneous group separation of acidic and basic drugs

    DEFF Research Database (Denmark)

    Huang, Chuixiu; Seip, Knut Fredrik; Gjelstad, Astrid

    2015-01-01

    at high concentration. This approach was further investigated from human plasma. Extraction recoveries were strongly dependent on dilution of plasma with buffer and on extraction time. Finally, this simultaneous EME/LPME approach was evaluated in combination with liquid chromatography (LC......Electromembrane extraction (EME) and liquid-phase microextraction (LPME) were combined in a single step for the first time to realize simultaneous and clear group separation of basic and acidic drugs. Using 2-nitrophenyl octyl ether as the supported liquid membrane (SLM) for EME and dihexyl ether...

  10. Dispersive liquid-liquid microextraction combined with graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Zeini Jahromi, Elham; Bidari, Araz; Assadi, Yaghoub; Milani Hosseini, Mohammad Reza; Jamali, Mohammad Reza

    2007-01-01

    Dispersive liquid-liquid microextraction (DLLME) technique was successfully used as a sample preparation method for graphite furnace atomic absorption spectrometry (GF AAS). In this extraction method, 500 μL methanol (disperser solvent) containing 34 μL carbon tetrachloride (extraction solvent) and 0.00010 g ammonium pyrrolidine dithiocarbamate (chelating agent) was rapidly injected by syringe into the water sample containing cadmium ions (interest analyte). Thereby, a cloudy solution formed. The cloudy state resulted from the formation of fine droplets of carbon tetrachloride, which have been dispersed, in bulk aqueous sample. At this stage, cadmium reacts with ammonium pyrrolidine dithiocarbamate, and therefore, hydrophobic complex forms which is extracted into the fine droplets of carbon tetrachloride. After centrifugation (2 min at 5000 rpm), these droplets were sedimented at the bottom of the conical test tube (25 ± 1 μL). Then a 20 μL of sedimented phase containing enriched analyte was determined by GF AAS. Some effective parameters on extraction and complex formation, such as extraction and disperser solvent type and their volume, extraction time, salt effect, pH and concentration of the chelating agent have been optimized. Under the optimum conditions, the enrichment factor 125 was obtained from only 5.00 mL of water sample. The calibration graph was linear in the rage of 2-20 ng L -1 with detection limit of 0.6 ng L -1 . The relative standard deviation (R.S.D.s) for ten replicate measurements of 20 ng L -1 of cadmium was 3.5%. The relative recoveries of cadmium in tap, sea and rivers water samples at spiking level of 5 and 10 ng L -1 are 108, 95, 87 and 98%, respectively. The characteristics of the proposed method have been compared with cloud point extraction (CPE), on-line liquid-liquid extraction, single drop microextraction (SDME), on-line solid phase extraction (SPE) and co-precipitation based on bibliographic data. Therefore, DLLME combined with

  11. Extraction of polycyclic aromatic hydrocarbons from smoked fish using pressurized liquid extraction with integrated fat removal

    DEFF Research Database (Denmark)

    Lund, Mette; Duedahl-Olesen, Lene; Christensen, Jan H.

    2009-01-01

    Quantification of polycyclic aromatic hydrocarbons (PAHs) in smoked fish products often requires multiple clean-up steps to remove fat and other compounds that may interfere with the chemical analysis. We present a novel pressurized liquid extraction (PLE) method that integrates exhaustive...

  12. CASH AND LIQUIDITY/LIQUIDITY AND LIQUIDITY RATIO

    Directory of Open Access Journals (Sweden)

    BEATRIX LIGHEZAN BREUER

    2012-12-01

    Full Text Available The present paper aims to present the correlation as well as the differences between liquidity/cash and liquidity ratio in terms of economic entities. Researches on this topic are based on the opinions of some specialists in accounting and in the economic-financial analysis, as well as on the national legal stipulations and the ones set out in the International Accounting Standards, the Financial report, respectively. The object of this paper is represented by the correlation between liquidity/cash and liquidity ratios representing the liquidity as current assets, assets implied in the determination of liquidity ratios. The end of the paper consists of the conclusions drawn from the issues presented in the paper but also our views on this research topic.

  13. Optimizing pressurized liquid extraction of microbial lipids using the response surface method.

    Science.gov (United States)

    Cescut, J; Severac, E; Molina-Jouve, C; Uribelarrea, J-L

    2011-01-21

    Response surface methodology (RSM) was used for the determination of optimum extraction parameters to reach maximum lipid extraction yield with yeast. Total lipids were extracted from oleaginous yeast (Rhodotorula glutinis) using pressurized liquid extraction (PLE). The effects of extraction parameters on lipid extraction yield were studied by employing a second-order central composite design. The optimal condition was obtained as three cycles of 15 min at 100°C with a ratio of 144 g of hydromatrix per 100 g of dry cell weight. Different analysis methods were used to compare the optimized PLE method with two conventional methods (Soxhlet and modification of Bligh and Dyer methods) under efficiency, selectivity and reproducibility criteria thanks to gravimetric analysis, GC with flame ionization detector, High Performance Liquid Chromatography linked to Evaporative Light Scattering Detector (HPLC-ELSD) and thin-layer chromatographic analysis. For each sample, the lipid extraction yield with optimized PLE was higher than those obtained with referenced methods (Soxhlet and Bligh and Dyer methods with, respectively, a recovery of 78% and 85% compared to PLE method). Moreover, the use of PLE led to major advantages such as an analysis time reduction by a factor of 10 and solvent quantity reduction by 70%, compared with traditional extraction methods. Copyright © 2010 Elsevier B.V. All rights reserved.

  14. Liquid metal extraction of Nd from NdFeB magnet scrap

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Yanchen [Iowa State Univ., Ames, IA (United States)

    1999-12-10

    This research involves using molten magnesium (Mg) to remove neodymium (Nd) from NdFeB magnet scrap by diffusion. The results show that liquid metal extraction of Nd may be a viable and inexpensive method for recovering the expensive rare earth element Nd for use in Mg castings.

  15. Liquid-liquid extraction of strongly protein bound BMS-299897 from human plasma and cerebrospinal fluid, followed by high-performance liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Xue, Y J; Pursley, Janice; Arnold, Mark

    2007-04-11

    BMS-299897 is a gamma-secretase inhibitor that is being developed for the treatment of Alzheimer's disease. Liquid-liquid extraction (LLE), chromatographic/tandem mass spectrometry (LC/MS/MS) methods have been developed and validated for the quantitation of BMS-299897 in human plasma and cerebrospinal fluid (CSF). Both methods utilized (13)C6-BMS-299897, the stable label isotope analog, as the internal standard. For the human plasma extraction method, two incubation steps were required after the addition of 5 mM ammonium acetate and the internal standard in acetonitrile to release the analyte bound to proteins prior to LLE with toluene. For the human CSF extraction method, after the addition of 0.5 N HCl and the internal standard, CSF samples were extracted with toluene and no incubation was required. The organic layers obtained from both extraction methods were removed and evaporated to dryness. The residues were reconstituted and injected into the LC/MS/MS system. Chromatographic separation was achieved isocratically on a MetaChem C18 Hypersil BDS column (2.0 mm x 50 mm, 3 microm). The mobile phase contained 10 mM ammonium acetate pH 5 and acetonitrile. Detection was by negative ion electrospray tandem mass spectrometry. The standard curves ranged from 1 to 1000 ng/ml for human plasma and 0.25-100 ng/ml for human CSF. Both standard curves were fitted to a 1/x weighted quadratic regression model. For both methods, the intra-assay precision was within 8.2% CV, the inter-assay precision was within 5.4% CV, and assay accuracy was within +/-7.4% of the nominal values. The validation and sample analysis results demonstrated that both methods had acceptable precision and accuracy across the calibration ranges.

  16. Application and optimization of microwave-assisted extraction and dispersive liquid-liquid microextraction followed by high-performance liquid chromatography for sensitive determination of polyamines in turkey breast meat samples.

    Science.gov (United States)

    Bashiry, Moein; Mohammadi, Abdorreza; Hosseini, Hedayat; Kamankesh, Marzieh; Aeenehvand, Saeed; Mohammadi, Zaniar

    2016-01-01

    A novel method based on microwave-assisted extraction and dispersive liquid-liquid microextraction (MAE-DLLME) followed by high-performance liquid chromatography (HPLC) was developed for the determination of three polyamines from turkey breast meat samples. Response surface methodology (RSM) based on central composite design (CCD) was used to optimize the effective factors in DLLME process. The optimum microextraction efficiency was obtained under optimized conditions. The calibration graphs of the proposed method were linear in the range of 20-200 ng g(-1), with the coefficient determination (R(2)) higher than 0.9914. The relative standard deviations were 6.72-7.30% (n = 7). The limits of detection were in the range of 0.8-1.4 ng g(-1). The recoveries of these compounds in spiked turkey breast meat samples were from 95% to 105%. The increased sensitivity in using the MAE-DLLME-HPLC-UV has been demonstrated. Compared with previous methods, the proposed method is an accurate, rapid and reliable sample-pretreatment method. Copyright © 2015 Elsevier Ltd. All rights reserved.

  17. Analysis of 99Tc in the radioactive liquid waste after extraction into suitable solvent

    International Nuclear Information System (INIS)

    Sonar, N.L.; Vaishali De; Pardeshi, V.; Raghvendra, Y.; Valsala, T.P.; Sonavane, M.S.; Kulkarni, Y.; Raj Kanwar

    2012-01-01

    99 Tc is one of the long lived fission product with high fission yield. >From radioactive waste management point of view it is very much essential to evaluate the concentration of technetium in the radioactive liquid waste in order to finalise the treatment process to extract/isolate it from the stream which is discharged to the environment. For the estimation of 99 Tc in the radioactive liquid waste stream, extraction of the stable complex of technetium-tetraphenyl arsonium chloride (TPAC) into chloroform followed by beta counting was studied. Various parameters like pH, time of equilibration, concentration of TPAC in chloroform, use of other solvent for extraction as well as interference of various other radionuclides present in the waste were also studied. The radioactive liquid waste being handled in plant contains high concentrations of salts in the form of sodium nitrate. Hence effect of salt concentration on the percentage extraction was also evaluated. The extraction behavior does not dependent on change in the pH of the solution. Almost 99.5% extraction was observed in the pH range of 1-13.0. High concentration of salt is affecting the extraction. However, this can be taken care by diluting the radioactive waste. It takes almost 90 min time for maximum extraction. Presence of radionuclides like 137 Cs, 90 Sr are not interfering the extraction of 99 Tc. However, 106 Ru is getting slightly extracted along with 99 Tc. The error due to 106 Ru can be eliminated by taking gamma spectrum and deducting the activity from the total beta activity to get 99 Tc activity. Nitrobenzene can be used for extraction of Tc-TPAC complex in place of chloroform. (author)

  18. 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°...

  19. (Liquid + liquid) equilibria of {benzene + cyclohexane + two ionic liquids} at different temperature and atmospheric pressure

    International Nuclear Information System (INIS)

    Sakal, Salem A.; Shen, Chong; Li, Chun-xi

    2012-01-01

    Highlights: ► (Liquid + liquid) equilibrium for two quaternary and two ternary systems were measured. ► The components include cyclohexane, benzene, [MIM][BF4], [MIM][ClO4] and [MMIM][DMP]. ► The (liquid + liquid) equilibrium data can be well correlated by the NRTL model. ► Separation of benzene and cyclohexane by pure ILs and their mixtures were discussed. - Abstract: (Liquid + liquid) equilibrium data of the following ternary and quaternary systems at different temperatures and mass fractions of ionic liquids (ILs) were measured at atmospheric pressure, i.e., {cyclohexane + benzene + 1,3-dimethylimidazolium dimethylphosphate ([MMIM][DMP])} at 298.2 K, {cyclohexane + benzene + 1-methylimidazolium tetrafluoroborate ([MIM][BF 4 ])} at 338.2 K, {cyclohexane + benzene + [MIM][BF 4 ] + [MMIM][DMP]} at (298.2 and 313.2) K, and {cyclohexane + benzene + 1-methylimidazolium perchlorate [MIM][ClO 4 ] + [MMIM][DMP]} at 298.2 K. The results indicate that both selectivity and distribution factor of the IL mixture for benzene are lower than that of pure IL [MMIM][DMP] at a specified condition, and decrease with the increase of the mass fraction of [MIM][BF 4 ] or [MIM][ClO 4 ] in its mixture of [MMIM][DMP] and the mole fraction of benzene. The extremely high selectivity of [MIM][BF 4 ] and [MIM][ClO 4 ] for aromatic compounds as predicted by the COSMOS-RS model is not justified by the present experimental results, and on the contrary, they show a relatively lower selectivity and extraction capacity for benzene than [MMIM][DMP].

  20. A modified approach for isolation of essential oil from fruit of Amorpha fruticosa Linn using microwave-assisted hydrodistillation concatenated liquid-liquid extraction.

    Science.gov (United States)

    Chen, Fengli; Jia, Jia; Zhang, Qiang; Gu, Huiyan; Yang, Lei

    2017-11-17

    In this work, a modified technique was developed to separate essential oil from the fruit of Amorpha fruticosa using microwave-assisted hydrodistillation concatenated liquid-liquid extraction (MHD-LLE). The new apparatus consists of two series-wound separation columns for separating essential oil, one is the conventional oil-water separation column, and the other is the extraction column of components from hydrosol using an organic solvent. Therefore, the apparatus can simultaneously collect the essential oil separated on the top of hydrosol and the components extracted from hydrosol using an organic solvent. Based on the yield of essential oil in the first and second separation columns, the effects of parameters were investigated by single factor experiments and Box-Behnken design. Under the optimum conditions (2mL ethyl ether as the extraction solvent in the second separation column, 12mL/g liquid-solid ratio, 4.0min homogenate time, 35min microwave irradiation time and 540W microwave irradiation power), satisfactory yields for the essential oil in the first separation column (10.31±0.33g/kg) and second separation column (0.82±0.03g/kg) were obtained. Compared with traditional methods, the developed method gave a higher yield of essential oil in a shorter time. In addition, GC-MS analysis of the essential oil indicated significant differences of the relative contents of individual volatile components in the essential oils obtained in the two separation columns. Therefore, the MHD-LLE technique developed here is a good alternative for the isolation of essential oil from A. fruticosa fruit as well as other herbs. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Pressurized liquid extraction of ginger (Zingiber officinale Roscoe) with bioethanol:

    DEFF Research Database (Denmark)

    Hu, Jiajin; Guo, Zheng; Glasius, Marianne

    2011-01-01

    To develop an efficient green extraction approach for recovery of bioactive compounds from natural plants, we examined the potential of pressurized liquid extraction (PLE) of ginger (Zingiber officinale Roscoe) with bioethanol/water as solvents. The advantages of PLE over other extraction...... approaches, in addition to reduced time/solvent cost, the extract of PLE showed a distinct constituent profile from that of Soxhlet extraction, with significantly improved recovery of diarylheptanoids, etc. Among the pure solvents tested for PLE, bioethanol yield the highest efficiency for recovering most...... constituents of gingerol-related compounds; while for a broad concentration spectrum of ethanol aqueous solutions, 70% ethanol gave the best performance in terms of yield of total extract, complete constituent profile and recovery of most gingerol-related components. PLE with 70% bioethanol operated at 1500...

  2. Role of an ionic liquid, 1-butyl-3-methylimidazolium 2-(2-methoxyethoxy)ethyl sulfate in extraction studies of gadolinium oxide

    Energy Technology Data Exchange (ETDEWEB)

    Sen, Kamalika [Calcutta Univ., Kolkata (India). Dept. of Chemistry; Wolterbeek, H.T. [Technical Univ. Delft (NL). Section RIH (Radiation and Isotopes in Health)

    2012-07-01

    The room temperature ionic liquid (RTIL), 1-butyl-3-methylimidazolium 2-(2-methoxyethoxy)ethyl sulfate was studied for its extraction behavior for {sup 159}Gd in an environmentally benign liquid-liquid extraction system. The gadolinium oxide when dissolved in nitric acid and extracted in an RTIL/dextran biphasic system, was found to get completely extracted in the IL phase. The otherwise difficult to dissolve gadolinium oxide was found to have some solubility in the IL studied. Biphasic systems consisting of IL/dextran and certain IL/salt were studied for the extraction behavior of Gd{sub 2}O{sub 3} dissolved in the above RTIL. A similar experiment was also done with acid-dissolved gadolinium oxide for comparison. (orig.)

  3. (Liquid + liquid) equilibria of perfluorocarbons with fluorinated ionic liquids

    International Nuclear Information System (INIS)

    Martinho, S.; Araújo, J.M.M.; Rebelo, L.P.N.; Pereiro, A.B.; Marrucho, I.M.

    2013-01-01

    Highlights: • (Liquid + liquid) equilibria perfluorocarbons and fluorinated ionic liquids. • Non-Random Two Liquid model was successfully applied. • Thermodynamic functions that describe the solvation process were calculated. -- Abstract: In order to evaluate the feasibility of partially replace perfluorocarbons (PFCs) with fluorinated ionic liquids (FILs) in PFCs-in-water emulsions, usually used for biomedical purposes, herein the (liquid + liquid) phase equilibria of FILs containing fluorinated chains longer than four carbons with PFCs were carried out in a wide range of temperatures. With this goal in mind, two PFCs (perfluorooctane and perfluorodecalin) were selected and the (liquid + liquid) equilibria of the binary mixtures of these PFCs and FILs were studied at atmospheric pressure in a temperature range from T (293.15 to 343.15) K. For these studies, FILs containing ammonium, pyridinium and imidazolium cations and different anions with fluorocarbon alkyl chains between 4 and 8 were included. Additionally, Non-Random Two Liquid (NRTL) thermodynamic model was successfully applied to correlate the behaviour of the PFCs + FILs binary mixtures. Moreover, thermodynamic functions that describe the solvation process were calculated from the experimental data

  4. Organic solvent-free air-assisted liquid-liquid microextraction for optimized extraction of illegal azo-based dyes and their main metabolite from spices, cosmetics and human bio-fluid samples in one step.

    Science.gov (United States)

    Barfi, Behruz; Asghari, Alireza; Rajabi, Maryam; Sabzalian, Sedigheh

    2015-08-15

    Air-assisted liquid-liquid microextraction (AALLME) has unique capabilities to develop as an organic solvent-free and one-step microextraction method, applying ionic-liquids as extraction solvent and avoiding centrifugation step. Herein, a novel and simple eco-friendly method, termed one-step air-assisted liquid-liquid microextraction (OS-AALLME), was developed to extract some illegal azo-based dyes (including Sudan I to IV, and Orange G) from food and cosmetic products. A series of experiments were investigated to achieve the most favorable conditions (including extraction solvent: 77μL of 1-Hexyl-3-methylimidazolium hexafluorophosphate; sample pH 6.3, without salt addition; and extraction cycles: 25 during 100s of sonication) using a central composite design strategy. Under these conditions, limits of detection, linear dynamic ranges, enrichment factors and consumptive indices were in the range of 3.9-84.8ngmL(-1), 0.013-3.1μgmL(-1), 33-39, and 0.13-0.15, respectively. The results showed that -as well as its simplicity, fastness, and use of no hazardous disperser and extraction solvents- OS-AALLME is an enough sensitive and efficient method for the extraction of these dyes from complex matrices. After optimization and validation, OS-AALLME was applied to estimate the concentration of 1-amino-2-naphthol in human bio-fluids as a main reductive metabolite of selected dyes. Levels of 1-amino-2-naphthol in plasma and urinary excretion suggested that this compound may be used as a new potential biomarker of these dyes in human body. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Liquid and solid self-microemulsifying drug delivery systems for improving the oral bioavailability of andrographolide from a crude extract of Andrographis paniculata.

    Science.gov (United States)

    Sermkaew, Namfa; Ketjinda, Wichan; Boonme, Prapaporn; Phadoongsombut, Narubodee; Wiwattanapatapee, Ruedeekorn

    2013-11-20

    The purpose of this study was to develop self-microemulsifying formulations of an Andrographis paniculata extract in liquid and pellet forms for an improved oral delivery of andrographolide. The optimized liquid self-microemulsifying drug delivery system (SMEDDS) was composed of A. paniculata extract (11.1%), Capryol 90 (40%), Cremophor RH 40 (40%) and Labrasol (8.9%). This liquid SMEDDS was further adsorbed onto colloidal silicon dioxide and microcrystalline cellulose, and converted to SMEDDS pellets by the extrusion/spheronization technique. The microemulsion droplet sizes of the liquid and pellet formulations after dilution with water were in the range of 23.4 and 30.3 nm. The in vitro release of andrographolide from the liquid SMEDDS and SMEDDS pellets was 97.64% (SD 1.97%) and 97.74% (SD 3.36%) within 15 min, respectively while the release from the initial extract was only 10%. The oral absorption of andrographolide was determined in rabbits. The C(max) value of andrographolide from the A. paniculata extract liquid SMEDDS and SMEDDS pellet formulations (equivalent to 17.5mg/kg of andrographolide) was 6-fold and 5-fold greater than the value from the initial extract in aqueous suspension (equivalent to 35 mg/kg of andrographolide), respectively. In addition, the AUC(0-12h) was increased 15-fold by the liquid SMEDDS and 13-fold by the SMEDDS pellets compared to the extract in aqueous suspension, respectively. The results clearly indicated that the liquid and solid SMEDDS could be effectively used to improve the dissolution and oral bioavailability that would also enable a reduction in the dose of the poorly water soluble A. paniculata extract. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. Selective Extraction of Organic Contaminants from Soil Using Pressurised Liquid Extraction

    Directory of Open Access Journals (Sweden)

    Rozita Osman

    2013-01-01

    Full Text Available This study focuses on the application of sorbents in pressurised liquid extraction (PLE cell to establish a selective extraction of a variety of organic contaminants (polycyclic aromatic hydrocarbons (PAHs, chlorpyrifos, phenol, pentachlorophenol, and sterols from soil. The selectivity and efficiency of each sorbent depend on the properties of the material, extracting solvent, capacity factor, organic compounds of interest, and PLE operating parameters (temperature, pressure, and extraction time. Several sorbents (silica, alumina, and Florisil were evaluated and with the proper choice of solvents, polar and nonpolar compounds were successfully separated in two fractions. Nonpolar compounds (PAHs, chlorpyrifos, and pentachlorophenol were recovered in the first fraction using a polar sorbent such as Florisil or alumina, and n-hexane as eluting solvent, while more polar compounds (phenol and sterols were recovered in the second fraction using methanol. Silica (5 g was found to be effective for selective extraction with the satisfactory recoveries for all compounds (PAHs from 87.1–96.2%, chlorpyrifos 102.9%, sterols from 93.7–100.5%, phenol 91.9%, and pentachlorophenol 106.2%. The efficiency and precision of this extraction approach and the existing EPA Method 3545 were compared.

