Integrated microreactor for enzymatic reaction automation: An easy step toward the quality control of monoclonal antibodies.

PubMed

Ladner, Yoann; Mas, Silvia; Coussot, Gaelle; Bartley, Killian; Montels, Jérôme; Morel, Jacques; Perrin, Catherine

2017-12-15

The main purpose of the present work is to provide a fully integrated miniaturized electrophoretic methodology in order to facilitate the quality control of monoclonal antibodies (mAbs). This methodology called D-PES, which stands for Diffusion-mediated Proteolysis combined with an Electrophoretic Separation, permits to perform subsequently mAb tryptic digestion and electrophoresis separation of proteolysis products in an automated manner. Tryptic digestion conditions were optimized regarding the influence of enzyme concentration and incubation time in order to achieve similar enzymatic digestion efficiency to that obtained with the classical methodology (off-line). Then, the optimization of electrophoretic separation conditions concerning the nature of background electrolyte (BGE), ionic strength and pH was realized. Successful and repeatable electrophoretic profiles of three mAbs digests (Trastuzumab, Infliximab and Tocilizumab), comparable to the off-line digestion profiles, were obtained demonstrating the feasibility and robustness of the proposed methodology. In summary, the use of the proposed and optimized in-line approach opens a new, fast and easy way for the quality control of mAbs. Copyright © 2017 Elsevier B.V. All rights reserved.

Biologically driven neural platform invoking parallel electrophoretic separation and urinary metabolite screening.

PubMed

Page, Tessa; Nguyen, Huong Thi Huynh; Hilts, Lindsey; Ramos, Lorena; Hanrahan, Grady

2012-06-01

This work reveals a computational framework for parallel electrophoretic separation of complex biological macromolecules and model urinary metabolites. More specifically, the implementation of a particle swarm optimization (PSO) algorithm on a neural network platform for multiparameter optimization of multiplexed 24-capillary electrophoresis technology with UV detection is highlighted. Two experimental systems were examined: (1) separation of purified rabbit metallothioneins and (2) separation of model toluene urinary metabolites and selected organic acids. Results proved superior to the use of neural networks employing standard back propagation when examining training error, fitting response, and predictive abilities. Simulation runs were obtained as a result of metaheuristic examination of the global search space with experimental responses in good agreement with predicted values. Full separation of selected analytes was realized after employing optimal model conditions. This framework provides guidance for the application of metaheuristic computational tools to aid in future studies involving parallel chemical separation and screening. Adaptable pseudo-code is provided to enable users of varied software packages and modeling framework to implement the PSO algorithm for their desired use.

Advanced air revitalization for optimized crew and plant environments

NASA Technical Reports Server (NTRS)

Lee, M. G.; Grigger, David J.; Brown, Mariann F.

1991-01-01

The Hybrid Air Revitalization System (HARS) closed ecosystem concept presented encompasses electrochemical CO2 and O2 separators, in conjunction with a mechanical condenser/separator for maintaining CO2, O2, and humidity levels in crew and plant habitats at optimal conditions. HARS requires no expendables, and allows flexible process control on the bases of electrochemical cell current, temperature, and airflow rate variations. HARS capacity can be easily increased through the incorporation of additional chemical cells. Detailed system flowcharts are provided.

Interior and exterior ballistics coupled optimization with constraints of attitude control and mechanical-thermal conditions

NASA Astrophysics Data System (ADS)

Liang, Xin-xin; Zhang, Nai-min; Zhang, Yan

2016-07-01

For solid launch vehicle performance promotion, a modeling method of interior and exterior ballistics associated optimization with constraints of attitude control and mechanical-thermal condition is proposed. Firstly, the interior and external ballistic models of the solid launch vehicle are established, and the attitude control model of the high wind area and the stage of the separation is presented, and the load calculation model of the drag reduction device is presented, and thermal condition calculation model of flight is presented. Secondly, the optimization model is established to optimize the range, which has internal and external ballistic design parameters as variables selected by sensitivity analysis, and has attitude control and mechanical-thermal conditions as constraints. Finally, the method is applied to the optimal design of a three stage solid launch vehicle simulation with differential evolution algorithm. Simulation results are shown that range capability is improved by 10.8%, and both attitude control and mechanical-thermal conditions are satisfied.

Liquid-Desiccant Vapor Separation Reduces the Energy Requirements of Atmospheric Moisture Harvesting.

PubMed

Gido, Ben; Friedler, Eran; Broday, David M

2016-08-02

An innovative atmospheric moisture harvesting system is proposed, where water vapor is separated from the air prior to cooling and condensation. The system was studied using a model that simulates its three interconnected cycles (air, desiccant, and water) over a range of ambient conditions, and optimal configurations are reported for different operation conditions. Model results were compared to specifications of commercial atmospheric moisture harvesting systems and found to represent saving of 5-65% of the electrical energy requirements due to the vapor separation process. We show that the liquid desiccant separation stage that is integrated into atmospheric moisture harvesting systems can work under a wide range of environmental conditions using low grade or solar heating as a supplementary energy source, and that the performance of the combined system is superior.

Rapid Method Development in Hydrophilic Interaction Liquid Chromatography for Pharmaceutical Analysis Using a Combination of Quantitative Structure-Retention Relationships and Design of Experiments.

PubMed

Taraji, Maryam; Haddad, Paul R; Amos, Ruth I J; Talebi, Mohammad; Szucs, Roman; Dolan, John W; Pohl, Chris A

2017-02-07

A design-of-experiment (DoE) model was developed, able to describe the retention times of a mixture of pharmaceutical compounds in hydrophilic interaction liquid chromatography (HILIC) under all possible combinations of acetonitrile content, salt concentration, and mobile-phase pH with R 2 > 0.95. Further, a quantitative structure-retention relationship (QSRR) model was developed to predict retention times for new analytes, based only on their chemical structures, with a root-mean-square error of prediction (RMSEP) as low as 0.81%. A compound classification based on the concept of similarity was applied prior to QSRR modeling. Finally, we utilized a combined QSRR-DoE approach to propose an optimal design space in a quality-by-design (QbD) workflow to facilitate the HILIC method development. The mathematical QSRR-DoE model was shown to be highly predictive when applied to an independent test set of unseen compounds in unseen conditions with a RMSEP value of 5.83%. The QSRR-DoE computed retention time of pharmaceutical test analytes and subsequently calculated separation selectivity was used to optimize the chromatographic conditions for efficient separation of targets. A Monte Carlo simulation was performed to evaluate the risk of uncertainty in the model's prediction, and to define the design space where the desired quality criterion was met. Experimental realization of peak selectivity between targets under the selected optimal working conditions confirmed the theoretical predictions. These results demonstrate how discovery of optimal conditions for the separation of new analytes can be accelerated by the use of appropriate theoretical tools.

Mixture class recovery in GMM under varying degrees of class separation: frequentist versus Bayesian estimation.

PubMed

Depaoli, Sarah

2013-06-01

Growth mixture modeling (GMM) represents a technique that is designed to capture change over time for unobserved subgroups (or latent classes) that exhibit qualitatively different patterns of growth. The aim of the current article was to explore the impact of latent class separation (i.e., how similar growth trajectories are across latent classes) on GMM performance. Several estimation conditions were compared: maximum likelihood via the expectation maximization (EM) algorithm and the Bayesian framework implementing diffuse priors, "accurate" informative priors, weakly informative priors, data-driven informative priors, priors reflecting partial-knowledge of parameters, and "inaccurate" (but informative) priors. The main goal was to provide insight about the optimal estimation condition under different degrees of latent class separation for GMM. Results indicated that optimal parameter recovery was obtained though the Bayesian approach using "accurate" informative priors, and partial-knowledge priors showed promise for the recovery of the growth trajectory parameters. Maximum likelihood and the remaining Bayesian estimation conditions yielded poor parameter recovery for the latent class proportions and the growth trajectories. (PsycINFO Database Record (c) 2013 APA, all rights reserved).

