WorldWideScience

Sample records for dispersed phase liquid

  1. Liquid-liquid and liquid-solid phase separation and flocculation for a charged colloidal dispersion

    International Nuclear Information System (INIS)

    Lai, S.K.; Wu, K.L.

    2002-01-01

    We model the intercolloidal interaction by a hard-sphere Yukawa repulsion to which is added the long-range van der Waals attraction. In comparison with the Derjaguin-Landau-Verwey-Overbeek repulsion, the Yukawa repulsion explicitly incorporates the spatial correlations between colloids and small ions. As a result, the repulsive part can be expressed analytically and has a coupling strength depending on the colloidal volume fraction. By use of this two-body potential of mean force and in conjunction with a second-order thermodynamic perturbation theory, we construct the colloidal Helmholtz free energy and use it to calculate the thermodynamic quantities, pressure and chemical potential, needed in the determination of the liquid-liquid and liquid-solid phase diagrams. We examine, in an aqueous charged colloidal dispersion, the effects of the Hamaker constant and particle size on the conformation of a stable liquid-liquid phase transition calculated with respect to the liquid-solid coexistence phases. We find that there exists a threshold Hamaker constant or particle size whose value demarcates the stable liquid-liquid coexistence phases from their metastable counterparts. Applying the same technique and using the energetic criterion, we extend our calculations to study the flocculation phenomenon in aqueous charged colloids. Here, we pay due attention to determining the loci of a stability curve stipulated for a given temperature T 0 , and obtain the parametric phase diagram of the Hamaker constant vs the coupling strength or, at given surface potential, the particle size. By imposing T 0 to be the critical temperature T c , i.e., setting k B T 0 (=k B T c ) equal to a reasonable potential barrier, we arrive at the stability curve that marks the irreversible reversible phase transition. The interesting result is that there occurs a minimum size for the colloidal particles below (above) which the colloidal dispersion is driven to an irreversible (reversible) phase

  2. Effect of silica nanoparticles on the phase inversion of liquid-liquid dispersions

    International Nuclear Information System (INIS)

    Asadabadi, Maliheh Raji; Abolghasemi, Hossein; Nasab, Payman Davoodi; Maragheh, Mohammad Ghannadi

    2013-01-01

    The effect of silica nanoparticles on phase inversion of liquid-liquid dispersions in a stirred vessel was investigated. The studied systems were toluene dispersed in water and vice versa. In the first set of experiments, phase inversion behavior of systems without Silica nanoparticles was evaluated and subsequent experiments were conducted in the presence of the nanoparticles. For this purpose, Silica nanoparticles of different concentrations (0.01, 0.03, 0.05, 0.07 wt%) were dispersed in water. The nanofluid stability was examined using an ultraviolet-visible (UV-vis) spectrophotometer. The results indicated that increase in silica nanoparticle concentrations up to 0.07 wt% led to increase in agitation speed of phase inversion 43-53.5% and 38.5-45% in the case of O/W and W/O dispersions, respectively. Consequently, the tendency of dispersions to inversion diminished as nanoparticle concentrations increased. Finally, 0.05 wt% of silica nanoparticle was selected as the optimum on the range studied

  3. Flashing liquid jets and two-phase droplet dispersion

    International Nuclear Information System (INIS)

    Cleary, Vincent; Bowen, Phil; Witlox, Henk

    2007-01-01

    The large-scale release of a liquid contained at upstream conditions above its local atmospheric boiling point is a scenario often given consideration in process industry risk analysis. Current-hazard quantification software often employs simplistic equilibrium two-phase approaches. Scaled water experiments have been carried out measuring droplet velocity and droplet size distributions for a range of exit orifice aspect ratios (L/d) and conditions representing low to high superheat. 2D Phase-Doppler Anemometry has been utilised to characterise droplet kinematics and spray quality. Droplet size correlations have been developed for non-flashing, the transition between non-flashing and flashing, and fully flashing jets. Using high-speed shadowography, transition between regimes is defined in terms of criteria identified in the external flow structure. An overview companion paper provides a wider overview of the problem and reports implementation of these correlations into consequence models and subsequent validation. The fluid utilised throughout is water, hence droplet correlations are developed in non-dimensional form to allow extrapolation to other fluids through similarity scaling, although verification of model performance for other fluids is required in future studies. Data is reduced via non-dimensionalisation in terms of the Weber number and Jakob number, essentially representing the fluid mechanics and thermodynamics of the system, respectively. A droplet-size distribution correlation has also been developed, conveniently presented as a volume undersize distribution based on the Rosin-Rammler distribution. Separate correlations are provided for sub-cooled mechanical break-up and fully flashing jets. This form of correlation facilitates rapid estimates of likely mass rainout quantities, as well as full distribution information for more rigorous two-phase thermodynamic modelling in the future

  4. Investigation of liquid phase axial dispersion in Taylor bubble flow by radiotracer residence time distribution analysis

    Directory of Open Access Journals (Sweden)

    Jin J.H.

    2013-05-01

    Full Text Available A gas-liquid Taylor bubble flow occurs in small diameter channels in which gas bubbles are separated by slugs of pure liquid. This type of flow regime is well suited for solid catalyzed gas-liquid reactors in which the reaction efficiency is a strong function of axial dispersion in the regions of pure liquid. This paper presents an experimental study of liquid phase axial dispersion in a Taylor bubble flow developed in a horizontal tube using high speed photography and radiotracer residence time distribution (RTD analysis. A parametric dependence of axial dispersion on average volume fraction of gas phase was also investigated by varying the relative volumetric flow rates of the two phases. 137mBa produced from a 137Cs/137mBa radionuclide generator was used as radiotracer and measurements were made using the NaI(Tl scintillation detectors. Validation of 137mBa in the form of barium chloride as aqueous phase radiotracer was also carried out. Axial Dispersion Model (ADM was used to simulate the hydrodynamics of the system and the results of the experiment are presented. It was observed that the system is characterized by very high values of Peclet Number (Pe∼102 which reveals an approaching plug type flow. The experimental and model estimated values of mean residence times were observed in agreement with each other.

  5. Lanthanide Phytanates: Liquid-Crystalline Phase Behavior, Colloidal Particle Dispersions, and Potential as Medical Imaging Agents

    Energy Technology Data Exchange (ETDEWEB)

    Conn, Charlotte E.; Panchagnula, Venkateswarlu; Weerawardena, Asoka; Waddington, Lynne J.; Kennedy, Danielle F.; Drummond, Calum J. (CSIRO/MHT); (CSIRO/MSE)

    2010-08-23

    Lanthanide salts of phytanic acid, an isoprenoid-type amphiphile, have been synthesized and characterized. Elemental analysis and FTIR spectroscopy were used to confirm the formed product and showed that three phytanate anions are complexed with one lanthanide cation. The physicochemical properties of the lanthanide phytanates were investigated using DSC, XRD, SAXS, and cross-polarized optical microscopy. Several of the hydrated salts form a liquid-crystalline hexagonal columnar mesophase at room temperature, and samarium(III) phytanate forms this phase even in the absence of water. Select lanthanide phytanates were dispersed in water, and cryo-TEM images indicate that some structure has been retained in the dispersed phase. NMR relaxivity measurements were conducted on these systems. It has been shown that a particulate dispersion of gadolinium(III) phytanate displays proton relaxivity values comparable to those of a commercial contrast agent for magnetic resonance imaging and a colloidal dispersion of europium(III) phytanate exhibits the characteristics of a fluorescence imaging agent.

  6. Lanthanide Phytanates: Liquid-Crystalline Phase Behavior, Colloidal Particle Dispersions, and Potential as Medical Imaging Agents

    International Nuclear Information System (INIS)

    Conn, Charlotte E.; Panchagnula, Venkateswarlu; Weerawardena, Asoka; Waddington, Lynne J.; Kennedy, Danielle F.; Drummond, Calum J.

    2010-01-01

    Lanthanide salts of phytanic acid, an isoprenoid-type amphiphile, have been synthesized and characterized. Elemental analysis and FTIR spectroscopy were used to confirm the formed product and showed that three phytanate anions are complexed with one lanthanide cation. The physicochemical properties of the lanthanide phytanates were investigated using DSC, XRD, SAXS, and cross-polarized optical microscopy. Several of the hydrated salts form a liquid-crystalline hexagonal columnar mesophase at room temperature, and samarium(III) phytanate forms this phase even in the absence of water. Select lanthanide phytanates were dispersed in water, and cryo-TEM images indicate that some structure has been retained in the dispersed phase. NMR relaxivity measurements were conducted on these systems. It has been shown that a particulate dispersion of gadolinium(III) phytanate displays proton relaxivity values comparable to those of a commercial contrast agent for magnetic resonance imaging and a colloidal dispersion of europium(III) phytanate exhibits the characteristics of a fluorescence imaging agent.

  7. Investigation of metal-matrix composite containing liquid-phase dispersion

    Czech Academy of Sciences Publication Activity Database

    Strunz, Pavel; Mukherji, D.; Gilles, R.; Geue, T.; Rösler, J.

    2012-01-01

    Roč. 340, 012098 (2012), s. 1-15 ISSN 1742-6588. [5th European Conference on Neutron Scattering. Praha, 17.07.2011-21.07.2011] R&D Projects: GA MPO FR-TI1/378 Grant - others:European Commission(XE) RII3-CT-2003-505925 Program:FP6 Institutional support: RVO:61389005 Keywords : metal-matrix composite * liquid-phase dispersion * strengthening * neutron diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism http://iopscience.iop.org/1742-6596/340/1/012098

  8. 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.

  9. 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.

  10. [Detecting Thallium in Water Samples using Dispersive Liquid Phase Microextraction-Graphite Furnace Atomic Absorption Spectroscopy].

    Science.gov (United States)

    Zhu, Jing; Li, Yan; Zheng, Bo; Tang, Wei; Chen, Xiao; Zou, Xiao-li

    2015-11-01

    To develope a method of solvent demulsification dispersive liquid phase microextraction (SD-DLPME) based on ion association reaction coupled with graphite furnace atomic absorption spectroscopy (GFAAS) for detecting thallium in water samples. Methods Thallium ion in water samples was oxidized to Tl(III) with bromine water, which reacted with Cl- to form TlCl4-. The ionic associated compound with trioctylamine was obtained and extracted. DLPME was completed with ethanol as dispersive solvent. The separation of aqueous and organic phase was achieved by injecting into demulsification solvent without centrifugation. The extractant was collected and injected into GFAAS for analysis. With palladium colloid as matrix modifier, a two step drying and ashing temperature programming process was applied for high precision and sensitivity. The linear range was 0.05-2.0 microg/L, with a detection limit of 0.011 microg/L. The relative standard derivation (RSD) for detecting Tl in spiked water sample was 9.9%. The spiked recoveries of water samples ranged from 94.0% to 103.0%. The method is simple, sensitive and suitable for batch analysis of Tl in water samples.

  11. Magnetic matrix solid phase dispersion assisted dispersive liquid liquid microextraction of ultra trace polychlorinated biphenyls in water prior to GC-ECD determination

    International Nuclear Information System (INIS)

    Diao, Chunpeng; Li, Cong; Yang, Xiao; Sun, Ailing; Liu, Renmin

    2016-01-01

    Magnetic matrix solid phase dispersion (MMSPD) assisted dispersive liquid liquid microextraction (DLLME) was applied to extract ultra traces of polychlorinated biphenyls (PCBs) from water samples prior to gas chromatography with electron capture detection. PCBs in water were adsorbed by micro particles of magnetic bamboo charcoal and then transferred into the elution solvent. PCBs in the elution solvent of the MMSPD were further concentrated into trace volume extraction solvent of the DLLME procedure. Under optimized conditions, good linearity in the range of 0.2–100 ng L"−"1 was obtained with regression coefficients (r) higher than 0.9987. Based on a signal-noise ratio of 3, the limits of detection (LODs) range from 0.05–0.1 ng L"−"1. These LODs are much lower than those of MMSPD or DLLME alone. Relative standard deviations are between 4.9–8.2 %. The method was successfully applied to the determination of PCBs in lake and river water. Relative recoveries were 85.5–117.4 % for the spiked environmental water samples. (author)

  12. Derivation of simplified basic equations of gas-liquid two-phase dispersed flow based on two-fluid model

    International Nuclear Information System (INIS)

    Kataoka, Isao; Tomiyama, Akio

    2004-01-01

    The simplified and physically reasonable basic equations for the gas-liquid dispersed flow were developed based on some appropriate assumptions and the treatment of dispersed phase as isothermal rigid particles. Based on the local instant formulation of mass, momentum and energy conservation of the dispersed flow, time-averaged equations were obtained assuming that physical quantities in the dispersed phase are uniform. These assumptions are approximately valid when phase change rate and/or chemical reaction rate are not so large at gas-liquid interface and there is no heat generation in within the dispersed phase. Detailed discussions were made on the characteristics of obtained basic equations and physical meanings of terms consisting the basic equations. It is shown that, in the derived averaged momentum equation, the terms of pressure gradient and viscous momentum diffusion do not appear and, in the energy equation, the term of molecular thermal diffusion heat flux does not appear. These characteristics of the derived equations were shown to be very consistent concerning the physical interpretation of the gas-liquid dispersed flow. Furthermore, the obtained basic equations are consistent with experiments for the dispersed flow where most of averaged physical quantities are obtained assuming that the distributions of those are uniform within the dispersed phase. Investigation was made on the problem whether the obtained basic equations are well-posed or ill-posed for the initial value problem. The eigenvalues of the simplified mass and momentum equations are calculated for basic equations obtained here and previous two-fluid basic equations with one pressure model. Well-posedness and ill-posedness are judged whether the eigenvalues are real or imaginary. The result indicated the newly developed basic equations always constitute the well-posed initial value problem while the previous two-fluid basic equations based on one pressure model constitutes ill

  13. Electrically Tunable Binary-Phase Fresnel Lens Based on Polymer Dispersed Liquid Crystal

    Directory of Open Access Journals (Sweden)

    Hui LI

    2017-08-01

    Full Text Available This is a proposal for a Fresnel lens with an electrically tunable binary-phase made of polymer dispersed liquid crystal (PDLC, which has relatively fast response time and low applied voltage. Simple fabrication is the major advantage of the proposed method. In this study, NOA65 and E7 were utilized with weight ratios of 60 wt.%: 40 wt.%. There was also the utilization of a relatively low intensity UV-light, 0.53 mW/cm2. The duration time of exposure was about 30 hours. The performance improvement of the Fresnel lens resulted from the infiltration of large LC droplet into the PDLC film. The phenomenon of black cross strip patterns could be explained with the use of the electro-hydrodynamics theory. The diffraction efficiency of the proposed lens was from 31.1 % to 41 % with the changes of externally applied voltage. This work presents an effective approach to get relatively complete phase separation in PDLC. The proposed method also provides great potential in developing high performance Fresnel lens.DOI: http://dx.doi.org/10.5755/j01.ms.23.2.16317

  14. 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.

  15. Matrix solid-phase dispersion coupled with homogeneous ionic liquid microextraction for the determination of sulfonamides in animal tissues using high-performance liquid chromatography.

    Science.gov (United States)

    Wang, Zhibing; He, Mengyu; Jiang, Chunzhu; Zhang, Fengqing; Du, Shanshan; Feng, Wennan; Zhang, Hanqi

    2015-12-01

    Matrix solid-phase dispersion coupled with homogeneous ionic liquid microextraction was developed and applied to the extraction of some sulfonamides, including sulfamerazine, sulfamethazine, sulfathiazole, sulfachloropyridazine, sulfadoxine, sulfisoxazole, and sulfaphenazole, in animal tissues. High-performance liquid chromatography was applied to the separation and determination of the target analytes. The solid sample was directly treated by matrix solid-phase dispersion and the eluate obtained was treated by homogeneous ionic liquid microextraction. The ionic liquid was used as the extraction solvent in this method, which may result in the improvement of the recoveries of the target analytes. To avoid using organic solvent and reduce environmental pollution, water was used as the elution solvent of matrix solid-phase dispersion. The effects of the experimental parameters on recoveries, including the type and volume of ionic liquid, type of dispersant, ratio of sample to dispersant, pH value of elution solvent, volume of elution solvent, amount of salt in eluate, amount of ion-pairing agent (NH4 PF6 ), and centrifuging time, were evaluated. When the present method was applied to the analysis of animal tissues, the recoveries of the analytes ranged from 85.4 to 118.0%, and the relative standard deviations were lower than 9.30%. The detection limits for the analytes were 4.3-13.4 μg/kg. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Preparation of milk samples for immunoassay and liquid chromatographic screening using matrix solid-phase dispersion.

    Science.gov (United States)

    Barker, S A; Long, A R

    1994-01-01

    The use of drugs to maintain the health and maximize the output of dairy cattle has made the monitoring of milk for such agents essential. Screening tests based on immunological, microbial inhibition, and bacterial receptor assays have been developed for the detection of violative levels of therapeutic substances. However, such assays are not infallible, and false positive or negative results can occur when contaminants bind receptors or compete for the binding of the target residues. Such effects may arise from dietary sources, diseases, or other variables. Thus, a violation by such a test is not definitive until further confirmation is obtained. Our laboratory has developed extraction procedures for several drugs used in dairy production. Our method uses matrix solid-phase dispersion (MSPD) to isolate drugs away from contaminants and to eliminate many possible interferences. MSPD can also be used to enhance the specificity of such assays by fractionating various classes of drugs that may cross-react. Similarly, such methods may be used for liquid chromatographic screening and confirmation of a suspect sample.

  17. Liquid agents for dispersion of hard alloys

    International Nuclear Information System (INIS)

    Putintseva, M.N.

    2006-01-01

    Effects of dispersant properties on granulometric, chemical, and phase composition of the products of WC hard alloy electroerosion are considered. It is established that an increase of liquid dispersant permittivity results in enhanced powder dispersity, and an increase of boiling temperature and kinematic viscosity of a hydrocarbon liquid promotes a carbon loss from WC and intensifies pyrolysis of the liquid.On electroerosion of WC base hard alloy in oil a powder particle consists of b-WC+W 2 C phases, in kerosine - of a-WC+b-WC, in distilled water - of W+W 2 C. The viscosity of liquid dispersants practically has no effect on powder particle size [ru

  18. Determination of Bisphenol A and Bisphenol AF in Vinegar samples by two-component mixed ionic liquid dispersive liquid-phase microextraction coupled with high performance liquid chromatography

    International Nuclear Information System (INIS)

    Tai, Z.; Liu, M.; Hu, X.; Yang, Y.

    2014-01-01

    This paper describes a sensitive and simple method for the determination of bisphenol A (BPA) and bisphenol AF (BPAF) in vinegar samples using two-component mixed ionic liquid dispersive liquid-phase microextraction coupled with high performance liquid chromatography. In this work, BPA and BPAF were selected as the model analytes, and two-component mixed ionic liquid included 1-butyl-3-methylimidazolium hexafluorophosphate ((C4Mim)PF6) and 1-hexyl-3-methyl-imidazolium hexafluorophosphate ((C6Mim)PF6) was used as the extraction solvent for the first time here. Parameters that affect the extraction efficiency were investigated. Under the optimum conditions, good linear relationships were discovered in the range of 1.0-100 micro g/L for BPA and 2.0-150 micro g/L for BPAF, respectively. Detection limits of proposed method based on the signal-to-noise ratio (S/N=3) were in the range of 0.15-0.38 micro g/L. The efficiencies of proposed method have also been demonstrated with spiked real vinegar samples. The result show this method/ procedure to be a more efficient approach for the determination of BPA and BPAF in real vinegar, presenting average recovery rate of 89.3-112 % and precision values of 0.9-13.5% (RSDs, n = 6). In comparison with traditional solid phase extraction procedures this method results in lower solvent consumption, low pollution levels, and faster sample preparation. (author)

  19. Quantitative Analysis of Piroxicam Using Temperature-Controlled Ionic Liquid Dispersive Liquid Phase Microextraction Followed By Stopped-Flow Injection Spectrofluorimetry

    Directory of Open Access Journals (Sweden)

    Mohammad Reza Ganjali

    2013-07-01

    Full Text Available Background:Piroxicam (PXM belongs to the wide class of non-steroidal anti-inflammatory drugs (NSAIDs. PXM has been widely applied in the treatment of rheumatoid arthritis, gonarthrosis, osteoarthritis, backaches, neuralgia, mialgia. In the presented work, a green and benign sample pretreatment method called temperature-controlled ionic liquid dispersive liquid phase microextraction (TCIL-DLPME was followed with stopped-flow injection spectrofluorimetry (SFIS for quantitation of PXM in pharmaceutical formulations and biological samples.Methods:Temperature-controlled ionic liquid dispersive liquid phase microextraction (TCIL-DLPME was applied as an environmentally friendly sample enrichment method to extract and isolate PXM prior to quantitation. Dispersion of 1-hexyl-3-methylimidazolium hexafluorophosphate ([Hmim][PF6] ionic liquid (IL through the sample aqueous solution was performed by applying a relatively high temperature. PXM was extracted into the extractor, and after phase separation, PXM in the final solution was determined by stopped-flow injection spectrofluorimetry (SFIS.Results and Major Conclusion:Different factors affecting the designed method such as IL amount, diluting agent, pH and temperature were investigated in details and optimized. The method provided a linear dynamic range of 0.2-150 μg l-1, a limit of detection (LOD of 0.046 μg l-1 and a relative standard deviation (RSD of 3.1%. Furthermore, in order to demonstrate the analytical applicability of the recommended method, it was applied for quantitation of PXM in real samples.

  20. Determination of antimony and tin in beverages using inductively coupled plasma-optical emission spectrometry after ultrasound-assisted ionic liquid dispersive liquid-liquid phase microextraction.

    Science.gov (United States)

    Biata, N Raphael; Nyaba, Luthando; Ramontja, James; Mketo, Nomvano; Nomngongo, Philiswa N

    2017-12-15

    The aim of this study was to develop a simple and fast ultrasound-assisted ionic liquid dispersive liquid-liquid phase microextraction (UA-IL-DLLME) method for preconcetration of trace antimony and tin in beverage samples. The novelty of this study was based on the application of ligandless UA-IL-DLLME using low-density ionic liquid and organic solvents for preconcentration of Sb and Sn. The concentration of Sb and Sn were quantified using ICP-OES. Under the optimum conditions, the calibration graph was found to be LOQ-250µgL -1 (r 2 =0.9987) for Sb and LOQ-350µgL -1 for Sn. The LOD and LOQ of Sb and Sn ranged from 1.2to 2.5ngL -1 and 4.0 to 8.3ngL -1 , respectively, with high preconcentration factors. The precisions (%RSD) of the proposed method ranged from 2.1% to 2.5% and 3.9% to 4.7% for Sb and Sn, respectively. The proposed method was successfully applied for determination of Sb and Sn in beverages. Copyright © 2017 Elsevier Ltd. All rights reserved.

  1. Dynamic simulation of dispersed gas-liquid two-phase flow using a discrete bubble model.

    NARCIS (Netherlands)

    Delnoij, E.; Lammers, F.A.; Kuipers, J.A.M.; van Swaaij, Willibrordus Petrus Maria

    1997-01-01

    In this paper a detailed hydrodynamic model for gas-liquid two-phase flow will be presented. The model is based on a mixed Eulerian-Lagrangian approach and describes the time-dependent two-dimensional motion of small, spherical gas bubbles in a bubble column operating in the homogeneous regime. The

  2. Sensitive determination of three aconitum alkaloids and their metabolites in human plasma by matrix solid-phase dispersion with vortex-assisted dispersive liquid-liquid microextraction and HPLC with diode array detection.

    Science.gov (United States)

    Wang, Xiaozhong; Li, Xuwen; Li, Lanjie; Li, Min; Liu, Ying; Wu, Qian; Li, Peng; Jin, Yongri

    2016-05-01

    A simple and sensitive method for determination of three aconitum alkaloids and their metabolites in human plasma was developed using matrix solid-phase dispersion combined with vortex-assisted dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection. The plasma sample was directly purified by matrix solid-phase dispersion and the eluate obtained was concentrated and further clarified by vortex-assisted dispersive liquid-liquid microextraction. Some important parameters affecting the extraction efficiency, such as type and amount of dispersing sorbent, type and volume of elution solvent, type and volume of extraction solvent, salt concentration as well as sample solution pH, were investigated in detail. Under optimal conditions, the proposed method has good repeatability and reproducibility with intraday and interday relative standard deviations lower than 5.44 and 5.75%, respectively. The recoveries of the aconitum alkaloids ranged from 73.81 to 101.82%, and the detection limits were achieved within the range of 1.6-2.1 ng/mL. The proposed method offered the advantages of good applicability, sensitivity, simplicity, and feasibility, which makes it suitable for the determination of trace amounts of aconitum alkaloids in human plasma samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. 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.

  4. Combination of saponification and dispersive liquid-liquid microextraction for the determination of tocopherols and tocotrienols in cereals by reversed-phase high-performance liquid chromatography.

    Science.gov (United States)

    Shammugasamy, Balakrishnan; Ramakrishnan, Yogeshini; Ghazali, Hasanah M; Muhammad, Kharidah

    2013-07-26

    A simple sample preparation technique coupled with reversed-phase high-performance liquid chromatography was developed for the determination of tocopherols and tocotrienols in cereals. The sample preparation procedure involved a small-scale hydrolysis of 0.5g cereal sample by saponification, followed by the extraction and concentration of tocopherols and tocotrienols from saponified extract using dispersive liquid-liquid microextraction (DLLME). Parameters affecting the DLLME performance were optimized to achieve the highest extraction efficiency and the performance of the developed DLLME method was evaluated. Good linearity was observed over the range assayed (0.031-4.0μg/mL) with regression coefficients greater than 0.9989 for all tocopherols and tocotrienols. Limits of detection and enrichment factors ranged from 0.01 to 0.11μg/mL and 50 to 73, respectively. Intra- and inter-day precision were lower than 8.9% and the recoveries were around 85.5-116.6% for all tocopherols and tocotrienols. The developed DLLME method was successfully applied to cereals: rice, barley, oat, wheat, corn and millet. This new sample preparation approach represents an inexpensive, rapid, simple and precise sample cleanup and concentration method for the determination of tocopherols and tocotrienols in cereals. Copyright © 2013 Elsevier B.V. All rights reserved.

  5. 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.

  6. Determination of free formaldehyde in cosmetics containing formaldehyde-releasing preservatives by reversed-phase dispersive liquid-liquid microextraction and liquid chromatography with post-column derivatization.

    Science.gov (United States)

    Miralles, Pablo; Chisvert, Alberto; Alonso, M José; Hernandorena, Sandra; Salvador, Amparo

    2018-03-30

    An analytical method for the determination of traces of formaldehyde in cosmetic products containing formaldehyde-releasing preservatives has been developed. The method is based on reversed-phase dispersive liquid-liquid microextraction (RP-DLLME), that allows the extraction of highly polar compounds, followed by liquid chromatography-ultraviolet/visible (LC-UV/vis) determination with post-column derivatization. The variables involved in the RP-DLLME process were studied to provide the best enrichment factors. Under the selected conditions, a mixture of 500 μL of acetonitrile (disperser solvent) and 50 μL of water (extraction solvent) was rapidly injected into 5 mL of toluene sample solution. The extracts were injected into the LC-UV/vis system using phosphate buffer 6 mmol L -1 at pH 2 as mobile phase. After chromatographic separation, the eluate merged with a flow stream of pentane-2,4-dione in ammonium acetate solution as derivatizing reagent and passed throughout a post-column reactor at 85 °C in order to derivatize formaldehyde into 3,5-diacetyl-1,4-dihydrolutidine, according to Hantzsch reaction, which was finally measured spectrophotometrically at 407 nm. The method was successfully validated showing good linearity, an enrichment factor of 86 ± 2, limits of detection and quantification of 0.7 and 2.3 ng mL -1 , respectively, and good repeatability (RSD < 9.2%). Finally, the proposed analytical method was applied to the determination of formaldehyde in different commercial cosmetic samples containing formaldehyde-releasing preservatives, such as bronopol, diazolidinyl urea, imidazolidinyl urea, and DMDM hydantoin, with good relative recovery values (91-113%) thus showing that matrix effects were negligible. The good analytical features of the proposed method besides of its simplicity and affordability, make it useful to carry out the quality control of cosmetic products containing formaldehyde-releasing preservatives. Copyright

  7. Etude sur la prédiction de l'inversion de phase Phase Inversion Behavior for Liquid Dispersions

    Directory of Open Access Journals (Sweden)

    Decarre S.

    2006-12-01

    Full Text Available En écoulement diphasique eau-huile dans lequel une des phases est dispersée dans l'autre, il peut se produire sous certaine condition d'écoulement une inversion de phase, la phase continue devenant dispersée. Ce phénomène, qui contrôle la nature de la phase mouillant la paroi de la conduite dans laquelle s'écoulent les phases, a des conséquences importantes sur la corrosion et sur la perte de charge. Nous présentons un modèle d'inversion, basé sur une approche thermodynamique, valable pour tous les régimes d'écoulement. Les données expérimentales utilisées pour la validation du modèle sont issues d'une étude bibliographique. En écoulement laminaire, cette approche conduit à des résultats similaires à ceux du modèle de Yeh. Pour la plupart des données disponibles, ce modèle prédit bien la fraction critique pour laquelle l'inversion de phase se produit. In two phase oil-water dispersed flow, a phase inversion may occur whereby the continuous phase becomes dispersed. This phenomenon which controls the nature of the phase in contact with the pipe has a great importance on the corrosion and on the pressure drop. A model for the phase inversion is presented, it is based on a thermodynamic approach, and it is valid for all flow regimes. Experimental data from the litterature are used to validate the model. In laminar flow, this approach gives similar results to those obtained by Yeh. For most data, the model agrees well with the experimental data.

  8. The effect of a micro bubble dispersed gas phase on hydrogen isotope transport in liquid metals under nuclear irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Fradera, J., E-mail: jfradera@ubu.es; Cuesta-López, S., E-mail: scuesta@ubu.es

    2013-12-15

    The present work intend to be a first step towards the understanding and quantification of the hydrogen isotope complex phenomena in liquid metals for nuclear technology. Liquid metals under nuclear irradiation in, e.g., breeding blankets of a nuclear fusion reactor would generate tritium which is to be extracted and recirculated as fuel. At the same time that tritium is bred, helium is also generated and may precipitate in the form of nano bubbles. Other liquid metal systems of a nuclear reactor involve hydrogen isotope absorption processes, e.g., tritium extraction system. Hence, hydrogen isotope absorption into gas bubbles modelling and control may have a capital importance regarding design, operation and safety. Here general models for hydrogen isotopes transport in liquid metal and absorption into gas phase, that do not depend on the mass transfer limiting regime, are exposed and implemented in OpenFOAM® CFD tool for 0D–3D simulations. Results for a 0D case show the impact of a He dispersed phase of nano bubbles on hydrogen isotopes inventory at different temperatures as well as the inventory evolution during a He nucleation event. In addition, 1D and 2D axisymmetric cases are exposed showing the effect of a He dispersed gas phase on hydrogen isotope permeation through a lithium lead eutectic alloy and the effect of vortical structures on hydrogen isotope transport at a backward facing step. Exposed results give a valuable insight on current nuclear technology regarding the importance of controlling hydrogen isotope transport and its interactions with nucleation event through gas absorption processes.

  9. 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.

  10. Density fluctuation in a screened Coulombic colloid dispersion: comparison of the liquid and cubic phases of lipid A-diphosphate

    International Nuclear Information System (INIS)

    Brown, Helen; Ross, D. Keith; Paradies, Henrich H.

    2004-01-01

    Light-, small-angle X-ray and neutron scattering measurements of the dynamic structure factor S(Q,t) of strong interacting dispersions of lipid A-diphosphate were recorded and analysed applying existing models of liquid state theory. Lipid A-diphosphate ordering was observed at low volume fractions (phi=2.2x10 -4 ) and at very low ionic strength (I=10 -5 M). Upon increasing the particle number density of lipid A-diphosphate a transformation of the lattices of the colloidal crystals from a BCC lattice (a=36.20 nm) to a FCC lattice (a=57.30 nm) occurred. This strongly suggests a similarity in the preformed liquid structure and the cubic colloidal phase. The fit of both S eff (Q) and the principle peak I p (Q) with the effective particle charge supports of the main conclusions drawn from the SANS experiments and the liquid state theory indicating the presence of long-range order for the dispersions of lipid A-diphosphate

  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. Dispersing powders in liquids

    CERN Document Server

    Nelson, RD

    1988-01-01

    This book provides powder technologists with laboratory procedures for selecting dispersing agents and preparing stable dispersions that can then be used in particle size characterization instruments. Its broader goal is to introduce industrial chemists and engineers to the phenomena, terminology, physical principles, and chemical considerations involved in preparing and handling dispersions on a commercial scale. The book introduces novices to: - industrial problems due to improper degree of dispersion; - the nomenclature used in describing particles; - the basic physica

  13. 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

  14. Optimization of dispersive liquid-phase microextraction based on solidified floating organic drop combined with high-performance liquid chromatography for the analysis of glucocorticoid residues in food.

    Science.gov (United States)

    Huang, Yuan; Zheng, Zhiqun; Huang, Liying; Yao, Hong; Wu, Xiao Shan; Li, Shaoguang; Lin, Dandan

    2017-05-10

    A rapid, simple, cost-effective dispersive liquid-phase microextraction based on solidified floating organic drop (SFOD-LPME) was developed in this study. Along with high-performance liquid chromatography, we used the developed approach to determine and enrich trace amounts of four glucocorticoids, namely, prednisone, betamethasone, dexamethasone, and cortisone acetate, in animal-derived food. We also investigated and optimized several important parameters that influenced the extraction efficiency of SFOD-LPME. These parameters include the extractant species, volumes of extraction and dispersant solvents, sodium chloride addition, sample pH, extraction time and temperature, and stirring rate. Under optimum experimental conditions, the calibration graph exhibited linearity over the range of 1.2-200.0ng/ml for the four analytes, with a reasonable linearity(r 2 : 0.9990-0.9999). The enrichment factor was 142-276, and the detection limits was 0.39-0.46ng/ml (0.078-0.23μg/kg). This method was successfully applied to analyze actual food samples, and good spiked recoveries of over 81.5%-114.3% were obtained. Copyright © 2017. Published by Elsevier B.V.

  15. New method based on combining ultrasonic assisted miniaturized matrix solid-phase dispersion and homogeneous liquid-liquid extraction for the determination of some organochlorinated pesticides in fish

    International Nuclear Information System (INIS)

    Rezaei, Farahnaz; Hosseini, Mohammad-Reza Milani

    2011-01-01

    Highlights: → Ultrasonic assisted miniaturized matrix solid-phase dispersion combined with HLLE was developed as a new method for the extraction of OCPs in fish. → The goal of this combination was to enhance the selectivity of HLLE procedure and to extend its application in biological samples. → This method proposed the advantages of good detection limits, lower consumption of reagents, and does not need any special instrumentation. - Abstract: In this study, ultrasonic assisted miniaturized matrix solid-phase dispersion (US-MMSPD) combined with homogeneous liquid-liquid extraction (HLLE) has been developed as a new method for the extraction of organochlorinated pesticides (OCPs) in fish prior to gas chromatography with electron capture detector (GC-ECD). In the proposed method, OCPs (heptachlor, aldrin, DDE, DDD, lindane and endrin) were first extracted from fish sample into acetonitrile by US-MMSPD procedure, and the extract was then used as consolute solvent in HLLE process. Optimal condition for US-MMSPD step was as follows: volume of acetonitrile, 1.5 mL; temperature of ultrasound, 40 deg. C; time of ultrasound, 10 min. For HLLE step, optimal results were obtained at the following conditions: volume of chloroform, 35 μL; volume of aqueous phase, 1.5 mL; volume of double distilled water, 0.5 mL; time of centrifuge, 10 min. Under the optimum conditions, the enrichment factors for the studied compounds were obtained in the range of 185-240, and the overall recoveries were ranged from 39.1% to 81.5%. The limits of detection were 0.4-1.2 ng g -1 and the relative standard deviations for 20 ng g -1 of the OCPs, varied from 3.2% to 8% (n = 4). Finally, the proposed method has been successfully applied to the analysis of the OCPs in real fish sample, and satisfactory results were obtained.

  16. New method based on combining ultrasonic assisted miniaturized matrix solid-phase dispersion and homogeneous liquid-liquid extraction for the determination of some organochlorinated pesticides in fish

    Energy Technology Data Exchange (ETDEWEB)

    Rezaei, Farahnaz [Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Narmak, Tehran 16846 (Iran, Islamic Republic of); Hosseini, Mohammad-Reza Milani, E-mail: drmilani@iust.ac.ir [Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Narmak, Tehran 16846 (Iran, Islamic Republic of); Electroanalytical Chemistry Research Center, Iran University of Science and Technology, Narmak, Tehran 16846 (Iran, Islamic Republic of)

    2011-09-30

    Highlights: {yields} Ultrasonic assisted miniaturized matrix solid-phase dispersion combined with HLLE was developed as a new method for the extraction of OCPs in fish. {yields} The goal of this combination was to enhance the selectivity of HLLE procedure and to extend its application in biological samples. {yields} This method proposed the advantages of good detection limits, lower consumption of reagents, and does not need any special instrumentation. - Abstract: In this study, ultrasonic assisted miniaturized matrix solid-phase dispersion (US-MMSPD) combined with homogeneous liquid-liquid extraction (HLLE) has been developed as a new method for the extraction of organochlorinated pesticides (OCPs) in fish prior to gas chromatography with electron capture detector (GC-ECD). In the proposed method, OCPs (heptachlor, aldrin, DDE, DDD, lindane and endrin) were first extracted from fish sample into acetonitrile by US-MMSPD procedure, and the extract was then used as consolute solvent in HLLE process. Optimal condition for US-MMSPD step was as follows: volume of acetonitrile, 1.5 mL; temperature of ultrasound, 40 deg. C; time of ultrasound, 10 min. For HLLE step, optimal results were obtained at the following conditions: volume of chloroform, 35 {mu}L; volume of aqueous phase, 1.5 mL; volume of double distilled water, 0.5 mL; time of centrifuge, 10 min. Under the optimum conditions, the enrichment factors for the studied compounds were obtained in the range of 185-240, and the overall recoveries were ranged from 39.1% to 81.5%. The limits of detection were 0.4-1.2 ng g{sup -1} and the relative standard deviations for 20 ng g{sup -1} of the OCPs, varied from 3.2% to 8% (n = 4). Finally, the proposed method has been successfully applied to the analysis of the OCPs in real fish sample, and satisfactory results were obtained.

  17. Simultaneous determination of phenolic compounds in Equisetum palustre L. by ultra high performance liquid chromatography with tandem mass spectrometry combined with matrix solid-phase dispersion extraction.

    Science.gov (United States)

    Wei, Zuofu; Pan, Youzhi; Li, Lu; Huang, Yuyang; Qi, Xiaolin; Luo, Meng; Zu, Yuangang; Fu, Yujie

    2014-11-01

    A method based on matrix solid-phase dispersion extraction followed by ultra high performance liquid chromatography with tandem mass spectrometry is presented for the extraction and determination of phenolic compounds in Equisetum palustre. This method combines the high efficiency of matrix solid-phase dispersion extraction and the rapidity, sensitivity, and accuracy of ultra high performance liquid chromatography with tandem mass spectrometry. The influential parameters of the matrix solid-phase dispersion extraction were investigated and optimized. The optimized conditions were as follows: silica gel was selected as dispersing sorbent, the ratio of silica gel to sample was selected to be 2:1 (400/200 mg), and 8 mL of 80% methanol was used as elution solvent. Furthermore, a fast and sensitive ultra high performance liquid chromatography with tandem mass spectrometry method was developed for the determination of nine phenolic compounds in E. palustre. This method was carried out within <6 min, and exhibited satisfactory linearity, precision, and recovery. Compared with ultrasound-assisted extraction, the proposed matrix solid-phase dispersion procedure possessed higher extraction efficiency, and was more convenient and time saving with reduced requirements on sample and solvent amounts. All these results suggest that the developed method represents an excellent alternative for the extraction and determination of active components in plant matrices. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Industrial application of liquid steel filtration out of dispersed nonmetallic phase in the continuous casting machine

    Directory of Open Access Journals (Sweden)

    K. Janiszewski

    2013-01-01

    Full Text Available Hitherto existing investigations concerning the ceramic filter use in the steel making processes (both of laboratory and industrial scale have given good results. The obtained results of filtration (in the laboratory have proved that this method may be used as an effective and cheap way of steel filtration from non-metallic inclusions. Placing filters in the tundish is the best location in consideration of limiting the possibility of secondary pollution of steel. Yet, the results presented in this paper, of an experiment prepared and carried out in the industrial environment, are the only positive results obtained, which are connected with so much quantities of liquid steel processed with use of the multi-hole ceramic filters.

  19. Electro-optic and thermo-optic and properties of phase separated polymer dispersed liquid crystal films

    Czech Academy of Sciences Publication Activity Database

    Malik, P.; Bubnov, Alexej M.; Raina, K.K.

    2008-01-01

    Roč. 494, č. 12 (2008), s. 242-251 ISSN 1542-1406 Institutional research plan: CEZ:AV0Z10100520 Keywords : polymer dispersed liquid crystals * electro-optics Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.537, year: 2008

  20. Design of amine modified polymer dispersants for liquid-phase exfoliation of transition metal dichalcogenide nanosheets and their photodetective nanocomposites

    Science.gov (United States)

    Lee, Jinseong; Hahnkee Kim, Richard; Yu, Seunggun; Babu Velusamy, Dhinesh; Lee, Hyeokjung; Park, Chanho; Cho, Suk Man; Jeong, Beomjin; Sol Kang, Han; Park, Cheolmin

    2017-12-01

    Liquid-phase exfoliation (LPE) of transition metal dichalcogenide (TMD) nanosheets is a facile, cost-effective approach to large-area photoelectric devices including photodetectors and non-volatile memories. Non-destructive exfoliation of nanosheets using macromolecular dispersing agents is beneficial in rendering the TMD nanocomposite films suitable for mechanically flexible devices. Here, an efficient LPE of molybdenum disulfide (MoS2) with an amine modified poly(styrene-co-maleic anhydride) co-polymer (AM-PSMA) is demonstrated, wherein the maleic anhydrides were converted into maleic imides with primary amines using N-Boc-(CH2) n -NH2. The exfoliation of nanosheets was facilitated through Lewis acid-base interaction between the primary amine and transition metal. The results demonstrate that the exfoliation depends upon both the fraction of primary amines in the polymer chain and their distance from the polymer backbone. Under optimized conditions of primary amine content and its distance from the backbone, AM-PSMA gave rise to a highly concentrated MoS2 nanosheet suspension that was stable for over 10 d. Exfoliation of several other TMDs was also achieved using the optimized AM-PSMA, indicating the scope of AM-PSMA applications. Furthermore, a flexible composite film of AM-PSMA and MoS2 nanosheets fabricated by vacuum-assisted filtration showed excellent photoconductive performances including a high I on/I off ratio of 102 and a fast photocurrent switching of 300 ms.

  1. Selective determination of inorganic cobalt in nutritional supplements by ultrasound-assisted temperature-controlled ionic liquid dispersive liquid phase microextraction and electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Berton, Paula; Martinis, Estefanía M.; Martinez, Luis D.; Wuilloud, Rodolfo G.

    2012-01-01

    Highlights: ► Synergy of ultrasound energy and TILDLME technique for improved metal extraction. ► Highly selective determination of inorganic Co species at trace levels. ► Speciation analysis of Co in several nutritional supplements with highly complex matrices. ► Development of an environmentally friendly microextraction technique with minimal waste production and sample consumption. - Abstract: In the present work, a simple and rapid analytical method based on application of ionic liquids (ILs) for inorganic Co(II) species (iCo) microextraction in a variety of nutrient supplements was developed. Inorganic Co was initially chelated with 1-nitroso-2-naphtol (1N2N) reagent followed by a modern technique named ultrasound-assisted temperature-controlled ionic liquid dispersive liquid phase microextraction (USA-TILDLME). The extraction was performed with 1-hexyl-3-methylimidazolium hexafluorophosphate [C 6 mim][PF 6 ] with the aid of ultrasound to improve iCo recovery. Finally, the iCo-enriched IL phase was solubilized in methanol and directly injected into an electrothermal atomic absorption spectrometer (ETAAS). Several parameters that could influence iCo microextraction and detection were carefully studied. Since the main difficulty in these samples is caused by high concentrations of potential interfering ions, different approaches were evaluated to eliminate interferences. The limit of detection (LOD) was 5.4 ng L −1 , while the relative standard deviation (RSD) was 4.7% (at 0.5 μg L −1 Co level and n = 10), calculated from the peak height of absorbance signals. Selective microextraction of iCo species was achieved only by controlling the pH value during the procedure. The method was thus successfully applied for determination of iCo species in nutritional supplements.

  2. Selective determination of inorganic cobalt in nutritional supplements by ultrasound-assisted temperature-controlled ionic liquid dispersive liquid phase microextraction and electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Berton, Paula; Martinis, Estefania M. [Analytical Chemistry Research and Development Group (QUIANID), (LISAMEN-CCT-CONICET-Mendoza), Av. Ruiz Leal S/N Parque General San Martin, M 5502 IRA Mendoza (Argentina); Martinez, Luis D. [INQUISAL-CONICET, Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis, San Luis (Argentina); Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gob.ar [Analytical Chemistry Research and Development Group (QUIANID), (LISAMEN-CCT-CONICET-Mendoza), Av. Ruiz Leal S/N Parque General San Martin, M 5502 IRA Mendoza (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina)

    2012-02-03

    Highlights: Black-Right-Pointing-Pointer Synergy of ultrasound energy and TILDLME technique for improved metal extraction. Black-Right-Pointing-Pointer Highly selective determination of inorganic Co species at trace levels. Black-Right-Pointing-Pointer Speciation analysis of Co in several nutritional supplements with highly complex matrices. Black-Right-Pointing-Pointer Development of an environmentally friendly microextraction technique with minimal waste production and sample consumption. - Abstract: In the present work, a simple and rapid analytical method based on application of ionic liquids (ILs) for inorganic Co(II) species (iCo) microextraction in a variety of nutrient supplements was developed. Inorganic Co was initially chelated with 1-nitroso-2-naphtol (1N2N) reagent followed by a modern technique named ultrasound-assisted temperature-controlled ionic liquid dispersive liquid phase microextraction (USA-TILDLME). The extraction was performed with 1-hexyl-3-methylimidazolium hexafluorophosphate [C{sub 6}mim][PF{sub 6}] with the aid of ultrasound to improve iCo recovery. Finally, the iCo-enriched IL phase was solubilized in methanol and directly injected into an electrothermal atomic absorption spectrometer (ETAAS). Several parameters that could influence iCo microextraction and detection were carefully studied. Since the main difficulty in these samples is caused by high concentrations of potential interfering ions, different approaches were evaluated to eliminate interferences. The limit of detection (LOD) was 5.4 ng L{sup -1}, while the relative standard deviation (RSD) was 4.7% (at 0.5 {mu}g L{sup -1} Co level and n = 10), calculated from the peak height of absorbance signals. Selective microextraction of iCo species was achieved only by controlling the pH value during the procedure. The method was thus successfully applied for determination of iCo species in nutritional supplements.

  3. 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)

  4. Liquid dispersion in trickle-bed reactors with gas-liquid cocurrent downflow

    International Nuclear Information System (INIS)

    Chu, C.F.; Ng, K.M.

    1986-01-01

    The flow pattern can deviate from ideal plug flow in both trickling and pulsing flows. The liquid dispersion in those flow regimes are investigated separately, as the mechanisms causing the deviation of flow pattern from plug flow are different. In trickling flow, the dispersion of the liquid phase occurs in the flow path which is determined with computer-generated packed column. Dispersion in pulsing flow is studied with a combination of the method of characteristics and analysis of liquid dispersion in the liquid slug and gas pulse. The axial dispersion coefficients are then determined based on Monte Carlo simulation. Finally, liquid dispersion in trickle beds containing porous packings is also discussed

  5. Rapid determination of hydrophilic phenols in olive oil by vortex-assisted reversed-phase dispersive liquid-liquid microextraction and screen-printed carbon electrodes.

    Science.gov (United States)

    Fernández, Elena; Vidal, Lorena; Canals, Antonio

    2018-05-01

    A novel approach is presented to determine hydrophilic phenols in olive oil samples, employing vortex-assisted reversed-phase dispersive liquid-liquid microextraction (RP-DLLME) for sample preparation and screen-printed carbon electrodes for voltammetric analysis. The oxidation of oleuropein, hydroxytyrosol, caffeic acid, ferulic acid and tyrosol was investigated, being caffeic acid and tyrosol selected for quantification. A matrix-matching calibration using sunflower oil as analyte-free sample diluted with hexane was employed to compensate matrix effects. Samples were analyzed under optimized RP-DLLME conditions, i.e., extractant phase, 1M HCl; extractant volume, 100µL; extraction time, 2min; centrifugation time, 10min; centrifugation speed, 4000rpm. The working range showed a good linearity between 0.075 and 2.5mgL -1 (r = 0.998, N = 7) for caffeic acid, and between 0.075 and 3mgL -1 (r = 0.999, N = 8) for tyrosol. The methodological limit of detection was empirically established at 0.022mgL -1 for both analytes, which is significantly lower than average contents found in olive oil samples. The repeatability was evaluated at two different spiking levels (i.e., 0.5mgL -1 and 2mgL -1 ) and coefficients of variation ranged from 8% to 11% (n = 5). The applicability of the proposed method was tested in olive oil samples of different quality (i.e., refined olive oil, virgin olive oil and extra virgin olive oil). Relative recoveries varied between 83% and 108% showing negligible matrix effects. Finally, fifteen samples were analyzed by the proposed method and a high correlation with the traditional Folin-Ciocalteu spectrophotometric method was obtained. Thereafter, the concentrations of the fifteen oil samples were employed as input variables in linear discriminant analysis in order to distinguish between olive oils of different quality. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Simultaneous determination of brazilin and protosappanin B in Caesalpinia sappan by ionic-liquid dispersive liquid-phase microextraction method combined with HPLC.

    Science.gov (United States)

    Xia, Zhaoyang; Li, Dongdong; Li, Qing; Zhang, Yan; Kang, Wenyi

    2017-11-13

    The conditions of heating, ionic liquid-based ultrasonic-assisted extraction combined with reverse-phase high performance liquid chromatography were optimized to simultaneously isolate and determinate brazilin and protosappanin B in Caesalpinia sappan. Ionic liquids, including [BMIM]Br, [BMIM]BF 4 , [BMIM]PF 6 and [HMIM]PF 6 , were selected as extraction solvents while methanol, acetone, acetonitrile, ethanol and water were selected as dispersants. The chromatographic column was Purospher star RP-C 18 (250 mm × 4.6 mm, 5 μm), a mixture of methanol and 0.2% phosphoric acid-water was used as mobile phase at a flow rate 0.65 mL/min. The result displayed that the extraction yields of brazilin and protosappanin B were highest when the concentration of [BMIM]Br methanol solution as extraction solvent was 0.5 mol/L and the solid-liquid ratio was 1:50 (g/mL). Under the optimal extraction conditions, the contents of brazilin showed a good linearity (r = 1.0000) within the range of 1.25-7.50 μg with the average recovery of 99.33%, the contents of protosappanin B also showed a good linearity (r = 0.9999) within the range of 0.50-3.00 μg with the average recovery of 98.31%. This experiment, which adopted environmentally friendly reagent as extraction solvent, not only improved the extraction efficiency, but also avoided the environmental pollution caused by organic solvent. Moreover, it was simple and reliable, and can be of important significance in the study of Traditional Chinese Medicine active ingredient extraction methods. The antibacterial activities of the ionic liquids and methanol extracts were determined using the paper disc diffusion method. The ionic liquid extract was found to possess antibacterial activity against Staphylococcus aureus and methicillin-resistant S. aureus (MIC value of 37.5 mg crude drug/mL), β-Lactamase producing S. aureus (MIC values of 18.8 mg crude drug/mL), but not against E. coli, Extended spectrum β-Lactamases E. coli

  7. 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.

  8. Ionic liquid ultrasound-assisted dispersive liquid-liquid microextraction based on solidification of the aqueous phase for preconcentration of heavy metals ions prior to determination by LC-UV.

    Science.gov (United States)

    Werner, Justyna

    2018-05-15

    Ionic liquid ultrasound-assisted dispersive liquid-liquid microextraction based on solidification of the aqueous phase was used for preconcentration of Ni 2+ , Co 2+ , Cd 2+ , Cu 2+ , Pb 2+ in natural water samples prior to liquid chromatography with UV detection. In the proposed method, the ammonium pyrrolidinedithiocarbamate was used as a complexing agent and the phosphonium ionic liquid trihexyl(tetradecyl)phosphonium bis[(2,4,4-trimethyl)pentyl]phosphinate (Cyphos IL 104) was used as an extractant. Ultrasound energy was used to disperse the extractant in the aqueous phase. After microextraction, the ionic liquid and aqueous phases were separated by centrifugation. Then the aqueous phase was frozen and the lighter than water ionic liquid phase containing metal ions complexes with pyrrolidinedithiocarbamate was separated and dissolved in a small volume of methanol prior to injection into the liquid chromatograph. Several parameters including the volume of extractant, the pH of the sample, the concentration of complexing agent, the time of ultrasound energy treatment, the time and speed of centrifugation and the effect of ionic strength were optimized. Under the optimized conditions (10 µL of Cyphos IL 104, pH = 5, 0.3% w/v ammonium pyrrolidinedithiocarbamate, 60 s of ultrasound use, 5 min/5000 rpm (2516×g) of centrifugation, 2.0 mg of NaCl), preconcentration factors were 211, 210, 209, 207 and 211 for Ni 2+ , Co 2+ , Cd 2+ , Cu 2+ and Pb 2+ respectively. Linearity was observed in the ranges 0.2-75.0 µg L -1 for Pb 2+ , Cd 2+ , Co 2+ and 0.5-100.0 µg L -1 for Cu 2+ , Ni 2+ . The limits of detection were 0.03 µg L -1 for Ni 2+ , 0.03 µg L -1 for Co 2+ , 0.03 µg L -1 for Cd 2+ , 0.02 µg L -1 for Cu 2+ , 0.02 µg L -1 for Pb 2+ , respectively. The accuracy of this method was evaluated by preconcentration and determination of Ni 2+ , Co 2+ , Cd 2+ , Cu 2+ , Pb 2+ in certified reference materials (TMRAIN-04 and NIST 1643e

  9. Comparison between dispersive solid-phase and dispersive liquid-liquid microextraction combined with spectrophotometric determination of malachite green in water samples based on ultrasound-assisted and preconcentration under multi-variable experimental design optimization.

    Science.gov (United States)

    Alipanahpour Dil, Ebrahim; Ghaedi, Mehrorang; Asfaram, Arash; Zare, Fahimeh; Mehrabi, Fatemeh; Sadeghfar, Fardin

    2017-11-01

    The ultrasound-assisted dispersive solid-phase microextraction (USA-DSPME) and the ultrasound-assisted dispersive liquid-liquid microextraction (USA-DLLME) developed for as an ultra preconcentration and/or technique for the determination of malachite green (MG) in water samples. Central composite design based on analysis of variance and desirability function guide finding best operational conditions and represent dependency of response to variables viz. volume of extraction, eluent and disperser solvent, pH, adsorbent mass and ultrasonication time has significant influence on methods efficiency. Optimum conditions was set for USA-DSPME as: 1mg CNTs/Zn:ZnO@Ni 2 P-NCs; 4min sonication time and 130μL eluent at pH 6.0. Meanwhile optimum point for USA-DLLME conditions were fixed at pH 6.0; 4min sonication time and 130, 650μL and 10mL of extraction solvent (CHCl 3 ), disperser solvent (ethanol) and sample volume, respectively. Under the above specified best operational conditions, the enrichment factors for the USA-DSPME and USA-DLLME were 88.89 and 147.30, respectively. The methods has linear response in the range of 20.0 to 4000.0ngmL -1 with the correlation coefficients (r) between 0.9980 to 0.9995, while its reasonable detection limits viz. 1.386 to 2.348ngmL -1 and good relative standard deviations varied from 1.1% to 2.8% (n=10) candidate this method for successful monitoring of analyte from various media. The relative recoveries of the MG dye from water samples at spiking level of 500ngmL -1 were in the range between 94.50% and 98.86%. The proposed methods has been successfully applied to the analysis of the MG dye in water samples, and a satisfactory result was obtained. Copyright © 2017. Published by Elsevier B.V.

  10. Simultaneous determination of seven synthetic colorants in wine by dispersive micro-solid-phase extraction coupled with reversed-phase high-performance liquid chromatography.

    Science.gov (United States)

    Zhang, Yun; Zhou, Hua; Wang, Yougang; Wu, Xianglun; Zhao, Yonggang

    2015-02-01

    A novel and effective dispersive micro-solid-phase extraction (d-µ-SPE) using ethanediamine-functionalized magnetic Fe3O4 polymer (EDA-MP) as an efficient adsorbent in wine sample was developed. Based on this, a simple and time-saving analytical method for the simultaneous determination of seven synthetic colorants (i.e., tartrazine, amaranth, carmine, sunset yellow, allura red, brilliant blue and erythrosine) in wine by reversed-phase high-performance liquid chromatography with an ultraviolet detector was established. The experimental parameters, including the chromatographic retention behavior of studied synthetic colorants, the effect of the usage amount of cross-linking monomer, the effect of the usage amount of EDA-MP on the recovery and the recyclability of the adsorbents, were studied in detail. The results showed that the EDA-MP could be reused efficiently at least six times. Under optimized conditions, the recoveries for all analytes were in the range of 88.6-105.2%, with the intraday relative standard deviations (RSDs) ranging from 2.1 to 8.2% and the interday RSDs ranging from 3.4 to 8.7%, and all the analytes had good linearities in the tested ranges with correlation coefficients (r(2)) >0.9995. The limits of quantification for seven synthetic colorants were between 0.12 and 0.45 mg L(-1). The developed method was successfully applied to wine samples, and it was confirmed that the EDA-MP particles were highly effective d-µ-SPE materials. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  11. 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.

  12. Determination of haloacetic acids in water using layered double hydroxides as a sorbent in dispersive solid-phase extraction followed by liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Alsharaa, Abdulnaser; Sajid, Muhammad; Basheer, Chanbasha; Alhooshani, Khalid; Lee, Hian Kee

    2016-09-01

    In the present study, highly efficient and simple dispersive solid-phase extraction procedure for the determination of haloacetic acids in water samples has been established. Three different types of layered double hydroxides were synthesized and used as a sorbent in dispersive solid-phase extraction. Due to the interesting behavior of layered double hydroxides in an acidic medium (pH˂4), the analyte elution step was not needed; the layered double hydroxides are simply dissolved in acid immediately after extraction to release the analytes which are then directly introduced into a liquid chromatography with tandem mass spectrometry system for analysis. Several dispersive solid-phase extraction parameters were optimized to increase the extraction efficiency of haloacetic acids such as temperature, extraction time and pH. Under optimum conditions, good linearity was achieved over the concentration range of 0.05-100 μg/L with detection limits in the range of 0.006-0.05 μg/L. The relative standard deviations were 0.33-3.64% (n = 6). The proposed method was applied to different water samples collected from a drinking water plant to determine the concentrations of haloacetic acids. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Selective ionic liquid ferrofluid based dispersive-solid phase extraction for simultaneous preconcentration/separation of lead and cadmium in milk and biological samples.

    Science.gov (United States)

    Fasih Ramandi, Negin; Shemirani, Farzaneh

    2015-01-01

    For the first time, a selective ionic liquid ferrofluid has been used in dispersive solid phase extraction (IL-FF-D-SPE) for simultaneous preconcentration and separation of lead and cadmium in milk and biological samples combined with flame atomic absorption spectrometry. To improve the selectivity of the ionic liquid ferrofluid, the surface of TiO2 nanoparticles with a magnetic core as sorbent was modified by loading 1-(2-pyridylazo)-2-naphtol. Due to the rapid injection of an appropriate amount of ionic liquid ferrofluid into the aqueous sample by a syringe, extraction can be achieved within a few seconds. In addition, based on the attraction of the ionic liquid ferrofluid to a magnet, no centrifugation step is needed for phase separation. The experimental parameters of IL-FF-D-SPE were optimized using a Box-Behnken design (BBD) after a Plackett-Burman screening design. Under the optimum conditions, the relative standard deviations of 2.2% and 2.4% were obtained for lead and cadmium, respectively (n=7). The limit of detections were 1.21 µg L(-1) for Pb(II) and 0.21 µg L(-1) for Cd(II). The preconcentration factors were 250 for lead and 200 for cadmium and the maximum adsorption capacities of the sorbent were 11.18 and 9.34 mg g(-1) for lead and cadmium, respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Concentration of organic compounds in natural waters with solid-phase dispersion based on advesicle modified silica prior to liquid chromatography.