  7. Ionic liquids in chemical engineering.

    Science.gov (United States)

    Werner, Sebastian; Haumann, Marco; Wasserscheid, Peter

    2010-01-01

    The development of engineering applications with ionic liquids stretches back to the mid-1990s when the first examples of continuous catalytic processes using ionic liquids and the first studies of ionic liquid-based extractions were published. Ever since, the use of ionic liquids has seen tremendous progress in many fields of chemistry and engineering, and the first commercial applications have been reported. The main driver for ionic liquid engineering applications is to make practical use of their unique property profiles, which are the result of a complex interplay of coulombic, hydrogen bonding and van der Waals interactions. Remarkably, many ionic liquid properties can be tuned in a wide range by structural modifications at their cation and anion. This review highlights specific examples of ionic liquid applications in catalysis and in separation technologies. Additionally, the application of ionic liquids as working fluids in process machines is introduced.

  8. Extraction of metal ions through ligand assisted ionic liquids

    International Nuclear Information System (INIS)

    Kumar, P.; Vincent, T.; Khanna, A.

    2014-01-01

    Extraction of Strontium by crown ether (DCH18C6) has been investigated in [BMIM][TF2N] Ionic Liquid (IL) giving higher extraction ~98% and distribution ratio as compared to other organic solvents (Dodecane, Hexane, & Isodecyl alcohol + Dodecane). Distribution ratio of Sr in IL at 0.15M DCH18C6 indicates an enhancement of 20000, 2000, 500 times over Dodecane, Hexane and 5% Isodecyl Alcohol + 95 % Dodecane at 0.01M aqueous acidity respectively. In presence of IL Sr extraction decreases with increase in HNO 3 concentration in aqueous phase whereas opposite trend was observed with organic solvents. Extraction of Sr initially increases with increase in DCH18C6 concentration in IL, finally reaching an asymptotic constant. Sr can be stripped from the organic phase by precipitating with K 2 SO 4 . (author)

  9. Liquid–liquid extraction of toluene from alkane with pyridinium based ionic liquid ([BPy][NO3] and [HPy][NO3]) at 298.15 K and atmospheric pressure

    International Nuclear Information System (INIS)

    Enayati, Mobin; Mokhtarani, Babak; Sharifi, Ali; Anvari, Sanam; Mirzaei, Mojtaba

    2016-01-01

    Highlights: • Extraction of toluene from alkane with pyridinium based ionic liquid was studied. • The ionic liquids [BPy][NO 3 ] and [HPy][NO 3 ] were used. • The effect of alkane chain length on selectivity of toluene was evaluated. • The effect of alkyl chain length of ionic liquids on toluene selectivity was investigated. • The experimental data were correlated with the NRTL model. - Abstract: The focus of this paper is to study the liquid−liquid extraction process for the separation of toluene from alkane employing the ionic liquids N-butylpyridinium nitrate, [BPy][NO 3 ], and N-hexylpyridinium nitrate, [HPy][NO 3 ], as a new solvents. New experimental data for the ternary systems of {[BPy][NO 3 ] (1) + heptane, or octane, or decane (2) + toluene (3)} and {[HPy][NO 3 ] (1) + heptane, or octane, or decane (2) + toluene (3)} at T = 298.15 K and atmospheric pressure are reported. The Othmer-Tobias and Hand correlation are examined to check the reliability of the experimental LLE data. The toluene distribution ratios and selectivity were calculated form the experimental data. The selectivity values are higher than unity which indicates the ILs, [BPy][NO 3 ] and [HPy][NO 3 ], used in this work are potential solvents to separate toluene from alkane. Besides, the effect of the alkane chain length in the selectivity values was evaluated. In addition, the result of the NRTL thermodynamic modeling shows, the experimental data were satisfactorily correlated.

  10. Trace recovery of uranium and rare earth contained in phosphates by liquid-liquid extraction in sulfuric attack liquor

    International Nuclear Information System (INIS)

    Bousquet, F.; Foraison, D.; Leveque, A.; Sabot, J.L.

    1980-06-01

    Uranium and rare earths can be recovered in sedimentary phosphates during the wet processing of the ore by sulfuric acid giving raw phosphoric acid at 30 per cent of P 2 O 5 . Practically all the uranium contained and only part of rare earths are put into solution in this treatment. Separation of these elements in the phosphoric solution is obtained by liquid-liquid extraction with alkylphosphoric acids and especially with their mono and di esters. Partition isotherms are determined and counter-current tests are effected. Uranium and rare earths reextraction from these solvents can be simultaneous or separate with aqueous solutions alkaline or containing HF or by antisynergism. Pros and cons of each reextraction process are discussed. In conclusion HDEHP or OPPA are recommended because of availability, stability and hydrodynamic, OPPA less selective with rare earths allows the recovery with uranium of ceric earths, yttrium and yttric earths [fr

  11. A microfluidic platform for the rapid determination of distribution coefficients by gravity assisted droplet-based liquid-liquid extraction

    DEFF Research Database (Denmark)

    Poulsen, Carl Esben; Wootton, Robert C. R.; Wolff, Anders

    2015-01-01

    The determination of pharmacokinetic properties of drugs, such as the distribution coefficient, D, is a crucial measurement in pharmaceutical research. Surprisingly, the conventional (gold standard) technique used for D measurements, the shake-flask method, is antiquated and unsuitable...... for the testing of valuable and scarce drug candidates. Herein we present a simple micro fluidic platform for the determination of distribution coefficients using droplet-based liquid-liquid extraction. For simplicity, this platform makes use of gravity to enable phase separation for analysis and is 48 times...... the apparent acid dissociation constant, pK', as a proxy for inter-system comparison. Our platform determines a pK' value of 7.24 ± 0.15, compared to 7.25 ± 0.58 for the shake-flask method in our hands and 7.21 for the shake-flask method in literature. Devices are fabricated using injection moulding, the batch...

  12. Solid-phase extraction followed by dispersive liquid-liquid microextraction for the sensitive determination of ecstasy compounds and amphetamines in biological samples

    Directory of Open Access Journals (Sweden)

    H. A. Mashayekhi

    2014-09-01

    Full Text Available A novel approach for the determination of ecstasy and amphetamines (3,4-methylenedioxymethylamphetamine (MDMA, Ecstasy, 3,4-methylenedioxyamphetamine (MDA, 3,4-methylenedioxyethylamphetamine (MDEA and 3,4-methylenedioxypropylamphetamine (MDPA in biological samples is presented. The analytes were extracted from the matrix and transferred to a small volume of a high density, water insoluble solvent using solid-phase extraction (SPE followed by dispersive liquid-liquid microextraction (DLLME. This combination not only resulted in a high enrichment factor, but also it could be used in complex matrices (biological samples. Some important extraction parameters, such as sample solution flow rate, sample pH, type and volume of extraction and disperser solvents as well as the salt addition, were studied and optimized. Under the optimized conditions, the calibration graphs were linear in the range of 0.5-500 µg L-1 and 1.0-500 µg L-1 with detection limits in the range of 0.1-0.3 µg L-1 and 0.2-0.7 µg L-1 in urine and plasma samples, respectively. The results showed that SPE-DLLME is a suitable method for the determination of ecstasy components and amphetamines in biological and water samples. DOI: http://dx.doi.org/10.4314/bcse.v28i3.3

  13. Evaluation of ionic liquids as solvent for aromatic extraction: Experimental, correlation and COSMO-RS predictions

    International Nuclear Information System (INIS)

    Calvar, Noelia; Domínguez, Irene; Gómez, Elena; Palomar, Jose; Domínguez, Ángeles

    2013-01-01

    Highlights: • BMimMSO 4 and BMimNTf 2 were studied as solvents to extract aromatic from aliphatic hydrocarbons. • Liquid + liquid equilibrium data were measured at 298.15 K and atmospheric pressure. • Selectivity and solute distribution ratio were obtained and compared with literature. • Experimental data were satisfactorily correlated using NRTL and UNIQUAC models. • COSMO-RS model was used as a predictive tool to describe the experimental LLE data for the studied ternary systems. -- Abstract: For the study of the separation of benzene or toluene from octane, nonane and cyclooctane, the ionic liquids 1-butyl-3-methylimidazolium methylsulfate, BMimMSO 4 , and 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide, BMimNTf 2 , were used as solvents. The (liquid + liquid) equilibria of the ternary systems {octane, or nonane, or (cyclooctane + benzene + BMimMSO 4 )}, and {(nonane + toluene + BMimMSO 4 ) or BMimNTf 2 } at T = 298.15 K were determined, and an analysis of the influence of the structure of each compound was carried out. Besides, the experimental data have been compared with literature data with sulfolane as solvent. The experimental results obtained have been correlated using NRTL and UNIQUAC models. Finally, COSMO-RS has been used to predict the (liquid + liquid) equilibrium of the systems studied. The differences between the predicted and experimental values were used to evaluate the ability of the COSMO-RS model to describe the impact of the structure of the alkane, aromatic and ionic liquid on the (liquid + liquid) equilibria

  14. Solid and Liquid Waste Drying Bag

    Science.gov (United States)

    Litwiller, Eric (Inventor); Hogan, John A. (Inventor); Fisher, John W. (Inventor)

    2009-01-01

    Method and system for processing waste from human activities, including solids, liquids and vapors. A fluid-impermeable bag, lined with a liquid-impermeable but vapor-permeable membrane, defining an inner bag, is provided. A vacuum force is provided to extract vapors so that the waste is moved toward a selected region in the inner bag, extracted vapors, including the waste vapors and vaporized portions of the waste liquids are transported across the membrane, and most or all of the solids remain within the liner. Extracted vapors are filtered, and sanitized components thereof are isolated and optionally stored. The solids remaining within the liner are optionally dried and isolated for ultimate disposal.

  15. Influence of ionic liquids on actinides extraction by diphenyl(dibutyl)carbamoylmethylphosphine oxide in different solvents from nitric acid solution

    International Nuclear Information System (INIS)

    Pribylova, G.A.

    2011-01-01

    Influence of ionic liquids (ILs) addition (1-50 wt%) on extraction efficiency of actinides by diphenyl(dibutyl)carbamoylmethylphosphine oxide (Ph 2 Bu 2 ) from 3 M HNO 3 has been studied. Am(III) distribution ratios in two-phase systems 0.1 M Ph 2 Bu 2 in either DCE or CHCl 3 -3 M HNO 3 depending on the nature of additional ionic liquids: imidazolium-based ILs: [C 4 mim][PF 6 ], [C 4 mim][BF 4 ] and phosphonium-based ILs: PPF 6 , PBF 4 and PCl were determined. The highest value of Am(III) extraction ratio change (1040) was found on addition of PPF 6 to Ph 2 Bu 2 in CHCl 3 . Extraction of Pu(IV) and U(VI) by 0.001 M Ph 2 Bu 2 in the presence of [C 4 mim][PF 6 ] in DCE, CHCl 3 or meta-nitrobenzotrifluoride (NBTF) have been investigated. The greatest enhancement of extraction efficiency was observed using CHCl 3 , the least polar studied solvent. Using a mixture of conventional solvent and ionic liquid as a solvent for extractant enables one to increase distribution ratios and reduce viscosity of organic phase as compared with ionic liquid viscosity. The marked increase of Am(III), Pu(IV) and U(VI) extraction extent by Ph 2 Bu 2 on addition of ionic liquids to the extent of 10 wt% permit one essentially to diminish amounts considerably more expensive carbamoylmethylphosphine oxide(the general name is CMPO) used in TRUEX process. (author)

  16. Extraction of butan-1-ol from water with ionic liquids at T = 308.15 K

    International Nuclear Information System (INIS)

    Domańska, Urszula; Królikowski, Marek

    2012-01-01

    Highlights: ► The LLE ternary phase diagrams with ionic liquids were measured. ► Separation of butan-1-ol/water system with tetracyanoborate-based ILs. ► Low solubility of water in [P 14,6,6,6 ][TCB] was observed. ► [P 14,6,6,6 ][TCB] is proposed for possible use in separation of butan-1-ol from aqueous phase. - Abstract: Ionic liquids (ILs) are novel green solvents that can be proposed for removing butan-1-ol from the aqueous fermentation media. Ternary (liquid + liquid) equilibrium data are presented for {ionic liquid (1) + butan-1-ol (2) + water (3)} at T = 308.15 K and ambient pressure to analyze the performance of the ionic liquid (IL) in the extraction of butan-1-ol from aqueous phase. The tetracyanoborate-based ILs have been studied: 1-hexyl-3-methylimidazolium tetracyanoborate, ([HMIM][TCB]), 1-decyl-3-methylimidazolium tetracyanoborate, ([DMIM][TCB]) and trihexyltetradecylphosphonium tetracyanoborate, ([P 14,6,6,6 ][TCB]). The results are discussed in terms of the selectivity and distribution ratio of separation of related systems. The complete miscibility in the binary liquid systems of butan-1-ol with all used ILs was observed. The imidazolium cation in comparison with phosphonium cation shows lower selectivity and distribution ratio. The IL with the longer alkyl chain at the cation shows higher selectivity and distribution ratio in this process. The non-random two liquid NRTL model was used successfully to correlate the experimental tie-lines and to calculate the phase composition error in mole fraction in the ternary systems. The average root mean square deviation (RMSD) of the phase composition was 0.0027. The data presented here indicates the usefulness of [P 14,6,6,6 ][TCB] as a solvent for the separation of butan-1-ol from water using solvent extraction. The density of [P 14,6,6,6 ][TCB] was measured as a function of temperature.

  17. Experimental and Model Studies on Continuous Separation of 2-Phenylpropionic Acid Enantiomers by Enantioselective Liquid-Liquid Extraction in Centrifugal Contactor Separators.

    Science.gov (United States)

    Feng, Xiaofeng; Tang, Kewen; Zhang, Pangliang; Yin, Shuangfeng

    2016-03-01

    Multistage enantioselective liquid-liquid extraction (ELLE) of 2-phenylpropionic acid (2-PPA) enantiomers using hydroxypropyl-β-cyclodextrin (HP-β-CD) as extractant was studied experimentally in a counter-current cascade of centrifugal contactor separators (CCSs). Performance of the process was evaluated by purity (enantiomeric excess, ee) and yield (Y). A multistage equilibrium model was established on the basis of single-stage model for chiral extraction of 2-PPA enantiomers and the law of mass conservation. A series of experiments on the extract phase/washing phase ratio (W/O ratio), extractant concentration, the pH value of aqueous phase, and the number of stages was conducted to verify the multistage equilibrium model. It was found that model predictions were in good agreement with the experimental results. The model was applied to predict and optimize the symmetrical separation of 2-PPA enantiomers. The optimal conditions for symmetric separation involves a W/O ratio of 0.6, pH of 2.5, and HP-β-CD concentration of 0.1 mol L(-1) at a temperature of 278 K, where eeeq (equal enantiomeric excess) can reach up to 37% and Yeq (equal yield) to 69%. By simulation and optimization, the minimum number of stages was evaluated at 98 and 106 for eeeq > 95% and eeeq > 97%. © 2016 Wiley Periodicals, Inc.

  18. Development of a surfactant liquid membrane extraction process for the cleansing of industrial aqueous effluents containing metallic cation traces

    International Nuclear Information System (INIS)

    Rapaumbya Akaye, Guy-Roland

    1994-01-01

    The purpose of this work was to develop a process of surfactant liquid membrane extraction to purify industrial waste solution containing Cu(II), Fe(III), and Zn(II) (about 0,1 g/L). The extractant is the ammonium salt of Cyanex 306 and Aliquat 336. The first part of this work deals with the study of the liquid-liquid extraction of the metals. The efficiency of the extractant has been shown for the extraction of each metal alone and for Cu(II) and Zn(II) in the case of a mixture of the three metals. During this study we have observed that Fe(III) is reduced to Fe(II) (which is not extracted by the salt of Cyanex 301) in presence of Cu(II) and the quaternary ammonium salt (Aliquat 336). The optimisation of the experimental conditions for the discontinuous surfactant liquid membrane process led us to choose the following composition of the emulsion: 1,5 % of Cyanex 301 salt, 2,5 % of ECA 4360, dodecan. The internal phase is an aqueous solution containing 3,5 mol/L of NaOH and 0,5 mol/L tri-ethanolamin The residual concentration of Cu(II) and Zn(II) in the external phase is very low. In the case of iron, only 60 % are extracted because of the reduction phenomenon (10 % in liquid-liquid extraction). The realisation of the continuous process in pulsed column, after optimisation of hydrodynamics conditions, leads to similar results. In stationary conditions, we obtain a raffinate containing less than 0,5 mg/L of Cu(II) and Zn(II) and 36 mg/L of iron. The internal phase contains about 2 g/L of Cu(II) an Zn(II). We tried and minimize the reduction of Fe(III) in surfactant liquid membrane process. Less than 16 % of iron cannot be reduced. This leads to a purification of only 84 % In the basis of these results, processes of purification have been proposed for effluents of various composition. They enable to purify the effluent and besides to concentrate the pollutants about twenty times. (author) [fr

  19. Headspace solid-phase microextraction (HS-SPME) and liquid-liquid extraction (LLE): comparison of the performance in classification of ecstasy tablets. Part 2.

    Science.gov (United States)

    Bonadio, Federica; Margot, Pierre; Delémont, Olivier; Esseiva, Pierre

    2008-11-20

    Headspace solid-phase microextraction (HS-SPME) is assessed as an alternative to liquid-liquid extraction (LLE) currently used for 3,4-methylenedioxymethampethamine (MDMA) profiling. Both methods were compared evaluating their performance in discriminating and classifying samples. For this purpose 62 different seizures were analysed using both extraction techniques followed by gas chromatography-mass spectroscopy (GC-MS). A previously validated method provided data for HS-SPME, whereas LLE data were collected applying a harmonized methodology developed and used in the European project CHAMP. After suitable pre-treatment, similarities between sample pairs were studied using the Pearson correlation. Both methods enable to distinguish between samples coming from the same pre-tabletting batches and samples coming from different pre-tabletting batches. This finding emphasizes the use of HS-SPME as an effective alternative to LLE, with additional advantages such as sample preparation and a solvent-free process.

  20. Studies on Three Liquid Phase Extraction (TLPE) system for separation of rare earths

    International Nuclear Information System (INIS)

    Yadav, Kartikey K.; Singh, D.K.; Anitha, M.; Singh, H.

    2014-01-01

    Three-liquid-phase extraction (TLPE) is relatively a new separation technique, which takes the advantage of the differences in physicochemical properties of three coexisted phases to achieve multi-phase liquid separation of two or more components in one-step extraction. TLPE system consists of three liquid layers namely an organic solvent phase (organophosphorous type) and two aqueous phases one rich in polymer phase (poly alkylene glycol) and other a salt solution. To study the feasibility of using such system for separation of rare earths, it is important to optimize the preparatory conditions by selective suitable polymer and salt solutions at an appropriate pH to obtain a stable three phase layers to effect the separation. D2EHPA (di-2-ethyl hexyl phosphoric acid) is a well- established extractant in the rare earth industry and has been chosen in the present work to form a TLPE with polymer and salt solution. In the present investigation after preparing the stable three phase, the feasibility of using TLPE has been examined to separate rare earths from a multicomponent solutions. This study has demonstrated the ability of TLPE having D2EHPA as organic phase to separate rare earths from a multicomponent system. Effect of pH, concentration and types of polymer, complexing agent and D2EHPA concentration has been studied. Variation in pH study indicated that 4.0 leads to extraction of rare earths in the polymer phase. PEG 600 was found to be best amongst the polymer investigated. Presence of DTPA as complexing agent in the salt solution having pH >4.0 resulted in enhanced extraction of rare earths in PEG phase

  1. Recent developments in the extraction separation method for treatment of high-level liquid waste

    International Nuclear Information System (INIS)

    Jiao Rongzhou; Song Chongli; Zhu Yongjun

    2000-01-01

    A description and review of the recent developments in the extraction separation method for partitioning transuranium elements from high-level liquid waste (HLLW) is presented. The extraction separation processes such as TRUEX process, DIAMEX process, DIDPA process, CTH process, TRPO process are briefly discussed

  2. Contacting gases and liquids

    International Nuclear Information System (INIS)

    Robinson, L.F.; Cahalan, M.J.

    1980-01-01

    A process is described for contacting substantially immiscible phases to transfer material from one phase to another, which comprises passing the phases through a contactor, while causing portions of at least one phase to be repeatedly passed through at least one other phase. One phase in the contactor is gaseous, and another liquid. A further phase can be liquid or solid The process may be used for extracting impurities from china clay, or extracting uranium values from ore with oxygen gas acting to oxidise the uranium. (author)

  3. Ionic liquid and aqueous two-phase extraction based on salting-out coupled with high-performance liquid chromatography for the determination of seven rare ginsenosides in Xue-Sai-Tong injection.