Investigation of aerodynamic design issues with regions of separated flow

NASA Technical Reports Server (NTRS)

Gally, Tom

1993-01-01

Existing aerodynamic design methods have generally concentrated on the optimization of airfoil or wing shapes to produce a minimum drag while satisfying some basic constraints such as lift, pitching moment, or thickness. Since the minimization of drag almost always precludes the existence of separated flow, the evaluation and validation of these design methods for their robustness and accuracy when separated flow is present has not been aggressively pursued. However, two new applications for these design tools may be expected to include separated flow and the issues of aerodynamic design with this feature must be addressed. The first application of the aerodynamic design tools is the design of airfoils or wings to provide an optimal performance over a wide range of flight conditions (multipoint design). While the definition of 'optimal performance' in the multipoint setting is currently being hashed out, it is recognized that given a wide range of flight conditions, it will not be possible to ensure a minimum drag constraint at all conditions, and in fact some amount of separated flow (presumably small) may have to be allowed at the more demanding flight conditions. Thus a multipoint design method must be tolerant of the existence of separated flow and may include some controls upon its extent. The second application is in the design of wings with extended high speed buffet boundaries of their flight envelopes. Buffet occurs on a wing when regions of flow separation have grown to the extent that their time varying pressures induce possible destructive effects upon the wing structure or adversely effect either the aircraft controllability or passenger comfort. A conservative approach to the expansion of the buffet flight boundary is to simply expand the flight envelope of nonseparated flow under the assumption that buffet will also thus be alleviated. However, having the ability to design a wing with separated flow and thus to control the location, extent and severity of the separated flow regions may allow aircraft manufacturers to gain an advantage in the early design stages of an aircraft, when configuration changes are relatively inexpensive to make. The goal of the summer research at NASA Langley Research Center (LaRC) was twofold: first, to investigate a particular airfoil design problem observed under conditions of strong shock induced flow separation on the upper surface of an airfoil at transonic conditions; and second, to suggest and investigate design methodologies for the prediction (or detection) and control of flow separation. The context of both investigations was to use an existing two dimensional Navier-Stokes flow solver and the constrained direct/iterative surface curvature (CDISC) design algorithm developed at LaRC. As a lead in to the primary task, it was necessary to gain a familiarity with both the design method and the computational analysis and to perform the FORTRAN coding needed to couple them together.

Optimal starting conditions for the rendezvous maneuver: Analytical and computational approach

NASA Astrophysics Data System (ADS)

Ciarcia, Marco

The three-dimensional rendezvous between two spacecraft is considered: a target spacecraft on a circular orbit around the Earth and a chaser spacecraft initially on some elliptical orbit yet to be determined. The chaser spacecraft has variable mass, limited thrust, and its trajectory is governed by three controls, one determining the thrust magnitude and two determining the thrust direction. We seek the time history of the controls in such a way that the propellant mass required to execute the rendezvous maneuver is minimized. Two cases are considered: (i) time-to-rendezvous free and (ii) time-to-rendezvous given, respectively equivalent to (i) free angular travel and (ii) fixed angular travel for the target spacecraft. The above problem has been studied by several authors under the assumption that the initial separation coordinates and the initial separation velocities are given, hence known initial conditions for the chaser spacecraft. In this paper, it is assumed that both the initial separation coordinates and initial separation velocities are free except for the requirement that the initial chaser-to-target distance is given so as to prevent the occurrence of trivial solutions. Two approaches are employed: optimal control formulation (Part A) and mathematical programming formulation (Part B). In Part A, analyses are performed with the multiple-subarc sequential gradient-restoration algorithm for optimal control problems. They show that the fuel-optimal trajectory is zero-bang, namely it is characterized by two subarcs: a long coasting zero-thrust subarc followed by a short powered max-thrust braking subarc. While the thrust direction of the powered subarc is continuously variable for the optimal trajectory, its replacement with a constant (yet optimized) thrust direction produces a very efficient guidance trajectory. Indeed, for all values of the initial distance, the fuel required by the guidance trajectory is within less than one percent of the fuel required by the optimal trajectory. For the guidance trajectory, because of the replacement of the variable thrust direction of the powered subarc with a constant thrust direction, the optimal control problem degenerates into a mathematical programming problem with a relatively small number of degrees of freedom, more precisely: three for case (i) time-to-rendezvous free and two for case (ii) time-to-rendezvous given. In particular, we consider the rendezvous between the Space Shuttle (chaser) and the International Space Station (target). Once a given initial distance SS-to-ISS is preselected, the present work supplies not only the best initial conditions for the rendezvous trajectory, but simultaneously the corresponding final conditions for the ascent trajectory. In Part B, an analytical solution of the Clohessy-Wiltshire equations is presented (i) neglecting the change of the spacecraft mass due to the fuel consumption and (ii) and assuming that the thrust is finite, that is, the trajectory includes powered subarcs flown with max thrust and coasting subarc flown with zero thrust. Then, employing the found analytical solution, we study the rendezvous problem under the assumption that the initial separation coordinates and initial separation velocities are free except for the requirement that the initial chaser-to-target distance is given. The main contribution of Part B is the development of analytical solutions for the powered subarcs, an important extension of the analytical solutions already available for the coasting subarcs. One consequence is that the entire optimal trajectory can be described analytically. Another consequence is that the optimal control problems degenerate into mathematical programming problems. A further consequence is that, vis-a-vis the optimal control formulation, the mathematical programming formulation reduces the CPU time by a factor of order 1000. Key words. Space trajectories, rendezvous, optimization, guidance, optimal control, calculus of variations, Mayer problems, Bolza problems, transformation techniques, multiple-subarc sequential gradient-restoration algorithm.

Simultaneous microemulsion liquid chromatographic analysis of fat-soluble vitamins in pharmaceutical formulations: optimization using genetic algorithm.

PubMed

Momenbeik, Fariborz; Roosta, Mostafa; Nikoukar, Ali Akbar

2010-06-11

An environmentally benign and simple method has been proposed for separation and determination of fat-soluble vitamins using isocratic microemulsion liquid chromatography. Optimization of parameters affecting the separation selectivity and efficiency including surfactant concentration, percent of cosurfactant (1-butanol), and percent of organic oily solvent (diethyl ether), temperature and pH were performed simultaneously using genetic algorithm method. A new software package, MLR-GA, was developed for this purpose. The results indicated that 73.6mM sodium dodecyl sulfate, 13.64% (v/v) 1-butanol, 0.48% (v/v) diethyl ether, column temperature of 32.5 degrees C and 0.02M phosphate buffer of pH 6.99 are the best conditions for separation of fat-soluble vitamins. At the optimized conditions, the calibration plots for the vitamins were obtained and detection limits (1.06-3.69microgmL(-1)), accuracy (recoveries>94.3), precision (RSD<3.96) and linearity (0.01-10mgmL(-1)) were estimated. Finally, the amount of vitamins in multivitamin syrup and a sample of fish oil capsule were determined. The results showed a good agreement with those reported by manufactures. Copyright 2010 Elsevier B.V. All rights reserved.

Response surface methodology for the determination of the design space of enantiomeric separations on cinchona-based zwitterionic chiral stationary phases by high performance liquid chromatography.