    Science.gov (United States)

    Parisis, Nikolaos A; Giokas, Dimosthenis L; Vlessidis, Athanasios G; Evmiridis, Nicholaos P

    2005-12-02

    The ability of vesicle-coated silica to aid the extraction of organic compounds from water prior to liquid chromatographic analysis is presented for the first time. The method is based on the formation of silica supported cationic multi-lamellar vesicles of gemini surfactants inherently ensuring the presence of hydrophilic and hydrophobic sites for the partitioning of analytes bearing different properties. Method development is illustrated by studying the adsolubilization of UV absorbing chemicals from swimming pool water. Due to the requirement for external energy input (intense shearing) a method based on solid-phase dispersion (SPD) was applied producing better results than off-line solid-phase extraction (SPE). Meticulous investigation of the experimental parameters was conducted in order to elucidate the mechanisms behind the proposed extraction pattern. Analyte recoveries were quantitative under the optimum experimental conditions offering recoveries higher than 96% with RSD values below 5%.

  15. Dispersive solid phase micro-extraction of mercury(II from environmental water and vegetable samples with ionic liquid modified graphene oxide nanoparticles

    Directory of Open Access Journals (Sweden)

    Nasrollahpour Atefeh

    2017-01-01

    Full Text Available A new dispersive solid phase micro-extraction (dispersive-SPME method for separation and preconcentration of mercury(II using ionic liquid modified magnetic reduced graphene oxide (IL-MrGO nanoparticles, prior to the measurement by cold vapour atomic absorption spectrometry (CV-AAS has been developed. The IL-MrGO composite was characterized by Brunauer– Emmett–Teller method (BET for adsorption-desorption measurement, thermogravimetric analysis (TGA, powder X-ray diffraction (XRD and X-ray photoelectron spectroscopy (XPS. The method is based on the sorption of mercury( II on IL-MrGO nanoparticles due to electrostatic interaction and complex formation of ionic liquid part of IL-MrGO with mercury(II. The effect of experimental parameters for preconcentration of mercury(II, such as solution type, concentration and volume of the eluent, pH, time of the sorption and desorption, amount of the sorbent and coexisting ion concentration have been optimized. Under the optimized conditions, a linear response was obtained in the concentration range of 0.08–10 ng mL-1 with a determination coefficient of 0.9995. The limit of detection (LOD of the method at a signal to noise ratio of 3 was 0.01 ng mL-1. Intra-day and inter-day precisions were obtained equal to 3.4 and 4.5 %, respectively. The dispersive solid phase micro-extraction of mercury(II on IL-MrGO nanoparticles coupled with cold vapour atomic absorption spectrometry was successfully used for extraction and determination of mercury(II in water and vegetable samples.

  16. Determination of phenolic acids and flavonoids in raw propolis by silica-supported ionic liquid-based matrix solid phase dispersion extraction high performance liquid chromatography-diode array detection.

    Science.gov (United States)

    Wang, Zhibing; Sun, Rui; Wang, Yuanpeng; Li, Na; Lei, Lei; Yang, Xiao; Yu, Aimin; Qiu, Fangping; Zhang, Hanqi

    2014-10-15

    The silica-supported ionic liquid (S-SIL) was prepared by impregnation and used as the dispersion adsorbent of matrix solid phase dispersion (MSPD) for the simultaneous extraction of eight phenolic acids and flavonoids, including caffeic acid, ferulic acid, morin, luteolin, quercetin, apigenin, chrysin, and kaempferide in raw propolis. High performance liquid chromatography with a Zorbax SB-C18 column (150mm×4.6mm, 3.5μm) was used for separation of the analytes. The mobile phase consisted of 0.2% phosphoric acid aqueous solution and acetonitrile and the flow rate of the mobile phase was 0.5mL/min. The experimental conditions for silica-supported ionic liquid-based matrix solid phase dispersion (S-SIL-based MSPD) were optimized. S-SIL containing 10% [C6MIM]Cl was used as dispersant, 20mL of n-hexane as washing solvent and 15mL of methanol as elution solvent. The ratio of S-SIL to sample was selected to be 4:1. The standard curves showed good linear relationship (r>0.9995). The limits of detection and quantification were in the range of 5.8-22.2ngmL(-1) and 19.2-74.0ngmL(-1), respectively. The relative standard deviations (RSDs) of intra-day and inter-day determination were lower than 8.80% and 11.19%, respectively. The recoveries were between 65.51% and 92.32% with RSDs lower than 8.95%. Compared with ultrasound-assisted extraction (UAE) and soxhlet extraction, the present method consumed less sample, organic solvent, and extraction time, although the extraction yields obtained by S-SIL-based MSPD are slightly lower than those obtained by UAE. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Flashing liquid jets and two-phase droplet dispersion I. Experiments for derivation of droplet atomisation correlations.

    Science.gov (United States)

    Cleary, Vincent; Bowen, Phil; Witlox, Henk

    2007-04-11

    The large-scale release of a liquid contained at upstream conditions above its local atmospheric boiling point is a scenario often given consideration in process industry risk analysis. Current-hazard quantification software often employs simplistic equilibrium two-phase approaches. Scaled water experiments have been carried out measuring droplet velocity and droplet size distributions for a range of exit orifice aspect ratios (L/d) and conditions representing low to high superheat. 2D Phase-Doppler Anemometry has been utilised to characterise droplet kinematics and spray quality. Droplet size correlations have been developed for non-flashing, the transition between non-flashing and flashing, and fully flashing jets. Using high-speed shadowography, transition between regimes is defined in terms of criteria identified in the external flow structure. An overview companion paper provides a wider overview of the problem and reports implementation of these correlations into consequence models and subsequent validation. The fluid utilised throughout is water, hence droplet correlations are developed in non-dimensional form to allow extrapolation to other fluids through similarity scaling, although verification of model performance for other fluids is required in future studies. Data is reduced via non-dimensionalisation in terms of the Weber number and Jakob number, essentially representing the fluid mechanics and thermodynamics of the system, respectively. A droplet-size distribution correlation has also been developed, conveniently presented as a volume undersize distribution based on the Rosin-Rammler distribution. Separate correlations are provided for sub-cooled mechanical break-up and fully flashing jets. This form of correlation facilitates rapid estimates of likely mass rainout quantities, as well as full distribution information for more rigorous two-phase thermodynamic modelling in the future.

  18. Solid-phase extraction combined with dispersive liquid-liquid microextraction and chiral liquid chromatography-tandem mass spectrometry for the simultaneous enantioselective determination of representative proton-pump inhibitors in water samples.

    Science.gov (United States)

    Zhao, Pengfei; Deng, Miaoduo; Huang, Peiting; Yu, Jia; Guo, Xingjie; Zhao, Longshan

    2016-09-01

    This report describes, for the first time, the simultaneous enantioselective determination of proton-pump inhibitors (PPIs-omeprazole, lansoprazole, pantoprazole, and rabeprazole) in environmental water matrices based on solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME) and chiral liquid chromatography-tandem mass spectrometry. The optimized results of SPE-DLLME were obtained with PEP-2 column using methanol-acetonitrile (1/1, v/v) as elution solvent, dichloroethane, and acetonitrile as extractant and disperser solvent, respectively. The separation and determination were performed using reversed-phase chromatography on a cellulose chiral stationary phase, a Chiralpak IC (250 mm × 4.6 mm, 5 μm) column, under isocratic conditions at 0.6 mL min(-1) flow rate. The analytes were detected in multiple reaction monitoring (MRM) mode by triple quadrupole mass spectrometry. Isotopically labeled internal standards were used to compensate matrix interferences. The method provided enrichment factors of around 500. Under optimal conditions, the mean recoveries for all eight enantiomers from the water samples were 89.3-107.3 % with 0.9-10.3 % intra-day RSD and 2.3-8.1 % inter-day RSD at 20 and 100 ng L(-1) levels. Correlation coefficients (r (2)) ≥ 0.999 were achieved for all enantiomers within the range of 2-500 μg L(-1). The method detection and quantification limits were at very low levels, within the range of 0.67-2.29 ng L(-1) and 2.54-8.68 ng L(-1), respectively. This method was successfully applied to the determination of the concentrations and enantiomeric fractions of the targeted analytes in wastewater and river water, making it applicable to the assessment of the enantiomeric fate of PPIs in the environment. Graphical Abstract Simultaneous enantioselective determination of representative proton-pump inhibitors in water samples.

  19. Ultra-preconcentration and determination of selected pharmaceutical and personal care products in different water matrices by solid-phase extraction combined with dispersive liquid-liquid microextraction prior to ultra high pressure liquid chromatography tandem mass spectrometry analysis.

    Science.gov (United States)

    Celano, Rita; Piccinelli, Anna Lisa; Campone, Luca; Rastrelli, Luca

    2014-08-15

    Pharmaceutical and personal care products (PPCPs) are one of the most important classes of emerging contaminants. The potential of ecological and environmental impacts associated with PPCPs are of particular concern because they continually penetrate the aquatic environment. This work describes a novel ultra-preconcentration technique for the rapid and highly sensitive analysis of selected PPCPs in environmental water matrices at ppt levels. Selected PPCPs were rapidly extracted and concentrated from large volumes of aqueous solutions (500 and 250mL) by solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME) and then analyzed using UHPLC-MS/MS. Experimental parameters were carefully investigated and optimized to achieve the best SPE-DLLME efficiency and higher enrichment factors. The best results were obtained using the ternary mixture acetonitrile/methanol/dichloromethane 3:3:4, v/v/v, both as SPE eluent and DLLME extractant/dispersive mixture. DLLME aqueous solution (5% NaCl, 10mgL(-1) TBAB) was also modified to improve the extraction efficiency of more hydrophilic PPCPs. Under the optimal conditions, an exhaustive extraction for most of the investigated analytes (recoveries >70%), with a precision (RSD drinking, sea, river and wastewater). Method detection and quantification limits were at very low ppt levels and below 1 and 3ngL(-1), respectively, for 15 of selected PPCPs. The proposed analytical procedure offers numerous advantages such as the simplicity of operation, rapidity, a high enrichment factor and sensitivity. So it is suitable for monitoring and studies of occurrence of PPCPs in different environmental compartments. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. Simultaneous Determination of Perfluorinated Compounds in Edible Oil by Gel-Permeation Chromatography Combined with Dispersive Solid-Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry.

    Science.gov (United States)

    Yang, Lili; Jin, Fen; Zhang, Peng; Zhang, Yanxin; Wang, Jian; Shao, Hua; Jin, Maojun; Wang, Shanshan; Zheng, Lufei; Wang, Jing

    2015-09-30

    A simple analytical method was developed for the simultaneous analysis of 18 perfluorinated compounds (PFCs) in edible oil. The target compounds were extracted by acetonitrile, purified by gel permeation chromatography (GPC) and dispersive solid-phase extraction (DSPE) using graphitized carbon black (GCB) and octadecyl (C18), and analyzed by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ES-MS/MS) in negative ion mode. Recovery studies were performed at three fortification levels. The average recoveries of all target PFCs ranged from 60 to 129%, with an acceptable relative standard deviation (RSD) (1-20%, n = 3). The method detection limits (MDLs) ranged from 0.004 to 0.4 μg/kg, which was significantly improved compared with the existing liquid-liquid extraction and cleanup method. The method was successfully applied for the analysis of all target PFCs in edible oil samples collected from markets in Beijing, China, and the results revealed that C6-C10 perfluorocarboxylic acid (PFCAs) and C7 perfluorosulfonic acid PFSAs were the major PFCs detected in oil samples.

  1. Extensible automated dispersive liquid–liquid microextraction

    Energy Technology Data Exchange (ETDEWEB)

    Li, Songqing; Hu, Lu; Chen, Ketao; Gao, Haixiang, E-mail: hxgao@cau.edu.cn

    2015-05-04

    Highlights: • An extensible automated dispersive liquid–liquid microextraction was developed. • A fully automatic SPE workstation with a modified operation program was used. • Ionic liquid-based in situ DLLME was used as model method. • SPE columns packed with nonwoven polypropylene fiber was used for phase separation. • The approach was applied to the determination of benzoylurea insecticides in water. - Abstract: In this study, a convenient and extensible automated ionic liquid-based in situ dispersive liquid–liquid microextraction (automated IL-based in situ DLLME) was developed. 1-Octyl-3-methylimidazolium bis[(trifluoromethane)sulfonyl]imide ([C{sub 8}MIM]NTf{sub 2}) is formed through the reaction between [C{sub 8}MIM]Cl and lithium bis[(trifluoromethane)sulfonyl]imide (LiNTf{sub 2}) to extract the analytes. Using a fully automatic SPE workstation, special SPE columns packed with nonwoven polypropylene (NWPP) fiber, and a modified operation program, the procedures of the IL-based in situ DLLME, including the collection of a water sample, injection of an ion exchange solvent, phase separation of the emulsified solution, elution of the retained extraction phase, and collection of the eluent into vials, can be performed automatically. The developed approach, coupled with high-performance liquid chromatography–diode array detection (HPLC–DAD), was successfully applied to the detection and concentration determination of benzoylurea (BU) insecticides in water samples. Parameters affecting the extraction performance were investigated and optimized. Under the optimized conditions, the proposed method achieved extraction recoveries of 80% to 89% for water samples. The limits of detection (LODs) of the method were in the range of 0.16–0.45 ng mL{sup −1}. The intra-column and inter-column relative standard deviations (RSDs) were <8.6%. Good linearity (r > 0.9986) was obtained over the calibration range from 2 to 500 ng mL{sup −1}. The proposed

  2. Extensible automated dispersive liquid–liquid microextraction

    International Nuclear Information System (INIS)

    Li, Songqing; Hu, Lu; Chen, Ketao; Gao, Haixiang

    2015-01-01

    Highlights: • An extensible automated dispersive liquid–liquid microextraction was developed. • A fully automatic SPE workstation with a modified operation program was used. • Ionic liquid-based in situ DLLME was used as model method. • SPE columns packed with nonwoven polypropylene fiber was used for phase separation. • The approach was applied to the determination of benzoylurea insecticides in water. - Abstract: In this study, a convenient and extensible automated ionic liquid-based in situ dispersive liquid–liquid microextraction (automated IL-based in situ DLLME) was developed. 1-Octyl-3-methylimidazolium bis[(trifluoromethane)sulfonyl]imide ([C 8 MIM]NTf 2 ) is formed through the reaction between [C 8 MIM]Cl and lithium bis[(trifluoromethane)sulfonyl]imide (LiNTf 2 ) to extract the analytes. Using a fully automatic SPE workstation, special SPE columns packed with nonwoven polypropylene (NWPP) fiber, and a modified operation program, the procedures of the IL-based in situ DLLME, including the collection of a water sample, injection of an ion exchange solvent, phase separation of the emulsified solution, elution of the retained extraction phase, and collection of the eluent into vials, can be performed automatically. The developed approach, coupled with high-performance liquid chromatography–diode array detection (HPLC–DAD), was successfully applied to the detection and concentration determination of benzoylurea (BU) insecticides in water samples. Parameters affecting the extraction performance were investigated and optimized. Under the optimized conditions, the proposed method achieved extraction recoveries of 80% to 89% for water samples. The limits of detection (LODs) of the method were in the range of 0.16–0.45 ng mL −1 . The intra-column and inter-column relative standard deviations (RSDs) were <8.6%. Good linearity (r > 0.9986) was obtained over the calibration range from 2 to 500 ng mL −1 . The proposed method opens a new avenue

  3. 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 .

  4. Mechanisms of dispersion during liquid hydrogen leakage

    International Nuclear Information System (INIS)

    Proust, C.; Gaston, D.

    2000-01-01

    INERIS conducts research programs with a mission of assessing and preventing accidental and chronic risks to people and the environment due to industrial plants, chemical substances and underground operation. This paper is a study of the dispersion mechanism of cryogenic hydrogen and the mechanisms of flame propagation in clouds of hydrogen. The objective is to contribute to the industrial control implementation of significant storage of hydrogen liquid that has pressure close to the atmospheric pressure. Within the framework of this program, the only interest is with the risk presented by escape of significant flow. This corresponds to accidental ruptures in tanks. The following four phases are looked at: the escape incident and the determination of the leak flow; the formation of the liquid layer and the vaporization of the hydrogen; the formation of the Hydrogen cloud in air; and the explosive ignition in the atmosphere, propagation of the explosive flame and evaluation of the pressure wave. This situation has been limited to dispersion in free air and does not consider the impact of containment

  5. 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.

  6. Dispersion relations of the acoustic modes in divalent liquid metals

    Directory of Open Access Journals (Sweden)

    Inui Masanori

    2017-01-01

    Full Text Available Collective dynamics in liquid Ca and liquid Cd was studied by inelastic x-ray scattering (IXS. Using our experimental technique to prepare proper sample cells and high performance of an IXS beamline (BL35XU at SPring-8 in Japan, the dynamic structure factor with reasonable statistics was obtained for these divalent liquid metals. For both liquids, the dynamic structure factor at low Q exhibits a central peak with a shoulder or small hump clearly visible on each side, and the inelastic excitation energy determined using the model function composed of Lorentzian and the damped harmonic oscillator function disperses with increasing Q. The dispersion curves of these liquids were compared with that of the longitudinal acoustic phonon in each crystalline phase. From these results, clear difference in the interatomic interaction be- tween liquid Ca and liquid Cd was inferred.

  7. Rapid and selective screening of melamine in bovine milk using molecularly imprinted matrix solid-phase dispersion coupled with liquid chromatography-ultraviolet detection.

    Science.gov (United States)

    Yan, Hongyuan; Cheng, Xiaoling; Sun, Ning; Cai, Tianyu; Wu, Ruijun; Han, Kun

    2012-11-01

    A simple, convenient and high selective molecularly imprinted matrix solid-phase dispersion (MI-MSPD) using water-compatible cyromazine-imprinted polymer as adsorbent was proposed for the rapid screening of melamine from bovine milk coupled with liquid chromatography-ultraviolet detection. The molecularly imprinted polymers (MIPs) synthesized by cyromazine as dummy template and reformative methanol-water system as reaction medium showed higher affinity and selectivity to melamine, and so they were applied as the specific dispersant of MSPD to extraction of melamine and simultaneously eliminate the effect of template leakage on quantitative analysis. Under the optimized conditions, good linearity was obtained in a range of 0.24-60.0μgg(-1) with the correlation coefficient of 0.9994. The recoveries of melamine at three spiked levels were ranged from 86.0 to 96.2% with the relative standard deviation (RSD)≤4.0%. This proposed MI-MSPD method combined the advantages of MSPD and MIPs, and could be used as an alternative tool for analyzing the residues of melamine in complex milk samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. Determination of ibuprofen enantiomers in breast milk using vortex-assisted matrix solid-phase dispersion and direct chiral liquid chromatography.

    Science.gov (United States)

    León-González, M E; Rosales-Conrado, N

    2017-09-08

    A mixture of β-cyclodextrin (β-CD) and primary and secondary amine (PSA) sorbents was employed for the extraction and quantification of ibuprofen enantiomers from human breast milk, combining a vortex-assisted matrix solid-phase dispersion method (MSPD) and direct chiral liquid chromatography (CLC) with ultraviolet detection (UV). The MSPD sample preparation procedure was optimized focusing on both the type and amount of dispersion/sorption sorbents and the nature of the elution solvent, in order to obtain acceptable recoveries and avoiding enantiomer conversion. These MSPD parameters were optimized with the aid of an experimental design approach. Hence, a factorial design was used for identification of the main variables affecting the extraction process of ibuprofen enantiomers. Under optimum selected conditions, MSPD combined with direct CLC-UV was successfully applied for ibuprofen enantiomeric determination in breast milk at enantiomer levels between 0.15 and 6.0μgg -1 . The proposed analytical method also provided good repeatability, with relative standard deviations of 6.4% and 8.3% for the intra-day and inter-day precision, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Automation of static and dynamic non-dispersive liquid phase microextraction. Part 2: Approaches based on impregnated membranes and porous supports.

    Science.gov (United States)

    Alexovič, Michal; Horstkotte, Burkhard; Solich, Petr; Sabo, Ján

    2016-02-11

    A critical overview on automation of modern liquid phase microextraction (LPME) approaches based on the liquid impregnation of porous sorbents and membranes is presented. It is the continuation of part 1, in which non-dispersive LPME techniques based on the use of the extraction phase (EP) in the form of drop, plug, film, or microflow have been surveyed. Compared to the approaches described in part 1, porous materials provide an improved support for the EP. Simultaneously they allow to enlarge its contact surface and to reduce the risk of loss by incident flow or by components of surrounding matrix. Solvent-impregnated membranes or hollow fibres are further ideally suited for analyte extraction with simultaneous or subsequent back-extraction. Their use can therefore improve the procedure robustness and reproducibility as well as it "opens the door" to the new operation modes and fields of application. However, additional work and time are required for membrane replacement and renewed impregnation. Automation of porous support-based and membrane-based approaches plays an important role in the achievement of better reliability, rapidness, and reproducibility compared to manual assays. Automated renewal of the extraction solvent and coupling of sample pretreatment with the detection instrumentation can be named as examples. The different LPME methodologies using impregnated membranes and porous supports for the extraction phase and the different strategies of their automation, and their analytical applications are comprehensively described and discussed in this part. Finally, an outlook on future demands and perspectives of LPME techniques from both parts as a promising area in the field of sample pretreatment is given. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Long-chain ionic liquid based mixed hemimicelles and magnetic dispersed solid-phase extraction for the extraction of fluorescent whitening agents in paper materials.

    Science.gov (United States)

    Wang, Qing; Qiu, Bin; Chen, Xianbo; Wang, Bin; Zhang, Hui; Zhang, Xiaoyuan

    2017-06-01

    A novel mixed hemimicelles and magnetic dispersive solid-phase extraction method based on long-chain ionic liquids for the extraction of five fluorescent whitening agents was established. The factors influenced on extraction efficiency were investigated. Under the optimal conditions, namely, the pH of sample solution at 8.0, the concentration of long chain ionic liquid at 0.5 mmol/L, the amount of Fe 3 O 4 nanoparticle at 12 mg, extraction time at 10 min, pH 6.0 of methanol as eluent, and the desorption time at 1 min, satisfactory results were obtained. Wide linear ranges (0.02-10 ng/mL) and good linearity were attained (0.9997-0.9999). The intraday and interday RSDs were 2.1-8.3%. Limits of detection were 0.004-0.01 ng/mL, which were decreased by almost an order of magnitude compared to direct detection without extraction. The present method was applied to extract the fluorescent whitening agents in two kinds of paper samples, obtaining satisfactory results. All showed results illustrated that the detection sensitivity was improved and the proposed method was a good choice for the enriching and monitoring of trace fluorescent whitening agents. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Ultrasound-assisted leaching-dispersive solid-phase extraction followed by liquid-liquid microextraction for the determination of polybrominated diphenyl ethers in sediment samples by gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Fontana, Ariel R; Lana, Nerina B; Martinez, Luis D; Altamirano, Jorgelina C

    2010-06-30

    Ultrasound-assisted leaching-dispersive solid-phase extraction followed by dispersive liquid-liquid microextraction (USAL-DSPE-DLLME) technique has been developed as a new analytical approach for extracting, cleaning up and preconcentrating polybrominated diphenyl ethers (PBDEs) from sediment samples prior gas chromatography-tandem mass spectrometry (GC-MS/MS) analysis. In the first place, PBDEs were leached from sediment samples by using acetone. This extract was cleaned-up by DSPE using activated silica gel as sorbent material. After clean-up, PBDEs were preconcentrated by using DLLME technique. Thus, 1 mL acetone extract (disperser solvent) and 60 microL carbon tetrachloride (extraction solvent) were added to 5 mL ultrapure water and a DLLME technique was applied. Several variables that govern the proposed technique were studied and optimized. Under optimum conditions, the method detection limits (MDLs) of PBDEs calculated as three times the signal-to-noise ratio (S/N) were within the range 0.02-0.06 ng g(-1). The relative standard deviations (RSDs) for five replicates were or =0.9991. Validation of the methodology was carried out by standard addition method at two concentration levels (0.25 and 1 ng g(-1)) and by comparing with a reference Soxhlet technique. Recovery values were > or =80%, which showed a satisfactory robustness of the analytical methodology for determination of low PBDEs concentration in sediment samples. Copyright 2010 Elsevier B.V. All rights reserved.

  12. Modeling of liquid phases

    CERN Document Server

    Soustelle, Michel

    2015-01-01

    This book is part of a set of books which offers advanced students successive characterization tool phases, the study of all types of phase (liquid, gas and solid, pure or multi-component), process engineering, chemical and electrochemical equilibria, and the properties of surfaces and phases of small sizes. Macroscopic and microscopic models are in turn covered with a constant correlation between the two scales. Particular attention has been given to the rigor of mathematical developments. This second volume in the set is devoted to the study of liquid phases.

  13. Determination of Triazine Herbicides in Drinking Water by Dispersive Micro Solid Phase Extraction with Ultrahigh-Performance Liquid Chromatography-High-Resolution Mass Spectrometric Detection.

    Science.gov (United States)

    Chen, Dawei; Zhang, Yiping; Miao, Hong; Zhao, Yunfeng; Wu, Yongning

    2015-11-11

    A novel dispersive micro solid phase extraction (DMSPE) method based on a polymer cation exchange material (PCX) was applied to the simultaneous determination of the 30 triazine herbicides in drinking water with ultrahigh-performance liquid chromatography-high-resolution mass spectrometric detection. Drinking water samples were acidified with formic acid, and then triazines were adsorbed by the PCX sorbent. Subsequently, the analytes were eluted with ammonium hydroxide/acetonitrile. The chromatographic separation was performed on an HSS T3 column using water (4 mM ammonium formate and 0.1% formic acid) and acetonitrile (0.1% formic acid) as the mobile phase. The method achieved LODs of 0.2-30.0 ng/L for the 30 triazines, with recoveries in the range of 70.5-112.1%, and the precision of the method was better than 12.7%. These results indicated that the proposed method had the advantages of convenience and high efficiency when applied to the analysis of the 30 triazines in drinking water.

  14. Three-dimensional ionic liquid functionalized magnetic graphene oxide nanocomposite for the magnetic dispersive solid phase extraction of 16 polycyclic aromatic hydrocarbons in vegetable oils.

    Science.gov (United States)

    Zhang, Yun; Zhou, Hua; Zhang, Zhe-Hua; Wu, Xiang-Lun; Chen, Wei-Guo; Zhu, Yan; Fang, Chun-Fu; Zhao, Yong-Gang

    2017-03-17

    In this paper, a novel three-dimensional ionic liquid functionalized magnetic graphene oxide nanocomposite (3D-IL@mGO) was prepared, and used as an effective adsorbent for the magnetic dispersive solid phase extraction (MSPE) of 16 polycyclic aromatic hydrocarbons (PAHs) in vegetable oil prior to gas chromatography-mass spectrometry (GC-MS). The properties of 3D-IL@mGO were characterized by scanning electron micrographs (SEM), X-ray photoelectron spectroscopy (XPS), vibrating sample magnetometer (VSM). The 3D-IL@mGO, functionalized by ionic liquid, exhibited high adsorption toward PAHs. Compared to molecularly imprinted solid phase extraction (MISPE), the MSPE method based on 3D-IL@mGO had less solvent consumption and low cost, and was more efficent to light PAHs in quantitative analysis. Furthermore, the rapid and accurate GC-MS method coupled with 3D-IL@mGO MSPE procedure was successfully applied for the analysis of 16 PAHs in eleven vegetable oil samples from supermarket in Zhejiang Province. The results showed that the concentrations of BaP in 3 out of 11 samples were higher than the legal limit (2.0μg/kg, Commission Regulation 835/2011a), the sum of 8 heavy PAHs (BaA, CHR, BbF, BkF, BaP, IcP, DaA, BgP) in 11 samples was between 3.03μg/kg and 229.5μg/kg. Validation results on linearity, specificity, accuracy, precision and stability, as well as on application to the analysis of PAHs in oil samples demonstrated the applicability to food safety risk monitoring in China. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. 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.

  16. Superparamagnetic graphene oxide-based dispersive-solid phase extraction for preconcentration and determination of tamsulosin hydrochloride in human plasma by high performance liquid chromatography-ultraviolet detection.

    Science.gov (United States)

    Pashaei, Yaser; Ghorbani-Bidkorbeh, Fatemeh; Shekarchi, Maryam

    2017-05-26

    In the present study, superparamagnetic graphene oxide-Fe 3 O 4 nanocomposites were successfully prepared by a modified impregnation method (MGO mi ) and their application as a sorbent in the magnetic-dispersive solid phase extraction (M-dSPE) mode to the preconcentration and determination of tamsulosin hydrochloride (TMS) in human plasma was investigated by coupling with high performance liquid chromatography-ultraviolet detection (HPLC-UV). The structure, morphology and magnetic properties of the prepared nanocomposites were characterized using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and vibrating sample magnetometry (VSM). Some factors affecting the extraction efficiency, including the pH value, amount of sorbent, extraction time, elution solvent and its volume, and desorption time were studied and optimized. Magnetic nanocomposites plasma extraction of TMS following HPLC analyses showed a linear calibration curve in the range of 0.5-50.0ngmL -1 with an acceptable correlation coefficient (R 2 =0.9988). The method was sensitive, with a low limit of detection (0.17ngmL -1 ) and quantification (0.48ngmL -1 ). Inter- and intra-day precision expressed as relative standard deviation (n=3) and the preconcentration factor, were found to be 5.6-7.2%, 2.9-4.2% and 10, respectively. Good recoveries (98.1-101.4%) with low relative standard deviations (4.2-5.0%) indicated that the matrices under consideration do not significantly affect the extraction process. Due to its high precision and accuracy, the developed method may be a HPLC-UV alternative with M-dSPE for bioequivalence analysis of TMS in human plasma. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Polymer Dispersed Liquid Crystal Displays

    Science.gov (United States)

    Doane, J. William

    The following sections are included: * INTRODUCTION AND HISTORICAL DEVELOPMENT * PDLC MATERIALS PREPARATION * Polymerization induced phase separation (PIPS) * Thermally induced phase separation (TIPS) * Solvent induced phase separation (SIPS) * Encapsulation (NCAP) * RESPONSE VOLTAGE * Dielectric and resistive effects * Radial configuration * Bipolar configuration * Other director configurations * RESPONSE TIME * DISPLAY CONTRAST * Light scattering and index matching * Incorporation of dyes * Contrast measurements * PDLC DISPLAY DEVICES AND INNOVATIONS * Reflective direct view displays * Large-scale, flexible displays * Switchable windows * Projection displays * High definition spatial light modulator * Haze-free PDLC shutters: wide angle view displays * ENVIRONMENTAL STABILITY * ACKNOWLEDGEMENTS * REFERENCES

  18. Application of dispersive solid-phase extraction and ultra-fast liquid chromatography-tandem quadrupole mass spectrometry in food additive residue analysis of red wine.

    Science.gov (United States)

    Chen, Xiao-Hong; Zhao, Yong-Gang; Shen, Hao-Yu; Jin, Mi-Cong

    2012-11-09

    A novel and effective dispersive solid-phase extraction (dSPE) procedure with rapid magnetic separation using ethylenediamine-functionalized magnetic polymer as an adsorbent was developed. The new procedure had excellent clean-up ability for the selective removal of the matrix in red wine. An accurate, simple, and rapid analytical method using ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) for the simultaneous determination of nine food additives (i.e., acesulfame, saccharin, sodium cyclamate, aspartame, benzoic acid, sorbic acid, stevioside, dehydroacetic acid, and neotame) in red wine was also used and validated. Recoveries ranging from 78.5% to 99.2% with relative standard deviations ranging from 0.46% to 6.3% were obtained using the new method. All target compounds showed good linearities in the tested range with correlation coefficients (r) higher than 0.9993. The limits of quantification for the nine food additives were between 0.10 μg/L and 50.0 μg/L. The proposed dSPE-UFLC-MS/MS method was successfully applied in the food-safety risk monitoring of real red wine in Zhejiang Province, China. Crown Copyright © 2012. Published by Elsevier B.V. All rights reserved.

  19. High performance preconcentration of inorganic Se species by dispersive micro-solid phase extraction with a nanosilica-ionic liquid hybrid material

    Science.gov (United States)

    Llaver, Mauricio; Coronado, Eduardo A.; Wuilloud, Rodolfo G.

    2017-12-01

    A highly sensitive and efficient dispersive micro-solid phase extraction (D-μ-SPE) method was developed for inorganic Se speciation analysis. A novel ionic liquid (IL)-nanomaterial hybrid consisting of 1-dodecyl-3-methylimidazolium bromide-functionalized nanosilica was used for the efficient retention of Se(IV) complexed with ammonium pyrrolidine dithiocarbamate, followed by elution with an ethyl acetate/Triton X-114 mixture and determination by electrothermal atomic absorption spectroscopy. The Se(VI) species was selectively determined by difference between total inorganic Se and Se(IV) after pre-reduction. The IL-nanomaterial hybrid was characterized by Fourier transform infrared spectroscopy and transmission electronic microscopy. Likewise, Se(IV) sorption capacity of the retention material and maximum amount of IL loaded on its surface were determined. Several factors concerning the functionalization, extraction and elution steps were optimized, yielding a 100% extraction efficiency for Se(IV) under optimal conditions. A limit of detection of 1.1 ng L- 1, a relative standard deviation of 5.7% and a 110-fold enhancement factor were obtained. The D-μ-SPE method was successfully applied to several water samples from different origins and compositions, including rain, tap, underground, river and sea.

  20. Dispersive liquid-phase microextraction with solidification of floating organic droplet coupled with high-performance liquid chromatography for the determination of Sudan dyes in foodstuffs and water samples.

    Science.gov (United States)

    Chen, Bo; Huang, Yuming

    2014-06-25

    Dispersive liquid-phase microextraction with solidification of floating organic drop (SFO-DLPME) is one of the most interesting sample preparation techniques developed in recent years. In this paper, a new, rapid, and efficient SFO-DLPME coupled with high-performance liquid chromatography (HPLC) was established for the extraction and sensitive detection of banned Sudan dyes, namely, Sudan I, Sudan II, Sudan III, and Sudan IV, in foodstuff and water samples. Various factors, such as the type and volume of extractants and dispersants, pH and volume of sample solution, extraction time and temperature, ion strength, and humic acid concentration, were investigated and optimized to achieve optimal extraction of Sudan dyes in one single step. After optimization of extraction conditions using 1-dodecanol as an extractant and ethanol as a dispersant, the developed procedure was applied for extraction of the target Sudan dyes from 2 g of food samples and 10 mL of the spiked water samples. Under the optimized conditions, all Sudan dyes could be easily extracted by the proposed SFO-DLPME method. Limits of detection of the four Sudan dyes obtained were 0.10-0.20 ng g(-1) and 0.03 μg L(-1) when 2 g of foodstuff samples and 10 mL of water samples were adopted, respectively. The inter- and intraday reproducibilities were below 4.8% for analysis of Sudan dyes in foodstuffs. The method was satisfactorily used for the detection of Sudan dyes, and the recoveries of the target for the spiked foodstuff and water samples ranged from 92.6 to 106.6% and from 91.1 to 108.6%, respectively. These results indicated that the proposed method is simple, rapid, sensitive, and suitable for the pre-concentration and detection of the target dyes in foodstuff samples.

  1. 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.

  2. Accurate determination of 3-alkyl-2-methoxypyrazines in wines by gas chromatography quadrupole time-of-flight tandem mass spectrometry following solid-phase extraction and dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Fontana, Ariel; Rodríguez, Isaac; Cela, Rafael

    2017-09-15

    A new reliable method for the determination 3-alkyl-2-methoxypyrazines (MPs) in wine samples based on the sequential combination of solid-phase extraction (SPE), dispersive liquid-liquid microextraction (DLLME) and gas chromatography (GC) quadrupole time-of-flight accurate tandem mass spectrometry (QTOF-MS/MS) is presented. Primary extraction of target analytes was carried out by using a reversed-phase Oasis HLB (200mg) SPE cartridge combined with acetonitrile as elution solvent. Afterwards, the SPE extract was submitted to DLLME concentration using 0.06mL carbon tetrachloride (CCl 4 ) as extractant. Under final working conditions, sample concentration factors above 379 times and limits of quantification (LOQs) between 0.3 and 2.1ngL -1 were achieved. Moreover, the overall extraction efficiency of the method was unaffected by the particular characteristics of each wine; thus, accurate results (relative recoveries from 84 to 108% for samples spiked at concentrations from 5 to 25ngL -1 ) were obtained using matrix-matched standards, without using standard additions over every sample. Highly selective chromatographic records were achieved considering a mass window of 5mDa, centered in the quantification product ion corresponding to each compound. Twelve commercial wines, elaborated with grapes from different varieties and geographical origins, were processed with the optimized method. The 2-isobutyl-3-methoxypyrazine (IBMP) was determined at levels above the LOQs of the method in half of the samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Preconcentration of uranium in water samples using dispersive liquid-liquid micro- extraction coupled with solid-phase extraction and determination with inductively coupled plasma-optical emission spectrometry

    Directory of Open Access Journals (Sweden)

    M. Rezaee,

    2015-10-01

    Full Text Available A new liquid phase microextraction method based on the dispersion of an extraction solvent into aqueous phase coupled with solid-phase extraction was investigated for the extraction, preconcentration and determination of uranium in water samples. 1-(2-Pyridylazo-2-naphthol reagent (PAN at pH 6.0 was used as a chelating agent prior to extraction. After concentration and purification of the samples in SPE C18 sorbent, 1.5 mL elution sample containing 40.0 µL chlorobenzene was injected into the 5.0 mL pure water. After extraction and centrifuging, the sedimented phase was evaporated and the residue was dissolved in nitric acid (0.5 M and was injected by injection valve into the ICP-OES. 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 optimum conditions, the calibration graph was linear in the range of 0.5-500 µg L-1. The detection limit was 0.1 µg L-1. The relative standard deviation (RSD at 5.0 µg L-1 concentration level was 6.6%. Finally, the developed method was successfully applied to the extraction and determination of uranium in the well, river, mineral, waste and tap water samples and satisfactory results were obtained.DOI: http://dx.doi.org/10.4314/bcse.v29i3.4

  4. Fast determination of seven synthetic pigments from wine and soft drinks using magnetic dispersive solid-phase extraction followed by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Chen, Xiao-Hong; Zhao, Yong-Gang; Shen, Hao-Yu; Zhou, Li-Xin; Pan, Sheng-Dong; Jin, Mi-Cong

    2014-06-13

    A novel, simple and sensitive method based on the use of magnetic dispersive solid-phase extraction (M-dSPE) procedure combined with ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) was developed to determine seven synthetic pigments (tartrazine, amaranth, carmine, sunset yellow, allura red, brilliant blue and erythrosine) in wines and soft drinks. An amino-functionalized low degrees of cross-linking magnetic polymer (NH2-LDC-MP) was synthesized via suspension polymerization, and characterized by transmission electron microscopy (TEM). The NH2-LDC-MP was used as the M-dSPE sorbent to remove the matrix from the solution, and the main factors affecting the extraction were investigated in detail. The obtained results demonstrated the higher extraction capacity of NH2-LDC-MP with recoveries between 84.0 and 116.2%. The limits of quantification (LOQs) for the seven synthetic pigments were between 1.51 and 5.0μg/L in wines and soft drinks. The developed M-dSPE UFLC-MS/MS method had been successfully applied to the real wines and soft drinks for food-safety risk monitoring in Zhejiang Province, China. The results showed that sunset yellow was in three out of thirty soft drink samples (2.95-42.6μg/L), and erythrosine in one out of fifteen dry red wine samples (3.22μg/L), respectively. It was confirmed that the NH2-LDC-MP was a kind of highly effective M-dSPE materials for the pigments analyses. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Analysis of chemical warfare agents in organic liquid samples with magnetic dispersive solid phase extraction and gas chromatography mass spectrometry for verification of the chemical weapons convention.

    Science.gov (United States)

    Singh, Varoon; Purohit, Ajay Kumar; Chinthakindi, Sridhar; Goud, Raghavender D; Tak, Vijay; Pardasani, Deepak; Shrivastava, Anchal Roy; Dubey, Devendra Kumar

    2016-05-27

    A simple, sensitive and low temperature sample preparation method is developed for detection and identification of Chemical Warfare Agents (CWAs) and scheduled esters in organic liquid using magnetic dispersive solid phase extraction (MDSPE) followed by gas chromatography-mass spectrometry analysis. The method utilizes Iron oxide@Poly(methacrylic acid-co-ethylene glycol dimethacrylate) resin (Fe2O3@Poly(MAA-co-EGDMA)) as sorbent. Variants of these sorbents were prepared by precipitation polymerization of methacrylic acid-co-ethylene glycol dimethacrylate (MAA-co-EGDMA) onto Fe2O3 nanoparticles. Fe2O3@poly(MAA-co-EGDMA) with 20% MAA showed highest recovery of analytes. Extractions were performed with magnetic microspheres by MDSPE. Parameters affecting the extraction efficiency were studied and optimized. Under the optimized conditions, method showed linearity in the range of 0.1-3.0μgmL(-1) (r(2)=0.9966-0.9987). The repeatability and reproducibility (relative standard deviations (RSDs) %) were in the range of 4.5-7.6% and 3.4-6.2% respectively for organophosphorous esters in dodecane. Limits of detection (S/N=3/1) and limit of quantification (S/N=10/1) were found to be in the range of 0.05-0.1μgmL(-1) and 0.1-0.12μgmL(-1) respectively in SIM mode for selected analytes. The method was successfully validated and applied to the extraction and identification of targeted analytes from three different organic liquids i.e. n-hexane, dodecane and silicon oil. Recoveries ranged from 58.7 to 97.3% and 53.8 to 95.5% at 3μgmL(-1) and 1μgmL(-1) spiking concentrations. Detection of diethyl methylphosphonate (DEMP) and O-Ethyl S-2-diisopropylaminoethyl methylphosphonothiolate (VX) in samples provided by the Organization for Prohibition of Chemical Weapons Proficiency Test (OPCW-PT) proved the utility of the developed method for the off-site analysis of CWC relevant chemicals. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Membranes as separators of dispersed emulsion phases

    OpenAIRE

    Lefferts, A.G.

    1997-01-01

    The reuse or discharge of industrial waste waters, containing small fractions of dispersed oil, requires a purification treatment for which membranes can be used. If only little oil is present, removal of the dispersed phase might be preferable to the more commonly applied removal of the continuous phase. For this purpose dispersed phase separators can be applied, which combine the features of conventional coalescers and membrane filtration. The membrane surface promotes coalescence ...

  7. 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.

  8. Bio-dispersive liquid liquid microextraction based on nano rhaminolipid aggregates combined with magnetic solid phase extraction using Fe3O4@PPy magnetic nanoparticles for the determination of methamphetamine in human urine.

    Science.gov (United States)

    Haeri, Seyed Ammar; Abbasi, Shahryar; Sajjadifar, Sami

    2017-09-15

    In the present investigation, extraction and preconcentration of methamphetamine in human urine samples was carried out using a novel bio-dispersive liquid liquid microextraction (Bio-DLLME) technique coupled with magnetic solid phase extraction (MSPE). Bio-DLLME is a kind of microextraction technique based nano-materials which have potential capabilities in many application fields. Bio-DLLME is based on the use of a binary part system consisting of methanol and nano rhaminolipid biosurfactant. Use of this binary mixture is ecologically accepted due to their specificity, biocompatibility and biodegradable nature. The potential of nano rhaminolipid biosurfactant as a biological agent in the extraction of organic compounds has been investigated in recent years. They are able to partition at the oil/water interfaces and reduce the interfacial tension in order to increase solubility of hydrocarbons. The properties of the prepared Fe 3 O 4 @PPy magnetic nanoparticles were characterized using Fourier transform infrared spectroscopy and X-ray diffraction methods The influences of the experimental parameters on the quantitative recovery of analyte were investigated. Under optimized conditions, the enrichment factor was 310, the calibration graph was linear in the methamphetamine concentration range from 1 to 60μgL -1 , with a correlation coefficient of 0.9998. The relative standard deviations for six replicate measurements was 5.2%. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Simultaneous extraction and determination of albendazole and triclabendazole by a novel syringe to syringe dispersive liquid phase microextraction-solidified floating organic drop combined with high performance liquid chromatography.

    Science.gov (United States)

    Asadi, Mohammad; Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad

    2016-08-17

    A syringe to syringe dispersive liquid phase microextraction-solidified floating organic drop was introduced and used for the simultaneous extraction of trace amounts of albendazole and triclabendazole from different matrices. The extracted analytes were determined by high performance liquid chromatography along with fluorescence detection. The analytical parameters affecting the microextraction efficiency including the nature and volume of the extraction solvent, sample volume, sample pH, ionic strength and the cycles of extraction were optimized. The calibration curves were linear in the range of 0.1-30.0 μg L(-1) and 0.2-30.0 μg L(-1) with determination coefficients of 0.9999 and 0.9998 for albendazole and triclabendazole respectively. The detection limits defined as three folds of the signal to noise ratio were found to be 0.02 μg L(-1) for albendazole and 0.06 μg L(-1) for triclabendazole. The inter-day and intra-day precision (RSD%) for both analytes at three concentration levels (0.5, 2.0 and 10.0 μg L(-1)) were in the range of 6.3-10.1% and 5.0-7.5% respectively. The developed method was successfully applied to determine albendazole and triclabendazole in water, cow milk, honey, and urine samples. Copyright © 2016. Published by Elsevier B.V.

  10. Dispersion of breakdown voltage of liquid helium

    International Nuclear Information System (INIS)

    Ishii, Itaru; Noguchi, Takuya

    1978-01-01

    As for the electrical insulation characteristics of liquid helium, the discrepancy among the measured values by each person is very large even in the fundamental DC breakdown voltage in uniform electric field. The dispersion of experimental values obtained in the experiments by the same person is also large. Hereafter, the difference among the mean values obtained by each experimenter will be referred to as ''deviation of mean values'', and the dispersion of measured values around the mean value obtained by the same person as ''deviation around the man value''. The authors have mainly investigated on the latter experimentally. The cryostat was made of stainless steel, and the innermost helium chamber was of 500 mm I.D. and approximately 1200 mm deep. The high voltage electrode was of brass sphere of 25 mm diameter, and the low voltage electrode was of brass plate. The experiment was conducted for liquid helium boiling at 4.2 K and 1 atm, and the breakdown voltage and time lag were measured by applying the approximately square wave impulses of fast rise and long tail, ramp and DC voltages. The cause of the deviation of mean values may be the presence of impurity particles or the effect of electrode shape. As for the deviation around the mean value, the dispersion is large, and its standard deviation may amount to 10 to 20% of the man value. The dispersion is not due to the statistical time lag, but is due to parameters that vary with breakdown. (Wakatsuki, Y.)

  11. Dispersive admicelle solid-phase extraction based on sodium dodecyl sulfate coated Fe3 O4 nanoparticles for the selective adsorption of three alkaloids in Gegen-Qinlian oral liquid before high-performance liquid chromatography.

    Science.gov (United States)

    Shi, Zhihong; Xu, Dan; Zhao, Xuan; Li, Xinghong; Shen, Huimin; Yang, Bing; Zhang, Hongyi

    2017-12-01

    A novel dispersive admicelle solid-phase extraction method based on sodium dodecyl sulfate-coated Fe 3 O 4 nanoparticles was developed for the selective adsorption of berberine, coptisine, and palmatine in Gegen-Qinlian oral liquid before high-performance liquid chromatography. Fe 3 O 4 nanoparticles were synthesized by a chemical coprecipitation method and characterized by using transmission electron microscopy. Under acidic conditions, the surface of Fe 3 O 4 nanoparticles was coated with sodium dodecyl sulfate to form a nano-sized admicelle magnetic sorbent. Owing to electrostatic interaction, the alkaloids were adsorbed onto the oppositely charged admicelle magnetic nanoparticles. The quick separation of the analyte-adsorbed nanoparticles from the sample solution was performed by using Nd-Fe-B magnet. Best extraction efficiency was achieved under the following conditions: 800 μL Fe 3 O 4 nanoparticles suspension (20 mg/mL), 150 μL sodium dodecyl sulfate solution (10 mg/mL), pH 2, and vortexing time 2 min for the extraction of alkaloids from 10 mL of diluted sample. Four hundred microliters of methanol was used to desorb the alkaloids by vortexing for 1 min. Satisfactory extraction recoveries were obtained in the range of 85.9-120.3%, relative standard deviations for intra- and interday precisions were less than 6.3 and 10.0%, respectively. Finally, the established method was successfully applied to analyze the alkaloids in two batches of Gegen-Qinlian oral liquids. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Dispersive solid phase extraction combined with ion-pair ultra high-performance liquid chromatography tandem mass spectrometry for quantification of nucleotides in Lactococcus lactis

    DEFF Research Database (Denmark)

    Magdenoska, Olivera; Martinussen, Jan; Thykær, Jette

    2013-01-01

    solid phase extraction with charcoal and subsequent analysis with ion-pair liquid chromatography coupled with electrospray ionization tandem mass spectrometry was established for quantification of intracellular pools of the 28 most important nucleotides. The method can handle extracts where cells leak...

  13. Speciation of As(III) and As(V) in water samples by graphite furnace atomic absorption spectrometry after solid phase extraction combined with dispersive liquid-liquid microextraction based on the solidification of floating organic drop.

    Science.gov (United States)

    Shamsipur, Mojtaba; Fattahi, Nazir; Assadi, Yaghoub; Sadeghi, Marzieh; Sharafi, Kiomars

    2014-12-01

    A solid phase extraction (SPE) coupled with dispersive liquid-liquid microextraction based on the solidification of floating organic drop (DLLME-SFO) method, using diethyldithiphosphate (DDTP) as a proper chelating agent, has been developed as an ultra preconcentration technique for the determination of inorganic arsenic in water samples prior to graphite furnace atomic absorption spectrometry (GFAAS). Variables affecting the performance of both steps were thoroughly investigated. Under optimized conditions, 100mL of As(ΙΙΙ) solution was first concentrated using a solid phase sorbent. The extract was collected in 2.0 mL of acetone and 60.0 µL of 1-undecanol was added into the collecting solvent. The mixture was then injected rapidly into 5.0 mL of pure water for further DLLME-SFO. Total inorganic As(III, V) was extracted similarly after reduction of As(V) to As(III) with potassium iodide and sodium thiosulfate and As(V) concentration was calculated by difference. A mixture of Pd(NO3)2 and Mg(NO3)2 was used as a chemical modifier in GFAAS. The analytical characteristics of the method were determined. The calibration graph was linear in the rage of 10-100 ng L(-1) with detection limit of 2.5 ng L(-1). Repeatability (intra-day) and reproducibility (inter-day) of method based on seven replicate measurements of 80 ng L(-1) of As(ΙΙΙ) were 6.8% and 7.5%, respectively. The method was successfully applied to speciation of As(III), As(V) and determination of the total amount of As in water samples and in a certified reference material (NIST RSM 1643e). Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Study of nonequilibrium dispersed two phase flow

    International Nuclear Information System (INIS)

    Reyes, J.N. Jr.

    1986-01-01

    Understanding the behavior of liquid droplets in a superheated steam environment is essential to the accurate prediction of nuclear fuel rod surface temperatures during the blowdown and reflood phase of a loss-of-coolant-accident (LOCA). In response to this need, this treatise presents several original and significant contributions to the field of thermofluid physics. The research contained herein presents a statistical derivation of the two-phase mass, momentum, and energy-conservation equations using a droplet continuity equation analogous to that used in the Kinetic Theory of Gases. Unlike the Eulerian volume and time-averaged conservation equations generally used to describe dispersed two-phase flow behavior, this statistical averaging approach results in an additional mass momentum or energy term in each of the respective conservation equations. Further, this study demonstrates that current definitions of the volumetric vapor generation rate used in the mass conservation equation are inappropriate results under certain circumstances. The mass conservation equation derived herein is used to obtain a new definition for the volumetric vapor-generation rate. Last, a simple two phase phenomenological model, based on the statistically averaged conservation equations, is presented and solved analytically. It is shown that the actual quality and vapor temperature, under these circumstances, depend on a single dimensionless group

  15. Anomalous dispersion enhanced Cerenkov phase-matching

    Energy Technology Data Exchange (ETDEWEB)

    Kowalczyk, T.C.; Singer, K.D. [Case Western Reserve Univ., Cleveland, OH (United States). Dept. of Physics; Cahill, P.A. [Sandia National Labs., Albuquerque, NM (United States)

    1993-11-01

    The authors report on a scheme for phase-matching second harmonic generation in polymer waveguides based on the use of anomalous dispersion to optimize Cerenkov phase matching. They have used the theoretical results of Hashizume et al. and Onda and Ito to design an optimum structure for phase-matched conversion. They have found that the use of anomalous dispersion in the design results in a 100-fold enhancement in the calculated conversion efficiency. This technique also overcomes the limitation of anomalous dispersion phase-matching which results from absorption at the second harmonic. Experiments are in progress to demonstrate these results.

  16. Use of dispersive liquid-liquid microextraction for simultaneous preconcentration of samarium, europium, gadolinium and dysprosium

    International Nuclear Information System (INIS)

    Mallah, M.H.; Atomic Energy Organization of Iran, Tehran; Shemirani, F.; Ghannadi Maragheh, M.

    2008-01-01

    A new preconcentration method of dispersive liquid-liquid microextraction (DLLME) was developed for simultaneous preconcentration of samarium, europium, gadolinium and dysprosium. DLLME technique was successfully used as a sample preparation method. In this preconcentration method, an appropriate mixture of extraction solvent, disperser solvent was injected rapidly into an aqueous solution containing Sm, Eu, Gd and Dy after complex formation using chelating reagent of the 1-(2-pyridylazo)-2-naphthol (PAN). After phase separation, 0.5 mL of the settled phase containing enriched analytes was determined by inductively coupled plasma optical emission spectrometry (ICP-OES). The main factors affected the preconcentration of Sm, Eu, Gd and Dy were extraction and dispersive solvent type and their volume, extraction time, volume of chelating agent (PAN), centrifuge speed and drying temperature of the samples. Under the best operating condition simultaneous preconcentration factors of 80, 100, 103 and 78 were obtained for Sm, Eu, Gd and Dy, respectively. (author)

  17. Effervescence-assisted dispersive solid-phase extraction using ionic-liquid-modified magnetic β-cyclodextrin/attapulgite coupled with high-performance liquid chromatography for fungicide detection in honey and juice.

    Science.gov (United States)

    Wu, Xiaoling; Yang, Miyi; Zeng, Haozhe; Xi, Xuefei; Zhang, Sanbing; Lu, Runhua; Gao, Haixiang; Zhou, Wenfeng

    2016-11-01

    In this study, a simple effervescence-assisted dispersive solid-phase extraction method was developed to detect fungicides in honey and juice. Most significantly, an innovative ionic-liquid-modified magnetic β-cyclodextrin/attapulgite sorbent was used because its large specific surface area enhanced the extraction capacity and also led to facile separation. A one-factor-at-a-time approach and orthogonal design were employed to optimize the experimental parameters. Under the optimized conditions, the entire extraction procedure was completed within 3 min. In addition, the calibration curves exhibited good linearity, and high enrichment factors were achieved for pure water and honey samples. For the honey samples, the extraction efficiencies for the target fungicides ranged from 77.0 to 94.3% with relative standard deviations of 2.3-5.44%. The detection and quantitation limits were in the ranges of 0.07-0.38 and 0.23-1.27 μg/L, respectively. Finally, the developed technique was successfully applied to real samples, and satisfactory results were achieved. This analytical technique is cost-effective, environmentally friendly, and time-saving. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. A combination of solid-phase extraction and dispersive solid-phase extraction effectively reduces the matrix interference in liquid chromatography-ultraviolet detection during pyraclostrobin analysis in perilla leaves.

    Science.gov (United States)

    Farha, Waziha; Rahman, Md Musfiqur; Abd El-Aty, A M; Jung, Da-I; Kabir, Md Humayun; Choi, Jeong-Heui; Kim, Sung-Woo; Im, So Jeong; Lee, Young-Jun; Shin, Ho-Chul; Kwon, Chan-Hyeok; Son, Young-Wook; Lee, Kang-Bong; Shim, Jae-Han

    2015-12-01

    Perilla leaves contain many interfering substances; thus, it is difficult to protect the analytes during identification and integration. Furthermore, increasing the amount of sample to lower the detection limit worsens the situation. To overcome this problem, we established a new method using a combination of solid-phase extraction and dispersive solid-phase extraction to analyze pyraclostrobin in perilla leaves by liquid chromatography with ultraviolet absorbance detection. The target compound was quantitated by external calibration with a good determination coefficient (R(2) = 0.997). The method was validated (in triplicate) with three fortification levels, and 79.06- 89.10% of the target compound was recovered with a relative standard deviation <4. The limits of detection and quantification were 0.0033 and 0.01 mg/kg, respectively. The method was successfully applied to field samples collected from two different areas at Gwangju and Muan. The decline in the resiudue concentrations was best ascribed to a first-order kinetic model with half-lives of 5.7 and 4.6 days. The variation between the patterns was attributed to humidity. Copyright © 2015 John Wiley & Sons, Ltd.

  19. Membranes as separators of dispersed emulsion phases

    NARCIS (Netherlands)

    Lefferts, A.G.

    1997-01-01

    The reuse or discharge of industrial waste waters, containing small fractions of dispersed oil, requires a purification treatment for which membranes can be used. If only little oil is present, removal of the dispersed phase might be preferable to the more commonly applied removal of the

  20. Mathematical modeling of disperse two-phase flows

    CERN Document Server

    Morel, Christophe

    2015-01-01

    This book develops the theoretical foundations of disperse two-phase flows, which are characterized by the existence of bubbles, droplets or solid particles finely dispersed in a carrier fluid, which can be a liquid or a gas. Chapters clarify many difficult subjects, including modeling of the interfacial area concentration. Basic knowledge of the subjects treated in this book is essential to practitioners of Computational Fluid Dynamics for two-phase flows in a variety of industrial and environmental settings. The author provides a complete derivation of the basic equations, followed by more advanced subjects like turbulence equations for the two phases (continuous and disperse) and multi-size particulate flow modeling. As well as theoretical material, readers will discover chapters concerned with closure relations and numerical issues. Many physical models are presented, covering key subjects including heat and mass transfers between phases, interfacial forces and fluid particles coalescence and breakup, a...

  1. Overview of the phase diagram of ionic magnetic colloidal dispersions

    International Nuclear Information System (INIS)

    Cousin, F.; Dubois, E.; Cabuil, V.; Boue, F.; Perzynski, R.

    2001-01-01

    We study ionic magnetic colloidal dispersions, which are constituted of γ-Fe 2 O 3 nanoparticles dispersed in water, and stabilized with electrostatic interparticle repulsion. The phase diagram PV versus Φ (P: osmotic pressure, V: particle volume, Φ: particle volume fraction) is explored, especially in the range of high Π and high Φ. The osmotic pressure P of the colloidal dispersion is known either by a measurement either because it is imposed during the sample preparation by osmotic compression. The structure of the colloidal dispersion is determined from Small Angle Neutron Scattering. Two regimes can be distinguished. At high pressure, fluid and solid phases can exist. Their structure is governed by strong electrostatic repulsion, the range of which is here evaluated. At low pressure, gas, liquid and glassy solids can exist. Their structure results from a sticky hard sphere potential. (author)

  2. Phase noise of dispersion-managed solitons

    International Nuclear Information System (INIS)

    Spiller, Elaine T.; Biondini, Gino

    2009-01-01

    We quantify noise-induced phase deviations of dispersion-managed solitons (DMS) in optical fiber communications and femtosecond lasers. We first develop a perturbation theory for the dispersion-managed nonlinear Schroedinger equation (DMNLSE) in order to compute the noise-induced mean and variance of the soliton parameters. We then use the analytical results to guide importance-sampled Monte Carlo simulations of the noise-driven DMNLSE. Comparison of these results with those from the original unaveraged governing equations confirms the validity of the DMNLSE as a model for many dispersion-managed systems and quantify the increased robustness of DMS with respect to noise-induced phase jitter.

  3. Liquid chromatography tandem mass spectrometry method using solid-phase extraction and bead-beating-assisted matrix solid-phase dispersion to quantify the fungicide tebuconazole in controlled frog exposure study: analysis of water and animal tissue

    DEFF Research Database (Denmark)

    Hansen, Martin; Poulsen, Rikke; Luong, Xuan

    2014-01-01

    and on tissue from exposed and non-exposed adult X. laevis. Using solid-phase extraction (SPE), the analytical method allows for quantification of tebuconazole at concentrations as low as 3.89 pg mL(-1) in 10 mL water samples. Using bead-beating-assisted matrix solid-phase dispersion (MSPD), it was possible...

  4. Magnetic dispersive solid-phase extraction based on modified magnetic nanoparticles for the detection of cocaine and cocaine metabolites in human urine by high-performance liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Yang, Feiyu; Zou, Yun; Ni, Chunfang; Wang, Rong; Wu, Min; Liang, Chen; Zhang, Jiabin; Yuan, Xiaoliang; Liu, Wenbin

    2017-11-01

    An easy-to-handle magnetic dispersive solid-phase extraction procedure was developed for preconcentration and extraction of cocaine and cocaine metabolites in human urine. Divinyl benzene and vinyl pyrrolidone functionalized silanized Fe 3 O 4 nanoparticles were synthesized and used as adsorbents in this procedure. Scanning electron microscopy, vibrating sample magnetometry, and infrared spectroscopy were employed to characterize the modified adsorbents. A high-performance liquid chromatography with mass spectrometry method for determination of cocaine and its metabolites in human urine sample has been developed with pretreatment of the samples by magnetic dispersive solid-phase extraction. The obtained results demonstrated the higher extraction capacity of the prepared nanoparticles with recoveries between 75.1 to 105.7% and correlation coefficients higher than 0.9971. The limits of detection for the cocaine and cocaine metabolites were 0.09-1.10 ng/mL. The proposed magnetic dispersive solid-phase extraction method provided a rapid, environmentally friendly and magnetic stuff recyclable approach and it was confirmed that the prepared adsorbents material was a kind of highly effective extraction materials for the trace cocaine and cocaine metabolites analyses in human urine. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. A new carbon-based magnetic material for the dispersive solid-phase extraction of UV filters from water samples before liquid chromatography-tandem mass spectrometry analysis.