    Science.gov (United States)

    Li, Lan-Jie; Jin, Yong-Ri; Wang, Xiao-Zhong; Liu, Ying; Wu, Qian; Shi, Xiao-Lei; Li, Xu-Wen

    2015-09-01

    A method of ionic liquid salt aqueous two-phase extraction coupled with high-performance liquid chromatography has been developed for the analysis of seven rare ginsenosides including Rg6 , F4 , 20(S)-Rg3 , 20(R)-Rg3 , Rk3 , Rk1 , and Rg5 in Xue-Sai-Tong injection. The injection was mixed with ionic liquid 1-butyl-3-methylimidazolium bromide aqueous solution, and a mixture was obtained. With the addition of sodium dodecyl sulfate and dipotassium phosphate into the mixture, the aqueous two-phase mixture was formed after ultrasonic treatment and centrifuged. Rare ginsenosides were extracted into the upper phase. To obtain a high extraction factors, various influences were considered systematically, such as the volume of ionic liquid, the category and amount of salts, the amount of sodium dodecyl sulfate, the pH value of system, and the time of ultrasonic treatment. Under the optimal condition, rare ginsenosides in Xue-Sai-Tong injection were enriched and detected, the recoveries of seven rare ginsenosides ranged from 90.05 to 112.55%, while relative standard deviations were lower than 2.50%. The developed method was reliable, rapid and sensitive for the determination of seven rare ginsenosides in the injections. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Optimization of Pressurized Liquid Extraction of Three Major Acetophenones from Cynanchum bungei Using a Box-Behnken Design

    Science.gov (United States)

    Li, Wei; Zhao, Li-Chun; Sun, Yin-Shi; Lei, Feng-Jie; Wang, Zi; Gui, Xiong-Bin; Wang, Hui

    2012-01-01

    In this work, pressurized liquid extraction (PLE) of three acetophenones (4-hydroxyacetophenone, baishouwubenzophenone, and 2,4-dihydroxyacetophenone) from Cynanchum bungei (ACB) were investigated. The optimal conditions for extraction of ACB were obtained using a Box-Behnken design, consisting of 17 experimental points, as follows: Ethanol (100%) as the extraction solvent at a temperature of 120 °C and an extraction pressure of 1500 psi, using one extraction cycle with a static extraction time of 17 min. The extracted samples were analyzed by high-performance liquid chromatography using an UV detector. Under this optimal condition, the experimental values agreed with the predicted values by analysis of variance. The ACB extraction yield with optimal PLE was higher than that obtained by soxhlet extraction and heat-reflux extraction methods. The results suggest that the PLE method provides a good alternative for acetophenone extraction. PMID:23203079

  5. Optimization of Pressurized Liquid Extraction of Three Major Acetophenones from Cynanchum bungei Using a Box-Behnken Design

    Directory of Open Access Journals (Sweden)

    Hui Wang

    2012-11-01

    Full Text Available In this work, pressurized liquid extraction (PLE of three acetophenones (4-hydroxyacetophenone, baishouwubenzophenone, and 2,4-dihydroxyacetophenone from Cynanchum bungei (ACB were investigated. The optimal conditions for extraction of ACB were obtained using a Box-Behnken design, consisting of 17 experimental points, as follows: Ethanol (100% as the extraction solvent at a temperature of 120 °C and an extraction pressure of 1500 psi, using one extraction cycle with a static extraction time of 17 min. The extracted samples were analyzed by high-performance liquid chromatography using an UV detector. Under this optimal condition, the experimental values agreed with the predicted values by analysis of variance. The ACB extraction yield with optimal PLE was higher than that obtained by soxhlet extraction and heat-reflux extraction methods. The results suggest that the PLE method provides a good alternative for acetophenone extraction.

  6. Determination of flumequine and oxolinic acid in sediments and soils by microwave-assisted extraction and liquid chromatography-fluorescence

    International Nuclear Information System (INIS)

    Prat, M.D.; Ramil, D.; Compano, R.; Hernandez-Arteseros, J.A.; Granados, M.

    2006-01-01

    A method is reported for the determination of the quinolones oxolinic acid and flumequine in aquatic sediments and agricultural soils. The analytes are extracted by liquid-liquid partitioning between a sample homogenated in an aqueous buffer solution and dichloromethane. Microwave-assisted extraction (MAE) was tested to improve the speed and efficiency of the extraction process. The parameters affecting the efficiency of MAE, such as irradiation time and temperature, were studied. The clean-up consists of back-extraction in 1 M sodium hydroxide. The determination is carried out by reversed phase liquid chromatography on an octyl silica-based column and fluorimetric detection. The optimised method was applied to the analysis of two sediments and one agricultural soil spiked with the analytes. The absolute recovery rates for the whole process range from 79% to 94% (RSD 3-7%), and detection limits are in the low μg kg -1 level

  7. Ionic Liquid Dispersive Liquid-Liquid Microextraction Method for the Determination of Irinotecan, an Anticancer Drug, in Water and Urine Samples Using UV-Vis Spectrophotometry.

    Science.gov (United States)

    Uysal, Deniz; Karadaş, Cennet; Kara, Derya

    2017-05-01

    A new, simple, efficient, and environmentally friendly ionic liquid dispersive liquid-liquid microextraction method was developed for the determination of irinotecan, an anticancer drug, in water and urine samples using UV-Vis spectrophotometry. The ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate was used as the extraction solvent, and ethanol was used as the disperser solvent. The main parameters affecting the extraction efficiency, including sample pH, volume of the ionic liquid, choice of the dispersive solvent and its volume, concentration of NaCl, and extraction and centrifugation times, were investigated and optimized. The effect of interfering species on the recovery of irinotecan was also examined. Under optimal conditions, the LOD (3σ) was 48.7 μg/L without any preconcentration. Because the urine sample was diluted 10-fold, the LOD for urine would be 487 μg/L. However, this could be improved 16-fold if preconcentration using a 40 mL aliquot of the sample is used. The proposed method was successfully applied to the determination of irinotecan in tap water, river water, and urine samples spiked with 10.20 mg/L for the water samples and 8.32 mg/L for the urine sample. The average recovery values of irinotecan determined were 99.1% for tap water, 109.4% for river water, and 96.1% for urine.

  8. Magnetic graphene oxide modified by imidazole-based ionic liquids for the magnetic-based solid-phase extraction of polysaccharides from brown alga.

    Science.gov (United States)

    Wang, Xiaoqin; Li, Guizhen; Row, Kyung Ho

    2017-08-01

    Magnetic graphene oxide was modified by four imidazole-based ionic liquids to synthesize materials for the extraction of polysaccharides by magnetic solid-phase extraction. Fucoidan and laminarin were chosen as the representative polysaccharides owing to their excellent pharmaceutical value and availability. Fourier transform infrared spectroscopy, field-emission scanning electron microscopy, and thermogravimetric analysis were applied to characterize the synthesized materials. Single-factor experiments showed that the extraction efficiency of polysaccharides was affected by the amount of ionic liquids for modification, solid-liquid ratio of brown alga and ethanol, the stirring time of brown alga and ionic liquid-modified magnetic graphene oxide materials, and amount of 1-(3-aminopropyl)imidazole chloride modified magnetic graphene oxide materials added to the brown alga sample solution. The results indicated that 1-(3-aminopropyl)imidazole chloride modified magnetic graphene oxide possessed better extraction ability than graphene oxide, magnetic graphene oxide, and other three ionic-liquid-modified magnetic graphene oxide materials. The highest extraction recoveries of fucoidan and laminarin extracted by 1-(3-aminopropyl)imidazole chloride modified magnetic graphene oxide were 93.3 and 87.2%, respectively. In addition, solid materials could be separated and reused easily owing to their magnetic properties. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Liquid phase micro-extraction: Towards the green methodology for ultratrace metals determination in aquatic ecosystems

    Directory of Open Access Journals (Sweden)

    López-López J. A.

    2013-04-01

    Full Text Available Heavy metals are normally found, in natural waters, in very low concentrations. Some of them are essential for life in low level; however, in higher level they are toxic. Therefore, analyzing their bio-available fraction is of main interest. Standard methodology is based in the collection of a number of samples from a water body. Collected samples must be stored, pre-treated and then analyzed. Pre-treatment usually involves pre-concentrating the metal, with the corresponding risk of contamination or loss of analyte. This way, punctual information is obtained from every sampling campaign. As an alternative, passive sampling techniques allow the continuous and coupled sampling-pre-treatment for heavy metals analysis, giving a better approach in the characterization of the studied water body. Liquid phase micro-extraction (LPME is a green analytical alternative for liquid-liquid extraction that promotes a reduction of sample volume, solvent needed and waste generation. Using these systems, polypropylene hollow fibers (HF with pores in their walls can be used. A few micro-liters of organic solvent are supported in the pores. The sample is placed in the outer part of the fiber and a receiving phase is placed in its inner part, allowing continuous liquid extraction of the metal from the sample. Several fibers with different physical features have been employed to analyzed total concentration and bio-availability of some heavy metals (Ag, Ni, Cu in natural water samples. Thanks to fibers configuration, devices for passive sampling based in HF-LPME could be designed. Advantages of this methodology over existing ones are supported because the receiving phase is liquid. As a consequence, retained metals do not need to be eluted from the acceptor prior to instrumental analysis.

  10. Determination of phthalate esters in distillates by ultrasound-vortex-assisted dispersive liquid-liquid micro-extraction (USVADLLME) coupled with gas chromatography/mass spectrometry.

    Science.gov (United States)

    Montevecchi, Giuseppe; Masino, Francesca; Zanasi, Luca; Antonelli, Andrea

    2017-04-15

    A method for the extraction of phthalate esters (PAEs) by Ultrasound-Vortex-Assisted Dispersive Liquid-Liquid Micro-Extraction (USVADLLME) approach was optimised and applied for the first time to a historical series of brandies. These contaminants are widely spread in the environment as a consequence of about half century of use in different fields of applications. The concern about these substances and the recent legal restrictions of China in distillates import need a quick and sensitive method for their quantification. The proposed method, moreover, is environmentally oriented due to the disposal of micro-quantities of solvent required. In fact, sub-ppm-limits of detection were achieved with a solvent volume as low as 160μL. The analysed samples were within the legal limits, except for some very ancient brandies whose contamination was probably due to a PAEs concentration effect as a consequence of long ageing and for the use of plastic pipelines no more operative. Copyright © 2016 Elsevier Ltd. All rights reserved.

  11. Separation by liquid-liquid extraction of actinides(III) from lanthanides(III) using new molecules: the picolinamides; Separation par extraction liquide-liquide des actinides(III) des lanthanides(III) par de nouvelles molecules: les picolinamides

    Energy Technology Data Exchange (ETDEWEB)

    Cordier, P Y [CEA Marcoule, Departement de Recherche en Retraitement et en Vitrification, 30 - Bagnols-sur-Ceze (France); [Clermont-Ferrand-2 Univ., 63 - Aubiere (France)

    1996-07-01

    In the field of long-lived radionuclides separation from waste generated during spent fuel reprocessing, the picolinamides have been chosen as potential extractants for the selective extraction of actinides (III) from lanthanides (III). The first studies initiated on the most simple molecule of the picolinamide family, namely 2-pyridinecarboxamide, pointed out that in an aqueous media the complexation stability constant between this ligand and Am(III) is roughly 10 times higher than the ones corresponding to Ln(III). The synthesis of lipophilic derivatives of 2-pyridinecarboxamide leaded to extraction experiments. The extraction of metallic cation by lipophilic picolinamides, according to a solvatation mechanism, is strongly dependent on the nature of the amide function: a primary amide function (group I) leads to a good extraction; on the contrary, there is a decrease for secondary (group II) and tertiary (group III) amide functions. From a theoretical point of view, this work leads finally to the following conclusions: confirmation of the importance of the presence of soft donor atoms within the extractants (nitrogen in our case) for An(III)/Ln(III). Also, sensitivity of this soft donor atom regarding the protonation reaction; prevalence in our case of the affinity of the extractant for the metallic cation over the lipophilia of the extractant to ensure good distribution coefficients. The extraction and Am(III)/Ln(III) separation performances of the picolinamides from pertechnetic media leads to the design of a possible flowsheet for the reprocessing of high level liquid waste, with the new idea of an integrated technetium reflux. (author) 105 refs.

  12. Ionic liquid based vortex assisted liquid-liquid microextraction combined with liquid chromatography mass spectrometry for the determination of bisphenols in thermal papers with the aid of response surface methodology.

    Science.gov (United States)

    Asati, Ankita; Satyanarayana, G N V; Panchal, Smita; Thakur, Ravindra Singh; Ansari, Nasreen G; Patel, Devendra K

    2017-08-04

    A sensitive, rapid and efficient ionic liquid-based vortex assisted liquid-liquid microextraction (IL-VALLME) with Liquid Chromatography Mass spectrometry (LC-MS/MS) method is proposed for the determination of bisphenols in thermal paper. Extraction factors were systematically optimized by response surface methodology. Experimental factors showing significant effects on the analytical responses were evaluated using design of experiment. The limit of detection for Bisphenol-A (BPA) and Bisphenol-S (BPS) in thermal paper were 1.25 and 0.93μgkg -1 respectively. The dynamic linearity range for BPA was between 4 and 100μgkg -1 and the determination of coefficient (R 2 ) was 0.996. The values of the same parameters were 3-100μgkg -1 and 0.998 for BPS. The extraction recoveries of BPA and BPS in thermal paper were 101% and 99%. Percent relative standard deviation (% RSD) for matrix effect and matrix match effects were not more than 10%, for both bisphenols. The proposed method uses a statistical approach for the analysis of bisphenols in environmental samples, and is easy, rapid, requires minimum organic solvents and efficient. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Extraction of triazole fungicides in environmental waters utilizing poly (ionic liquid)-functionalized magnetic adsorbent.

    Science.gov (United States)

    Liu, Cheng; Liao, Yingmin; Huang, Xiaojia

    2017-11-17

    This work prepared a new poly (ionic liquid)-functionalized magnetic adsorbent (PFMA) for the extraction of triazole fungicides (TFs) in environmental waters prior to determination by high performance liquid chromatography/diode array detection (HPLC-DAD). A polymerizable ionic liquid, 1-methyl-3-allylimidazolium bis(trifluoromethylsulfonyl)imide was employed to copolymerize with divinylbenzene on the surface of modified magnetite to fabricate the PFMA. The morphology, spectroscopic and magnetic properties of the new adsorbent were investigated by different techniques. A series of key parameters that influence the extraction performance including the amount of PFMA, desorption solvent, adsorption and desorption time, sample pH value and ionic strength were optimized in detail. Under the optimum conditions, the prepared PFMA could extract targeted TFs effectively and quickly under the format of magnetic solid-phase extraction (MSPE). Satisfactory linearities were achieved in the range of 0.1-200.0μg/L for triadimenol and 0.05-200.0μg/L for other TFs with good coefficients of determination above 0.99 for all analytes. The limits of detection (S/N=3) and limits of quantification (S/N=10) for TFs were in the range of 0.0050-0.0078μg/L and 0.017-0.026μg/L, respectively. Environmental waters including lake, river and well waters were used to demonstrate the applicability of developed MSPE-HPLC-DAD method, and satisfactory recoveries and repeatability were obtained. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. In situ liquid-liquid extraction as a sample preparation method for matrix-assisted laser desorption/ionization MS analysis of polypeptide mixtures

    DEFF Research Database (Denmark)

    Kjellström, Sven; Jensen, Ole Nørregaard

    2003-01-01

    A novel liquid-liquid extraction (LLE) procedure was investigated for preparation of peptide and protein samples for matrix-assisted laser desorption/ionization mass spectrometry (MALDI MS). LLE using ethyl acetate as the water-immiscible organic solvent enabled segregation of hydrophobic...... matrix to the organic solvent enhanced the efficiency of the LLE-MALDI MS method for analysis of hydrophobic peptides and proteins. LLE-MALDI MS enabled the detection of the hydrophobic membrane protein bacteriorhodopsin as a component in a simple protein mixture. Peptide mixtures containing...... phosphorylated, glycosylated, or acylated peptides were successfully separated and analyzed by the in situ LLE-MALDI MS technique and demonstrate the potential of this method for enhanced separation and structural analysis of posttranslationally modified peptides in proteomics research....

  15. Multiclass method for the determination of pharmaceuticals and personal care products in compost from sewage sludge using ultrasound and salt-assisted liquid-liquid extraction followed by ultrahigh performance liquid chromatography-tandem mass spectrometry analysis.

    Science.gov (United States)

    Luque-Muñoz, A; Vílchez, J L; Zafra-Gómez, A

    2017-07-21

    An analytical method for the analysis of 16 pharmaceuticals and personal care products in compost from sewage sludge is successfully validated. Ultrasound assisted extraction with a mixture of acetonitrile:ethyl acetate (1:1, v/v) containing 10% (v/v) of acetic acid was carried out. Two cycles of extraction of 10min were applied. A clean-up of the extracts using salt-assisted liquid-liquid extraction (SALLE) was also included. Experimental design was used for the optimization of the main parameters involved in the extraction and cleaned-up steps. The chromatographic separation was carried out by ultrahigh performance liquid chromatography using a mobile phase gradient mixture of a 13mM buffer ammonium formate solution (pH 9.25) (solvent A) and methanol (solvent B). An ACQUITY UPLC ® BEH C18 column (1.7μm; 2.1×50mm) column was used. Analytes were separated in less than 11min. The compounds were detected and quantified using single reaction monitoring electrospray tandem mass spectrometry. The limits of detection calculated ranged from 0.5 to 4ngg -1 d.w., and the limits of quantification from 2 to 13ngg -1 d.w. Recoveries from 93% to 111%, with relative standar deviations lower than 11% in all cases, were obtained. The method was applied to natural compost samples. High concentrations of some analytes were found. Ketoprofen (510ngg -1 d.w.), methylparaben (240ngg -1 d.w.), diclofenac (175ngg -1 d.w.) and flufenamic acid (128ngg -1 d.w.) were the most abundant. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Sensitive determination of estrogens in environmental waters treated with polymeric ionic liquid-based stir cake sorptive extraction and liquid chromatographic analysis.

    Science.gov (United States)

    Chen, Lei; Mei, Meng; Huang, Xiaojia; Yuan, Dongxing

    2016-05-15

    A simple, sensitive and environmentally friendly method using polymeric ionic liquid-based stir cake sorptive extraction followed by high performance liquid chromatography with diode array detection (HPLC/DAD) has been developed for efficient quantification of six selected estrogens in environmental waters. To extract trace estrogens effectively, a poly (1-ally-3-vinylimidazolium chloride-co-ethylene dimethacrylate) monolithic cake was prepared and used as the sorbent of stir cake sorptive extraction (SCSE). The effects of preparation conditions of sorbent and extraction parameters of SCSE for estrogens were investigated and optimized. Under optimal conditions, the developed method showed satisfactory analytical performance for targeted analytes. Low limits of detection (S/N=3) and quantification limits (S/N=10) were achieved within the range of 0.024-0.057 µg/L and 0.08-0.19 µg/L, respectively. Good linearity of method was obtained for analytes with the correlation coefficients (R(2)) above 0.99. At the same time, satisfactory method repeatability and reproducibility was achieved in terms of intra- and inter-day precisions, respectively. Finally, the established SCSE-HPLC/DAD method was successfully applied for the determination of estrogens in different environmental water samples. Recoveries obtained for the determination of estrogens in spiked samples ranged from 71.2% to 108%, with RSDs below 10% in all cases. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. Double-phase liquid membrane extraction for the analysis of pesticides

    International Nuclear Information System (INIS)

    Mohd Marsin Sanagi; Nurul Auni Zainal Abidin; Heng, See Hong; Wan Aini Wan Ibrahim

    2008-01-01

    A simple and solvent minimized sample preparation technique based on two-phase hollow fiber-protected liquid-phase micro extraction was investigated for HPLC analysis of selected pesticides in water samples. Four pesticides (procymidon, methidathion, quinalphos, and vinclozolin) were considered as target analysts. Parameters such as extraction solvent, salt concentration, stirring speed, extraction time, and pH value were optimized using spiked deionised water samples. The analysts were extracted from 12 mL water samples through organic solvent (n-hexane and isooctane) immobilized in the pores of a porous polypropylene hollow fiber into 50 μL acceptor phase present inside the hollow fiber. Excellent separations of analytes were obtained on C18 column using acetonitrile-water ratio of 55:45 v/v at elevated flow rate of 0.8 mL/ min. (author)

  18. Application of salting-out effect equation to modelling of liquid-liquid distribution systems

    International Nuclear Information System (INIS)

    Pitsch, H.K.

    1986-03-01

    Physicochemical interpretation of salting-out is reviewed and effects of the medium on liquid-liquid distribution equilibria are described by two non-specific parameters of salting-out agents: total concentration of species in the aqueous phase and water activity. Thus extraction of a given constituent in various media can be forecasted with few data. Different uranyl and technetium (VII) extraction systems are analyzed to show the potentiality of the method. Coextraction of nitric acid and uranyl nitrate by tributyl phosphate is used to show the possibility of modelling complex distribution systems in industrial conditions [fr

  19. Recovery of salicylic acid from aqueous solution by solvent extraction and supported liquid membrane using TOMAC as carrier

    International Nuclear Information System (INIS)

    Kouki, Noura; Tayeb, Rafik; Dhahbi, Mahmoud

    2009-01-01

    Conventional sewage treatment plants do not fully degrade residues of pharmaceuticals, so that they are introduced into the aquatic environment. On this basis, the demand for the development of efficient systems for removing these compounds from water has assumed a great research interest. Membrane operations are increasingly employed in many industrial sectors as important alternative technologies to the classical processes of separation. Among membrane-based separation processes, the use of supported liquid membranes (SLMs) has received growing attention during recent years. In our work we had tried to recover a pharmaceutical product, salicylic acid (S.A), from an aqueous solution by solvent extraction and supported liquid membrane using an ionic liquid: the tri octylmethylammonium chloride (TOMAC) as carrier. Ionic liquids has been revealed as interesting clean alternatives to classical solvents and their use as a liquid phase results in the stabilization of the SLMs duo to their negligible vapour pressure, the possibility of minimising their solubility in the surrounding phases by adequate selection of the cation and anion, and the greater capillary force associated with their high viscosity. For this reason we had studied the influence of different parameters which could affect the efficiency of the transport: pH of the feed phase, the nature of the strippant, the concentration of the strippant, the nature of the support and the initial concentration of the salicylic acid in the feed phase. We had noticed that the pH of the feed solution had no effect of the percentage extraction and after 24 hours we can extract completely our solute. TOMAC seemed to be a good extractant but we found difficult to strip salicylic acid from the TOMAC phase and this could be related to the formation of water micro environments in the ionic liquid membrane.

  20. In-situ ionic liquid dispersive liquid-liquid microextraction using a new anion-exchange reagent combined Fe3O4 magnetic nanoparticles for determination of pyrethroid pesticides in water samples.

    Science.gov (United States)

    Fan, Chen; Liang, You; Dong, Hongqiang; Ding, Guanglong; Zhang, Wenbing; Tang, Gang; Yang, Jiale; Kong, Dandan; Wang, Deng; Cao, Yongsong

    2017-07-04

    In this work, in-situ ionic liquid dispersive liquid-liquid microextraction combined ultrasmall Fe 3 O 4 magnetic nanoparticles was developed as a kind of pretreatment method to detect pyrethroid pesticides in water samples. New anion-exchange reagents including Na[DDTC] and Na[N(CN) 2 ] were optimized for in-situ extraction pyrethroids, which showed enhanced microextraction performance. Pyrethroids were enriched by hydrophilic ionic liquid [P 4448 ][Br] (aqueous solution, 200 μL, 0.2 mmol mL -1 ) reaction in-situ with anion-exchange reagent Na[N(CN) 2 ] (aqueous solution, 300 μL, 0.2 mmol mL -1 ) forming hydrophobic ionic liquid as extraction agent in water sample (10 mL). Ultrasmall superparamagnetic iron oxide nanoparticles (30 mg) were used to collect the mixture of ionic liquid and pyrethroids followed by elution with acetonitrile. The extraction of ionic liquid strategies was unique and efficiently fulfilled with high enrichment factors (176-213) and good recoveries (80.20-117.31%). The method was successively applied to the determination of pyrethroid pesticides in different kinds of water samples with the limits of detection ranged from 0.16 to 0.21 μg L -1 . The proposed method is actually nanometer-level microextraction (average size 80 nm) with the advantages of simplicity, rapidity, and sensitivity. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Polonium-210 assay using a background-rejecting extractive liquid-scintillation method

    International Nuclear Information System (INIS)

    Case, C.N.; McDowell, W.J.