PubMed

Hanafi, Rasha Sayed; Lämmerhofer, Michael

2018-01-26

Quality-by-Design approach for enantioselective HPLC method development surpasses Quality-by-Testing in offering the optimal separation conditions with the least number of experiments and in its ability to describe the method's Design Space visually which helps to determine enantiorecognition to a significant extent. Although some schemes exist for enantiomeric separations on Cinchona-based zwitterionic stationary phases, the exact design space and the weights by which each of the chromatographic parameters influences the separation have not yet been statistically studied. In the current work, a screening design followed by a Response Surface Methodology optimization design were adopted for enantioseparation optimization of 3 model drugs namely the acidic Fmoc leucine, the amphoteric tryptophan and the basic salbutamol. The screening design proved that the acid/base additives are of utmost importance for the 3 chiral drugs, and that among 3 different pairs of acids and bases, acetic acid and diethylamine is the couple able to provide acceptable resolution at variable conditions. Visualization of the response surface of the retention factor, separation factor and resolution helped describe accurately the magnitude by which each chromatographic factor (% MeOH, concentration and ratio of acid base modifiers) affects the separation while interacting with other parameters. The global optima compromising highest enantioresolution with the least run time for the 3 chiral model drugs varied extremely, where it was best to set low % methanol with equal ratio of acid-base modifiers for the acidic drug, very high % methanol and 10-fold higher concentration of the acid for the amphoteric drug while 20 folds of the base modifier with moderate %methanol were needed for the basic drug. Considering the selected drugs as models for many series of structurally related compounds, the design space defined and the optimum conditions computed are the key for method development on cinchona-based chiral stationary phases. Copyright © 2017 Elsevier B.V. All rights reserved.

Optimal Control Modification Adaptive Law for Time-Scale Separated Systems

NASA Technical Reports Server (NTRS)

Nguyen, Nhan T.

2010-01-01

Recently a new optimal control modification has been introduced that can achieve robust adaptation with a large adaptive gain without incurring high-frequency oscillations as with the standard model-reference adaptive control. This modification is based on an optimal control formulation to minimize the L2 norm of the tracking error. The optimal control modification adaptive law results in a stable adaptation in the presence of a large adaptive gain. This study examines the optimal control modification adaptive law in the context of a system with a time scale separation resulting from a fast plant with a slow actuator. A singular perturbation analysis is performed to derive a modification to the adaptive law by transforming the original system into a reduced-order system in slow time. A model matching conditions in the transformed time coordinate results in an increase in the actuator command that effectively compensate for the slow actuator dynamics. Simulations demonstrate effectiveness of the method.

Optimal Control Modification for Time-Scale Separated Systems

NASA Technical Reports Server (NTRS)

Nguyen, Nhan T.

2012-01-01

Recently a new optimal control modification has been introduced that can achieve robust adaptation with a large adaptive gain without incurring high-frequency oscillations as with the standard model-reference adaptive control. This modification is based on an optimal control formulation to minimize the L2 norm of the tracking error. The optimal control modification adaptive law results in a stable adaptation in the presence of a large adaptive gain. This study examines the optimal control modification adaptive law in the context of a system with a time scale separation resulting from a fast plant with a slow actuator. A singular perturbation analysis is performed to derive a modification to the adaptive law by transforming the original system into a reduced-order system in slow time. A model matching conditions in the transformed time coordinate results in an increase in the actuator command that effectively compensate for the slow actuator dynamics. Simulations demonstrate effectiveness of the method.

Separation of three phenolic high-molecular-weight compounds from the crude extract of Terminalia Chebula Retz. by ultrasound-assisted extraction and high-speed counter-current chromatography.

PubMed

Zou, Deng-lang; Chen, Tao; Li, Hong-mei; Chen, Chen; Zhao, Jing-yang; Li, Yu-lin

2016-04-01

This study presents an efficient strategy for separation of three phenolic compounds with high molecular weight from the crude extract of Terminalia chebula Retz. by ultrasound-assisted extraction and high-speed counter-current chromatography. The ultrasound-assisted extraction conditions were optimized by response surface methodology and the results showed the target compounds could be well enriched under the optimized extraction conditions. Then the crude extract was directly separated by high-speed counter-current chromatography without any pretreatment using n-hexane/ethyl acetate/methanol/water (1:7:0.5:3, v/v/v/v) as the solvent system. In 180 min, 13 mg of A, 18 mg of B, and 9 mg of C were obtained from 200 mg of crude sample. Their structures were identified as Chebulagic acid (A, 954 Da), Chebulinic acid (B, 956 Da), and Ellagic acid (C) by (1) H NMR spectroscopy. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simplex optimization of headspace factors for headspace gas chromatography determination of residual solvents in pharmaceutical products.

PubMed

Grodowska, Katarzyna; Parczewski, Andrzej

2013-01-01

The purpose of the present work was to find optimum conditions of headspace gas chromatography (HS-GC) determination of residual solvents which usually appear in pharmaceutical products. Two groups of solvents were taken into account in the present examination. Group I consisted of isopropanol, n-propanol, isobutanol, n-butanol and 1,4-dioxane and group II included cyclohexane, n-hexane and n-heptane. The members of the groups were selected in previous investigations in which experimental design and chemometric methods were applied. Four factors were taken into consideration in optimization which describe HS conditions: sample volume, equilibration time, equilibrium temperature and NaCl concentration in a sample. The relative GC peak area served as an optimization criterion which was considered separately for each analyte. Sequential variable size simplex optimization strategy was used and the progress of optimization was traced and visualized in various ways simultaneously. The optimum HS conditions appeared different for the groups of solvents tested, which proves that influence of experimental conditions (factors) depends on analyte properties. The optimization resulted in significant signal increase (from seven to fifteen times).

Capillary electrophoresis for aluminum ion speciation: Optimized separation conditions for complex polycation mixtures.

PubMed

Ouadah, Nesrine; Moire, Claudine; Brothier, Fabien; Kuntz, Jean-François; Deschaume, Olivier; Bartic, Carmen; Cottet, Hervé

2018-06-01

Aluminum chlorohydrates (ACH) are used in numerous applications and commercial products on a global scale including water treatment, catalysis or antiperspirants. They are complex mixtures of water soluble aluminum polycations of different degrees of polymerization, that are difficult to separate and quantify due to their susceptibility to depolymerize in solution when placed out of equilibrium, which is inherent to any separation process. We recently achieved the first capillary electrophoresis separation and characterization of ACH oligomers using 4-morpholineethanesulfonic acid (MES) as background electrolyte counter-ion. MES stabilizes the separated ACH oligomers during the electrophoretic process leading to highly repeatable and fast separations. In this work, the separation of ACH oligomers was further studied and perfected by varying the ionic strength, MES concentration and pH of the background electrolyte. Complex electrophoretic behavior is reported for the separation of Al 13 , Al 30 and Na + ions according to these experimental parameters. The transformation of the electropherograms in effective mobility scale and the use of the slope-plot approach are used to better understand the observed changes in selectivity/resolution. Optimal conditions (700 mM MES at 25 mM ionic strength containing 0.1 mM didodecyldimethylammonium bromide for dynamic capillary coating, pH 4.8) obtained for the separation of ACH oligomers are used for the baseline separation of samples difficult to analyze with other methods, including different molecular, aggregated and colloidal forms of aluminum from the Al 13 , Al 30 and Na + mixture, validating the rationale of the approach. Copyright © 2018. Published by Elsevier B.V.

Influence of particle size and shell thickness of core-shell packing materials on optimum experimental conditions in preparative chromatography.

PubMed

Horváth, Krisztián; Felinger, Attila

2015-08-14

The applicability of core-shell phases in preparative separations was studied by a modeling approach. The preparative separations were optimized for two compounds having bi-Langmuir isotherms. The differential mass balance equation of chromatography was solved by the Rouchon algorithm. The results show that as the size of the core increases, larger particles can be used in separations, resulting in higher applicable flow rates, shorter cycle times. Due to the decreasing volume of porous layer, the loadability of the column dropped significantly. As a result, the productivity and economy of the separation decreases. It is shown that if it is possible to optimize the size of stationary phase particles for the given separation task, the use of core-shell phases are not beneficial. The use of core-shell phases proved to be advantageous when the goal is to build preparative column for general purposes (e.g. for purification of different products) in small scale separations. Copyright © 2015 Elsevier B.V. All rights reserved.