    Science.gov (United States)

    Piovesana, Susy; Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Samperi, Roberto; Zenezini Chiozzi, Riccardo; Laganà, Aldo

    2017-07-01

    Magnetic solid-phase extraction is one of the most promising new extraction methods for liquid samples before ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis. Several types of materials, including carbonaceous ones, have been prepared for this purpose. In this paper, for the first time, the preparation, characterization, and sorption capability of Fe 3 O 4 -graphitized carbon black (mGCB) composite toward some compounds of environmental interest were investigated. The synthesized mGCB consisted of micrometric GCB particles with 55 m 2  g -1 surface area bearing some carbonyl and hydroxyl functionalities and the surface partially decorated by Fe 3 O 4 microparticles. The prepared mGCB was firstly tested as an adsorbent for the extraction from surface water of 50 pollutants, including estrogens, perfluoroalkyl compounds, UV filters, and quinolones. The material showed good affinity to many of the tested compounds, except carboxylates and glucoronates; however, some compounds were difficult to desorb. Ten UV filters belonging to the chemical classes of benzophenones and p-aminobenzoates were selected, and parameters were optimized for the extraction of these compounds from surface water before UHPLC-MS/MS determination. Then, the method was validated in terms of linearity, trueness, intra-laboratory precision, and detection and quantification limits. In summary, the method performance (trueness, expressed as analytical recovery, 85-114%; RSD 5-15%) appears suitable for the determination of the selected compounds at the level of 10-100 ng L -1 , with detection limits in the range of 1-5 ng L -1 . Finally, the new method was compared with a published one, based on conventional solid-phase extraction with GCB, showing similar performance in real sample analysis. Graphical Abstract Workflow of the analytical method based on magnetic solid-phase extraction followed by LC-MS/MS determination.

  6. Computational design and fabrication of core-shell magnetic molecularly imprinted polymer for dispersive micro-solid-phase extraction coupled with high-performance liquid chromatography for the determination of rhodamine 6G.

    Science.gov (United States)

    Xie, Jin; Xie, Jie; Deng, Jian; Fang, Xiangfang; Zhao, Haiqing; Qian, Duo; Wang, Hongjuan

    2016-06-01

    A novel core-shell magnetic nano-adsorbent with surface molecularly imprinted polymer coating was fabricated and then applied to dispersive micro-solid-phase extraction followed by determination of rhodamine 6G using high-performance liquid chromatography. The molecularly imprinted polymer coating was prepared by copolymerization of dopamine and m-aminophenylboronic acid (functional monomers), in the presence of rhodamine 6G (template). The selection of the suitable functional monomers was based on the interaction between different monomers and the template using the density functional theory. The ratios of the monomers to template were further optimized by an OA9 (3(4) ) orthogonal array design. The binding performances of the adsorbent were evaluated by static, kinetic, and selective adsorption experiments. The results reveal that the adsorbent possesses remarkable affinity and binding specificity for rhodamine 6G because of the enhanced Lewis acid-base interaction between the B(Ш) embedded in the imprinted cavities and the template. The nano-adsorbent was successfully applied to dispersive micro-solid-phase extraction coupled to high-performance liquid chromatography for the trace determination of rhodamine 6G in samples with a detection limit of 2.7 nmol/L. Spiked recoveries ranged from 93.0-99.1, 89.5-92.7, and 86.9-105% in river water, matrimony vine and paprika samples, respectively, with relative standard deviations of less than 4.3%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Stabilization of liquid crystal dispersions with acrylamide copolymers

    Energy Technology Data Exchange (ETDEWEB)

    Park, S.J.; Kim, M.H.; Lee, J.R. [Korea Research Institute of Chemical Technology, Taejon (Korea, Republic of)

    1999-03-01

    The effects of hydrophobic moieties(styrene and methyl methacrylate) on the stability of a liquid crystal(LC, E-7)-in-water dispersion stabilized by copolymers of hydrophilic acrylamide with hydrophobic monomers have been studied in terms of nematic curvilinear aligned phase(NCAP) system. It was observed that the preferential adsorption hydrophobic moieties onto LC droplet surface resulted in steric stabilization of the dispersion, due to increasing the interfacial tension of LC and reducing the LC droplet size. According to the interfacial tension, coalescence time, and sedimented layer thickness measurements, it was proposed that the presence of hydrophobic moieties allows to form the apolar microenvironment in the round of LC droplet and finally reduces the anchoring effect between LC and the polymeric wall. 16 refs., 10 figs.

  8. Morphological studies of polymer dispersed liquid crystal materials

    International Nuclear Information System (INIS)

    Han, Jin-Woo

    2006-01-01

    In this work, we have studied the morphologies of polymer dispersed liquid crystals (PDLCs) based on E7/NOA61. Scanning electron microscope studies show that the PDLC morphology is strongly affected by the LC concentration and the cure temperature. A typical PDLC morphology with isolated LC droplets dispersed in a polymer matrix is only observed at low LC compositions and at low cure temperatures. Increasing either the LC composition or the cure temperature results in a polymer ball morphology, in which LCs exist in irregularly shaped voids in the polymer network structure. It is shown that the transition between these two morphologies can be qualitatively explained using a pseudo-binary phase diagram.

  9. Dispersed-phase catalysis in coal liquefaction

    International Nuclear Information System (INIS)

    Utz, B.R.; Cugini, A.V.; Frommell, E.A.

    1990-01-01

    This paper reports that the specific reaction (activation) conditions for the conversion of catalyst precursors to unsupported catalyst have a direct effect on the catalytic activity and dispersion. The importance of reaction intermediates in decomposition of ammonium heptamolybdate and ammonium tetrathiomolybdate, and the sensitivity of these intermediates to reaction conditions, were studied in coal liquefaction systems. Recent results indicate that optimization of activation conditions facilitates the formation of a highly dispersed and active form of molybdenum disulfide for coal liquefaction. The use of the catalyst precursors ammonium heptamolybdate, ammonium tetrathiomolybdate, and molybdenum trisulfide for the conversion of coal to soluble products will be discussed. The use of an unsupported dispersed-phase catalyst for direct coal liquefaction is not a novel concept and has been employed in may studies with varying success. Dispersed-phase catalysts soluble and oil-soluble salts, and as finely divided powders. While some methods of catalyst introduction give higher dispersion of the catalyst and greater activity for the liquefaction of coal, all of the techniques allow the formation of a finely dispersed inorganic phase

  10. Investigation of Factors Influencing Dispersion of Liquid Hydrocarbons in Porous Media

    Directory of Open Access Journals (Sweden)

    Hussain Ali Baker

    2016-08-01

    Full Text Available An experimental work has been done to study the major factors that affect the axial dispersion of some hydrocarbons during liquid-liquid miscible displacement. Kerosene and gas oil are used as displacing phase while seven liquid hydrocarbons of high purity represent the displaced phase, three of the liquids are aromatics and the rest are of paraffinic base. In conducting the experiments, two packed beds of different porosity and permeability are used as porous media. The results showed that the displacement process is not a piston flow, breakthrough of displacing fluids are shown before one pore volume has been injected. The processes are stable with no evidence of viscous fingering. Dispersion model as adapted by Brigham et.al (1961 is used to determine the axial dispersion coefficient of displacing fluid. The results show an increasing in dispersion coefficient as the interstitial velocity and viscosity ratio increases.

  11. Determination of clenbuterol in bovine liver by combining matrix solid phase dispersion and molecularly imprinted solid phase extraction followed by liquid chromatography/electrospray ion trap multiple stage mass spectrometry

    NARCIS (Netherlands)

    Crescenzi, C; Bayoudh, S; Cormack, P.A G; Klein, T; Ensing, K

    2001-01-01

    Matrix solid-phase dispersion(MSPD) is a new sample pretreatment for solid samples. This technique greatly simplifies sample pretreatment but, nonetheless, the extracts often still require an extra cleanup step that is both laborious and time-consuming. The potential;of combining MSPD with

  12. Phase behavior and phase inversion for dispersant systems

    International Nuclear Information System (INIS)

    Solheim, A.; Brandvik, P.J.

    1991-06-01

    This report describes some preliminary phase behavior studies and phase inversion temperature measurements in seawater, bunker oil and dispersant. The objectives have been to find new ways of characterizing dispersants for dispersing oil spill at sea and, perhaps, to throw new lights on the mechanism of dispersion formation (oil-in-water emulsification). The work has been focussed on the relation to phase behavior and the existence of microemulsion in equilibrium with excess oil and water phases. The dispersing process is also compared to the recommended conditions for emulsion formation. When forming an oil-in-water emulsion in an industrial process, it is recommended to choose an emulsifier which gives a phase inversion temperature (PIT) which is 20 - 60 o C higher than the actual temperature for use. The emulsification process must take place close to the PIT which is the temperature at which the emulsion change from oil-in-water emulsion to water-in-oil emulsion when the system is stirred. This condition corresponds to the temperature where the phase behavior change character. The purpose has been to find out if the composition of the dispersants corresponds to the recommendations for oil-in-water emulsification. The amount of experimental work has been limited. Two kinds of experiments have been carried out. Phase behavior studies have been done for seawater, bunker oil and four different dispersants where one had an optimal composition. The phase behavior was hard to interpret and is not recommended for standard dispersants test. The other experimental technique was PIT-measurements by conductivity measurements versus temperature. 4 figs., 1 tab., 4 refs

  13. Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G.

    2015-08-01

    A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L- 1 and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L- 1 of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract.

  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. Lyotropic Liquid Crystal Phases from Anisotropic Nanomaterials

    Directory of Open Access Journals (Sweden)

    Ingo Dierking

    2017-10-01

    Full Text Available Liquid crystals are an integral part of a mature display technology, also establishing themselves in other applications, such as spatial light modulators, telecommunication technology, photonics, or sensors, just to name a few of the non-display applications. In recent years, there has been an increasing trend to add various nanomaterials to liquid crystals, which is motivated by several aspects of materials development. (i addition of nanomaterials can change and thus tune the properties of the liquid crystal; (ii novel functionalities can be added to the liquid crystal; and (iii the self-organization of the liquid crystalline state can be exploited to template ordered structures or to transfer order onto dispersed nanomaterials. Much of the research effort has been concentrated on thermotropic systems, which change order as a function of temperature. Here we review the other side of the medal, the formation and properties of ordered, anisotropic fluid phases, liquid crystals, by addition of shape-anisotropic nanomaterials to isotropic liquids. Several classes of materials will be discussed, inorganic and mineral liquid crystals, viruses, nanotubes and nanorods, as well as graphene oxide.

  16. Crystalline liquids: the blue phases

    Science.gov (United States)

    Wright, David C.; Mermin, N. David

    1989-04-01

    The blue phases of cholesteric liquid crystals are liquids that exhibit orientational order characterized by crystallographic space-group symmetries. We present here a pedagogical introduction to the current understanding of the equilibrium structure of these phases accompanied by a general overview of major experimental results. Using the Ginzburg-Landau free energy appropriate to the system, we first discuss in detail the character and stability of the usual helical phase of cholesterics, showing that for certain parameter ranges the helical phase is unstable to the appearance of one or more blue phases. The two principal models for the blue phases are two limiting cases of the Ginzburg-Landau theory. We explore each limit and conclude with some general considerations of defects in both models and an exact minimization of the free energy in a curved three-dimensional space.

  17. Jet noise reduction via dispersed phase injection

    Science.gov (United States)

    Greska, Brent; Krothapalli, Anjaneyulu; Arakeri, Vijay

    2001-11-01

    A recently developed hot jet aeroacoustics facility at FMRL,FAMU-FSU College of Engineering has been used to study the far field noise characteristics of hot supersonic jets as influenced by the injection of a dispersed phase with low mass loading.The measured SPL from a fully expanded Mach 1.36 hot jet shows a peak value of about 139 dB at 40 deg from the jet axis.By injecting atomized water,the SPL are reduced in the angular region of about 30 deg to 50 deg with the maximum reduction being about 2 dB at 40 deg.However,with the use of non atomized aqueous polymer solution as a dispersed phase the noise levels are reduced over all angular positions by at least 1 dB with the maximum reduction being about 3 dB at 40 deg.The injection of a dispersed phase readily kills the screech; the initial results show promise and optimization studies are underway to find methods of further noise reduction.

  18. Polymer dispersed liquid crystals. Pt.1 Concept, Preparation and Materials

    International Nuclear Information System (INIS)

    Hakemi, H. A.; Santangelo, M.

    1998-01-01

    It is more than a decade since Polymer Dispersed Liquid Crystal (PDLC) film technology became the subject of a world-wide scientific and industrial research and development for commercial applications as large-area reflective displays and electrooptical windows, for privacy, security and light transmission control. In view of current interest and intensive fundamental and industrial research on PDLC, the authors attempt to provide a review of the state-of-art of this technology, from concept to its industrial production, in a series of articles. In the present introductory part, the authors discuss the basic concept, the principle of operation, the materials and the preparation techniques of a PDLC device by phase separation method [it

  19. Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G.

    2015-01-01

    A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L −1 and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L −1 of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract. - Highlights: • Efficient retention and preconcentration of As by combining an IL with MWCNTs • Determination of As by ETAAS with direct injection of MWCNTs • Thermal degradation of MWCNTs in the graphite furnace of ETAAS • Highly sensitive speciation and determination of As in garlic

  20. Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gob.ar

    2015-08-01

    A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L{sup −1} and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L{sup −1} of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract. - Highlights: • Efficient retention and preconcentration of As by combining an IL with MWCNTs • Determination of As by ETAAS with direct injection of MWCNTs • Thermal degradation of MWCNTs in the graphite furnace of ETAAS • Highly sensitive speciation and determination of As in garlic.

  1. Liquid-liquid phase transition in Stillinger-Weber silicon

    International Nuclear Information System (INIS)

    Beaucage, Philippe; Mousseau, Normand

    2005-01-01

    It was recently demonstrated that Stillinger-Weber silicon undergoes a liquid-liquid first-order phase transition deep into the supercooled region (Sastry and Angell 2003 Nat. Mater. 2 739). Here we study the effects of perturbations on this phase transition. We show that the order of the liquid-liquid transition changes with negative pressure. We also find that the liquid-liquid transition disappears when the three-body term of the potential is strengthened by as little as 5%. This implies that the details of the potential could affect strongly the nature and even the existence of the liquid-liquid phase

  2. Liquid phase chromatography on microchips

    DEFF Research Database (Denmark)

    Kutter, Jörg Peter

    2012-01-01

    explosive development of, in particular, chromatographic separation systems on microchips, has, however, slowed down in recent years. This review takes a closer, critical look at how liquid phase chromatography has been implemented in miniaturized formats over the past several years, what is important...

  3. 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.

  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. Liquid Crystal Phases of Colloidal Platelets and their Use as Nanocomposite Templates

    NARCIS (Netherlands)

    Mourad, M.C.D.|info:eu-repo/dai/nl/304837563

    2009-01-01

    This thesis explores the gelation and liquid crystal phase behavior of colloidal dispersions of platelike particles as well as the use of such dispersions for the generation of nanocomposites. We report on the sol-gel, sol-glass and liquid crystal phase transitions of positively charged colloidal

  6. 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

  7. Chemical and phase composition of powders obtained by electroerosion dispersion from alloys WC-Co

    International Nuclear Information System (INIS)

    Putintseva, M.N.

    2004-01-01

    A consideration is given to the dependence of chemical and phase compositions of dispersed powders on the conditions, the medium of electroerosion dispersing and the content of cobalt in an initial alloy. It is shown that dissociation of carbon from tungsten carbide proceeds even on dispersing in liquid hydrocarbon-containing media (kerosene and machine oil). The phase composition is determined to a large extent by a medium of dispersing and a cobalt content in the initial alloy. In all powders complex tungsten-cobalt carbides and even Co 7 W 6 intermetallic compounds are found [ru

  8. Chemical and Phase Composition of Powders Obtained by Electroerosion Dispersion from WC - Co Alloys

    Science.gov (United States)

    Putintseva, M. N.

    2004-03-01

    The dependence of the chemical and phase composition of dispersed powders on the mode and medium of electroerosion dispersion and the content of cobalt in the initial alloy is considered. It is shown that the dissociation of carbon from tungsten carbide occurs even in dispersion in liquid hydrocarbon-bearing media (kerosene and industrial oils). The phase composition is primarily determined by the dispersion medium and the content of cobalt in the initial alloy. Compound tungsten-cobalt carbides and even a Co7W6 intermetallic are determined in all the powders.

  9. Nanoparticle dispersion in liquid metals by electromagnetically induced acoustic cavitation

    International Nuclear Information System (INIS)

    Kaldre, Imants; Bojarevičs, Andris; Grants, Ilmārs; Beinerts, Toms; Kalvāns, Matīss; Milgrāvis, Mikus; Gerbeth, Gunter

    2016-01-01

    Aim of this study is to investigate experimentally the effect of magnetically induced cavitation applied for the purpose of nanoparticle dispersion in liquid metals. The oscillating magnetic force due to the azimuthal induction currents and the axial magnetic field excites power ultrasound in the sample. If the fields are sufficiently high then it is possible to achieve the acoustic cavitation threshold in liquid metals. Cavitation bubble collapses are known to create microscale jets with a potential to break nanoparticle agglomerates and disperse them. The samples are solidified under the contactless ultrasonic treatment and later analyzed by electron microscopy and energy-dispersive X-ray spectroscopy (EDX). It is observed that SiC nanoparticles are dispersed in an aluminum magnesium alloy, whereas in tin the same particles remain agglomerated in micron-sized clusters despite a more intense cavitation.

  10. Non-ionic detergent Triton X-114 Based vortex- synchronized matrix solid-phase dispersion method for the simultaneous determination of six compounds with various polarities from Forsythiae Fructus by ultra high-performance liquid chromatography.

    Science.gov (United States)

    Du, Kunze; Li, Jin; Tian, Fei; Chang, Yan-Xu

    2018-02-20

    A simple nonionic detergent - based vortex- synchronized matrix solid-phase dispersion (ND-VSMSPD) method was developed to extract bioactive compounds in Forsythiae Fructus coupled with ultra high-performance liquid chromatography (UHPLC). Nonionic detergent Triton 114 was firstly used as a green elution reagent in vortex- synchronized MSPD procedure. The optimum parameters were investigated to attain the best results, including Florisil as sorbent, 2mL 10% (v/v) nonionic detergent Triton X-114 as the elution reagent, 1:1 of sample/sorbent ratio, grinding for 3min, and whirling for 2min. The recoveries of the six compounds in Forsythiae Fructus were in the range of 95-104% (RSD arctigenin (r≥0.999). It was proved that the extraction yields of almost all compounds attained by the established vortex- synchronized MSPD, which required lower sample, reagent and time, were higher than the normal MSPD and the traditional ultrasonic-assisted extraction. Consequently, this developed vortex- synchronized MSPD coupled with simple UHPLC method could be efficiently applies to extract and analyze the target compounds in real Forsythiae Fructus samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Development and Validation of a Liquid Chromatography-Tandem Mass Spectrometry Method Coupled with Dispersive Solid-Phase Extraction for Simultaneous Quantification of Eight Paralytic Shellfish Poisoning Toxins in Shellfish

    Science.gov (United States)

    Yang, Xianli; Zhou, Lei; Tan, Yanglan; Shi, Xizhi; Zhao, Zhiyong; Nie, Dongxia; Zhou, Changyan; Liu, Hong

    2017-01-01

    In this study, a high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for simultaneous determination of eight paralytic shellfish poisoning (PSP) toxins, including saxitoxin (STX), neosaxitoxin (NEO), gonyautoxins (GTX1–4) and the N-sulfo carbamoyl toxins C1 and C2, in sea shellfish. The samples were extracted by acetonitrile/water (80:20, v/v) with 0.1% formic and purified by dispersive solid-phase extraction (dSPE) with C18 silica and acidic alumina. Qualitative and quantitative detection for the target toxins were conducted under the multiple reaction monitoring (MRM) mode by using the positive electrospray ionization (ESI) mode after chromatographic separation on a TSK-gel Amide-80 HILIC column with water and acetonitrile. Matrix-matched calibration was used to compensate for matrix effects. The established method was further validated by determining the linearity (R2 ≥ 0.9900), average recovery (81.52–116.50%), sensitivity (limits of detection (LODs): 0.33–5.52 μg·kg−1; limits of quantitation (LOQs): 1.32–11.29 μg·kg−1) and precision (relative standard deviation (RSD) ≤ 19.10%). The application of this proposed approach to thirty shellfish samples proved its desirable performance and sufficient capability for simultaneous determination of multiclass PSP toxins in sea foods. PMID:28661471

  12. 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

    International Nuclear Information System (INIS)

    Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji; Shakerian, Farid; Shiralian Esfahani, Golnaz

    2013-01-01

    Graphical abstract: Pass the sample through the basic alumina column ⇒ elute retained uranium along with the cations ⇒ convert the uranium to its anionic benzoate complex ⇒ extract its ion pair with malachite green into small volume of chloroform by DLLME ⇒ measure its absorption at 621 nm using fiber optic-linear array detection spectrophotometry. -- Highlights: • By combination of SPE and DDLME a high preconcentration factor of 2500 was obtained. • Development of SPE-DDLME-Spectrophotometric method for det. of trace amounts of uranium. • Ultra trace amount of uranium in water samples was det. by the proposed method. • The detection limit of the proposed method is comparable to the most sensitive method. • The proposed method is a free interference spectrophotometric method for uranium det. -- Abstract: 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

  13. Continuous gas-phase hydroformylation of 1-butene using supported ionic liquid phase (SILP) catalysts

    DEFF Research Database (Denmark)

    Haumann, Marco; Dentler, Katharina; Joni, Joni

    2007-01-01

    The concept of supported ionic liquid phase (SILP) catalysis has been extended to 1-butene hydroformylation. A rhodium-sulfoxantphos complex was dissolved in [BMIM][n-C8H17OSO3] and this solution was highly dispersed on silica. Continuous gas-phase experiments in a fixed-bed reactor revealed...

  14. Preparation and Characterization of Silicone Liquid Core/Polymer Shell Microcapsules via Internal Phase Separation

    DEFF Research Database (Denmark)

    Gonzalez, Lidia; Kostrzewska, Malgorzata; Ma, Baoguang

    2014-01-01

    Microcapsules with a silicone liquid core surrounded by a polymeric shell were synthesisedthrough the controlled phase separation. The dispersed silicone phase consisted of the shellpolymer PMMA, a good solvent for the PMMA (dichloromethane, DCM) and a poor solvent(methylhydrosiloxane dimethylsil......Microcapsules with a silicone liquid core surrounded by a polymeric shell were synthesisedthrough the controlled phase separation. The dispersed silicone phase consisted of the shellpolymer PMMA, a good solvent for the PMMA (dichloromethane, DCM) and a poor solvent...

  15. Measurement of liquid holdup and axial dispersion in trickle bed reactors using radiotracer technique

    International Nuclear Information System (INIS)

    Pant, H.J.; Saroha, A.K.; Nikam, K.D.P.

    2000-01-01

    The holdup and axial dispersion of aqueous phase has been measured in trickle bed reactors as a function of liquid and gas flow rates using radioisotope tracer technique. Experiments were carried out in the glass column of inner diameter of 15.2x10 -2 m column for air-water system using three different types of packings i.e. non-porous glass beads, porous catalyst of tablet and extrudate shape. The range of liquid and gas flow rates used were 8.3x10 -5 - 3.3x1- -4 m 3 /s and 0 - 6.67x10 -4 m 3 /s, respectively. Residence time distributions of liquid phase and gas phase were measured and mean residence times were determined. The values of liquid holdup were calculated from the measured mean residence times. It was observed that the liquid holdup increases with increase in liquid flow rates and was independent of increase in gas flow rates used in the study. Two-parameter axial dispersion model was used to simulate measured residence time distribution data and values of mean residence time and Peclet number were obtained. It was observed that the values of Peclet number increases with increase in liquid flow rate for glass beads and tablets and remains almost constant for extrudates. The values of mean residence time obtained from model simulation were found to be in good agreement with the values measured experimentally. (author)

  16. Experimental Investigation of the Dispersion of Liquids by Ejection Atomizers

    Science.gov (United States)

    Arkhipov, V. A.; Bondarchuk, S. S.; Evsevleev, M. Ya.; Zharova, I. K.; Zhukov, A. S.; Zmanovskii, S. V.; Kozlov, E. A.; Konovalenko, A. I.; Trofimov, V. F.

    2013-11-01

    This paper presents the results of an experimental investigation of the dispersivity of liquid droplets in the spray cone of ejection atomizers. The calculational droplet size distribution function was measured by the method of low angles of the probe laser radiation scattering indicatrix on a pneumohydraulic bench under cold blow conditions. The efficiency of the proposed circuit designs of atomizers has been analyzed.

  17. 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.

  18. Dichroic dye-dependent studies in guest-host polymer-dispersed liquid crystal films

    Energy Technology Data Exchange (ETDEWEB)

    Malik, Praveen, E-mail: pmalik100@yahoo.co [Department of Physics, Dr. B.R. Ambedkar National Institute of Technology, Jalandhar 144011, Punjab (India); Raina, K.K. [Liquid Crystal Group, Materials Research Laboratory, School of Physics and Materials Science, Thapar University, Patiala 147004, Punjab (India)

    2010-01-01

    Guest-host polymer-dispersed liquid crystal (GHPDLC) films were prepared using a nematic liquid crystal, photo-curable polymer and dichroic dye (anthraquinone blue) by polymerization-induced phase separation (PIPS) technique. Non-ionic dichroic dye (1%, 2% and 4% wt./wt. ratio) was taken as guest in PDLC host. Polarizing microscopy shows that in the absence of electric field, liquid crystal (LC) droplets in polymer matrix mainly exhibit bipolar configuration, however, relatively at higher field, maltese-type crosses were observed. Our results show that approx1% dye-doped PDLC film shows better transmission and faster response times over pure polymer-dispersed nematic liquid crystal (PDNLC) and higher concentrated (2% and 4%) GHPDLC films.

  19. Dichroic dye-dependent studies in guest-host polymer-dispersed liquid crystal films

    International Nuclear Information System (INIS)

    Malik, Praveen; Raina, K.K.

    2010-01-01

    Guest-host polymer-dispersed liquid crystal (GHPDLC) films were prepared using a nematic liquid crystal, photo-curable polymer and dichroic dye (anthraquinone blue) by polymerization-induced phase separation (PIPS) technique. Non-ionic dichroic dye (1%, 2% and 4% wt./wt. ratio) was taken as guest in PDLC host. Polarizing microscopy shows that in the absence of electric field, liquid crystal (LC) droplets in polymer matrix mainly exhibit bipolar configuration, however, relatively at higher field, maltese-type crosses were observed. Our results show that ∼1% dye-doped PDLC film shows better transmission and faster response times over pure polymer-dispersed nematic liquid crystal (PDNLC) and higher concentrated (2% and 4%) GHPDLC films.

  20. 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.

  1. Surfactant mediated liquid phase exfoliation of graphene

    Science.gov (United States)

    Narayan, Rekha; Kim, Sang Ouk

    2015-10-01

    Commercialization of graphene based applications inevitably requires cost effective mass production. From the early days of research on graphene, direct liquid phase exfoliation (LPE) of graphite has been considered as the most promising strategy to produce high-quality mono or few-layer graphene sheets in solvent dispersion forms. Substantial success has been achieved thus far in the LPE of graphene employing numerous solvent systems and suitable surfactants. This invited review article principally showcase the recent research progress as well as shortcomings of surfactant assisted LPE of graphene. In particular, a comprehensive assessment of the quality and yield of the graphene sheets produced by different categories of the surfactants are summarized. Future direction of LPE methods is also proposed for the eventual success of commercial applications.

  2. Liquid phase sintered superconducting cermet

    International Nuclear Information System (INIS)

    Ray, S.P.

    1990-01-01

    This patent describes a method of making a superconducting cermet having superconducting properties with improved bulk density, low porosity and in situ stabilization. It comprises: forming a structure of a superconducting ceramic material having the formula RM 2 Cu 3 O (6.5 + x) wherein R is one or more rare earth elements capable of reacting to form a superconducting ceramic, M is one or more alkaline earth metal elements selected from barium and strontium capable of reacting to form a superconducting ceramic, x is greater than 0 and less than 0.5; and a precious metal compound in solid form selected from the class consisting of oxides, sulfides and halides of silver; and liquid phase sintering the mixture at a temperature wherein the precious metal of the precious metal compound is molten and below the melting point of the ceramic material. The liquid phase sintering is carried out for a time less than 36 hours but sufficient to improve the bulk density of the cermet

  3. Liquid phase exfoliated graphene for electronic applications

    Science.gov (United States)

    Sukumaran, Sheena S.; Jinesh, K. B.; Gopchandran, K. G.

    2017-09-01

    Graphene dispersions were prepared using the liquid phase exfoliation method with three different surfactants. One surfactant was used from each of the surfactant types, anionic, cationic, and non-ionic; those used, were sodium dodecylbenzene sulfonate (SDBS), cetyltrimethylammonium bromide (CTAB) and polyvinylpyrrolidone (PVP), respectively. Raman spectroscopy was used to investigate the number of layers and the nature of any defects present in the exfoliated graphene. The yield of graphene was found to be less with the non-ionic surfactant, PVP. The deconvolution of 2D peaks at ~2700 cm-1 indicated that graphene prepared using these surfactants resulted in sheets consisting of few-layer graphene. The ratio of intensity of the D and G bands in the Raman spectra showed that edge defect density is high for samples prepared with SDBS compared to the other two, and is attributed to the smaller size of the graphene sheets, as shown in the electron micrographs. In the case of the dispersion in PVP, it is found that the sizes of the graphene sheets are highly sensitive to the concentration of the surfactant used. Here, we have made an attempt to investigate the local density of states in the graphene sheets by measuring the tunnelling current-voltage characteristics. Graphene layers have shown consistent p-type behaviour when exfoliated with SDBS and n-type behaviour when exfoliated with CTAB, with a larger band gap for graphene exfoliated using CTAB. Hence, in addition to the known advantages of liquid phase exfoliation, we found that by selecting suitable surfactants, to a certain extent it is possible to tune the band gap and determine the type of majority carriers.

  4. Dispersions of silica nanoparticles in ionic liquids investigated with advanced rheology

    International Nuclear Information System (INIS)

    Wittmar, Alexandra; Ruiz-Abad, David; Ulbricht, Mathias

    2012-01-01

    The colloidal stabilities of dispersions of unmodified and surface-functionalized SiO 2 nanoparticles in hydrophobic and hydrophilic imidazolium-based ionic liquids were studied with advanced rheology at three temperatures (25, 100, and 200 °C). The rheological behavior of the dispersions was strongly affected by the ionic liquids hydrophilicity, by the nanoparticles surface, by the concentration of the nanoparticles in the dispersion as well as by the temperature. The unmodified hydrophilic nanoparticles showed a better compatibility with the hydrophilic ionic liquid. The SiO 2 surface functionalization with hydrophobic groups clearly improved the colloidal stability of the dispersions in the hydrophobic ionic liquid. The temperature increase was found to lead to a destabilization in all studied systems, especially at higher concentrations. The results of this study imply that ionic liquids with tailored properties could be used in absorbers directly after reactors for gas-phase synthesis of nanoparticles or/and as solvents for their further surface functionalization without agglomeration or aggregation.

  5. 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...

  6. Ultrasound-assisted dispersive magnetic solid phase extraction based on amino-functionalized Fe3O4 adsorbent for recovery of clomipramine from human plasma and its determination by high performance liquid chromatography: Optimization by experimental design.

    Science.gov (United States)

    Hamidi, Fatemeh; Hadjmohammadi, Mohammad Reza; Aghaie, Ali B G

    2017-09-15

    The applicability of Amino-functionalized Fe 3 O 4 nanoparticles (NPs) as an effective adsorbent was developed for the extraction and determination of clomipramine (CLP) in plasma sample by ultrasound-assisted dispersive magnetic solid phase extraction (UADM-SPE) and high-performance liquid chromatography-ultraviolet (HPLC-UV) detection. Fabrication of the Fe 3 O 4 @SiO 2 -NH 2 magnetic nanoparticles confirmed by Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The effect of different extraction parameters (i.e. pH of the sample solution, the amount of magnetic nanoparticles (MNPs), sample volume, temperature and sonication time) on the extraction recovery of CLP were investigated by response surface methodology through central composite design (CCD). The optimum condition is obtained when the affecting parameters are set to: pH of the sample solution=9, the amount of MNPs=37mg, sample volume=23mL, 25°C temperature and sonication time=1min. Under the optimum condition, extraction recovery was 90.6% with relative standard deviation of 3.5%, and enrichment factor of 117. The linear range for determination of CLP was 0.017-0.70mgL -1 with a determination coefficient (R 2 ) of 0.999. Limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.0167mgL -1 , respectively. The established UADM-SPE-HPLC-UV method was rapid, simple and efficient for determination of CLP in human plasma samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. A magnetic-based dispersive micro-solid-phase extraction method using the metal-organic framework HKUST-1 and ultra-high-performance liquid chromatography with fluorescence detection for determining polycyclic aromatic hydrocarbons in waters and fruit tea infusions.

    Science.gov (United States)

    Rocío-Bautista, Priscilla; Pino, Verónica; Ayala, Juan H; Pasán, Jorge; Ruiz-Pérez, Catalina; Afonso, Ana M

    2016-03-04

    A hybrid material composed by the metal-organic framework (MOF) HKUST-1 and Fe3O4 magnetic nanoparticles (MNPs) has been synthetized in a quite simple manner, characterized, and used in a magnetic-assisted dispersive micro-solid-phase extraction (M-d-μSPE) method in combination with ultra-high-performance liquid chromatography (UHPLC) and fluorescence detection (FD). The application was devoted to the determination of 8 heavy polycyclic aromatic hydrocarbons (PAHs) in different aqueous samples, specifically tap water, wastewaters, and fruit tea infusion samples. The overall M-d-μSPE-UHPLC-FD method was optimized and validated. The method is characterized by: its simplicity in both the preparation of the hybrid material (simple mixing) and the magnetic-assisted approach (∼10min extraction time), the use of low sorbent amounts (20mg of HKUST-1 and 5mg of Fe3O4 MNPs), and the low organic solvent consumption in the overall M-d-μSPE-UHPLC-FD method (1.5mL of acetonitrile in the M-d-μSPE method and 2.8mL of acetonitrile in the UHPLC-FD run). The resulting method has high sensitivity, with LODs down to 0.8ngL(-1); adequate intermediate precision, with relative standard deviation values (RSD) always lower than 6.3% (being the range 5.9-9.0% in tap water for a spiked level of 45ngL(-1), 6.1-14% in wastewaters for a spiked level of 45ngL(-1), and 7.2-17% in fruit tea infusion samples for a spiked level of 45ngL(-1)); and adequate relative recoveries, with average values of 82% in tap water, and 94% and 75% in wastewater and fruit tea infusion samples, respectively, if using the proper matrix-matched calibration. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Hairy root culture in a liquid-dispersed bioreactor: characterization of spatial heterogeneity.

    Science.gov (United States)

    Williams, G R; Doran, P M

    2000-01-01

    A liquid-dispersed reactor equipped with a vertical mesh cylinder for inoculum support was developed for culture of Atropa belladonna hairy roots. The working volume of the culture vessel was 4.4 L with an aspect ratio of 1.7. Medium was dispersed as a spray onto the top of the root bed, and the roots grew radially outward from the central mesh cylinder to the vessel wall. Significant benefits in terms of liquid drainage and reduced interstitial liquid holdup were obtained using a vertical rather than horizontal support structure for the biomass and by operating the reactor with cocurrent air and liquid flow. With root growth, a pattern of spatial heterogeneity developed in the vessel. Higher local biomass densities, lower volumes of interstitial liquid, lower sugar concentrations, and higher root atropine contents were found in the upper sections of the root bed compared with the lower sections, suggesting a greater level of metabolic activity toward the top of the reactor. Although gas-liquid oxygen transfer to the spray droplets was very rapid, there was evidence of significant oxygen limitations in the reactor. Substantial volumes of non-free-draining interstitial liquid accumulated in the root bed. Roots near the bottom of the vessel trapped up to 3-4 times their own weight in liquid, thus eliminating the advantages of improved contact with the gas phase offered by liquid-dispersed culture systems. Local nutrient and product concentrations in the non-free-draining liquid were significantly different from those in the bulk medium, indicating poor liquid mixing within the root bed. Oxygen enrichment of the gas phase improved neither growth nor atropine production, highlighting the greater importance of liquid-solid compared with gas-liquid oxygen transfer resistance. The absence of mechanical or pneumatic agitation and the tendency of the root bed to accumulate liquid and impede drainage were identified as the major limitations to reactor performance. Improved

  9. Double salts of ionic-liquid-based surfactants in microextraction: application of their mixed hemimicelles as novel sorbents in magnetic-assisted micro-dispersive solid-phase extraction for the determination of phenols.

    Science.gov (United States)

    Trujillo-Rodríguez, María J; Pino, Verónica; Anderson, Jared L; Ayala, Juan H; Afonso, Ana M

    2015-11-01

    The use of mixed hemimicelles of ionic liquid (IL)-based surfactants in a magnetic-based micro-dispersive solid-phase extraction (m-μdSPE) approach is described. Not only is the symmetric monocationic IL-based surfactant 1,3-didodecylimidazolium bromide (C12C12Im-Br) studied for first time in m-μdSPE, but double-salt (DS) IL (DSIL)-based surfactants are also examined. Nine DSIL-based surfactants were formed by combination of C12C12Im-Br with other IL-based surfactants, including nonsymmetric monocationic and dicationic ILs combined at three different molar fractions. The analytical application was focused on the determination of a group of eight phenols, including bisphenol A, in water samples. The best results were obtained with the DSIL formed by C12C12Im-Br (molar fraction 0.5) and 1-hexadecyl-3-methylimidazolium bromide (C16MIm-Br), after proper optimization of the overall method in combination with high-performance liquid chromatography (HPLC) and diode-array detection (DAD). The optimum conditions for 100 mL of water samples require a small amount (10 mg) of Fe3O4 magnetic nanoparticles, a low content (5.0 mg of C12C12Im-Br and 3.9 mg of C16MIm-Br) of the selected DSIL, pH 11, a sonication time of 2.5 min, and an equilibration time of 5 min with the aid of NdFeB magnets, followed by elution of phenols, evaporation, and reconstitution with 0.5 mL of acetonitrile. The overall m-μdSPE-HPLC-DAD method is characterized for limits of detection down to 1.3 μg · L(-1), intraday relative standard deviations lower than 13 % (n = 3), and interday relative standard deviations lower than 17 % (n = 9), with a spiking level of 15 μg · L(-1); with enrichment factors between 15.7 and 141, and average relative recoveries of 99.9 %.

  10. Simultaneous determination of a variety of endocrine disrupting compounds in carrot, lettuce and amended soil by means of focused ultrasonic solid-liquid extraction and dispersive solid-phase extraction as simplified clean-up strategy.

    Science.gov (United States)

    Mijangos, L; Bizkarguenaga, E; Prieto, A; Fernández, L A; Zuloaga, O

    2015-04-10

    The present study is focused on the development of an analytical method based on focused ultrasonic solid-liquid extraction (FUSLE) followed by dispersive solid-phase extraction (dSPE) clean-up and liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS) optimised for the simultaneous analysis of certain endocrine disrupting compounds (EDCs), including alkylphenols (APs), bisphenol A (BPA), triclosan (TCS) and several hormones and sterols in vegetables (lettuce and carrot) and amended soil samples. Different variables affecting the chromatographic separation, the electrospray ionisation and mass spectrometric detection were optimised in order to improve the sensitivity of the separation and detection steps. Under the optimised extraction conditions (sonication of 5min at 33% of power with pulse times on of 0.8s and pulse times off of 0.2s in 10mL of n-hexane:acetone (30:70, v:v) mixture using an ice bath), different dSPE clean-up sorbents, such as Florisil, Envi-Carb, primary-secondary amine bonded silica (PSA) and C18, or combinations of them were evaluated for FUSLE extracts before LC-MS/MS. Apparent recoveries and precision in terms of relative standard deviation (RSDs %) of the method were determined at two different fortification levels (according to the matrix and the analyte) and values in the 70-130% and 2-27% ranges, respectively, were obtained for most of the target analytes and matrices. Matrix-matched calibration approach and the use of labelled standards as surrogates were needed for the properly quantification of most analytes and matrices. Method detection limits (MDLs), estimated with fortified samples, in the ranges of 0.1-100ng/g for carrot, 0.2-152ng/g for lettuce and 0.9-31ng/g for amended soil were obtained. The developed methodology was applied to the analysis of 11 EDCs in both real vegetable bought in a local market and in compost (from a local wastewater treatment plant, WWTP) amended soil samples. Copyright © 2015

  11. 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).

  12. 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.

  13. Carbon nanotubes: are they dispersed or dissolved in liquids?

    Directory of Open Access Journals (Sweden)

    Premkumar Thathan

    2011-01-01

    Full Text Available Abstract Carbon nanotubes (CNTs constitute a novel class of nanomaterials with remarkable applications in diverse domains. However, the main intrincsic problem of CNTs is their insolubility or very poor solubility in most of the common solvents. The basic key question here is: are carbon nanotubes dissolved or dispersed in liquids, specifically in water? When analyzing the scientific research articles published in various leading journals, we found that many researchers confused between "dispersion" and "solubilization" and use the terms interchangeably, particularly when stating the interaction of CNTs with liquids. In this article, we address this fundamental issue to give basic insight specifically to the researchers who are working with CNTs as well asgenerally to scientists who deal with nano-related research domains.

  14. Simultaneous determination and qualitative analysis of six types of components in Naoxintong capsule by miniaturized matrix solid-phase dispersion extraction coupled with ultra high-performance liquid chromatography with photodiode array detection and quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Wang, Huilin; Jiang, Yan; Ding, Mingya; Li, Jin; Hao, Jia; He, Jun; Wang, Hui; Gao, Xiu-Mei; Chang, Yan-Xu

    2018-02-03

    A simple and effective sample preparation process based on miniaturized matrix solid-phase dispersion was developed for simultaneous determination of phenolic acids (gallic acid, chlorogenic acid, ferulic acid, 3,5-dicaffeoylqunic acid, 1,5-dicaffeoylqunic acid, rosmarinic acid, lithospermic acid, and salvianolic acid B), flavonoids (kaempferol-3-O-rutinoside, calycosin, and formononetin), lactones (ligustilide and butyllidephthalide), monoterpenoids (paeoniflorin), phenanthraquinones (cryptotanshinone), and furans (5-hydroxymethylfurfural) in Naoxintong capsule by ultra high-performance liquid chromatography. The optimized condition was that 25 mg Naoxintong powder was blended homogeneously with 100 mg Florisil PR for 4 min. One milliliter of methanol/water (75:25, v/v) acidified by 0.05% formic acid was selected to elute all components. It was found that the recoveries of the six types of components ranged from 61.36 to 96.94%. The proposed miniaturized matrix solid-phase dispersion coupled with ultra high-performance liquid chromatography was successfully applied to simultaneous determination of the six types of components in Naoxintong capsules. The results demonstrated that the proposed miniaturized matrix solid-phase dispersion coupled with ultra high-performance liquid chromatography could be used as an environmentally friendly tool for the extraction and determination of multiple bioactive components in natural products. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. 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

  16. Determination of five antiarrhythmic drugs in human plasma by dispersive liquid-liquid microextraction and high-performance liquid chromatography.

    Science.gov (United States)

    Jouyban, Abolghasem; Sorouraddin, Mohammad Hossein; Farajzadeh, Mir Ali; Somi, Mohammad Hossein; Fazeli-Bakhtiyari, Rana

    2015-03-01

    A fast and sensitive high-performance liquid chromatography (HPLC) method with ultraviolet (UV) detection was developed and validated for the simultaneous quantitation of five antiarrhythmic drugs (metoprolol, propranolol, carvedilol, diltiazem, and verapamil) in human plasma samples. It involves dispersive liquid-liquid microextraction (DLLME) of the desired drugs from 660 µL plasma and separation using isocratic elution with UV detection at 200 nm. The complete separation of all analytes was achieved within 7 min. Acetonitrile (as disperser solvent) resulting from the protein precipitation procedure was mixed with 100 µL dichloromethane (as an extraction solvent) and rapidly injected into 5 mL aqueous solution (pH 11.5) containing 1% (w/v), NaCl. After centrifugation, the sedimented phase containing enriched analytes was collected and evaporated to dryness. The residue was re-dissolved in 50 µL de-ionized water (acidified to pH 3) and injected into the HPLC system for analysis. Under the optimal conditions, the enrichment factors and extraction recoveries ranged between 4.4-10.8 and 33-82%, respectively. The suggested method was linear (r(2) ≥0.997) over a dynamic range of 0.02-0.80 µg mL(-1) in plasma. The intra- and inter-days relative standard deviation (RSD%) and relative error (RE%) values of the method were below 20%, which shows good precision and accuracy. Finally, this method was applied to the analysis of real plasma samples obtained from the patients treated with these drugs. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Spectrophotometric determination of mercury in water samples after preconcentration using dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Lemos, Valfredo Azevedo; dos Santos, Liz Oliveira; Silva, Eldevan dos Santos; Vieira, Emanuel Vitor dos Santos

    2012-01-01

    A simple method for the determination of mercury in water samples after preconcentration using dispersive liquid-liquid microextraction is described. The procedure is based on the extraction of mercury in the form of a complex and its subsequent determination by spectrophotometry. The complex is formed between Hg(II) and 2-(2-benzothiazolylazo)-p-cresol. The detection at 650 nm is performed directly in the metal-rich phase, which is spread on a triacetylcellulose membrane. The method eliminates the need to use a cuvet or large quantities of samples and reagents. The parameters that influence the preconcentration were studied, and the analytical characteristics were determined. The enrichment factor and the consumptive index for this method were 64 and 0.16 mL, respectively. The LOD (3.3 microg/L) and LOQ (11.1 microg/L) were also determined. The accuracy of the method was tested by the determination of mercury in certified reference materials BCR 397 (Human Hair) and SRM 2781 (Domestic Sludge). The method was applied to the determination of mercury in samples of drinking water, sea water, and river water.

  18. Recent development of ionic liquid stationary phases for liquid chromatography.

    Science.gov (United States)

    Shi, Xianzhe; Qiao, Lizhen; Xu, Guowang

    2015-11-13

    Based on their particular physicochemical characteristics, ionic liquids have been widely applied in many fields of analytical chemistry. Many types of ionic liquids were immobilized on a support like silica or monolith as stationary phases for liquid chromatography. Moreover, different approaches were developed to bond covalently ionic liquids onto the supporting materials. The obtained ionic liquid stationary phases show multi-mode mechanism including hydrophobic, hydrophilic, hydrogen bond, anion exchange, π-π, and dipole-dipole interactions. Therefore, they could be used in different chromatographic modes including ion-exchange, RPLC, NPLC and HILIC to separate various classes of compounds. This review mainly summarizes the immobilized patterns and types of ionic liquid stationary phases, their retention mechanisms and applications in the recent five years. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Supported ionic liquid-phase (SILP) catalysis

    DEFF Research Database (Denmark)

    Riisager, Anders; Fehrmann, Rasmus; Wasserscheid, P.

    2005-01-01

    The concept of supported ionic liquid-phase (SILP) catalysis has been demonstrated for gas- and liquid-phase continuous fixed-bed reactions using rhodium phosphine catalyzed hydroformylation of propene and 1-octene as examples. The nature of the support had important influence on both the catalytic...

  20. Conductivity of liquid lithium electrolytes with dispersed mesoporous silica particles

    International Nuclear Information System (INIS)

    Sann, K.; Roggenbuck, J.; Krawczyk, N.; Buschmann, H.; Luerßen, B.; Fröba, M.; Janek, J.

    2012-01-01

    Highlights: ► The conductivity of disperse lithium electrolytes with mesoporous fillers is studied. ► In contrast to other investigations in literature, no conductivity enhancement could be observed for standard battery electrolytes and typical mesoporous fillers in various combinations. ► Disperse electrolytes can become relevant in terms of battery safety. ► Dispersions of silicas and electrolyte with LiPF 6 as conducting salt are not stable, although the silicas were dried prior to preparation and the electrolyte water content was controlled. Surface modification of the fillers improved the stability. ► The observed conductivity decrease varied considerably for various fillers. - Abstract: The electrical conductivity of disperse electrolytes was systematically measured as a function of temperature (0 °C to 60 °C) and filler content for different types of fillers with a range of pore geometry, pore structure and specific surface area. As fillers mesoporous silicas SBA-15, MCM-41 and KIT-6 with pore ranges between 3 nm and 15 nm were dispersed in commercially available liquid lithium electrolytes. As electrolytes 1 M of lithium hexafluorophosphate (LiPF 6 ) in a mixture of ethylene carbonate (EC) and diethylene carbonate (DEC) at the ratio 3:7 (wt/wt) and the same solvent mixture with 0.96 M lithium bis(trifluoromethanesulfon)imide (LiTFSI) were used. No conductivity enhancement could be observed, but with respect to safety aspects the highly viscous disperse pastes might be useful. The conductivity decrease varied considerably for the different fillers.

  1. Spectral phase shift and residual angular dispersion of an accousto-optic programme dispersive filter

    International Nuclear Information System (INIS)

    Boerzsoenyi, A.; Meroe, M.

    2010-01-01

    Complete text of publication follows. There is an increasing demand for active and precise dispersion control of ultrashort laser pulses. In chirped pulse amplification (CPA) laser systems, the dispersion of the optical elements of the laser has to be compensated at least to the fourth order to obtain high temporal contrast compressed pulses. Nowadays the most convenient device for active and programmable control of spectral phase and amplitude of broadband laser pulses is the acousto-optic programmable dispersive filter (AOPDF), claimed to be able to adjust the spectral phase up to the fourth order. Although it has been widely used, surprisingly enough there has been only a single, low resolution measurement reported on the accuracy of the induced spectral phase shift of the device. In our paper we report on the first systematic experiment aiming at the precise characterization of an AOPDF device. In the experiment the spectral phase shift of the AOPDF device was measured by spectrally and spatially resolved interferometry, which is especially powerful tool to determine small dispersion values with high accuracy. Besides the spectral phase dispersion, we measured both the propagation direction angular dispersion (PDAD) and the phase front angular dispersion (PhFAD). Although the two quantities are equal for plane waves, there may be noticeable difference for Gaussian pulses. PDAD was determined simply by focusing the beam on the slit of an imaging spectrograph, while PhFAD was measured by the use of an inverted Mach-Zehnder interferometer and an imaging spectrograph. In the measurements, the spectral phase shift and both types of angular dispersion have been recorded upon the systematic change of all the accessible functions of the acousto-optic programmable dispersive filter. The measured values of group delay dispersion (GDD) and third order dispersion (TOD) have been found to agree with the preset values within the error of the measurement (1 fs 2 and 10 fs 3

  2. Liquid / liquid biphasic electrochemistry in ultra-turrax dispersed acetonitrile / aqueous electrolyte systems

    International Nuclear Information System (INIS)

    Watkins, John D.; Amemiya, Fumihiro; Atobe, Mahito; Bulman-Page, Philip C.; Marken, Frank

    2010-01-01

    Unstable acetonitrile | aqueous emulsions generated in situ with ultra-turrax agitation are investigated for applications in dual-phase electrochemistry. Three modes of operation for liquid / liquid aqueous-organic electrochemical processes are demonstrated with no intentionally added electrolyte in the organic phase based on (i) the formation of a water-soluble product in the aqueous phase in the presence of the organic phase, (ii) the formation of a product and ion transfer at the liquid / liquid-electrode triple phase boundary, and (iii) the formation of a water-insoluble product in the aqueous phase which then transfers into the organic phase. A three-electrode electrolysis cell with ultra-turrax agitator is employed and characterised for acetonitrile / aqueous 2 M NaCl two phase electrolyte. Three redox systems are employed in order to quantify the electrolysis cell performance. The one-electron reduction of Ru(NH 3 ) 6 3+ in the aqueous phase is employed to determine the rate of mass transport towards the electrode surface and the effect of the presence of the acetonitrile phase. The one-electron oxidation of n-butylferrocene in acetonitrile is employed to study triple phase boundary processes. Finally, the one-electron reduction of cobalticenium cations in the aqueous phase is employed to demonstrate the product transfer from the electrode surface into the organic phase. Potential applications in biphasic electrosynthesis are discussed.

  3. Time evolution of the drop size distribution for liquid-liquid dispersion in an agitated tank

    Czech Academy of Sciences Publication Activity Database

    Šulc, R.; Kysela, Bohuš; Ditl, P.

    2018-01-01

    Roč. 72, č. 3 (2018), s. 543-553 ISSN 0366-6352 R&D Projects: GA ČR GA16-20175S Institutional support: RVO:67985874 Keywords : liquid–liquid dispersion * drop breakup * drop size distribution * time evolution Subject RIV: BK - Fluid Dynamics Impact factor: 1.258, year: 2016

  4. Raman scattering temperature measurements for water vapor in nonequilibrium dispersed two-phase flow

    International Nuclear Information System (INIS)

    Anastasia, C.M.; Neti, S.; Smith, W.R.; Chen, J.C.

    1982-09-01

    The objective of this investigation was to determine the feasibility of using Raman scattering as a nonintrusive technique to measure vapor temperatures in dispersed two-phase flow. The Raman system developed for this investigation is described, including alignment of optics and optimization of the photodetector for photon pulse counting. Experimentally obtained Raman spectra are presented for the following single- and two-phase samples: liquid water, atmospheric nitrogen, superheated steam, nitrogen and water droplets in a high void fraction air/water mist, and superheated water vapor in nonequilibrium dispersed flow

  5. Interaction of dispersed cubic phases with blood components

    DEFF Research Database (Denmark)

    Bode, J C; Kuntsche, Judith; Funari, S S

    2013-01-01

    The interaction of aqueous nanoparticle dispersions, e.g. based on monoolein/poloxamer 407, with blood components is an important topic concerning especially the parenteral way of administration. Therefore, the influence of human and porcine plasma on dispersed cubic phases was investigated. Part...... activity of cubic phases based on monoolein and poloxamer 188, on soy phosphatidylcholine, glycerol dioleate and polysorbate 80 or the parenteral fat emulsion Lipofundin MCT 20%....

  6. Ultrasonic absorption and velocity dispersion of binary mixture liquid crystal MBBA/EBBA

    International Nuclear Information System (INIS)

    Choi, K.

    1979-01-01

    The effect of phase transitions and the partial magnetic alignment for liquid crystal molecules on the ultrasonic absorption and velocity dispersion has been investigated. The binary mixture of Shiff base liquid crystals MBBA/EBBA (55:45 mole %) showed anomalous ultrasonic absorption and velocity dispersion at eutectic (Tsub(m) = -20 0 C) and clearing point (Tsub(c) = 50 0 C) at the frequency range of 5 MHz, 10MHz, 15MHz and 30 MHz. The experimental data were analyzed in terms of relaxation time and Fixman theory. The anisotropy of the propagation velocity due to the magnetic alignment was about 0.9% (the deviation between velocities propagating parallel and perpendicular to the applied field). (author)

  7. 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)

  8. Supported Ionic Liquid Phase (SILP) catalysis

    DEFF Research Database (Denmark)

    Riisager, Anders; Fehrmann, Rasmus; Haumann, Marco

    2006-01-01

    Applications of ionic liquids to replace conventional solvents in homogeneous transition-metal catalysis have increased significantly during the last decade. Biphasic ionic liquid/organic liquid systems offer advantages with regard to product separation, catalyst stability, and recycling...... but utilise in the case of fast chemical reactions only a small amount of expensive ionic liquid and catalyst. The novel Supported Ionic Liquid Phase (SILP) catalysis concept overcomes these drawbacks and allows the use of fixed-bed reactors for continuous reactions. In this Microreview the SILP catalysis...

  9. Determination of statin drugs in hospital effluent with dispersive liquid-liquid microextraction and quantification by liquid chromatography.

    Science.gov (United States)

    Martins, Ayrton F; Frank, Carla da S; Altissimo, Joseline; de Oliveira, Júlia A; da Silva, Daiane S; Reichert, Jaqueline F; Souza, Darliana M

    2017-08-24

    Statins are classified as being amongst the most prescribed agents for treating hypercholesterolaemia and preventing vascular diseases. In this study, a rapid and effective liquid chromatography method, assisted by diode array detection, was designed and validated for the simultaneous quantification of atorvastatin (ATO) and simvastatin (SIM) in hospital effluent samples. The solid phase extraction (SPE) of the analytes was optimized regarding sorbent material and pH, and the dispersive liquid-liquid microextraction (DLLME), in terms of pH, ionic strength, type and volume of extractor/dispersor solvents. The performance of both extraction procedures was evaluated in terms of linearity, quantification limits, accuracy (recovery %), precision and matrix effects for each analyte. The methods proved to be linear in the concentration range considered; the quantification limits were 0.45 µg L -1 for ATO and 0.75 µg L -1 for SIM; the matrix effect was almost absent in both methods and the average recoveries remained between 81.5-90.0%; and the RSD values were <20%. The validated methods were applied to the quantification of the statins in real samples of hospital effluent; the concentrations ranged from 18.8 µg L -1 to 35.3 µg L -1 for ATO, and from 30.3 µg L -1 to 38.5 µg L -1 for SIM. Since the calculated risk quotient was ≤192, the occurrence of ATO and SIM in hospital effluent poses a potential serious risk to human health and the aquatic ecosystem.

  10. 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.

  11. 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.

  12. Evaluating the Liquid Liquid Phase Transition Hypothesis of Supercoooled Water

    Science.gov (United States)

    Limmer, David; Chandler, David

    2011-03-01

    To explain the anomalous behavior of supercooled water it has been conjectured that buried within an experimentally inaccessible region of liquid water's phase diagram there exists a second critical point, which is the terminus of a first order transition line between two distinct liquid phases. The so-called liquid-liquid phase transition (LLPT) has since generated much study, though to date there is no consensus on its existence. In this talk, we will discuss our efforts to systematically study the metastable phase diagram of supercooled water through computer simulation. By employing importance-sampling techniques, we have calculated free energies as a function of the density and long-range order to determine unambiguously if two distinct liquid phases exist. We will argue that, contrary to the LLPT hypothesis, the observed phenomenology can be understood as a consequence of the limit of stability of the liquid far away from coexistence. Our results suggest that homogeneous nucleation is the cause of the increased fluctuations present upon supercooling. Further we will show how this understanding can be extended to explain experimental observations of hysteresis in confined supercooled water systems.

  13. Investigation of the propagation characteristics in turbulent dispersed two-phase flow

    International Nuclear Information System (INIS)

    Sami, S.M.

    1980-01-01

    The propagation characteristics of turbulent dispersed two-phase flows have been studied experimentally using the Pitot tube associated with a conical hot-film anemometer. It is found that the mixture velocity increases with decreasing volumetric mixing ratio of the air and water. The void fraction distribution shows homogeneity across the test section in the special case of fully developed boundary layer two-phase flow. An expression is obtained which relates the local mixture velocity to the local void fraction, gas and liquid densities, and volumetric gas-liquid ratio

  14. Study of axial mixing, holdup and slip velocity of dispersed phase in a pulsed sieve plate extraction column using radiotracer technique.

    Science.gov (United States)

    Ghiyas Ud Din; Imran Rafiq Chughtai; Hameed Inayat, Mansoor; Hussain Khan, Iqbal

    2009-01-01

    Axial mixing, holdup and slip velocity of dispersed phase which are parameters of fundamental importance in the design and operation of liquid-liquid extraction pulsed sieve plate columns have been investigated. Experiments for residence time distribution (RTD) analysis have been carried out for a range of pulsation frequency and amplitude in a liquid-liquid extraction pulsed sieve plate column with water as dispersed and kerosene as continuous phase using radiotracer technique. The column was operated in emulsion region and (99m)Tc in the form of sodium pertechnetate eluted from a (99)Mo/(99m)Tc generator was used to trace the dispersed phase. Axial dispersed plug flow model with open-open boundary condition and two points measurement method was used to simulate the hydrodynamics of dispersed phase. It has been observed that the axial mixing and holdup of dispersed phase increases with increase in pulsation frequency and amplitude until a maximum value is achieved while slip velocity decreases with increase in pulsation frequency and amplitude until it approaches a minimum value. Short lived and low energy radiotracer (99m)Tc in the form of sodium pertechnetate was found to be a good water tracer to study the hydrodynamics of a liquid-liquid extraction pulsed sieve plate column operating with two immiscible liquids, water and kerosene. Axial dispersed plug flow model with open-open boundary condition was found to be a suitable model to describe the hydrodynamics of dispersed phase in the pulsed sieve plate extraction column.