    1981-01-01

    This paper describes a procedure which combines solvent extraction with alpha liquid scintillation spectrometry. Pulse shape discrimination electronics are used to reject beta and gamma pulses and to lower the background count to acceptable levels. Concentration of 210 Po and separation from interferring elements are accomplished using a H 3 Po 4 -HCl solution with TOPO combined with a scintillor in toluene

  2. PREFACE: Functionalized Liquid Liquid Interfaces

    Science.gov (United States)

    Girault, Hubert; Kornyshev, Alexei A.; Monroe, Charles W.; Urbakh, Michael

    2007-09-01

    Most natural processes take place at interfaces. For this reason, surface science has been a focal point of modern research. At solid-liquid interfaces one can induce various species to adsorb or react, and thus may study interactions between the substrate and adsorbates, kinetic processes, optical properties, etc. Liquid-liquid interfaces, formed by immiscible liquids such as water and oil, have a number of distinctive features. Both sides of the interface are amenable to detailed physical and chemical analysis. By chemical or electrochemical means, metal or semiconductor nanoparticles can be formed or localised at the interface. Surfactants can be used to tailor surface properties, and also to place organic molecular or supermolecular constructions at the boundary between the liquids. Electric fields can be used to drive ions from one fluid to another, or even change the shape of the interface itself. In many cases, both liquids are optically transparent, making functionalized liquid-liquid interfaces promising for various optical applications based on the transmission or reflection of light. An advantage common to most of these systems is self-assembly; because a liquid-liquid interface is not mechanically constrained like a solid-liquid interface, it can easily access its most stable state, even after it has been driven far from equilibrium. This special issue focuses on four modes of liquid-liquid interfacial functionalization: the controlled adsorption of molecules or nanoparticles, the formation of adlayers or films, electrowetting, and ion transfer or interface-localized reactions. Interfacial adsorption can be driven electrically, chemically, or mechanically. The liquid-liquid interface can be used to study how anisotropic particles orient at a surface under the influence of a field, how surfactants interact with other adsorbates, and how nanoparticles aggregate; the transparency of the interface also makes the chirality of organic adsorbates amenable to

  3. Continuous extraction of molten chloride salts with liquid cadmium alloys

    International Nuclear Information System (INIS)

    Chow, L.S.; Basco, J.K.; Ackerman, J.P.; Johnson, T.R.

    1993-01-01

    A pyrochemical method is being developed at Argonne National Laboratory (ANL) to provide contnuous multistage extractions between molten chloride salts and liquid cadmium alloys at 500 degrees C. The extraction method will be used to recover transuranic (TRU) elements from the process salt in the electroretiner used in the pyrochemical reprocessing of spent fuel from the Integral Fast Reactor (IFR). The IFR is one of the Department of Energy's advanced power reactor concepts. The recovered TRU elements are returned to the electrorefiner. The extracted salt undergoes further processing to remove rare earths and other fission products so that most of the purified salt can also be returned to the electrorefiner, thereby extending the useful life of the process salt many times

  4. Rapid determination of 226Ra in drinking water samples using dispersive liquid-liquid microextraction coupled with liquid scintillation counting

    International Nuclear Information System (INIS)

    Sadi, B.K.; Chunsheng Li; Kramer, G.H.; Johnson, C.L.; Queenie Ko; Lai, E.P.C.

    2011-01-01

    A new radioanalytical method was developed for rapid determination of 226 Ra in drinking water samples. The method is based on extraction and preconcentration of 226 Ra from a water sample to an organic solvent using a dispersive liquid-liquid microextraction (DLLME) technique followed by radiometric measurement using liquid scintillation counting. In DLLME for 226 Ra, a mixture of an organic extractant (toluene doped with dibenzo-21-crown-7 and 2-theonyltrifluoroacetone) and a disperser solvent (acetonitrile) is rapidly injected into the water sample resulting in the formation of an emulsion. Within the emulsion, 226 Ra reacts with dibenzo-21-crown-7 and 2-theonyltrifluoroacetone and partitions into the fine droplets of toluene. The water/toluene phases were separated by addition of acetonitrile as a de-emulsifier solvent. The toluene phase containing 226 Ra was then measured by liquid scintillation counting. Several parameters were studied to optimize the extraction efficiency of 226 Ra, including water immiscible organic solvent, disperser and de-emulsifier solvent type and their volume, chelating ligands for 226 Ra and their concentrations, inorganic salt additive and its concentration, and equilibrium pH. With the optimized DLLME conditions, the accuracy (expressed as relative bias, B r ) and method repeatability (expressed as relative precision, S B ) were determined by spiking 226 Ra at the maximum acceptable concentration level (0.5 Bq L -1 ) according to the Guidelines for Canadian Drinking Water Quality. Accuracy and repeatability were found to be less than -5% (B r ) and less than 6% (S B ), respectively, for both tap water and bottled natural spring water samples. The minimum detectable activity and sample turnaround time for determination of 226 Ra was 33 mBq L -1 and less than 3 h, respectively. The DLLME technique is selective for extraction of 226 Ra from its decay progenies. (author)

  5. Rapid determination of alkaloids in Macleaya cordata using ionic liquid extraction followed by multiple reaction monitoring UPLC-MS/MS analysis.

    Science.gov (United States)

    Li, Linqiu; Huang, Mingyuan; Shao, Junli; Lin, Bokun; Shen, Qing

    2017-02-20

    The ultrasonic-assisted extraction (UAE) and ionic liquid based dispersive liquid-liquid microextraction (IL-DLLME) have been successfully applied in extracting of six alkaloids from M. cordata. 1-hexyl-3-methylimidazolium tetrafluoroborate ([C 6 MIM][BF 4 ]) aqueous solution was used as extraction solvent. The target analytes in raw material were deposited into a single drop of 1-hexyl-3-methylimidazolium hexafluorophosphate ([C 6 MIM][PF 6 ]), which was in situ formed by mixing [C 6 MIM][BF 4 ] and potassium hexafluorophosphate ([K][PF 6 ]. Afterwards, the extract was analyzed by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) in multiple-reaction monitoring (MRM) mode. The proposed method was fully validated in terms of linearity (0.9983-0.9992), LOD (0.080ngmL -1 ), LOQ (0.25ngmL -1 ), intra-day precision (MS/MS is powerful and practical for analyzing alkaloids in M. cordata., and it also has great potential for comprehensive quality control of other herbal medicines. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Pressurised liquid extraction of flavonoids in onions. Method development and validation

    DEFF Research Database (Denmark)

    Søltoft, Malene; Christensen, J.H.; Nielsen, J.

    2009-01-01

    A rapid and reliable analytical method for quantification of flavonoids in onions was developed and validated. Five extraction methods were tested on freeze-dried onions and subsequently high performance liquid chromatography (HPLC) with UV detection was used for quantification of seven flavonoids...... extraction methods. However. PLE was the preferred extraction method because the method can be highly automated, use only small amounts of solvents, provide the cleanest extracts, and allow the extraction of light and oxygen-sensitive flavonoids to be carried out in an inert atmosphere protected from light......-step PLE method showed good selectivity, precision (RSDs = 3.1-11%) and recovery of the extractable flavonoids (98-99%). The method also appeared to be a multi-method, i.e. generally applicable to, e.g. phenolic acids in potatoes and carrots....

  7. Ultrasound assisted extraction combined with dispersive liquid-liquid microextraction (US-DLLME)-a fast new approach to measure phthalate metabolites in nails.

    Science.gov (United States)

    Alves, Andreia; Vanermen, Guido; Covaci, Adrian; Voorspoels, Stefan

    2016-09-01

    A new, fast, and environmentally friendly method based on ultrasound assisted extraction combined with dispersive liquid-liquid microextraction (US-DLLME) was developed and optimized for assessing the levels of seven phthalate metabolites (including the mono(ethyl hexyl) phthalate (MEHP), mono(2-ethyl-5-hydroxyhexyl) phthalate (5-OH-MEHP), mono(2-ethyl-5-oxohexyl) phthalate (5-oxo-MEHP), mono-n-butyl phthalate (MnBP), mono-isobutyl phthalate (MiBP), monoethyl phthalate (MEP), and mono-benzyl phthalate (MBzP)) in human nails by UPLC-MS/MS. The optimization of the US-DLLME method was performed using a Taguchi combinatorial design (L9 array). Several parameters such as extraction solvent, solvent volume, extraction time, acid, acid concentration, and vortex time were studied. The optimal extraction conditions achieved were 180 μL of trichloroethylene (extraction solvent), 2 mL trifluoroacetic acid in methanol (2 M), 2 h extraction and 3 min vortex time. The optimized method had a good precision (6-17 %). The accuracy ranged from 79 to 108 % and the limit of method quantification (LOQm) was below 14 ng/g for all compounds. The developed US-DLLME method was applied to determine the target metabolites in 10 Belgian individuals. Levels of the analytes measured in nails ranged between <12 and 7982 ng/g. The MEHP, MBP isomers, and MEP were the major metabolites and detected in every sample. Miniaturization (low volumes of organic solvents used), low costs, speed, and simplicity are the main advantages of this US-DLLME based method. Graphical Abstract Extraction and phase separation of the US-DLLME procedure.

  8. Extractive liquid-liquid spectrophotometric procedure for the determination of thiocyanate ions employing the ion pair reagent amiloride monohydrochloride

    International Nuclear Information System (INIS)

    Bashammakh, A.S.; Bahaffi, S.O.; Al-Sibaai, A.A.; Al-Wael, H.O.; El-Shahawi, M.S.

    2007-01-01

    An accurate, inexpensive and less laborious liquid-liquid extractive spectrophotometric procedure for the determination of thiocyanate ions in aqueous media has been developed. The method has been based upon the formation of a yellow colored complex ion associate of the ion-pairing reagent 1-(3, 5-diamino-6-chloropyrazinecarboxyl) guanidine hydrochloride monohydrate, namely amiloride hydrochloride, DPG + .Cl - and the thiocyanate ions in aqueous media containing HNO 3 (0.5 mol L -1 ) and subsequent extraction with 4-methyl-2-pentanone. The absorption electronic spectrum of the ion associate showed one well-defined peak at λ max 366 nm. The stoichiometric mole ratio of DPG + .Cl - to the thiocyanate ions is 1:1.The effective molar absorptivity (ε) of the ion associate at λ max 366 nm is 1.1 ± 0.1 x 10 4 L mol -1 cm -1 . The extraction constants (K d , K ex , and β) enabled a simple and convenient use of the developed binary ion associate for the extractive spectrophotometric determination of traces of thiocyanate ions in the aqueous media. Beer's law and Ringbom's plots are obeyed in the concentration range 0.05-10 and 0.1-7 μg mL -1 of the thiocyanate ions, respectively with a relative standard deviation of ±2.3%. The calculated lower limits of detection (LOD) and quantitation (LOQ) of the developed procedure for the thiocyanate ions were found equal to 0.02 and 0.066 μg mL -1 , respectively. The developed method has been applied for the determination of trace amounts of thicyanate ions in tap-, waste- and natural water samples and compared successfully with the reported methods at the 95% confidence level. The proposed method was also applied successfully for the determination of thiocyanate ions in saliva samples

  9. Lipid extraction from microalgae using a single ionic liquid

    Science.gov (United States)

    Salvo, Roberto Di; Reich, Alton; Dykes, Jr., H. Waite H.; Teixeira, Rodrigo

    2013-05-28

    A one-step process for the lysis of microalgae cell walls and separation of the cellular lipids for use in biofuel production by utilizing a hydrophilic ionic liquid, 1-butyl-3-methylimidazolium. The hydrophilic ionic liquid both lyses the microalgae cell walls and forms two immiscible layers, one of which consists of the lipid contents of the lysed cells. After mixture of the hydrophilic ionic liquid with a suspension of microalgae cells, gravity causes a hydrophobic lipid phase to move to a top phase where it is removed from the mixture and purified. The hydrophilic ionic liquid is recycled to lyse new microalgae suspensions.

  10. Ionic Liquids as Benign Solvents for the Extraction of Aromatics

    International Nuclear Information System (INIS)

    Hossain, Md. Anwar; Lee, Jeesun; Kim, Dai Hyun; Nguyen, Dinh Quan; Cheong, Minserk; Kim, Hoon Sik

    2012-01-01

    Ionic liquids (ILs) have been extensively investigated as promising alternatives to conventional organic solvents such as sulfolane and N,N-dimethylformamide for the selective extraction of aromatic hydrocarbons from the C 6 -C 10 hydrocarbon mixtures produced from the cracking processes of naphtha and light oils. The most important advantage of ILs over conventional organic solvents is that they are immiscible with aliphatic hydrocarbons, and thus the back extraction of ILs from the raffinate phases and top hydrocarbon-rich layers is not necessary. In this paper, a brief review on the state of the art in the utilization of ILs for aromatics separation is presented

  11. Determination of species activities in organic phase. Modelling of liquid-liquid extraction system using uniquac and unifac models; Determination des activites des especes en phase organique. Application d`uniquac et unifac a la modelisation des systemes d`extraction liquide-liquide

    Energy Technology Data Exchange (ETDEWEB)

    Rat, B. [CEA Saclay, 91 - Gif-sur-Yvette (France). Dept. de Recherche en Retraitement et en Vitrification]|[Paris-6 Univ., 75 (France)

    1998-12-31

    The aim of nuclear fuel reprocessing is to separate reusable elements, uranium and plutonium from the other elements, fission products and minor actinides. PUREX process uses liquid-liquid extraction as separation method. Numerical codes for modelling the extraction operations of PUREX process use a semi-empirical model to represent the partition of species. To improve the precision and precision and predictive nature of the models, we looked for a theoretical tool which permits to quantify medium effects, especially in the organic phase, for which few models are available. The Sergeivskii-Dannus model permits to quantify deviations from ideality in organic phase equilibrated with aqueous phase, but with parameters depending on extractant/diluent ratio. We decided to investigate UNIQUAC and UNIFAC models which permit to estimate activity coefficients in non-electrolytic phases taking account of the mutual interactions of molecules and their morphology. UNIFAC is based on UNIQUAC but molecules are considered as structural groups assemblies. Before applying these model to extraction systems, we investigate their abilities to describe simple systems, binary and ternary systems. UNIQUAC has been applied to TBP/diluent mixtures and permits to estimate activity coefficients for diluents whose interactions with TPB are very different in nature and strength. Group contribution (UNIFAC) applied to TBP/alkane mixtures permits to represent the effect of lengthening alkane chain but not the effect of branching. UNIQUAC fails to describe the TBP/diluent/water/non-extractable-salt systems in case of strong TBP diluent interactions. In order to obtain a correct description of these systems, we used the Chem-UNIFAC model, where the INIFAC equation is supplemented with chemical equilibria allowing explicitly for complexes formation and where group contribution is used to describes complexes. We have with Chem-UNIFAC a model available which can take the effect of the diluent into

  12. Electrochemical assessment of water|ionic liquid biphasic systems towards cesium extraction from nuclear waste.

    Science.gov (United States)

    Stockmann, T Jane; Zhang, Jing; Montgomery, Anne-Marie; Ding, Zhifeng

    2014-04-22

    A room temperature ionic liquid (IL) composed of a quaternary alkylphosphonium (trihexyltetradecylphosphonium, P66614(+)) and tetrakis(pentafluorophenyl)borate anion (TB(-)) was employed within a water|P66614TB (w|P66614TB or w|IL) biphasic system to evaluate cesium ion extraction in comparison to that with a traditional water|organic solvent (w|o) combination. (137)Cs is a major contributor to the radioactivity of spent nuclear fuel as it leaves the reactor, and its extraction efficiency is therefore of considerable importance. The extraction was facilitated by the ligand octyl(phenyl)-N,N'-diisobutylcarbamoylphosphine oxide (CMPO) used in TRans-Uranium EXtraction processes and investigated through well established liquid|liquid electrochemistry. This study gave access to the metal ion to ligand (1:n) stoichiometry and overall complexation constant, β, of the interfacial complexation reaction which were determined to be 1:3 and 1.6×10(11) at the w|P66614TB interface while the study at w|o elicited an n equal to 1 with β equal to 86.5. Through a straightforward relationship, these complexation constant values were converted to distribution coefficients, δ(α), with the ligand concentrations studied for comparison to other studies present in the literature; the w|o and w|IL systems gave δ(α) of 2 and 8.2×10(7), respectively, indicating a higher overall extraction efficiency for the latter. For the w|o system, the metal ion-ligand stoichiometries were confirmed through isotopic distribution analysis of mass spectra obtained by the direct injection of an emulsified water-organic solvent mixture into an electron spray ionization mass spectrometer. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Experimental and modeling studies on the enantio-separation of 3,5-dinitrobenzoyl-(R),(S)-leucine by continuous liquid-liquid extraction in a cascade of centrifugal contactor separators

    NARCIS (Netherlands)

    Schuur, Boelo; Winkelman, Jozef G.M.; Vries, Johannes G. de; Heeres, Hero J.

    2010-01-01

    The continuous enantioselective liquid–liquid extraction of aqueous 3,5-dinitrobenzoyl-(R),(S)-leucine (AR,S) using O-(1-t-butylcarbamoyl)-11-octadecylsulfinyl-10,11-dihydro-quinine (C,a cinchona alkaloid) as extractant in 1,2-dichloroethane (DCE) was studied experimentally in a countercurrently

  14. Direct extraction of genomic DNA from maize with aqueous ionic liquid buffer systems for applications in genetically modified organisms analysis.

    Science.gov (United States)

    Gonzalez García, Eric; Ressmann, Anna K; Gaertner, Peter; Zirbs, Ronald; Mach, Robert L; Krska, Rudolf; Bica, Katharina; Brunner, Kurt

    2014-12-01

    To date, the extraction of genomic DNA is considered a bottleneck in the process of genetically modified organisms (GMOs) detection. Conventional DNA isolation methods are associated with long extraction times and multiple pipetting and centrifugation steps, which makes the entire procedure not only tedious and complicated but also prone to sample cross-contamination. In recent times, ionic liquids have emerged as innovative solvents for biomass processing, due to their outstanding properties for dissolution of biomass and biopolymers. In this study, a novel, easily applicable, and time-efficient method for the direct extraction of genomic DNA from biomass based on aqueous-ionic liquid solutions was developed. The straightforward protocol relies on extraction of maize in a 10 % solution of ionic liquids in aqueous phosphate buffer for 5 min at room temperature, followed by a denaturation step at 95 °C for 10 min and a simple filtration to remove residual biopolymers. A set of 22 ionic liquids was tested in a buffer system and 1-ethyl-3-methylimidazolium dimethylphosphate, as well as the environmentally benign choline formate, were identified as ideal candidates. With this strategy, the quality of the genomic DNA extracted was significantly improved and the extraction protocol was notably simplified compared with a well-established method.

  15. Luminescence screening of enrofloxacin and ciprofloxacin residues in swine liver after dispersive liquid - liquid microextraction cleanup

    Science.gov (United States)

    A rapid luminescence method was developed to screen residues of enrofloxacin (ENRO) and its metabolite, ciprofloxacin (CIPRO), in swine liver. Target analytes were extracted in acetonitrile-2.5% trifluoroacetic acid-NaCl, cleaned up by dispersive liquid-liquid microextraction (DLLME), and finally de...

  16. Mathematical modeling of liquid/liquid hollow fiber membrane contactor accounting for interfacial transport phenomena: Extraction of lanthanides as a surrogate for actinides

    International Nuclear Information System (INIS)

    Rogers, J.D.

    1994-01-01

    This report is divided into two parts. The second part is divided into the following sections: experimental protocol; modeling the hollow fiber extractor using film theory; Graetz model of the hollow fiber membrane process; fundamental diffusive-kinetic model; and diffusive liquid membrane device-a rigorous model. The first part is divided into: membrane and membrane process-a concept; metal extraction; kinetics of metal extraction; modeling the membrane contactor; and interfacial phenomenon-boundary conditions-applied to membrane transport

  17. The TRUEX [TRansUranium EXtraction] process and the management of liquid TRU [transuranic] waste

    International Nuclear Information System (INIS)

    Schulz, W.W.; Horwitz, E.P.

    1987-01-01

    The TRUEX process is a new generic liquid-liquid extraction process for removal of all actinides from acidic nitrate or chloride nuclear waste solutions. Because of its high efficiency and great flexibility, the TRUEX process appears destined to be widely used in the US and possibly in other countries for cost-effective management and disposal of transuranic (TRU) wastes. In the US, TRU wastes are those that contain ≥3.7 x 10 6 Bq/kg) of TRU elements with half-lives greater than 20 y. This paper gives a brief review of the relevant chemistry and summarizes the current status of development and deployment of the TRUEX (TRansUranium EXtraction) process flowsheets to treat specific acidic waste solutions at several US Department of Energy sites. 19 refs., 4 figs., 4 tabs

  18. Liquid-liquid extraction/headspace/gas chromatographic/mass spectrometric determination of benzene, toluene, ethylbenzene, (o-, m- and p-)xylene and styrene in olive oil using surfactant-coated carbon nanotubes as extractant.

    Science.gov (United States)

    Carrillo-Carrión, Carolina; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel

    2007-11-09

    BTEX-S compounds are widely distributed in the environment and can be present in different foodstuffs, including olive oil. Taking into account the risks of the exposure to these compounds, analytical methods for their determination in different matrices are mandatory. In this paper, the use of surfactant-coated multiwalled carbon nanotubes as additive in liquid-liquid extraction is applied for the determination of single-ring aromatic compounds in olive oil samples. After sample treatment, the aqueous extracts are subsequently analyzed by headspace/gas chromatography/mass spectrometry allowing the determination of BTEX-S within ca. 15 min. Each stage of the proposed LLE/HS/GC/MS configuration involves a selectivity enhancement avoiding the interference of other compounds of the sample matrix. Limits of detection were in the range 0.25 ng mL(-1) (obtained for ethylbenzene) and 0.43 ng mL(-1) (for benzene). The repeatability of the proposed method expressed as RSD varied between 1.9% (styrene) and 3.3% (benzene) (n=11).