Optimal Control of Airfoil Flow Separation using Fluidic Excitation

NASA Astrophysics Data System (ADS)

Shahrabi, Arireza F.

This thesis deals with the control of flow separation around a symmetric airfoils with the aid of multiple synthetic jet actuators (SJAs). CFD simulation methods have been implemented to uncover the flow separation regimes and associated properties such as frequencies and momentum ratio. In the first part of the study, the SJA was studied thoroughly. Large Eddy Simulations (LES) were performed for one individual cavity; the time history of SJA of the outlet velocity profile and the net momentum imparted to the flow were analyzed. The studied SJA is asymmetrical and operates with the aid of a piezoelectric (PZT) ceramic circular plate actuator. A three-dimensional mesh for the computational domain of the SJA and the surrounding volume was developed and was used to evaluate the details of the airflow conditions inside the SJA as well as at the outlet. The vibration of the PZT ceramic actuator was used as a boundary condition in the computational model to drive the SJA. Particular attention was given to developing a predictive model of the SJA outlet velocity. Results showed that the SJA velocity output is correlated to the PZT ceramic plate vibration, especially for the first frequency mode. SJAs are a particular class of zero net mass flux (ZNMF) fluidic devices with net imparted momentum to the flow. The net momentum imparted to the flow in the separated region is such that positive enhancement during AFC operations is achieved. Flows around the NACA 0015 airfoil were simulated for a range of operating conditions. Attention was given to the active open and closed loop control solutions for an airfoil with SJA at different angles of attack and flap angles. A large number of simulations using RANS & LES models were performed to study the effects of the momentum ratio (Cμ) in the range of 0 to 11% and of the non-dimensional frequency, F+, in the range of 0 to 2 for the control of flow separation at a practical angle of attack and flap angle. The optimum value of Cμ as well as F+ were evaluated and discussed. The computational model predictions showed good agreement with the experimental data. It was observed that different angles of attack and flap angles have different requirements for the minimum value of the momentum coefficient, Cμ, in order for the SJA to be effective for control of separation. It was also found that the variation of F + noticeably affects the lift and drag forces acting on the airfoil. The optimum values of parameters during open loop control simulations have been applied in order to introduce the optimal open loop control outcome. An innovative approach has been implemented to formulate optimal frequencies and momentum ratios of vortex shedding which depends on angle of attack and static pressure of the separation zone in the upper chord. Optimal open loop results have been compared with the optimal closed loop results. Cumulative case studies in the matter of angle of attacks, flap angles, Re, Cμ and F+ provide a convincing collection of evidence to the following conclusion. An improvement of a direct closed loop control was demonstrated, and an analytical formula describing the properties of a separated flow and vortex shedding was proposed. Best AFC solutions are offered by providing optimal frequencies and momentum ratios at a variety of flow conditions.

The roles of xylan and lignin in oxalic acid pretreated corncob during separate enzymatic hydrolysis and ethanol fermentation

Treesearch

Jae-Won Lee; Rita C.L.B. Rodrigues; Hyun Joo Kim; In-Gyu Choi; Thomas W. Jeffries

2010-01-01

High yields of hemicellulosic and cellulosic sugars are critical in obtaining economical conversion of agricultural residues to ethanol. To optimize pretreatment conditions, we evaluated oxalic acid loading rates, treatment temperatures and times in a 23 full factorial design. Response-surface analysis revealed an optimal oxalic acid pretreatment...

Pilot trial on separation conditions for diaper recycling.

PubMed

Kim, Kyung-Shin; Cho, Hee-Sun

2017-09-01

By utilizing laboratory-scale tests, the optimal separation conditions for diaper recycling were identified, and then, these conditions were validated by a pilot trial. In this research, we determined the mass balances derived during various processing steps and identified the most feasible procedures to use for separating each material in the output flow. The results showed that drum screening was not able to remove all the fiber and super absorbent particles (SAP) in the plastic-rich fraction and that cellulose enzyme treatment can be a good solution. To achieve better separation of fibers and SAP, slot screening followed by a cleaner is a potential option. A feasible diaper recycling process was recommended based on these results. This process involves screening and enzymatic treatment for the plastic fraction, and screening, cleaning, and thickening for the fiber fraction. Treatment procedures were also proposed for the SAP fraction and rejected materials. Copyright © 2017. Published by Elsevier Ltd.

Combined use of l-alanine tert butyl ester lactate and trimethyl-β-cyclodextrin for the enantiomeric separations of 2-arylpropionic acids nonsteroidal anti-inflammatory drugs.

PubMed

Mavroudi, Maria C; Kapnissi-Christodoulou, Constantina P

2015-10-01

In this study, a new CE method, employing a binary system of trimethyl-β-CD (TM-β-CD) and a chiral amino acid ester-based ionic liquid (AAIL), was developed for the chiral separation of seven 2-arylpropionic acid nonsteroidal anti-inflammatory drugs (NSAIDs). In particular, the enantioseparation of ibuprofen, ketoprofen, carprofen, indoprofen, flurbiprofen, naproxen, and fenoprofen was improved significantly by supporting the BGE with the chiral AAIL l-alanine tert butyl ester lactate (l-AlaC4 Lac). Parameters, such as concentrations of TM-β-CD and l-AlaC4 Lac, and buffer pH, were systematically examined in order to optimize the chiral separation of each NSAID. It was observed that the addition of the AAIL into the BGE improved both resolution and efficiency significantly. After optimization of separation conditions, baseline separation (Rs >1.5) of five of the analytes was achieved in less than 11 min, while the resolution of ibuprofen and flurbiprofen was approximately 1.2. The optimized enantioseparation conditions for all analytes involve a BGE of 5 mM sodium acetate/acetic acid (pH 5.0), an applied voltage of 30 kV, and a temperature of 20°C. In addition, the results obtained by computing the %-RSD values of the EOF and the two enantiomer peaks, demonstrated excellent run-to-run, batch-to-batch, and day-to-day reproducibilities. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Speciation of inorganic tellurium from seawater by ICP-MS following magnetic SPE separation and preconcentration.

PubMed

Huang, Chaozhang; Hu, Bin

2008-03-01

A new method was developed for the speciation of inorganic tellurium species in seawater by inductively coupled plasma-MS (ICP-MS) following selective magnetic SPE (MSPE) separation. Within the pH range of 2-9, tellurite (Te(IV)) could be quantitatively adsorbed on gamma-mercaptopropyltrimethoxysilane (gamma-MPTMS) modified silica-coated magnetic nanoparticles (MNPs), while the tellurate (Te(VI)) was not retained and remained in solution. Without filtration or centrifugation, these tellurite-loaded MNPs could be separated easily from the aqueous solution by simply applying external magnetic field. The Te(IV) adsorbed on the MNPs could be recovered quantitatively using a solution containing 2 mol/L HCl and 0.03 mol/L K2Cr2O7. Te(VI) was reduced to Te(IV) by L-cysteine prior to the determination of total tellurium, and its assay was based on subtracting Te(IV) from total tellurium. The parameters affecting the separation were investigated systematically and the optimal separation conditions were established. Under the optimal conditions, the LOD obtained for Te(IV) was 0.079 ng/L, while the precision was 7.0% (C = 10 ng/L, n = 7). The proposed method was successfully applied to the speciation of inorganic tellurium in seawater.

Synthetic Vortex Generator Jets Used to Control Separation on Low-Pressure Turbine Airfoils

NASA Technical Reports Server (NTRS)

Ashpis, David E.; Volino, Ralph J.