  15. Study of axial mixing, holdup and slip velocity of dispersed phase in a pulsed sieve plate extraction column using radiotracer technique

    International Nuclear Information System (INIS)

    Ghiyas Ud Din; Imran Rafiq Chughtai; Mansoor Hameed Inayat; Iqbal Hussain Khan

    2009-01-01

    Axial mixing, holdup and slip velocity of dispersed phase which are parameters of fundamental importance in the design and operation of liquid-liquid extraction pulsed sieve plate columns have been investigated. Experiments for residence time distribution (RTD) analysis have been carried out for a range of pulsation frequency and amplitude in a liquid-liquid extraction pulsed sieve plate column with water as dispersed and kerosene as continuous phase using radiotracer technique. The column was operated in emulsion region and 99m Tc in the form of sodium pertechnetate eluted from a 99 Mo/ 99m Tc generator was used to trace the dispersed phase. Axial dispersed plug flow model with open-open boundary condition and two points measurement method was used to simulate the hydrodynamics of dispersed phase. It has been observed that the axial mixing and holdup of dispersed phase increases with increase in pulsation frequency and amplitude until a maximum value is achieved while slip velocity decreases with increase in pulsation frequency and amplitude until it approaches a minimum value. Short lived and low energy radiotracer 99m Tc in the form of sodium pertechnetate was found to be a good water tracer to study the hydrodynamics of a liquid-liquid extraction pulsed sieve plate column operating with two immiscible liquids, water and kerosene. Axial dispersed plug flow model with open-open boundary condition was found to be a suitable model to describe the hydrodynamics of dispersed phase in the pulsed sieve plate extraction column.

  16. Exfoliation in ecstasy: liquid crystal formation and concentration-dependent debundling observed for single-wall nanotubes dispersed in the liquid drug γ-butyrolactone

    Science.gov (United States)

    Bergin, Shane D.; Nicolosi, Valeria; Giordani, Silvia; de Gromard, Antoine; Carpenter, Leslie; Blau, Werner J.; Coleman, Jonathan N.

    2007-11-01

    Large-scale debundling of single-walled nanotubes has been demonstrated by dilution of nanotube dispersions in the solvent γ-butyrolactone. This liquid, sometimes referred to as 'liquid ecstasy', is well known for its narcotic properties. At high concentrations the dispersions form an anisotropic, liquid crystalline phase which can be removed by mild centrifugation. At lower concentrations an isotropic phase is observed with a biphasic region at intermediate concentrations. By measuring the absorbance before and after centrifugation, as a function of concentration, the relative anisotropic and isotropic nanotube concentrations can be monitored. The upper limit of the pure isotropic phase was CNT~0.004 mg ml-1, suggesting that this can be considered the nanotube dispersion limit in γ-butyrolactone. After centrifugation, the dispersions are stable against sedimentation and further aggregation for a period of 8 weeks at least. Atomic-force-microscopy studies on films deposited from the isotropic phase reveal that the bundle diameter distribution decreases dramatically as concentration is decreased. Detailed data analysis suggests the presence of an equilibrium bundle number density. A population of individual nanotubes is always observed which increases with decreasing concentration until almost 40% of all dispersed objects are individual nanotubes at a concentration of 6 × 10-4 mg ml-1. The number density of individual nanotubes peaks at a concentration of ~6 × 10-3 mg ml-1 where almost 10% of the nanotubes by mass are individualized.

  17. Exfoliation in ecstasy: liquid crystal formation and concentration-dependent debundling observed for single-wall nanotubes dispersed in the liquid drug γ-butyrolactone

    International Nuclear Information System (INIS)

    Bergin, Shane D; Nicolosi, Valeria; Giordani, Silvia; Gromard, Antoine de; Carpenter, Leslie; Blau, Werner J; Coleman, Jonathan N

    2007-01-01

    Large-scale debundling of single-walled nanotubes has been demonstrated by dilution of nanotube dispersions in the solvent γ-butyrolactone. This liquid, sometimes referred to as 'liquid ecstasy', is well known for its narcotic properties. At high concentrations the dispersions form an anisotropic, liquid crystalline phase which can be removed by mild centrifugation. At lower concentrations an isotropic phase is observed with a biphasic region at intermediate concentrations. By measuring the absorbance before and after centrifugation, as a function of concentration, the relative anisotropic and isotropic nanotube concentrations can be monitored. The upper limit of the pure isotropic phase was C NT ∼0.004 mg ml -1 , suggesting that this can be considered the nanotube dispersion limit in γ-butyrolactone. After centrifugation, the dispersions are stable against sedimentation and further aggregation for a period of 8 weeks at least. Atomic-force-microscopy studies on films deposited from the isotropic phase reveal that the bundle diameter distribution decreases dramatically as concentration is decreased. Detailed data analysis suggests the presence of an equilibrium bundle number density. A population of individual nanotubes is always observed which increases with decreasing concentration until almost 40% of all dispersed objects are individual nanotubes at a concentration of 6 x 10 -4 mg ml -1 . The number density of individual nanotubes peaks at a concentration of ∼6 x 10 -3 mg ml -1 where almost 10% of the nanotubes by mass are individualized

  18. 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.

  19. A new chiral residue analysis method for triazole fungicides in water using dispersive liquid-liquid microextraction (DLLME).

    Science.gov (United States)

    Luo, Mai; Liu, Donghui; Zhou, Zhiqiang; Wang, Peng

    2013-09-01

    A rapid, simple, reliable, and environment-friendly method for the residue analysis of the enantiomers of four chiral fungicides including hexaconazole, triadimefon, tebuconazole, and penconazole in water samples was developed by dispersive liquid-liquid microextraction (DLLME) pretreatment followed by chiral high-performance liquid chromatography (HPLC)-DAD detection. The enantiomers were separated on a Chiralpak IC column by HPLC applying n-hexane or petroleum ether as mobile phase and ethanol or isopropanol as modifier. The influences of mobile phase composition and temperature on the resolution were investigated and most of the enantiomers could be completely separated in 20 min under optimized conditions. The thermodynamic parameters indicated that the separation was enthalpy-driven. The elution orders were detected by both circular dichroism detector (CD) and optical rotatory dispersion detector (ORD). Parameters affecting the DLLME performance for pretreatment of the chiral fungicides residue in water samples, such as the extraction and dispersive solvents and their volume, were studied and optimized. Under the optimum microextraction condition the enrichment factors were over 121 and the linearities were 30-1500 µg L(-1) with the correlation coefficients (R(2)) over 0.9988 and the recoveries were between 88.7% and 103.7% at the spiking levels of 0.5, 0.25, and 0.05 mg L(-1) (for each enantiomer) with relative standard deviations varying from 1.38% to 6.70% (n = 6) The limits of detection (LODs) ranged from 8.5 to 29.0 µg L(-1) (S/N = 3). © 2013 Wiley Periodicals, Inc.

  20. Comment on "Spontaneous liquid-liquid phase separation of water"

    Science.gov (United States)

    Limmer, David T.; Chandler, David

    2015-01-01

    Yagasaki et al. [Phys. Rev. E 89, 020301 (2014), 10.1103/PhysRevE.89.020301] present results from a molecular dynamics trajectory illustrating coarsening of ice, which they interpret as evidence of transient coexistence between two distinct supercooled phases of liquid water. We point out that neither two distinct liquids nor criticality are demonstrated in this simulation study. Instead, the illustrated trajectory is consistent with coarsening behaviors analyzed and predicted in earlier work by others.

  1. Comment on "Spontaneous liquid-liquid phase separation of water".

    Science.gov (United States)

    Limmer, David T; Chandler, David

    2015-01-01

    Yagasaki et al. [Phys. Rev. E 89, 020301 (2014)] present results from a molecular dynamics trajectory illustrating coarsening of ice, which they interpret as evidence of transient coexistence between two distinct supercooled phases of liquid water. We point out that neither two distinct liquids nor criticality are demonstrated in this simulation study. Instead, the illustrated trajectory is consistent with coarsening behaviors analyzed and predicted in earlier work by others.

  2. 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.

  3. Fully-automated in-syringe dispersive liquid-liquid microextraction for the determination of caffeine in coffee beverages.

    Science.gov (United States)

    Frizzarin, Rejane M; Maya, Fernando; Estela, José M; Cerdà, Víctor

    2016-12-01

    A novel fully-automated magnetic stirring-assisted lab-in-syringe analytical procedure has been developed for the fast and efficient dispersive liquid-liquid microextraction (DLLME) of caffeine in coffee beverages. The procedure is based on the microextraction of caffeine with a minute amount of dichloromethane, isolating caffeine from the sample matrix with no further sample pretreatment. Selection of the relevant extraction parameters such as the dispersive solvent, proportion of aqueous/organic phase, pH and flow rates have been carefully evaluated. Caffeine quantification was linear from 2 to 75mgL(-1), with detection and quantification limits of 0.46mgL(-1) and 1.54mgL(-1), respectively. A coefficient of variation (n=8; 5mgL(-1)) of a 2.1% and a sampling rate of 16h(-1), were obtained. The procedure was satisfactorily applied to the determination of caffeine in brewed, instant and decaf coffee samples, being the results for the sample analysis validated using high-performance liquid chromatography. Copyright © 2016 Elsevier Ltd. All rights reserved.

  4. Study of memory effects in polymer dispersed liquid crystal films

    International Nuclear Information System (INIS)

    Han, Jinwoo

    2006-01-01

    In this work, we have studied the memory effects in polymer dispersed liquid crystal films. We found that optical responses, such as the memory effects, of the films depended strongly on the morphology. For example, memory effects were observed for films with polymer ball morphologies; however, only weak hysteresis effects were observed for films with droplet morphologies. In particular, a stronger memory effect was observed for films with more complicated polymer ball structures. Coincidentally, T TE , the temperature at which the memory state is thermally erased, was generally higher for the films exhibiting a stronger memory effect. In addition, studies of the temporal evolution of the films show that the memory effects become stronger after films have been kept on the shelf for a period of time. This change is likely to be associated with a modification of surface anchoring properties at the LC-polymer interface.

  5. Theoretical study of liquid droplet dispersion in a venturi scrubber.

    Science.gov (United States)

    Fathikalajahi, J; Talaie, M R; Taheri, M

    1995-03-01

    The droplet concentration distribution in an atomizing scrubber was calculated based on droplet eddy diffusion by a three-dimensional dispersion model. This model is also capable of predicting the liquid flowing on the wall. The theoretical distribution of droplet concentration agrees well with experimental data given by Viswanathan et al. for droplet concentration distribution in a venturi-type scrubber. The results obtained by the model show a non-uniform distribution of drops over the cross section of the scrubber, as noted by the experimental data. While the maximum of droplet concentration distribution may depend on many operating parameters of the scrubber, the results of this study show that the highest uniformity of drop distribution will be reached when penetration length is approximately equal to one-fourth of the depth of the scrubber. The results of this study can be applied to evaluate the removal efficiency of a venturi scrubber.

  6. The recent developments in dispersive liquid–liquid microextraction for preconcentration and determination of inorganic analytes

    Directory of Open Access Journals (Sweden)

    H.M. Al-Saidi

    2014-12-01

    Full Text Available Recently, increasing interest on the use of dispersive liquid–liquid microextraction (DLLME developed in 2006 by Rezaee has been found in the field of separation science. DLLME is miniaturized format of liquid–liquid extraction in which acceptor-to-donor phase ratio is greatly reduced compared with other methods. In the present review, the combination of DLLME with different analytical techniques such as atomic absorption spectrometry (AAS, inductively coupled plasma-optical emission spectrometry (ICP-OES, gas chromatography (GC, and high-performance liquid chromatography (HPLC for preconcentration and determination of inorganic analytes in different types of samples will be discussed. Recent developments in DLLME, e.g., displacement-DLLME, the use of an auxiliary solvent for adjustment of density of extraction mixture, and the application of ionic liquid-based DLLME in determination of inorganic species even in the presence of high content of salts are presented in the present review. Finally, comparison of DLLME with the other liquid-phase microextraction approaches and limitations of this technique are provided.

  7. Liquid Crystals - The 'Fourth' Phase of Matter

    Indian Academy of Sciences (India)

    possibilities of novel technological applications. Liquid crystalline materials ... advanced instrumentation, including laptops and futuristic flat panel displays. .... The twist grain-boundary phase is formed when the layers of a smectic A phase are .... the optic axis) is uniformly oriented parallel to the glass plate. (see Figure IIa).

  8. Glass-liquid-glass reentrance in mono-component colloidal dispersions

    International Nuclear Information System (INIS)

    Ramirez-Gonzalez, P E; Medina-Noyola, M; Vizcarra-Rendon, A; Guevara-Rodriguez, F de J

    2008-01-01

    The self-consistent generalized Langevin equation (SCGLE) theory of colloid dynamics is employed to describe the ergodic-non-ergodic transition in model mono-disperse colloidal dispersions whose particles interact through hard-sphere plus short-ranged attractive forces. The ergodic-non-ergodic phase diagram in the temperature-concentration state space is determined for the hard-sphere plus attractive Yukawa model within the mean spherical approximation for the static structure factor by solving a remarkably simple equation for the localization length of the colloidal particles. Finite real values of this property signals non-ergodicity and determines the non-ergodic parameters f(k) and f s (k). The resulting phase diagram for this system, which involves the existence of reentrant (repulsive and attractive) glass states, is compared with the corresponding prediction of mode coupling theory. Although both theories coincide in the general features of this phase diagram, there are also clear qualitative differences. One of the most relevant is the SCGLE prediction that the ergodic-attractive glass transition does not preempt the gas-liquid phase transition, but always intersects the corresponding spinodal curve on its high-concentration side. We also calculate the ergodic-non-ergodic phase diagram for the sticky hard-sphere model to illustrate the dependence of the predicted SCGLE dynamic phase diagram on the choice of one important constituent element of the SCGLE theory

  9. Glass-liquid-glass reentrance in mono-component colloidal dispersions

    Energy Technology Data Exchange (ETDEWEB)

    Ramirez-Gonzalez, P E; Medina-Noyola, M [Instituto de Fisica ' Manuel Sandoval Vallarta' , Universidad Autonoma de San Luis Potosi, Alvaro Obregon 64, 78000 San Luis Potosi, SLP (Mexico); Vizcarra-Rendon, A [Unidad Academica de Fisica, Universidad Autonoma de Zacatecas, Paseo la Bufa y Calzada Solidaridad, 98600, Zacatecas, Zac. (Mexico); Guevara-Rodriguez, F de J [Coordinacion de IngenierIa Molecular, Instituto Mexicano del Petroleo, Eje Central Lazaro Cardenas 152, 07730 Mexico, DF (Mexico)

    2008-05-21

    The self-consistent generalized Langevin equation (SCGLE) theory of colloid dynamics is employed to describe the ergodic-non-ergodic transition in model mono-disperse colloidal dispersions whose particles interact through hard-sphere plus short-ranged attractive forces. The ergodic-non-ergodic phase diagram in the temperature-concentration state space is determined for the hard-sphere plus attractive Yukawa model within the mean spherical approximation for the static structure factor by solving a remarkably simple equation for the localization length of the colloidal particles. Finite real values of this property signals non-ergodicity and determines the non-ergodic parameters f(k) and f{sub s}(k). The resulting phase diagram for this system, which involves the existence of reentrant (repulsive and attractive) glass states, is compared with the corresponding prediction of mode coupling theory. Although both theories coincide in the general features of this phase diagram, there are also clear qualitative differences. One of the most relevant is the SCGLE prediction that the ergodic-attractive glass transition does not preempt the gas-liquid phase transition, but always intersects the corresponding spinodal curve on its high-concentration side. We also calculate the ergodic-non-ergodic phase diagram for the sticky hard-sphere model to illustrate the dependence of the predicted SCGLE dynamic phase diagram on the choice of one important constituent element of the SCGLE theory.

  10. Introducing a new and rapid microextraction approach based on magnetic ionic liquids: Stir bar dispersive liquid microextraction

    International Nuclear Information System (INIS)

    Chisvert, Alberto; Benedé, Juan L.; Anderson, Jared L.; Pierson, Stephen A.; Salvador, Amparo

    2017-01-01

    principles of SBSE and DLLME is presented. • Magnetic ionic liquids (MILs) are used as extraction phase. • At low stirring rate, it acts as SBSE; at higher rates MILs are dispersed as in DLLME. • The determination of lipophilic UV filters in waters is chosen as model application. • The method has been developed and validated obtaining good analytical features.

  11. Liquid phase and supercooled liquid phase welding of bulk metallic glasses

    International Nuclear Information System (INIS)

    Kawamura, Y.

    2004-01-01

    Recent progress on welding in bulk metallic glasses (BMGs) has been reviewed. BMGs have been successfully welded to BMGs or crystalline metals by liquid phase welding using explosion, pulse-current and electron-beam methods, and by supercooled liquid phase welding using friction method. Successful welding of the liquid phase methods was due to the high glass-forming ability of the BMGs and the high concentration of welding energy in these methods. In contrast, the supercooled liquid phase welding was successful due to the thermally stable supercooled liquid state of the BMGs and the superplasticity and viscous flow of the supercooled liquid. The successful welding of BMGs to BMGs and crystalline materials is promising for the future development of BMGs as engineering materials

  12. 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.

  13. Stabilization of liquid crystal dispersion by nonionic surfactant/acrylamide copolymer containing hydrophobic moieties

    Energy Technology Data Exchange (ETDEWEB)

    Park, S.J.; Kim, M.H.; Lee, J.R. [Korea Research Institute of Chemical Technology, Taejon (Korea)

    1999-07-01

    The effect of nonionic surfactant (H(OCH){sub 2}-OC{sub 6}H{sub 4}-C{sub 9}H{sub 19}, NP-8) and acrylamide copolymer containing nonylphenyl groups as hydrophobic moieties on the stabilization of liquid crystal (LC)-in-water dispersion has been studied. According to cloud point and adsorption measurements, the hydrophobically strong interaction between NP-8 and the nonylphenol moieties is formed. And the addition of surfactant increases the stability of LC dispersion and improve the electrooptical properties of the nematic curvilinear aligned phase (NCAP) composite film. It is due to the presence of surfactant which allows the formation of nonpolar microenvironment in the round of LC droplet and finally reduces the anchoring effect between LC and the polymeric wall. 21 refs., 8 figs.

  14. Modified ionic liquid cold-induced aggregation dispersive liquid-liquid microextraction followed by atomic absorption spectrometry for trace determination of zinc in water and food samples

    International Nuclear Information System (INIS)

    Zeeb, M.; Sadeghi, M.

    2011-01-01

    We report on a new method for the microextraction and determination of zinc (II). The ion is accumulated via ionic-liquid cold-induced aggregation dispersive liquid-liquid microextraction (IL-CIA-DLLME) followed by flame atomic absorption spectrometry (FAAS). The ionic liquid (IL) 1-hexyl-3-methylimidazolium hexafluorophosphate is dispersed into a heated sample solution containing sodium hexafluorophosphate as a common ion source. The solution is then placed in an ice-water bath upon which a cloudy solution forms due to the decrease of the solubility of the IL. Zinc is complexed with 8-hydroxyquinoline and extracted into the IL. The enriched phase is dissolved in a diluting agent and introduced to the FAAS. The method is not influenced by variations in the ionic strength of the sample solution. Factors affecting the performance were evaluated and optimized. At optimum conditions, the limit of detection is 0.18 μg L -1 , and the relative standard deviation is 3.0% (at n=5). The method was validated by recovery experiments and by analyzing a certified reference material and successfully applied to the determination of Zn (II) in water and food samples. (author)

  15. 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.

  16. 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.

  17. Strongly coupled dispersed two-phase flows; Ecoulements diphasiques disperses fortement couples

    Energy Technology Data Exchange (ETDEWEB)

    Zun, I.; Lance, M.; Ekiel-Jezewska, M.L.; Petrosyan, A.; Lecoq, N.; Anthore, R.; Bostel, F.; Feuillebois, F.; Nott, P.; Zenit, R.; Hunt, M.L.; Brennen, C.E.; Campbell, C.S.; Tong, P.; Lei, X.; Ackerson, B.J.; Asmolov, E.S.; Abade, G.; da Cunha, F.R.; Lhuillier, D.; Cartellier, A.; Ruzicka, M.C.; Drahos, J.; Thomas, N.H.; Talini, L.; Leblond, J.; Leshansky, A.M.; Lavrenteva, O.M.; Nir, A.; Teshukov, V.; Risso, F.; Ellinsen, K.; Crispel, S.; Dahlkild, A.; Vynnycky, M.; Davila, J.; Matas, J.P.; Guazelli, L.; Morris, J.; Ooms, G.; Poelma, C.; van Wijngaarden, L.; de Vries, A.; Elghobashi, S.; Huilier, D.; Peirano, E.; Minier, J.P.; Gavrilyuk, S.; Saurel, R.; Kashinsky, O.; Randin, V.; Colin, C.; Larue de Tournemine, A.; Roig, V.; Suzanne, C.; Bounhoure, C.; Brunet, Y.; Tanaka, A.T.; Noma, K.; Tsuji, Y.; Pascal-Ribot, S.; Le Gall, F.; Aliseda, A.; Hainaux, F.; Lasheras, J.; Didwania, A.; Costa, A.; Vallerin, W.; Mudde, R.F.; Van Den Akker, H.E.A.; Jaumouillie, P.; Larrarte, F.; Burgisser, A.; Bergantz, G.; Necker, F.; Hartel, C.; Kleiser, L.; Meiburg, E.; Michallet, H.; Mory, M.; Hutter, M.; Markov, A.A.; Dumoulin, F.X.; Suard, S.; Borghi, R.; Hong, M.; Hopfinger, E.; Laforgia, A.; Lawrence, C.J.; Hewitt, G.F.; Osiptsov, A.N.; Tsirkunov, Yu. M.; Volkov, A.N.

    2003-07-01

    This document gathers the abstracts of the Euromech 421 colloquium about strongly coupled dispersed two-phase flows. Behaviors specifically due to the two-phase character of the flow have been categorized as: suspensions, particle-induced agitation, microstructure and screening mechanisms; hydrodynamic interactions, dispersion and phase distribution; turbulence modulation by particles, droplets or bubbles in dense systems; collective effects in dispersed two-phase flows, clustering and phase distribution; large-scale instabilities and gravity driven dispersed flows; strongly coupled two-phase flows involving reacting flows or phase change. Topic l: suspensions particle-induced agitation microstructure and screening mechanisms hydrodynamic interactions between two very close spheres; normal stresses in sheared suspensions; a critical look at the rheological experiments of R.A. Bagnold; non-equilibrium particle configuration in sedimentation; unsteady screening of the long-range hydrodynamic interactions of settling particles; computer simulations of hydrodynamic interactions among a large collection of sedimenting poly-disperse particles; velocity fluctuations in a dilute suspension of rigid spheres sedimenting between vertical plates: the role of boundaries; screening and induced-agitation in dilute uniform bubbly flows at small and moderate particle Reynolds numbers: some experimental results. Topic 2: hydrodynamic interactions, dispersion and phase distribution: hydrodynamic interactions in a bubble array; A 'NMR scattering technique' for the determination of the structure in a dispersion of non-brownian settling particles; segregation and clustering during thermo-capillary migration of bubbles; kinetic modelling of bubbly flows; velocity fluctuations in a homogeneous dilute dispersion of high-Reynolds-number rising bubbles; an attempt to simulate screening effects at moderate particle Reynolds numbers using an hybrid formulation; modelling the two-phase

  18. The nuclear liquid gas phase transition and phase coexistence

    International Nuclear Information System (INIS)

    Chomaz, Ph.

    2001-01-01

    In this talk we will review the different signals of liquid gas phase transition in nuclei. From the theoretical side we will first discuss the foundations of the concept of equilibrium, phase transition and critical behaviors in infinite and finite systems. From the experimental point of view we will first recall the evidences for some strong modification of the behavior of hot nuclei. Then we will review quantitative detailed analysis aiming to evidence phase transition, to define its order and phase diagram. Finally, we will present a critical discussion of the present status of phase transitions in nuclei and we will draw some lines for future development of this field. (author)

  19. The nuclear liquid gas phase transition and phase coexistence

    Energy Technology Data Exchange (ETDEWEB)

    Chomaz, Ph

    2001-07-01

    In this talk we will review the different signals of liquid gas phase transition in nuclei. From the theoretical side we will first discuss the foundations of the concept of equilibrium, phase transition and critical behaviors in infinite and finite systems. From the experimental point of view we will first recall the evidences for some strong modification of the behavior of hot nuclei. Then we will review quantitative detailed analysis aiming to evidence phase transition, to define its order and phase diagram. Finally, we will present a critical discussion of the present status of phase transitions in nuclei and we will draw some lines for future development of this field. (author)

  20. Chromatic dispersion of liquid crystal infiltrated capillary tubes and photonic crystal fibers

    DEFF Research Database (Denmark)

    Rasmussen, Per Dalgaard; Lægsgaard, Jesper; Bang, Ole

    2006-01-01

    We consider chromatic dispersion of capillary tubes and photonic crystal fibers infiltrated with liquid crystals. A perturbative scheme for inclusion of material dispersion of both liquid crystal and the surrounding waveguide material is derived. The method is used to calculate the chromatic...

  1. 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.

  2. Ligandless-dispersive liquid-liquid microextraction of trace amount of copper ions

    Energy Technology Data Exchange (ETDEWEB)

    Mohammadi, Sayed Zia, E-mail: szmohammadi@yahoo.com [Department of Chemistry, Payame Noor University (PNU), Kerman (Iran, Islamic Republic of); Afzali, Daryoush [Environment Department, Institute Research of Environmental Sciences, International Center for Science, High Technology and Environmental Sciences, Kerman (Iran, Islamic Republic of); Baghelani, Yar Mohammad [Department of Chemistry, Payame Noor University (PNU), Kerman (Iran, Islamic Republic of)

    2009-10-27

    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{sup -1}-0.6 {mu}g mL{sup -1} of copper with R{sup 2} = 0.9985. Detection limit was 0.5 ng mL{sup -1} in original solution (3S{sub b}/m) and the relative standard deviation for seven replicate determination of 0.2 {mu}g mL{sup -1} copper was {+-}1.4%. The proposed method has been applied for determination of copper in standard and water samples with satisfactory results.

  3. 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.

  4. Quantitation of tetrabromobisphenol-A from dust sampled on consumer electronics by dispersed liquid-liquid microextraction

    International Nuclear Information System (INIS)

    Di Napoli-Davis, Gina; Owens, Janel E.

    2013-01-01

    Tetrabromobisphenol-A (TBBPA) is a brominated flame retardant used worldwide. Despite its widespread use, there are few data concerning environmental concentrations of TBBPA. Thus, the objective of this work was to optimize an ultrasound-assisted dispersed liquid-liquid microextraction (DLLME) method to analyze swabbed surfaces of consumer electronics to determine TBBPA concentrations. Upon sample preparation with DLLME, TBBPA was derivatized with acetic anhydride and then analyzed by gas chromatography–mass spectrometry (GC/MS). Using a 13 C 12 -TBBPA internal standard to improve precision and quantitation, a recovery study was performed. At concentrations of 250–1000 ng/mL, recoveries were 104–106%. Sample preparation with solid phase extraction had comparable recoveries, although overall, improved analyte recovery and precision were achieved with DLLME. In a small survey study, TBBPA concentrations in dust collected from 100 cm 2 areas on electronic surfaces (monitor, microwave, refrigerator, and TV) were determined to range from less than the LOQ to 523 ng/mL. -- Highlights: •Tetrabromobisphenol-A (TBBPA) concentrations in dust samples were determined. •Dust samples were collected from surfaces of consumer electronics. •Dispersed liquid-liquid microextraction was used to prepare samples for GC/MS. •A 13 C 12 -labeled internal standard was used to improve precision and quantitation. •TBBPA was found in dust samples at levels below LOQ to 523 ng/mL. -- This work describes the analysis of the brominated flame retardant, tetrabromobisphenol-A (TBBPA), from dust sampled on surfaces of consumer electronics

  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. Ionic liquid-based dispersive microextraction of nitro toluenes in water samples

    International Nuclear Information System (INIS)

    Berton, Paula; Regmi, Bishnu P.; Spivak, David A.; Warner, Isiah M.

    2014-01-01

    We describe a method for dispersive liquid-liquid microextraction of nitrotoluene-based compounds. This method is based on use of the room temperature ionic liquid (RTIL) 1-hexyl-4-methylpyridinium bis(trifluoromethylsulfonyl)imide as the accepting phase, and is shown to work well for extraction of 4-nitrotoluene, 2,4-dinitrotoluene, and 2,4,6-trinitrotoluene. Separation and subsequent detection of analytes were accomplished via HPLC with UV detection. Several parameters that influence the efficiency of the extraction were optimized using experimental design. In this regard, a Plackett–Burman design was used for initial screening, followed by a central composite design to further optimize the influencing variables. For a 5-mL water sample, the optimized IL-DLLME procedure requires 26 mg of the RTIL as extraction solvent and 680 μL of methanol as the dispersant. Under optimum conditions, limits of detection (LODs) are lower than 1.05 μg L −1 . Relative standard deviations for 6 replicate determinations at a 4 μg L −1 analyte level are <4.3 % (calculated using peak areas). Correlation coefficients of >0.998 were achieved. This method was successfully applied to extraction and determination of nitrotoluene-based compounds in spiked tap and lake water samples. (author)

  7. Overcoming the challenges of conventional dispersive liquid-liquid microextraction: analysis of THMs in chlorinated swimming pools.

    Science.gov (United States)

    Faraji, Hakim; Helalizadeh, Masoumeh; Kordi, Mohammad Reza

    2018-01-01

    A rapid, simple, and sensitive approach to the analysis of trihalomethanes (THMs) in swimming pool water samples has been developed. The main goal of this study was to overcome or to improve the shortcomings of conventional dispersive liquid-liquid microextraction (DLLME) and to maximize the realization of green analytical chemistry principles. The method involves a simple vortex-assisted microextraction step, in the absence of the dispersive solvent, followed by salting-out effect for the elimination of the centrifugation step. A bell-shaped device and a solidifiable solvent were used to simplify the extraction solvent collection after phase separation. Optimization of the independent variables was performed by using chemometric methods in three steps. The method was statistically validated based on authentic guidance documents. The completion time for extraction was less than 8 min, and the limits of detection were in the range between 4 and 72 ng L -1 . Using this method, good linearity and precision were achieved. The results of THMs determination in different real samples showed that in some cases the concentration of total THMs was more than threshold values of THMs determined by accredited healthcare organizations. This method indicated satisfactory analytical figures of merit. Graphical Abstract A novel green microextraction technique for overcoming the challenges of conventional DLLME. The proposed procedure complies with the principles of green/sustainable analytical chemistry, comprising decreasing the sample size, making easy automation of the process, reducing organic waste, diminishing energy consumption, replacing toxic reagents with safer reagents, and enhancing operator safety.

  8. 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.

  9. Applied optics. Multiwavelength achromatic metasurfaces by dispersive phase compensation.

    Science.gov (United States)

    Aieta, Francesco; Kats, Mikhail A; Genevet, Patrice; Capasso, Federico

    2015-03-20

    The replacement of bulk refractive optical elements with diffractive planar components enables the miniaturization of optical systems. However, diffractive optics suffers from large chromatic aberrations due to the dispersion of the phase accumulated by light during propagation. We show that this limitation can be overcome with an engineered wavelength-dependent phase shift imparted by a metasurface, and we demonstrate a design that deflects three wavelengths by the same angle. A planar lens without chromatic aberrations at three wavelengths is also presented. Our designs are based on low-loss dielectric resonators, which introduce a dense spectrum of optical modes to enable dispersive phase compensation. The suppression of chromatic aberrations in metasurface-based planar photonics will find applications in lightweight collimators for displays, as well as chromatically corrected imaging systems. Copyright © 2015, American Association for the Advancement of Science.

  10. Coordinate, Momentum and Dispersion operators in Phase space representation

    International Nuclear Information System (INIS)

    Rakotoson, H.; Raoelina Andriambololona; Ranaivoson, R.T.R.; Raboanary, R.

    2017-07-01

    The aim of this paper is to present a study on the representations of coordinate, momentum and dispersion operators in the framework of a phase space representation of quantum mechanics that we have introduced and studied in previous works. We begin in the introduction section with a recall about the concept of representation of operators on wave function spaces. Then, we show that in the case of the phase space representation the coordinate and momentum operators can be represented either with differential operators or with matrices. The explicit expressions of both the differential operators and matrices representations are established. Multidimensional generalization of the obtained results are performed and phase space representation of dispersion operators are given.

  11. Optical bistability and limiting in polymer dispersed liquid crystal

    Energy Technology Data Exchange (ETDEWEB)

    Yshino, K.; Tagawa, A.; Sadohara, Y.; Ozaki, M. (Osaka University, Osaka (Japan). Faculty of Engineering); Munezawa, T. (Ajinomoto Co. Inc., Tokyo (Japan)); Nomura, Y. (Takiron Co. Ltd., Osaka (Japan))

    1991-04-15

    The linear electro-optical effect of polymer dispersed liquid crystal (PDLC) and the nonlinear optical response of electrically feedbacked PDLC were studied. Electro-optical limiting and bistability were observed in PDLCs with negative and positive feedback, respectively. In the PDLC film with positive feedback gain, an optical hysteresis loop shifted toward a high intensity region with decreasing magnitude of the feedback gain. The switching between high and low transmission states in an optical bistable region was realized by controlling incident light, and the on-off switching by superimposing light pulse on incident light for an extremely short period (several hundreds {mu}s). As the light pulse was strong, the minimum pulse width required for switching was as short as 500 {mu}s or less. The on-off switching was also realized by shutting out the incident light for a period equivalent to the pulse width. Slower response times of the PDLC film required longer minimum pulse widths. 12 refs., 11 figs.

  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. Turbulence modification due to bubbles and particles in dispersed two-phase upflows in a vertical pipe

    International Nuclear Information System (INIS)

    Hosokawa, Shigeo; Tomiyama, Akio

    1999-01-01

    One of the key issues in two-phase turbulence modeling is the turbulence modification due to the momentum exchange between the dispersed and continuous phases. As for the gas-liquid two-phase flows in vertical pipes, Serizawa and Kataoka carried out detailed measurement of turbulence intensity and detected the turbulence modification. Gore and Crowe pointed out that the modification is well correlated with the ratio of a particle diameter to a turbulence length scale (d/l t ). However the modification may depend on not only the length scales but also the eddy viscosities of shear-induced and particle-induced turbulence. Hosokawa et al. proposed the ratio φ of the eddy viscosity induced by a dispersed phase to the shear-induced eddy viscosity and confirmed that measured turbulence modification was well correlated with φ for a gas-solid two-phase flow. In this study, we examine whether or not φ is also applicable to gas-liquid and solid-liquid two-phase dispersed upflows in vertical pipes. Using the eddy viscosity ratio instead of d/l t , we could obtain much better correlation. The critical point at which no modification occurred was close to φ = 1, irrespective of a type of a two-phase dispersed flow. Consequently, we could confirm that the eddy viscosity ratio is a more appropriate parameter for correlating the turbulent modification than the conventional critical parameter d/l t . (author)

  14. Transport of Liquid Phase Organic Solutes in Liquid Crystalline Membranes

    OpenAIRE

    Han, Sangil

    2010-01-01

    Porous cellulose nitrate membranes were impregnated with 8CB and PCH5 LCs (liquid crystals) and separations of solutes dissolved in aqueous phases were performed while monitoring solute concentration via UV-VIS spectrometry. The diffusing organic solutes, which consist of one aromatic ring and various functional groups, were selected to exclude molecular size effects on the diffusion and sorption. We studied the effects on solute transport of solute intra-molecular hydrogen bonding and so...

  15. Investigation of a polymer-dispersed liquid crystal system by NMR diffusometry and relaxometry

    Energy Technology Data Exchange (ETDEWEB)

    Tang, Mingxue

    2013-02-26

    Polymer-dispersed liquid crystals (PDLCs) are polymer composites containing a dispersion of liquid crystal droplets in polymer networks. PDLCs have attracted much attention due to their unique properties and potential usage. The properties of PDLCs depend on the degree of phase separation and the size of liquid crystal droplets. To investigate the structure will help us to better understand and optimize PDLCs.The main aim of this PhD thesis was to investigate PDLCs by NMR techniques. Diffusion constants and spin-lattice relaxation times in the laboratory (T{sub 1}) and rotating frame (T{sub 1{rho}}) were measured for PDLCs as well as precursor mixtures based on the trifunctional monomer trimethylolpropane triacrylate (TMPTA) and the commercial nematic mixture E7. The variation of the main dipolar splitting of {sup 1}H spectra with increasing temperature was analyzed to obtain the nematic-to-isotropic phase transition temperature and the nematic order parameter of E7 and, for comparison, the nematic liquid crystal 5CB.Diffusion constants in TMPTA/E7 mixtures, measured by pulsed-field gradient NMR, increase for both E7 and TMPTA as the mass fraction of E7 increases, due to the lower viscosity of E7. E7 in the PDLC diffuses more slowly than in the bulk because of the hindrance by the polymer matrix. T{sub 1} and T{sub 1{rho}} relaxation times in the liquid or liquid-crystalline phases of TMPTA and bulk E7 are higher than in the PDLC and the pure polymer, due to the lower mobility in the polymer samples. T{sub 1{rho}} in the PDLC is even shorter than in the pure polymer, indicating an anti-softening effect caused by E7 molecules. In bulk E7, the well-ordered rod-like molecules exhibit a unique H-C dipolar coupling, which leads to oscillations in the cross-polarization curve. However, in the PDLC, the anchoring effect at the boundary between the polymer and LC droplets disturbs the molecular order resulting in a smooth cross polarization curve.

  16. Investigation of a polymer-dispersed liquid crystal system by NMR diffusometry and relaxometry

    International Nuclear Information System (INIS)

    Tang, Mingxue

    2013-01-01

    Polymer-dispersed liquid crystals (PDLCs) are polymer composites containing a dispersion of liquid crystal droplets in polymer networks. PDLCs have attracted much attention due to their unique properties and potential usage. The properties of PDLCs depend on the degree of phase separation and the size of liquid crystal droplets. To investigate the structure will help us to better understand and optimize PDLCs.The main aim of this PhD thesis was to investigate PDLCs by NMR techniques. Diffusion constants and spin-lattice relaxation times in the laboratory (T 1 ) and rotating frame (T 1ρ ) were measured for PDLCs as well as precursor mixtures based on the trifunctional monomer trimethylolpropane triacrylate (TMPTA) and the commercial nematic mixture E7. The variation of the main dipolar splitting of 1 H spectra with increasing temperature was analyzed to obtain the nematic-to-isotropic phase transition temperature and the nematic order parameter of E7 and, for comparison, the nematic liquid crystal 5CB.Diffusion constants in TMPTA/E7 mixtures, measured by pulsed-field gradient NMR, increase for both E7 and TMPTA as the mass fraction of E7 increases, due to the lower viscosity of E7. E7 in the PDLC diffuses more slowly than in the bulk because of the hindrance by the polymer matrix. T 1 and T 1ρ relaxation times in the liquid or liquid-crystalline phases of TMPTA and bulk E7 are higher than in the PDLC and the pure polymer, due to the lower mobility in the polymer samples. T 1ρ in the PDLC is even shorter than in the pure polymer, indicating an anti-softening effect caused by E7 molecules. In bulk E7, the well-ordered rod-like molecules exhibit a unique H-C dipolar coupling, which leads to oscillations in the cross-polarization curve. However, in the PDLC, the anchoring effect at the boundary between the polymer and LC droplets disturbs the molecular order resulting in a smooth cross polarization curve.

  17. Automated dispersive liquid-liquid microextraction coupled to high performance liquid chromatography - cold vapour atomic fluorescence spectroscopy for the determination of mercury species in natural water samples.

    Science.gov (United States)

    Liu, Yao-Min; Zhang, Feng-Ping; Jiao, Bao-Yu; Rao, Jin-Yu; Leng, Geng

    2017-04-14

    An automated, home-constructed, and low cost dispersive liquid-liquid microextraction (DLLME) device that directly coupled to a high performance liquid chromatography (HPLC) - cold vapour atomic fluorescence spectroscopy (CVAFS) system was designed and developed for the determination of trace concentrations of methylmercury (MeHg + ), ethylmercury (EtHg + ) and inorganic mercury (Hg 2+ ) in natural waters. With a simple, miniaturized and efficient automated DLLME system, nanogram amounts of these mercury species were extracted from natural water samples and injected into a hyphenated HPLC-CVAFS for quantification. The complete analytical procedure, including chelation, extraction, phase separation, collection and injection of the extracts, as well as HPLC-CVAFS quantification, was automated. Key parameters, such as the type and volume of the chelation, extraction and dispersive solvent, aspiration speed, sample pH, salt effect and matrix effect, were thoroughly investigated. Under the optimum conditions, linear range was 10-1200ngL -1 for EtHg + and 5-450ngL -1 for MeHg + and Hg 2+ . Limits of detection were 3.0ngL -1 for EtHg + and 1.5ngL -1 for MeHg + and Hg 2+ . Reproducibility and recoveries were assessed by spiking three natural water samples with different Hg concentrations, giving recoveries from 88.4-96.1%, and relative standard deviations <5.1%. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Solid-phase extraction versus matrix solid-phase dispersion: Application to white grapes.

    Science.gov (United States)

    Dopico-García, M S; Valentão, P; Jagodziñska, A; Klepczyñska, J; Guerra, L; Andrade, P B; Seabra, R M

    2007-11-15

    The use of matrix solid-phase dispersion (MSPD) was tested to, separately, extract phenolic compounds and organic acids from white grapes. This method was compared with a more conventional analytical method previously developed that combines solid liquid extraction (SL) to simultaneously extract phenolic compounds and organic acids followed by a solid-phase extraction (SPE) to separate the two types of compounds. Although the results were qualitatively similar for both techniques, the levels of extracted compounds were in general quite lower on using MSPD, especially for organic acids. Therefore, SL-SPE method was preferred to analyse white "Vinho Verde" grapes. Twenty samples of 10 different varieties (Alvarinho, Avesso, Asal-Branco, Batoca, Douradinha, Esganoso de Castelo Paiva, Loureiro, Pedernã, Rabigato and Trajadura) from four different locations in Minho (Portugal) were analysed in order to study the effects of variety and origin on the profile of the above mentioned compounds. Principal component analysis (PCA) was applied separately to establish the main sources of variability present in the data sets for phenolic compounds, organic acids and for the global data. PCA of phenolic compounds accounted for the highest variability (77.9%) with two PCs, enabling characterization of the varieties of samples according to their higher content in flavonol derivatives or epicatechin. Additionally, a strong effect of sample origin was observed. Stepwise linear discriminant analysis (SLDA) was used for differentiation of grapes according to the origin and variety, resulting in a correct classification of 100 and 70%, respectively.

  19. Ionic liquid stationary phases for gas chromatography.

    Science.gov (United States)

    Poole, Colin F; Poole, Salwa K

    2011-04-01

    This article provides a summary of the development of ionic liquids as stationary phases for gas chromatography beginning with early work on packed columns that established details of the retention mechanism and established working methods to characterize selectivity differences compared with molecular stationary phases through the modern development of multi-centered cation and cross-linked ionic liquids for high-temperature applications in capillary gas chromatography. Since there are many reviews on ionic liquids dealing with all aspects of their chemical and physical properties, the emphasis in this article is placed on the role of gas chromatography played in the design of ionic liquids of low melting point, high thermal stability, high viscosity, and variable selectivity for separations. Ionic liquids provide unprecedented opportunities for extending the selectivity range and temperature-operating range of columns for gas chromatography, an area of separation science that has otherwise been almost stagnant for over a decade. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. A highly selective and sensitive ultrasonic assisted dispersive liquid phase microextraction based on deep eutectic solvent for determination of cadmium in food and water samples prior to electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Zounr, Rizwan Ali; Tuzen, Mustafa; Deligonul, Nihal; Khuhawar, Muhammad Yar

    2018-07-01

    A simple, fast, green, sensitive and selective ultrasonic assisted deep eutectic solvent liquid-phase microextraction technique was used for preconcentration and extraction of cadmium (Cd) in water and food samples by electrothermal atomic absorption spectrometry (ETAAS). In this technique, a synthesized reagent (Z)-N-(3,5-diphenyl-1H-pyrrol-2-yl)-3,5-diphenyl-2H-pyrrol-2-imine (Azo) was used as a complexing agent for Cd. The main factors effecting the pre-concentration and extraction of Cd such as effect of pH, type and composition of deep eutectic solvent (DES), volume of DES, volume of complexing agent, volume of tetrahydrofuran (THF) and ultrasonication time have been examined in detail. At optimum conditions the value of pH and molar ratio of DES were found to be 6.0 and 1:4 (ChCl:Ph), respectively. The detection limit (LOD), limit of quantification (LOQ), relative standard deviation (RSD) and preconcentration factor (PF) were observed as 0.023 ng L -1 , 0.161 ng L -1 , 3.1% and 100, correspondingly. Validation of the developed technique was observed by extraction of Cd in certified reference materials (CRMs) and observed results were successfully compared with certified values. The developed procedure was practiced to various food, beverage and water samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

  1. Dispersive liquid-liquid microextraction of copper ions as neocuproine complex in environmental aqueous samples.

    Science.gov (United States)

    Shariati, Shahab; Golshekan, Mostafa

    2011-06-01

    In the present study, a simple and efficient extraction method based on dispersive liquid-liquid microextraction prior to UV-Vis spectrophotometry was developed for the preconcentration and determination of copper ions in environmental samples. Briefly, cupric ions (Cu II) were reduced to cuprous (Cu I) with addition of hydroxyl amine hydrochloride and formed hydrophobic chelates with neocuproine. Then, a proper mixture of acetonitrile (as dispersive solvent) and choloroform (as extraction solvent) was rapidly injected into the solution and a cloudy solution was formed. After centrifuging, choloroform was sedimented at the bottom of a conical tube and diluted with 100 µL of methanol for further UV-Vis spectrophotometry measurement. An orthogonal array design (OAD) was employed to study the effects of different parameters on the extraction efficiency. Under the optimum experimental conditions, a preconcentration factor up to 63.6 was achieved for extraction from 5.0 mL of sample solution. The limit of detection (LOD) based on S/N = 3 was 0.33 µg L-1 and the calibration curve was linear in the range of 1-200 µg L-1 with reasonable linearity (r2 > 0.997). Finally, the accuracy of the proposed method was successfully evaluated by determination of trace amounts of copper ions in different water samples and satisfactory results were obtained.

  2. Determination of 24 personal care products in fish bile using hybrid solvent precipitation and dispersive solid phase extraction cleanup with ultrahigh performance liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Yao, Li; Lv, Yin-Zhi; Zhang, Li-Juan; Liu, Wang-Rong; Zhao, Jian-Liang; Liu, You-Sheng; Zhang, Qian-Qian; Ying, Guang-Guo

    2018-05-25

    Personal care products (PCPs) are ubiquitous in aquatic environments owing to the continuous discharge of domestic wastewater from highly urbanized regions. These PCPs can be adsorbed by fish and thereafter usually enter the bile of the fish through biliary excretion. In this study, a sensitive method based on a combination of hybrid solvent precipitation and dispersive solid phase extraction (d-SPE) purification was developed to simultaneously extract and detect 24 PCPs, namely, 16 biocides, 4 synthetic musks, and 4 benzotriazoles, from fish bile. Hybrid precipitation on solid phase extraction (SPE) tubes was applied to remove phospholipids and proteins, and a d-SPE procedure was used for further purification. The extraction solvents for the hybrid precipitation/SPE tubes and d-SPE materials were optimized. The method performance for bile samples both with and without enzyme hydrolysis using β-glucuronidase/aryl-sulfatase were validated. The 24 PCPs in fish bile were spiked with standard concentrations of 10 ng/mL, 20 ng/mL, 100 ng/mL, and 200 ng/mL to evaluate recoveries, which ranged from 70 to 120% for 16, 16, 22, and 21 analytes with hydrolysis, respectively, and 70-120% for 14, 15, 23, and 23 analytes without hydrolysis, respectively. The quantification limits for target PCPs were in the range 0.26-7.38 ng/mL [excluding musk xylene (MX) and musk ketone (MK)] and 0.20-9.48 ng/mL (excluding MX and MK) for bile samples with and without enzyme hydrolysis, respectively. After enzyme hydrolysis, 12 PCPs were detected in bile from fish collected from the Yangtze River, with a maximum detected concentration of 460 ng/mL, for triclosan (TCS). The hydrolysis reaction indicated that high percentages of glucuronide and sulfate metabolites for some PCPs, i.e. four parabens and TCS, existed in the bile. Copyright © 2018 Elsevier B.V. All rights reserved.

  3. Exfoliation in ecstasy: liquid crystal formation and concentration-dependent debundling observed for single-wall nanotubes dispersed in the liquid drug {gamma}-butyrolactone

    Energy Technology Data Exchange (ETDEWEB)

    Bergin, Shane D [School of Physics, Trinity College Dublin, University of Dublin, Dublin 2 (Ireland); Nicolosi, Valeria [School of Physics, Trinity College Dublin, University of Dublin, Dublin 2 (Ireland); Giordani, Silvia [School of Physics, Trinity College Dublin, University of Dublin, Dublin 2 (Ireland); Gromard, Antoine de [School of Physics, Trinity College Dublin, University of Dublin, Dublin 2 (Ireland); Carpenter, Leslie [School of Physics, Trinity College Dublin, University of Dublin, Dublin 2 (Ireland); Blau, Werner J [School of Physics, Trinity College Dublin, University of Dublin, Dublin 2 (Ireland); Coleman, Jonathan N [School of Physics, Trinity College Dublin, University of Dublin, Dublin 2 (Ireland)

    2007-11-14

    Large-scale debundling of single-walled nanotubes has been demonstrated by dilution of nanotube dispersions in the solvent {gamma}-butyrolactone. This liquid, sometimes referred to as 'liquid ecstasy', is well known for its narcotic properties. At high concentrations the dispersions form an anisotropic, liquid crystalline phase which can be removed by mild centrifugation. At lower concentrations an isotropic phase is observed with a biphasic region at intermediate concentrations. By measuring the absorbance before and after centrifugation, as a function of concentration, the relative anisotropic and isotropic nanotube concentrations can be monitored. The upper limit of the pure isotropic phase was C{sub NT}{approx}0.004 mg ml{sup -1}, suggesting that this can be considered the nanotube dispersion limit in {gamma}-butyrolactone. After centrifugation, the dispersions are stable against sedimentation and further aggregation for a period of 8 weeks at least. Atomic-force-microscopy studies on films deposited from the isotropic phase reveal that the bundle diameter distribution decreases dramatically as concentration is decreased. Detailed data analysis suggests the presence of an equilibrium bundle number density. A population of individual nanotubes is always observed which increases with decreasing concentration until almost 40% of all dispersed objects are individual nanotubes at a concentration of 6 x 10{sup -4} mg ml{sup -1}. The number density of individual nanotubes peaks at a concentration of {approx}6 x 10{sup -3} mg ml{sup -1} where almost 10% of the nanotubes by mass are individualized.

  4. 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...

  5. Cooling and spreading of corium during its fall into water in a pressurised water nuclear plant severe accident: description of mechanical and thermal interactions in a three phase flow during spreading of cold or heated spheres in a liquid pool; Refroidissement et dispersion du corium lors de sa chute dans l'eau pendant un accident severe de reacteur nucleaire a eau pressurisee: description des interactions mecaniques et thermiques en ecoulement triphasique lors de la dispersion de spheres solides froides ou chaudes dans un bain liquide

    Energy Technology Data Exchange (ETDEWEB)

    Duplat, F

    1998-10-26

    In the frame of nuclear safety studies about corium and water interactions, we address spreading and cooling stage of corium fragments in a liquid pool. Considering the complexity of encountered flow regimes and mechanical and thermal interactions coupling, modelling validation is based on a thermal-hydraulic computer code (MC3D). A bibliographical study shows that classical modelling of three phase flow is based on constitutive laws already established in the case of two phase flow. The present study states a complete analysis of BILLEAU experiments and defines a characterisation method for a sphere cloud. Some complementary QUEOS experiments are also described. Mechanical interaction terms such as added mass, lift and turbulent dispersion have been presented in the frame of a three phase flow and their influence has been tested in numerical simulations of BILLEAU tests. The effect of film vapour overheat, as well as particle diameter evolution have been studied. Moreover a radiative heat transfer modelling developed in Karlsruhe research centre (FZK) has been analysed and completed. Numerical simulations achieved for this study show that mechanical and thermal behaviour of the system are actually coupled. Taking into account lift and turbulent dispersion terms as well as heat transfer modifications all wed better results. This study also presents some considerations about flow regimes identification as a preliminary for studies about numerical diffusion that was already estimated in the present state of the computer code MC3D. (author)

  6. 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.

  7. 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 = ...

  8. (Liquid + liquid) phase behavior for systems containing (aromatic + TBA + methylcyclohexane)

    International Nuclear Information System (INIS)

    Ghanadzadeh, H.; Ghanadzadeh, A.

    2004-01-01

    The determination region of solubility of TBA (tert-butanol) with representative compounds of the gasoline was investigated experimentally at temperature of 298.2 K. Type 1 (liquid + liquid) phase diagrams were obtained for (methylcyclohexane + TBA + aromatic compounds). These results were correlated simultaneously by the UNIQUAC model. The values of the interaction parameters between each pair of components in the systems were obtained for the UNIQUAC model using the experimental result. The root mean square deviation (RMSD) between the observed and calculated mole percents was 1.88 for (methylcyclohexane + TBA + benzene), 2.45 for (methylcyclohexane + TBA + toluene) and 2.86 for (methylcyclohexane + TBA + ethylbenzene). The mutual solubility of methylcyclohexane and aromatic compounds (e.g., benzene toluene and ethylbenzene (BTE)) was also investigated by the addition of TBA at temperature of 298.2 K

  9. Multimycotoxin LC-MS/MS Analysis in Tea Beverages after Dispersive Liquid-Liquid Microextraction (DLLME).

    Science.gov (United States)

    Pallarés, Noelia; Font, Guillermina; Mañes, Jordi; Ferrer, Emilia

    2017-11-29

    The aim of the present study was to develop a multimycotoxin liquid chromatography tandem mass spectrometry (LC-MS/MS) method with a dispersive liquid-liquid microextraction procedure (DLLME) for the analysis of AFs, 3aDON, 15aDON, NIV, HT-2, T-2, ZEA, OTA, ENNs, and BEA in tea beverages and to evaluate their mycotoxin contents. The proposed method was characterized in terms of linearity, limits of detection (LODs), limits of quantification (LOQs), recoveries, repeatability (intraday precision), reproducibility (interday precision), and matrix effects to check suitability. The results show LODs in the range of 0.05-10 μg/L, LOQs in the range of 0.2-33 μg/L, and recoveries in the range of 65-127% (RSD tea, red tea, green tea, and green mint tea. The results show that, of the analyzed mycotoxins, AFB2, AFG2, 15aDON, AFG1, and ENB were detected in the samples. AFB2 (14.4-32.2 μg/L) and 15aDON (60.5-61 μg/L) presented the highest levels. Green mint tea contained the highest concentration of mycotoxins. The risk assessment study shows that the population is not much exposed to mycotoxins through the consumption of tea beverages.

  10. 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.

  11. Crystal-liquid-gas phase transitions and thermodynamic similarity

    CERN Document Server

    Skripov, Vladimir P; Schmelzer, Jurn W P

    2006-01-01

    Professor Skripov obtained worldwide recognition with his monograph ""Metastable liquids"", published in English by Wiley & Sons. Based upon this work and another monograph published only in Russia, this book investigates the behavior of melting line and the properties of the coexisting crystal and liquid phase of simple substances across a wide range of pressures, including metastable states of the coexisting phases. The authors derive new relations for the thermodynamic similarity for liquid-vapour phase transition, as well as describing solid-liquid, liquid-vapor and liquid-liquid phase tra

  12. Partitioning of fresh crude oil between floating, dispersed and sediment phases: Effect of exposure order to dispersant and granular materials.

    Science.gov (United States)

    Boglaienko, Daria; Tansel, Berrin

    2016-06-15

    When three or more high and low energy substrates are mixed, wetting order can significantly affect the behavior of the mixture. We analyzed the phase distribution of fresh floating Louisiana crude oil into dispersed, settled and floating phases depending on the exposure sequence to Corexit 9500A (dispersant) and granular materials. In the experiments artificial sea water at salinity 34‰ was used. Limestone (2.00-0.300 mm) and quartz sand (0.300-0.075 mm) were used as the natural granular materials. Dispersant Corexit 9500A increased the amount of dispersed oil up to 33.76 ± 7.04%. Addition of granular materials after the dispersant increased dispersion of oil to 47.96 ± 1.96%. When solid particles were applied on the floating oil before the dispersant, oil was captured as oil-particle aggregates and removed from the floating layer. However, dispersant addition led to partial release of the captured oil, removing it from the aggregated form to the dispersed and floating phases. There was no visible oil aggregation with the granular materials when quartz or limestone was at the bottom of the flask before the addition of oil and dispersant. The results show that granular materials can be effective when applied from the surface for aggregating or dispersing oil. However, the granular materials in the sediments are not effective neither for aggregating nor dispersing floating oil. Copyright © 2016 Elsevier Ltd. All rights reserved.

  13. 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.

  14. Unconventional phase transitions in liquid crystals

    Science.gov (United States)

    Kats, E. I.

    2017-12-01

    According to classical textbooks on thermodynamics or statistical physics, there are only two types of phase transitions: continuous, or second-order, in which the latent heat L is zero, and first-order, in which L ≠ 0. Present-day textbooks and monographs also mention another, stand-alone type—the Berezinskii-Kosterlitz-Thouless transition, which exists only in two dimensions and shares some features with first- and second-order phase transitions. We discuss examples of non-conventional thermodynamic behavior (i.e., which is inconsistent with the theoretical phase transition paradigm now universally accepted). For phase transitions in smectic liquid crystals, mechanisms for nonconventional behavior are proposed and the predictions they imply are examined.

  15. Determination of spirocyclic tetronic/tetramic acid derivatives and neonicotinoid insecticides in fruits and vegetables by liquid chromatography and mass spectrometry after dispersive liquid-liquid microextraction.

    Science.gov (United States)

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

    2016-07-01

    Dispersive liquid-liquid microextraction was used to preconcentrate three spirocyclic tetronic/tetramic acid derivatives (spirotetramat, spiromesifen and spirodiclofen) and five neonicotinoid (thiamethoxam, chlotianidin, imidacloprid, acetamiprid and thiacloprid) insecticides previously extracted from fruit and vegetable matrices with acetonitrile. The organic enriched phase was evaporated, reconstituted in 25μL acetonitrile and analyzed by reversed-phase liquid chromatography with tandem mass spectrometry using a triple quadrupole in selected reaction monitoring mode. Enrichment factors in the 15-100 range were obtained. A matrix effect was observed, the detection limits varying between 0.025 and 0.5ngg(-1), depending on the compound and the sample matrix. The developed method was applied to the analysis of 25 samples corresponding to five different fruit and vegetable matrices. Only thiamethoxam was detected in a lemon sample at a concentration close to the quantification limit, and spiromesifen and spirotetramat at concentrations between 11.6 and 54.5ngg(-1). Copyright © 2016 Elsevier Ltd. All rights reserved.

  16. Phase transitions in liquids with directed intermolecular bonding

    OpenAIRE

    Son, L.; Ryltcev, R.

    2005-01-01

    Liquids with quasi - chemical bonding between molecules are described in terms of vertex model. It is shown that this bonding results in liquid - liquid phase transition, which occurs between phases with different mean density of intermolecular bonds. The transition may be suggested to be a universal phenomena for those liquids.

  17. Magnetic liquid metal two-phase flow research. Phase 1. Final report

    International Nuclear Information System (INIS)

    Graves, R.D.

    1983-04-01

    The Phase I research demonstrates the feasibility of the magnetic liquid metal (MLM) two-phase flow concept. A dispersion analysis is presented based on a complete set of two-phase-flow equations augmented to include stresses due to magnetic polarization of the fluid. The analysis shows that the stability of the MLM two-phase flow is determined by the magnetic Mach number, the slip ratio, geometry of the flow relative to the applied magnetic field, and by the voidage dependence of the interfacial forces. Results of a set of experiments concerned with magnetic effects on the dynamics of single bubble motion in an aqueous-based, viscous, conducting magnetic fluid are presented. Predictions in the theoretical literature are qualitatively verified using a bench-top experimental apparatus. In particular, applied magnetic fields are seen to lead to reduced bubble size at fixed generating orifice pressure

  18. 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.

  19. Dispersion strengthened ferritic alloy for use in liquid-metal fast breeder reactors (LMFBRS)

    International Nuclear Information System (INIS)

    Fischer, J.J.

    1978-01-01

    A dispersion-strengthened ferritic alloy is provided which has high-temperature strength and is readily fabricable at ambient temperatures, and which is useful as structural elements of liquid-metal fast breeder reactors. 4 tables

  20. Thermodynamic phase behavior of API/polymer solid dispersions.

    Science.gov (United States)

    Prudic, Anke; Ji, Yuanhui; Sadowski, Gabriele

    2014-07-07

    To improve the bioavailability of poorly soluble active pharmaceutical ingredients (APIs), these materials are often integrated into a polymer matrix that acts as a carrier. The resulting mixture is called a solid dispersion. In this work, the phase behaviors of solid dispersions were investigated as a function of the API as well as of the type and molecular weight of the carrier polymer. Specifically, the solubility of artemisinin and indomethacin was measured in different poly(ethylene glycol)s (PEG 400, PEG 6000, and PEG 35000). The measured solubility data and the solubility of sulfonamides in poly(vinylpyrrolidone) (PVP) K10 and PEG 35000 were modeled using the perturbed-chain statistical associating fluid theory (PC-SAFT). The results show that PC-SAFT predictions are in a good accordance with the experimental data, and PC-SAFT can be used to predict the whole phase diagram of an API/polymer solid dispersion as a function of the kind of API and polymer and of the polymer's molecular weight. This remarkably simplifies the screening process for suitable API/polymer combinations.