  19. Mathematical Modeling for the Extraction of Uranium and Molybdenum with Emulsion Liquid Membrane, Including Industrial Application and Cost Evaluation of the Uranium Recovery

    International Nuclear Information System (INIS)

    Kris Tri Basuki

    2008-01-01

    Emulsion liquid membrane systems are double emulsion drops. Two immiscible phases are separated by a third phase which is immiscible with the other two phases. The liquid membrane systems were classified into two types: (1) carrier mediated mass transfer, (2) mass transfer without any reaction involved. Uranium extraction, molybdenum extraction and solvent extraction were used as purposed elements for each type of the membrane systems in the derivation of their mathematical models. Mass transfer in emulsion liquid membrane (ELM) systems has been modeled by several differential and algebraic equations. The models take into account the following : mass transfer of the solute from the bulk external phase to the external phase-membrane interface; an equilibrium reaction between the solute and the carrier to form the solute-carrier complex at the interface; mass transfer by diffusion of the solute-carrier complex in the membrane phase to the membrane-internal phase interface; another equilibrium reaction of the solute-carrier complex to release the solute at the membrane-internal phase interface into the internal phase. Models with or without the consideration of film resistances were developed and compared. The models developed in this study can predict the extraction rate through emulsion liquid membranes theoretically. All parameters required in the models can be determined before an experimental extraction run. Experimental data from literature (uranium extraction) and (molybdenum extraction and solvent extraction) were used to test the models. The agreements between the theoretical predictions and the experimental data were very good. The advantages of emulsion liquid membrane systems over traditional methods were discussed. The models developed in this research can be used directly for the design of emulsion liquid membrane systems. The results of this study represent a very significant step toward the practical applications of the emulsion liquid membrane

  20. Development and validation of an automated liquid-liquid extraction GC/MS method for the determination of THC, 11-OH-THC, and free THC-carboxylic acid (THC-COOH) from blood serum.

    Science.gov (United States)

    Purschke, Kirsten; Heinl, Sonja; Lerch, Oliver; Erdmann, Freidoon; Veit, Florian

    2016-06-01

    The analysis of Δ(9)-tetrahydrocannabinol (THC) and its metabolites 11-hydroxy-Δ(9)-tetrahydrocannabinol (11-OH-THC), and 11-nor-9-carboxy-Δ(9)-tetrahydrocannabinol (THC-COOH) from blood serum is a routine task in forensic toxicology laboratories. For examination of consumption habits, the concentration of the phase I metabolite THC-COOH is used. Recommendations for interpretation of analysis values in medical-psychological assessments (regranting of driver's licenses, Germany) include threshold values for the free, unconjugated THC-COOH. Using a fully automated two-step liquid-liquid extraction, THC, 11-OH-THC, and free, unconjugated THC-COOH were extracted from blood serum, silylated with N-methyl-N-(trimethylsilyl) trifluoroacetamide (MSTFA), and analyzed by GC/MS. The automation was carried out by an x-y-z sample robot equipped with modules for shaking, centrifugation, and solvent evaporation. This method was based on a previously developed manual sample preparation method. Validation guidelines of the Society of Toxicological and Forensic Chemistry (GTFCh) were fulfilled for both methods, at which the focus of this article is the automated one. Limits of detection and quantification for THC were 0.3 and 0.6 μg/L, for 11-OH-THC were 0.1 and 0.8 μg/L, and for THC-COOH were 0.3 and 1.1 μg/L, when extracting only 0.5 mL of blood serum. Therefore, the required limit of quantification for THC of 1 μg/L in driving under the influence of cannabis cases in Germany (and other countries) can be reached and the method can be employed in that context. Real and external control samples were analyzed, and a round robin test was passed successfully. To date, the method is employed in the Institute of Legal Medicine in Giessen, Germany, in daily routine. Automation helps in avoiding errors during sample preparation and reduces the workload of the laboratory personnel. Due to its flexibility, the analysis system can be employed for other liquid-liquid extractions as

  1. Design and calculation of tritium extraction from liquid LiPb by bubble columns for ITER

    International Nuclear Information System (INIS)

    Xie, Bo

    2009-04-01

    A mathematical model describing the complex fluid-dynamics of a bubble extractor from liquid LiPb loop for ITER is presented. A parametric analysis of the extraction efficiency of a bubble column as a function of the process parameters is carried out and the design of a bubble extractor system is proposed. On this base, a mathematical model is built by taking into consideration the kinetics of deuterium desorption from liquid LiPb alloy. The calculation data of deuterium release-behavior from liquid LiPb under different operating conditions of temperature and deuterium partial pressures and helium gas flow-rates in the liquid LiPb alloy are obtained. These results have shown that the overall re- lease process is governed by the diffusion of deuterium atoms in the LiPb and by the heterogeneous reaction at the gas-eutectic interface of the deuterium atoms recombination under the probable working temperature range. (authors)

  2. (Vapour + liquid) equilibria of ternary systems with ionic liquids using headspace gas chromatography

    International Nuclear Information System (INIS)

    Mokhtarani, Babak; Gmehling, Juergen

    2010-01-01

    (Vapour + liquid) equilibrium (VLE) data for the ternary systems (hexane + benzene), (hexane + cyclohexane), (benzene + cyclohexane), and (ethanol + water) with an ionic liquid as entrainer for extractive distillation were measured by headspace gas chromatography. As ionic liquids, 1-hexyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [HMIM][BTI], 1-octyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [OMIM][BTI], 1-octyl-3-methyl-imidazolium trifluoro-methanesulfonate [OMIM][OTF], and 1-butyl-3-methyl-imidazolium trifluoro-methanesulfonate [BMIM][OTF] were used. The experimental data show that the ionic liquids investigated have a great influence on the separation factors of the systems (hexane + benzene), (hexane + cyclohexane), and (benzene + cyclohexane). The experimental data were compared with the predicted results using mod. UNIFAC (Do). The predicted results are in good agreement with the experimental data.

  3. (Vapour + liquid) equilibria of ternary systems with ionic liquids using headspace gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Mokhtarani, Babak [Chemistry and Chemical Engineering Research Center of Iran, P.O. Box 14335-186, Tehran (Iran, Islamic Republic of); Gmehling, Juergen, E-mail: gmehling@tech.chem.uni-oldenburg.d [Carl von Ossietzky Universitaet Oldenburg, Technische Chemie, D-26111 Oldenburg (Germany)

    2010-08-15

    (Vapour + liquid) equilibrium (VLE) data for the ternary systems (hexane + benzene), (hexane + cyclohexane), (benzene + cyclohexane), and (ethanol + water) with an ionic liquid as entrainer for extractive distillation were measured by headspace gas chromatography. As ionic liquids, 1-hexyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [HMIM][BTI], 1-octyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [OMIM][BTI], 1-octyl-3-methyl-imidazolium trifluoro-methanesulfonate [OMIM][OTF], and 1-butyl-3-methyl-imidazolium trifluoro-methanesulfonate [BMIM][OTF] were used. The experimental data show that the ionic liquids investigated have a great influence on the separation factors of the systems (hexane + benzene), (hexane + cyclohexane), and (benzene + cyclohexane). The experimental data were compared with the predicted results using mod. UNIFAC (Do). The predicted results are in good agreement with the experimental data.

  4. Combination of solid-phase extraction with dispersive liquid-liquid microextraction followed by GC-MS for determination of pesticide residues from water, milk, honey and fruit juice.

    Science.gov (United States)

    Shamsipur, Mojtaba; Yazdanfar, Najmeh; Ghambarian, Mahnaz

    2016-08-01

    In this work, an effective preconcentration method for the extraction and determination of traces of multi-residue pesticides was developed using solid-phase extraction (SPE) coupled with dispersive liquid-liquid microextraction and gas chromatography-mass spectrometry (GC-MS). Variables affecting the performance of both extraction steps such as type and volume of elution and extraction solvents, breakthrough volume, salt addition, extraction time were thoroughly investigated. The proposed method resulted in good linearities (R(2)>0.9915) over the ranges of 1-10,000ngkg(-1), limits of detection (LODs) in the range of 0.5-1.0ngkg(-1) at S/N=3, and precision of RSD% of ⩽11.8. Under optimal conditions, the preconcentration factors were obtained in the range of 2362-10,593 for 100mL sample solutions. Comparison of the proposed method with other ones demonstrated that SPE-DLLME method provides higher extraction efficiency and larger preconcentration factor for determination of pesticides residues. Further, it is simple, inexpensive, highly sensitive, and can be successfully applied to separation, preconcentration and determination of the pesticides (and other noxious materials) in different real food samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. Separation of benzene from alkanes by solvent extraction with 1-ethylpyridinium ethylsulfate ionic liquid

    International Nuclear Information System (INIS)

    Gomez, Elena; Dominguez, Irene; Calvar, Noelia; Dominguez, Angeles

    2010-01-01

    The (liquid + liquid) equilibrium (LLE) data for ternary mixtures {alkane + benzene + 1-ethylpyridinium ethylsulfate ([EPy][EtSO 4 ])} at T = (283.15 and 298.15) K and atmospheric pressure are presented. The alkanes used were hexane and heptane. The cloud point method was used to determinate the binodal curve, and the tie-line compositions were obtained by density measurements. The LLE data obtained were used to calculate distribution coefficients and selectivity values. The consistency of tie-line data was ascertained by applying the Othmer-Tobias and Hand equations. Correlation of the experimental tie-lines was conducted through the use of NRTL equation, which provides good correlation of the experimental data. The results show that [EPy][EtSO 4 ] can be used as an alternative solvent in liquid extraction processes for the removal of benzene from its mixtures with alkanes.

  6. Analysis of major antioxidants from extracts of Myrmecodia pendans by UV/visible spectrophotometer, liquid chromatography/tandem mass spectrometry, and high-performance liquid chromatography/UV techniques.

    Science.gov (United States)

    Engida, Adam Mekonnen; Faika, Sitti; Nguyen-Thi, Bich Thuyen; Ju, Yi-Hsu

    2015-06-01

    In the present work, heat reflux extraction with ethanol/water (80:20; v/v) as the solvent was used to extract antioxidants from Myrmecodia pendans. The crude extract (CE) was fractionated using hexane and ethyl acetate. Ethyl acetate fraction (EAF) and aqueous fraction were collected. Antioxidant activity against 1,1-diphenyl-2-picrylhydrazyl-radical radical and ferric reducing power of the CE, EAF, and aqueous fraction were evaluated. EAF showed comparable antioxidant activity against 1,1-diphenyl-2-picrylhydrazyl-radical radical and ferric reducing power to those of the CE. UV/visible, liquid chromatography/electrospray ionization/tandem mass spectrometry, and high-performance liquid chromatography were employed for identifying the major antioxidant compounds in the EAF. Three major phenolic compounds (rosmarinic acid, procyanidin B1, and polymer of procyanidin B1) were identified. The first two compounds were confirmed and quantified by high-performance liquid chromatography using authentic standards, but confirmation of the third compound was hampered by a lack of commercial standard. Concentrations of rosmarinic acid and procyanidin B1 in the EAF were found to be 20.688 ± 1.573 mg/g dry sample and 3.236 ± 0.280 mg/g dry sample, respectively. All these three compounds are reported for the first time in sarang semut. Copyright © 2014. Published by Elsevier B.V.

  7. Analysis of major antioxidants from extracts of Myrmecodia pendans by UV/visible spectrophotometer, liquid chromatography/tandem mass spectrometry, and high-performance liquid chromatography/UV techniques

    Directory of Open Access Journals (Sweden)

    Adam Mekonnen Engida

    2015-06-01

    Full Text Available In the present work, heat reflux extraction with ethanol/water (80:20; v/v as the solvent was used to extract antioxidants from Myrmecodia pendans. The crude extract (CE was fractionated using hexane and ethyl acetate. Ethyl acetate fraction (EAF and aqueous fraction were collected. Antioxidant activity against 1,1-diphenyl-2-picrylhydrazyl-radical radical and ferric reducing power of the CE, EAF, and aqueous fraction were evaluated. EAF showed comparable antioxidant activity against 1,1-diphenyl-2-picrylhydrazyl-radical radical and ferric reducing power to those of the CE. UV/visible, liquid chromatography/electrospray ionization/tandem mass spectrometry, and high-performance liquid chromatography were employed for identifying the major antioxidant compounds in the EAF. Three major phenolic compounds (rosmarinic acid, procyanidin B1, and polymer of procyanidin B1 were identified. The first two compounds were confirmed and quantified by high-performance liquid chromatography using authentic standards, but confirmation of the third compound was hampered by a lack of commercial standard. Concentrations of rosmarinic acid and procyanidin B1 in the EAF were found to be 20.688 ± 1.573 mg/g dry sample and 3.236 ± 0.280 mg/g dry sample, respectively. All these three compounds are reported for the first time in sarang semut.

  8. Separation of americium by liquid-liquid extraction using diglycol-amides water-soluble complexing agents

    Energy Technology Data Exchange (ETDEWEB)

    Chapron, S.; Marie, C.; Pacary, V.; Duchesne, M.T.; Miguirditchian, M. [CEA, Centre de Marcoule, Nuclear Energy Division, RadioChemistry and Processses Departement, 30207 Bagnols-sur-Ceze (France); Arrachart, G.; Pellet-Rostaing, S. [Institut de Chimie Separative de Marcoule, LTSM, Bat 426, F-30207 Bagnols-sur- Ceze (France)

    2016-07-01

    Recycling americium (Am) alone from spent nuclear fuels is an important option studied for the future nuclear cycle (Generation IV systems) since Am belongs to the main contributors of the long-term radiotoxicity and heat power of final waste. Since 2008, a liquid-liquid extraction process called EXAm has been developed by the CEA to allow the recovery of Am alone from a PUREX raffinate (a dissolution solution already cleared from U, Np and Pu). A mixture of DMDOHEMA (N,N'-dimethyl-N,N'-dioctyl-2-(2-(hexyloxy)ethyl)-malonamide) and HDEHP (di-2-ethylhexylphosphoric acid) in TPH is used as the solvent and the Am/Cm selectivity is improved using TEDGA (N,N,N',N'-tetraethyl-diglycolamide) as a selective complexing agent to maintain Cm and heavier lanthanides in the acidic aqueous phase (5 M HNO{sub 3}). Americium is then stripped selectively from light lanthanides at low acidity (pH=3) with a poly-aminocarboxylic acid. The feasibility of sole Am recovery was already demonstrated during hot tests in ATALANTE facility and the EXAm process was adapted to a concentrated raffinate to optimize the process compactness. The speciation of TEDGA complexes formed in the aqueous phase with Am, Cm and lanthanides was studied to better understand and model the behavior of TEDGA in the process. Some Ln-TEDGA species are extracted into the organic phase and this specific chemistry might play a role in the Am/Cm selectivity improvement. Hence the hydrophilicity-lipophilicity balance of the complexing agent is an important parameter. In this comprehensive study, new analogues of TEDGA were synthesized and tested in the EXAm process conditions to understand the relationship between their structure and selectivity. New derivatives of TEDGA with different N-alkyl chain lengths and ramifications were synthesized. The impact of lipophilicity on ligand partitioning and Am/Cm selectivity was investigated. (authors)

  9. Multi-responsive ionic liquid emulsions stabilized by microgels

    NARCIS (Netherlands)

    Monteillet, H.; Workamp, M.; Li, X.; Schuur, Boelo; Kleijn, J.M.; Leermakers, F.; Sprakel, J.

    2014-01-01

    We present a complete toolbox to use responsive ionic liquid (IL) emulsions for extraction purposes. IL emulsions stabilized by responsive microgels are shown to allow rapid extraction and reversible breaking and re-emulsification. Moreover, by using a paramagnetic ionic liquid, droplets can be

  10. Direct Capture of Organic Acids From Fermentation Media Using Ionic Liquids

    Energy Technology Data Exchange (ETDEWEB)

    Klasson, K.T.

    2004-11-03

    Several ionic liquids have been investigated for the extraction of organic acids from fermentation broth. Partitioning of representative organic acids (lactic, acetic, and succinic) between aqueous solution and nine hydrophobic ionic liquids was measured. The extraction efficiencies were strongly dependent on pH of the aqueous phase. Distribution coefficient was very good (approximately 60) at low succinic acid concentrations for one of the ionic liquids (trihexyltetradecylphosphonium methanesulfonate) at neutral pH. However, this ionic liquid had to be diluted with nonanol due to its high viscosity in order to be useful. A diluent (trioctylamine) was also added to this mixture. The results suggest that an extraction system based on ionic liquids may be feasible for succinic acid recovery from fermentation broth and that two ideal extraction stages are needed to reduce the concentration from 33 g/L to 1 g/L of succinic acid. Further studies are needed to evaluate other issues related to practical applications, including ionic liquid loss in the process, toxicity effects of ionic liquids during simultaneous fermentation and extractions.

  11. Application of numerical modelling to scaling-up of electrically induced extraction from an organic mixture using an ionic liquid

    Directory of Open Access Journals (Sweden)

    Kamiński Kamil

    2016-03-01

    Full Text Available Liquid-liquid extraction provides an environmentally friendly process as an alternative to azeotropic distillation, pervaporation and reverse osmosis because these techniques require the use of large amounts of energy, may involve volatile organic compounds, and operation at high pressure.

  12. Quantification of VX Nerve Agent in Various Food Matrices by Solid-Phase Extraction Ultra-Performance Liquid ChromatographyTime-of-Flight Mass Spectrometry

    Science.gov (United States)

    2016-04-01

    QUANTIFICATION OF VX NERVE AGENT IN VARIOUS FOOD MATRICES BY SOLID - PHASE EXTRACTION ULTRA-PERFORMANCE...TITLE AND SUBTITLE Quantification of VX Nerve Agent in Various Food Matrices by Solid - Phase Extraction Ultra-Performance Liquid Chromatography...QUANTIFICATION OF VX NERVE AGENT IN VARIOUS FOOD MATRICES BY SOLID - PHASE EXTRACTION ULTRA-PERFORMANCE LIQUID CHROMATOGRAPHY–TIME-OF-FLIGHT MASS

  13. Ionic liquid-based microwave-assisted extraction of essential oil and biphenyl cyclooctene lignans from Schisandra chinensis Baill fruits.

    Science.gov (United States)

    Ma, Chun-hui; Liu, Ting-ting; Yang, Lei; Zu, Yuan-gang; Chen, Xiaoqiang; Zhang, Lin; Zhang, Ying; Zhao, Chunjian

    2011-12-02

    Ionic liquid-based microwave-assisted extraction (ILMAE) has been successfully applied in extracting essential oil and four kinds of biphenyl cyclooctene lignans from Schisandra chinensis Baill. 0.25 M 1-lauryl-3-methylimidazolium bromide ionic liquid is selected as solvent. The optimum parameters of dealing with 25.0 g sample are 385 W irradiation power, 40 min microwave extraction time and 1:12 solid-liquid ratio. The yields of essential oil and lignans are 12.12±0.37 ml/kg and 250.2±38.2 mg/kg under the optimum conditions. The composition of the essential oil extracted by hydro-distillation, steam-distillation and ILMAE is analyzed by GC-MS. With ILMAE method, the energy consumption time has not only been shortened to 40 min (hydro-distillation 3.0 h for extracting essential oil and reflux extraction 4.0 h for extracting lignans, respectively), but also the extraction efficiency has been improved (extraction of lignans and distillation of essential oil at the same time) and reduces the environmental pollution. S. chinensis materials treated by different methods are observed by scanning electronic microscopy. Micrographs provide more evidence to prove that ILMAE is a better and faster method. The experimental results also indicate that ILMAE is a simple and efficient technique for sample preparation. Copyright © 2011 Elsevier B.V. All rights reserved.

  14. A simple and sensitive HPLC method for analysis of imipramine in human plasma with UV detection and liquid-liquid extraction: Application in bioequivalence studies.

    Science.gov (United States)

    Rezazadeh, Mahboubeh; Emami, Jaber

    2016-01-01

    High-performance liquid chromatography (HPLC) methods employing ultraviolet (UV) detector are not sufficiently sensitive to measure the low plasma concentrations following single oral dose of imipramine. Therefore, in the present study a simple, rapid and yet sensitive HPLC method with UV detection was developed and validated for quantitation of imipramine in human plasma samples. An efficient liquid-liquid extraction (LLE) of imipramine from plasma with the mixture of hexane/isoamyl alcohol (98:2) and back extraction of the drug in acidic medium concomitant with evaporation of organic phase allowed the use of UV detector to conveniently measure plasma levels of this compound as low level as 3 ng/ml. Separation was achieved on a μ-Bondapak C18 HPLC column using sodium hydrogen phosphate solution (0.01 M)/acetonitrile (60/40 v/v) at pH 3.5 ± 0.1 at 1.5 ml/min. Trimipramine was used as the internal standard for analysis of plasma samples. The retention times for imipramine and trimipramine were 4.3 and 5.2 min, respectively. Calibration curve was linear in the range of 3-40 ng/ml using human plasma with the average extraction recovery of 85 ± 5%. Imipramine was found to be stable in plasma samples with no evidence of degradation during three freeze-thaw cycles and three months storage at -70°C. The current validated method was finally applied in bioequivalence studies of two different imipramine products according to a standard two-way crossover design with a two weeks washout period.

  15. Fast quantification of short chain fatty acids and ketone bodies by liquid chromatography-tandem mass spectrometry after facile derivatization coupled with liquid-liquid extraction.

    Science.gov (United States)

    Zeng, Mingfei; Cao, Huachuan

    2018-04-15

    Short chain fatty acids (SCFA) and ketone bodies recently emerged as important physiological relevant metabolites because of their association with microbiota, immunology, obesity and other metabolic states. They were commonly analyzed by GC-MS with long run time and laborious sample preparation. In this study we developed a novel LC-MS/MS method using fast derivatization coupled with liquid-liquid extraction to detect SCFA and ketone bodies in plasma and feces. Several different derivatization reagents were evaluated to compare the efficiency, the sensitivity and chromatographic separation of structural isomers. O‑benzylhydroxylamine was selected for its superior overall performance in reaction time and isomeric separation that allowed the measurement of each SCFAs and ketone bodies free from interferences. The derivatization procedure is facile and reproducible in aqueous-organic medium, which abolished the evaporation procedure hampering the analysis of volatile short chain acids. Enhancement in sensitivity remarkably improved the detection limit of SCFA and ketone bodies to sub-fmol level. This novel method was applied to quantify these metabolites in fecal and plasma samples from lean and DIO mouse. Copyright © 2018 Elsevier B.V. All rights reserved.

  16. Review of algorithms for modeling metal distribution equilibria in liquid-liquid extraction processes

    Directory of Open Access Journals (Sweden)

    Lozano, L. J.