2005-01-01

Low-pressure turbine (LPT) airfoils are subject to increasingly stronger pressure gradients as designers impose higher loading in an effort to improve efficiency and lower cost by reducing the number of airfoils in an engine. When the adverse pressure gradient on the suction side of these airfoils becomes strong enough, the boundary layer will separate. Separation bubbles, particularly those that fail to reattach, can result in a significant loss of lift and a subsequent degradation of engine efficiency. The problem is particularly relevant in aircraft engines. Airfoils optimized to produce maximum power under takeoff conditions may still experience boundary layer separation at cruise conditions because of the thinner air and lower Reynolds numbers at altitude. Component efficiency can drop significantly between takeoff and cruise conditions. The decrease is about 2 percent in large commercial transport engines, and it could be as large as 7 percent in smaller engines operating at higher altitudes. Therefore, it is very beneficial to eliminate, or at least reduce, the separation bubble.

Separation and purification of both tea seed polysaccharide and saponin from camellia cake extract using macroporous resin.

PubMed

Yang, Pengjie; Zhou, Mingda; Zhou, Chengyun; Wang, Qian; Zhang, Fangfang; Chen, Jian

2015-02-01

A novel method to separate and purify tea seed polysaccharide and tea seed saponin from camellia cake extract by macroporous resin was developed. Among four kinds of resins (AB-8, NKA-9, XDA-6, and D4020) tested, AB-8 macroporous resin possessed optimal separating capacity for the two substances and thus was selected for the separation, in which deionized water was used to elute tea seed polysaccharide, 0.25% NaOH solution to remove the undesired pigments, and 90% ethanol to elute tea seed saponin. Further dynamic adsorption/desorption experiments on AB-8 resin-based column chromatography were conducted to obtain the optimal parameters. Under optimal dynamic adsorption and desorption conditions, 18.7 and 11.8% yield of tea seed polysaccharide and tea seed saponin were obtained with purities of 89.2 and 96.0%, respectively. The developed method provides a potential approach for the large-scale production of tea seed polysaccharide and tea seed saponin from camellia cake. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimizing the separation performance of a gas centrifuge

NASA Astrophysics Data System (ADS)

Wood, H. G.

1997-11-01

Gas centrifuges were originally developed for the enrichment of U^235 from naturally occurring uranium for the purpose of providing fuel for nuclear power reactors and material for nuclear weapons. This required the separation of a binary mixture composed of U^235 and U^238. Since the end of the cold war, a surplus of enriched uranium exists on the world market, but many centrifuge plants exist in numerous countries. These circumstances together with the growing demand for stable isotopes for chemical and physical research and in medical science has led to the exploration of alternate applications of gas centrifuge technology. In order to acieve these multi-component separations, existing centrifuges must be modified or new centrifuges must be designed. In either case, it is important to have models of the internal flow fields to predict the separation performance and algorithms to seek the optimal operating conditions of the centrifuges. Here, we use the Onsager pancake model of the internal flow field, and we present an optimization strategy which exploits a similarity parameter in the pancake model. Numerical examples will be presented.

Quantitative structure-retention relationships applied to development of liquid chromatography gradient-elution method for the separation of sartans.

PubMed

Golubović, Jelena; Protić, Ana; Otašević, Biljana; Zečević, Mira

2016-04-01

QSRR are mathematically derived relationships between the chromatographic parameters determined for a representative series of analytes in given separation systems and the molecular descriptors accounting for the structural differences among the investigated analytes. Artificial neural network is a technique of data analysis, which sets out to emulate the human brain's way of working. The aim of the present work was to optimize separation of six angiotensin receptor antagonists, so-called sartans: losartan, valsartan, irbesartan, telmisartan, candesartan cilexetil and eprosartan in a gradient-elution HPLC method. For this purpose, ANN as a mathematical tool was used for establishing a QSRR model based on molecular descriptors of sartans and varied instrumental conditions. The optimized model can be further used for prediction of an external congener of sartans and analysis of the influence of the analyte structure, represented through molecular descriptors, on retention behaviour. Molecular descriptors included in modelling were electrostatic, geometrical and quantum-chemical descriptors: connolly solvent excluded volume non-1,4 van der Waals energy, octanol/water distribution coefficient, polarizability, number of proton-donor sites and number of proton-acceptor sites. Varied instrumental conditions were gradient time, buffer pH and buffer molarity. High prediction ability of the optimized network enabled complete separation of the analytes within the run time of 15.5 min under following conditions: gradient time of 12.5 min, buffer pH of 3.95 and buffer molarity of 25 mM. Applied methodology showed the potential to predict retention behaviour of an external analyte with the properties within the training space. Connolly solvent excluded volume, polarizability and number of proton-acceptor sites appeared to be most influential paramateres on retention behaviour of the sartans. Copyright © 2015 Elsevier B.V. All rights reserved.

Hybrid-drive implosion system for ICF targets

DOEpatents

Mark, James W.

1988-08-02

Hybrid-drive implosion systems (20,40) for ICF targets (10,22,42) are described which permit a significant increase in target gain at fixed total driver energy. The ICF target is compressed in two phases, an initial compression phase and a final peak power phase, with each phase driven by a separate, optimized driver. The targets comprise a hollow spherical ablator (12) surroundingly disposed around fusion fuel (14). The ablator is first compressed to higher density by a laser system (24), or by an ion beam system (44), that in each case is optimized for this initial phase of compression of the target. Then, following compression of the ablator, energy is directly delivered into the compressed ablator by an ion beam driver system (30,48) that is optimized for this second phase of operation of the target. The fusion fuel (14) is driven, at high gain, to conditions wherein fusion reactions occur. This phase separation allows hydrodynamic efficiency and energy deposition uniformity to be individually optimized, thereby securing significant advantages in energy gain. In additional embodiments, the same or separate drivers supply energy for ICF target implosion.

Hybrid-drive implosion system for ICF targets

DOEpatents

Mark, James W.

1988-01-01

Hybrid-drive implosion systems (20,40) for ICF targets (10,22,42) are described which permit a significant increase in target gain at fixed total driver energy. The ICF target is compressed in two phases, an initial compression phase and a final peak power phase, with each phase driven by a separate, optimized driver. The targets comprise a hollow spherical ablator (12) surroundingly disposed around fusion fuel (14). The ablator is first compressed to higher density by a laser system (24), or by an ion beam system (44), that in each case is optimized for this initial phase of compression of the target. Then, following compression of the ablator, energy is directly delivered into the compressed ablator by an ion beam driver system (30,48) that is optimized for this second phase of operation of the target. The fusion fuel (14) is driven, at high gain, to conditions wherein fusion reactions occur. This phase separation allows hydrodynamic efficiency and energy deposition uniformity to be individually optimized, thereby securing significant advantages in energy gain. In additional embodiments, the same or separate drivers supply energy for ICF target implosion.

Hybrid-drive implosion system for ICF targets

DOEpatents

Mark, J.W.K.

1987-10-14

Hybrid-drive implosion systems for ICF targets are described which permit a significant increase in target gain at fixed total driver energy. The ICF target is compressed in two phases, an initial compression phase and a final peak power phase, with each phase driven by a separate, optimized driver. The targets comprise a hollow spherical ablator surroundingly disposed around fusion fuel. The ablator is first compressed to higher density by a laser system, or by an ion beam system, that in each case is optimized for this initial phase of compression of the target. Then, following compression of the ablator, energy is directly delivered into the compressed ablator by an ion beam driver system that is optimized for this second phase of operation of the target. The fusion fuel is driven, at high gain, to conditions wherein fusion reactions occur. This phase separation allows hydrodynamic efficiency and energy deposition uniformity to be individually optimized, thereby securing significant advantages in energy gain. In additional embodiments, the same or separate drivers supply energy for ICF target implosion. 3 figs.

Optimization of elution salt concentration in stepwise elution of protein chromatography using linear gradient elution data. Reducing residual protein A by cation-exchange chromatography in monoclonal antibody purification.