  1. Liquid phase microextraction of pesticides: a review on current methods

    International Nuclear Information System (INIS)

    Farajzadeh, Mir Ali; Sorouraddin, Saeed Mohammad; Mogaddam, Mohammad Reza Afshar

    2014-01-01

    Liquid phase microextraction (LPME) enables analytes to be extracted with a few microliters of an organic solvent. LPME is a technique for sample preparation that is extremely simple, affordable and virtually a solvent-free. It can provide a high degree of selectivity and enrichment by eliminating carry-over between single runs. A variety of solvents are known for the extraction of the various analytes. These features have led to the development of techniques such as single drop microextraction, hollow fiber LPME, dispersive liquid-liquid microextraction, and others. LPME techniques have been applied to the analysis of pharmaceuticals, food, beverages, and pesticides. This review covers the history of LPME methods, and then gives a comprehensive collection of their application to the preconcentration and determination of pesticides in various matrices. Specific sections cover (a) sample treatment techniques in general, (b) single-drop microextraction, (c) extraction based on the use of ionic liquids, (d) solidified floating organic drop microextraction, and various other techniques. (author)

  2. Centrifugeless dispersive liquid-liquid microextraction based on salting-out phenomenon followed by high performance liquid chromatography for determination of Sudan dyes in different species.

    Science.gov (United States)

    Bazregar, Mohammad; Rajabi, Maryam; Yamini, Yadollah; Arghavani-Beydokhti, Somayeh; Asghari, Alireza

    2018-04-01

    In this work, a novel method, namely centrifugeless dispersive liquid-liquid microextraction, is introduced for the efficient extraction of banned Sudan dyes from foodstuff and water samples. In this method, which is based upon the salting-out phenomenon, in order to accelerate the extraction process, the extraction solvent (1-undecanol, 75 μL) is dispersed into the sample solution. Then the mixture is passed through a small column filled with 5 g sodium chloride, used as a separating reagent. In this condition, fine droplets of the extraction solvent are floated on the mixture, and the phase separation is simply achieved. This method is environmentally friendly, simple, and very fast, so that the overall extraction time is only 7 min. Under the optimal experimental conditions, the preconcentration factors in the range of 90-121 were obtained for the analytes. Also good linearities were obtained in the range of 2.5-1200 ng mL -1 (r 2  ≥ 0.993). Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. Evaluation of a novel metal-organic framework as an adsorbent for the extraction of multiclass pesticides from coconut palm (Cocos nucifera L.): An analytical approach using matrix solid-phase dispersion and liquid chromatography.

    Science.gov (United States)

    de Jesus, Jemmyson Romário; Wanderley, Kaline Amaral; Alves Júnior, Severino; Navickiene, Sandro

    2017-08-01

    We report the synthesis, characterization, and application of [Zn(1,4-benzenedicarboxylate)(H 2 O) 2 ] n , Zn(1,4-benzenedicarboxylate) 0.99 (NH 2 -1,4-benzenedicarboxylate) 0.01 (H 2 O) 2 ] n , [Zn(1,4-benzenedicarboxylate) 0.95 (NH 2 -1,4-benzenedicarboxylate) 0.05 (H 2 O) 2 ] n , and [Zn(1,4-benzenedicarboxylate) 0.9 (NH 2 -1,4-benzenedicarboxylate) 0.1 (H 2 O) 2 ] n as sorbents for the extraction of multiclass pesticides from coconut palm. Liquid chromatography with ultraviolet diode array detection was used as the analysis technique, and the experiments were performed at one fortification level (0.1 μg/g). The recoveries were 47-67, 51-70, 58-72, and 64-76% for [Zn(1,4-benzenedicarboxylate)(H 2 O) 2 ] n , Zn(1,4-benzenedicarboxylate) 0.99 (NH 2 -1,4-benzenedicarboxylate) 0.01 (H 2 O) 2 ] n , [Zn(1,4-benzenedicarboxylate) 0.95 (NH 2 -1,4-benzenedicarboxylate) 0.05 (H 2 O) 2 ] n , and [Zn(1,4-benzenelate) 0.95 (NH 2 -1,4-benzenedicarboxylate) 0.05 (H 2 O) 2 ] n , and [Zn(1,4-benzenedicarboxylate) 0.9 (NH 2 -1,4-benzenedicarboxylate) 0.1 (H 2 O) 2 ] n , respectively, with relative standard deviation ranging from 1 to 7% (n = 3). Detection and quantification limits were 0.01-0.05 and 0.05-0.2 μg/g, respectively, for the different pesticides studied. The method developed was linear over the range tested (0.01-10.0 μg/g) with r 2  > 0.9991. A direct comparison of [Zn(1,4-benzenedicarboxylate) 0.9 (NH 2 -1,4-benzenedicarboxylate) 0.1 (H 2 O) 2 ] n with the commercially available neutral alumina showed that [Zn(1,4-benzenedicarboxylate) 0.9 (NH 2 -1,4-benzenedicarboxylate) 0.1 (H 2 O) 2 ] n was a similar extracting phase for the pesticides investigated. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Growth of plant root cultures in liquid- and gas-dispersed reactor environments.

    Science.gov (United States)

    McKelvey, S A; Gehrig, J A; Hollar, K A; Curtis, W R

    1993-01-01

    The growth of Agrobacterium transformed "hairy root" cultures of Hyoscyamus muticus was examined in various liquid- and gas-dispersed bioreactor configurations. Reactor runs were replicated to provide statistical comparisons of nutrient availability on culture performance. Accumulated tissue mass in submerged air-sparged reactors was 31% of gyratory shake-flask controls. Experiments demonstrate that poor performance of sparged reactors is not due to bubble shear damage, carbon dioxide stripping, settling, or flotation of roots. Impaired oxygen transfer due to channeling and stagnation of the liquid phase are the apparent causes of poor growth. Roots grown on a medium-perfused inclined plane grew at 48% of gyratory controls. This demonstrates the ability of cultures to partially compensate for poor liquid distribution through vascular transport of nutrients. A reactor configuration in which the medium is sprayed over the roots and permitted to drain down through the root tissue was able to provide growth rates which are statistically indistinguishable (95% T-test) from gyratory shake-flask controls. In this type of spray/trickle-bed configuration, it is shown that distribution of the roots becomes a key factor in controlling the rate of growth. Implications of these results regarding design and scale-up of bioreactors to produce fine chemicals from root cultures are discussed.

  5. Polarization-Independent Electrically Tunable Holographic Polymer Dispersed Liquid Crystals Grating Doped with Chiral Molecules

    Directory of Open Access Journals (Sweden)

    Hui LI

    2017-08-01

    Full Text Available This study proposes a holographic grating made of polymer dispersed liquid crystal (PDLC, with a small amount of chiral molecules doped into PDLC material. The major advantage of this grating is that it is independent of light polarization. This characteristic was verified by applying the interference beam intensity of a He-Cd laser at 150 mW/cm2, with an incidence angle between the two interference beams of 24°, for an irradiation curing duration of 120 s. The observed periodic structure of the grating is consistent with the theoretical value. As chiral molecules are doped, nematic-LC experiences a phase-change in the grating. However, the electro-optical features are only slightly affected. This proposed grating has greatly potential in 3D imaging because of its polarization-independent feature.DOI: http://dx.doi.org/10.5755/j01.ms.23.2.16312

  6. Transflective multiplexing of holographic polymer dispersed liquid crystal using Si additives

    Directory of Open Access Journals (Sweden)

    2011-01-01

    Full Text Available Morphology, grating formation dynamics and electro-optical performance of transflective multiplexing with holographic polymer dispersed liquid crystal (HPDLC were investigated in the presence of silica nanoparticles (Aerosil R812 (RS and modified Aerosil 200 (MS and silicon monomer (vinyltrimethoxy silane (VTMS by using three coherent laser beams. The addition of Si additive significantly augmented the diffraction efficiencies of transmission and reflection gratings due to the enhanced phase separation with large LC channels. The film was driven only with Si additives which are enriched at the polymer-LC interfaces. As the additive content increased, driving voltage decreased to a minimum of 30 V at 2.0 wt% VTMS. It was found that the interface modification and large droplet size are crucial to operate the film. Among the three types of Si additive, VTMS showed the highest electro-optical performance due to its low viscosity and high reactivity.

  7. Determination of Trace Amounts of Lead with ETAAS After Single Drop Microextraction and Dispersive Liquid Liquid Microextraction Methods

    Directory of Open Access Journals (Sweden)

    Efeçınar M.

    2013-04-01

    Full Text Available Two liquid-phase microextraction procedures, single-drop microextraction (SDME and dispersive liquid–liquid microextraction (DLLME, have been developed for the determination of lead by electrothermal atomic absorption spectrometry (ETAAS. Both methods were based on the formation of lead iodide-Rhodamine B complex which is in phosphoric acid medium. In the presence of KI, anionic lead iodide was complexed with Rhodamine B as an ion-association complex. Several factors that may be affected on the SDME and DLLME methods were optimized. In the optimum experimental conditions, the limit of detection (3s and the enhancement factor were 0.008 μgL−1 and 152 for SDME and 0.0129 μgL−1 and 89 for DLLME respectively. The relative standard deviation (RSD for eight replicate determinations of 0.25 μgL−1 Pb was 4.6% for SDME and 0.5 μgL−1 Pb was 2.9% for DLLME. The developed methods were validated by the analysis of certified reference materials, and applied successfully to the determination of lead in several water and food samples.

  8. The new phases of liquid 3He

    International Nuclear Information System (INIS)

    Leggett, A.J.

    1976-01-01

    Comments are made on two new phases of liquid 3 He, referred to as 3 He-A and 3 He-B, discovered in the temperature region below 3 mk. It has been assumed that these new phases are anisotropic superfluids, and a general picture of them is presented, which has been successful in explaining at least qualitatively, many of the static, dynamic and transport properties of the new phases. Whilst the qualitative behaviour is in good agreement with theory there are, however, some quantitative discrepancies. In many cases these may be due to orientational and geometric effects not yet understood. One of the most fruitful areas for comparison of theory and experiment is the NMR behaviour and the dynamic nuclear magnetism. The anomalous behaviour observed arises because the nuclear dipole energy, although very small, can act coherently in the superfluid state. (U.K.)

  9. Dispersive liquid-liquid microextraction followed by flow injection-inductively coupled plasma mass spectrometry (FI-ICPMS) determination of 14 lanthanides from ground water

    International Nuclear Information System (INIS)

    Chandrasekaran, K.; Karunasagar, D.; Arunachalam, J.

    2011-01-01

    The aim of the present work was to develop a dispersive liquid-liquid microextraction (DLLME) method for the sensitive determination of REEs at a few parts per billion in groundwater by flow injection-inductively coupled plasma mass spectrometry (FI-ICPMS). In the developed method, methanol (500 μl) and chloroform (200μl) were used as the disperser and extractant respectively. The REEs were complexed with 4-(2-pyridylazo resorcinol) (PAR) at a pH of 7. Acetate ion was added as an auxiliary ligand for neutralization of the charge on the lanthanide-PAR complex. The disperser (MeOH) - extraction solvent (CHCl 3 ) mixture was rapidly injected using a disposable syringe, thereby forming a cloudy solution. The lanthanide-PAR complex was extracted into the fine droplets of the chloroform dispersed in the aqueous phase. The solution was centrifuged and the aqueous layer at the top was discarded. The REEs were back extracted from the chloroform layer with nitric acid for determination by ICPMS. Important parameters for complex formation and extraction, such as volume of extraction/disperser solvent, extraction time, pH and concentration of the chelating agent and the auxiliary ligand are being optimized using ICP-MS. The optimization is being carried out at 5 μg L -1 concentration level of REE in the initial water sample. Preliminary studies have shown an extraction recovery of 80-85% for all the 14 lanthanide elements and these will be presented

  10. 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.

  11. Hypercrosslinked particles for the extraction of sweeteners using dispersive solid-phase extraction from environmental samples.

    Science.gov (United States)

    Lakade, Sameer S; Zhou, Qing; Li, Aimin; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa M

    2018-04-01

    This work presents a new extraction material, namely, Q-100, based on hypercrosslinked magnetic particles, which was tested in dispersive solid-phase extraction for a group of sweeteners from environmental samples. The hypercrosslinked Q-100 magnetic particles had the advantage of suitable pore size distribution and high surface area, and showed good retention behavior toward sweeteners. Different dispersive solid-phase extraction parameters such as amount of magnetic particles or extraction time were optimized. Under optimum conditions, Q-100 showed suitable apparent recovery, ranging in the case of river water sample from 21 to 88% for all the sweeteners, except for alitame (12%). The validated method based on dispersive solid-phase extraction using Q-100 followed by liquid chromatography with tandem mass spectrometry provided good linearity and limits of quantification between 0.01 and 0.1 μg/L. The method was applied to analyze samples from river water and effluent wastewater, and four sweeteners (acesulfame, saccharin, cyclamate, and sucralose) were found in both types of sample. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. In-syringe dispersive liquid-liquid microextraction with liquid chromatographic determination of synthetic pyrethroids in surface water

    Directory of Open Access Journals (Sweden)

    Saeed S. Albaseer

    2012-03-01

    Full Text Available An indigenously fabricated in laboratory glass syringe was used for in-syringe dispersive liquid-liquid microextraction (is-DLLME and preconcentration of synthetic pyrethroids (SPs from surface waters suitable for their determination by high performance liquid chromatography. In contrast to classical DLLME, is-DLLME allows the use of lighter-than-water organic solvents and the analysis of environmental contaminants’ samples without prior filtration, which is of great importance due to the high affinity of pyrethroids to adsorb to solid particulates present in environmental samples. The effects of various parameters on the extraction efficiency were evaluated and optimized systemically using one-factor-at-a-time method (OFAT and statistically using full factorial design (24. Three SPs (viz.; cypermethrin, resmethrin and permethrin were analyzed. The method showed good accuracy with RSD% in the range of of 4.8–6.9%. The method detection limits of the three pesticides ranged from 0.14 to 0.16 ng mL-1. The proposed method was applied for the determination of synthetic pyrethroids in lake water

  13. Non-conventional solvents in liquid phase microextraction and aqueous biphasic systems.

    Science.gov (United States)

    An, Jiwoo; Trujillo-Rodríguez, María J; Pino, Verónica; Anderson, Jared L

    2017-06-02

    The development of rapid, convenient, and high throughput sample preparation approaches such as liquid phase microextraction techniques have been continuously developed over the last decade. More recently, significant attention has been given to the replacement of conventional organic solvents used in liquid phase microextraction techniques in order to reduce toxic waste and to improve selectivity and/or extraction efficiency. With these objectives, non-conventional solvents have been explored in liquid phase microextraction and aqueous biphasic systems. The utilized non-conventional solvents include ionic liquids, magnetic ionic liquids, and deep eutectic solvents. They have been widely used as extraction solvents or additives in various liquid phase microextraction modes including dispersive liquid-liquid microextraction, single-drop microextraction, hollow fiber-liquid phase microextraction, as well as in aqueous biphasic systems. This review provides an overview into the use of non-conventional solvents in these microextraction techniques in the past 5 years (2012-2016). Analytical applications of the techniques are also discussed. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Glass phase expelling during liquid phase sintering of YSZ

    International Nuclear Information System (INIS)

    Souza, Milton Ferreira de; Souza, Dulcina Pinatti Ferreira de

    1998-01-01

    Expelling of the liquid phase during sintering of Zr O 2 -6.5 mol % Y 2 O 3 - 0.5 mol % Pr 2 O 3 ceramic was observed as a result of grain coarsening. ZrO 2 - 7.0 mol % Y 2 O 3 samples, without Pr 2 O 3 addition, do not show this effect under the same sintering conditions. The expelling process is caused by surface tension forces and attracting van der Waals forces between the grains, coupled with the existence of two glass phases on the grain boundaries. The amount of expelled glass phase increases with grain growth, but saturates above 16 μm average grain size. (author)

  15. A dispersive liquid--liquid microextraction methodology for copper (II) in environmental samples prior to determination using microsample injection flame atomic absorption spectrometry.

    Science.gov (United States)

    Alothman, Zeid A; Habila, Mohamed; Yilmaz, Erkan; Soylak, Mustafa

    2013-01-01

    A simple, environmentally friendly, and efficient dispersive liquid-liquid microextraction method combined with microsample injection flame atomic absorption spectrometry was developed for the separation and preconcentration of Cu(II). 2-(5-Bromo-2-pyridylazo)-5-(diethylamino)phenol (5-Br-PADAP) was used to form a hydrophobic complex of Cu(II) ions in the aqueous phase before extraction. To extract the Cu(II)-5-Br-PADAP complex from the aqueous phase to the organic phase, 2.0 mL of acetone as a disperser solvent and 200 microL of chloroform as an extraction solvent were used. The influences of important analytical parameters, such as the pH, types and volumes of the extraction and disperser solvents, amount of chelating agent, sample volume, and matrix effects, on the microextraction procedure were evaluated and optimized. Using the optimal conditions, the LOD, LOQ, preconcentration factor, and RSD were determined to be 1.4 microg/L, 4.7 microg/L, 120, and 6.5%, respectively. The accuracy of the proposed method was investigated using standard addition/recovery tests. The analysis of certified reference materials produced satisfactory analytical results. The developed method was applied for the determination of Cu in real samples.

  16. Surface modification and characterization for dispersion stability of inorganic nanometer-scaled particles in liquid media

    International Nuclear Information System (INIS)

    Kamiya, Hidehiro; Iijima, Motoyuki

    2010-01-01

    Inorganic nanoparticles are indispensable for science and technology as materials, pigments and cosmetics products. Improving the dispersion stability of nanoparticles in various liquids is essential for those applications. In this review, we discuss why it is difficult to control the stability of nanoparticles in liquids. We also overview the role of surface interaction between nanoparticles in their dispersion and characterization, e.g. by colloid probe atomic force microscopy (CP-AFM). Two types of surface modification concepts, post-synthesis and in situ modification, were investigated in many previous studies. Here, we focus on post-synthesis modification using adsorption of various kinds of polymer dispersants and surfactants on the particle surface, as well as surface chemical reactions of silane coupling agents. We discuss CP-AFM as a technique to analyze the surface interaction between nanoparticles and the effect of surface modification on the nanoparticle dispersion in liquids. (topical review)

  17. Surface modification and characterization for dispersion stability of inorganic nanometer-scaled particles in liquid media

    Directory of Open Access Journals (Sweden)

    Hidehiro Kamiya and Motoyuki Iijima

    2010-01-01

    Full Text Available Inorganic nanoparticles are indispensable for science and technology as materials, pigments and cosmetics products. Improving the dispersion stability of nanoparticles in various liquids is essential for those applications. In this review, we discuss why it is difficult to control the stability of nanoparticles in liquids. We also overview the role of surface interaction between nanoparticles in their dispersion and characterization, e.g. by colloid probe atomic force microscopy (CP-AFM. Two types of surface modification concepts, post-synthesis and in situ modification, were investigated in many previous studies. Here, we focus on post-synthesis modification using adsorption of various kinds of polymer dispersants and surfactants on the particle surface, as well as surface chemical reactions of silane coupling agents. We discuss CP-AFM as a technique to analyze the surface interaction between nanoparticles and the effect of surface modification on the nanoparticle dispersion in liquids.

  18. Liquid phase hot atom chemistry: At crossroads

    International Nuclear Information System (INIS)

    Rack, E.P.; Veterans Administration Medical Center, Omaha, NE

    1981-01-01

    The state of current research in liquid phase hot atom chemistry is discussed. Four classes of experimental approaches are high-lighted. These include 1) primary physical data for (n,γ)-activated 128 I, (I.T.)-activated 130 I and effects on chemical reactivity; 2) the density-variation technique involving iodine reactions with saturated and unsaturated hydrocarbons; 3) stereochemistry experiments on chlorocarbon molecules with single and multiple chiral centers; and 4) experiments employing dilute aqueous solutions of halogenerated biomolecules in the ice state, exposed to neutron irradiation. (orig.) [de

  19. A phase space approach to wave propagation with dispersion.

    Science.gov (United States)

    Ben-Benjamin, Jonathan S; Cohen, Leon; Loughlin, Patrick J

    2015-08-01

    A phase space approximation method for linear dispersive wave propagation with arbitrary initial conditions is developed. The results expand on a previous approximation in terms of the Wigner distribution of a single mode. In contrast to this previously considered single-mode case, the approximation presented here is for the full wave and is obtained by a different approach. This solution requires one to obtain (i) the initial modal functions from the given initial wave, and (ii) the initial cross-Wigner distribution between different modal functions. The full wave is the sum of modal functions. The approximation is obtained for general linear wave equations by transforming the equations to phase space, and then solving in the new domain. It is shown that each modal function of the wave satisfies a Schrödinger-type equation where the equivalent "Hamiltonian" operator is the dispersion relation corresponding to the mode and where the wavenumber is replaced by the wavenumber operator. Application to the beam equation is considered to illustrate the approach.

  20. Modelling of Dispersed Gas-Liquid Flow using LBGK and LPT Approach

    Science.gov (United States)

    Agarwal, Alankar; Prakash, Akshay; Ravindra, B.

    2017-11-01

    The dynamics of gas bubbles play a significant, if not crucial, role in a large variety of industrial process that involves using reactors. Many of these processes are still not well understood in terms of optimal scale-up strategies.An accurate modeling of bubbles and bubble swarms become important for high fidelity bioreactor simulations. This study is a part of the development of robust bubble fluid interaction modules for simulation of industrial-scale reactors. The work presents the simulation of a single bubble rising in a quiescent water tank using current models presented in the literature for bubble-fluid interaction. In this multiphase benchmark problem, the continuous phase (water) is discretized using the Lattice Bhatnagar-Gross and Krook (LBGK) model of Lattice Boltzmann Method (LBM), while the dispersed gas phase (i.e. air-bubble) modeled with the Lagrangian particle tracking (LPT) approach. The cheap clipped fourth order polynomial function is used to model the interaction between two phases. The model is validated by comparing the simulation results for terminal velocity of a bubble at varying bubble diameter and the influence of bubble motion in liquid velocity with the theoretical and previously available experimental data. This work is supported by the ``Centre for Development of Advanced Computing (C-DAC), Pune'' by providing the advanced computational facility in PARAM Yuva-II.

  1. Annular dispersed flow analysis model by Lagrangian method and liquid film cell method

    International Nuclear Information System (INIS)

    Matsuura, K.; Kuchinishi, M.; Kataoka, I.; Serizawa, A.

    2003-01-01

    A new annular dispersed flow analysis model was developed. In this model, both droplet behavior and liquid film behavior were simultaneously analyzed. Droplet behavior in turbulent flow was analyzed by the Lagrangian method with refined stochastic model. On the other hand, liquid film behavior was simulated by the boundary condition of moving rough wall and liquid film cell model, which was used to estimate liquid film flow rate. The height of moving rough wall was estimated by disturbance wave height correlation. In each liquid film cell, liquid film flow rate was calculated by considering droplet deposition and entrainment flow rate. Droplet deposition flow rate was calculated by Lagrangian method and entrainment flow rate was calculated by entrainment correlation. For the verification of moving rough wall model, turbulent flow analysis results under the annular flow condition were compared with the experimental data. Agreement between analysis results and experimental results were fairly good. Furthermore annular dispersed flow experiments were analyzed, in order to verify droplet behavior model and the liquid film cell model. The experimental results of radial distribution of droplet mass flux were compared with analysis results. The agreement was good under low liquid flow rate condition and poor under high liquid flow rate condition. But by modifying entrainment rate correlation, the agreement become good even under high liquid flow rate. This means that basic analysis method of droplet and liquid film behavior was right. In future work, verification calculation should be carried out under different experimental condition and entrainment ratio correlation also should be corrected

  2. Optical phase conjugation for time-domain undoing of dispersive self-phase-modulation effects

    International Nuclear Information System (INIS)

    Fisher, R.A.; Suydam, B.R.; Yevick, D.

    1983-01-01

    We show that the temporal distortion and spectral broadening of a pulse generated by the combined effects of group-velocity dispersion and self-phase modulation is removed by reflection of a cw-pumped, broadband, unity-reflecting Kerr-like optical phase conjugator followed by retraversal of the nonlinear medium. We also examine numerically the effects of finite linear loss in the material, of nonunity conjugate reflectivity, and of finite conjugator thickness

  3. The removal of fatty acids from edible oil : removal of the dispersed phase of a water-in-oil dispersion by a hydrophilic membrane

    NARCIS (Netherlands)

    Keurentjes, J.T.F.; Doornbusch, G.I.; Riet, van 't K.

    1991-01-01

    Fatty acids can be extracted from an oil phase by forming a dispersed phase of saponified fatty acids/water/isopropanol in oil. This dispersion can be separated in the two phases by two membranes of opposite polarity in series. In this study the separation of the water phase from the dispersion by a

  4. Gas flow headspace liquid phase microextraction.

    Science.gov (United States)

    Yang, Cui; Qiu, Jinxue; Ren, Chunyan; Piao, Xiangfan; Li, Xifeng; Wu, Xue; Li, Donghao

    2009-11-06

    There is a trend towards the use of enrichment techniques such as microextraction in the analysis of trace chemicals. Based on the theory of ideal gases, theory of gas chromatography and the original headspace liquid phase microextraction (HS-LPME) technique, a simple gas flow headspace liquid phase microextraction (GF-HS-LPME) technique has been developed, where the extracting gas phase volume is increased using a gas flow. The system is an open system, where an inert gas containing the target compounds flows continuously through a special gas outlet channel (D=1.8mm), and the target compounds are trapped on a solvent microdrop (2.4 microL) hanging on the microsyringe tip, as a result, a high enrichment factor is obtained. The parameters affecting the enrichment factor, such as the gas flow rate, the position of the microdrop, the diameter of the gas outlet channel, the temperatures of the extracting solvent and of the sample, and the extraction time, were systematically optimized for four types of polycyclic aromatic hydrocarbons. The results were compared with results obtained from HS-LPME. Under the optimized conditions (where the extraction time and the volume of the extracting sample vial were fixed at 20min and 10mL, respectively), detection limits (S/N=3) were approximately a factor of 4 lower than those for the original HS-LPME technique. The method was validated by comparison of the GF-HS-LPME and HS-LPME techniques using data for PAHs from environmental sediment samples.

  5. 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.

  6. Diagnostics for liquid dispersion due to a high-speed impact with accident or vulnerability assessment application

    International Nuclear Information System (INIS)

    Jepsen, Richard A; O'Hern, Timothy; Demosthenous, Byron; Bystrom, Ed; Nissen, Mark; Romero, Edward; Yoon, Sam S

    2009-01-01

    The high-speed impact and subsequent dispersion of a large liquid slug is of interest for assessing vulnerability of structures when subjected to such an event. The Weber number associated with such liquid impacts is generally between 10 5 and 10 8 . Because of the experiment scale and destructive nature of these high-energy impacts, most traditional diagnostics are difficult to implement. Therefore, unique diagnostics were employed in several tests to gather information on impact force, spreading instability, slug break-up, ejection velocity, droplet deformation and spray characteristics. Measurement techniques discussed here include high-speed photometrics, particle image velocimetry (PIV), TrackEye particle analysis, speckle correlation, single-pass schlieren imaging, phase Doppler particle analyzer (PDPA) and load cell measurements as applied to large-scale, high-speed liquid impacts

  7. The initial phase of sudden releases of superheated liquid

    International Nuclear Information System (INIS)

    Schmidli, J.

    1994-04-01

    The catastrophic failure of a pressure vessel containing a liquefied substance, leading to an instantaneous release of its whole contents is considered as one of the major technological hazards. Due to the rapid depressurization caused by vessel failure, the fluid becomes superheated and unstable. Part of the fluid will evaporate using its internal energy and the two-phase mixture forming will be accelerated. This flashing process can be very violent, as experiments and incidents actually happened have shown. In the past, a number of dispersion models were developed to predict the history of an instantaneous release. In most of these models the source term is considered to be a gas volume at rest and not a rapidly expanding aerosol, as could be observed. Furthermore, it is usually assumed that all of the remaining fluid is entrained into the expanding cloud and nothing is deposited on the ground to form a pool. This work concentrates on the initial phase of the sudden release of superheated liquids with the aim to gain a better understanding of the flashing process and of the physical mechanisms involved, leading to a reliable prediction of the source term. Therefore, more than 400 experiments with propane, butane, refrigerant 12 and 114 were conducted. The experiments were initiated by shattering spherical glass flasks of different sizes. The main parameters varied were the liquid superheat and the filling level of the vessel. Using high-speed video and movie recordings and very fast responding measurement devices, it was possible to study the initial phase of such releases during which gravity plays no role. For sufficiently large released internal energy, the initial evolution of the release was always spherical with a constant radial expansion velocity during he first milliseconds until instabilities appeared at the surface of the droplet/vapor cloud that was formed. For all the experimental conditions, the fraction of the initial liquid falling on the ground

  8. 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%. 

  9. Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD) and Dispersive Solid Phase Extraction (d-SPE) of Plant Samples

    Science.gov (United States)

    Sowa, Ireneusz; Wójciak-Kosior, Magdalena; Strzemski, Maciej; Sawicki, Jan; Staniak, Michał; Dresler, Sławomir; Szwerc, Wojciech; Mołdoch, Jarosław; Latalski, Michał

    2018-01-01

    Polyaniline (PANI) is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME). In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI) was used for dispersive solid phase extraction (d-SPE) and matrix solid–phase extraction (MSPD). The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD) quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples. PMID:29565297

  10. Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD and Dispersive Solid Phase Extraction (d-SPE of Plant Samples

    Directory of Open Access Journals (Sweden)

    Ireneusz Sowa

    2018-03-01

    Full Text Available Polyaniline (PANI is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME. In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI was used for dispersive solid phase extraction (d-SPE and matrix solid–phase extraction (MSPD. The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples.

  11. Periodic radio variability in NRAO 530: phase dispersion minimization analysis

    International Nuclear Information System (INIS)

    Lu Junchao; Lin Jiming; Qiu Hongbing; Wang Junyi; An Tao

    2012-01-01

    A periodicity analysis of the radio light curves of the blazar NRAO 530 at 14.5, 8.0, and 4.8 GHz is presented employing an improved phase dispersion minimization technique. The result, which shows two persistent periodic components of ∼ 6 and ∼ 10 yr at all three frequencies, is consistent with the results obtained with the Lomb-Scargle periodogram and weighted wavelet Z-transform algorithms. The reliability of the derived periodicities is confirmed by the Monte Carlo numerical simulations which show a high statistical confidence. (Quasi-)Periodic fluctuations of the radio luminosity of NRAO 530 might be associated with the oscillations of the accretion disk triggered by hydrodynamic instabilities of the accreted flow. (research papers)

  12. Axial dispersion, holdup and slip velocity of dispersed phase in a pulsed sieve plate extraction column by radiotracer residence time distribution analysis.

    Science.gov (United States)

    Din, Ghiyas Ud; Chughtai, Imran Rafiq; Inayat, Mansoor Hameed; Khan, Iqbal Hussain

    2008-12-01

    Axial dispersion, holdup and slip velocity of dispersed phase have been investigated for a range of dispersed and continuous phase superficial velocities in a pulsed sieve plate extraction column using radiotracer residence time distribution (RTD) analysis. Axial dispersion model (ADM) was used to simulate the hydrodynamics of the system. It has been observed that increase in dispersed phase superficial velocity results in a decrease in its axial dispersion and increase in its slip velocity while its holdup increases till a maximum asymptotic value is achieved. An increase in superficial velocity of continuous phase increases the axial dispersion and holdup of dispersed phase until a maximum value is obtained, while slip velocity of dispersed phase is found to decrease in the beginning and then it increases with increase in superficial velocity of continuous phase.

  13. Phase Modulation for postcompensation of dispersion in 160-Gb/s systems

    DEFF Research Database (Denmark)

    Siahlo, Andrei; Clausen, A. T.; Oxenløwe, Leif Katsuo

    2005-01-01

    Tunable postcompensation of second-order dispersion by sinusoidal phase modulation is realized for a 160-Gb/s optical transmission system. Accumulated dispersions with magnitudes up to 4 ps/nm are compensated in the receiver end.......Tunable postcompensation of second-order dispersion by sinusoidal phase modulation is realized for a 160-Gb/s optical transmission system. Accumulated dispersions with magnitudes up to 4 ps/nm are compensated in the receiver end....

  14. Reduction of the barium concentration presents in liquid effluents by mean of non-dispersive extraction in hollow fiber modules

    International Nuclear Information System (INIS)

    Duperle Yaruro, Gladys; Pena, Dario Yesid; Escalante Hernandez, Humberto

    2008-01-01

    This work has been focused on the study of the viability of barium removal, present in a waste liquid phase, by means of non-dispersive extraction (NDE) in hollow fiber modules. An organic solution based on DEPHA (Bis-2-ethylhexyl phosphate) 30% (v/v), isopropilic alcohol 30% (v/v) and kerosene is used as selective extraction medium. For the extraction process was made a contactor with five hollow microporous propilenic fibers. A solution contained 100 ppm of BaCl 2 H 2 O, level concentration very equal as generated on the petroleum industrial wastes, is used as liquid phase. a efficiency of 95,25% is obtained when the NDE take place at pH = 9, and them 9 hours of process

  15. One-step displacement dispersive liquid-liquid microextraction coupled with graphite furnace atomic absorption spectrometry for the selective determination of methylmercury in environmental samples.

    Science.gov (United States)

    Liang, Pei; Kang, Caiyan; Mo, Yajun

    2016-01-01

    A novel method for the selective determination of methylmercury (MeHg) was developed by one-step displacement dispersive liquid-liquid microextraction (D-DLLME) coupled with graphite furnace atomic absorption spectrometry. In the proposed method, Cu(II) reacted with diethyldithiocarbamate (DDTC) to form Cu-DDTC complex, which was used as the chelating agent instead of DDTC for the dispersive liquid-liquid microextraction (DLLME) of MeHg. Because the stability of MeHg-DDTC is higher than that of Cu-DDTC, MeHg can displace Cu from the Cu-DDTC complex and be preconcentrated in a single DLLME procedure. MeHg could be extracted into the extraction solvent phase at pH 6 while Hg(II) remained in the sample solution. Potential interference from co-existing metal ions with lower DDTC complex stability was largely eliminated without the need of any masking reagent. Under the optimal conditions, the limit of detection of this method was 13.6ngL(-1) (as Hg), and an enhancement factor of 81 was achieved with a sample volume of 5.0mL. The proposed method was successfully applied for the determination of trace MeHg in some environmental samples with satisfactory results. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Nickel nanostructured materials from liquid phase photodeposition

    International Nuclear Information System (INIS)

    Giuffrida, Salvatore; Condorelli, Guglielmo G.; Costanzo, Lucia L.; Ventimiglia, Giorgio; Nigro, Raffaella Lo; Favazza, Maria; Votrico, Enrico; Bongiorno, Corrado; Fragala, Ignazio L.

    2007-01-01

    Liquid Phase Photo-Deposition (LPPD) technique has been used to obtain both colloidal particles and thin films of metallic and chloride nickel from solutions of only precursor Ni(acac) 2 (acac=2,4-pentandionato). Metallic nickel was obtained from ethanol solutions by direct nickel(II) photoreduction at 254 nm and by acetone sensitised reaction at 300 nm. In this latter process the rate was higher than in the first one. NiCl 2 was formed from CCl 4 solution by a solvent-initiated reaction. TEM analysis, performed on colloidal particles of nickel, showed that their dimensions are in the range 2-4 nm. The films did not present carbon contamination and were characterized by AFM, XPS and GIXRD. Metallic films consisted of particles of 20-40 nm that are the result of the aggregation of smaller crystallites (4-5 nm). Larger agglomerations (around 200 nm) have been observed for NiCl 2 films

  17. 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)

  18. 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)

  19. Binary Solvents Dispersive Liquid—Liquid Microextraction (BS-DLLME) Method for Determination of Tramadol in Urine Using High-Performance Liquid Chromatography

    Science.gov (United States)

    2014-01-01

    Background 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. Results 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%. Conclusions 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. PMID:24495475

  20. Semiconductor nanocrystals dispersed in imidazolium-based ionic liquids: a spectroscopic and morphological investigation

    International Nuclear Information System (INIS)

    Panniello, Annamaria; Binetti, Enrico; Ingrosso, Chiara; Curri, M. Lucia; Agostiano, Angela; Tommasi, Raffaele; Striccoli, Marinella

    2013-01-01

    A growing interest is devoted to the study of imidazolium-based ionic liquids as innovative materials to combine with functional elements for advanced technological applications. Materials based on semiconductor and oxide nanocrystals in ionic liquids can be promising for their integration in lithium batteries, as well as in innovative solar cells. Although the physical chemical properties and the solvation dynamics of bare ionic liquids have been extensively studied, their combination with colloidal nanocrystals still remains almost unexplored. Here, the optical properties of organic-capped luminescent cadmium selenide nanocrystals coated by a shell of zinc sulfide (CdSe(ZnS)) dispersed in 1,3-dialkyl imidazolium ionic liquids have been investigated, also in dependence of the alkyl chain length on the imidazolium ring and of the anion nature, by using both time-integrated and time-resolved optical spectroscopy. The observed variations in decay profiles of the ionic liquid in presence of colloidal nanocrystals suggest that the dispersion of the nanostructures induces modifications in the ionic liquid structural order. Finally, atomic force microscopy analysis has provided insight into the topography of the investigated dispersions deposited as film, confirming the organization of the ionic liquids in super-structures, also upon nanocrystal incorporation.

  1. A Study on Fluid Dispersion after Liquid Filled Missile Impact

    International Nuclear Information System (INIS)

    Shin, Sang Shup; Hahm, Daegi; Choi, In-Kil

    2015-01-01

    In order to fire damage evaluations by fuel included transportation crash, the fire duration should be analyzed that consider the fuel spread range, amount of leaked fuel, and various ignition sources. The water slug impact test performed in Sandia National Laboratory (SNL) in 2002 was representative. The cloud of mist dispersion range of the dyed red water and ejection velocity of water after impact were analyzed using Particle Image Velocimetry (PIV) method and numerical simulation. In this study, the included fluid was modeled by using smooth particle hydrodynamics (SPH) technique. The fluid dispersion range following impact was analyzed by considering the particle velocity and flying distance. The result values obtained through this study were compared to the water slug (WS) test results. And the applicability of an analysis method was verified by comparing the WS test results. The results and methodology obtained through this study can be utilized to damage assessment, fuel spread and fire risk for large infrastructures such as nuclear power plants following an aircraft impact. In this study, the included fluid was modeled by using smooth particle hydrodynamics (SPH) technique; the fluid spread range following an impact was analyzed. The radius of fluid spread on the numerical analysis became conservative than the WS test results. However, the shape of the cloud is similar to the WS test results

  2. A Study on Fluid Dispersion after Liquid Filled Missile Impact

    Energy Technology Data Exchange (ETDEWEB)

    Shin, Sang Shup; Hahm, Daegi; Choi, In-Kil [KAERI, Daejeon (Korea, Republic of)

    2015-05-15

    In order to fire damage evaluations by fuel included transportation crash, the fire duration should be analyzed that consider the fuel spread range, amount of leaked fuel, and various ignition sources. The water slug impact test performed in Sandia National Laboratory (SNL) in 2002 was representative. The cloud of mist dispersion range of the dyed red water and ejection velocity of water after impact were analyzed using Particle Image Velocimetry (PIV) method and numerical simulation. In this study, the included fluid was modeled by using smooth particle hydrodynamics (SPH) technique. The fluid dispersion range following impact was analyzed by considering the particle velocity and flying distance. The result values obtained through this study were compared to the water slug (WS) test results. And the applicability of an analysis method was verified by comparing the WS test results. The results and methodology obtained through this study can be utilized to damage assessment, fuel spread and fire risk for large infrastructures such as nuclear power plants following an aircraft impact. In this study, the included fluid was modeled by using smooth particle hydrodynamics (SPH) technique; the fluid spread range following an impact was analyzed. The radius of fluid spread on the numerical analysis became conservative than the WS test results. However, the shape of the cloud is similar to the WS test results.

  3. Possibilities of practical usage of dispersed aluminim oxidation by liquid water

    Science.gov (United States)

    Larichev, M. N.; Laricheva, O. O.; Shaitura, N. S.; Shkolnikov, E. I.

    2012-12-01

    The goal of this work is to show the possibility of practical usage of the environmentally pure oxidation process of preliminarily dispersed aluminum (aluminum powders of the ASD or PAD grade according to TU (Technical Specifications) 48-5-226-87, which are serially produced in industry) with liquid water in order to obtain gaseous hydrogen in volumes sufficient to provide the operation of energizers based on airhydrogen fuel cells (AHFC) for portable and stationary devices (up to 3 kW). It is shown that the synthesis of aluminum oxides-hydroxides with the specified phase and chemical compositions as well as the particle shape and size can be provided simultaneously with producing commercial hydrogen. The practical usage of hydrogen, which is formed in the oxidation reaction of metallic aluminum with liquid water at pressures close to atmospheric (particularly, to service AHFCs), requires reaction intensification to increase the oxidation rate of aluminum. In this work, we considered the aspects of practical implementation of thermal, ultrasonic, and chemical activation as well as their combinations for this purpose. As the chemical activator of oxidation, we used the additives of calcium oxide (<5% of the mass of oxidized aluminum). Application of each activation method affects the phase and chemical compositions as well as the structure of formed aluminum hydroxides, which provides the possibility of their reproducible production. Thus, simultaneously with the production of commercial hydrogen, solid oxidation products satisfying the needs of industry in aluminum oxides and having the specified composition, purity, and particle shape and size can be synthesized. The acquired experimental results and elements of the design of specially developed industrial apparatuses, which were used when performing this work, can be applied when designing the model of the hydrogen generator—the prototype of the hydrogen generator for portable and stationary devices or devices

  4. Memory effect of polymer dispersed liquid crystal by hybridization with nanoclay

    Directory of Open Access Journals (Sweden)

    2010-01-01

    Full Text Available The electro-optical performances of polymer dispersed liquid crystal (PDLC were investigated in the presence of organically modified clays. With the addition and increasing amount of modified clay, driving voltage and memory effect, viz. transparent state of the film after the electricity is off simultaneously increased due most likely to the increased viscosity. Among the two types of modifier, 4-(4-aminophenyl benzonitrile having greater chemical affinity with LC than hexylamine, gave finer dispersion of clay in liquid crystal, greater viscosity, larger driving voltage and response time, and greater memory effect.

  5. Long-range dipolar order and dispersion forces in polar liquids

    Science.gov (United States)

    Besford, Quinn Alexander; Christofferson, Andrew Joseph; Liu, Maoyuan; Yarovsky, Irene

    2017-11-01

    Complex solvation phenomena, such as specific ion effects, occur in polar liquids. Interpretation of these effects in terms of structure and dispersion forces will lead to a greater understanding of solvation. Herein, using molecular dynamics, we probe the structure of polar liquids through specific dipolar pair correlation functions that contribute to the potential of mean force that is "felt" between thermally rotating dipole moments. It is shown that unique dipolar order exists at separations at least up to 20 Å for all liquids studied. When the structural order is compared with a dipolar dispersion force that arises from local co-operative enhancement of dipole moments, a strong agreement is found. Lifshitz theory of dispersion forces was compared with the structural order, where the theory is validated for all liquids that do not have significant local dipole correlations. For liquids that do have significant local dipole correlations, specifically liquid water, Lifshitz theory underestimates the dispersion force by a factor of 5-10, demonstrating that the force that leads to the increased structure in liquid water is missed by Lifshitz theory of van der Waals forces. We apply similar correlation functions to an ionic aqueous system, where long-range order between water's dipole moment and a single chloride ion is found to exist at 20 Å of separation, revealing a long-range perturbation of water's structure by an ion. Furthermore, we found that waters within the 1st, 2nd, and 3rd solvation shells of a chloride ion exhibit significantly enhanced dipolar interactions, particularly with waters at larger distances of separation. Our results provide a link between structures, dispersion forces, and specific ion effects, which may lead to a more robust understanding of solvation.

  6. Droplet behavior analysis in consideration of droplet entrainment from liquid film in annular dispersed flow

    International Nuclear Information System (INIS)

    Matsuura, Keizo; Otake, Hiroshi; Kataoka, Isao; Serizawa, Akimi

    2000-01-01

    A method of droplet behavior simulation in an annular dispersed flow has been developed. In this method, both droplet deposition and entrainment from liquid film are considered. The Lagrangian method and stochastic model are used to analyze droplet diffusion and deposition behavior in a turbulent flow, and droplet entrainment from liquid film is calculated by an entrainment correlation. For the verification of this method, Gill's experiment is analyzed, in which the transition from annular flow with no entrainment to equilibrium annular dispersed flow was observed. Analysis results can also show the similar transition tendency. The experimental results of radial distribution of droplet mass flux are compared with analysis results. The agreement is good for low liquid flow rate, but entrainment rate must be adjusted for high liquid flow rate, in which gas turbulence is thought to be modified by high droplet density. In future work the effect of high droplet density on turbulence should be considered. (author)

  7. Antiwear performance of ionic liquid+graphene dispersions with anomalous viscosity-temperature behavior

    OpenAIRE

    Pamies Porras, Ramón Francisco; Arias Pardilla, Joaquín; Espinosa Rodríguez, Tulia; Carrión Vilches, Francisco José; Bermúdez Olivares, María Dolores; Sanes Molina, José; Avilés González, María Dolores

    2018-01-01

    New dispersions of few-layers graphene (G) in 1-ethyl-3-methylimidazolium ([EMIM]) ionic liquids (ILs) with dicyanamide ([DCA]) or bis(trifluoromethylsulfonyl)imide ([TFSI]) anions have been obtained by mechanical mixing and sonication. IL+0.5 wt% G dispersions show constant viscosity values from 357K (for IL = [EMIM][DCA]) or from 385K (for IL = [EMIM][TFSI]) to 393K. IL + G dispersions with G > 0.5 wt% show linear viscosity increases with increasing temperature, from 306K (for [EMIM][DCA]+1...

  8. Multiresidue analysis of oestrogenic compounds in cow, goat, sheep and human milk using core-shell polydopamine coated magnetic nanoparticles as extraction sorbent in micro-dispersive solid-phase extraction followed by ultra-high-performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Socas-Rodríguez, Bárbara; Hernández-Borges, Javier; Herrera-Herrera, Antonio V; Rodríguez-Delgado, Miguel Ángel

    2018-03-01

    In this work, the suitability of Fe 3 O 4 nanoparticles coated with polydopamine was evaluated as sorbent for the extraction of a group of 21 compounds with oestrogenic activity including seven phytoestrogens, six mycotoxins as well as four synthetic and four natural oestrogens from different types of milk, including sheep milk, in which the evaluation of oestrogenic compounds have never been developed before. Extraction was carried out using magnetic micro-dispersive solid-phase extraction after a previous deproteinisation step. Separation, determination and quantification of the target analytes were achieved by ultra-high-performance liquid chromatography coupled to triple quadrupole-tandem mass spectrometry. The methodology was validated for five milk samples using 17β-estradiol-2,4,16,16,17-d 5 as internal standard for natural and synthetic oestrogens, β-zearalanol-10,10,11,12,12-d 5 for mycotoxins and prunetin for phytoestrogens. Recovery values ranged from 70 to 120% for the five types of matrices with relative standard deviation values lower than 18%. Limits of quantification of the method were in the range 0.55-11.8 μg L -1 for all samples. Graphical abstract General scheme of the multiresidue analysis of oestrogenic compounds in milk using core-shell polydopamine coated magnetic nanoparticles as extraction sorbent in μ-dSPE.

  9. Dispersed-fringe-accumulation-based left-subtract-right method for fine co-phasing of a dispersed fringe sensor.

    Science.gov (United States)

    Li, Yang; Wang, Shengqian; Rao, Changhui

    2017-05-20

    In this paper, a dispersed-fringe-accumulation (DFA)-based left-subtract-right (LSR) piston estimation method (DFA-LSR), in which the dispersed fringe image is accumulated in the dispersed direction, and then the LSR method is used to estimate the piston error, is proposed for dispersed fringe sensors (DFS) in the fine co-phasing stage. The DFS is usually used to detect the piston errors (optical path difference) between different segmented mirrors or synthetic aperture telescopes. The DFA-LSR makes up for the shortcomings of the main peak position (MPP) method, which suffers from the constant offset in the pixel counts. The analysis and experiment results show that the proposed method can keep relatively better performance even at the condition of poor signal-to-noise ratio, compared with the MPP method in fine co-phasing stage.

  10. Simultaneous determination of pyrethroids and pyrethrins by dispersive liquid-liquid microextraction and liquid chromatography triple quadrupole mass spectrometry in environmental samples.

    Science.gov (United States)

    Ccanccapa-Cartagena, Alexander; Masiá, Ana; Picó, Yolanda

    2017-08-01

    A simple and environmentally friendly dispersive liquid-liquid microextraction (DLLME) method coupled with electrospray ionization liquid chromatography triple quadrupole mass spectrometry (LC-QqQ-MS/MS) was developed for the simultaneous determination of 17 synthetic and natural pyrethroids. A comparison of solid-phase extraction (SPE) versus DLLME for water samples and only "dilute and shoot" versus the additional extract cleanup by DLLME for sediment samples is reported. Chloroform was the extracting solvent in the DLLME technique for both water and sediment samples. Ultrasonic energy was applied to fully extract the analytes into fine droplets, providing high recoveries in short times. Method detection limits (MDLs) ranged from 0.12 to 0.62 ng L -1 and recoveries from 70 to 119% with RSD values 2-15% (n = 5) for water samples. In sediment samples, MDLs ranged from 0.50 to 2.50 ng g -1 and recoveries from 71 to 112% with RSDs 2-16% (n = 5). The proposed method showed a good linearity within the range of 10-500 ng mL -1 , with coefficients of determination (R 2 ) higher than 0.99. Matrix effects were observed for most compounds in water and sediment (ME% Albufera wetland and Turia River. Acrinathrin (48 ng g -1 ) and etofenprox (16 ng g -1 ) were detected in sediment samples. Graphical abstract Pyrethrins and pyrethroid determination in water and sediments by DLLME and LC-MS/MS.

  11. Liquid-liquid phase transition and glass transition in a monoatomic model system.

    Science.gov (United States)

    Xu, Limei; Buldyrev, Sergey V; Giovambattista, Nicolas; Stanley, H Eugene

    2010-01-01

    We review our recent study on the polyamorphism of the liquid and glass states in a monatomic system, a two-scale spherical-symmetric Jagla model with both attractive and repulsive interactions. This potential with a parametrization for which crystallization can be avoided and both the glass transition and the liquid-liquid phase transition are clearly separated, displays water-like anomalies as well as polyamorphism in both liquid and glassy states, providing a unique opportunity to study the interplay between the liquid-liquid phase transition and the glass transition. Our study on a simple model may be useful in understanding recent studies of polyamorphism in metallic glasses.

  12. 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.

  13. Measurement of phase interaction in dispersed gas-particle two-phase flow by phase-doppler anemometry

    OpenAIRE

    Mergheni Ali Mohamed; Ben Ticha Hmaied; Sautet Jen-Charles; Godard Gille; Ben Nasrallah Sassi

    2008-01-01

    For simultaneous measurement of size and velocity distributions of continuous and dispersed phases in a two-phase flow a technique phase-Doppler anemometry was used. Spherical glass particles with a particle diameter range from 102 up to 212 µm were used. In this two-phase flow an experimental results are presented which indicate a significant influence of the solid particles on the flow characteristics. The height of influence of these effects depends on the local position in the jet. Near t...

  14. Droplets in annular-dispersed gas-liquid pipe-flows

    NARCIS (Netherlands)

    Van 't Westende, J.M.C.

    2008-01-01

    Annular-dispersed gas-liquid pipe-flows are commonly encountered in many industrial applications, and have already been studied for many decades. However, due to the great complexity of this type of flow, there are still many phenomena that are poorly understood. The aim of this thesis is to shed

  15. The initial phase of sudden releases of superheated liquid

    International Nuclear Information System (INIS)

    Schmidli, J.; Yadigaroglu, G.

    1994-01-01

    Series of experiments were conducted with refrigerants-114, -12, propane and butane to investigate the initial phase of sudden releases of superheated liquids due to the catastrophic failure of the vessel containing them. The experiments were initiated by shattering spherical flasks of 100 to 2000 ml containing the liquefied, pressurized gases. The variable parameters were the initial superheat, the filling level, the height of the flask above ground, and the relative humidity of the surrounding air. It was found that the initial flashing process is not determined by homogeneous nucleation, but rather by surface instabilities which lead to an evaporation wave traveling from the initial surface towards the center of the released mass. Cloud shape and expansion velocity could be determined from high speed recordings covering the initial stage of the release during which gravity has no influence. When the internal energy was sufficient, it was observed that the expanding droplet/vapor cloud initially propagated spherically with a constant expansion velocity, until Rayleigh-Taylor type instabilities appeared at its surface. Information about the pool which can be formed on the ground, the pressure decay within the flask, the droplet size, and the cloud temperature was collected. The experimental findings for the expansion velocity, as well as for the pool fraction, were the base for a nondimensional analysis leading to correlations which describe the initial phase of such releases and can be used to define the ''source term'' for turbulent dispersion models. (author) 5 figs., 1 tab., 15 refs

  16. Spontaneous phase separation during self-assembly in bi-dispersed spherical iron oxide nanoparticle monolayers

    International Nuclear Information System (INIS)

    Stanley, Jacob; Boucheron, Leandra; Shpyrko, Oleg; Lin, Binhua; Meron, Mati

    2015-01-01

    Recent developments in the synthesis of iron oxide nanoparticles have resulted in the ability to fabricate roughly spherical particles with extremely high size uniformity (low polydispersity). These particles can form self-assembled monolayer films at an air-water interface. When the polydispersity of the particles is low, these monolayers can be well-ordered over a length scale dozens of times the particle size. The van der Waals force between the particles is what drives this self-assembly. Through the use of Grazing Incidence X-Ray Diffraction we demonstrate that, when these films are formed at the liquid surface from bi-dispersed solutions containing 10 and 20 nm spherical particles suspended in chloroform, the particles phase separate into well-ordered patches during the self-assembly process. Furthermore, the domain sizes of these phase separated regions are at most 2–3 times smaller than that of a film comprising only mono-dispersed particles and their degree of disorder is comparable. This is shown for multiple solutions with differing ratios of 10 and 20 nm particles

  17. Spontaneous phase separation during self-assembly in bi-dispersed spherical iron oxide nanoparticle monolayers

    Energy Technology Data Exchange (ETDEWEB)

    Stanley, Jacob; Boucheron, Leandra; Shpyrko, Oleg, E-mail: lin@cars.uchicago.edu, E-mail: oshpyrko@physics.ucsd.edu [Department of Physics, University of California, San Diego, La Jolla, California 92093 (United States); Lin, Binhua, E-mail: lin@cars.uchicago.edu, E-mail: oshpyrko@physics.ucsd.edu; Meron, Mati [Center for Advanced Radiation Sources (CARS), University of Chicago, Chicago, Illinois 60637 (United States)

    2015-04-20

    Recent developments in the synthesis of iron oxide nanoparticles have resulted in the ability to fabricate roughly spherical particles with extremely high size uniformity (low polydispersity). These particles can form self-assembled monolayer films at an air-water interface. When the polydispersity of the particles is low, these monolayers can be well-ordered over a length scale dozens of times the particle size. The van der Waals force between the particles is what drives this self-assembly. Through the use of Grazing Incidence X-Ray Diffraction we demonstrate that, when these films are formed at the liquid surface from bi-dispersed solutions containing 10 and 20 nm spherical particles suspended in chloroform, the particles phase separate into well-ordered patches during the self-assembly process. Furthermore, the domain sizes of these phase separated regions are at most 2–3 times smaller than that of a film comprising only mono-dispersed particles and their degree of disorder is comparable. This is shown for multiple solutions with differing ratios of 10 and 20 nm particles.

  18. Contribution to the study of second phases particles dispersion in polycrystalline uranium dioxide

    International Nuclear Information System (INIS)

    Peres, V.

    1994-06-01

    To reduce fission gas release of irradiated polycrystalline uranium dioxide, the dispersion of intragranular nanometric particles of second phase necessary to pin gas bubbles may complete the advantage of a large-grained fuel microstructure. Moreover, intergranular glass films may improve high temperatures mechanical properties of UO 2 . In this study, mixtures of additives composed of ''corindon'' structure oxides that enhance the fuel grain growth and composed of different oxides with variable solid solubilities in the UO 2 matrix were achieved. Additives with a negligible solubility inhibit grain boundaries motion except those, such as silica, that involve a liquid phase at the sintering temperature. Rare earth oxides that form stable solid solutions with UO 2 cannot lead to precipitation, but have no effect on the fuel grain growth doped with ''corindon'' type oxides. A chromium oxide excess allows the creation of a fuel microstructure described by large grains and intragranular spherical Cr 2 O 3 inclusions observed by scanning electron microscopy. Values for the bulk lattice diffusion coefficient of Cr 3+ cations in UO 2 can be deduced from the experimental growth of those dispersed particles by an Ostwald ripening mechanism. The formation of small precipitated metal particles inside the uranium dioxide matrix induced by the internal reduction of a solid solution has not been performed. However, direct reduction of insoluble chromium oxide particles is easy and produces metallic intragranular precipitates. (author). 119 refs., 112 figs., 33 tabs., 5 annexes

  19. Void fraction fluctuations in two-phase gas-liquid flow

    International Nuclear Information System (INIS)

    Ulbrich, R.

    1987-01-01

    Designs of the apparatus in which two-phase gas-liquid flow occurs are usually based on the mean value of parameters such as pressure drop and void fraction. The flow of two-phase mixtures generally presents a very complicated flow structure, both in terms of the unsteady formation on the interfacial area and in terms of the fluctuations of the velocity, pressure and other variables within the flow. When the gas void fraction is near 0 or 1 / bubble or dispersed flow regimes / then oscillations of void fraction are very small. The intermittent flow such as plug and slug/ froth is characterized by alternately flow portions of liquid and gas. It influences the change of void fractions in time. The results of experimental research of gas void fraction fluctuations in two-phase adiabatic gas-liquid flow in a vertical pipe are presented

  20. Nickel nanostructured materials from liquid phase photodeposition

    Energy Technology Data Exchange (ETDEWEB)

    Giuffrida, Salvatore, E-mail: sgiuffrida@unict.it; Condorelli, Guglielmo G.; Costanzo, Lucia L.; Ventimiglia, Giorgio [Universita degli Studi di Catania and INSTM UdR di, Dipartimento di Scienze Chimiche (Italy); Nigro, Raffaella Lo [IMM-CNR (Italy); Favazza, Maria; Votrico, Enrico [Universita degli Studi di Catania and INSTM UdR di, Dipartimento di Scienze Chimiche (Italy); Bongiorno, Corrado [IMM-CNR (Italy); Fragala, Ignazio L. [Universita degli Studi di Catania and INSTM UdR di, Dipartimento di Scienze Chimiche (Italy)

    2007-08-15

    Liquid Phase Photo-Deposition (LPPD) technique has been used to obtain both colloidal particles and thin films of metallic and chloride nickel from solutions of only precursor Ni(acac){sub 2} (acac=2,4-pentandionato). Metallic nickel was obtained from ethanol solutions by direct nickel(II) photoreduction at 254 nm and by acetone sensitised reaction at 300 nm. In this latter process the rate was higher than in the first one. NiCl{sub 2} was formed from CCl{sub 4} solution by a solvent-initiated reaction. TEM analysis, performed on colloidal particles of nickel, showed that their dimensions are in the range 2-4 nm. The films did not present carbon contamination and were characterized by AFM, XPS and GIXRD. Metallic films consisted of particles of 20-40 nm that are the result of the aggregation of smaller crystallites (4-5 nm). Larger agglomerations (around 200 nm) have been observed for NiCl{sub 2} films.

  1. Preliminary investigation of liquid phase sintering in ferrous systems

    International Nuclear Information System (INIS)

    Klein, J.