    2005-10-01

    Full Text Available This work focuses on general guidelines to be considered for application of least-squares routines and artificial neural networks (ANN in the estimation of metal distribution equilibria in liquid-liquid extraction process. The goal of the procedure in the statistical method is to find the values of the equilibrium constants (Kj for the reactions involved in the metal extraction which minimizes the differences between experimental distribution coefficient (Dexp and theoretical distribution coefficients according to the mechanism proposed (Dtheor- In the first part of the article, results obtained with the most frequently routine reported in the bibliography are compared with those obtained using the algorithms previously discussed. In the second part, the main features of a single back-propagation neural network for the same purpose are discussed, and the results obtained are compared with those obtained with the classical methods.

    El trabajo presenta las líneas generales a considerar para la estimación del equilibrio de distribución de metales en procesos de extracción líquido-líquido, según dos métodos: algoritmo clásico de mínimos cuadrados y redes neuronales artificiales. El objetivo del procedimiento, en el caso del método estadístico, es encontrar los valores de las constantes de equilibrio (Kj para las reacciones involucradas en la extracción del metal, que minimizan las diferencias entre el coeficiente de distribución experimental y el coeficiente de distribución teórico, de acuerdo al mecanismo propuesto. En la primera parte del artículo se comparan los resultados obtenidos a partir de los algoritmos usados más habitualmente en la bibliografía, con los datos obtenidos mediante el algoritmo previamente descrito. En la segunda parte, se presentan las características fundamentales para aplicar una red neuronal sencilla con algoritmo back-propagation y los

  17. Extraction of three bioactive diterpenoids from Andrographis paniculata: effect of the extraction techniques on extract composition and quantification of three andrographolides using high-performance liquid chromatography.

    Science.gov (United States)

    Kumar, Satyanshu; Dhanani, Tushar; Shah, Sonal

    2014-10-01

    Andrographis paniculata (Burm.f.) wall.ex Nees (Acanthaceae) or Kalmegh is an important medicinal plant finding uses in many Ayurvedic formulations. Diterpenoid compounds andrographolides (APs) are the main bioactive phytochemicals present in leaves and herbage of A. paniculata. The efficiency of supercritical fluid extraction (SFE) using carbon dioxide was compared with the solid-liquid extraction techniques such as solvent extraction, ultrasound-assisted solvent extraction and microwave-assisted solvent extraction with methanol, water and methanol-water as solvents. Also a rapid and validated reverse-phase high-performance liquid chromatography-diode array detection method was developed for the simultaneous determination of the three biologically active compounds, AP, neoandrographolide and andrograpanin, in the extracts of A. paniculata. Under the best SFE conditions tested for diterpenoids, which involved extraction at 60°C and 100 bar, the extractive efficiencies were 132 and 22 µg/g for AP and neoandrographolide, respectively. The modifier percentage significantly affected the extraction efficiency. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  18. Liquidity risk and contagion for liquid funds

    OpenAIRE

    Darolles , Serge; Dudek , Jeremy; Le Fol , Gaëlle

    2014-01-01

    Fund managers face liquidity problems but they have to distinguish the market liquidity risk implied by their assets and the funding liquidity risk. This latter is due to both the liquidity mismatch between assets and liabilities and the redemption risk due to the possible outflows from clients. The main contribution of this paper is the analysis of contagion looking at common market liquidity problems to detect funding liquidity problems. Using the CDS Bond Spread basis as a liquidity indica...

  19. Simultaneous quantification of major flavonoids in "Bawanghua", the edible flower of Hylocereus undatus using pressurised liquid extraction and high performance liquid chromatography.

    Science.gov (United States)

    Yi, Yan; Zhang, Qing-Wen; Li, Song-Lin; Wang, Ying; Ye, Wen-Cai; Zhao, Jing; Wang, Yi-Tao

    2012-11-15

    A pressurised liquid extraction (PLE) and high performance liquid chromatography (HPLC) method was developed for simultaneous quantification of six major flavonoids in edible flower of Hylocereus undatus. In order to achieve the baseline separation of two pairs of isomers, the HPLC conditions were optimised with different kind of reversed phase columns and mobile phase gradient programs. In addition, the solvent concentration, extraction temperature, extraction time and flush cycle for PLE were also optimised. Zorbax SB-C8 (100×2.1 mm, 1.8 μm) column was chosen with acetonitrile and water containing 0.1% trifluoroacetic acid as mobile phase, the six analytes were eluted with baseline separation. The calibration curves showed good linearity (r(2)>0.9994) with LODs and LOQs less than 0.90 and 3.60 ng respectively. The RSDs for intra- and inter-day repeatability was not more than 1.09% and 1.79% respectively. The overall recovery of the assay was 96.9-105.2%. The sample was stable for at least 12 h. The newly established method was successfully applied to quantify six flavonoids in different parts of "Bawanghua", and the commercial samples from different locations. Copyright © 2012 Elsevier Ltd. All rights reserved.

  20. Separation of cesium from intermediate level liquid radioactive waste by solvent extraction with antioxidants

    International Nuclear Information System (INIS)

    Gulis, G.

    1989-01-01

    Antioxidants AO 2246, AO 4, AO 4K, AO 301 (Czechoslovakia) and NOCRAC 2246 (Japan) were tested as extracting agents for the separation of cesiium by solvent extraction with substituted phenols. The following effects on extraction were studied: pH of water phase, influence of diluent and of antioxidant concentration, extraction time, influence of salt content. The extraction of cesium from liquid radioactive waste was tested. The best results were obtained by NOCRAC 2246 in nitrobenzene, the extraction efficiency was 92.3% with pH 13.23. (author) 7 refs.; 5 figs.; 4 tabs

  1. From Funding Liquidity to Market Liquidity

    DEFF Research Database (Denmark)

    Dick-Nielsen, Jens; Lund, Jesper; Gyntelberg, Jacob

    This paper shows empirically that funding liquidity drives market liquidity. As it becomes harder to secure term funding in the money markets, liquidity deteriorates in the Danish bond market. We show that the first principal component of bond market liquidity is driven by the market makers...... for other European government bonds using MTS data. The findings suggest that regulatory bond based liquidity buffers for banks will have limited effectiveness....

  2. Ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate, an efficient solvent for extraction of acetone from aqueous solutions

    International Nuclear Information System (INIS)

    Saien, Javad; Badieh, Marjan Mohammadi Sarab; Norouzi, Mahdi; Salehzadeh, Sadegh

    2015-01-01

    Highlights: • The use of HMIMPF_6 as a green ionic was feasible in the extraction of acetone from water. • The binodal curves were determined by cloud point measurement method. • High level separation factor of acetone between the ionic liquid and water were achieved. • The thermodynamic properties of HMIMPF_6 were obtained by the Density Functional Theory calculations. • The NRTL and UNIQUAC models were applied satisfactorily to correlate the equilibrium data. - Abstract: (Liquid + liquid) equilibrium (LLE) of the chemical system of {water + acetone + 1-Hexyl-3-methylimidazolium hexafluorophosphate (HMIMPF_6) ionic liquid} was studied at different temperatures of (293.2, 298.2 and 303.2) K and under atmospheric pressure of 81.5 kPa. The results show that HMIMPF_6 provides the acetone distribution coefficient and separation factor values within (0.8813 to 1.2351) and (3.0 to 54.4), respectively; indicating the high capability of the ionic liquid for extraction of acetone from aqueous solutions. In most cases, acetone solubility in the ionic liquid is higher than in water, especially at higher solute concentrations. Meanwhile, higher separation factor is relevant to the lower temperature due to lower (water + ionic liquid) miscibility. The consistency of tie line data, at each temperature, was examined with Othmer–Tobias correlation. The values were nicely reproduced with the well-known NRTL and UNIQUAC models. Accordingly, the required thermodynamic properties of HMIMPF_6 were obtained by the Density Functional Theory (DFT) calculations, carried out at the M06/6-311++G"∗"∗ level of theory. The root mean square deviations (RMSD) between experimental and model concentration values were 0.0192 and 0.0255, respectively; indicating close agreement of the both models.

  3. The Influence of Lactic Acid Concentration on the Separation of Light Rare Earth Elements by Continuous Liquid-Liquid Extraction with 2-Ethylhexyl Phosphonic Acid Mono-2-ethylhexyl Ester

    Science.gov (United States)

    de Carvalho Gomes, Rafael; Seruff, Luciana Amaral; Scal, Maira Labanca Waineraich; Vera, Ysrael Marrero

    2018-02-01

    The separation of rare earth elements (REEs) using solvent extraction adding complexing agents appears to be an alternative to saponification of the extractant. We evaluated the effect of lactic acid concentration on didymium (praseodymium and neodymium) and lanthanum extraction with 2-ethylhexyl phosphonic acid mono-2-ethyl hexyl ester [HEH(EHP)] as extractant. First, we investigated in batch experiments the separation of lanthanum (La) and didymium (Pr and Nd) using McCabe-Thiele diagrams to estimate the number of extraction stages when the feed solution was or was not conditioned with lactic acid. Additionally, we conducted continuous liquid-liquid extraction experiments and evaluated the influence of lactic acid concentration on the REE extraction and separation. The tests showed that the extraction percentage of REEs and the separation factor Pr/La increased when the lactic acid concentration increased, but the didymium purity decreased. Lanthanum, praseodymium, and neodymium extraction rate were 23.0, 89.7, and 99.2 pct, respectively, with 1:1 aqueous/organic volume flow rate and feed solution doped with 0.52 mol L-1 lactic acid. The highest didymium purity reached was 92.0 pct with 0.26 mol L-1 lactic acid concentration.

  4. Miniaturised pressurised liquid extraction aromatic hydrocarbons from soil and sediment with subsequent large-volume injection-gas chromatography

    NARCIS (Netherlands)

    Ramos, L.; Vreuls, J.J.; Brinkman, U.A.T.

    2000-01-01

    Analyte extraction is the main limitation when developing at-line, or on-line, procedures for the preparation of (semi)solid environmental samples. Pressurised liquid extraction (PLE) is an analyte- and matrix-independent technique which provides cleaner extracts than the time-consuming classical

  5. Ionic liquid ultrasound assisted dispersive liquid-liquid microextraction method for preconcentration of trace amounts of rhodium prior to flame atomic absorption spectrometry determination

    Energy Technology Data Exchange (ETDEWEB)

    Molaakbari, Elaheh [Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Young Research Society, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Mostafavi, Ali, E-mail: mostafavi.ali@gmail.com [Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Afzali, Daryoush [Environment and Nanochemistry Department, Research Institute of Environmental Science, International Center for Science, High Technology and Environmental Science, Kerman (Iran, Islamic Republic of); Mineral Industries Research Center, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of)

    2011-01-30

    In this article, we consider ionic liquid based ultrasound-assisted dispersive liquid-liquid microextraction of trace amounts of rhodium from aqueous samples and show that this is a fast and reliable sample pre-treatment for the determination of rhodium ions by flame atomic absorption spectrometry. The Rh(III) was transferred into its complex with 2-(5-bromo-2-pyridylazo)-5-diethylamino phenol as a chelating agent, and an ultrasonic bath with the ionic liquid, 1-octyl-3-methylimidazolium bis (trifluoromethylsulfonyl) imide at room temperature was used to extract the analyte. The centrifuged rhodium complex was then enriched in the form of ionic liquid droplets and prior to its analysis by flame atomic absorption spectrometry, 300 {mu}L ethanol was added to the ionic liquid-rich phase. Finally, the influence of various parameters on the recovery of Rh(III) was optimized. Under optimum conditions, the calibration graph was linear in the range of 4.0-500.0 ng mL{sup -1}, the detection limit was 0.37 ng mL{sup -1} (3S{sub b}/m, n = 7) and the relative standard deviation was {+-}1.63% (n = 7, C = 200 ng mL{sup -1}). The results show that ionic liquid based ultrasound assisted dispersive liquid-liquid microextraction, combined with flame atomic absorption spectrometry, is a rapid, simple, sensitive and efficient analytical method for the separation and determination of trace amounts of Rh(III) ions with minimum organic solvent consumption.

  6. Rapid screening of oxytetracycline residue in catfish muscle by dispersive liquid-liquid microextraction and europium-sensitized luminescence

    Science.gov (United States)

    Oxytetracycline (OTC) residue in catfish muscle was screened by dispersive liquid-liquid microextraction (DLLME) and europium-sensitized luminescence (ESL). After extraction in EDTA, HCl, and acetonitrile, cleanup was carried out by DLLME, and ESL was measured at microgram = 385 nm and wavelength = ...

  7. Skin whitening and anti-corrugation activities of glycoprotein fractions from liquid extracts of boiled sea cucumber.

    Science.gov (United States)

    Kim, So Jung; Park, So Yun; Hong, Sun-Mee; Kwon, Eun-Hye; Lee, Taek-Kyun

    2016-10-01

    To determine skin whitening and wrinkle improvement efficacy, glycoprotein fractions were extracted from liquid extracts of boiled sea cucumber and their effects on tyrosine and elastase inhibitory activities were assayed. Fractions above and below 50 kDa (>50 kDa and 50 kDa enhanced tyrosinase and elastase inhibitory activities by 50.84% and 28.78%, respectively. Correlations of the >50 kDa concentration with tyrosinase inhibitory (R2 = 0.968) and elastase inhibitory (R2 = 0.983) efficacy were significant. >50 kDa glycoprotein fraction isolated from liquid extracts of boiled sea cucumber, which can serve as a functional cosmetic ingredient for whitening and wrinkle improvement of skin. Copyright © 2016 Hainan Medical University. Production and hosting by Elsevier B.V. All rights reserved.

  8. Liquid fuels production from biomass. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Levy, P. F.; Sanderson, J. E.; Ashare, E.; Wise, D. L.; Molyneaux, M. S.

    1980-06-30

    The current program to convert biomass into liquid hydrocarbon fuels is an extension of a previous program to ferment marine algae to acetic acid. In that study it was found that marine algae could be converted to higher aliphatic organic acids and that these acids could be readily removed from the fermentation broth by membrane or liquid-liquid extraction. It was then proposed to convert these higher organic acids via Kolbe electrolysis to aliphatic hydrocarbons, which may be used as a diesel fuel. The specific goals for the current porgram are: (1) establish conditions under which substrates other than marine algae may be converted in good yield to organic acids, here the primary task is methane suppression; (2) modify the current 300-liter fixed packed bed batch fermenter to operate in a continuous mode; (3) change from membrane extraction of organic acids to liquid-liquid extraction; (4) optimize the energy balance of the electrolytic oxidation process, the primary task is to reduce the working potential required for the electrolysis while maintaining an adequate current density; (5) scale the entire process up to match the output of the 300 liter fermenter; and (6) design pilot plant and commercial size plant (1000 tons/day) processes for converting biomass to liquid hydrocarbon fuels and perform an economic analysis for the 1000 ton/day design.

  9. Extraction and Chromatographic Determination of Shikimic Acid in Chinese Conifer Needles with 1-Benzyl-3-methylimidazolium Bromide Ionic Liquid Aqueous Solutions

    Science.gov (United States)

    Chen, Fengli; Hou, Kexin; Li, Shuangyang; Zu, Yuangang; Yang, Lei

    2014-01-01

    An ionic liquids-based ultrasound-assisted extraction (ILUAE) method was successfully developed for extracting shikimic acid from conifer needles. Eleven 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were investigated and 1-benzyl-3-methylimidazolium bromide solution was selected as the solvent. The conditions for ILUAE, including the ionic liquid concentration, ultrasound power, ultrasound time, and liquid-solid ratio, were optimized. The proposed method had good recovery (99.37%–100.11%) and reproducibility (RSD, n = 6; 3.6%). ILUAE was an efficient, rapid, and simple sample preparation technique that showed high reproducibility. Based on the results, a number of plant species, namely, Picea koraiensis, Picea meyeri, Pinus elliottii, and Pinus banksiana, were identified as among the best resources of shikimic acid. PMID:24782942

  10. Determination of desipramine in biological samples using liquid-liquid-liquid microextraction combined with in-syringe derivatization, gas chromatography, and nitrogen/phosphorus detection.

    Science.gov (United States)

    Saraji, Mohammad; Mehrafza, Narges; Bidgoli, Ali Akbar Hajialiakbari; Jafari, Mohammad Taghi

    2012-10-01

    A method was established for the determination of desipramine in biological samples using liquid-liquid-liquid microextraction followed by in-syringe derivatization and gas chromatography-nitrogen phosphorus detection. The extraction method was based on the use of two immiscible organic solvents. n-Dodecane was impregnated in the pores of the hollow fiber and methanol was placed inside the lumen of the fiber as the acceptor phase. Acetic anhydride was used as the reagent for the derivatization of the analyte inside the syringe barrel. Parameters that affect the extraction efficiency (composition of donor and acceptor phase, ionic strength, sample temperature, and extraction time) as well as derivatization efficiency (amount of acetic anhydride and reaction time and temperature) were investigated. The limit of detection was 0.02 μg/L with intra and interday RSDs of 2.6 and 7.7%, respectively. The linearity of the method was in the range of 0.2-20 μg/L (r(2) = 0.9986). The method was successfully applied to determine desipramine in human plasma and urine. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Experimental (solid + liquid) or (liquid + liquid) phase equilibria of (amine + nitrile) binary mixtures

    International Nuclear Information System (INIS)

    Domanska, Urszula; Marciniak, Malgorzata

    2007-01-01

    (Solid + liquid) phase diagrams have been determined for (hexylamine, or octylamine, or 1,3-diaminopropane + acetonitrile) mixtures. Simple eutectic systems have been observed in these mixtures. (Liquid + liquid) phase diagrams have been determined for (octylamine, or decylamine + propanenitrile, or + butanenitrile) mixtures. Mixtures with propanenitrile and butanenitrile show immiscibility in the liquid phase with an upper critical solution temperature, UCST. (Solid + liquid) phase diagrams have been correlated using NRTL, NRTL 1, Wilson and UNIQUAC equations. (Liquid + liquid) phase diagrams have been correlated using NRTL equation

  12. Ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction combined with electrothermal atomic absorption spectrometry for a sensitive determination of cadmium in water samples

    International Nuclear Information System (INIS)

    Li Shengqing; Cai Shun; Hu Wei; Chen Hao; Liu Hanlan

    2009-01-01

    A new method was developed for the determination of cadmium in water samples using ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction (IL-based USA-DLLME) followed by electrothermal atomic absorption spectrometry (ETAAS). The IL-based USA-DLLME procedure is free of volatile organic solvents, and there is no need for a dispersive solvent, in contrast to conventional DLLME. The ionic liquid, 1-hexyl-3-methylimidazolium hexafluorophosphate (HMIMPF 6 ), was quickly disrupted by an ultrasonic probe for 1 min and dispersed in water samples like a cloud. At this stage, a hydrophobic cadmium-DDTC complex was formed and extracted into the fine droplets of HMIMPF 6 . After centrifugation, the concentration of the enriched cadmium in the sedimented phase was determined by ETAAS. Some effective parameters of the complex formation and microextraction, such as the concentration of the chelating agent, the pH, the volume of the extraction solvent, the extraction time, and the salt effect, have been optimized. Under optimal conditions, a high extraction efficiency and selectivity were reached for the extraction of 1.0 ng of cadmium in 10.0 mL of water solution employing 73 μL of HMIMPF 6 as the extraction solvent. The enrichment factor of the method is 67. The detection limit was 7.4 ng L - 1 , and the characteristic mass (m 0 , 0.0044 absorbance) of the proposed method was 0.02 pg for cadmium (Cd). The relative standard deviation (RSD) for 11 replicates of 50 ng L - 1 Cd was 3.3%. The method was applied to the analysis of tap, well, river, and lake water samples and the Environmental Water Reference Material GSBZ 50009-88 (200921). The recoveries of spiked samples were in the range of 87.2-106%.

  13. Demonstration of pyropartitioning process by using genuine high-level liquid waste. Reductive-extraction of actinide elements from chlorination product

    International Nuclear Information System (INIS)

    Uozumi, Koichi; Iizuka, Masatoshi; Kurata, Masaki; Ougier, Michel; Malmbeck, Rikard; Winckel, Stefaan van

    2009-01-01

    The pyropartitioning process separates the minor actinide elements (MAs) together with uranium and plutonium from the high-level liquid waste generated at the Purex reprocessing of spent LWR fuel and introduces them to metallic fuel cycle. For the demonstration of this technology, a series experiment using 520g of genuine high-level liquid waste was started and the conversion of actinide elements to their chlorides was already demonstrated by denitration and chlorination. In the present study, a reductive extraction experiment in molten salt/liquid cadmium system to recover actinide elements from the chlorination product of the genuine high-level liquid waste was performed. The results of the experiment are as following; 1) By the addition of the cadmium-lithium alloy reductant, almost all of plutonium and MAs in the initial high-level liquid waste were recovered in the cadmium phase. It means no mass loss during denitration, chlorination, and reductive-extraction. 2) The separation factor values of plutonium, MAs, and rare-earth fission product elements versus uranium agreed with the literature values. Therefore, actinide elements will be separated from fission product elements in the actual system. Hence, the pyropartitioning process was successfully demonstrated. (author)

  14. (Liquid + liquid) equilibrium at T = 298.15 K for ternary mixtures of alkane + aromatic compounds + imidazolium-based ionic liquids

    International Nuclear Information System (INIS)

    Domínguez, Irene; Requejo, Patricia F.; Canosa, José; Domínguez, Ángeles

    2014-01-01

    Highlights: • The LLE ternary phase diagrams with 2 imidazolium-based ionic liquids were measured. • The LLE data were experimental determined at T = 298.15 K and p = 1 atm. • Mixtures of (octane or nonane) and (benzene or toluene or ethylbenzene) were studied. • LLE experimental data were correlated with NRTL and UNIQUAC thermodynamic models. - Abstract: Ionic liquids, with their unique and tunable properties, can be an advantageous alternative as extractive solvents in separation processes involving systems containing aliphatic and aromatic hydrocarbons. In this work, (liquid + liquid) equilibrium (LLE) data for the ternary systems {nonane (1) + benzene (2) + 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide, [BMim][NTf 2 ] (3)}, {octane (1) + benzene (2) + 1-methyl-3-propylimidazolium bis(trifluoromethylsulfonyl)imide, [PMim][NTf 2 ] (3)}, and {nonane (1) + aromatic compound (benzene or toluene or ethylbenzene) (2) + [PMim][NTf 2 ] (3)} were determined at T = 298.15 K and atmospheric pressure. Selectivity and solute distribution ratio, derived from the equilibrium data, were used to determine if this ionic liquid can be considered as a potential solvent for the separation of aromatic compounds (benzene, toluene, and ethylbenzene) from alkanes (octane and nonane). The experimental data were satisfactorily correlated with NRTL and UNIQUAC models

  15. Dispersive liquid-liquid microextraction followed by high-performance liquid chromatography-ultraviolet detection to determination of opium alkaloids in human plasma.