PubMed

Ishihara, Takashi; Kadoya, Toshihiko; Endo, Naomi; Yamamoto, Shuichi

2006-05-05

Our simple method for optimization of the elution salt concentration in stepwise elution was applied to the actual protein separation system, which involves several difficulties such as detection of the target. As a model separation system, reducing residual protein A by cation-exchange chromatography in human monoclonal antibody (hMab) purification was chosen. We carried out linear gradient elution experiments and obtained the data for the peak salt concentration of hMab and residual protein A, respectively. An enzyme-linked immunosorbent assay was applied to the measurement of the residual protein A. From these data, we calculated the distribution coefficient of the hMab and the residual protein A as a function of salt concentration. The optimal salt concentration of stepwise elution to reduce the residual protein A from the hMab was determined based on the relationship between the distribution coefficient and the salt concentration. Using the optimized condition, we successfully performed the separation, resulting in high recovery of hMab and the elimination of residual protein A.

Numerical Investigations of an Optimized Airfoil with a Rotary Cylinder

NASA Astrophysics Data System (ADS)

Gada, Komal; Rahai, Hamid

2015-11-01

Numerical Investigations of an optimized thin airfoil with a rotary cylinder as a control device for reducing separation and improving lift to drag ratio have been performed. Our previous investigations have used geometrical optimization for development of an optimized airfoil with increased torque for applications in a vertical axis wind turbine. The improved performance was due to contributions of lift to torque at low angles of attack. The current investigations have been focused on using the optimized airfoil for micro-uav applications with an active flow control device, a rotary cylinder, to further control flow separation, especially during wind gust conditions. The airfoil has a chord length of 19.66 cm and a width of 25 cm with 0.254 cm thickness. Previous investigations have shown flow separation at approximately 85% chord length at moderate angles of attack. Thus the rotary cylinder with a 0.254 cm diameter was placed slightly downstream of the location of flow separation. The free stream mean velocity was 10 m/sec. and investigations have been performed at different cylinder's rotations with corresponding tangential velocities higher than, equal to and less than the free stream velocity. Results have shown more than 10% improvement in lift to drag ratio when the tangential velocity is near the free stream mean velocity. Graduate Assistant, Center for Energy and Environmental Research and Services (CEERS), College of Engineering, California State University, Long Beach.

Einstein-Podolsky-Rosen-like separability indicators for two-mode Gaussian states

NASA Astrophysics Data System (ADS)

Marian, Paulina; Marian, Tudor A.

2018-02-01

We investigate the separability of the two-mode Gaussian states (TMGSs) by using the variances of a pair of Einstein-Podolsky-Rosen (EPR)-like observables. Our starting point is inspired by the general necessary condition of separability introduced by Duan et al (2000 Phys. Rev. Lett. 84 2722). We evaluate the minima of the normalized forms of both the product and sum of such variances, as well as that of a regularized sum. Making use of Simon’s separability criterion, which is based on the condition of positivity of the partial transpose (PPT) of the density matrix (Simon 2000 Phys. Rev. Lett. 84 2726), we prove that these minima are separability indicators in their own right. They appear to quantify the greatest amount of EPR-like correlations that can be created in a TMGS by means of local operations. Furthermore, we reconsider the EPR-like approach to the separability of TMGSs which was developed by Duan et al with no reference to the PPT condition. By optimizing the regularized form of their EPR-like uncertainty sum, we derive a separability indicator for any TMGS. We prove that the corresponding EPR-like condition of separability is manifestly equivalent to Simon’s PPT one. The consistency of these two distinct approaches (EPR-like and PPT) affords a better understanding of the examined separability problem, whose explicit solution found long ago by Simon covers all situations of interest.

Integration of phase separation with ultrasound-assisted salt-induced liquid-liquid microextraction for analyzing the fluoroquinones in human body fluids by liquid chromatography.

PubMed

Wang, Huili; Gao, Ming; Wang, Mei; Zhang, Rongbo; Wang, Wenwei; Dahlgren, Randy A; Wang, Xuedong

2015-03-15

Herein, we developed a novel integrated device to perform phase separation based on ultrasound-assisted salt-induced liquid-liquid microextraction for determination of five fluoroquinones (FQs) in human body fluids. The integrated device consisted of three simple HDPE components used to separate the extraction solvent from the aqueous phase prior to retrieving the extractant. A series of extraction parameters were optimized using the response surface method based on central composite design. Optimal conditions consisted of 945μL acetone extraction solvent, pH 2.1, 4.1min stir time, 5.9g Na2SO4, and 4.0min centrifugation. Under optimized conditions, the limits of detection (at S/N=3) were 0.12-0.66μgL(-1), the linear range was 0.5-500μgL(-1) and recoveries were 92.6-110.9% for the five FQs extracted from plasma and urine. The proposed method has several advantages, such as easy construction from inexpensive materials, high extraction efficiency, short extraction time, and compatibility with HPLC analysis. Thus, this method shows excellent prospects for sample pretreatment and analysis of FQs in human body fluids. Copyright © 2015 Elsevier B.V. All rights reserved.

Optimization of yield in magnetic cell separations using nickel nanowires of different lengths.

PubMed

Hultgren, Anne; Tanase, Monica; Felton, Edward J; Bhadriraju, Kiran; Salem, Aliasger K; Chen, Christopher S; Reich, Daniel H

2005-01-01

Ferromagnetic nanowires are shown to perform both high yield and high purity single-step cell separations on cultures of NIH-3T3 mouse fibroblast cells. The nanowires are made by electrochemical deposition in nanoporous templates, permitting detailed control of their chemical and physical properties. When added to fibroblast cell cultures, the nanowires are internalized by the cells via the integrin-mediated adhesion pathway. The effectiveness of magnetic cell separations using Ni nanowires 350 nm in diameter and 5-35 micrometers long in field gradients of 40 T/m was compared to commercially available superparamagnetic beads. The percent yield of the separated populations is found to be optimized when the length of the nanowire is matched to the diameter of the cells in the culture. Magnetic cell separations performed under these conditions achieve 80% purity and 85% yield, a 4-fold increase over the beads. This effect is shown to be robust when the diameter of the cell is changed within the same cell line using mitomycin-C.

New on-line separation workflow of microbial metabolites via hyphenation of analytical and preparative comprehensive two-dimensional liquid chromatography.

PubMed

Yan, Xia; Wang, Li-Juan; Wu, Zhen; Wu, Yun-Long; Liu, Xiu-Xiu; Chang, Fang-Rong; Fang, Mei-Juan; Qiu, Ying-Kun

2016-10-15

Microbial metabolites represent an important source of bioactive natural products, but always exhibit diverse of chemical structures or complicated chemical composition with low active ingredients content. Traditional separation methods rely mainly on off-line combination of open-column chromatography and preparative high performance liquid chromatography (HPLC). However, the multi-step and prolonged separation procedure might lead to exposure to oxygen and structural transformation of metabolites. In the present work, a new two-dimensional separation workflow for fast isolation and analysis of microbial metabolites from Chaetomium globosum SNSHI-5, a cytotoxic fungus derived from extreme environment. The advantage of this analytical comprehensive two-dimensional liquid chromatography (2D-LC) lies on its ability to analyze the composition of the metabolites, and to optimize the separation conditions for the preparative 2D-LC. Furthermore, gram scale preparative 2D-LC separation of the crude fungus extract could be performed on a medium-pressure liquid chromatograph×preparative high-performance liquid chromatography system, under the optimized condition. Interestingly, 12 cytochalasan derivatives, including two new compounds named cytoglobosin Ab (3) and isochaetoglobosin Db (8), were successfully obtained with high purity in a short period of time. The structures of the isolated metabolites were comprehensively characterized by HR ESI-MS and NMR. To be highlighted, this is the first report on the combination of analytical and preparative 2D-LC for the separation of microbial metabolites. The new workflow exhibited apparent advantages in separation efficiency and sample treatment capacity compared with conventional methods. Copyright © 2016 Elsevier B.V. All rights reserved.