    1975-04-01

    Liquid phase sintering was utilized to achieve, by a simple compaction and sintering procedure involving short times and moderate temperatures, a virtually full dense high carbon Fe:C alloy and high boron Fe:B alloy. Parameters such as powder characteristics and mixing, compacting pressure, heating program and the liquid phase fraction were found to influence the sintered density. The response of the Fe:C alloy to a heat treatment is reported along with preliminary experiments in the iron base ternary system Fe:W:C. Residual porosities observed in microstructures of certain liquid phase sintered compacts were accounted for by a proposed capillary flow of the liquid phase and a local densification competing against an overall densification. Some general recommendations are made for liquid phase sintering of powder aggregates. 15 fig., 7 tables

  2. Flexible, ferroelectric nanoparticle doped polymer dispersed liquid crystal devices for lower switching voltage and nanoenergy generation

    Science.gov (United States)

    Nimmy John, V.; Varanakkottu, Subramanyan Namboodiri; Varghese, Soney

    2018-06-01

    Flexible polymer dispersed liquid crystal (F-PDLC) devices were fabricated using transparent conducting ITO/PET film. Polymerization induced phase separation (PIPS) method was used for pure and ferroelectric BaTiO3 (BTO) and ZnO doped PDLC devices. The distribution of nanoparticles in the PDLC and the formation of micro cavities were studied using field emission scanning electron microscopy (FESEM). It was observed that the addition of ferroelectric BTO nanoparticles has reduced the threshold voltage (Vth) and saturation voltage (Vsat) of FNP-PDLC by 85% and 41% respectively due to the spontaneous polarization of ferroelectric nanoparticles. The ferroelectric properties of BTO and ZnO in the fabricated devices were investigated using dynamic contact electrostatic force microscopy (DC EFM). Flexing the device can generate a potential due to the piezo-tribo electric effect of the ferroelectric nanomaterial doped in the PDLC matrix, which could be utilized as an energy generating system. The switching voltage after multiple flexing was also studied and found to be in par with non-flexing situations.

  3. Liquid contrabands classification based on energy dispersive X-ray diffraction and hybrid discriminant analysis

    International Nuclear Information System (INIS)

    YangDai, Tianyi; Zhang, Li

    2016-01-01

    Energy dispersive X-ray diffraction (EDXRD) combined with hybrid discriminant analysis (HDA) has been utilized for classifying the liquid materials for the first time. The XRD spectra of 37 kinds of liquid contrabands and daily supplies were obtained using an EDXRD test bed facility. The unique spectra of different samples reveal XRD's capability to distinguish liquid contrabands from daily supplies. In order to create a system to detect liquid contrabands, the diffraction spectra were subjected to HDA which is the combination of principal components analysis (PCA) and linear discriminant analysis (LDA). Experiments based on the leave-one-out method demonstrate that HDA is a practical method with higher classification accuracy and lower noise sensitivity than the other methods in this application. The study shows the great capability and potential of the combination of XRD and HDA for liquid contrabands classification.

  4. Liquid contrabands classification based on energy dispersive X-ray diffraction and hybrid discriminant analysis

    Energy Technology Data Exchange (ETDEWEB)

    YangDai, Tianyi [Department of Engineering Physics, Tsinghua University, Beijing 100084 (China); Key Laboratory of Particle & Radiation Imaging (Tsinghua University), Ministry of Education (China); Zhang, Li, E-mail: zhangli@nuctech.com [Department of Engineering Physics, Tsinghua University, Beijing 100084 (China); Key Laboratory of Particle & Radiation Imaging (Tsinghua University), Ministry of Education (China)

    2016-02-01

    Energy dispersive X-ray diffraction (EDXRD) combined with hybrid discriminant analysis (HDA) has been utilized for classifying the liquid materials for the first time. The XRD spectra of 37 kinds of liquid contrabands and daily supplies were obtained using an EDXRD test bed facility. The unique spectra of different samples reveal XRD's capability to distinguish liquid contrabands from daily supplies. In order to create a system to detect liquid contrabands, the diffraction spectra were subjected to HDA which is the combination of principal components analysis (PCA) and linear discriminant analysis (LDA). Experiments based on the leave-one-out method demonstrate that HDA is a practical method with higher classification accuracy and lower noise sensitivity than the other methods in this application. The study shows the great capability and potential of the combination of XRD and HDA for liquid contrabands classification.

  5. Liquid contrabands classification based on energy dispersive X-ray diffraction and hybrid discriminant analysis

    Science.gov (United States)

    YangDai, Tianyi; Zhang, Li

    2016-02-01

    Energy dispersive X-ray diffraction (EDXRD) combined with hybrid discriminant analysis (HDA) has been utilized for classifying the liquid materials for the first time. The XRD spectra of 37 kinds of liquid contrabands and daily supplies were obtained using an EDXRD test bed facility. The unique spectra of different samples reveal XRD's capability to distinguish liquid contrabands from daily supplies. In order to create a system to detect liquid contrabands, the diffraction spectra were subjected to HDA which is the combination of principal components analysis (PCA) and linear discriminant analysis (LDA). Experiments based on the leave-one-out method demonstrate that HDA is a practical method with higher classification accuracy and lower noise sensitivity than the other methods in this application. The study shows the great capability and potential of the combination of XRD and HDA for liquid contrabands classification.

  6. Laser--Doppler anemometry technique applied to two-phase dispersed flows in a rectangular channel

    International Nuclear Information System (INIS)

    Lee, S.L.; Srinivasan, J.

    1979-01-01

    A new optical technique using Laser--Doppler anemometry has been applied to the local measurement of turbulent upward flow of a dilute water droplet--air two-phase dispersion in a vertical rectangular channel. Individually examined were over 20,000 droplet signals coming from each of a total of ten transversely placed measuring points, the closest of which to the channel wall was 250 μ away from the wall. Two flows of different patterns due to different imposed flow conditions were investigated, one with and the other without a liquid film formed on the channel wall. Reported are the size and number density distribution and the axial and lateral velocity distributions for the droplets as well as the axial and lateral velocity distributions for the air

  7. Polarization and switching properties of holographic polymer-dispersed liquid-crystal gratings. I. Theoretical model

    Science.gov (United States)

    Sutherland, Richard L.

    2002-12-01

    Polarization properties and electro-optical switching behavior of holographic polymer-dispersed liquid-crystal (HPDLC) reflection and transmission gratings are studied. A theoretical model is developed that combines anisotropic coupled-wave theory with an elongated liquid-crystal-droplet switching model and includes the effects of a statistical orientational distribution of droplet-symmetry axes. Angle- and polarization-dependent switching behaviors of HPDLC gratings are elucidated, and the effects on dynamic range are described. A new type of electro-optical switching not seen in ordinary polymer-dispersed liquid crystals, to the best of the author's knowledge, is presented and given a physical interpretation. The model provides valuable insight to the physics of these gratings and can be applied to the design of HPDLC holographic optical elements.

  8. Faraday rotation dispersion microscopy imaging of diamagnetic and chiral liquids with pulsed magnetic field.

    Science.gov (United States)

    Suwa, Masayori; Nakano, Yusuke; Tsukahara, Satoshi; Watarai, Hitoshi

    2013-05-21

    We have constructed an experimental setup for Faraday rotation dispersion imaging and demonstrated the performance of a novel imaging principle. By using a pulsed magnetic field and a polarized light synchronized to the magnetic field, quantitative Faraday rotation images of diamagnetic organic liquids in glass capillaries were observed. Nonaromatic hydrocarbons, benzene derivatives, and naphthalene derivatives were clearly distinguished by the Faraday rotation images due to the difference in Verdet constants. From the wavelength dispersion of the Faraday rotation images in the visible region, it was found that the resonance wavelength in the UV region, which was estimated based on the Faraday B-term, could be used as characteristic parameters for the imaging of the liquids. Furthermore, simultaneous acquisition of Faraday rotation image and natural optical rotation image was demonstrated for chiral organic liquids.

  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. Monolithic Approach to Oxide Dispersion Strengthened Aluminum, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Nassau Stern Company is investigating an approach for manufacturing oxide dispersion strengthened (ODS) aluminum in bulk rather than powder form. The approach...

  11. Measurement of phase interaction in dispersed gas-particle two-phase flow by phase-doppler anemometry

    Directory of Open Access Journals (Sweden)

    Mergheni Ali Mohamed

    2008-01-01

    Full Text Available For simultaneous measurement of size and velocity distributions of continuous and dispersed phases in a two-phase flow a technique phase-Doppler anemometry was used. Spherical glass particles with a particle diameter range from 102 up to 212 µm were used. In this two-phase flow an experimental results are presented which indicate a significant influence of the solid particles on the flow characteristics. The height of influence of these effects depends on the local position in the jet. Near the nozzle exit high gas velocity gradients exist and therefore high turbulence production in the shear layer of the jet is observed. Here the turbulence intensity in the two-phase jet is decreased compared to the single-phase jet. In the developed zone the velocity gradient in the shear layer is lower and the turbulence intensity reduction is higher. .

  12. Gas holdup in a reciprocating plate bioreactor: Non-Newtonian - liquid phase

    Directory of Open Access Journals (Sweden)

    Naseva Olivera S.

    2002-01-01

    Full Text Available The gas holdup was studied in non-newtonian liquids in a gas-liquid and gas-liquid-solid reciprocating plate bioreactor. Aqueous solutions of carboxy methyl cellulose (CMC; Lucel, Lučane, Yugoslavia of different degrees of polymerization (PP 200 and PP 1000 and concentration (0,5 and 1%, polypropylene spheres (diameter 8.3 mm; fraction of spheres: 3.8 and 6.6% by volume and air were used as the liquid, solid and gas phase. The gas holdup was found to be dependent on the vibration rate, the superficial gas velocity, volume fraction of solid particles and Theological properties of the liquid ohase. Both in the gas-liquid and gas-liquid-solid systems studied, the gas holdup increased with increasing vibration rate and gas flow rate. The gas holdup was higher in three-phase systems than in two-phase ones under otter operating conditions being the same. Generally the gas holdup increased with increasing the volume fraction of solid particles, due to the dispersion action of the solid particles, and decreased with increasing non-Newtonian behaviour (decreasing flow index i.e. with increasing degree of polymerization and solution concentration of CMC applied, as a result of gas bubble coalescence.

  13. SOLID-PHASE EXTRACTION FOLLOWED BY DISPERSIVE LIQUID ...

    African Journals Online (AJOL)

    Preferred Customer

    Due to the widespread abuse of amphetamine, methamphetamine and the ... amphetamine (MDPA), drug testing for amphetamines is routinely done in ... assess amphetamines compounds in human urine samples using gas ... Italy) were prepared in methanol at a concentration of 1 mg mL-1 and stored at –18 ºC; working.

  14. Atomization of liquids in a Pease-Anthony Venturi scrubber. Part II. Droplet dispersion.

    Science.gov (United States)

    Gonçalves, J A S; Costa, M A M; Aguiar, M L; Coury, J R

    2004-12-10

    Droplet distribution is of fundamental importance to the performance of a Venturi scrubber. Ensuring good liquid distribution can increase performance at minimal liquid usage. In this study, droplet dispersion in a rectangular Pease-Anthony Venturi scrubber, operating horizontally, was examined both theoretically and experimentally. The Venturi throat cross-section was 24 mm x 35 mm, and the throat length varied from 63 to 140 mm. Liquid was injected through a single orifice (1.0 mm diameter) on the throat wall. This arrangement allowed the study of the influence of jet penetration on droplet distribution. Gas velocity at the throat was 58.3 and 74.6 m/s, and the liquid flow rate was 286, 559 and 853 ml/min. A probe with a 2.7 mm internal diameter was used to isokinetically remove liquid from several positions inside the equipment. It was possible to study liquid distribution close to the injection point. A new model for droplet dispersion, which incorporates the new description of the jet atomization process developed by the present authors in the first article of this series, is proposed and evaluated. The model predicted well the experimental data.

  15. Investigation of flow dynamics of liquid phase in a pilot-scale trickle bed reactor using radiotracer technique

    International Nuclear Information System (INIS)

    Pant, H.J.; Sharma, V.K.

    2016-01-01

    A radiotracer investigation was carried out to measure residence time distribution (RTD) of liquid phase in a trickle bed reactor (TBR). The main objectives of the investigation were to investigate radial and axial mixing of the liquid phase, and evaluate performance of the liquid distributor/redistributor at different operating conditions. Mean residence times (MRTs), holdups (H) and fraction of flow flowing along different quadrants were estimated. The analysis of the measured RTD curves indicated radial non-uniform distribution of liquid phase across the beds. The overall RTD of the liquid phase, measured at the exit of the reactor was simulated using a multi-parameter axial dispersion with exchange model (ADEM), and model parameters were obtained. The results of model simulations indicated that the TBR behaved as a plug flow reactor at most of the operating conditions used in the investigation. The results of the investigation helped to improve the existing design as well as to design a full-scale industrial TBR for petroleum refining applications. - Highlights: • Residence time distributions of liquid phase were measured in a trickle bed reactor. • Bromine-82 as ammonium bromide was used as a radiotracer. • Mean residence times, holdups and radial distribution of liquid phase were quantified. • Axial dispersion with exchange model was used to simulate the measured data. • The trickle bed reactor behaved as a plug flow reactor.

  16. Use of Dispersive Liquid-Liquid Microextraction and UV-Vis Spectrophotometry for the Determination of Cadmium in Water Samples

    Directory of Open Access Journals (Sweden)

    J. Pérez-Outeiral

    2014-01-01

    Full Text Available A simple and inexpensive method for cadmium determination in water using dispersive liquid-liquid microextraction and ultraviolet-visible spectrophotometry was developed. In order to obtain the best experimental conditions, experimental design was applied. Calibration was made in the range of 10–100 μg/L, obtaining good linearity (R2 = 0.9947. The obtained limit of detection based on calibration curve was 8.5 μg/L. Intra- and interday repeatability were checked at two levels, obtaining relative standard deviation values from 9.0 to 13.3%. The enrichment factor had a value of 73. Metal interferences were also checked and tolerable limits were evaluated. Finally, the method was applied to cadmium determination in real spiked water samples. Therefore, the method showed potential applicability for cadmium determination in highly contaminated liquid samples.

  17. 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.

  18. 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.

  19. 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

  20. 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.

  1. Effervescence-assisted dispersive liquid-liquid microextraction using a solid effervescent agent as a novel dispersion technique for the analysis of fungicides in apple juice.

    Science.gov (United States)

    Jiang, Wenqing; Chen, Xiaochu; Liu, Fengmao; You, Xiangwei; Xue, Jiaying

    2014-11-01

    A novel effervescence-assisted dispersive liquid-liquid microextraction method has been developed for the determination of four fungicides in apple juice samples. In this method, a solid effervescent agent is added into samples to assist the dispersion of extraction solvent. The effervescent agent is environmentally friendly and only produces an increase in the ionic strength and a negligible variation in the pH value of the aqueous sample, which does not interfere with the extraction of the analytes. The parameters affecting the extraction efficiency were investigated including the composition of effervescent agent, effervescent agent amount, formulation of effervescent agent, adding mode of effervescent agent, type and volume of extraction solvent, and pH. Under optimized conditions, the method showed a good linearity within the range of 0.05-2 mg/L for pyrimethanil, fludioxonil, and cyprodinil, and 0.1-4 mg/L for kresoxim-methyl, with the correlation coefficients >0.998. The limits of detection for the method ranged between 0.005 and 0.01 mg/L. The recoveries of the target fungicides in apple juice samples were in the range of 72.4-110.8% with the relative standard deviations ranging from 1.2 to 6.8%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Comparing two tetraalkylammonium ionic liquids. I. Liquid phase structure

    Energy Technology Data Exchange (ETDEWEB)

    Lima, Thamires A.; Paschoal, Vitor H.; Faria, Luiz F. O.; Ribeiro, Mauro C. C., E-mail: mccribei@iq.usp.br [Laboratório de Espectroscopia Molecular, Departamento de Química Fundamental, Instituto de Química, Universidade de São Paulo, CP 26077, CEP 05513-970 São Paulo, SP (Brazil); Giles, Carlos [Departamento de Física da Matéria Condensada, Instituto de Física Gleb Wataghin, Universidade Estadual de Campinas, 13083-859 Campinas, SP (Brazil)

    2016-06-14

    X-ray scattering experiments at room temperature were performed for the ionic liquids n-butyl-trimethylammonium bis(trifluoromethanesulfonyl)imide, [N{sub 1114}][NTf{sub 2}], and methyl-tributylammonium bis(trifluoromethanesulfonyl)imide, [N{sub 1444}][NTf{sub 2}]. The peak in the diffraction data characteristic of charge ordering in [N{sub 1444}][NTf{sub 2}] is shifted to longer distances in comparison to [N{sub 1114}][NTf{sub 2}], but the peak characteristic of short-range correlations is shifted in [N{sub 1444}][NTf{sub 2}] to shorter distances. Molecular dynamics (MD) simulations were performed for these ionic liquids using force fields available from the literature, although with new sets of partial charges for [N{sub 1114}]{sup +} and [N{sub 1444}]{sup +} proposed in this work. The shifting of charge and adjacency peaks to opposite directions in these ionic liquids was found in the static structure factor, S(k), calculated by MD simulations. Despite differences in cation sizes, the MD simulations unravel that anions are allowed as close to [N{sub 1444}]{sup +} as to [N{sub 1114}]{sup +} because anions are located in between the angle formed by the butyl chains. The more asymmetric molecular structure of the [N{sub 1114}]{sup +} cation implies differences in partial structure factors calculated for atoms belonging to polar or non-polar parts of [N{sub 1114}][NTf{sub 2}], whereas polar and non-polar structure factors are essentially the same in [N{sub 1444}][NTf{sub 2}]. Results of this work shed light on controversies in the literature on the liquid structure of tetraalkylammonium based ionic liquids.

  3. Introducing a new and rapid microextraction approach based on magnetic ionic liquids: Stir bar dispersive liquid microextraction.

    Science.gov (United States)

    Chisvert, Alberto; Benedé, Juan L; Anderson, Jared L; Pierson, Stephen A; Salvador, Amparo

    2017-08-29

    With the aim of contributing to the development and improvement of microextraction techniques, a novel approach combining the principles and advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) is presented. This new approach, termed stir bar dispersive liquid microextraction (SBDLME), involves the addition of a magnetic ionic liquid (MIL) and a neodymium-core magnetic stir bar into the sample allowing the MIL coat the stir bar due to physical forces (i.e., magnetism). As long as the stirring rate is maintained at low speed, the MIL resists rotational (centrifugal) forces and remains on the stir bar surface in a manner closely resembling SBSE. By increasing the stirring rate, the rotational forces surpass the magnetic field and the MIL disperses into the sample solution in a similar manner to DLLME. After extraction, the stirring is stopped and the MIL returns to the stir bar without the requirement of an additional external magnetic field. The MIL-coated stir bar containing the preconcentrated analytes is thermally desorbed directly into a gas chromatographic system coupled to a mass spectrometric detector (TD-GC-MS). This novel approach opens new insights into the microextraction field, by using the benefits provided by SBSE and DLLME simultaneously, such as automated thermal desorption and high surface contact area, respectively, but most importantly, it enables the use of tailor-made solvents (i.e., MILs). To prove its utility, SBDLME has been used in the extraction of lipophilic organic UV filters from environmental water samples as model analytical application with excellent analytical features in terms of linearity, enrichment factors (67-791), limits of detection (low ng L -1 ), intra- and inter-day repeatability (RSD<15%) and relative recoveries (87-113%, 91-117% and 89-115% for river, sea and swimming pool water samples, respectively). Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Air-assisted dispersive liquid-liquid microextraction based on a new hydrophobic deep eutectic solvent for the preconcentration of benzophenone-type UV filters from aqueous samples.

    Science.gov (United States)

    Ge, Dandan; Zhang, Yi; Dai, Yixiu; Yang, Shumin

    2018-04-01

    Deep eutectic solvents are considered as new and green solvents that can be widely used in analytical chemistry such as microextraction. In the present work, a new dl-menthol-based hydrophobic deep eutectic solvent was synthesized and used as extraction solvents in an air-assisted dispersive liquid-liquid microextraction method for preconcentration and extraction of benzophenone-type UV filters from aqueous samples followed by high-performance liquid chromatography with diode array detection. In an experiment, the deep eutectic solvent formed by dl-menthol and decanoic acid was added to an aqueous solution containing the UV filters, and then the mixture was sucked up and injected five times by using a glass syringe, and a cloudy state was achieved. After extraction, the solution was centrifuged and the upper phase was subjected to high-performance liquid chromatography for analysis. Various parameters such as the type and volume of the deep eutectic solvent, number of pulling, and pushing cycles, solution pH and salt concentration were investigated and optimized. Under the optimum conditions, the developed method exhibited low limits of detection and limits of quantitation, good linearity, and precision. Finally, the proposed method was successfully applied to determine the benzophenone-type filters in environmental water samples with relative recoveries of 88.8-105.9%. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Nanocomposites with Liquid-Like Multiwalled Carbon Nanotubes Dispersed in Epoxy Resin without Solvent Process

    Directory of Open Access Journals (Sweden)

    Xi Zhang

    2014-01-01

    Full Text Available Liquid-like multiwall carbon nanotubes (MWNTs were prepared with as-received carboxylic MWNTs-COOH and poly(ethylene oxide-block-poly(propylene oxide-block-poly(ethylene oxide (PEO-b-PPO-b-PEO through hydrogen bonding. The sample has liquid-like behavior above 58°C. The MWNTs content is 26.6 wt%. The liquid-like MWNTs nanofluids were incorporated into epoxy matrix with solvent-free process and dispersed well. When the liquid-like MWNTs nanofluids content is up to 1 wt%, the impact toughness of the nanocomposite is 153% higher than the pure epoxy matrix.

  6. 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

  7. Thermodynamic and kinetic simulation of transient liquid-phase bonding

    Science.gov (United States)

    Lindner, Brad

    The use of numeric computational methods for the simulation of materials systems is becoming more prevalent and an understanding of these tools may soon be a necessity for Materials Engineers and Scientists. The applicability of numerical simulation methods to transient liquid-phase (TLP) bonding is evaluated using a type 316L/MBF-51 material system. The comparisons involve the calculation of bulk diffusivities, tracking of interface positions during dissolution, widening, and isothermal solidification stages, as well as comparison of elemental composition profiles. The simulations were performed with Thermo-Calc and DICTRA software packages and the experiments with differential scanning calorimetry (DSC), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and optical microscopic methods. Analytical methods are also discussed to enhance understanding. The results of the investigation show that while general agreement between simulations and experiments can be obtained, assumptions made with the simulation programs may cause difficulty in interpretation of the results unless the user has sufficient, mathematical, thermodynamic, kinetic, and simulation background.

  8. Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry

    Science.gov (United States)

    2016-01-01

    Levetiracetam (LEV) is an antiepileptic drug that is clinically effective in generalized and partial epilepsy syndromes. The use of this drug has been increasing in clinical practice and intra- or -interindividual variability has been exhibited for special population. For this reason, bioanalytical methods are required for drug monitoring in biological matrices. So this work presents a dispersive liquid-liquid microextraction method followed by gas chromatography-mass spectrometry (DLLME-GC-MS) for LEV quantification in human plasma. However, due to the matrix complexity a previous purification step is required. Unlike other pretreatment techniques presented in the literature, for the first time, a procedure employing ultrafiltration tubes Amicon® (10 kDa porous size) without organic solvent consumption was developed. GC-MS analyses were carried out using a linear temperature program, capillary fused silica column, and helium as the carrier gas. DLLME optimized parameters were type and volume of extraction and dispersing solvents, salt addition, and vortex agitation time. Under chosen parameters (extraction solvent: chloroform, 130 μL; dispersing solvent: isopropyl alcohol, 400 μL; no salt addition and no vortex agitation time), the method was completely validated and all parameters were in agreement with the literature recommendations. LEV was quantified in patient's plasma sample using less than 550 μL of organic solvent. PMID:27830105

  9. Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Greyce Kelly Steinhorst Alcantara

    2016-01-01

    Full Text Available Levetiracetam (LEV is an antiepileptic drug that is clinically effective in generalized and partial epilepsy syndromes. The use of this drug has been increasing in clinical practice and intra- or -interindividual variability has been exhibited for special population. For this reason, bioanalytical methods are required for drug monitoring in biological matrices. So this work presents a dispersive liquid-liquid microextraction method followed by gas chromatography-mass spectrometry (DLLME-GC-MS for LEV quantification in human plasma. However, due to the matrix complexity a previous purification step is required. Unlike other pretreatment techniques presented in the literature, for the first time, a procedure employing ultrafiltration tubes Amicon® (10 kDa porous size without organic solvent consumption was developed. GC-MS analyses were carried out using a linear temperature program, capillary fused silica column, and helium as the carrier gas. DLLME optimized parameters were type and volume of extraction and dispersing solvents, salt addition, and vortex agitation time. Under chosen parameters (extraction solvent: chloroform, 130 μL; dispersing solvent: isopropyl alcohol, 400 μL; no salt addition and no vortex agitation time, the method was completely validated and all parameters were in agreement with the literature recommendations. LEV was quantified in patient’s plasma sample using less than 550 μL of organic solvent.

  10. 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)

  11. Measurements of liquid-phase turbulence in gas–liquid two-phase flows using particle image velocimetry

    International Nuclear Information System (INIS)

    Zhou, Xinquan; Doup, Benjamin; Sun, Xiaodong

    2013-01-01

    Liquid-phase turbulence measurements were performed in an air–water two-phase flow loop with a circular test section of 50 mm inner diameter using a particle image velocimetry (PIV) system. An optical phase separation method-–planar laser-induced fluorescence (PLIF) technique—which uses fluorescent particles and an optical filtration technique, was employed to separate the signals of the fluorescent seeding particles from those due to bubbles and other noises. An image pre-processing scheme was applied to the raw PIV images to remove the noise residuals that are not removed by the PLIF technique. In addition, four-sensor conductivity probes were adopted to measure the radial distribution of the void fraction. Two benchmark tests were performed: the first was a comparison of the PIV measurement results with those of similar flow conditions using thermal anemometry from previous studies; the second quantitatively compared the superficial liquid velocities calculated from the local liquid velocity and void fraction measurements with the global liquid flow rate measurements. The differences of the superficial liquid velocity obtained from the two measurements were bounded within ±7% for single-phase flows and two-phase bubbly flows with the area-average void fraction up to 18%. Furthermore, a preliminary uncertainty analysis was conducted to investigate the accuracy of the two-phase PIV measurements. The systematic uncertainties due to the circular pipe curvature effects, bubble surface reflection effects and other potential uncertainty sources of the PIV measurements were discussed. The purpose of this work is to facilitate the development of a measurement technique (PIV-PLIF) combined with image pre-processing for the liquid-phase turbulence in gas–liquid two-phase flows of relatively high void fractions. The high-resolution data set can be used to more thoroughly understand two-phase flow behavior, develop liquid-phase turbulence models, and assess high

  12. Ionic Liquid Epoxy Composite Cryotanks, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — The objective of this work is to determine the optimal process for manufacturing lightweight linerless cryogenic storage tanks using ionic liquid epoxy composite...

  13. 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.

  14. Small-angle light scattering symmetry breaking in polymer-dispersed liquid crystal films with inhomogeneous electrically controlled interface anchoring

    Energy Technology Data Exchange (ETDEWEB)

    Loiko, V. A., E-mail: loiko@ifanbel.bas-net.by; Konkolovich, A. V. [National Academy of Sciences of Belarus, Stepanov Institute of Physics (Belarus); Zyryanov, V. Ya. [Russian Academy of Sciences, Kirensky Institute of Physics, Federal Research Center “Krasnoyarsk Scientific Center,” Siberian Branch (Russian Federation); Miskevich, A. A. [National Academy of Sciences of Belarus, Stepanov Institute of Physics (Belarus)

    2017-03-15

    We have described the method of analyzing and reporting on the results of calculation of the small-angle structure of radiation scattered by a polymer-dispersed liquid crystal film with electrically controlled interfacial anchoring. The method is based on the interference approximation of the wave scattering theory and the hard disk model. Scattering from an individual liquid crystal droplet has been described using the anomalous diffraction approximation extended to the case of droplets with uniform and nonuniform interface anchoring at the droplet–polymer boundary. The director field structure in an individual droplet is determined from the solution of the problem of minimizing the volume density of the free energy. The electrooptical effect of symmetry breaking in the angular distribution of scattered radiation has been analyzed. This effect means that the intensities of radiation scattered within angles +θ{sub s} and–θ{sub s} relative to the direction of illumination in the scattering plane can be different. The effect is of the interference origin and is associated with asymmetry of the phase shift of the wavefront of an incident wave from individual parts of the droplet, which appears due to asymmetry of the director field structure in the droplet, caused by nonuniform anchoring of liquid crystal molecules with the polymer on its surface. This effect is analyzed in the case of normal illumination of the film depending on the interfacial anchoring at the liquid crystal–polymer interface, the orientation of the optical axes of droplets, their concentration, sizes, anisometry, and polydispersity.

  15. Determination of ten pyrethroids in various fruit juices: comparison of dispersive liquid-liquid microextraction sample preparation and QuEChERS method combined with dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Zhang, Yaohai; Zhang, Xuelian; Jiao, Bining

    2014-09-15

    Dispersive liquid-liquid microextraction (DLLME) sample preparation and the quick, easy, cheap, effective, rugged and safe (QuEChERS) method combined with DLLME were developed and compared for the analysis of ten pyrethroids in various fruit juices using gas chromatography-electron capture detection (GC-ECD). QuEChERS-DLLME method has found its widespread applications to all the fruit juices including those samples with more complex matrices (orange, lemon, kiwi and mango) while DLLME was confined to the fruit juices with simpler matrices (apple, pear, grape and peach). The two methods provided acceptable recoveries and repeatability. In addition, the applicabilities of two methods were demonstrated with the real samples and further confirmed by gas chromatography-mass spectrometry (GC-MS). Copyright © 2014. Published by Elsevier Ltd.

  16. Dispersive liquid-liquid microextraction for simultaneous determination of cadmium, cobalt, lead and nickel in water samples by inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Dos Santos Silva, E.; Correia, L.O.; Dos Santos, L.O.; Dos Santos Vieira, E.V.; Lemos, V.A.

    2012-01-01

    We report on a new method for the dispersive liquid-liquid microextraction of Cd(II), Co(II), Pb(II) and Ni (II) from water samples prior to their simultaneous determination by inductively coupled plasma optical emission spectrometry (ICP-OES). The procedure is based on the injection of a ternary solvent system composed of appropriate quantities of extraction solvent (trichloroethylene), dispersive solvent (ethanol), and the chelating reagent 2-(2'-benzothiazolylazo)-p-cresol into the sample solution. The solution turns turbid immediately after injection, and the analytes are extracted into the droplets of the organic phase which was dried and dissolved in a mixture of Triton X-114, nitric acid, and ethanol. The metal ions in this mixture were quantified by ICP-OES. The detection limits under optimized conditions are 0.2, 0.3, 0.2 and 0.7 μg L -1 for Cd(II), Co(II), Pb(II) and Ni(II), respectively. The enrichment factors were also calculated for Cd (13), Co (11), Pb (11) and Ni (8). The procedure was applied to the determination of cadmium, cobalt, lead and nickel in certified reference material (waterway sediment) and water samples. (author)

  17. Simultaneous derivatisation and preconcentration of parabens in food and other matrices by isobutyl chloroformate and dispersive liquid-liquid microextraction followed by gas chromatographic analysis.

    Science.gov (United States)

    Jain, Rajeev; Mudiam, Mohana Krishna Reddy; Chauhan, Abhishek; Ch, Ratnasekhar; Murthy, R C; Khan, Haider A

    2013-11-01

    A simple, rapid and economical method has been proposed for the quantitative determination of parabens (methyl, ethyl, propyl and butyl paraben) in different samples (food, cosmetics and water) based on isobutyl chloroformate (IBCF) derivatisation and preconcentration using dispersive liquid-liquid microextraction in single step. Under optimum conditions, solid samples were extracted with ethanol (disperser solvent) and 200 μL of this extract along with 50 μL of chloroform (extraction solvent) and 10 μL of IBCF was rapidly injected into 2 mL of ultra-pure water containing 150 μL of pyridine to induce formation of a cloudy state. After centrifugation, 1 μL of the sedimented phase was analysed using gas chromatograph-flame ionisation detector (GC-FID) and the peaks were confirmed using gas chromatograph-positive chemical ionisation-mass spectrometer (GC-PCI-MS). Method was found to be linear over the range of 0.1-10 μg mL(-1) with square of correlation coefficient (R(2)) in the range of 0.9913-0.9992. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.029-0.102 μg mL(-1) and 0.095-0.336 μg mL(-1) with a signal to noise ratio of 3:1 and 10:1, respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

  18. Dynamic Time Multiplexing Fabrication of Holographic Polymer Dispersed Liquid Crystals for Increased Wavelength Sensitivity

    Science.gov (United States)

    Fontecchio, Adam K. (Inventor); Rai, Kashma (Inventor)

    2017-01-01

    Described herein is a new holographic polymer dispersed liquid crystal (HPDLC) medium with broadband reflective properties, and a new technique for fabrication of broadband HPDLC mediums. The new technique involves dynamic variation of the holography setup during HPDLC formation, enabling the broadening of the HPDLC medium's wavelength response. Dynamic variation of the holography setup may include the rotation and/or translation of one or more motorized stages, allowing for time and spatial, or angular, multiplexing through variation of the incident angles of one or more laser beams on a pre-polymer mixture during manufacture. An HPDLC medium manufactured using these techniques exhibits improved optical response by reflecting a broadband spectrum of wavelengths. A new broadband holographic polymer dispersed liquid crystal thin film polymeric mirror stack with electrically-switchable beam steering capability is disclosed. XXXX Described herein is a new holographic polymer dispersed liquid crystal (HPDLC) medium with broadband reflective properties, and a new technique for fabrication of broadband 10 HPDLC mediums. The new technique involves dynamic variation of the holography setup during HPDLC formation, enabling the broadening of the HPDLC medium's wavelength response. Dynamic variation of the holography setup may include the rotation and/or translation of one or more 15 motorized stages, allowing for time and spatial, or angular, multiplexing through variation of the incident angles of one or more laser beams on a pre-polymer mixture during manufacture. An HPDLC medium manufactured using these techniques exhibits improved optical response by reflecting 20 a broadband spectrum of wavelengths. A new broadband holographic polymer dispersed liquid crystal thin film polymeric mirror stack with electrically switchable beam steering capability is disclosed.

  19. Frequency and Temperature Dependence of Fabrication Parameters in Polymer Dispersed Liquid Crystal Devices

    Science.gov (United States)

    Torres, Juan C.; Vergaz, Ricardo; Barrios, David; Sánchez-Pena, José Manuel; Viñuales, Ana; Grande, Hans Jürgen; Cabañero, Germán

    2014-01-01

    A series of polymer dispersed liquid crystal devices using glass substrates have been fabricated and investigated focusing on their electrical properties. The devices have been studied in terms of impedance as a function of frequency. An electric equivalent circuit has been proposed, including the influence of the temperature on the elements into it. In addition, a relevant effect of temperature on electrical measurements has been observed. PMID:28788632

  20. Frequency and Temperature Dependence of Fabrication Parameters in Polymer Dispersed Liquid Crystal Devices

    Directory of Open Access Journals (Sweden)

    Juan C. Torres

    2014-05-01

    Full Text Available A series of polymer dispersed liquid crystal devices using glass substrates have been fabricated and investigated focusing on their electrical properties. The devices have been studied in terms of impedance as a function of frequency. An electric equivalent circuit has been proposed, including the influence of the temperature on the elements into it. In addition, a relevant effect of temperature on electrical measurements has been observed.

  1. Dispersion forces and small-angle neutron scattering from liquid noble metals

    International Nuclear Information System (INIS)

    March, N.H.

    1988-01-01

    Maggs and Ashcroft [Phys. Rev. letts., 59,113 (1987)] have re-opened the question of the analogy between the cohesion of a molecular crystal, in which dispersion forces play a major role, and that in a metal crystal with polarizable ion cores. It is pointed out that small-angle neutron scattering from liquid noble metals could be used to test their predictions. (author)

  2. Application of microwave irradiation to organic liquid phase reactions

    International Nuclear Information System (INIS)

    Huang Kun; Liu Hua; Ji Xuelin

    1994-01-01

    Microwave irradiation has been used in organic liquid phase reactions to significantly reduce the reaction time and improve the yield. The proposed mechanism, the development of techniques and reactions, such as Diels-Alder, ene, rearrangement reactions etc., are discussed

  3. Structure factors and phonon dispersion in liquid Li0.61Na0.39 alloy

    International Nuclear Information System (INIS)

    Pratap, Arun; Lad, Kirit N.; Raval, K.G.

    2004-01-01

    The phonon spectra for liquid Li and Na have been computed through the phenomenological model of Bhatia and Singh for disordered systems like liquids and glasses and the obtained results have been compared with the available data obtained by inelastic neutron scattering (INS) and inelastic X-ray scattering (IXS) experiments. The effective pair potentials and their space derivatives are important ingredients in the computation of the dispersion curves. The pair potentials are obtained using the pseudo-potential theory. The empty core model proposed by Ashcroft is widely used for pseudo-potential calculations for alkali metals. But, it is thought to be unsuitable for Li because of its simple 1s electronic structure. However, it can be used with an additional term known as Born-Mayer (BM) core term. The influence of the BM core term on the phonon dispersion is discussed. The same pseudo-potential formalism has been employed to obtain the dispersion relation in liquid Li 0.61 Na 0.39 alloy. Apart from the phonon spectra, the Ashcroft-Langreth structure factors in the alloy are derived in the Percus-Yevick approximation. (author)

  4. Experimental and theoretical investigation of droplet dispersion in venturi scrubbers with axial liquid injection

    Energy Technology Data Exchange (ETDEWEB)

    Mokhtarian, N.; Talaei, A.; Karimikhosroabadi, M. [Islamic Azad University, Shahreza Branch, Shahreza (Iran); Sadeghi, F. [Chemical Engineering Department, University of Isfahan, Isfahan (Iran); Talaie, M.R.

    2009-05-15

    Droplet dispersion in a Venturi scrubber with axial liquid injection was investigated both experimentally and theoretically. The main objective of this study was to develop a mathematical model to predict droplet dispersion in a Venturi scrubber with axial liquid injection. The effects of the Peclet number and droplet size distribution on droplet dispersion were studied using the developed model. Sampling of the droplets was carried out, isokinetically, in 16 positions at the end of the throat section. The experimental data were used to find the parameters of the developed model, such as the Peclet number. From the results of this study, it was found that the Peclet number was not constant across the cross section of the scrubber channel. In order to achieve a better agreement between the results of the model and the experimental data, it was required to consider Peclet number variations across the Venturi channel. It was also revealed that the parameter representing the width of the Rosin-Rammler distribution of droplet size could not be considered constant and it was influenced significantly by the operating parameters such as liquid flow rate and gas velocity. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

  5. Going full circle: phase-transition thermodynamics of ionic liquids.

    Science.gov (United States)

    Preiss, Ulrich; Verevkin, Sergey P; Koslowski, Thorsten; Krossing, Ingo

    2011-05-27

    We present the full enthalpic phase transition cycle for ionic liquids (ILs) as examples of non-classical salts. The cycle was closed for the lattice, solvation, dissociation, and vaporization enthalpies of 30 different ILs, relying on as much experimental data as was available. High-quality dissociation enthalpies were calculated at the G3 MP2 level. From the cycle, we could establish, for the first time, the lattice and solvation enthalpies of ILs with imidazolium ions. For vaporization, lattice, and dissociation enthalpies, we also developed new prediction methods in the course of our investigations. Here, as only single-ion values need to be calculated and the tedious optimization of an ion pair can be circumvented, the computational time is short. For the vaporization enthalpy, a very simple approach was found, using a surface term and the calculated enthalpic correction to the total gas-phase energy. For the lattice enthalpy, the most important constituent proved to be the calculated conductor-like screening model (COSMO) solvation enthalpy in the ideal electric conductor. A similar model was developed for the dissociation enthalpy. According to our assessment, the typical error of the lattice enthalpy would be 9.4 kJ mol(-1), which is less than half the deviation we get when using the (optimized) Kapustinskii equation or the recent volume-based thermodynamics (VBT) theory. In contrast, the non-optimized VBT formula gives lattice enthalpies 20 to 140 kJ mol(-1) lower than the ones we assessed in the cycle, because of the insufficient description of dispersive interactions. Our findings show that quantum-chemical calculations can greatly improve the VBT approaches, which were parameterized for simple, inorganic salts with ideally point-shaped charges. In conclusion, we suggest the term "augmented VBT", or "aVBT", to describe this kind of theoretical approach. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Vortex-assisted magnetic β-cyclodextrin/attapulgite-linked ionic liquid dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography for the fast determination of four fungicides in water samples.

    Science.gov (United States)

    Yang, Miyi; Xi, Xuefei; Wu, Xiaoling; Lu, Runhua; Zhou, Wenfeng; Zhang, Sanbing; Gao, Haixiang

    2015-02-13

    A novel microextraction technique combining magnetic solid-phase microextraction (MSPME) with ionic liquid dispersive liquid-liquid microextraction (IL-DLLME) to determine four fungicides is presented in this work for the first time. The main factors affecting the extraction efficiency were optimized by the one-factor-at-a-time approach and the impacts of these factors were studied by an orthogonal design. Without tedious clean-up procedure, analytes were extracted from the sample to the adsorbent and organic solvent and then desorbed in acetonitrile prior to chromatographic analysis. Under the optimum conditions, good linearity and high enrichment factors were obtained for all analytes, with correlation coefficients ranging from 0.9998 to 1.0000 and enrichment factors ranging 135 and 159 folds. The recoveries for proposed approach were between 98% and 115%, the limits of detection were between 0.02 and 0.04 μg L(-1) and the RSDs changed from 2.96 to 4.16. The method was successfully applied in the analysis of four fungicides (azoxystrobin, chlorothalonil, cyprodinil and trifloxystrobin) in environmental water samples. The recoveries for the real water samples ranged between 81% and 109%. The procedure proved to be a time-saving, environmentally friendly, and efficient analytical technique. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Interfacial tension-induced transport of nonaqueous phase liquids in model aquifer systems

    International Nuclear Information System (INIS)

    Anderson, M.A.

    1994-01-01

    Nonaqueous phase liquids (NAPLs) such as organic solvents and fuel are common contaminants in soils and groundwater. Spills, leaking underground storage tanks, and improper disposal practices all result in the release and movement of NAPLs through soils. Movement of NAPLs through soil is considered to result from gravity- and /or capillarity-driven immiscible phase flow. Dispersive and convective transport of dissolved components, volatilization, sorption, and degradation are also considered important processes in NAPL contamination. An additional transport mechanism in which NAPLs spread on water surfaces due to differential adhesive and cohesive attractive forces is demonstrated in this study. 22 refs., 5 figs., 1 tab

  8. 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)

  9. Ionic Liquid-Modified Thermosets and Their Nanocomposites: Dispersion, Exfoliation, Degradation, and Cure

    Science.gov (United States)

    Throckmorton, James A.

    This dissertation explores the application of a room temperature ionic liquid (RTIL) to problems in the chemistry, processing, and modification of thermosetting polymers. In particular, the solution properties and reaction chemistry of 1-ethyl-3-methyl imidazolium dicyanamide (EMIM-DCN) are applied to problems of nanoparticle dispersion and processing, graphite exfoliation, cyanate ester (CE) cure, and the environmental degradation of CEs. Nanoparticle Dispersion: Nanocomposite processing can be simplified by using the same compound as both a nanoparticle solvent and an initiator for polymerization. This dual-function molecule can be designed both for solvent potential and reaction chemistry. EMIM-DCN, previously shown by our lab to act as an epoxy initiator, is used in the synthesis of silica and acid expanded graphite composites. These composites are then characterized for particle dispersion and physical properties. Individual particle dispersion of silica nanocomposites is shown, and silica nanocomposites at low loading show individual particle dispersion and improved modulus and fracture toughness. GNP nanocomposites show a 70% increase in modulus along with a 10-order of magnitude increase in electrical conductivity at 6.5 vol%, and an electrical percolation threshold of 1.7 vol%. Direct Graphite Exfoliation By Laminar Shear: This work presents a laminar-shear alternative to chemical processing and chaotic flow-fields for the direct exfoliation of graphite and the single-pot preparation of nanocomposites. Additionally, we develop the theory of laminar flow through a 3-roll mill, and apply that theory to the latest developments in the theory of graphite interlayer shear. The resulting nanocomposite shows low electrical percolation (0.5 vol%) and low thickness (1-3 layer) graphite/graphene flakes. Additionally, the effect of processing conditions by rheometry and comparison with solvent-free conditions reveal the interactions between processing and matrix

  10. The liquid to vapor phase transition in excited nuclei

    Energy Technology Data Exchange (ETDEWEB)

    Elliott, J.B.; Moretto, L.G.; Phair, L.; Wozniak, G.J.; Beaulieu, L.; Breuer, H.; Korteling, R.G.; Kwiatkowski, K.; Lefort, T.; Pienkowski, L.; Ruangma, A.; Viola, V.E.; Yennello, S.J.

    2001-05-08

    For many years it has been speculated that excited nuclei would undergo a liquid to vapor phase transition. For even longer, it has been known that clusterization in a vapor carries direct information on the liquid-vapor equilibrium according to Fisher's droplet model. Now the thermal component of the 8 GeV/c pion + 197 Au multifragmentation data of the ISiS Collaboration is shown to follow the scaling predicted by Fisher's model, thus providing the strongest evidence yet of the liquid to vapor phase transition.

  11. ANALYSIS OF BASIC PSYCHOTROPIC DRUGS IN BIOLOGICAL FLUIDS AND TISSUES BY REVERSED-PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY.

    Science.gov (United States)

    Petruczynik, Anna; Waksmundzka-Hajnos, Monika

    2017-03-01

    The review of the RP HPLC analysis of basic psychotropic drugs is presented. It contains sample preparation methods with centrifugation, protein precipitation, liquid-liquid extraction (LLE), dispersive liquid-liquid microextraction (DLLME), solid-phase extraction (SPE), solid-phase microextraction (SPME), microwave-assisted extraction (MAE) and RP-HPLC analysis. Chromatographic behavior of basic drugs in aqueous media - eluents used in reversed phase systems is discussed. Methods of blocking of residue surface silanols' interaction are mentioned. Analytical methods used for the analysis are divided into parts according with the above methods: the use of low-pH eluents, the use of high-pH eluents, the use of silanol blockers, special stationary phases for basic analytes. Literature connected with the sample preparation methods and analytical systems for the drug analysis are cited in details and presented also in Table 1.

  12. 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.

  13. Simultaneous determination of atorvastatin and valsartan in human plasma by solid-based disperser liquid-liquid microextraction followed by high-performance liquid chromatography-diode array detection.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Khorram, Parisa; Pazhohan, Azar

    2016-04-01

    A simple, sensitive, and efficient method has been developed for simultaneous estimation of valsartan and atorvastatin in human plasma by combination of solid-based dispersive liquid-liquid microextraction and high performance liquid chromatography-diode array detection. In the proposed method, 1,2-dibromoethane (extraction solvent) is added on a sugar cube (as a solid disperser) and it is introduced into plasma sample containing the analytes. After manual shaking and centrifugation, the resultant sedimented phase is subjected to back extraction into a small volume of sodium hydrogen carbonate solution using air-assisted liquid-liquid microextraction. Then the cloudy solution is centrifuged and the obtained aqueous phase is transferred into a microtube and analyzed by the separation system. Under the optimal conditions, extraction recoveries are obtained in the range of 81-90%. Calibration curves plotted in drug-free plasma sample are linear in the ranges of 5-5000μgL(-1) for valsartan and 10-5000μgL(-1) for atorvastatin with the coefficients of determination higher than 0.997. Limits of detection and quantification of the studied analytes in plasma sample are 0.30-2.6 and 1.0-8.2μgL(-1), respectively. Intra-day (n=6) and inter-days (n=4) precisions of the method are satisfactory with relative standard deviations less than 7.4% (at three levels of 10, 500, and 2000μgL(-1), each analyte). These data suggest that the method can be successfully applied to determine trace amounts of valsartan and atorvastatin in human plasma samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Highly Selective Continuous Gas-Phase Methoxycarbonylation of Ethylene with Supported Ionic Liquid Phase (SILP) Catalysts

    DEFF Research Database (Denmark)

    Khokarale, Santosh Govind; Garcia Suárez, Eduardo José; Fehrmann, Rasmus

    2017-01-01

    Supported ionic liquid phase (SILP) technology was applied for the first time to the Pd-catalyzed continuous, gas-phase methoxycarbonylation of ethylene to selectively produce methyl propanoate (MP) in high yields. The influence of catalyst and reaction parameters such as, for example, ionic liquid...

  15. Liquid-Liquid Phase Transition and Glass Transition in a Monoatomic Model System

    Directory of Open Access Journals (Sweden)

    Nicolas Giovambattista

    2010-12-01

    Full Text Available We review our recent study on the polyamorphism of the liquid and glass states in a monatomic system, a two-scale spherical-symmetric Jagla model with both attractive and repulsive interactions. This potential with a parametrization for which crystallization can be avoided and both the glass transition and the liquid-liquid phase transition are clearly separated, displays water-like anomalies as well as polyamorphism in both liquid and glassy states, providing a unique opportunity to study the interplay between the liquid-liquid phase transition and the glass transition. Our study on a simple model may be useful in understanding recent studies of polyamorphism in metallic glasses.

  16. Hierarchical opal grating films prepared by slide coating of colloidal dispersions in binary liquid media.

    Science.gov (United States)

    Lee, Wonmok; Kim, Seulgi; Kim, Seulki; Kim, Jin-Ho; Lee, Hyunjung

    2015-02-15

    There are active researches on well ordered opal films due to their possible applications to various photonic devices. A recently developed slide coating method is capable of rapid fabrication of large area opal films from aqueous colloidal dispersion. In the current study, the slide coating of polystyrene colloidal dispersions in water/i-propanol (IPA) binary media is investigated. Under high IPA content in a dispersing medium, resulting opal film showed a deterioration of long range order, as well as a decreased film thickness due to dilution effect. From the binary liquid, the dried opal films exhibited the unprecedented topological groove patterns with varying periodic distances as a function of alcohol contents in the media. The groove patterns were consisted of the hierarchical structures of the terraced opal layers with periodic thickness variations. The origin of the groove patterns was attributed to a shear-induced periodic instability of colloidal concentration within a thin channel during the coating process which was directly converted to a groove patterns in a resulting opal film due to rapid evaporation of liquid. The groove periods of opal films were in the range of 50-500 μm, and the thickness differences between peak and valley of the groove were significantly large enough to be optically distinguishable, such that the coated films can be utilized as the optical grating film to disperse infra-red light. Utilizing a lowered hydrophilicity of water/IPA dispersant, an opal film could be successfully coated on a flexible Mylar film without significant dewetting problem. Copyright © 2014 Elsevier Inc. All rights reserved.

  17. Smoothing by spectral dispersion using random phase modulation for inertial confinement fusion

    International Nuclear Information System (INIS)

    Rothenberg, J.E.

    1995-01-01

    Numerical simulations of beam smoothing using random phase modulation and grating dispersion are presented. Spatial spectra of the target illumination show that significantly improved smoothing at low spatial frequency is achieved while maintaining uniform intensity in the laser amplifier

  18. Two-Order-Parameter Description of Liquids: Critical Phenomena and Phase Separation of Supercooled Liquids

    OpenAIRE

    Tanaka, Hajime

    1997-01-01

    Because of the isotropic and disordered nature of liquids, the anisotropy hidden in intermolecular interactions are often neglected. Accordingly, the order parameter describing a simple liquid has so far been believed to be only density. In contrast to this common sense, we propose that two order parameters, namely, density and bond order parameters, are required to describe the phase behavior of liquids since they intrinsically tend to form local bonds. This model gives us clear physical exp...

  19. Terminal velocity of liquids and granular materials dispersed by a high explosive

    Science.gov (United States)

    Loiseau, J.; Pontalier, Q.; Milne, A. M.; Goroshin, S.; Frost, D. L.

    2018-04-01

    The explosive dispersal of a layer of solid particles or a layer of liquid surrounding a spherical high-explosive charge generates a turbulent, multiphase flow. Shock compression of the material layer during the initial acceleration may partially consolidate the material, leading to the formation of jet-like structures when the layer fragments and sheds particles upon release. Similarly, release of a shock-compressed liquid shell causes the nucleation of cavitation sites, leading to the radial breakup of the shell and the formation of jets upon expansion. In the current study, a wide variety of granular materials and liquids were explosively dispersed. The maximum terminal jet tip or shell velocity was measured using high-speed videography. Charges were constructed using thin-walled glass bulbs of various diameters and contained a central C-4 charge surrounded by the material to be dispersed. This permitted variation of the ratio of material mass to charge mass (M/C) from 4 to 300. Results indicated that material velocity broadly correlates with predictions of the Gurney model. For liquids, the terminal velocity was accurately predicted by the Gurney model. For granular materials, Gurney over-predicted the terminal velocity by 25-60%, depending on the M/C ratio, with larger M/C values exhibiting larger deficits. These deficits are explained by energy dissipation during the collapse of voids in the granular material bed. Velocity deficits were insensitive to the degree of jetting and granular material properties. Empirical corrections to the Gurney model are presented with improved agreement with the dry powder experimental velocities.

  20. Terminal velocity of liquids and granular materials dispersed by a high explosive

    Science.gov (United States)

    Loiseau, J.; Pontalier, Q.; Milne, A. M.; Goroshin, S.; Frost, D. L.

    2018-05-01

    The explosive dispersal of a layer of solid particles or a layer of liquid surrounding a spherical high-explosive charge generates a turbulent, multiphase flow. Shock compression of the material layer during the initial acceleration may partially consolidate the material, leading to the formation of jet-like structures when the layer fragments and sheds particles upon release. Similarly, release of a shock-compressed liquid shell causes the nucleation of cavitation sites, leading to the radial breakup of the shell and the formation of jets upon expansion. In the current study, a wide variety of granular materials and liquids were explosively dispersed. The maximum terminal jet tip or shell velocity was measured using high-speed videography. Charges were constructed using thin-walled glass bulbs of various diameters and contained a central C-4 charge surrounded by the material to be dispersed. This permitted variation of the ratio of material mass to charge mass ( M/ C) from 4 to 300. Results indicated that material velocity broadly correlates with predictions of the Gurney model. For liquids, the terminal velocity was accurately predicted by the Gurney model. For granular materials, Gurney over-predicted the terminal velocity by 25-60%, depending on the M/ C ratio, with larger M/ C values exhibiting larger deficits. These deficits are explained by energy dissipation during the collapse of voids in the granular material bed. Velocity deficits were insensitive to the degree of jetting and granular material properties. Empirical corrections to the Gurney model are presented with improved agreement with the dry powder experimental velocities.

  1. Development of a dispersive liquid-liquid microextraction method for the determination of polychlorinated biphenyls in water

    International Nuclear Information System (INIS)

    Rezaei, Fatemeh; Bidari, Araz; Birjandi, Afsoon Pajand; Milani Hosseini, Mohammad Reza; Assadi, Yaghoub

    2008-01-01

    A very simple and powerful microextraction procedure, the dispersive liquid-liquid microextraction (DLLME), was used for the determination of the content of 10 polychlorinated biphenyls (PCBs) in water samples, using gas chromatography coupled with electron-capture detection (GC-ECD). The appropriate amount of acetone (disperser solvent) and chlorobenzene (extraction solvent) at the microlevel volume was used for this procedure. The conditions for the microextraction performance were investigated and optimized. The optimized method exhibited a good linearity (R 2 > 0.996) over the studied range (0.005-2 μg L -1 ), illustrating a satisfactory precision level with R.S.D. values between 4.1% and 11.0%. The values of the detection limit (S/N = 3) were found to be lower than 0.002 μg L -1 . Furthermore, a large enrichment factor for the analytes (up to a 540-fold) was achieved in a very short time for only a 5.00-mL water sample. The effectiveness of the method towards real samples was tested by analyzing well, river and seawater samples. The relative recoveries of the well, river and seawater samples, which had been spiked with different levels of PCBs were equal to 92.0-114.0%, 97.0-102.0% and 96.0-103.0%, respectively. The attained results demonstrated that DLLME combined with GC-ECD was a fast and inexpensive technique for the PCBs determination in water samples

  2. Determination of lead in environmental waters with dispersive liquid-liquid microextraction prior to atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    Zhou, Qingxiang; Zhao, Na; Xie, Guohong

    2011-01-01

    This paper established a new, rapid and sensitive method for the determination of lead in water samples preconcentrated by dispersive liquid-liquid microextraction (DLLME) prior to atomic fluorescence spectrometry. Dithizone was used as the chelating agent. In the DLLME procedure, lead formed lead-dithizone complex and migrated into the carbon tetrachloride micro-droplets. Important factors that would affect the extraction efficiency had been investigated including the kind and volume of extraction solvent and dispersive solvent, sample pH, the amount of chelating agent, extraction time and centrifugation time. The results showed that the coexisting ions containing in water samples had no obvious negative effect on the determination of lead. The experimental results indicated that the proposed method had a good linear range of 0.01-100 ng mL -1 (r 2 = 0.9990). The precision was 2.12% (RSD, n = 7) and the detection limit was 0.95 ng L -1 . Proposed method was validated with four real environmental samples and the results indicated that the proposed method was excellent for the future use and satisfied spiked recoveries were in the range of 92.9-97.4%.

  3. Hydrophilic interaction chromatography combined with dispersive liquid-liquid microextraction as a preconcentration tool for the simultaneous determination of the panel of underivatized neurotransmitters in human urine samples.

    Science.gov (United States)

    Konieczna, Lucyna; Roszkowska, Anna; Niedźwiecki, Maciej; Bączek, Tomasz

    2016-01-29

    A simple and sensitive method using dispersive liquid-liquid microextraction (DLLME) followed by liquid chromatography coupled to mass spectrometry (LC-MS) with a hydrophilic interaction chromatography (HILIC) column was developed for the simultaneous determination of 13 compounds of different polarities, comprising monoamine neurotransmitters (dopamine, norepinephrine, epinephrine and serotonin) along with their respective precursors and metabolites, in human urine samples. The microextraction procedure was based on the fast injection of a mixture of ethanol (disperser solvent) and dichloromethane (extraction solvent) into a human urine sample, forming a cloudy solution in the Eppendorf tube. After centrifugation, the sedimented phase was collected and subsequently analyzed by LC-HILIC-MS in about 12min without a derivatization step. The separation was performed on an XBridge Amide™ BEH column 3.0×100mm, 3.5mm and the mobile phase consisted of phase A: 10mM ammonium formate buffer in water pH 3.0 and phase B: 10 mM ammonium formate buffer in acetonitrile, under gradient program elution. Tyrosine, tryptophan, 5-hydroxytryptophan, dopamine, epinephrine, norepinephrine, serotonin, 3-methoxytyramine, 5-hydroxyindole-3-acetic acid, 3,4-dihydroxy-l-phenylalanine and norvaline (internal standard) were detected in the positive ionization mode. While vanillylmandelic acid, homovanillic acid, 3,4-dihydroxyphenylacetic acid and 3,4-dihydroxybenzylamine (internal standard) were detected in the negative ionization mode. Parameters influencing DLLME and LC-HILIC-MS were investigated. Under the optimum conditions, the proposed method exhibited a low detection limit (5-10ngmL(-1)), and good linearity with R between 0.9991 and 0.9998. The recoveries in human urine samples were 99.0%±3.6%. for the 13 studied biogenic amines with intra- and inter-day RSDs of 0.24-9.55% and 0.31-10.0%, respectively. The developed DLLME-LC-MS method could be successfully applied for the

  4. Industrial aspects of gas-liquid two-phase flow

    International Nuclear Information System (INIS)

    Hewitt, G.F.

    1977-01-01

    The lecture begins by reviewing the various types of plant in which two phase flow occurs. Specifically, boiling plant, condensing plant and pipelines are reviewed, and the various two phase flow problems occurring in them are described. Of course, many other kinds of chemical engineering plant involve two phase flow, but are somewhat outside the scope of this lecture. This would include distillation columns, vapor-liquid separators, absorption towers etc. Other areas of industrial two phase flow which have been omitted for space reasons from this lecture are those concerned with gas/solids, liquid/solid and liquid/liquid flows. There then follows a description of some of the two phase flow processes which are relevant in industrial equipment and where special problems occur. The topics chosen are as follows: (1) pressure drop; (2) horizontal tubes - separation effects non-uniformites in heat transfer coefficient, effect of bends on dryout; (3) multicomponent mixtures - effects in pool boiling, mass transfer effects in condensation and Marangoni effects; (4) flow distribution - manifold problems in single phase flow, separation effects at a single T-junction in two phase flow and distribution in manifolds in two phase flow; (5) instability - oscillatory instability, special forms of instability in cryogenic systems; (6) nucleate boiling - effect of variability of surface, unresolved problems in forced convective nucleate boiling; and (7) shell side flows - flow patterns, cross flow boiling, condensation in cross flow

  5. Effect of Foam on Liquid Phase Mobility in Porous Media

    NARCIS (Netherlands)

    Eftekhari, A.A.; Farajzadeh, R.

    2017-01-01

    We investigate the validity of the assumption that foam in porous media reduces the mobility of gas phase only and does not impact the liquid-phase mobility. The foam is generated by simultaneous injection of nitrogen gas and a surfactant solution into sandstone cores and its strength is varied by

  6. Combination of dispersive liquid-liquid microextraction with flame atomic absorption spectrometry using microsample introduction for determination of lead in water samples.