    Science.gov (United States)

    Ahmadi-Jouibari, Toraj; Fattahi, Nazir; Shamsipur, Mojtaba; Pirsaheb, Meghdad

    2013-11-01

    A novel, simple, rapid and sensitive dispersive liquid-liquid microextraction method based on the solidification of floating organic drop (DLLME-SFO) combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was used to determine opium alkaloids in human plasma. During the extraction procedure, plasma protein was precipitated by using a mixture of zinc sulfate solution and acetonitrile. Some effective parameters on extraction were studied and optimized. Under the optimum conditions (extraction solvent: 30.0 μl 1-undecanol; disperser solvent: 470 μl acetone; pH: 9; salt addition: 1%(w/v) NaCl and extraction time: 0.5 min), calibration curves are linear in the range of 1.5-1000 μgl(-1) and limit of detections (LODs) are in the range of 0.5-5 μgl(-1). The relative standard deviations (RSDs) for 100 μgl(-1) of morphine and codeine, 10.0 μgl(-1) of papaverine and 20.0 μgl(-1) of noscapine in diluted human plasma are in the range of 4.3-7.4% (n=5). Finally, the method was successfully applied in the determination of opium alkaloids in the actual human plasma samples. The relative recoveries of plasma samples spiked with alkaloids are 88-110.5%. The obtained results show that DLLME-SFO combined with HPLC-UV is a fast and simple method for the determination of opium alkaloids in human plasma. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. Inhibitory activity of a standardized elderberry liquid extract against clinically-relevant human respiratory bacterial pathogens and influenza A and B viruses

    Directory of Open Access Journals (Sweden)

    Domann Eugen

    2011-02-01

    Full Text Available Abstract Background Black elderberries (Sambucus nigra L. are well known as supportive agents against common cold and influenza. It is further known that bacterial super-infection during an influenza virus (IV infection can lead to severe pneumonia. We have analyzed a standardized elderberry extract (Rubini, BerryPharma AG for its antimicrobial and antiviral activity using the microtitre broth micro-dilution assay against three Gram-positive bacteria and one Gram-negative bacteria responsible for infections of the upper respiratory tract, as well as cell culture experiments for two different strains of influenza virus. Methods The antimicrobial activity of the elderberry extract was determined by bacterial growth experiments in liquid cultures using the extract at concentrations of 5%, 10%, 15% and 20%. The inhibitory effects were determined by plating the bacteria on agar plates. In addition, the inhibitory potential of the extract on the propagation of human pathogenic H5N1-type influenza A virus isolated from a patient and an influenza B virus strain was investigated using MTT and focus assays. Results For the first time, it was shown that a standardized elderberry liquid extract possesses antimicrobial activity against both Gram-positive bacteria of Streptococcus pyogenes and group C and G Streptococci, and the Gram-negative bacterium Branhamella catarrhalis in liquid cultures. The liquid extract also displays an inhibitory effect on the propagation of human pathogenic influenza viruses. Conclusion Rubini elderberry liquid extract is active against human pathogenic bacteria as well as influenza viruses. The activities shown suggest that additional and alternative approaches to combat infections might be provided by this natural product.

  17. Ternary (liquid + liquid) equilibria of {trifluorotris(perfluoroethyl)phosphate based ionic liquids + thiophene + heptane}

    International Nuclear Information System (INIS)

    Marciniak, Andrzej; Królikowski, Marek

    2012-01-01

    Highlights: ► Ternary (liquid + liquid) equilibria for 3 ionic liquid + thiophene + heptane systems. ► The influence of ionic liquid structure on phase diagrams is discussed. ► High selectivity for separation of heptane/thiophene is observed. - Abstract: Ternary (liquid + liquid) equilibria for three systems containing ionic liquids {(4-(2-methoxyethyl)-4-methylmorpholinium trifluorotris(perfluoroethyl)phosphate, 1-(2-methoxyethyl)-1-methylpiperidinium trifluorotris(perfluoroethyl)phosphate, 1-(2-methoxyethyl)-1-methylpyrrolidinium trifluorotris(perfluoroethyl)phosphate) + thiophene + heptane} have been determined at T = 298.15 K. All systems showed high solubility of thiophene in the ionic liquid and low solubility of heptane. The solute distribution coefficient and the selectivity were calculated for all systems. High values of selectivity were obtained. The experimental results have been correlated using NRTL model. The influence of ionic liquid structure on phase equilibria is discussed.

  18. Ligandless-dispersive liquid-liquid microextraction of trace amount of copper ions

    International Nuclear Information System (INIS)

    Mohammadi, Sayed Zia; Afzali, Daryoush; Baghelani, Yar Mohammad

    2009-01-01

    In the present work, a new ligandless-dispersive liquid-liquid microextraction (LL-DLLME) method has been developed for preconcentration trace amounts of copper as a prior step to its determination by flame atomic absorption spectrometry. In the proposed approach 1,2-dicholorobenzene and ethanol were used as extraction and dispersive solvents, respectively. Some factors influencing on the extraction efficiency of copper and its subsequent determination were studied and optimized, such as the extraction and dispersive solvent type and volume, pH of sample solution, extraction time and salting out effect. Under the optimal conditions, the calibration curve was linear in the range of 1.0 ng mL -1 -0.6 μg mL -1 of copper with R 2 = 0.9985. Detection limit was 0.5 ng mL -1 in original solution (3S b /m) and the relative standard deviation for seven replicate determination of 0.2 μg mL -1 copper was ±1.4%. The proposed method has been applied for determination of copper in standard and water samples with satisfactory results.

  19. The liquid-liquid extraction of chloro-(trichlorostannato)-rhodium(I/III) and -ruthenium (II) complexes from dilute hydrochloric acid into 4-methylpentan-2-one

    International Nuclear Information System (INIS)

    Wyrley-Birch, J.M.

    1984-10-01

    The effect of stannous chloride on the liquid-liquid extraction of rhodium and ruthenium from hydrochloric acid solutions into 4-methyl-pentan-2-one (MIBK)/hexane mixtures was studied in detail. Stannous chloride concentrations were found to considerably increase the efficiency of the extraction of rhodium and ruthenium into the organic phase. Chloro-(trichlorostannato)-rhodium (I/III) complexes were formed at room temperature. The rate of chloro-(trichlorostannato)-ruthenium (II) complex formation was extremely slow at room temperature, but increased on heating of the aqueous solutions. The amount of rhodium and ruthenium extracted into the organic phase depend on the Sn(II):M molar ratio, the HCl, H sup(+) and Cl sup(-) concentrations, as well as the equilibration time. A 119 Sn NMR study of the MIBK extracts, showed that the stoichiometry of the chloro-(trichlorostannato)-rhodium (I/III) complexes extracted into the organic phase was dependent on the Sn(II):Rh(III) molar ratio as well as the HCl, H sup(+) and Cl sup(-) concentrations in the aqueous phase. The predominant species observed in the organic phase from HCl solutions containing Sn(II):Rh(III) ratios >= 5:1, was shown to be an hydrido complex having the form [RhH(SnCl 3 ) 4 Cl] 3 sup(-) or [RhH(SnCl 3 ) 4 ]2 sup(-). An essentially quantitative separation of rhodium and ruthenium was achieved utilising the variation in the rates of rhodium-tin and ruthenium-tin complex formation

  20. Iron species determination by task-specific ionic liquid-based in situ solvent formation dispersive liquid-liquid microextraction combined with flame atomic absorption spectrometry.

    Science.gov (United States)

    Sadeghi, Susan; Ashoori, Vahid

    2017-10-01

    The task-specific ionic liquid (TSIL) of 1-ethyl-3-methylimidazolium bromide functionalized with 8-hydroxyquinoline was used as a chelating agent and extracting solvent for dispersive liquid-liquid microextraction and subsequent determination of Fe(III) by flame atomic absorption spectrometry. The in situ solvent formation of TSIL using KPF 6 provided the desired water-immiscible ionic liquid. The total Fe concentration could be determined after pre-oxidation of Fe(II) to Fe(III). Various factors affecting the proposed extraction procedure were optimized. The proposed analytical conditions were: sample pH 5, TSIL amount 0.3% (w/v), KPF 6 amount 0.15% (w/v), anti-sticking 0.1% (w/v) and salt concentration 5% (w/v). Under optimal conditions, the linear dynamic ranges for Fe(III) and total Fe were 20-80 and 20-110 ng mL -1 , respectively, with a detection limit of 6.9 ng mL -1 for Fe(III) and relative standard deviation of 2.2%. The proposed method was successfully applied to the determination of trace Fe(III) in water (underground, tap, refined water and artificial sea water) and beverage (apple, tomato, and tea) samples. The developed method offers advantages such as simplicity, ease of operation, and extraction of Fe(III) from aqueous solutions without the use of organic solvent. It was successfully applied for iron speciation in different real samples. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

  1. Dispersive liquid-liquid microextraction for metals enrichment: a useful strategy for improving sensitivity of laser-induced breakdown spectroscopy in liquid samples analysis.

    Science.gov (United States)

    Aguirre, M A; Selva, E J; Hidalgo, M; Canals, A

    2015-01-01

    A rapid and efficient Dispersive Liquid-Liquid Microextraction (DLLME) followed by Laser-Induced Breakdown Spectroscopy detection (LIBS) was evaluated for simultaneous determination of Cr, Cu, Mn, Ni and Zn in water samples. Metals in the samples were extracted with tetrachloromethane as pyrrolidinedithiocarbamate (APDC) complexes, using vortex agitation to achieve dispersion of the extractant solvent. Several DLLME experimental factors affecting extraction efficiency were optimized with a multivariate approach. Under optimum DLLME conditions, DLLME-LIBS method was found to be of about 4.0-5.5 times more sensitive than LIBS, achieving limits of detection of about 3.7-5.6 times lower. To assess accuracy of the proposed DLLME-LIBS procedure, a certified reference material of estuarine water was analyzed. Copyright © 2014 Elsevier B.V. All rights reserved.

  2. Recent development of ionic liquid membranes

    Directory of Open Access Journals (Sweden)

    Junfeng Wang

    2016-04-01

    Full Text Available The interest in ionic liquids (IL is motivated by its unique properties, such as negligible vapor pressure, thermal stability, wide electrochemical stability window, and tunability of properties. ILs have been highlighted as solvents for liquid–liquid extraction and liquid membrane separation. To further expand its application in separation field, the ionic liquid membranes (ILMs and its separation technology have been proposed and developed rapidly. This paper is to give a comprehensive overview on the recent applications of ILMs for the separation of various compounds, including organic compounds, mixed gases, and metal ions. Firstly, ILMs was classified into supported ionic liquid membranes (SILMs and quasi-solidified ionic liquid membranes (QSILMs according to the immobilization method of ILs. Then, preparation methods of ILMs, membrane stability as well as applications of ILMs in the separation of various mixtures were reviewed. Followed this, transport mechanisms of gaseous mixtures and organic compounds were elucidated in order to better understand the separation process of ILMs. This tutorial review intends to not only offer an overview on the development of ILMs but also provide a guide for ILMs preparations and applications. Keywords: Ionic liquid membrane, Supported ionic liquid membrane, Qusai-solidified ionic liquid membrane, Stability, Application

  3. Extraction of metals from liquid effluent using modified inorganic ion exchangers

    International Nuclear Information System (INIS)

    Hudson, M.J.

    1993-01-01

    Inorganic ion exchangers such as goethite, titanium (IV) oxide; silica and zeolites have been modified to examine the extraction of ruthenium; technetium and cobalt from liquid effluent. In addition, tin (IV) hydrogenphosphate and antimony hydrogenphosphate have been also examined in the modified and unmodified forms. It has been shown that some of the above reagents are able to remove the required metal ions from aqueous solution at the trace and mg L -1 levels. (author)

  4. Development of multi-residue method for the determination of pesticides in cereal matrices by isotopic dilution associated to liquid chromatography coupled to tandem mass spectrometry after pressurized liquid extraction

    International Nuclear Information System (INIS)

    El Mrabet, Khadija

    2008-01-01

    Pesticides are nowadays considered as toxic for human health. The maximal residues levels authorized in water and foodstuff are more and more strict. Therefore, selective analytical techniques are necessary for their identification and their quantification. The aim of this thesis was to develop a multi-residue method for the determination of pesticides by isotopic dilution associated to liquid chromatography (LC) coupled with tandem mass spectrometry (MS"2) after pressurized liquid extraction. In a first step, an analysis method of phenyl-ureas and triazines in groundwater by isotopic dilution associated to LC/MS"2 after solid phase extraction has been developed. The method has been validated and evaluated by participating to an inter-laboratory study. Concerning cereals, an extraction method of pesticides associated to an analysis by LC/MS"2 has been developed for thirty-eight pesticides representative of twenty-six chemicals families and fourteen labeled compounds in wheat. The analysis has been carried out in reversed phase chromatography. Separation and detection conditions have been optimized. A global analytical protocol consisting of a pressurized liquid extraction step using acetonitrile at 100 deg. C and at 100 bars and followed by purification step of the resulting extract on a polymeric sorbent was developed. The developed method enables to extract thirty-eight pesticides and fourteen labeled compounds from wheat with recovery yield about 85% (RSD =4%, n=3). Moreover, the results show that the application of isotopic dilution can be complex. Although some improvements need to be added regarding experimentation of aged matrices or contaminated samples, the potential of the method has been demonstrated. (author) [fr

  5. Parallel artificial liquid membrane extraction as an efficient tool for removal of phospholipids from human plasma.

    Science.gov (United States)

    Ask, Kristine Skoglund; Bardakci, Turgay; Parmer, Marthe Petrine; Halvorsen, Trine Grønhaug; Øiestad, Elisabeth Leere; Pedersen-Bjergaard, Stig; Gjelstad, Astrid

    2016-09-10

    Generic Parallel Artificial Liquid Membrane Extraction (PALME) methods for non-polar basic and non-polar acidic drugs from human plasma were investigated with respect to phospholipid removal. In both cases, extractions in 96-well format were performed from plasma (125μL), through 4μL organic solvent used as supported liquid membranes (SLMs), and into 50μL aqueous acceptor solutions. The acceptor solutions were subsequently analysed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) using in-source fragmentation and monitoring the m/z 184→184 transition for investigation of phosphatidylcholines (PC), sphingomyelins (SM), and lysophosphatidylcholines (Lyso-PC). In both generic methods, no phospholipids were detected in the acceptor solutions. Thus, PALME appeared to be highly efficient for phospholipid removal. To further support this, qualitative (post-column infusion) and quantitative matrix effects were investigated with fluoxetine, fluvoxamine, and quetiapine as model analytes. No signs of matrix effects were observed. Finally, PALME was evaluated for the aforementioned drug substances, and data were in accordance with European Medicines Agency (EMA) guidelines. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Extraction of Biomolecules Using Phosphonium-Based Ionic Liquids + K3PO4 Aqueous Biphasic Systems

    Science.gov (United States)

    Louros, Cláudia L. S.; Cláudio, Ana Filipa M.; Neves, Catarina M. S. S.; Freire, Mara G.; Marrucho, Isabel M.; Pauly, Jérôme; Coutinho, João A. P.

    2010-01-01

    Aqueous biphasic systems (ABS) provide an alternative and efficient approach for the extraction, recovery and purification of biomolecules through their partitioning between two liquid aqueous phases. In this work, the ability of hydrophilic phosphonium-based ionic liquids (ILs) to form ABS with aqueous K3PO4 solutions was evaluated for the first time. Ternary phase diagrams, and respective tie-lines and tie-lines length, formed by distinct phosphonium-based ILs, water, and K3PO4 at 298 K, were measured and are reported. The studied phosphonium-based ILs have shown to be more effective in promoting ABS compared to the imidazolium-based counterparts with similar anions. Moreover, the extractive capability of such systems was assessed for distinct biomolecules (including amino acids, food colourants and alkaloids). Densities and viscosities of both aqueous phases, at the mass fraction compositions used for the biomolecules extraction, were also determined. The evaluated IL-based ABS have been shown to be prospective extraction media, particularly for hydrophobic biomolecules, with several advantages over conventional polymer-inorganic salt ABS. PMID:20480041

  7. A novel extraction technique based on carbon nanotubes reinforced hollow fiber solid/liquid microextraction for the measurement of piroxicam and diclofenac combined with high performance liquid chromatography.

    Science.gov (United States)

    Song, Xin-Yue; Shi, Yan-Ping; Chen, Juan

    2012-10-15

    A novel design of carbon nanotubes reinforced hollow fiber solid/liquid phase microextraction (CNTs-HF-SLPME) was developed to determine piroxicam and diclofenac in different real water samples. Functionalized multi-walled carbon nanotubes (MWCNTs) were held in the pores of hollow fiber with sol-gel technology. The pores and lumen of carbon nanotubes reinforced hollow fiber were subsequently filled with a μL volume of organic solvent (1-octanol), and then the whole assembly was used for the extraction of the target analytes in direct immersion sampling mode. The target analytes were extracted from the sample by two extractants, one of which is organic solvent placed inside the pores and lumen of hollow fiber and the other one is CNTs held in the pores of hollow fiber. After extraction, the analytes were desorbed in acetonitrile and analyzed using high performance liquid chromatography. This novel extraction mode showed more excellent extraction performance in comparison with conventional hollow fiber liquid microextraction (without adding CNTs) and carbon nanotubes reinforced hollow fiber solid microextraction (CNTs held in the pores of hollow fiber, but no organic solvents placed inside the lumen of hollow fiber) under the respective optimum conditions. This method provided 47- and 184-fold enrichment factors for piroxicam and diclofenac, respectively, good inter-fiber repeatability and batch-to-batch reproducibility. Linearity was observed in the range of 20-960 μg L(-1) for piroxicam, and 10-2560 μg L(-1) for diclofenac, with correlation coefficients of 0.9985 and 0.9989, respectively. The limits of detection were 4.58 μg L(-1) for piroxicam and 0.40 μg L(-1) for diclofenac. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. Liquidity risk and the performance of UK mutual funds

    OpenAIRE

    Foran, Jason; O'Sullivan, Niall

    2014-01-01

    We examine the role of liquidity risk, both as a stock characteristic as well as systematic liquidity risk, in UK mutual fund performance for the first time. Using four alternative measures of stock liquidity we extract principal components across stocks in order to construct systematic or market liquidity factors. We find that on average UK mutual funds are tilted towards liquid stocks (except for small stock funds as might be expected) but that, counter-intuitively, liquidity as a stock cha...

  9. Development of an ionic-liquid-based dispersive liquid-liquid microextraction method for the determination of antichagasic drugs in human breast milk: Optimization by central composite design.

    Science.gov (United States)

    Padró, Juan M; Pellegrino Vidal, Rocío B; Echevarria, Romina N; Califano, Alicia N; Reta, Mario R

    2015-05-01

    Chagas disease constitutes a major public health problem in Latin America. Human breast milk is a biological sample of great importance for the analysis of therapeutic drugs, as unwanted exposure through breast milk could result in pharmacological effects in the nursing infant. Thus, the goal of breast milk drug analysis is to inquire to which extent a neonate may be exposed to a drug during lactation. In this work, we developed an analytical technique to quantify benznidazole and nifurtimox (the two antichagasic drugs currently available for medical treatment) in human breast milk, with a simple sample pretreatment followed by an ionic-liquid-based dispersive liquid-liquid microextraction combined with high-performance liquid chromatography and UV detection. For this technique, the ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate has been used as the "extraction solvent." A central composite design was used to find the optimum values for the significant variables affecting the extraction process: volume of ionic liquid, volume of dispersant solvent, ionic strength, and pH. At the optimum working conditions, the average recoveries were 77.5 and 89.7%, the limits of detection were 0.06 and 0.09 μg/mL and the interday reproducibilities were 6.25 and 5.77% for benznidazole and nifurtimox, respectively. The proposed methodology can be considered sensitive, simple, robust, accurate, and green. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Identification of fermentation inhibitors in wood hydrolyzates and removal of inhibitors by ion exchange and liquid-liquid extraction

    Science.gov (United States)

    Luo, Caidian

    1998-12-01

    Common methods employed in the ethanol production from biomass consist of chemical or enzymatic degradation of biomass into sugars and then fermentation of sugars into ethanol or other chemicals. However, some degradation products severely inhibit the fermentation processes and substantially reduce the efficiency of ethanol production. How to remove inhibitors from the reaction product mixture and increase the production efficiency are critical in the commercialization of any processes of energy from biomass. The present study has investigated anion exchange and liquid-liquid extraction as potential methods for inhibitor removal. An analytical method has been developed to identify the fermentation inhibitors in a hydrolyzate. The majority of inhibitors present in hybrid poplar hydrolyzate have positively been identified. Ion exchange with weak basic Dowex-MWA-1 resin has been proved to be an effective mean to remove fermentation inhibitors from hybrid poplar hydrolyzate and significantly increase the fermentation productivity. Extraction with n-butanol might be a preferred way to remove inhibitors from wood hydrolyzates and improve the fermentability of sugars in the hydrolyzates. n-Butanol also removes some glucose, mannose and xylose from the hydrolyzate. Inhibitor identification reveals that lignin and sugar degradation compounds including both aromatic and aliphatic aldehydes and carboxylic acids formed in hydrolysis, plus fatty acids and other components from wood extractives are major fermentation inhibitors in Sacchromyces cerevisiae fermentation. There are 35 components identified as fermentation inhibitors. Among them, 4-hydroxy benzoic acid, 3,4-dihydroxy benzoic acid, syringic acid, syringaldehyde, and ferulic acid are among the most abundant aromatic inhibitors in hybrid poplar hydrolyzate. The conversion of aldehyde groups into carboxylic acid groups in the nitric acid catalyzed hydrolysis reduces the toxicity of the hydrolyzate. A wide spectrum of

  11. Parallel artificial liquid membrane extraction as an efficient tool for removal of phospholipids from human plasma

    DEFF Research Database (Denmark)

    Ask, Kristine Skoglund; Bardakci, Turgay; Parmer, Marthe Petrine

    2016-01-01

    Generic Parallel Artificial Liquid Membrane Extraction (PALME) methods for non-polar basic and non-polar acidic drugs from human plasma were investigated with respect to phospholipid removal. In both cases, extractions in 96-well format were performed from plasma (125μL), through 4μL organic...