Optimization of startup and shutdown operation of simulated moving bed chromatographic processes.

PubMed

Li, Suzhou; Kawajiri, Yoshiaki; Raisch, Jörg; Seidel-Morgenstern, Andreas

2011-06-24

This paper presents new multistage optimal startup and shutdown strategies for simulated moving bed (SMB) chromatographic processes. The proposed concept allows to adjust transient operating conditions stage-wise, and provides capability to improve transient performance and to fulfill product quality specifications simultaneously. A specially tailored decomposition algorithm is developed to ensure computational tractability of the resulting dynamic optimization problems. By examining the transient operation of a literature separation example characterized by nonlinear competitive isotherm, the feasibility of the solution approach is demonstrated, and the performance of the conventional and multistage optimal transient regimes is evaluated systematically. The quantitative results clearly show that the optimal operating policies not only allow to significantly reduce both duration of the transient phase and desorbent consumption, but also enable on-spec production even during startup and shutdown periods. With the aid of the developed transient procedures, short-term separation campaigns with small batch sizes can be performed more flexibly and efficiently by SMB chromatography. Copyright © 2011 Elsevier B.V. All rights reserved.

[Preparation and performance characterization of gold nanoparticles modified chiral capillary electrochromatography stationary phase].

PubMed

Xiong, Lele; Li, Ruijun; Ji, Yibing

2017-07-08

Gold nanoparticles (GNPs, 15 nm) were prepared and introduced to amino groups derived silica monolithic column. Bovine serum albumin (BSA) was immobilized via covalent modification method onto the carboxylic functionalized GNPs to afford chiral stationary phase (CSP) for enantioseparation. GNPs were well dispersed and successfully incorporated onto the columns with the contents as high as 17.18% by characterization method such as transmission electron microscopy (TEM), ultraviolet (UV)-visible absorption spectra and scanning electron microscopy (SEM). The preparation conditions of the BSA modified CSP were optimized and 10% (v/v) 3-aminopropyltriethoxysilane (APTES) and 15 g/L BSA were selected as appropriate reaction conditions. The enantioseparation performance of the BSA modified CSP has been investigated by capillary electrochromatography (CEC). Enantiomers of tryptophan, ephedrine and atenolol were resolved, and the baseline separation of tryptophan was achieved. Meanwhile, the influences of pH value, buffer concentrations and applied voltages used on the chiral separation were studied, and the optimal separation conditions were 10 mmol/L phosphate buffer at pH 7.4 and 15 kV applied voltages. In comparison with the BSA modified CSP prepared by physical adsorption, the CSP prepared by covalent modification method had better separation results, and the analytes could be separated directly without pre-column derivatization. In addition, the prepared BSA modified CSP exhibited good run to run repeatability with relative standard deviations (RSDs) of the migration times and selectivity factors not more than 2.3% and 0.96%, respectively. This work offers a good thinking for modification with other proteins or other types of chiral selectors.

Simultaneous separation/enrichment and detection of trace ciprofloxacin and lomefloxacin in food samples using thermosensitive smart polymers aqueous two-phase flotation system combined with HPLC.

PubMed

Lu, Yang; Chen, Bo; Yu, Miao; Han, Juan; Wang, Yun; Tan, Zhenjiang; Yan, Yongsheng

2016-11-01

Smart polymer aqueous two phase flotation system (SPATPF) is a new separation and enrichment technology that integrated the advantages of the three technologies, i.e., aqueous two phase system, smart polymer and flotation sublation. Ethylene oxide and propylene oxide copolymer (EOPO)-(NH4)2SO4 SPATPF is a pretreatment technique, and it is coupled with high-performance liquid chromatography to analyze the trace ciprofloxacin and lomefloxacin in real food samples. The optimized conditions of experiment were determined in the multi-factor experiment by using response surface methodology. The flotation efficiency of lomefloxacin and ciprofloxacin was 94.50% and 98.23% under the optimized conditions. The recycling experimentsshowed that the smart polymer EOPO could use repeatedly, which will reduce the cost in the future application. Copyright © 2016 Elsevier Ltd. All rights reserved.

Rapid analysis of clenbuterol, salbutamol, procaterol, and fenoterol in pharmaceuticals and human urine by capillary electrophoresis.

PubMed

Sirichai, Somsak; Khanatharana, Proespichaya

2008-09-15

Capillary electrophoresis (CE) with UV detection for the simultaneous and short-time analysis of clenbuterol, salbutamol, procaterol, fenoterol is described and validated. Optimized conditions were found to be a 10 mmoll(-1) borate buffer (pH 10.0), an separation voltage of 19 kV, and a separation temperature of 32 degrees C. Detection was set at 205 nm. Under the optimized conditions, analyses of the four analytes in pharmaceutical and human urine samples were carried out in approximately 1 min. The interference of the sample matrix was not observed. The LOD (limits of detection) defined at S/N of 3:1 was found between 0.5 and 2.0 mgl(-1) for the analytes. The linearity of the detector response was within the range from 2.0 to 30 mgl(-1) with correlation coefficient >0.996.

Optimisation of resolution in micellar electrokinetic chromatography by multivariate evaluation of electrolytes.

PubMed

Mikaeli, S; Thorsén, G; Karlberg, B

2001-01-12

A novel approach to multivariate evaluation of separation electrolytes for micellar electrokinetic chromatography is presented. An initial screening of the experimental parameters is performed using a Plackett-Burman design. Significant parameters are further evaluated using full factorial designs. The total resolution of the separation is calculated and used as response. The proposed scheme has been applied to the optimisation of the separation of phenols and the chiral separation of (+)-1-(9-anthryl)-2-propyl chloroformate-derivatized amino acids. A total of eight experimental parameters were evaluated and optimal conditions found in less than 48 experiments.

Chiral ligand-exchange high-performance liquid chromatography with copper (II)-L-phenylalanine complexes for separation of 3,4-dimethoxy-α-methylphenylalanine racemes.

PubMed

Jia, Dong-Xu; Ai, Zheng-Gui; Xue, Ya-Ping; Zheng, Yu-Guo

2014-11-01

L-3, 4-dimethoxy-α-methylphenylalanine (L-DMMD) is an important intermediate for the synthesis of 3-hydroxy-α-methyl-L-tyrosine (L-methyldopa). This paper describes an efficient, accurate, and low-priced method of high-performance liquid chromatography (HPLC) using chiral mobile phase and conventional C18 column to separate L-DMMD from its enantiomers. The effects of ligands, copper salts, organic modifiers, pHs of mobile phase, and temperatures on the retention factors (k') and selectivity (α) were evaluated to achieve optimal separation performance. Then, thermal analysis of the optimal separation conditions was investigated as well. It was confirmed that the optimal mobile phase was composed of 20 % (v/v) methanol, 8 mM L-phenylalanine (L-Phe), and 4 mM cupric sulfate in water of pH 3.2, and the column temperature was set at 20 °C. Baseline separation of two enantiomers could be obtained through the conventional C18 column with a resolution (R) of 3.18 in less than 18 min. Thermodynamic data (∆∆H and ∆∆S) obtained by Van't Hoff plots revealed the chiral separation was an enthalpy-controlled process. To the best of our knowledge, this is the first report regarding the enantioseparation of DMMD by chiral ligand-exchange HPLC.

Optimizing and developing a continuous separation system for the wet process separation of aluminum and polyethylene in aseptic composite packaging waste.