    Science.gov (United States)

    Naseri, Mohammad Taghi; Hemmatkhah, Payam; Hosseini, Mohammad Reza Milani; Assadi, Yaghoub

    2008-03-03

    The dispersive liquid-liquid microextraction (DLLME) was combined with the flame atomic absorption spectrometry (FAAS) for determination of lead in the water samples. Diethyldithiophosphoric acid (DDTP), carbon tetrachloride and methanol were used as chelating agent, extraction solvent and disperser solvent, respectively. A new FAAS sample introduction system was employed for the microvolume nebulization of the non-flammable chlorinated organic extracts. Injection of 20 microL volumes of the organic extract into an air-acetylene flame provided very sensitive spike-like and reproducible signals. Some effective parameters on the microextraction and the complex formation were selected and optimized. These parameters include extraction and disperser solvent type as well as their volume, extraction time, salt effect, pH and amount of the chelating agent. Under the optimized conditions, the enrichment factor of 450 was obtained from a sample volume of 25.0 mL. The enhancement factor, calculated as the ratio of the slopes of the calibration graphs with and without preconcentration, which was about 1000. The calibration graph was linear in the range of 1-70 microgL(-1) with a detection limit of 0.5 microgL(-1). The relative standard deviation (R.S.D.) for seven replicate measurements of 5.0 and 50 microgL(-1) of lead were 3.8 and 2.0%, respectively. The relative recoveries of lead in tap, well, river and seawater samples at the spiking level of 20 microgL(-1) ranged from 93.8 to 106.2%. The characteristics of the proposed method were compared with those of the liquid-liquid extraction (LLE), cloud point extraction (CPE), on-line and off-line solid-phase extraction (SPE) as well as co-precipitation, based on bibliographic data. Operation simplicity, rapidity, low cost, high enrichment factor, good repeatability, and low consumption of the extraction solvent at a microliter level are the main advantages of the proposed method.

  7. Combination of dispersive liquid-liquid microextraction with flame atomic absorption spectrometry using microsample introduction for determination of lead in water samples

    International Nuclear Information System (INIS)

    Naseri, Mohammad Taghi; Hemmatkhah, Payam; Hosseini, Mohammad Reza Milani; Assadi, Yaghoub

    2008-01-01

    The dispersive liquid-liquid microextraction (DLLME) was combined with the flame atomic absorption spectrometry (FAAS) for determination of lead in the water samples. Diethyldithiophosphoric acid (DDTP), carbon tetrachloride and methanol were used as chelating agent, extraction solvent and disperser solvent, respectively. A new FAAS sample introduction system was employed for the microvolume nebulization of the non-flammable chlorinated organic extracts. Injection of 20 μL volumes of the organic extract into an air-acetylene flame provided very sensitive spike-like and reproducible signals. Some effective parameters on the microextraction and the complex formation were selected and optimized. These parameters include extraction and disperser solvent type as well as their volume, extraction time, salt effect, pH and amount of the chelating agent. Under the optimized conditions, the enrichment factor of 450 was obtained from a sample volume of 25.0 mL. The enhancement factor, calculated as the ratio of the slopes of the calibration graphs with and without preconcentration, which was about 1000. The calibration graph was linear in the range of 1-70 μg L -1 with a detection limit of 0.5 μg L -1 . The relative standard deviation (R.S.D.) for seven replicate measurements of 5.0 and 50 μg L -1 of lead were 3.8 and 2.0%, respectively. The relative recoveries of lead in tap, well, river and seawater samples at the spiking level of 20 μg L -1 ranged from 93.8 to 106.2%. The characteristics of the proposed method were compared with those of the liquid-liquid extraction (LLE), cloud point extraction (CPE), on-line and off-line solid-phase extraction (SPE) as well as co-precipitation, based on bibliographic data. Operation simplicity, rapidity, low cost, high enrichment factor, good repeatability, and low consumption of the extraction solvent at a microliter level are the main advantages of the proposed method

  8. Indication of liquid-liquid phase transition in CuZr-based melts

    DEFF Research Database (Denmark)

    Zhou, C.; Hu, L.N.; Sun, Q.J.

    2013-01-01

    We study the dynamic behavior of CuZr-based melts well above the liquidus temperature. The results show a discontinuous change in viscosity during cooling, which is attributed to an underlying liquid-liquid phase transition (LLPT) in these melts. The LLPT is further verified by thermodynamic...

  9. CO2 Capture with Liquid-Liquid Phase Change Solvents: A Thermodynamic Study

    DEFF Research Database (Denmark)

    Waseem Arshad, Muhammad; Fosbøl, Philip Loldrup; von Solms, Nicolas

    2017-01-01

    by the quaternary H2O-DEEAMAPA-CO2 system which gives liquid-liquid phase split when reacted with carbon dioxide. A total of 94 model parameters and 6 thermodynamic properties were fitted to approximately 1500 equilibrium and thermal experimental data consisting of pureamine vapor pressure (Pvap), vapor...

  10. Plasma-treated carbonyl iron particles as a dispersed phase in magnetorheological fluids

    OpenAIRE

    Sedlačík, M.; Pavlínek, V.; Lehocký, M.; Mráček, A.; Grulich, O.; Švrčinová, P. (Petra); Filip, P. (Petr); Vesel, A.

    2011-01-01

    The aim of this paper is to document suitability of plasma-treated carbonyl iron particles as a dispersed phase in magnetorheological fluids. Surface-modified carbonyl iron particles were prepared via their exposure to 50% argon and 50% octafluorocyclobutane plasma. The X-ray photoelectron spectroscopy was used for analysis of chemical bonding states in the surface layer. Plasma-treated particles were adopted for a dispersed phase in magnetorheological (MR) fluids, and the MR behaviour was in...

  11. Effect of Foam on Liquid Phase Mobility in Porous Media

    DEFF Research Database (Denmark)

    Eftekhari, Ali Akbar; Farajzadeh, R.

    2017-01-01

    We investigate the validity of the assumption that foam in porous media reduces the mobility of gas phase only and does not impact the liquid-phase mobility. The foam is generated by simultaneous injection of nitrogen gas and a surfactant solution into sandstone cores and its strength is varied...... by changing surfactant type and concentration. We find, indeed, that the effect of foam on liquid-phase mobility is not pronounced and can be ignored. Our new experimental results and analyses resolve apparent discrepancies in the literature. Previously, some researchers erroneously applied relative...

  12. Dispersive liquid-liquid microextraction for the determination of vitamins D and K in foods by liquid chromatography with diode-array and atmospheric pressure chemical ionization-mass spectrometry detection.

    Science.gov (United States)

    Viñas, Pilar; Bravo-Bravo, María; López-García, Ignacio; Hernández-Córdoba, Manuel

    2013-10-15

    A simple and rapid method was developed using reversed-phase liquid chromatography (LC) with both diode array (DAD) and atmospheric pressure chemical ionization mass spectrometric (APCI-MS) detection, for the simultaneous analysis of the vitamins ergocalciferol (D2), cholecalciferol (D3), phylloquinone (K1), menaquinone-4 (K2) and a synthetic form of vitamin K, menadione (K3). The Taguchi experimental method, an orthogonal array design (OAD), was used to optimize an efficient and clean preconcentration step based on dispersive liquid-liquid microextraction (DLLME). A factorial design was applied with six factors and three levels for each factor, namely, carbon tetrachloride volume, methanol volume, aqueous sample volume, pH of sample, sodium chloride concentration and time of the centrifugation step. The DLLME optimized procedure consisted of rapidly injecting 3 mL of acetonitrile (disperser solvent) containing 150 µL carbon tetrachloride (extraction solvent) into the aqueous sample, thereby forming a cloudy solution. Phase separation was performed by centrifugation, and the sedimented phase was evaporated with nitrogen, reconstituted with 50 µL of acetonitrile, and injected. The LC analyses were carried out using a mobile phase composed of acetonitrile, 2-propanol and water, under gradient elution. Quantification was carried out by the standard additions method. The APCI-MS spectra, in combination with UV spectra, permitted the correct identification of compounds in the food samples. The method was validated according to international guidelines and using a certified reference material. The validated method was applied for the analysis of vitamins D and K in infant foods and several green vegetables. There was little variability in the forms of vitamin K present in vegetables, with the most abundant vitamer in all the samples being phylloquinone, while menadione could not be detected. Conversely, cholecalciferol, which is present in food of animal origin, was

  13. Electrically Tunable Reflective Terahertz Phase Shifter Based on Liquid Crystal

    Science.gov (United States)

    Yang, Jun; Xia, Tianyu; Jing, Shuaicheng; Deng, Guangsheng; Lu, Hongbo; Fang, Yong; Yin, Zhiping

    2018-02-01

    We present a reflective spatial phase shifter which operates at terahertz regime above 325 GHz. The controllable permittivity of the nematic liquid crystals was utilized to realize a tunable terahertz (THz) reflective phase shifter. The reflective characteristics of the terahertz electromagnetic waves and the liquid crystal parameters were calculated and analyzed. We provide the simulation results for the effect of the incident angle of the plane wave on the reflection. The experiment was carried out considering an array consisting of 30 × 30 patch elements, printed on a 20 × 20 mm quartz substrate with 1-mm thickness. The phase shifter provides a tunable phase range of 300° over the frequency range of 325 to 337.6 GHz. The maximum phase shift of 331° is achieved at 330 GHz. The proposed phase shifter is a potential candidate for THz applications, particularly for reconfigurable reflectarrays.

  14. Determination of benzimidazoles in meat samples by capillary zone electrophoresis tandem mass spectrometry following dispersive liquid-liquid microextraction.

    Science.gov (United States)

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

    2017-03-24

    A novel method based on capillary zone electrophoresis-tandem mass spectrometry has been proposed and validated for the identification and simultaneous quantification of twelve benzimidazoles in meat samples. Electrophoretic separation was carried out using 500mM formic acid (pH 2.2) as background electrolyte and applying a voltage of 25kV at 25°C. In order to improve the sensitivity, stacking mode injection was applied, using as injection solvent a mixture of 30:70 acetonitrile/water at 50mbar for 75s. Sensitivity enhancement factors from 74 to 317 were obtained under these conditions. Detection using an ion trap as analyzer, operating in multiple reactions monitoring mode was employed. The main MS/MS parameters as well as the composition of the sheath liquid and other electrospray variables were optimized in order to obtain the highest sensitivity and precision in conjunction with an unequivocal identification. The method was applied to poultry and pork muscle samples. The deproteinization of samples and extraction of benzimidazoles was carried out with acetonitrile. MgSO 4 and NaCl were added as salting-out agents. Subsequently, dispersive liquid-liquid microextraction was applied as clean up procedure. The organic layer (acetonitrile, used as dispersant) containing the benzimidazoles was mixed with the extractant (chloroform) and both were injected in water, producing a cloudy solution. Recoveries for fortified samples were higher than 70%, with relative standard deviations lower than 16% were obtained in all cases. The limits of detection were below 3μgkg -1 , demonstrating the applicability of this fast, simple, and environmentally friendly method. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Extraction and Determination of Crocin in Saffron Samples by Dispersive Liquid-Liquid Microextraction

    Directory of Open Access Journals (Sweden)

    Somayeh Heydari

    2016-11-01

    Full Text Available The main component responsible for color in saffron is crocin with the chemical formula of C44H64O24. Crocin is one of several carotenoids in nature that is soluble in water. This solubility is one of the reasons for its widespread usage as a colorant in food and medicine compared to other carotenoids. The coloring strength of saffron is one of the major factors that determine the quality of the saffron stigma. It will be evaluated with measuring of crocin. Microextraction is the newest and easiest method that can be successfully applied for the preconcentration and separation of crocin in saffron samples. The advantages of this method are faster, cheaper and easier analysis by UV-Vis spectrophotometry in measurement of crocin compared to the chromatographic analysis methods. The studies showed that the type and volume of disperser and extractant solvent have a significant effect on the efficiency of crocin extraction. In this work, acetone as the disperser solvent and dichlorometane as the extractant solvent were found to be suitable combinations. Under the optimal conditions, the calibration curve was linear in the range of 0.15-0.00001 μg mL-1 and the limit of detection (LOD was calculated based on 3 Sb/m (where, Sb and m are the standard deviation of the blank and slop ratio of the calibration curve respectively was 0.000008 μg mL-1. The procedure was applied to saffron samples and the good recovery percent for the saffron samples was obtained.

  16. Phase dispersion of Raman and Rayleigh-enhanced four-wave mixings in femtosecond polarization beats

    International Nuclear Information System (INIS)

    Yan, Zhao; Zhi-Qiang, Nie; Chang-Biao, Li; Yan-Peng, Zhang; Chen-Li, Gan; Huai-Bin, Zheng; Yuan-Yuan, Li; Ke-Qing, Lu

    2009-01-01

    Based on color-locking noisy field correlation in three Markovian stochastic models, phase dispersions of the Raman- and Rayleigh-enhanced four-wave mixing (FWM) have been investigated. The phase dispersions are modified by both linewidth and time delay for negative time delay, but only by linewidth for positive time delay. Moreover, the results under narrowband condition are close to the nonmodified nonlinear dispersion and absorption of the material. Homodyne and heterodyne detections of the Raman, the Rayleigh and the mixing femtosecond difference-frequency polarization beats have also been investigated, separately

  17. Liquid crystal blue phases: stability, field effects and alignment

    OpenAIRE

    Gleeson, HF; Miller, RJ; Tian, L; Görtz, V; Goodby, JW

    2015-01-01

    The blue phases are fascinating structures in liquid crystals, fluids that exhibit cubic structures that have true crystalline order. The blue phases were discovered in the 1970s and were the subject of extensive research in the 1980s, when a deep understanding of many of their properties was established. The discovery that the blue phases could be stabilised to exist over wide temperature ranges meant that they became more than scientific curiosities and led to a recent resurgence in researc...

  18. Discontinuous structural phase transition of liquid metal and alloys (2)

    International Nuclear Information System (INIS)

    Wang, Li; Liu, Jiantong

    2004-01-01

    The diameter (d f ) of diffusion fluid cluster before and after phase transition has been calculated in terms of the paper ''Discontinuous structural phase transition of liquid metal and alloy (1)'' Physics Letters. A 326 (2004) 429-435, to verify quantitatively the discontinuity of structural phase transition; the phenomena of thermal contraction and thermal expansion during the phase transition, together with the evolution model of discontinuous structural phase transition are also discussed in this Letter to explore further the nature of structural transition; In addition, based on the viscosity experimental result mentioned in paper [Y. Waseda, The Structure of Non-Crystalline Materials--Liquids and Amorphous Solids, McGraw-Hill, New York, 1980], we present an approach to draw an embryo of the liquid-liquid (L-L) phase diagram for binary alloys above liquidus in the paper, expecting to guide metallurgy process so as to improve the properties of alloys. The idea that controls amorphous structure and its properties by means of the L-L phase diagram for alloys and by the rapid cooling technique to form the amorphous alloy has been brought forward in the end

  19. Automatic discrimination of bubbles and slugs in two-phase gas-liquid flow and measurement of the respective velocities

    International Nuclear Information System (INIS)

    Fitremann, J.M.; Guilpin, C.; Postaire, J.

    1976-01-01

    The measurement of the interface velocity in a two-phase gas-liquid flow is a difficult problem, owing to the dispersion of the velocity components of individual bubbles, gas-slugs, droplets, waves, etc. An entirely automatic method is presented, it gives the velocity of slugs and bubbles independently, by discrimination of local phase probe signals into a 'slug' signal and a 'bubble' signal feeding a shape-recognition program. Both discriminated void fractions are also calculated by the apparatus [fr

  20. Development of a robust ionic liquid-based dispersive liquid-liquid microextraction against high concentration of salt for preconcentration of trace metals in saline aqueous samples: Application to the determination of Pb and Cd

    International Nuclear Information System (INIS)

    Yousefi, Seyed Reza; Shemirani, Farzaneh

    2010-01-01

    A new ionic liquid-based dispersive liquid-liquid microextraction method was developed for preconcentration and determination of compounds in aqueous samples containing very high salt concentrations. This method can solve the problems associated with the limited application of the conventional IL-based DLLME in these samples. This is believed to arise from dissolving of the ionic liquids in aqueous samples with high salt content. In this method, the robustness of microextraction system against high salt concentration (up to 40%, w/v) is increased by introducing a common ion of the ionic liquid into the sample solution. The proposed method was applied satisfactorily to the preconcentration of lead and cadmium in saline samples. After preconcentration, the settled IL-phase was dissolved in 100 μL ethanol and aspirated into the flame atomic absorption spectrometer (FAAS) using a home-made microsample introduction system. Several variables affecting the microextraction efficiency were investigated and optimized. Under the optimized conditions and preconcentration of only 10 mL of sample, the enhancement factors of 273 and 311 and the detection limits of 0.6 μg L -1 and 0.03 μg L -1 were obtained for lead and cadmium, respectively. Validation of the method was performed by both an analysis of a certified reference material (CRM) and comparison of results with those obtained by ISO standard method.

  1. Nanosize Copper Dispersed Ionic Liquids As an Electrolyte of New Dye-Sensitized Solar Cells

    Directory of Open Access Journals (Sweden)

    Fu-Lin Chen

    2009-01-01

    Full Text Available To enhance the electrical conductivity of the electrolyte for a newly developed dye-sensitized solar cell (DSSC, metallic copper (Cu encapsulated within the carbon shell (Cu@C nanoparticles dispersed in a room temperature ionic liquid (RTIL (e.g., [bmim+][PF6−] has been studied in the present work. By the pulsed-field gradient spin-echo NMR method, the self-diffusion coefficients of cations and anions of the RTIL have been determined. The self-diffusion coefficient of the [bmim+] cations in the RTIL dispersed with 0.08% of Cu@C nanoparticles is increased by 35%. The electrical conductivity of the Cu@C dispersed RTIL is also increased by 65% (1.0 → 2.3 ms/cm. It is very clear the nanosize Cu@C dispersed RTIL with a relatively greater diffusion coefficient and electrical conductivity can be a very effective electrolyte especially utilized in DSSCs.

  2. Liquid phase conversion of Glycerol to Propanediol over highly ...

    Indian Academy of Sciences (India)

    characterization results showed that the copper metal was well-dispersed over MgO support and a new phase. Cu-MgO was ... Currently propanediols are produced from petroleum derivatives .... of MgO.15 Barret-Joyner-Halenda (BJH) method is applied to ..... number of available Cu sites with respect to glycerol as. 0.8. 1.0.

  3. Observation of diffusion phenomena of liquid phase with multiple components

    International Nuclear Information System (INIS)

    Eguchi, Wataru

    1979-01-01

    The diffusion phenomena of liquid phase with multiple components was directly observed, and the factors contributing to complex material transfer were investigated, comparing to the former experimental results. The most excellent method of observing the diffusion behavior of liquid phase used heretofore is to trace the time history of concentration distribution for each component in unsteady diffusion process. The method of directly observing the concentration distribution is usually classified into the analysis of diffused samples, the checking of radioactive isotope tracers, and the measurement of light refraction and transmission. The most suitable method among these is to trace this time history by utilizing the spectrophotometer of position scanning type. An improved spectrophotometer was manufactured for trial. The outline of the measuring system and the detail of the optical system of this new type spectrophotometer are explained. The resolving power for position measurement is described with the numerical calculation. As for the observation examples of the diffusion phenomena of liquid phase with multiple components, the diffusion of multiple electrolytes in aqueous solution, the observation of the material transfer phenomena accompanied by heterogeneous and single phase chemical reaction, and the observation of concentration distribution in the liquid diaphragm in a reaction absorption system are described. For each experimental item, the test apparatus, the sample material, the test process, the test results and the evaluation are explained in detail, and the diffusion phenomena of liquid phase with multiple components were pretty well elucidated. (Nakai, Y.)

  4. NIR-Vis-UV Light-Responsive Actuator Films of Polymer-Dispersed Liquid Crystal/Graphene Oxide Nanocomposites.

    Science.gov (United States)

    Cheng, Zhangxiang; Wang, Tianjie; Li, Xiao; Zhang, Yihe; Yu, Haifeng

    2015-12-16

    To take full advantage of sunlight for photomechanical materials, NIR-vis-UV light-responsive actuator films of polymer-dispersed liquid crystal (PDLC)/graphene oxide (GO) nanocomposites were fabricated. The strategy is based on phase transition of LCs from nematic to isotropic phase induced by combination of photochemical and photothermal processes in the PDLC/GO nanocomposites. Upon mechanical stretching of the film, both topological shape change and mesogenic alignment occurred in the separated LC domains, enabling the film to respond to NIR-vis-UV light. The homodispersed GO flakes act as photoabsorbent and nanoscale heat source to transfer NIR or VIS light into thermal energy, heating the film and photothermally inducing phase transition of LC microdomains. By utilizing photochemical phase transition of LCs upon UV-light irradiation, one azobenzene dye was incorporated into the LC domains, endowing the nanocomposite films with UV-responsive property. Moreover, the light-responsive behaviors can be well-controlled by adjusting the elongation ratio upon mechanical treatment. The NIR-vis-UV light-responsive PDLC/GO nanocomposite films exhibit excellent properties of easy fabrication, low-cost, and good film-forming and mechanical features, promising their numerous applications in the field of soft actuators and optomechanical systems driven directly by sunlight.

  5. Measurement and simulation of the turbulent dispersion of a radioactive tracer in a two-phase flow system

    Energy Technology Data Exchange (ETDEWEB)

    Hensel, F; Rohde, U

    1998-10-01

    The turbulent dispersion of a radiotracer in an experimental setup with a natural convection liquid-gaseous flow was investigated. A liquid-gaseous bubbly flow was generated in a narrow tank by injection of pressurized air into water or by catalytic disintegration of H{sub 2}O{sub 2}. Turbulent Prandtl numbers for gas and tracer dispersion were varied. In the case of higher gas superficial velocities (J{sub gas}{approx}5-15 mm/s), a reasonable agreement was achieved between calculated and measured tracer transport velocity and dispersion coefficient values. A nearly linear correlation between j{sub gas} and D was found in agreement with other authors. The calculation results contribute to a better understanding of the phenomena and interpretation of the measurement results as well as to the validation of the CFD code for turbulent two-phase flow applications. Further investigations are necessary to improve the agreement in the cases of H{sub 2}O{sub 2} disintegration and low gas superficial velocities. (orig.)

  6. Measurement and simulation of the turbulent dispersion of a radioactive tracer in a two-phase flow system

    International Nuclear Information System (INIS)

    Hensel, F.; Rohde, U.

    1998-01-01

    The turbulent dispersion of a radiotracer in an experimental setup with a natural convection liquid-gaseous flow was investigated. A liquid-gaseous bubbly flow was generated in a narrow tank by injection of pressurized air into water or by catalytic disintegration of H 2 O 2 . Turbulent Prandtl numbers for gas and tracer dispersion were varied. In the case of higher gas superficial velocities (J gas ∼5-15 mm/s), a reasonable agreement was achieved between calculated and measured tracer transport velocity and dispersion coefficient values. A nearly linear correlation between j gas and D was found in agreement with other authors. The calculation results contribute to a better understanding of the phenomena and interpretation of the measurement results as well as to the validation of the CFD code for turbulent two-phase flow applications. Further investigations are necessary to improve the agreement in the cases of H 2 O 2 disintegration and low gas superficial velocities. (orig.)

  7. Analysis of Piroxicam in Pharmaceutical Formulation and Human Urine by Dispersive Liquid–Liquid Microextraction Combined with Spectrophotometry

    Directory of Open Access Journals (Sweden)

    Nakisa Seyyedeh Tutunchi

    2013-02-01

    Full Text Available Purpose: Piroxicam, is non–steroidal anti–inflammatory and analgesic agent, which is widely used in the treatment of patients with rheumatologic disorders. A new analytical approach based on the dispersive liquid–liquid microextraction (DLLME has been developed for the extraction and determination of PX in pharmaceutical preparation and human urine. Methods: From the PX standard solution or solutions prepared from real samples, aliquot volumes were pipetted into centrifuge tubes and mixed with acetate buffer at pH 3.0 and NaCl solution. The contents were subjected to the DLLME, so 700 μL of methanol containing 70 μL of chloroform was injected rapidly into a sample solution. A cloudy solution was rapidly produced and the PX extracted into dispersed fine droplets. The mixture was centrifuged, thus these fine droplets of chloroform were settled. The supernatant aqueous phase was readily decanted, then the remained organic phase was diluted with ethanol and the absorbance measured at 355 ± 3 nm against a reagent blank. Results: The main factors affecting the extraction efficiency such as pH, extraction and disperser solvent types and etc. were studied and optimized systematically. Under optimized conditions, the calibration graphs were linear over the range of 0.2 to 4.8 μg/mL. The limit of detection and relative standard deviation were found to be 0.058 μg/mL and 2.83%, respectively. Relative recoveries in the spiked samples ranged from 97 to 110%. Conclusion: Using the developed method PX can be analyzed in pharmaceutical formulation and human urine sample in a simpler, cheaper and more rapid manner.

  8. An airborne dispersion/dose assessment computer program. Phase 1

    International Nuclear Information System (INIS)

    Scott, C.K.; Kennedy, E.R.; Hughs, R.

    1991-05-01

    The Atomic Energy Control Board (AECB) staff have a need for an airborne dispersion-dose assessment computer programme for a microcomputer. The programme must be capable of analyzing the dispersion of both radioactive and non-radioactive materials. A further requirement of the programme is that it be implemented on the AECB complex of microcomputers and that it have an advanced graphical user interface. A survey of computer programs was conducted to determine which, if any, could meet the AECB's requirements in whole or in part. Ten programmes were selected for detailed review including programs for nuclear and non-radiological emergencies. None of the available programmes for radiation dose assessment meets all the requirements for reasons of user interaction, method of source term estimation or site specificity. It is concluded that the best option for meeting the AECB requirements is to adopt the CAMEO programme (specifically the ALOHA portion) which has a superior graphical user interface and add the necessary models for radiation dose assessment

  9. Gas phase dispersion in a small rotary kiln

    International Nuclear Information System (INIS)

    Spencer, B.B.

    1981-07-01

    A study was made of nonideal flow of gas in a rotary kiln reactor. A rotating tube 0.165 m in diameter by 2.17 m long, with internal lifting flights, was operated at room temperature. Rotational speeds from 2.0 to 7.0 rpm, air flow rates from 0.351 to 4.178 m 3 /h, and solid contents of 0.0, 5.1, and 15.3% of tube volume were studied. Residence time distribution of the gas was measured by means of the pulse injection technique using a helium tracer. A model was developed based on dispersive flow that exchanges with a deadwater region. Two parameters, a dispersion number describing bulk gas flow and an interchange factor describing exchange between the flow region and the gas trapped in the solids bed, were sufficient to correlate the data, but these parameters are sensitive to experimental error. The model is applicable to analysis of other flow systems, such as packed beds

  10. Distribution of dispersed oil phase in hydrocarbon fermentations

    Energy Technology Data Exchange (ETDEWEB)

    Ho, C S; Erickson, L E

    1978-04-01

    Recent experimental results show that the spreading coefficient frequently becomes positive when Candida lipolytica is cultivated on n-hexadecane. The effects of oil spreading at the surface of air bubbles in an airlift fermentor are examined using a mathematical model. The distribution of the oil phase with position and among the phases is determined using computer simulation. The simulation results qualitatively explain some of the experimental observations which have been previously reported.

  11. High transmittance optical films based on quantum dot doped nanoscale polymer dispersed liquid crystals

    Science.gov (United States)

    Gandhi, Sahil Sandesh; Chien, Liang-Chy

    2016-04-01

    We propose a simple way to fabricate highly transparent nanoscale polymer dispersed liquid crystal (nano-PDLC) films between glass substrates and investigate their incident angle dependent optical transmittance properties with both collimated and Lambertian intensity distribution light sources. We also demonstrate that doping nano-PDLC films with 0.1% InP/ZnS core/shell quantum dots (QD) results in a higher optical transmittance. This work lays the foundation for such nanostructured composites to potentially serve as roll-to-roll coatable light extraction or brightness enhancement films in emissive display applications, superior to complex nanocorrugation techniques proposed in the past.

  12. Spatial heterogeneity in liquid–liquid phase transition

    International Nuclear Information System (INIS)

    Duan Yun-Rui; Li Tao; Wu Wei-Kang; Li Jie; Zhou Xu-Yan; Liu Si-Da; Li Hui

    2017-01-01

    Molecular dynamics simulations are performed to investigate the liquid–liquid phase transition (LLPT) and the spatial heterogeneity in Al–Pb monotectic alloys. The results reveal that homogeneous liquid Al–Pb alloy undergoes an LLPT, separating into Al-rich and Pb-rich domains, which is quite different from the isocompositional liquid water with a transition between low-density liquid (LDL) and high-density liquid (HDL). With spatial heterogeneity becoming large, LLPT takes place correspondingly. The relationship between the cooling rate, relaxation temperature and percentage of Al and the spatial heterogeneity is also reported. This study may throw light on the relationship between the structure heterogeneity and LLPT, which provides novel strategies to control the microstructures in the fabrication of the material with high performance. (paper)

  13. Quantum phase transitions in semilocal quantum liquids

    Science.gov (United States)

    Iqbal, Nabil; Liu, Hong; Mezei, Márk

    2015-01-01

    We consider several types of quantum critical phenomena from finite-density gauge-gravity duality which to different degrees lie outside the Landau-Ginsburg-Wilson paradigm. These include: (i) a "bifurcating" critical point, for which the order parameter remains gapped at the critical point, and thus is not driven by soft order parameter fluctuations. Rather it appears to be driven by "confinement" which arises when two fixed points annihilate and lose conformality. On the condensed side, there is an infinite tower of condensed states and the nonlinear response of the tower exhibits an infinite spiral structure; (ii) a "hybridized" critical point which can be described by a standard Landau-Ginsburg sector of order parameter fluctuations hybridized with a strongly coupled sector; (iii) a "marginal" critical point which is obtained by tuning the above two critical points to occur together and whose bosonic fluctuation spectrum coincides with that postulated to underly the "Marginal Fermi Liquid" description of the optimally doped cuprates.

  14. Scattering of Neutrons by Liquid Bromine; Diffusion des neutrons par le brome liquide; R; Dispersion de neutrones por bromo liquido

    Energy Technology Data Exchange (ETDEWEB)

    Coote, G E; Haywood, B C [Atomic Energy of Canada Ltd., Chalk River, Ontario (Canada)

    1963-01-15

    Neutrons of 0.037 eV and 0.0088 eV were scattered from a thin sample of liquid bromine at room temperature, and the energy distributions of the scattered neutrons measured at angles from 10{sup o} to 160{sup o} by the time-of-flight method. The angular distribution confirms the results of a previous study by Caglioti. Spectra were expressed in the form of the ''scattering law'' S({alpha},{beta}) of Egelstaff and analysed to derive the generalized frequency distribution p({beta}) of atomic motions in the liquid. The function p({beta}) has a broad smooth peak centred at {beta}{approx}0.3, and shows no evidence for discrete levels in the measured range 0<{beta}< 0.8: the general shape of the curve supports the 'quasi-crystalline' picture of the liquid. Difficulty in the absolute normalization of p({beta}) is discussed. (author) [French] Des neutrons de 0,037 eV et 0,0088 eV ont ete dissuses par un echantillon mince de brome liquide a la temperature ambiante; on a mesure, par la methode du temps de vol, les distributions d'energies des neutrons diffuses, pour des angles compris entre 10{sup o} et 160{sup o}. La distribution angulaire confirme les resultats d'une etude anterieure faite par Caglioti. Les spectres ont ete exprimes d'apres la ''loi de dispersion'' S({alpha},{beta}) d'Egelstaff et analyses pour determiner la distribution generalisee des frequences p({beta}) des mouvements atomiques dans le liquide. La fonction p({beta}) comporte un pic large et a faible pente dont le centre est a {beta} {approx} 0,3 et ne presente aucune indication de niveaux discrets dans la gamme mesuree 0 < {beta} < 0,8; la forme generale de la courbe confirme l'image ''quasi cristalline'' du liquide. Les auteurs examinent les difficultes qui s'opposent a la normalisation absolue de p({beta}). (author) [Spanish] Los autores han estudiado la dispersion de neutrones de 0,037 eV y 0,0088 eV en una muestra de bromo liquido de espesor reducido, a temperatura ambiente. La distribucion

  15. Laser-induced partial oxidation of cyclohexane in liquid phase

    International Nuclear Information System (INIS)

    Oshima, Y.; Wu, X.W.; Koda, S.

    1995-01-01

    A laser-induced partial oxidation of cyclohexane was studied in the liquid phase. With KrF excimer laser (248 nm) irradiation to neat liquid cyclohexane in which O 2 was dissolved, cyclohexanol and cyclohexanone were obtained with very high selectivities, together with cyclohexane as a minor product. Radical recombination reactions to produce dicyclohexyl ether and bicyclohexyl also took place, while these products were not observed in the gas phase reaction. These experimental results were considered to be due not only to higher concentration of cyclohexane but to the cage effect in the liquid phase oxidation. To clarify the reaction progress including the photoabsorption process, the effects of laser intensity and O 2 pressure on product distribution were studied. (author)

  16. Characterisation of GERDA Phase-I detectors in liquid argon

    Energy Technology Data Exchange (ETDEWEB)

    Barnabe Heider, Marik; Schoenert, Stefan [Max-Planck-Institut fuer Kernphysik (Germany); Gusev, Konstantin [Russian Research Center, Kurchatov Institute (Russian Federation); Joint Institute for Nuclear Research (Russian Federation)

    2009-07-01

    GERDA will search for neutrinoless double beta decay in {sup 76}Ge by submerging bare enriched HPGe detectors in liquid argon. In GERDA Phase-I, reprocessed enriched-Ge detectors, which were previously operated by the Heidelberg-Moscow and IGEX collaborations, and reprocessed natural-Ge detectors from Genius-TF, will be redeployed. We have tested the operation and performance of bare HPGe detectors in liquid nitrogen and in liquid argon over more than three years with three non-enriched p-type prototype detectors. The detector handling and mounting procedures have been defined and the Phase-I detector technology, the low-mass assembly and the long-term stability in liquid argon have been tested successfully. The Phase-I detectors were reprocessed by Canberra Semiconductor NV, Olen, according to their standard technology but without the evaporation of a passivation layer. After their reprocessing, the detectors have been mounted in their low-mass holders and their characterisation in liquid argon performed. The leakage current, the counting characteristics and the efficiency of the detectors have been measured. The testing of the detectors was carried out in the liquid argon test stand of the GERDA underground Detector Laboratory (GDL) at LNGS. The detectors are now stored underground under vacuum until their operation in GERDA.

  17. Manipulating Liquids With Acoustic Radiation Pressure Phased Arrays

    Science.gov (United States)

    Oeftering, Richard C.

    1999-01-01

    High-intensity ultrasound waves can produce the effects of "Acoustic Radiation Pressure" (ARP) and "acoustic streaming." These effects can be used to propel liquid flows and to apply forces that can be used to move or manipulate floating objects or liquid surfaces. NASA's interest in ARP includes the remote-control agitation of liquids and the manipulation of bubbles and drops in liquid experiments and propellant systems. A high level of flexibility is attained by using a high-power acoustic phased array to generate, steer, and focus a beam of acoustic waves. This is called an Acoustic Radiation Pressure Phased Array, or ARPPA. In this approach, many acoustic transducer elements emit wavelets that converge into a single beam of sound waves. Electronically coordinating the timing, or "phase shift," of the acoustic waves makes it possible to form a beam with a predefined direction and focus. Therefore, a user can direct the ARP force at almost any desired point within a liquid volume. ARPPA lets experimenters manipulate objects anywhere in a test volume. This flexibility allow it to be used for multiple purposes, such as to agitate liquids, deploy and manipulate drops or bubbles, and even suppress sloshing in spacecraft propellant tanks.

  18. 2D director calculation for liquid crystal optical phased array

    International Nuclear Information System (INIS)

    Xu, L; Zhang, J; Wu, L Y

    2005-01-01

    A practical numerical model for a liquid crystal cell is set up based on the geometrical structure of liquid crystal optical phased arrays. Model parameters include width and space of electrodes, thickness of liquid crystal layer, alignment layers and glass substrates, pre-tilted angles, dielectric constants, elastic constants and so on. According to electrostatic field theory and Frank-Oseen elastic continuum theory, 2D electric potential distribution and 2D director distribution are calculated by means of the finite difference method on non-uniform grids. The influence of cell sizes on director distribution is analyzed. The fringe field effect between electrodes is also discussed

  19. Applications of liquid-phase microextraction in the sample preparation of environmental solid samples.

    Science.gov (United States)

    Prosen, Helena

    2014-05-23

    Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc.) published in the last decade. Several innovative liquid-phase microextraction (LPME) techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME), hollow fiber-liquid phase microextraction (HF-LPME), dispersive liquid-liquid microextraction (DLLME). Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

  20. Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

    Directory of Open Access Journals (Sweden)

    Helena Prosen

    2014-05-01

    Full Text Available Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc. published in the last decade. Several innovative liquid-phase microextraction (LPME techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME, hollow fiber-liquid phase microextraction (HF-LPME, dispersive liquid-liquid microextraction (DLLME. Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

  1. Numerical investigation of particle-blast interaction during explosive dispersal of liquids and granular materials

    Science.gov (United States)

    Pontalier, Q.; Lhoumeau, M.; Milne, A. M.; Longbottom, A. W.; Frost, D. L.

    2018-04-01

    Experiments show that when a high-explosive charge with embedded particles or a charge surrounded by a layer of liquid or granular material is detonated, the flow generated is perturbed by the motion of the particles and the blast wave profile differs from that of an ideal Friedlander form. Initially, the blast wave overpressure is reduced due to the energy dissipation resulting from compaction, fragmentation, and heating of the particle bed, and acceleration of the material. However, as the blast wave propagates, particle-flow interactions collectively serve to reduce the rate of decay of the peak blast wave overpressure. Computations carried out with a multiphase hydrocode reproduce the general trends observed experimentally and highlight the transition between the particle acceleration/deceleration phases, which is not accessible experimentally, since the particles are obscured by the detonation products. The dependence of the particle-blast interaction and the blast mitigation effectiveness on the mitigant to explosive mass ratio, the particle size, and the initial solid volume fraction is investigated systematically. The reduction in peak blast overpressure is, as in experiments, primarily dependent on the mass ratio of material to explosive, with the particle size, density, and initial porosity of the particle bed playing secondary roles. In the near field, the blast overpressure decreases sharply with distance as the particles are accelerated by the flow. When the particles decelerate due to drag, energy is returned to the flow and the peak blast overpressure recovers and reaches values similar to that of a bare explosive charge for low mass ratios. Time-distance trajectory plots of the particle and blast wave motion with the pressure field superimposed, illustrate the weak pressure waves generated by the motion of the particle layer which travel upstream and perturb the blast wave motion. Computation of the particle and gas momentum flux in the multiphase

  2. Numerical investigation of particle-blast interaction during explosive dispersal of liquids and granular materials

    Science.gov (United States)

    Pontalier, Q.; Lhoumeau, M.; Milne, A. M.; Longbottom, A. W.; Frost, D. L.

    2018-05-01

    Experiments show that when a high-explosive charge with embedded particles or a charge surrounded by a layer of liquid or granular material is detonated, the flow generated is perturbed by the motion of the particles and the blast wave profile differs from that of an ideal Friedlander form. Initially, the blast wave overpressure is reduced due to the energy dissipation resulting from compaction, fragmentation, and heating of the particle bed, and acceleration of the material. However, as the blast wave propagates, particle-flow interactions collectively serve to reduce the rate of decay of the peak blast wave overpressure. Computations carried out with a multiphase hydrocode reproduce the general trends observed experimentally and highlight the transition between the particle acceleration/deceleration phases, which is not accessible experimentally, since the particles are obscured by the detonation products. The dependence of the particle-blast interaction and the blast mitigation effectiveness on the mitigant to explosive mass ratio, the particle size, and the initial solid volume fraction is investigated systematically. The reduction in peak blast overpressure is, as in experiments, primarily dependent on the mass ratio of material to explosive, with the particle size, density, and initial porosity of the particle bed playing secondary roles. In the near field, the blast overpressure decreases sharply with distance as the particles are accelerated by the flow. When the particles decelerate due to drag, energy is returned to the flow and the peak blast overpressure recovers and reaches values similar to that of a bare explosive charge for low mass ratios. Time-distance trajectory plots of the particle and blast wave motion with the pressure field superimposed, illustrate the weak pressure waves generated by the motion of the particle layer which travel upstream and perturb the blast wave motion. Computation of the particle and gas momentum flux in the multiphase

  3. Influence of the Fin on Two-Dimensional Characteristics of Dispersed Flow With Wall Liquid Film in the Vicinity of Obstacle

    International Nuclear Information System (INIS)

    Stosic, Zoran V.; Stevanovic, Vladimir D.; Serizawa, Akimi

    2002-01-01

    Spacers have positive effects on the heat transfer enhancement and critical heat flux (CHF) increase downstream of their location in the boiling channel. These effects are further increased by the inclusion of the fin on the spacer rear edge. Numerical simulation of a separation in a high void gas phase and dispersed droplets flow around a spacer, with a liquid film flowing on the wall, is performed. Mechanisms leading to the CHF increase due to the two-phase flow separation and liquid film thickening downstream the spacer are demonstrated. Numerical simulations of gas phase, entrained droplets and wall liquid film flows were performed with the three-fluid model and with the application of the high order numerical scheme for the liquid film surface interface tracking. Predicted is a separation of gas and entrained droplets streams around the spacer without and with a fin inclined 30 and 60 degrees to the wall, as well as a change of wall liquid film thickness in the vicinity of spacer. Results of liquid film dynamic behaviour are compared with the recently obtained experimental results. Multi-dimensional characteristics of surface waves on the liquid film were measured with newly developed ultrasonic transmission technique in a 3 3 rod bundle test section with air-water flow under atmospheric conditions. Obtained numerical results are in good agreement with experimental observations. The presented investigation gives insight into the complex mechanisms of separated two-phase flow with wall liquid film around the spacer and support thermal-hydraulic design and optimisation of flow obstacles in various thermal equipment. (authors)

  4. Dispersive Liquid-Liquid Microextraction Combined with Ultrahigh Performance Liquid Chromatography/Tandem Mass Spectrometry for Determination of Organophosphate Esters in Aqueous Samples

    Directory of Open Access Journals (Sweden)

    Haiying Luo

    2014-01-01

    Full Text Available A new technique was established to identify eight organophosphate esters (OPEs in this work. It utilised dispersive liquid-liquid microextraction in combination with ultrahigh performance liquid chromatography/tandem mass spectrometry. The type and volume of extraction solvents, dispersion agent, and amount of NaCl were optimized. The target analytes were detected in the range of 1.0–200 µg/L with correlation coefficients ranging from 0.9982 to 0.9998, and the detection limits of the analytes were ranged from 0.02 to 0.07 µg/L (S/N=3. The feasibility of this method was demonstrated by identifying OPEs in aqueous samples that exhibited spiked recoveries, which ranged between 48.7% and 58.3% for triethyl phosphate (TEP as well as between 85.9% and 113% for the other OPEs. The precision was ranged from 3.2% to 9.3% (n=6, and the interprecision was ranged from 2.6% to 12.3% (n=5. Only 2 of the 12 selected samples were tested to be positive for OPEs, and the total concentrations of OPEs in them were 1.1 and 1.6 µg/L, respectively. This method was confirmed to be simple, fast, and accurate for identifying OPEs in aqueous samples.

  5. 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.

  6. A new liquid-phase-separation glaze containing neodymium oxide

    International Nuclear Information System (INIS)

    Jing, S.; Xianque, C.; Luxing, K.; Pentecost, J.L.

    1986-01-01

    A color-changeable opaque glaze containing neodymium oxide was investigated. Results show that the glaze is a new example of the liquid-phase-separation type. The discrete phase droplets are from 50 to 500 nm in size. They are rich in Nd, Zn, Ca, and Mg and the continuous phase is rich in Si, Al, and K. The concentration of the discrete phase is approx. =45%. The large number of discrete droplets and the zinc oxide in the glaze increase its opacity to cover the selective light absorption and scattering of the neodymium ion and reduce the opalescence effect

  7. Determination of valproic acid in human plasma using dispersive liquid-liquid microextraction followed by gas chromatography-flame ionization detection

    Science.gov (United States)

    Fazeli-Bakhtiyari, Rana; Panahi-Azar, Vahid; Sorouraddin, Mohammad Hossein; Jouyban, Abolghasem

    2015-01-01

    Objective(s): Dispersive liquid-liquid microextraction coupled with gas chromatography (GC)-flame ionization detector was developed for the determination of valproic acid (VPA) in human plasma. Materials and Methods: Using a syringe, a mixture of suitable extraction solvent (40 µl chloroform) and disperser (1 ml acetone) was quickly added to 10 ml of diluted plasma sample containing VPA (pH, 1.0; concentration of NaCl, 4% (w/v)), resulting in a cloudy solution. After centrifugation (6000 rpm for 6 min), an aliquot (1 µl) of the sedimented organic phase was removed using a 1-µl GC microsyringe and injected into the GC system for analysis. One variable at a time optimization method was used to study various parameters affecting the extraction efficiency of target analyte. Then, the developed method was fully validated for its accuracy, precision, recovery, stability, and robustness. Results: Under the optimum extraction conditions, good linearity range was obtained for the calibration graph, with correlation coefficient higher than 0.998. Limit of detection and lower limit of quantitation were 3.2 and 6 μg/ml, respectively. The relative standard deviations of intra and inter-day analysis of examined compound were less than 11.5%. The relative recoveries were found in the range of 97 to 107.5%. Finally, the validated method was successfully applied to the analysis of VPA in patient sample. Conclusion: The presented method has acceptable levels of precision, accuracy and relative recovery and could be used for therapeutic drug monitoring of VPA in human plasma. PMID:26730332

  8. Liquid crystal alignment in electro-responsive nanostructured thermosetting materials based on block copolymer dispersed liquid crystal

    Energy Technology Data Exchange (ETDEWEB)

    Tercjak, A; Garcia, I; Mondragon, I [Materials-Technologies Group, Departamento IngenierIa Quimica y M Ambiente, Escuela Politecnica, Universidad PaIs Vasco/Euskal Herriko Unibertsitatea, Plaza Europa 1, E-20018 Donostia-San Sebastian (Spain)], E-mail: scptesza@sc.ehu.es, E-mail: inaki.mondragon@ehu.es

    2008-07-09

    Novel well-defined nanostructured thermosetting systems were prepared by modification of a diglicydylether of bisphenol-A epoxy resin (DGEBA) with 10 or 15 wt% amphiphilic poly(styrene-b-ethylene oxide) block copolymer (PSEO) and 30 or 40 wt% low molecular weight liquid crystal 4'-(hexyl)-4-biphenyl-carbonitrile (HBC) using m-xylylenediamine (MXDA) as a curing agent. The competition between well-defined nanostructured materials and the ability for alignment of the liquid crystal phase in the materials obtained has been studied by atomic and electrostatic force microscopy, AFM and EFM, respectively. Based on our knowledge, this is the first time that addition of an adequate amount (10 wt%) of a block copolymer to 40 wt% HBC-(DGEBA/MXDA) leads to a well-organized nanostructured thermosetting system (between a hexagonal and worm-like ordered structure), which is also electro-responsive with high rate contrast. This behavior was confirmed using electrostatic force microscopy (EFM), by means of the response of the HBC liquid crystal phase to the voltage applied to the EFM tip. In contrast, though materials containing 15 wt% PSEO and 30 wt% HBC also form a well-defined nanostructured thermosetting system, they do not show such a high contrast between the uncharged and charged surface.

  9. Liquid crystal alignment in electro-responsive nanostructured thermosetting materials based on block copolymer dispersed liquid crystal.

    Science.gov (United States)

    Tercjak, A; Garcia, I; Mondragon, I

    2008-07-09

    Novel well-defined nanostructured thermosetting systems were prepared by modification of a diglicydylether of bisphenol-A epoxy resin (DGEBA) with 10 or 15 wt% amphiphilic poly(styrene-b-ethylene oxide) block copolymer (PSEO) and 30 or 40 wt% low molecular weight liquid crystal 4'-(hexyl)-4-biphenyl-carbonitrile (HBC) using m-xylylenediamine (MXDA) as a curing agent. The competition between well-defined nanostructured materials and the ability for alignment of the liquid crystal phase in the materials obtained has been studied by atomic and electrostatic force microscopy, AFM and EFM, respectively. Based on our knowledge, this is the first time that addition of an adequate amount (10 wt%) of a block copolymer to 40 wt% HBC-(DGEBA/MXDA) leads to a well-organized nanostructured thermosetting system (between a hexagonal and worm-like ordered structure), which is also electro-responsive with high rate contrast. This behavior was confirmed using electrostatic force microscopy (EFM), by means of the response of the HBC liquid crystal phase to the voltage applied to the EFM tip. In contrast, though materials containing 15 wt% PSEO and 30 wt% HBC also form a well-defined nanostructured thermosetting system, they do not show such a high contrast between the uncharged and charged surface.

  10. Liquid crystal alignment in electro-responsive nanostructured thermosetting materials based on block copolymer dispersed liquid crystal

    International Nuclear Information System (INIS)

    Tercjak, A; Garcia, I; Mondragon, I

    2008-01-01

    Novel well-defined nanostructured thermosetting systems were prepared by modification of a diglicydylether of bisphenol-A epoxy resin (DGEBA) with 10 or 15 wt% amphiphilic poly(styrene-b-ethylene oxide) block copolymer (PSEO) and 30 or 40 wt% low molecular weight liquid crystal 4'-(hexyl)-4-biphenyl-carbonitrile (HBC) using m-xylylenediamine (MXDA) as a curing agent. The competition between well-defined nanostructured materials and the ability for alignment of the liquid crystal phase in the materials obtained has been studied by atomic and electrostatic force microscopy, AFM and EFM, respectively. Based on our knowledge, this is the first time that addition of an adequate amount (10 wt%) of a block copolymer to 40 wt% HBC-(DGEBA/MXDA) leads to a well-organized nanostructured thermosetting system (between a hexagonal and worm-like ordered structure), which is also electro-responsive with high rate contrast. This behavior was confirmed using electrostatic force microscopy (EFM), by means of the response of the HBC liquid crystal phase to the voltage applied to the EFM tip. In contrast, though materials containing 15 wt% PSEO and 30 wt% HBC also form a well-defined nanostructured thermosetting system, they do not show such a high contrast between the uncharged and charged surface

  11. 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.

  12. 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.

  13. Influence of second phase dispersion on void formation during irradiation

    International Nuclear Information System (INIS)

    Sundararaman, M.; Banerjee, S.; Krishnan, R.

    Irradiation-induced void formation in alloys has been found to be strongly influenced by the microstructure, the important microstructural parameters being the dislocation density and the nature, density and distribution of second-phase precipitates. The effects of various types of precipitates on void swelling have been examined using the generally-accepted model of void formation : void embryos are assumed to grow in a situation where equal numbers of vacancies and interstitials are continuously generated by the incident irradiation, the interstitials being somewhat perferentially absorbed in some sinks present in the material. The mechanism of the trapping of defects by a distribution of precipitates has been discussed and the available experimental results on the suppression of void formation in materials containing coherent precipitates have been reviewed. Experimental results on the microstructure developed in a nickel-base alloys, Inconel-718 (considered to be a candidate material for structural applications in fast reactors), have been presented. The method of determination of the coherency strain associated with the precipitates has been illustrated with the help of certain observations made on this alloy. The major difficulty in using a two-phase alloy in an irradiation environment is associated with the irradiation-induced instability of the precipitates. Several processes such as precipitate dislocation (in which the incident radiation removes the outer layer of precipitates by recoil), enhanced diffusion disordering, fragmentation of precipitates, etc. are responsible for bringinq about a significant change in the structure of a two-phase material during irradiation. The effect of these processes on the continued performance of a two-phase alloy subjected to irradiation at an elevated temperature has been discussed. (auth.)

  14. Optimisation of ultrasound-assisted reverse micelles dispersive liquid-liquid micro-extraction by Box-Behnken design for determination of acetoin in butter followed by high performance liquid chromatography.

    Science.gov (United States)

    Roosta, Mostafa; Ghaedi, Mehrorang; Daneshfar, Ali

    2014-10-15

    A novel approach, ultrasound-assisted reverse micelles dispersive liquid-liquid microextraction (USA-RM-DLLME) followed by high performance liquid chromatography (HPLC) was developed for selective determination of acetoin in butter. The melted butter sample was diluted and homogenised by n-hexane and Triton X-100, respectively. Subsequently, 400μL of distilled water was added and the microextraction was accelerated by 4min sonication. After 8.5min of centrifugation, sedimented phase (surfactant-rich phase) was withdrawn by microsyringe and injected into the HPLC system for analysis. The influence of effective variables was optimised using Box-Behnken design (BBD) combined with desirability function (DF). Under optimised experimental conditions, the calibration graph was linear over the range of 0.6-200mgL(-1). The detection limit of method was 0.2mgL(-1) and coefficient of determination was 0.9992. The relative standard deviations (RSDs) were less than 5% (n=5) while the recoveries were in the range of 93.9-107.8%. Copyright © 2014. Published by Elsevier Ltd.

  15. FORTRAN program for calculating liquid-phase and gas-phase thermal diffusion column coefficients

    International Nuclear Information System (INIS)

    Rutherford, W.M.

    1980-01-01

    A computer program (COLCO) was developed for calculating thermal diffusion column coefficients from theory. The program, which is written in FORTRAN IV, can be used for both liquid-phase and gas-phase thermal diffusion columns. Column coefficients for the gas phase can be based on gas properties calculated from kinetic theory using tables of omega integrals or on tables of compiled physical properties as functions of temperature. Column coefficients for the liquid phase can be based on compiled physical property tables. Program listings, test data, sample output, and users manual are supplied for appendices

  16. Separating DDTs in edible animal fats using matrix solid-phase dispersion extraction with activated carbon filter, Toyobo-KF.

    Science.gov (United States)

    Furusawa, Naoto

    2006-09-01

    A technique is presented for the economical, routine, and quantitative analysis of contamination by dichloro-diphenyl-trichloroethanes (DDTs) [pp'-DDT, pp'-dichlorodiphenyl dichloroethylene, and pp'-dichlorodiphenyl dichloreothane in beef tallow and chicken fat samples, based on their separation using matrix solid-phase dispersion (MSPD) extraction with Toyobo-KF, an activated carbon fiber. Toyobo-KF is a newly applied MSPD sorbent, and it is followed by reversed-phase high-performance liquid chromatography (HPLC) with a photodiode array detector. The resulting analytical performance parameters [recoveries of spiked DDTs (0.1, 0.2, and 0.4 microg/g) > or = 81%, with relative standard deviations of < or = 8% (n = 5), and quantitation limits < or = 0.03 microg/g], with minimal handling and cost-efficiency, indicate that the present MSPD-HPLC method may be a useful tool for routine monitoring of DDT contamination in meat.

  17. Drift flux model as approximation of two fluid model for two phase dispersed and slug flow in tube

    Energy Technology Data Exchange (ETDEWEB)

    Nigmatulin, R.I.

    1995-09-01

    The analysis of one-dimensional schematizing for non-steady two-phase dispersed and slug flow in tube is presented. Quasi-static approximation, when inertia forces because of the accelerations of the phases may be neglected, is considered. Gas-liquid bubbly and slug vertical upward flows are analyzed. Non-trivial theoretical equations for slip velocity for these flows are derived. Juxtaposition of the derived equations for slip velocity with the famous Zuber-Findlay correlation as cross correlation coefficients is criticized. The generalization of non-steady drift flux Wallis theory taking into account influence of wall friction on the bubbly or slug flows for kinematical waves is considered.

  18. Drift flux model as approximation of two fluid model for two phase dispersed and slug flow in tube

    International Nuclear Information System (INIS)

    Nigmatulin, R.I.

    1995-01-01

    The analysis of one-dimensional schematizing for non-steady two-phase dispersed and slug flow in tube is presented. Quasi-static approximation, when inertia forces because of the accelerations of the phases may be neglected, is considered. Gas-liquid bubbly and slug vertical upward flows are analyzed. Non-trivial theoretical equations for slip velocity for these flows are derived. Juxtaposition of the derived equations for slip velocity with the famous Zuber-Findlay correlation as cross correlation coefficients is criticized. The generalization of non-steady drift flux Wallis theory taking into account influence of wall friction on the bubbly or slug flows for kinematical waves is considered

  19. Surface-bonded ionic liquid stationary phases in high-performance liquid chromatography--a review.

    Science.gov (United States)

    Pino, Verónica; Afonso, Ana M

    2012-02-10

    Ionic liquids (ILs) are a class of ionic, nonmolecular solvents which remain in liquid state at temperatures below 100°C. ILs possess a variety of properties including low to negligible vapor pressure, high thermal stability, miscibility with water or a variety of organic solvents, and variable viscosity. IL-modified silica as novel high-performance liquid chromatography (HPLC) stationary phases have attracted considerable attention for their differential behavior and low free-silanol activity. Indeed, around 21 surface-confined ionic liquids (SCIL) stationary phases have been developed in the last six years. Their chromatographic behavior has been studied, and, despite the presence of a positive charge on the stationary phase, they showed considerable promise for the separation of neutral solutes (not only basic analytes), when operated in reversed phase mode. This aspect points to the potential for truly multimodal stationary phases. This review attempts to summarize the state-of-the-art about SCIL phases including their preparation, chromatographic behavior, and analytical performance. Copyright © 2011 Elsevier B.V. All rights reserved.

  20. Liquid-liquid phase separation in internally mixed magnesium sulfate/glutaric acid particles

    Science.gov (United States)

    Wu, Feng-Min; Wang, Xiao-Wei; Jing, Bo; Zhang, Yun-Hong; Ge, Mao-Fa

    2018-04-01

    The confocal Raman microscopy is utilized to investigate the liquid-liquid phase separation (LLPS) of mixed magnesium sulfate/glutaric acid (MgSO4/GA) droplets deposited on a hydrophobic polytetrafluoroethylene (PTFE) substrate and a hydrophilic quartz substrate. Raman spectra collected from different regions of the mixed droplets provide detailed information of component distributions for MgSO4 and GA. During the dehydration process, the MgSO4/GA mixed particles show the initial liquid-liquid phase separation between 85% and 80% relative humidity (RH) on both the hydrophobic and hydrophilic substrates. For the droplets deposited on the two substrates, the inner phase of droplets is dominated by aqueous MgSO4, which is surrounded by a rich GA organic layer due to the surface tension effects. In addition, the crystallization of GA could be observed in the organic aqueous phase while it is inhibited in the inner MgSO4 phase due to the effects of gel formation of MgSO4 at low RH. The Raman spectra reveal that with decreasing RH the morphology of the mixed droplet evolves from a uniform droplet to the structure of LLPS with the GA crystallizing in the outer layer and MgSO4 gel formed in the inner phase. These findings contribute to the further understanding of the role of interactions between inorganic salts and organic acids on the morphological evolution and environmental effects of atmospheric aerosols under ambient RH conditions.

  1. 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

  2. Growth of high purity semiconductor epitaxial layers by liquid phase ...

    Indian Academy of Sciences (India)

    Unknown

    semiconductor materials in high purity form by liquid phase epitaxy (LPE) technique. Various possible sources of impurities in such ... reference to the growth of GaAs layers. The technique of growing very high purity layers ... the inner walls of the gas lines and (e) the containers for storing, handling and cleaning of the mate-.

  3. Frustrated smectic liquid crystalline phases in lactic acid derivatives

    Czech Academy of Sciences Publication Activity Database

    Glogarová, Milada; Novotná, Vladimíra

    2016-01-01

    Roč. 89, č. 7-8 (2016), s. 829-839 ISSN 0141-1594 R&D Projects: GA ČR GA15-02843S Institutional support: RVO:68378271 Keywords : field * liquid crystals * TGB phases Subject RIV: JJ - Other Materials Impact factor: 1.060, year: 2016

  4. Investigations on the liquid crystalline phases of cation-induced ...

    Indian Academy of Sciences (India)

    liquid crystalline phases of Li–DNA system could be useful in the production of ... undergo unidirectional ordering (the solution starts to become birefringent under ... was spread over the glass slides with a cover slip and sealed with a neutral ...

  5. Monitoring aged reversed-phase high performance liquid chromatography columns

    NARCIS (Netherlands)

    Bolck, A; Smilde, AK; Bruins, CHP

    1999-01-01

    In this paper, a new approach for the quality assessment of routinely used reversed-phase high performance liquid chromatography columns is presented. A used column is not directly considered deteriorated when changes in retention occur. If attention is paid to the type and magnitude of the changes,

  6. Liquid-phase separation with the rotational particle separator

    NARCIS (Netherlands)

    Kemenade, van H.P.; Mondt, E.; Hendriks, A.J.A.M.; Verbeek, P.H.J.

    2003-01-01

    Recently, the rotational particle separator (RPS) was introduced as a new technique for separating solid and/or liquid particles of 0.1 m and larger from gases. In this patented technique the principles of centrifugation are exploited to enhance separation of small-sized phases and particulate

  7. High purity liquid phase epitaxial gallium arsenide nuclear radiation detector

    International Nuclear Information System (INIS)

    Alexiev, D.; Butcher, K.S.A.

    1991-11-01

    Surface barrier radiation detector made from high purity liquid phase epitaxial gallium arsenide wafers have been operated as X- and γ-ray detectors at various operating temperatures. Low energy isotopes are resolved including 241 Am at 40 deg C. and the higher gamma energies of 235 U at -80 deg C. 15 refs., 1 tab., 6 figs

  8. 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 ...