  12. Simultaneous micro-electromembrane extractions of anions and cations using multiple free liquid membranes and acceptor solutions

    Czech Academy of Sciences Publication Activity Database

    Kubáň, Pavel; Boček, Petr

    2016-01-01

    Roč. 908, FEB (2016), s. 113-120 ISSN 0003-2670 R&D Projects: GA ČR(CZ) GA13-05762S Institutional support: RVO:68081715 Keywords : free liquid membranes * micro-electromembrane extraction * simultaneous extractions Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.950, year: 2016

  13. Simultaneous micro-electromembrane extractions of anions and cations using multiple free liquid membranes and acceptor solutions

    Czech Academy of Sciences Publication Activity Database

    Kubáň, Pavel; Boček, Petr

    2016-01-01

    Roč. 908, FEB (2016), s. 113-120 ISSN 0003-2670 R&D Projects: GA ČR(CZ) GA13-05762S Institutional support: RVO:68081715 Keywords : free liquid membranes * micro-electromembrane extraction * simultaneous extractions Subject RIV: CB - Analytical Chemistry , Separation Impact factor: 4.950, year: 2016

  14. Homogeneous liquid-liquid extraction (HoLLE) via flotation combined with gas chromatography-flame ionization detection as a very simple, rapid and sensitive method for the determination of fenitrothion in water samples.

    Science.gov (United States)

    Mashayekhi, Hossein Ali

    2013-01-01

    Homogeneous liquid-liquid extraction via flotation assistance (HoLLE-FA) and gas chromatography-flame ionization detection (GC-FID) was presented for the extraction and determination of fenitrothion in water samples. In this work, a rapid, simple and efficient HoLLE-FA method was developed based on applying low-density organic solvents without employing centrifugation. A special extraction cell was designed to facilitate the collection of low-density solvent extraction in the determination of fenitrothion in water samples. The water sample solution was added into an extraction cell that contained an appropriate mixture of extraction and homogeneous solvents. By using air flotation, the organic solvent was collected at the conical part of the designed cell. Under the optimum conditions, the method performance was studied in terms of the linear dynamic range (LDR from 1.0 up to 100 μg L⁻¹), linearity (r² > 0.998), and precision (repeatability extraction and determination of fenitrothion in three different water samples.

  15. The thermophysical properties of metallic liquids

    CERN Document Server

    Iida, Takamichi

    2015-01-01

    The main purpose of materials science and engineering is to make the best use of all the elements in the periodic table. This leads to the effective use and conservation of natural resources. For this purpose, in any liquid metallic processing operation, accurate data for the thermophysical properties of all metallic liquids (i.e. liquid metals, semimetals, and semiconductors) is needed. However, in addition, a clear understanding of the essence of their thermophysical properties, based on these data, is indispensable. The second volume continues from the first volume to provide explanations for the thermophysical properties of metallic liquids. The two volumes identify new dimensionless parameters, extracted from the velocity of sound. In spite of being simple parameters, they provide useful information on the nature and behaviour of metallic liquids. This volume covers several basic concepts needed to understand the thermophysical properties of metallic liquids and for developing reliable models to accurate...

  16. Effect of pressurized liquids on extraction of antioxidants from Chlorella vulgaris.

    Science.gov (United States)

    Cha, Kwang Hyun; Kang, Suk Woo; Kim, Chul Young; Um, Byung Hun; Na, Ye Rim; Pan, Cheol-Ho

    2010-04-28

    Chlorella vulgaris is a green microalga that contains various antioxidants, such as carotenoids and chlorophylls. In this study, antioxidants from C. vulgaris were extracted using pressurized liquid extraction (PLE), which has been recently used for bioactive compound extraction. The antioxidant capacity of individual compounds in chlorella was determined by online HPLC ABTS(*+) analysis. According to the antioxidant analysis of total extracts, the extraction yield, radical scavenging activity, and phenolic compounds using PLE were relatively high compared to those obtained using maceration or ultrasound-assisted extraction. On the basis of online HPLC ABTS(*+) analysis, the 15 major antioxidants from chlorella extracts were identified as hydrophilic compounds, lutein and its isomers, chlorophylls, and chlorophyll derivatives. Using PLE at high temperature (85-160 degrees C) significantly increased antioxidant extraction from chlorella, improving the formation of hydrophilic compounds and yielding more antioxidative chlorophyll derivatives. Online HPLC ABTS(*+) analysis was a useful tool for the separation of main antioxidants from PLE extracts and allowed the simultaneous measurement of their antioxidant capacity, which clearly showed that PLE is an excellent method for extracting antioxidants from C. vulgaris.

  17. Application of Ionic Liquids in Hydrometallurgy

    Science.gov (United States)

    Park, Jesik; Jung, Yeojin; Kusumah, Priyandi; Lee, Jinyoung; Kwon, Kyungjung; Lee, Churl Kyoung

    2014-01-01

    Ionic liquids, low temperature molten salts, have various advantages manifesting themselves as durable and environmentally friendly solvents. Their application is expanding into various fields including hydrometallurgy due to their unique properties such as non-volatility, inflammability, low toxicity, good ionic conductivity, and wide electrochemical potential window. This paper reviews previous literatures and our recent results adopting ionic liquids in extraction, synthesis and processing of metals with an emphasis on the electrolysis of active/light, rare earth, and platinum group metals. Because the research and development of ionic liquids in this area are still emerging, various, more fundamental approaches are expected to popularize ionic liquids in the metal manufacturing industry. PMID:25177864

  18. Extraction of rare earth elements with organophosphorus extractants as carriers in supported liquid membranes

    International Nuclear Information System (INIS)

    Kopunec, R.; Benitez, J.C.

    1991-01-01

    The membrane extraction of Y, Ce, Eu, Tm and their binary mixtures Ce-Y, Ce-Eu, Ce-Tm with supported liquid membranes containing TBP and HDEHP as carriers in decane-dodecane hydrocarbon solvent, has been studied. Upon extraction with TBP aqueous nitrate solutions of rare earth elements (REE) were used as feed phase. In some cases they also contained EDTA or DCTA. In most cases, the receiving phase was an aqueous solution of EDTA. Extraction with HDEHP was performed from nitrate and chloride solutions and the receiving phase was the corresponding dilute acid. Pertraction of an element through a membrane was studied as a function of time and of initial composition of phases. The results are presented in the following forms: flux of metal through membrane, coefficients of permeability, separation factors and effective diffusion coefficients. (author) 24 refs.; 8 figs.; 3 tabs

  19. Separation by liquid-liquid extraction of actinides(III) from lanthanides(III) using new molecules: the picolinamides

    International Nuclear Information System (INIS)

    Cordier, P.Y.

    1996-07-01

    In the field of long-lived radionuclides separation from waste generated during spent fuel reprocessing, the picolinamides have been chosen as potential extractants for the selective extraction of actinides (III) from lanthanides (III). The first studies initiated on the most simple molecule of the picolinamide family, namely 2-pyridinecarboxamide, pointed out that in an aqueous media the complexation stability constant between this ligand and Am(III) is roughly 10 times higher than the ones corresponding to Ln(III). The synthesis of lipophilic derivatives of 2-pyridinecarboxamide leaded to extraction experiments. The extraction of metallic cation by lipophilic picolinamides, according to a solvatation mechanism, is strongly dependent on the nature of the amide function: a primary amide function (group I) leads to a good extraction; on the contrary, there is a decrease for secondary (group II) and tertiary (group III) amide functions. From a theoretical point of view, this work leads finally to the following conclusions: confirmation of the importance of the presence of soft donor atoms within the extractants (nitrogen in our case) for An(III)/Ln(III). Also, sensitivity of this soft donor atom regarding the protonation reaction; prevalence in our case of the affinity of the extractant for the metallic cation over the lipophilia of the extractant to ensure good distribution coefficients. The extraction and Am(III)/Ln(III) separation performances of the picolinamides from pertechnetic media leads to the design of a possible flowsheet for the reprocessing of high level liquid waste, with the new idea of an integrated technetium reflux. (author)

  20. Analysis of drugs of abuse in human plasma by dispersive liquid-liquid microextraction and high-performance liquid chromatography.

    Science.gov (United States)

    Fernández, P; Regenjo, M; Bermejo, A M; Fernández, A M; Lorenzo, R A; Carro, A M

    2015-04-01

    Opioids and cocaine are widely used at present, both for recreational purposes and as drugs of abuse. This raises the need to develop new analytical methods specifically designed for the simultaneous detection of several drugs of abuse in biological samples. In this work, dispersive liquid-liquid microextraction (DLLME) was assessed as a new sample treatment for the simultaneous extraction of morphine (MOR), 6-acetylmorphine (6AM), cocaine (COC), benzoylecgonine (BZE) and methadone (MET) from human plasma. Preliminary assays were done before developing an experimental design based on a Uniform Network Doehlert which allowed the optimum extraction conditions to be identified, namely: a volume of extractant solvent (chloroform) and dispersant solvent (acetonitrile) of 220 µl and 3.2 ml, respectively; 0.2 g of NaCl as a salting-out additive; pH 10.6 and ultrasound stirring for 3.5 min. The resulting extracts were analyzed by high-performance liquid chromatography with photodiode array detection (HPLC-PDA), using an XBridge® RP18 column (250 × 4.6 mm i.d., 5 µm particle size). Calibration graphs were linear over the concentration range 0.1-10 µg ml⁻¹, and detection limits ranged from 13.9 to 28.5 ng ml⁻¹. Precision calculated at three different concentration levels in plasma was included in the range 0.1-6.8% RSD. Recoveries of the five drugs were all higher than 84% on average. Finally the proposed method was successfully applied to 22 plasma samples from heroin, cocaine and/or methadone users, and the most frequently detected drug was benzoylecgonine, followed by methadone, cocaine and morphine. Copyright © 2014 John Wiley & Sons, Ltd.

  1. Simultaneous extraction and quantification of albendazole and triclabendazole using vortex-assisted hollow-fiber liquid-phase microextraction combined with high-performance liquid chromatography.

    Science.gov (United States)

    Asadi, Mohammad; Haji Shabani, Ali Mohammad; Dadfarnia, Shayessteh

    2016-06-01

    A novel, simple, and rapid vortex-assisted hollow-fiber liquid-phase microextraction method was developed for the simultaneous extraction of albendazole and triclabendazole from various matrices before their determination by high-performance liquid chromatography with fluorescence detection. Several factors influencing the microextraction efficiency including sample pH, nature and volume of extraction solvent, ionic strength, vortex time, and sample volume were investigated and optimized. Under the optimal conditions, the limits of detection were 0.08 and 0.12 μg/L for albendazole and triclabendazole, respectively. The calibration curves were linear in the concentration ranges of 0.3-50.0 and 0.4-50.0 μg/L with the coefficients of determination of 0.9999 and 0.9995 for albendazole and triclabendazole, respectively. The interday and intraday relative standard deviations for albendazole and triclabendazole at three concentration levels (1.0, 10.0, and 30.0 μg/L) were in the range of 6.0-11.0 and 5.0-7.9%, respectively. The developed method was successfully applied to determine albendazole and triclabendazole in water, milk, honey, and urine samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Extraction of acetanilides in rice using ionic liquid-based matrix solid phase dispersion-solvent flotation.

    Science.gov (United States)

    Zhang, Liyuan; Wang, Changyuan; Li, Zuotong; Zhao, Changjiang; Zhang, Hanqi; Zhang, Dongjie

    2018-04-15

    Ionic liquid-based matrix solid phase dispersion-solvent flotation coupled with high performance liquid chromatography was developed for the determination of the acetanilide herbicides, including metazachlor, propanil, alachlor, propisochlor, pretilachlor, and butachlor in rice samples. Some experimental parameters, including the type of dispersant, the mass ratio of dispersant to sample, pH of sample solution, the type of extraction solvent, the type of ionic liquid, flotation time, and flow rate of N 2 were optimized. The average recoveries of the acetanilide herbicides at spiked concentrations of 50, 125, and 250 µg/kg ranged from 89.4% to 108.7%, and relative standard deviations were equal to or lower than 7.1%, the limits of quantification were in the range of 38.0 to 84.7 µg/kg. Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. Automated on-line liquid–liquid extraction system for temporal mass spectrometric analysis of dynamic samples

    Energy Technology Data Exchange (ETDEWEB)

    Hsieh, Kai-Ta; Liu, Pei-Han [Department of Applied Chemistry, National Chiao Tung University, 1001 University Rd, Hsinchu, 300, Taiwan (China); Urban, Pawel L. [Department of Applied Chemistry, National Chiao Tung University, 1001 University Rd, Hsinchu, 300, Taiwan (China); Institute of Molecular Science, National Chiao Tung University, 1001 University Rd, Hsinchu, 300, Taiwan (China)

    2015-09-24

    Most real samples cannot directly be infused to mass spectrometers because they could contaminate delicate parts of ion source and guides, or cause ion suppression. Conventional sample preparation procedures limit temporal resolution of analysis. We have developed an automated liquid–liquid extraction system that enables unsupervised repetitive treatment of dynamic samples and instantaneous analysis by mass spectrometry (MS). It incorporates inexpensive open-source microcontroller boards (Arduino and Netduino) to guide the extraction and analysis process. Duration of every extraction cycle is 17 min. The system enables monitoring of dynamic processes over many hours. The extracts are automatically transferred to the ion source incorporating a Venturi pump. Operation of the device has been characterized (repeatability, RSD = 15%, n = 20; concentration range for ibuprofen, 0.053–2.000 mM; LOD for ibuprofen, ∼0.005 mM; including extraction and detection). To exemplify its usefulness in real-world applications, we implemented this device in chemical profiling of pharmaceutical formulation dissolution process. Temporal dissolution profiles of commercial ibuprofen and acetaminophen tablets were recorded during 10 h. The extraction-MS datasets were fitted with exponential functions to characterize the rates of release of the main and auxiliary ingredients (e.g. ibuprofen, k = 0.43 ± 0.01 h{sup −1}). The electronic control unit of this system interacts with the operator via touch screen, internet, voice, and short text messages sent to the mobile phone, which is helpful when launching long-term (e.g. overnight) measurements. Due to these interactive features, the platform brings the concept of the Internet-of-Things (IoT) to the chemistry laboratory environment. - Highlights: • Mass spectrometric analysis normally requires sample preparation. • Liquid–liquid extraction can isolate analytes from complex matrices. • The proposed system automates

  4. Automated on-line liquid–liquid extraction system for temporal mass spectrometric analysis of dynamic samples

    International Nuclear Information System (INIS)

    Hsieh, Kai-Ta; Liu, Pei-Han; Urban, Pawel L.

    2015-01-01

    Most real samples cannot directly be infused to mass spectrometers because they could contaminate delicate parts of ion source and guides, or cause ion suppression. Conventional sample preparation procedures limit temporal resolution of analysis. We have developed an automated liquid–liquid extraction system that enables unsupervised repetitive treatment of dynamic samples and instantaneous analysis by mass spectrometry (MS). It incorporates inexpensive open-source microcontroller boards (Arduino and Netduino) to guide the extraction and analysis process. Duration of every extraction cycle is 17 min. The system enables monitoring of dynamic processes over many hours. The extracts are automatically transferred to the ion source incorporating a Venturi pump. Operation of the device has been characterized (repeatability, RSD = 15%, n = 20; concentration range for ibuprofen, 0.053–2.000 mM; LOD for ibuprofen, ∼0.005 mM; including extraction and detection). To exemplify its usefulness in real-world applications, we implemented this device in chemical profiling of pharmaceutical formulation dissolution process. Temporal dissolution profiles of commercial ibuprofen and acetaminophen tablets were recorded during 10 h. The extraction-MS datasets were fitted with exponential functions to characterize the rates of release of the main and auxiliary ingredients (e.g. ibuprofen, k = 0.43 ± 0.01 h"−"1). The electronic control unit of this system interacts with the operator via touch screen, internet, voice, and short text messages sent to the mobile phone, which is helpful when launching long-term (e.g. overnight) measurements. Due to these interactive features, the platform brings the concept of the Internet-of-Things (IoT) to the chemistry laboratory environment. - Highlights: • Mass spectrometric analysis normally requires sample preparation. • Liquid–liquid extraction can isolate analytes from complex matrices. • The proposed system automates the

  5. Rapid determination of some beta-blockers in complicated matrices by tandem dispersive liquid-liquid microextraction followed by high performance liquid chromatography.

    Science.gov (United States)

    Hemmati, Maryam; Asghari, Alireza; Bazregar, Mohammad; Rajabi, Maryam

    2016-11-01

    In this research work, an efficient tandem dispersive liquid-liquid microextraction (TDLLME) procedure coupled with high performance liquid chromatography-ultraviolet detection (HPLC-UV) was successfully applied for the determination of beta-blockers in human plasma and pharmaceutical wastewater samples. High clean-up and preconcentration factor are easily and rapidly feasible via this novel, cheap, and safe microextraction method, leading to high quality experimental data. It consists of two sequential dispersive liquid-liquid microextraction methods, accomplished via air/ultrasonic agitation and air agitation, respectively. In order to enrich the optimal values for the mentioned procedures, the Box-Behnken design (BBD) combined with the desirability function (DF) was used. The optimum values were found to be 11.0 % (w/v) of the salt amount, an initial pH value of 12.0, 103 μL of organic extractant phase, and 45 μL of aqueous extractant phase with pH value of 2.0, resulted in reasonable recovery percentages with a logical desirability. Under optimal experimental conditions, good linear ranges (3-2000 ng mL -1 for metoprolol and 2.5-2500 ng mL -1 for propranolol with the correlation of determinations (R 2 s) higher than 0.99) and low limits of detection (0.8 and 1.0 ng mL -1 for propranolol and metoprolol, respectively) were obtainable. Also, TDLLME-HPLC-UV provided good proper repeatabilities (relative standard deviations (RSDs) below 5.7 %, n = 3) and high enrichment factors (EFs) of 75-100. Graphical abstract TDLLME of beta-blockers from complicated matrices.

  6. A systematic review and meta-analysis of pneumonia associated with thin liquid vs. thickened liquid intake in patients who aspirate.

    Science.gov (United States)

    Kaneoka, Asako; Pisegna, Jessica M; Saito, Hiroki; Lo, Melody; Felling, Katey; Haga, Nobuhiko; LaValley, Michael P; Langmore, Susan E

    2017-08-01

    To investigate whether drinking thin liquids with safety strategies increases the risk for pneumonia as compared with thickened liquids in patients who have demonstrated aspiration of thin liquids. Seven electronic databases, one clinical register, and three conference archives were searched. No language or publication date restrictions were imposed. Reference lists were scanned and authors and experts in the field were contacted. A blind review was performed by two reviewers for published or unpublished randomized controlled trials and prospective non-randomized trials comparing the incidence of pneumonia with intake of thin liquids plus safety strategies vs. thickened liquids in adult patients who aspirated on thin liquids. The data were extracted from included studies. Odds ratios (OR) for pneumonia were calculated from the extracted data. Risk of bias was also assessed with the included published trials. Seven studies out of 2465 studies including 650 patients met the inclusion criteria. All of the seven studies excluded patients with more than one known risk factor for pneumonia. Six studies compared thin water protocols to thickened liquids for pneumonia prevention. A meta-analysis was done on the six studies, showing no significant difference for pneumonia risk (OR = 0.82; 95% CI = 0.05-13.42; p = 0.89). There was no significant difference in the risk of pneumonia in aspirating patients who took thin liquids with safety strategies compared with those who took thickened liquids only. This result, however, is generalizable only for patients with low risk of pneumonia.

  7. Optimization of pressurized liquid extraction by response surface methodology of Goji berry (Lycium barbarum L.) phenolic bioactive compounds.

    Science.gov (United States)

    Tripodo, Giusy; Ibáñez, Elena; Cifuentes, Alejandro; Gilbert-López, Bienvenida; Fanali, Chiara

    2018-01-03

    Pressurized liquid extraction (PLE) has been used for the first time in this work to extract phenolic compounds from Goji berries according to a multilevel factorial design using response surface methodology. The global yield (% w/dw, weight/dry-weight), total phenolic content (TPC), total flavonoid (TF) and antioxidant activity (determined via ABTS assay, expressed as TEAC value) were used as response variables to study the effects of temperature (50-180°C) and green solvent composition (mixtures of ethanol/water). Phenolic compounds characterization was performed by high performance liquid chromatography-diode array detector-tandem mass spectrometry (HPLC-DAD-MS/MS). The optimum PLE conditions predicted by the model were as follows: 180°C and 86% ethanol in water with a good desirability value of 0.815. The predicted conditions were confirmed experimentally and once the experimental design was validated for commercial fruit samples, the PLE extraction of phenolic compounds from three different varieties of fruit samples (Selvatico mongolo, Bigol, and Polonia) was performed. Nine phenolic compounds were tentatively identified in these extracts, including phenolic acids and their derivatives, and flavonols. The optimized PLE conditions were compared to a conventional solid-liquid extraction, demonstrating that PLE is a useful alternative to extract phenolic compounds from Goji berry. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. New sample preparation method based on task-specific ionic liquids for extraction and determination of copper in urine and wastewater.

    Science.gov (United States)

    Trtić-Petrović, Tatjana; Dimitrijević, Aleksandra; Zdolšek, Nikola; Đorđević, Jelena; Tot, Aleksandar; Vraneš, Milan; Gadžurić, Slobodan

    2018-01-01

    In this study, four hydrophilic ionic liquids (ILs) containing 1-alkyl-3-methylimidazolim cation and either salicylate or chloride anions were synthetized and studied as new task-specific ionic liquids (TSILs) suitable for aqueous biphasic system (ABS) formation and selective one-step extraction of copper(II). TSILs are designed so that the anion is responsible for forming the complex with metal(II) and preventing hydrolysis of metal cations at very strong alkaline pH, whereas the cation is responsible for selective extraction of metal(II)-salicylate complexes. It was found that 1-butyl-3-methylimidazolium salicylate could be used for selective extraction of Cu(II) in the presence of Zn(II), Cd(II), and Pb(II) at very alkaline solution without metal hydroxide formation. It was assumed that formation of metal(II)-salicylate complexes prevents the hydrolysis of the metal ions in alkaline solutions. The determined stability constants for Cu(II)-salicylate complexes, where salicylate was derived from different ionic liquids, indicated that there was no significant influence of the cation of the ionic liquid on the stability of the complexes. The ABS based on 1-butyl-3-methylimidazolium salicylate has been applied as the sample preparation step prior to voltammetric determination of Cu(II). The effect of volume of aqueous sample and IL and extraction time were investigated and optimum extraction conditions were determined. The obtained detection limits were 8 ng dm -3 . The optimized method was applied for the determination of Cu(II) in tap water, wastewater, and urine. The study indicated that application of the ABS based on 1-butyl-3-methylimidazolium salicylate ionic liquid could be successfully applied as the sample preparation method for the determination of Cu(II) from various environmental samples. Graphical abstract Aqueous biphasic system based on task-specific ionic liquid as a sample pretreatment for selective determination of Cu(II) in biological and

  9. Liquid-liquid phase transition in Stillinger-Weber silicon

    International Nuclear Information System (INIS)