  9. Application of dispersive liquid-liquid microextraction for the preconcentration of eight parabens in real samples and their determination by high-performance liquid chromatography.

    Science.gov (United States)

    Shen, Xiong; Liang, Jian; Zheng, Luxia; Lv, Qianzhou; Wang, Hong

    2017-11-01

    A simple and sensitive method for the simultaneous determination of eight parabens in human plasma and urine samples was developed. The samples were preconcentrated using dispersive liquid-liquid microextraction based on the solidification of floating organic drops and determined by high-performance liquid chromatography with ultraviolet detection. The influence of variables affecting the extraction efficiency was investigated and optimized using Placket-Burman design and Box-Behnken design. The optimized values were: 58 μL of 1-decanol (as extraction solvent), 0.65 mL methanol (as disperser solvent), 1.5% w/v NaCl in 5.0 mL of sample solution, pH 10.6, and 4.0 min centrifugation at 4000 rpm. The extract was injected into the high-performance liquid chromatography system for analysis. Under the optimum conditions, the linear ranges for eight parabens in plasma and urine were 1.0-1000 ng/mL, with correlation coefficients above 0.994. The limit of detection was 0.2-0.4 and 0.1-0.4 ng/mL for plasma and urine samples, respectively. Relative recoveries were between 80.3 and 110.7%, while relative standard deviations were less than 5.4%. Finally, the method was applied to analyze the parabens in 98 patients of primary breast cancer. Results showed that parabens existed widely, at least one paraben detected in 96.9% (95/98) of plasma samples and 98.0% (96/98) of urine samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Structural crossover in a supercooled metallic liquid and the link to a liquid-to-liquid phase transition

    Energy Technology Data Exchange (ETDEWEB)

    Lan, S.; Ma, J. L.; Fan, J. [Department of Physics and Material Science, City University of Hong Kong 83 Tat Chee Ave., Kowloon (Hong Kong); Blodgett, M.; Kelton, K. F. [Department of Physics and Institute of Materials Science and Engineering, Washington University One Brookings Drive, St. Louis, Missouri 63130-4899 (United States); Wang, X.-L., E-mail: xlwang@cityu.edu.hk [Department of Physics and Material Science, City University of Hong Kong 83 Tat Chee Ave., Kowloon (Hong Kong); City University of Hong Kong Shenzhen Research Institute, Shenzhen 518057 (China)

    2016-05-23

    Time-resolved synchrotron measurements were carried out to capture the structure evolution of an electrostatically levitated metallic-glass-forming liquid during free cooling. The experimental data shows a crossover in the liquid structure at ∼1000 K, about 115 K below the melting temperature and 150 K above the crystallization temperature. The structure change is characterized by a dramatic growth in the extended-range order below the crossover temperature. Molecular dynamics simulations have identified that the growth of the extended-range order was due to an increased correlation between solute atoms. These results provide structural evidence for a liquid-to-liquid-phase-transition in the supercooled metallic liquid.

  11. Acidic ionic liquids for n-alkane isomerization in a liquid-liquid or slurry-phase reaction mode

    Energy Technology Data Exchange (ETDEWEB)

    Meyer, C.; Hager, V.; Geburtig, D.; Kohr, C.; Wasserscheid, P. [Erlangen-Nuernberg Univ. (Germany). Lehrstuhl fuer Chemische Reaktionstechnik; Haumann, M. [Chemical Reaction Engineering, FAU Busan Campus, Korea (Korea, Republic of)

    2011-07-01

    Highly acidic ionic liquid (IL) catalysts offer the opportunity to convert n-alkanes at very low reaction temperatures. The results of IL catalyzed isomerization and cracking reactions of pure n-octane are presented. Influence of IL composition, [C{sub 4}C{sub 1}Im]Cl / AlCl{sub 3} / H{sub 2}SO{sub 4} and [C{sub 4}C{sub 1}Im]Cl / AlCl{sub 3} / 1-chlorooctane, on catalyst activity and selectivities to branched alkanes was investigated. Acidic chloroaluminate IL catalysts form liquid-liquid biphasic systems with unpolar organic product mixtures. Thus, recycling of the acidic IL is enabled by simple phase separation in the liquid-liquid biphasic reaction mode or the IL can be immobilized on an inorganic support with a large specific surface area. These supported ionic liquid phase (SILP) catalysts offer the advantage to get a macroscopically heterogeneous system while still preserving all benefits of the homogeneous catalyst which can be used for the slurry-phase n-alkane isomerization. The interaction of the solid support and acidic IL influences strongly the catalytic activity. (orig.)

  12. Ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction combined with graphite furnace atomic absorption spectrometric for selenium speciation in foods and beverages.

    Science.gov (United States)

    Tuzen, Mustafa; Pekiner, Ozlem Zeynep

    2015-12-01

    A rapid and environmentally friendly ultrasound assisted ionic liquid dispersive liquid liquid microextraction (USA-IL-DLLME) was developed for the speciation of inorganic selenium in beverages and total selenium in food samples by using graphite furnace atomic absorption spectrometry. Some analytical parameters including pH, amount of complexing agent, extraction time, volume of ionic liquid, sample volume, etc. were optimized. Matrix effects were also investigated. Enhancement factor (EF) and limit of detection (LOD) for Se(IV) were found to be 150 and 12 ng L(-1), respectively. The relative standard deviation (RSD) was found 4.2%. The accuracy of the method was confirmed with analysis of LGC 6010 Hard drinking water and NIST SRM 1573a Tomato leaves standard reference materials. Optimized method was applied to ice tea, soda and mineral water for the speciation of Se(IV) and Se(VI) and some food samples including beer, cow's milk, red wine, mixed fruit juice, date, apple, orange, grapefruit, egg and honey for the determination of total selenium. Copyright © 2015 Elsevier Ltd. All rights reserved.

  13. Profile of MIBI liquid phase radiopharmaceutical for myocardial imaging

    International Nuclear Information System (INIS)

    I Daruwati; ME Sriyani; NK Oekar; N Zainuddin; KA Hanafiah

    2016-01-01

    The 99m Tc-MIBI radiopharmaceutical has been used in nuclear medicine in Indonesia for myocardial imaging. BATAN researchers have mastered the technology to manufacture MIBI as a lyophilized kit. A reformulation of MIBI radiopharmaceutical has been conducted to improve the stability of the kit especially in the liquid-phase kit. Basically, radiopharmaceuticals in liquid form are not different from the dry kit. However in the manufacturing of liquid-phase kit, lyophilization process was not done. To improve the stability of liquid kit, a reformulation of the components was conducted by using two separate vials (Formulation 2) and the characteristics were compared with the one-vial formulation (Formulation 1). The MIBI Formulation 2 consists of two vials, vial A containing 0.06 mg of SnCl 2 2H 2 O and 2.6 mg Sodium Citrate 2H 2 O and vial B containing 0.5 mg of [Cu(MIBI) 4 ]BF 4 , 1 mg of cysteine hydrochloride, and 20 mg of mannitol. The purposes of this study were to determine the stability of two different formulations of MIBI as a liquid-phase kit, to compare their stability in different storage condition such as in refrigerator and freezer, and to compare the ratio of activities attained between target and nontarget organs after injection to animal model. As a diagnostic agent, MIBI was reconstituted with Technetium-99m as radionuclide tracer to 99m Tc-MIBI labeled compound. The radiochemical purity of 99m Tc-MIBI was determined by chromatography method using alumina thin-layer chromatography paper as the stationary phase and ethanol 95% as the mobile phase. The results showed MIBI Formulation 2 has a higher stability than Formulation 1. Formulation 2 also maintained a 96.68% radiochemical purity under 52-day storage and attained a target-to-nontarget activity ratio of 8.22. (author)

  14. Frequency doubling in poled polymers using anomalous dispersion phase-matching

    Energy Technology Data Exchange (ETDEWEB)

    Kowalczyk, T.C.; Singer, K.D. [Case Western Reserve Univ., Cleveland, OH (United States). Dept. of Physics; Cahill, P.A. [Sandia National Labs., Albuquerque, NM (United States)

    1995-10-01

    The authors report on a second harmonic generation in a poled polymer waveguide using anomalous dispersion phase-matching. Blue light ({lambda} = 407 nm) was produced by phase-matching the lowest order fundamental and harmonic modes over a distance of 32 {micro}m. The experimental conversion efficiency was {eta} = 1.2 {times} 10{sup {minus}4}, in agreement with theory. Additionally, they discuss a method of enhancing the conversion efficiency for second harmonic generation using anomalous dispersion phase-matching to optimize Cerenkov second harmonic generation. The modeling shows that a combination of phase-matching techniques creates larger conversion efficiencies and reduces critical fabrication requirements of the individual phase-matching techniques.

  15. Solvation thermodynamics of phenylalcohols in lamellar phase surfactant dispersions

    International Nuclear Information System (INIS)

    Martyniak, A.; Scheuermann, R.; Dilger, H.; Tucker, I.M.; Burkert, T.; Hashmi, A.S.K.; Vujosevic', D.; Roduner, E.

    2006-01-01

    The distribution and the stability of five phenylalcohols in a lamellar phase composed of simple bilayers separated by water at 298 and 348K is explored using avoided-level-crossing muon-spin resonance (ALC-μSR). The dependence of the alignment of the bilayer chains on temperature appears to be a crucial factor determining the phenylalcohol partitioning: increasing order of the surfactant tails leads to expulsion of the solute. Moreover, we observed a systematic trend, the longer the chain the deeper the phenyl group dips into the lipid bilayer. Recent studies have shown that the hydrophobic effect is adequate to describe membrane partitioning of small amphiphilic molecules. The solvation thermodynamic properties ΔG sol , ΔH sol , and ΔS sol which determine the solute transfer from the double layer into water prove that the distribution also strongly depends on shape, chemical nature and different structure of phenylalcohols

  16. Solvation thermodynamics of phenylalcohols in lamellar phase surfactant dispersions

    Energy Technology Data Exchange (ETDEWEB)

    Martyniak, A. [Institut fuer Physikalische Chemie, University of Stuttgart, Pfaffenwaldring 55, D-70569 Stuttgart (Germany); Scheuermann, R. [Laboratory for muon Spin Spectroscopy, Paul Scherrer Institute, CH-5232 Villigen (Switzerland); Dilger, H. [Institut fuer Physikalische Chemie, University of Stuttgart, Pfaffenwaldring 55, D-70569 Stuttgart (Germany); Tucker, I.M. [Unilever Research and Development, Port Sunlight, Wirral CH63 3JW (United Kingdom); Burkert, T. [Institut fuer Organische Chemie, University of Stuttgart, Pfaffenwaldring 55, D-70569 Stuttgart (Germany); Hashmi, A.S.K. [Institut fuer Organische Chemie, University of Stuttgart, Pfaffenwaldring 55, D-70569 Stuttgart (Germany); Vujosevic' , D. [Institut fuer Physikalische Chemie, University of Stuttgart, Pfaffenwaldring 55, D-70569 Stuttgart (Germany); Roduner, E. [Institut fuer Physikalische Chemie, University of Stuttgart, Pfaffenwaldring 55, D-70569 Stuttgart (Germany)]. E-mail: e.roduner@ipc.uni-stuttgart.de

    2006-03-31

    The distribution and the stability of five phenylalcohols in a lamellar phase composed of simple bilayers separated by water at 298 and 348K is explored using avoided-level-crossing muon-spin resonance (ALC-{mu}SR). The dependence of the alignment of the bilayer chains on temperature appears to be a crucial factor determining the phenylalcohol partitioning: increasing order of the surfactant tails leads to expulsion of the solute. Moreover, we observed a systematic trend, the longer the chain the deeper the phenyl group dips into the lipid bilayer. Recent studies have shown that the hydrophobic effect is adequate to describe membrane partitioning of small amphiphilic molecules. The solvation thermodynamic properties {delta}G{sub sol}, {delta}H{sub sol}, and {delta}S{sub sol} which determine the solute transfer from the double layer into water prove that the distribution also strongly depends on shape, chemical nature and different structure of phenylalcohols.

  17. Magnetic stirrer induced dispersive ionic-liquid microextraction for the determination of vanadium in water and food samples prior to graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem Gul; Tuzen, Mustafa

    2015-04-01

    A new dispersive liquid-liquid microextraction, magnetic stirrer induced dispersive ionic-liquid microextraction (MS-IL-DLLME) was developed to quantify the trace level of vanadium in real water and food samples by graphite furnace atomic absorption spectrometry (GFAAS). In this extraction method magnetic stirrer was applied to obtained a dispersive medium of 1-butyl-3-methylimidazolium hexafluorophosphate [C4MIM][PF6] in aqueous solution of (real water samples and digested food samples) to increase phase transfer ratio, which significantly enhance the recovery of vanadium - 4-(2-pyridylazo) resorcinol (PAR) chelate. Variables having vital role on desired microextraction methods were optimised to obtain the maximum recovery of study analyte. Under the optimised experimental variables, enhancement factor (EF) and limit of detection (LOD) were achieved to be 125 and 18 ng L(-1), respectively. Validity and accuracy of the desired method was checked by analysis of certified reference materials (SLRS-4 Riverine water and NIST SRM 1515 Apple leaves). The relative standard deviation (RSD) for 10 replicate determinations at 0.5 μg L(-1) of vanadium level was found to be <5.0%. This method was successfully applied to real water and acid digested food samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

  18. 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)

  19. Liquid Phase Sintering of Highly Alloyed Stainless Steel

    DEFF Research Database (Denmark)

    Mathiesen, Troels

    1996-01-01

    Liquid phase sintering of stainless steel is usually applied to improve corrosion resistance by obtaining a material without an open pore system. The dense structure normally also give a higher strength when compared to conventional sintered steel. Liquid phase sintrering based on addition...... of boride to AISI 316L type steels have previously been studied, but were found to be sensitive to intergranular corrosion due to formation of intermetallic phases rich in chromium and molybdenum. In order to improve this system further, new investigations have focused on the use of higher alloyed stainless...... steel as base material. The stainless base powders were added different amounts and types of boride and sintered in hydrogen at different temperatures and times in a laboratory furnace. During sintering the outlet gas was analyzed and subsequently related to the obtained microstructure. Thermodynamic...

  20. Lyotropic liquid crystalline phase behaviour in amphiphile-protic ionic liquid systems.

    Science.gov (United States)

    Chen, Zhengfei; Greaves, Tamar L; Fong, Celesta; Caruso, Rachel A; Drummond, Calum J

    2012-03-21

    Approximate partial phase diagrams for nine amphiphile-protic ionic liquid (PIL) systems have been determined by synchrotron source small angle X-ray scattering, differential scanning calorimetry and cross polarised optical microscopy. The binary phase diagrams of some common cationic (hexadecyltrimethyl ammonium chloride, CTAC, and hexadecylpyridinium bromide, HDPB) and nonionic (polyoxyethylene (10) oleyl ether, Brij 97, and Pluronic block copolymer, P123) amphiphiles with the PILs, ethylammonium nitrate (EAN), ethanolammonium nitrate (EOAN) and diethanolammonium formate (DEOAF), have been studied. The phase diagrams were constructed for concentrations from 10 wt% to 80 wt% amphiphile, in the temperature range 25 °C to >100 °C. Lyotropic liquid crystalline phases (hexagonal, cubic and lamellar) were formed at high surfactant concentrations (typically >50 wt%), whereas at thermal stability of the phases formed by these surfactants persisted to temperatures above 100 °C. The phase behaviour of amphiphile-PIL systems was interpreted by considering the PIL cohesive energy, liquid nanoscale order, polarity and ionicity. For comparison the phase behaviour of the four amphiphiles was also studied in water.

  1. Rapid determination of 9 aromatic amines in mainstream cigarette smoke by modified dispersive liquid liquid microextraction and ultraperformance convergence chromatography tandem mass spectrometry.

    Science.gov (United States)

    Deng, Huimin; Yang, Fei; Li, Zhonghao; Bian, Zhaoyang; Fan, Ziyan; Wang, Ying; Liu, Shanshan; Tang, Gangling

    2017-07-21

    Aromatic amines in mainstream cigarette smoke have long been monitored due to their carcinogenic toxicity. In this work, a reliable and rapid method was developed for the simultaneous determination of 9 aromatic amines in mainstream cigarette smoke by modified dispersive liquid liquid microextraction (DLLME) and ultraperformance convergence chromatography tandem mass spectrometry (UPC 2 -MS/MS). Briefly, the particulate phase of the cigarette smoke was captured by a Cambridge filter pad, and diluted hydrogen chloride aqueous solution is employed to extract the aromatic amines under mechanical shaking. After alkalization with sodium hydroxide solution, small amount of toluene was introduced to further extract and enrich aromatic amines by modified DLLME under vortexing. After centrifugation, toluene phase was purified by a universal QuEChERS cleanup kit and was finally analyzed by UPC 2 -MS/MS. Attributing to the superior performance of UPC 2 -MS/MS, this novel approach allowed the separation and determination of 9 aromatic amines within 5.0min with satisfactory resolution and sensitivity. The proposed method was finally validated using Kentucky reference cigarette 3R4F, and emission levels of targeted aromatic amines determined were comparable to previously reported methods At three different spiked levels, the recoveries of most analytes were ranged from 74.01% to 120.50% with relative standard deviation (RSD) less than 12%, except that the recovery of p-toluidine at low spiked level and 3-aminobiphenyl at medium spiked level was 62.77% and 69.37% respectively. Thus, this work provides a novel alternative method for the simultaneous analysis of 9 aromatic amines in mainstream cigarette smoke. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Liquid-phase and solid-phase radioimmunoassay with herpes simplex virus type 1 nucleocapsids

    International Nuclear Information System (INIS)

    Bystricka, M.; Rajcani, J.; Libikova, H.; Sabo, A.; Foeldes, O.; Sadlon, J.

    1985-01-01

    Liquid-phase radioimmunoassay and solid-phase radioimmunoassay are described using 125 I-labelled or immobilized nucleocapsids (NC) of herpes simplex virus (HSV) type1. These techniques appeared sensitive and specific for quantitation of HSV-NC antigens and corresponding antibodies. (author)

  3. Vapor phase versus liquid phase grafting of meso-porous alumina

    NARCIS (Netherlands)

    Sripathi, V.G.P.; Mojet, Barbara; Nijmeijer, Arian; Benes, Nieck Edwin

    2013-01-01

    Functionalization of meso-porous c-alumina has been performed by grafting of 3-Aminopropyltrimethoxysilane (3APTMS) simultaneously from either the liquid phase or from the vapor phase. In both cases, after grafting nitrogen physisorption indicates that the materials remain meso-porous with

  4. Water Phase Diagram Is Significantly Altered by Imidazolium Ionic Liquid

    DEFF Research Database (Denmark)

    Chaban, V. V.; Prezhdo, O. V.

    2014-01-01

    We report unusually large changes in the boiling temperature, saturated vapor pressure, and structure of the liquid-vapor interface for a range of 1-butyl-3-methyl tetrafluoroborate, [C4C1IM][BF4]-water mixtures. Even modest molar fractions of [C4C1IM][BF4] significantly affect the phase behavior...... of water, as represented, for instance, by strong negative deviations from Raoult's law, extending far beyond the standard descriptions. The investigation was carried out using classical molecular dynamics employing a specifically refined force field. The changes in the liquid-vapor interface and saturated...

  5. Horizontal liquid film-mist two phase flow, (1)

    International Nuclear Information System (INIS)

    Akagawa, Koji; Sakaguchi, Tadashi; Fujii, Terushige; Nakatani, Yoji; Nakaseko, Kosaburo.

    1979-01-01

    The characteristics of liquid film in annular spray flow, the generation of droplets from liquid film and the transport of droplets to a wall are the important matters in the planning and design of nuclear reactor cooling system and the channels of steam generators. The study on the liquid film spray flow is scarce, and its characteristics are not yet elucidated. The purpose of this series of studies is to clarify the characteristics of liquid film, the generation, diffusion and distribution of droplets and pressure loss in the liquid film spray flow composed of the liquid film on the lower wall and spraying gas flow in a rectangular, horizontal channel. In this paper, the concentration distribution and the diffusion coefficient of droplets on a cross section in the region of flow completion are reported. The experimental apparatuses and the experimental method, the flow rate of droplets and the velocity distribution of gas phase, the concentration distribution and the diffusion coefficient of droplets, and the diameter of generated droplets are explained. The equation for the concentration distribution of droplets using dimensionless characteristic value was derived. The mean diffusion coefficient of droplets was constant on a cross section, and the effects of gravity and turbulent diffusion can be evaluated. (Kako, I.)

  6. Plasmas in Multiphase Media: Bubble Enhanced Discharges in Liquids and Plasma/Liquid Phase Boundaries

    Energy Technology Data Exchange (ETDEWEB)

    Kushner, Mark Jay [University of Michigan

    2014-07-10

    In this research project, the interaction of atmospheric pressure plasmas with multi-phase media was computationally investigated. Multi-phase media includes liquids, particles, complex materials and porous surfaces. Although this investigation addressed fundamental plasma transport and chemical processes, the outcomes directly and beneficially affected applications including biotechnology, medicine and environmental remediation (e.g., water purification). During this project, we made advances in our understanding of the interaction of atmospheric pressure plasmas in the form of dielectric barrier discharges and plasma jets with organic materials and liquids. We also made advances in our ability to use computer modeling to represent these complex processes. We determined the method that atmospheric pressure plasmas flow along solid and liquid surfaces, and through endoscopic like tubes, deliver optical and high energy ion activation energy to organic and liquid surfaces, and produce reactivity in thin liquid layers, as might cover a wound. We determined the mechanisms whereby plasmas can deliver activation energy to the inside of liquids by sustaining plasmas in bubbles. These findings are important to the advancement of new technology areas such as plasma medicine

  7. Phase stability analysis of liquid-liquid equilibrium with stochastic methods

    Directory of Open Access Journals (Sweden)

    G. Nagatani

    2008-09-01

    Full Text Available Minimization of Gibbs free energy using activity coefficient models and nonlinear equation solution techniques is commonly applied to phase stability problems. However, when conventional techniques, such as the Newton-Raphson method, are employed, serious convergence problems may arise. Due to the existence of multiple solutions, several problems can be found in modeling liquid-liquid equilibrium of multicomponent systems, which are highly dependent on the initial guess. In this work phase stability analysis of liquid-liquid equilibrium is investigated using the NRTL model. For this purpose, two distinct stochastic numerical algorithms are employed to minimize the tangent plane distance of Gibbs free energy: a subdivision algorithm that can find all roots of nonlinear equations for liquid-liquid stability analysis and the Simulated Annealing method. Results obtained in this work for the two stochastic algorithms are compared with those of the Interval Newton method from the literature. Several different binary and multicomponent systems from the literature were successfully investigated.

  8. Glass and liquid phase diagram of a polyamorphic monatomic system

    Science.gov (United States)

    Reisman, Shaina; Giovambattista, Nicolas

    2013-02-01

    We perform out-of-equilibrium molecular dynamics (MD) simulations of a monatomic system with Fermi-Jagla (FJ) pair potential interactions. This model system exhibits polyamorphism both in the liquid and glass state. The two liquids, low-density (LDL) and high-density liquid (HDL), are accessible in equilibrium MD simulations and can form two glasses, low-density (LDA) and high-density amorphous (HDA) solid, upon isobaric cooling. The FJ model exhibits many of the anomalous properties observed in water and other polyamorphic liquids and thus, it is an excellent model system to explore qualitatively the thermodynamic properties of such substances. The liquid phase behavior of the FJ model system has been previously characterized. In this work, we focus on the glass behavior of the FJ system. Specifically, we perform systematic isothermal compression and decompression simulations of LDA and HDA at different temperatures and determine "phase diagrams" for the glass state; these phase diagrams varying with the compression/decompression rate used. We obtain the LDA-to-HDA and HDA-to-LDA transition pressure loci, PLDA-HDA(T) and PHDA-LDA(T), respectively. In addition, the compression-induced amorphization line, at which the low-pressure crystal (LPC) transforms to HDA, PLPC-HDA(T), is determined. As originally proposed by Poole et al. [Phys. Rev. E 48, 4605 (1993)], 10.1103/PhysRevE.48.4605 simulations suggest that the PLDA-HDA(T) and PHDA-LDA(T) loci are extensions of the LDL-to-HDL and HDL-to-LDL spinodal lines into the glass domain. Interestingly, our simulations indicate that the PLPC-HDA(T) locus is an extension, into the glass domain, of the LPC metastability limit relative to the liquid. We discuss the effects of compression/decompression rates on the behavior of the PLDA-HDA(T), PHDA-LDA(T), PLPC-HDA(T) loci. The competition between glass polyamorphism and crystallization is also addressed. At our "fast rate," crystallization can be partially suppressed and the

  9. Resistive sensing of gaseous nitrogen dioxide using a dispersion of single-walled carbon nanotubes in an ionic liquid

    Energy Technology Data Exchange (ETDEWEB)

    Mishra, Prabhash [Solidstate Electronics Research Laboratory (SERL), Faculty of Engineering and Technology, Jamia Millia Islamia, Jamia Nagar, New Delhi 110025 (India); Department of Nanoengineering, Samara State Aerospace University, 443086 Samara (Russian Federation); Pavelyev, V.S. [Department of Nanoengineering, Samara State Aerospace University, 443086 Samara (Russian Federation); Patel, Rajan [Center for Interdisciplinary Research in Basic Sciences (CIRBSc), Jamia Millia Islamia, Jamia Nagar, New Delhi 110025 (India); Islam, S.S., E-mail: sislam@jmi.ac.in [Solidstate Electronics Research Laboratory (SERL), Faculty of Engineering and Technology, Jamia Millia Islamia, Jamia Nagar, New Delhi 110025 (India)

    2016-06-15

    Graphical abstract: Ionic liquid ([C6-mim]PF6) used as dispersant agent for SWCNTs: An investigations were carried out to find the structural quality and surface modification for sensor application. - Highlights: • An effective technique based on Ionic liquids (IL) and their use as a dispersant. • Electron microscopy and spectroscopy for structure characterization. • Covalent linkage of ILs with SWNTs and dispersion of SWCNTs. • The IL-wrapped sensing film, capable for detecting trace levels of gas. - Abstract: Single-walled carbon nanotubes (SWCNTs) were dispersed in an imidazolium-based ionic liquid (IL) and investigated in terms of structural quality, surface functionalization and inter-CNT force. Analysis by field emission electron microscopy and transmission electron microscopy shows the IL layer to coat the SWNTs, and FTIR and Raman spectroscopy confirm strong binding of the ILs to the SWNTs. Two kinds of resistive sensors were fabricated, one by drop casting of IL-wrapped SWCNTs, the other by conventional dispersion of SWCNTs. Good response and recovery to NO{sub 2} is achieved with the IL-wrapped SWCNTs material upon UV-light exposure, which is needed because decrease the desorption energy barrier to increase the gas molecule desorption. NO{sub 2} can be detected in the 1–20 ppm concentration range. The sensor is not interfered by humidity due to the hydrophobic tail of PF6 (ionic liquid) that makes our sensor highly resistant to moisture.

  10. Heat transfer by gas-liquid mixture in forced turbulent flow with weak vaporization of the liquid phase (1962); Transfert de chaleur par melange de liquide et de gaz en convection forcee turbulente avec faible vaporisation de la phase liquide (1962)

    Energy Technology Data Exchange (ETDEWEB)

    Huyghe, J; Mondin, G [Commissariat a l' Energie Atomique, Grenoble (France). Centre d' Etudes Nucleaires

    1962-07-01

    The present study deals with measures of heat transfer and pressure drop in two-phase liquid flow. The stream is of annular dispersed type, obtained by introducing a small quantity of liquid in a gas turbulent flow. The heat transfer experiments are performed without vaporization of the liquid phase. A notable improvement of the heat transfer coefficient of such a stream is observed, compared with a gas-alone or liquid-alone flow. The improvement concerning the gas-alone is of about 20 when it is compared with the same gas Reynolds's number, of about 8 when it is compared with the same total mass flow rate. A hydrodynamic study of the flow pattern lets us know the original structure of the flow, and allows to foresee the experimental results by means of a simplified theory. (authors) [French] II est fait etat de mesures de transfert thermique et de perte de charge dans un ecoulement en double phase gaz-liquide. L'ecoulement est du type annulaire disperse, obtenu par injection d'une faible quantite de liquide dans un ecoulement gazeux en regime turbulent. Les experiences de transfert thermique sont menees sans vaporisation de la phase liquide. On note une amelioration sensible du coefficient de transfert thermique dans un tel ecoulement par rapport a un ecoulement de gaz seul ou de liquide seul. L'augmentation est de l'ordre de 20 par rapport au gaz seul si on opere a meme nombre de REYNOLDS du gaz, de l'ordre de 8 si on opere a meme debit massique total. Une etude hydrodynamique rapide de l'ecoulement permet de connaitre la structure originale de l'ecoulement, puis de prevoir par une theorie simplifiee le phenomene thermique observe. (auteurs)

  11. 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.

  12. [Determination of four phenolic endocrine disruptors in environmental water samples by high performance liquid chromatography-fluorescence detection using dispersive liquid-liquid microextraction coupled with derivatization].

    Science.gov (United States)

    Wang, Xiaoyan; Qi, Weimei; Zhao, Xian'en; Lü, Tao; Wang, Xiya; Zheng, Longfang; Yan, Yehao; You, Jinmao

    2014-06-01

    To achieve accurate, fast and sensitive detection of phenolic endocrine disruptors in small volume of environmental water samples, a method of dispersive liquid-liquid microextraction (DLLME) coupled with fluorescent derivatization was developed for the determination of bisphenol A, nonylphenol, octylphenol and 4-tert-octylphenol in environmental water samples by high performance liquid chromatography-fluorescence detection (HPLC-FLD). The DLLME and derivatization conditions were investigated, and the optimized DLLME conditions for small volume of environmental water samples (pH 4.0) at room temperature were as follows: 70 microL chloroform as extraction solvent, 400 microL acetonitrile as dispersing solvent, vortex mixing for 3 min, and then high-speed centrifugation for 2 min. Using 2-[2-(7H-dibenzo [a, g] carbazol-7-yl)-ethoxy] ethyl chloroformate (DBCEC-Cl) as precolumn derivatization reagent, the stable derivatives of the four phenolic endocrine disruptors were obtained in pH 10.5 Na2CO3-NaHCO3 buffer/acetonitrile at 50 degrees C for 3 min, and then separated within 10 min by HPLC-FLD. The limits of detection (LODs) were in the range of 0.9-1.6 ng/L, and the limits of quantification (LOQs) were in the range of 3.8-7.1 ng/L. This method had perfect linearity, precision and recovery results, and showed obvious advantages and practicality comparing to the previously reported methods. It is a convenient and validated method for the routine analysis of phenolic endocrine disruptors in waste water of paper mill, lake water, domestic wastewater, tap water, etc.

  13. Multiplexing storage using angular variation in a transmission holographic polymer dispersed liquid crystal

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Eun-Hee; Jung, Yeon-Gil, E-mail: jungyg@changwon.ac.kr

    2015-12-01

    Simultaneous angular multiplexing of transmission gratings in a holographic polymer dispersed liquid crystal (HPDLC) film as a function of resin and film compositions, irradiation intensity, and cell thickness has been studied by exposing the material to three coherent laser beams. It was found that the diffraction efficiency monotonically increases with irradiation intensity and cell gap, whereas a maximum of 43% is obtained at specific compositions of trimethylolpropane triacrylate (TMPTA)/N-vinylpyrrolidone (NVP) = 8/1 and polymer/LC = 65/35. The multiplexed gratings have been captured using SEM imaging and the reconstructed images using a charge-coupled device camera, showing successful reconstructed images of gratings. - Highlights: • Multiplex images were well recorded using simultaneous angular method. • The periodic structures of the LC and polymer regions were well prepared. • The angular selectivity was variable nevertheless fabrication by three beams. • The images were successfully reconstructed in gratings of same spot.

  14. Multiplexing storage using angular variation in a transmission holographic polymer dispersed liquid crystal

    International Nuclear Information System (INIS)

    Kim, Eun-Hee; Jung, Yeon-Gil

    2015-01-01

    Simultaneous angular multiplexing of transmission gratings in a holographic polymer dispersed liquid crystal (HPDLC) film as a function of resin and film compositions, irradiation intensity, and cell thickness has been studied by exposing the material to three coherent laser beams. It was found that the diffraction efficiency monotonically increases with irradiation intensity and cell gap, whereas a maximum of 43% is obtained at specific compositions of trimethylolpropane triacrylate (TMPTA)/N-vinylpyrrolidone (NVP) = 8/1 and polymer/LC = 65/35. The multiplexed gratings have been captured using SEM imaging and the reconstructed images using a charge-coupled device camera, showing successful reconstructed images of gratings. - Highlights: • Multiplex images were well recorded using simultaneous angular method. • The periodic structures of the LC and polymer regions were well prepared. • The angular selectivity was variable nevertheless fabrication by three beams. • The images were successfully reconstructed in gratings of same spot.

  15. Fabrication of Microcapsules for Dye-Doped Polymer-Dispersed Liquid Crystal-Based Smart Windows.

    Science.gov (United States)

    Kim, Mingyun; Park, Kyun Joo; Seok, Seunghwan; Ok, Jong Min; Jung, Hee-Tae; Choe, Jaehoon; Kim, Do Hyun

    2015-08-19

    A dye-doped polymer-dispersed liquid crystal (PDLC) is an attractive material for application in smart windows. Smart windows using a PDLC can be operated simply and have a high contrast ratio compared to those of other devices that employed photochromic or thermochromic material. However, in conventional dye-doped PDLC methods, dye contamination can cause problems and has a limited degree of commercialization of electric smart windows. Here, we report on an approach to resolve dye-related problems by encapsulating the dye in monodispersed capsules. By encapsulation, a fabricated dye-doped PDLC had a contrast ratio of >120 at 600 nm. This fabrication method of encapsulating the dye in a core-shell structured microcapsule in a dye-doped PDLC device provides a practical platform for dye-doped PDLC-based smart windows.

  16. Co marker determination in rumen liquid sample by energy dispersive X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, Eduardo de; Nascimento Filho, Virgilio F.; Massoni, Paulo R. [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Lab. de Instrumentacao Nuclear (LIN)]. E-mail: edualm@usp.br; Leite, Laudi C.; Lanna, Dante P.D. [Escola Superior de Agricultura ' Luiz de Queiroz' (ESALQ/USP), Piracicaba, SP (Brazil). Dept. de Zootecnia. Lab. de Anatomia e Fisiologia Animal (LAFA)]. E-mail: lcleite@ciagri.usp.br

    2007-07-01

    The Co element is used in nutritional studies as marker. This paper describes an analytical methodology for Co determination in rumen liquid sample using energy dispersive X-ray spectrometry (EDXRF). 200 {mu}L of the sample were dried at 60 deg C on 6.35 {mu}m Mylar film. Ga was used as internal standard. The excitation was carried out utilizing Mo target X-ray tube (Zr filter) at 30 kV / 20 mA. The acquisition time was 200 s. The accuracy of this methodology was assessed through standard addition method, the recovery obtained was 98.7 % for Co. The detection limit was 0.15 mg / L for this element. (author)

  17. Co marker determination in rumen liquid sample by energy dispersive X-ray fluorescence

    International Nuclear Information System (INIS)

    Almeida, Eduardo de; Nascimento Filho, Virgilio F.; Massoni, Paulo R.; Leite, Laudi C.; Lanna, Dante P.D.

    2007-01-01

    The Co element is used in nutritional studies as marker. This paper describes an analytical methodology for Co determination in rumen liquid sample using energy dispersive X-ray spectrometry (EDXRF). 200 μL of the sample were dried at 60 deg C on 6.35 μm Mylar film. Ga was used as internal standard. The excitation was carried out utilizing Mo target X-ray tube (Zr filter) at 30 kV / 20 mA. The acquisition time was 200 s. The accuracy of this methodology was assessed through standard addition method, the recovery obtained was 98.7 % for Co. The detection limit was 0.15 mg / L for this element. (author)

  18. Electro-optical properties of low viscosity driven holographic polymer dispersed liquid crystals

    Science.gov (United States)

    Moon, K. R.; Bae, S. Y.; Kim, B. K.

    2015-04-01

    Relative diffraction efficiency (RDE), operating voltage, and response times are most important performance characteristics of holographic polymer dispersed liquid crystals (HPDLC). Two types of triallyl isocyanurate (TI) having different structures were incorporated into the conventional transmission grating of HPDLC. Premix viscosity decreased by 13-18% with up to 3% TI, beyond which it increased. TI eliminated induction period and augmented initial grating formation rate at all contents. Saturation RDE increased over 200% while threshold voltage and rise time decreased to about half and 2/3, respectively up to 3% TI, beyond which the tendencies were reversed. Among the two TIs, low viscosity monomer (TA) showed high RDE, while high miscibility monomer (TE) low characteristic voltages and short response times. It is concluded that grating formation is largely favored by low viscosity, while interface tensions and electro-optical performances by miscibility at similar viscosities.

  19. Resolving dispersion and induction components for polarisable molecular simulations of ionic liquids

    Science.gov (United States)

    Pádua, Agílio A. H.

    2017-05-01

    One important development in interaction potential models, or atomistic force fields, for molecular simulation is the inclusion of explicit polarisation, which represents the induction effects of charged or polar molecules on polarisable electron clouds. Polarisation can be included through fluctuating charges, induced multipoles, or Drude dipoles. This work uses Drude dipoles and is focused on room-temperature ionic liquids, for which fixed-charge models predict too slow dynamics. The aim of this study is to devise a strategy to adapt existing non-polarisable force fields upon addition of polarisation, because induction was already contained to an extent, implicitly, due to parametrisation against empirical data. Therefore, a fraction of the van der Waals interaction energy should be subtracted so that the Lennard-Jones terms only account for dispersion and the Drude dipoles for induction. Symmetry-adapted perturbation theory is used to resolve the dispersion and induction terms in dimers and to calculate scaling factors to reduce the Lennard-Jones terms from the non-polarisable model. Simply adding Drude dipoles to an existing fixed-charge model already improves the prediction of transport properties, increasing diffusion coefficients, and lowering the viscosity. Scaling down the Lennard-Jones terms leads to still faster dynamics and densities that match experiment extremely well. The concept developed here improves the overall prediction of density and transport properties and can be adapted to other models and systems. In terms of microscopic structure of the ionic liquids, the inclusion of polarisation and the down-scaling of Lennard-Jones terms affect only slightly the ordering of the first shell of counterions, leading to small decreases in coordination numbers. Remarkably, the effect of polarisation is major beyond first neighbours, significantly weakening spatial correlations, a structural effect that is certainly related to the faster dynamics of

  20. Pharmaceutical Perspective on Opalescence and Liquid-Liquid Phase Separation in Protein Solutions.

    Science.gov (United States)

    Raut, Ashlesha S; Kalonia, Devendra S

    2016-05-02

    Opalescence in protein solutions reduces aesthetic appeal of a formulation and can be an indicator of the presence of aggregates or precursor to phase separation in solution signifying reduced product stability. Liquid-liquid phase separation of a protein solution into a protein-rich and a protein-poor phase has been well-documented for globular proteins and recently observed for monoclonal antibody solutions, resulting in physical instability of the formulation. The present review discusses opalescence and liquid-liquid phase separation (LLPS) for therapeutic protein formulations. A brief discussion on theoretical concepts based on thermodynamics, kinetics, and light scattering is presented. This review also discusses theoretical concepts behind intense light scattering in the vicinity of the critical point termed as "critical opalescence". Both opalescence and LLPS are affected by the formulation factors including pH, ionic strength, protein concentration, temperature, and excipients. Literature reports for the effect of these formulation factors on attractive protein-protein interactions in solution as assessed by the second virial coefficient (B2) and the cloud-point temperature (Tcloud) measurements are also presented. The review also highlights pharmaceutical implications of LLPS in protein solutions.

  1. Effect of ionic liquids on the dispersion of zinc oxide and silica nanoparticles, vulcanisation behaviour and properties of NBR composites

    Directory of Open Access Journals (Sweden)

    M. Maciejewska

    2014-12-01

    Full Text Available The aim of this work was to study the activity of several alkylpyrrolidinium, alkylpyridinium, alkylpiperidinium and benzylimidazolium ionic liquids (ILs for the purpose of improving the dispersion degree of vulcanisation activator and filler nanoparticles in the acrylonitrile-butadiene elastomer (NBR. The effect of the ionic liquids on the vulcanisation kinetics of the rubber compounds, crosslink density and mechanical properties of the vulcanisates and their resistance to thermo-oxidative and UV ageing was studied. The use of ionic liquids allowed for a homogeneous dispersion of nanoparticles in the elastomer without detrimental effects on the vulcanisation process. The physical properties and the thermal stability of the obtained vulcanisates were significantly improved. Ionic liquids increased the crosslink density of the vulcanisates and their damping properties. Pirydinium and piperidinium hexafluorophosphates were most effective at increasing the crosslink density and improving the properties of NBR composites.

  2. Determination of Organophosphorus Pesticides in Soil by Dispersive Liquid–Liquid Microextraction and Gas Chromatography

    Science.gov (United States)

    Yang, Zhonghua; Liu, Yu; Liu, Donghui; Zhou, Zhiqiang

    2012-01-01

    In this article, a rapid and sensitive sample pretreatment technique for the determination of organophosphorus pesticides (OPPs) in soil samples is developed by using dispersive liquid–liquid microextraction (DLLME) combined with gas chromatography–flame photometric detection. Experimental conditions, including the kind of extraction and disperser solvent and their volumes, the extraction time, and the salt addition, are investigated, and the following experiment factors are used: 20 µL chlorobenzene as the extraction solvent; 1.0 mL acetonitrile as the disperser solvent; no addition of salt; and an extraction time of 1 min. Under the optimum conditions, the linearities for the three target OPPs (ethoprophos, chlorpyriphos, and profenofos) are obtained by five points in the concentration range of 2.5–1500 µg/kg, and three replicates are used for each point. Correlation coefficients vary from 0.9987 to 0.9997. The repeatability is tested by spiking soil samples at a concentration level of 5.0 µg/kg. The relative standard deviation (n = 3) varied between 2.0% and 6.6%. The limits of detection, based on a signal-to-noise ratio (S/N) of 3, range from 200 to 500 pg/g. This method is applied to the analysis of the spiked samples S1, S2, and S3, which are collected from the China Agriculture University's orchard, lawn, and garden, respectively. The recoveries for each target analyte are in the range between 87.9% and 108.0%, 87.4% and 108.0%, and 86.7% and 107.2%, respectively. PMID:22291051

  3. A fully automated effervescence assisted dispersive liquid–liquid microextraction based on a stepwise injection system. Determination of antipyrine in saliva samples

    International Nuclear Information System (INIS)

    Medinskaia, Kseniia; Vakh, Christina; Aseeva, Darina; Andruch, Vasil; Moskvin, Leonid; Bulatov, Andrey

    2016-01-01

    A first attempt to automate the effervescence assisted dispersive liquid–liquid microextraction (EA-DLLME) has been reported. The method is based on the aspiration of a sample and all required aqueous reagents into the stepwise injection analysis (SWIA) manifold, followed by simultaneous counterflow injection of the extraction solvent (dichloromethane), the mixture of the effervescence agent (0.5 mol L"−"1 Na_2CO_3) and the proton donor solution (1 mol L"−"1 CH_3COOH). Formation of carbon dioxide microbubbles generated in situ leads to the dispersion of the extraction solvent in the whole aqueous sample and extraction of the analyte into organic phase. Unlike the conventional DLLME, in the case of EA-DLLME, the addition of dispersive solvent, as well as, time consuming centrifugation step for disruption of the cloudy state is avoided. The phase separation was achieved by gentle bubbling of nitrogen stream (2 mL min"−"1 during 2 min). The performance of the suggested approach is demonstrated by determination of antipyrine in saliva samples. The procedure is based on the derivatization of antipyrine by nitrite-ion followed by EA-DLLME of 4-nitrosoantipyrine and subsequent UV–Vis detection using SWIA manifold. The absorbance of the yellow-colored extract at the wavelength of 345 nm obeys Beer's law in the range of 1.5–100 µmol L"−"1 of antipyrine in saliva. The LOD, calculated from a blank test based on 3σ, was 0.5 µmol L"−"1. - Highlights: • First attempt to automate the effervescence assisted dispersive liquid–liquid microextraction. • Automation based on Stepwise injection analysis manifold in flow batch system. • Counterflow injection of extraction solvent and the effervescence agent. • Phase separation performed by gentle bubbling of nitrogen. • Application for the determination of antipyrine in saliva samples.

  4. Speciation of mercury in water samples by dispersive liquid-liquid microextraction combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Jia Xiaoyu; Han Yi; Liu Xinli [State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Science, Changchun 130022 (China); Graduate School of Chinese Academy of Sciences, Beijing 100039 (China); Duan Taicheng, E-mail: tcduan@ciac.jl.cn [State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Science, Changchun 130022 (China); Chen Hangting, E-mail: htchen@ciac.jl.cn [State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Science, Changchun 130022 (China)

    2011-01-15

    The dispersive liquid-liquid microextraction (DLLME) combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry for the speciation of mercury in water samples was described. Firstly methylmercury (MeHg{sup +}) and mercury (Hg{sup 2+}) were complexed with sodium diethyldithiocarbamate, and then the complexes were extracted into carbon tetrachloride by using DLLME. Under the optimized conditions, the enrichment factors of 138 and 350 for MeHg{sup +} and Hg{sup 2+} were obtained from only 5.00 mL sample solution. The detection limits of the analytes (as Hg) were 0.0076 ng mL{sup -1} for MeHg{sup +} and 0.0014 ng mL{sup -1} for Hg{sup 2+}, respectively. The relative standard deviations for ten replicate measurements of 0.5 ng mL{sup -1} MeHg{sup +} and Hg{sup 2+} were 6.9% and 4.4%, respectively. Standard reference material of seawater (GBW(E)080042) was analyzed to verify the accuracy of the method and the results were in good agreement with the certified values. Finally, the developed method was successfully applied for the speciation of mercury in three environmental water samples.

  5. Simultaneous determination of six synthetic phenolic antioxidants in edible oils using dispersive liquid-liquid microextraction followed by high-performance liquid chromatography with diode array detection.

    Science.gov (United States)

    Xu, Shuangjiao; Liu, Liangliang; Wang, Yanqin; Zhou, Dayun; Kuang, Meng; Fang, Dan; Yang, Weihua; Wei, Shoujun; Xiao, Aiping; Ma, Lei

    2016-08-01

    A simple, rapid, organic-solvent- and sample-saving pretreatment technique, called dispersive liquid-liquid microextraction, was developed for the determination of six synthetic phenolic antioxidants from edible oils before high-performance liquid chromatography with diode array detection. The entire procedure was composed of a two-step microextraction and a centrifugal process and could be finished in about 5 min, only consuming only 25 mg of sample and 1 mL of the organic solvent for each extraction. The influences of several important parameters on the microextraction efficiency were thoroughly investigated. Recovery assays for oil samples were spiked at three concentration levels, 50, 100 and 200 mg/kg, and provided recoveries in the 86.3-102.5% range with a relative standard deviation below 3.5%. The intra-day and inter-day precisions for the analysis were less than 3.8%. The proposed method was successfully applied for the determination of synthetic phenolic antioxidants in different oil samples, and satisfactory results were obtained. Thus, the developed method represents a viable alternative for the quality control of synthetic phenolic antioxidant concentrations in edible oils. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Sensitive determination of melamine in milk and powdered infant formula samples by high-performance liquid chromatography using dabsyl chloride derivatization followed by dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Faraji, M; Adeli, M

    2017-04-15

    A new and sensitive pre-column derivatization with dabsyl chloride followed by dispersive liquid-liquid microextraction was developed for the analysis of melamine (MEL) in raw milk and powdered infant formula samples by high performance liquid chromatography (HPLC) with visible detection. Derivatization with dabsyl chloride leads to improving sensitivity and hydrophobicity of MEL. Under optimum conditions of derivatization and microextraction steps, the method yielded a linear calibration curve ranging from 1.0 to 500μgL -1 with a determination coefficient (R 2 ) of 0.9995. Limit of detection and limit of quantification were 0.1 and 0.3μgL -1 , respectively. The relative standard deviation (RSD%) for intra-day (repeatability) and inter-day (reproducibility) at 25 and 100μgL -1 levels of MEL was less than 7.0% (n=6). Finally, the proposed method was successfully applied for the preconcentration and determination of MEL in different raw milk and powdered infant formula, and satisfactory results were obtained (relative recovery ⩾94%). Copyright © 2016 Elsevier Ltd. All rights reserved.

  7. 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.

  8. Facile and sensitive determination of N-nitrosamines in food samples by high-performance liquid chromatography via combining fluorescent labeling with dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Lu, Shuaimin; Wu, Di; Li, Guoliang; Lv, Zhengxian; Gong, Peiwei; Xia, Lian; Sun, Zhiwei; Chen, Guang; Chen, Xuefeng; You, Jinmao; Wu, Yongning

    2017-11-01

    The intake of N-nitrosamines (NAs) from foodstuffs is considered to be an important influence factor for several cancers. But the rapid and sensitive screening of NAs remains a challenge in the field of food safety. Inspired by that, a sensitive and rapid method was demonstrated for determination of five NAs (Nitrosopyrrolidine, Nitrosodimethylamine, Nitrosodiethylamine, Nitrosodipropylamine and Nitrosodibutylamine) using dispersive liquid-liquid microextraction (DLLME) followed by high-performance liquid chromatography with fluorescence detection (HPLC-FLD). The NAs were firstly denitrosated and labeled by 2-(11H-benzo[a]carbazol-11-yl) ethyl carbonochloridate (BCEC-Cl) and finally enriched by DLLME. Furthermore, the main DLLME conditions were optimized systematically. Under the optimal conditions, satisfactory limits of detection (LODs) were obtained with a range of 0.01-0.07ngg -1 , which were significantly lower than the reported methods. The developed method showed many merits including rapidity, simplicity, high sensitivity and excellent selectivity, which shows a broad prospect in food safety analysis. Copyright © 2017 Elsevier Ltd. All rights reserved.

  9. Speciation of mercury in water samples by dispersive liquid-liquid microextraction combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Jia Xiaoyu; Han Yi; Liu Xinli; Duan Taicheng; Chen Hangting

    2011-01-01

    The dispersive liquid-liquid microextraction (DLLME) combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry for the speciation of mercury in water samples was described. Firstly methylmercury (MeHg + ) and mercury (Hg 2+ ) were complexed with sodium diethyldithiocarbamate, and then the complexes were extracted into carbon tetrachloride by using DLLME. Under the optimized conditions, the enrichment factors of 138 and 350 for MeHg + and Hg 2+ were obtained from only 5.00 mL sample solution. The detection limits of the analytes (as Hg) were 0.0076 ng mL -1 for MeHg + and 0.0014 ng mL -1 for Hg 2+ , respectively. The relative standard deviations for ten replicate measurements of 0.5 ng mL -1 MeHg + and Hg 2+ were 6.9% and 4.4%, respectively. Standard reference material of seawater (GBW(E)080042) was analyzed to verify the accuracy of the method and the results were in good agreement with the certified values. Finally, the developed method was successfully applied for the speciation of mercury in three environmental water samples.

  10. Dispersion theory and sum rules for the non-minimum phase problem in optical spectroscopy

    International Nuclear Information System (INIS)

    Peiponen, Kai-Erik

    2009-01-01

    Dispersion relations and sum rules for integer powers of an optical response function are given in the case of the non-minimum phase problem. These relations were obtained using the concept of the Hilbert transform and Blaschke product. The theory presented in this paper is useful both in basic and applied studies of non-minimum phase functions in optics, and also other fields of physics such as high energy physics.

  11. Immobilization of molecular catalysts in supported ionic liquid phases.

    Science.gov (United States)

    Van Doorslaer, Charlie; Wahlen, Joos; Mertens, Pascal; Binnemans, Koen; De Vos, Dirk

    2010-09-28

    In a supported ionic liquid phase (SILP) catalyst system, an ionic liquid (IL) film is immobilized on a high-surface area porous solid and a homogeneous catalyst is dissolved in this supported IL layer, thereby combining the attractive features of homogeneous catalysts with the benefits of heterogeneous catalysts. In this review reliable strategies for the immobilization of molecular catalysts in SILPs are surveyed. In the first part, general aspects concerning the application of SILP catalysts are presented, focusing on the type of catalyst, support, ionic liquid and reaction conditions. Secondly, organic reactions in which SILP technology is applied to improve the performance of homogeneous transition-metal catalysts are presented: hydroformylation, metathesis reactions, carbonylation, hydrogenation, hydroamination, coupling reactions and asymmetric reactions.

  12. Effect of a Polymercaptan Material on the Electro-Optical Properties of Polymer-Dispersed Liquid Crystal Films

    OpenAIRE

    Yujian Sun; Cuihong Zhang; Le Zhou; Hua Fang; Jianhua Huang; Haipeng Ma; Yi Zhang; Jie Yang; Lan-Ying Zhang; Ping Song; Yanzi Gao; Jiumei Xiao; Fasheng Li; Kexuan Li

    2016-01-01

    Polymer-dispersed liquid crystal (PDLC) films were prepared by the ultraviolet-light-induced polymerization of photopolymerizable monomers in nematic liquid crystal/chiral dopant/thiol-acrylate reaction monomer composites. The effects of the chiral dopant and crosslinking agents on the electro-optical properties of the PDLC films were systematically investigate. While added the chiral dopant S811 into the PDLC films, the initial off-state transmittance of the films was decreased. It was found...

  13. Dispersive solid-phase imprinting of proteins for the production of plastic antibodies

    DEFF Research Database (Denmark)

    Ashley, Jon; Feng, Xiaotong; Halder, Arnab

    2018-01-01

    We describe a novel dispersive solid-phase imprinting technique for the production of nano-sized molecularly imprinted polymers (nanoMIPs) as plastic antibodies. The template was immobilized on in-house synthesized magnetic microspheres instead of conventional glass beads. As a result, high...

  14. Does nanoparticles dispersed in a phase change material improve melting characteristics?

    NARCIS (Netherlands)

    Farsani, Rouhollah Yadollahi; Raisi, Afrasiab; Nadooshan, Afshin Ahmadi; Vanapalli, Srinivas

    2017-01-01

    Nanoparticles dispersed in a phase change material alter the thermo-physical properties of the base material, such as thermal conductivity, viscosity, and specific heat capacity. These properties combined with the configuration of the cavity, and the location of the heat source, influence the

  15. Rapid and sensitive analysis of polychlorinated biphenyls and acrylamide in food samples using ionic liquid-based in situ dispersive liquid-liquid microextraction coupled to headspace gas chromatography.

    Science.gov (United States)

    Zhang, Cheng; Cagliero, Cecilia; Pierson, Stephen A; Anderson, Jared L

    2017-01-20

    A simple and rapid ionic liquid (IL)-based in situ dispersive liquid-liquid microextraction (DLLME) method was developed and coupled to headspace gas chromatography (HS-GC) employing electron capture (ECD) and mass spectrometry (MS) detection for the analysis of polychlorinated biphenyls (PCBs) and acrylamide at trace levels from milk and coffee samples. The chemical structures of the halide-based ILs were tailored by introducing various functional groups to the cations to evaluate the effect of different structural features on the extraction efficiency of the target analytes. Extraction parameters including the molar ratio of IL to metathesis reagent and IL mass were optimized. The effects of HS oven temperature and the HS sample vial volume on the analyte response were also evaluated. The optimized in situ DLLME method exhibited good analytical precision, good linearity, and provided detection limits down to the low ppt level for PCBs and the low ppb level for acrylamide in aqueous samples. The matrix-compatibility of the developed method was also established by quantifying acrylamide in brewed coffee samples. This method is much simpler and faster compared to previously reported GC-MS methods using solid-phase microextraction (SPME) for the extraction/preconcentration of PCBs and acrylamide from complex food samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. A software to measure phase-velocity dispersion from ambient-noise correlations and its application to the SNSN data

    Science.gov (United States)

    Sadeghisorkhani, Hamzeh; Gudmundsson, Ólafur

    2017-04-01

    Graphical software for phase-velocity dispersion measurements of surface waves in noise-correlation traces, called GSpecDisp, is presented. It is an interactive environment for the measurements and presentation of the results. It measures phase-velocity dispersion curves in the frequency domain based on matching of the real part of the cross-correlation spectrum with the appropriate Bessel function. The inputs are time-domain cross-correlations in SAC format. It can measure two types of phase-velocity dispersion curves; 1- average phase-velocity of a region, and 2- single-pair phase velocity. The average phase-velocity dispersion curve of a region can be used as a reference curve to automatically select the dispersion curves from each single-pair cross-correlation in that region. It also allows the users to manually refine the selections. Therefore, no prior knowledge is needed for an unknown region. GSpecDisp can measure the phase velocity of Rayleigh and Love waves from all possible components of the noise correlation tensor, including diagonal and off-diagonal components of the tensor. First, we explain how GSpecDisp is applied to measure phase-velocity dispersion curves. Then, we demonstrate measurement results on synthetic and real data from the Swedish National Seismic Network (SNSN). We compare the results with two other methods of phase-velocity dispersion measurements. Finally, we compare phase-velocity dispersion curves of Rayleigh waves obtained from different components of the correlation tensor.

  17. Group-velocity dispersion effects on quantum noise of a fiber optical soliton in phase space

    International Nuclear Information System (INIS)

    Ju, Heongkyu; Lee, Euncheol

    2010-01-01

    Group-velocity dispersion (GVD) effects on quantum noise of ultrashort pulsed light are theoretically investigated at the soliton energy level, using Gaussian-weighted pseudo-random distribution of phasors in phase space for the modeling of quantum noise properties including phase noise, photon number noise, and quantum noise shape in phase space. We present the effects of GVD that mixes the different spectral components in time, on the self-phase modulation(SPM)-induced quantum noise properties in phase space such as quadrature squeezing, photon-number noise, and tilting/distortion of quantum noise shape in phase space, for the soliton that propagates a distance of the nonlinear length η NL = 1/( γP 0 ) (P 0 is the pulse peak power and γ is the SPM parameter). The propagation dependence of phase space quantum noise properties for an optical soliton is also provided.

  18. 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.

  19. Characterization of ultrashort laser pulses employing self-phase modulation dispersion-scan technique

    Science.gov (United States)

    Sharba, A. B.; Chekhlov, O.; Wyatt, A. S.; Pattathil, R.; Borghesi, M.; Sarri, G.

    2018-03-01

    We present a new phase characterization technique for ultrashort laser pulses that employs self-phase modulation (SPM) in the dispersion scan approach. The method can be implemented by recording a set of nonlinearly modulated spectra generated with a set of known chirp values. The unknown phase of the pulse is retrieved by linking the recorded spectra to the initial spectrum of the pulse via a phase function guessed by a function minimization iterative algorithm. This technique has many advantages over the dispersion scan techniques that use frequency conversion processes. Mainly, the use of SPM cancels out the phase and group velocity mismatch errors and dramatically widens the spectral acceptance of the nonlinear medium and the range of working wavelength. The robustness of the technique is demonstrated with smooth and complex phase retrievals using numerical examples. The method is shown to be not affected by the spatial distribution of the beam or the presence of nonlinear absorption process. In addition, we present an efficient method for phase representation based on a summation of a set of Gaussian functions. The independence of the functions from each other prevents phase coupling of any kind and facilitates a flexible phase representation.

  20. Effects of gold nanoparticles on the electro-optical properties of a polymer dispersed liquid crystal

    Science.gov (United States)

    Hinojosa, A.; Shive, C.; Sharma, Suresh

    2010-03-01

    We have studied the electro-optical properties of a polymer-dispersed liquid crystal (PDLC) as functions of relative concentrations of gold nanoparticles. PDLC samples were synthesized between indium-tin-oxide (ITO) coated glass slides, separated by SiO2 spacers, by using liquid crystal E44, a monofunctional acrylic oligomer (CN135), and a tetrafunctional crosslinker (SR295). A UV photoinitiator (SR1124) was used to facilitate the curing of the monomer exposed to UV radiation from a Hg spectral lamp. A He-Ne laser was used to measure optical transmission through the PDLC as a function of applied ac electric field (1 kHz). The PDLC without gold nanoparticles shows the expected behavior; transmission through the PDLC increases from a minimum (opaque) to a maximum (transparent) with increasing electric field. The electro-optical behavior of the PDLC is altered significantly (e. g., relatively low switching field) upon addition of relatively low concentrations of gold nanoparticles into the starting PDLC syrup. We present electro-optical data as functions of gold nanoparticle concentration and discuss possible mechanism to understand our results.

  1. Problems of selectivity in liquid-phase oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Emanuel, N M

    1978-07-01

    Based on a kinetic analysis of a generalized scheme for radical-chain process and on published experimental results, factors determining the selectivities of various liquid-phase oxidations of organic compounds are examined, including the kinetic chain length, molecular and chain decomposition of products, and competing routes in the initiated oxidation or autoxidation of hydrocarbons to peroxides. Also discussed are selective inhibition of undesirable routes in chain reactions, e.g., styrene and acetaldehyde co-oxidation; activation of molecular oxygen by variable-valence metal compounds used as homogeneous catalysts; modeling of fermentative processes by oxidation of hydrocarbons in complex catalytic systems, e.g., hydroxylation of alkanes, epoxidation or carbonylation of olefins, or oxidation of alcohols and ketones to acids; and the mechanisms of heterogeneous catalysis