PubMed

Yan, Dahai; Peng, Zheng; Liu, Yuqiang; Li, Li; Huang, Qifei; Xie, Minghui; Wang, Qi

2015-01-01

The consumption of milk in China is increasing as living standards rapidly improve, and huge amounts of aseptic composite milk packaging waste are being generated. Aseptic composite packaging is composed of paper, polyethylene, and aluminum. It is difficult to separate the polyethylene and aluminum, so most of the waste is currently sent to landfill or incinerated with other municipal solid waste, meaning that enormous amounts of resources are wasted. A wet process technique for separating the aluminum and polyethylene from the composite materials after the paper had been removed from the original packaging waste was studied. The separation efficiency achieved using different separation reagents was compared, different separation mechanisms were explored, and the impacts of a range of parameters, such as the reagent concentration, temperature, and liquid-solid ratio, on the separation time and aluminum loss ratio were studied. Methanoic acid was found to be the optimal separation reagent, and the suitable conditions were a reagent concentration of 2-4 mol/L, a temperature of 60-80°C, and a liquid-solid ratio of 30 L/kg. These conditions allowed aluminum and polyethylene to be separated in less than 30 min, with an aluminum loss ratio of less than 3%. A mass balance was produced for the aluminum-polyethylene separation system, and control technique was developed to keep the ion concentrations in the reaction system stable. This allowed a continuous industrial-scale process for separating aluminum and polyethylene to be developed, and a demonstration facility with a capacity of 50t/d was built. The demonstration facility gave polyethylene and aluminum recovery rates of more than 98% and more than 72%, respectively. Separating 1t of aluminum-polyethylene composite packaging material gave a profit of 1769 Yuan, meaning that an effective method for recycling aseptic composite packaging waste was achieved. Copyright © 2014 Elsevier Ltd. All rights reserved.

High Temperature Polybenzimidazole Hollow Fiber Membranes for Hydrogen Separation and Carbon Dioxide Capture from Synthesis Gas

DOE PAGES

Singh, Rajinder P.; Dahe, Ganpat J.; Dudeck, Kevin W.; ...

2014-12-31

Sustainable reliance on hydrocarbon feedstocks for energy generation requires CO₂ separation technology development for energy efficient carbon capture from industrial mixed gas streams. High temperature H₂ selective glassy polymer membranes are an attractive option for energy efficient H₂/CO₂ separations in advanced power production schemes with integrated carbon capture. They enable high overall process efficiencies by providing energy efficient CO₂ separations at process relevant operating conditions and correspondingly, minimized parasitic energy losses. Polybenzimidazole (PBI)-based materials have demonstrated commercially attractive H₂/CO₂ separation characteristics and exceptional tolerance to hydrocarbon fuel derived synthesis (syngas) gas operating conditions and chemical environments. To realize a commerciallymore » attractive carbon capture technology based on these PBI materials, development of high performance, robust PBI hollow fiber membranes (HFMs) is required. In this work, we discuss outcomes of our recent efforts to demonstrate and optimize the fabrication and performance of PBI HFMs for use in pre-combustion carbon capture schemes. These efforts have resulted in PBI HFMs with commercially attractive fabrication protocols, defect minimized structures, and commercially attractive permselectivity characteristics at IGCC syngas process relevant conditions. The H₂/CO₂ separation performance of these PBI HFMs presented in this document regarding realistic process conditions is greater than that of any other polymeric system reported to-date.« less

Electrochemical CO2 and O2 separation for crew and plant environments

NASA Technical Reports Server (NTRS)

Lee, M. G.; Grigger, David J.; Foerg, Sandra L.

1992-01-01

The study describes a closed ecosystem concept that includes electrochemical CO2 and O2 separators and a moisture condenser/separator for maintaining CO2, O2, and humidity levels in the crew and plant habitats at their respective optimal conditions. The key processes of this concept are aqueous electrolyte-based electrochemical CO2 and O2 separations. The principles and cell characteristics of these electrochemical gas separation processes are described. Also presented are descriptions of test hardware and the test results of the Electrochemical CO2 Separator (ECS) and the Electrochemical O2 Separator (EOS), and the combination of the ECS and the EOS. The test results proved that the ECS and EOS processes for the combined concept are viable.

Separation of no-carrier-added rhenium from bulk tantalum by the sodium malonate-PEG aqueous biphasic system.

PubMed

Dutta, Binita; Lahiri, Susanta; Tomar, B S

2014-02-01

The aqueous biphasic system (ABS) involving sodium malonate-polyethylene glycol (PEG) phases has been applied for the first time for separation of no-carrier-added (183)Re (T1/2=70 d) from α-particle irradiated bulk tantalum target. The various ABS conditions were applied for investigating the separation by varying pH, temperature, PEG-molecular weight, concentration of salt. The extraction pattern was hardly affected by change in pH and the molecular weight of PEG. One step separation of nca (183)Re from Ta was achieved at the optimal conditions of (i) 50% (w/w) PEG-4000-2 M sodium malonate, 40 °C and (ii) 50% (w/w) PEG-4000-3 M sodium malonate, room temperature (27 °C). © 2013 Published by Elsevier Ltd.

Nonaqueous capillary electrophoresis of dextromethorphan and its metabolites.

PubMed

Pelcová, Marta; Langmajerová, Monika; Cvingráfová, Eliška; Juřica, Jan; Glatz, Zdeněk

2014-10-01

This study deals with the nonaqueous capillary electrophoretic separation of dextromethorphan and its metabolites using a methanolic background electrolyte. The optimization of separation conditions was performed in terms of the resolution of dextromethorphan and dextrorphan and the effect of separation temperature, voltage, and the characteristics of the background electrolyte were studied. Complete separation of all analytes was achieved in 40 mM ammonium acetate dissolved in methanol. Hydrodynamic injection was performed at 3 kPa for 4 s. The separation voltage was 20 kV accompanied by a low electric current. The ultraviolet detection was performed at 214 nm, the temperature of the capillary was 25°C. These conditions enabled the separation of four analytes plus the internal standard within 9 min. Further, the developed method was validated in terms of linearity, sensitivity, and repeatability. Rat liver perfusate samples were subjected to the nonaqueous capillary electrophoretic method to illustrate its applicability. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Recovery of ferrous and nonferrous metal from ASR by physical separation

NASA Astrophysics Data System (ADS)

Kim, Min-gyu; Han, Oh-hyung; Park, Chul-hyun

2017-04-01

A recycle ratio of waste automobiles in Korea is low, compared to that of the advanced countries. Especially in its recycle, separation of automotive shredder residue (ASR), the residual fraction of approximate 25% obtained after dismantling and shredding from waste car, is needed. However ASR is cannot be effectively separated due to its heterogeneous materials and coated or laminated complexes and then is largely deposited in land-fill sites as waste. In this study ASR was separated by a series of physical processing operations such as comminution, air classification and magnetic separation and electrostatic separations. In particular it focuses on estimating the optimal conditions of magnetic and electrostatic separations for improving the separation efficiency of valuable ferrous and non-ferrous metals such as iron (Fe), aluminum, copper and etc. In magnetic separation, 91.5% Fe grade and 91% recovery could be obtained at conditions of particle size under 10mm and magnetic intensity of 400 gauss. In corona electrostatic separation for recovering nonferrous metals, a grade of 79.2% and recovery of 90.7% could be successfully achieved under conditions of -6mm particle size, 50kV electrode potential, 35rpm drum speed and 20 degree splitter position, respectively. Acknowledgments This study was supported by the R&D Center for Valuable Recycling (Global-Top R&BD Program) of the Ministry of Environment. (Project No. 2016002250001)

An integrated biodesulfurization process, including inoculum preparation, desulfurization and sulfate removal in a single step, for removing sulfur from oils.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tangaromsuk, Jantana; Borole, Abhijeet P; Kruatrachue, Maleeya

2008-01-01

BACKGROUND: A single-stage reactor, in which the growth of bacterial culture, induction of desulfurizing enzymes, and desulfurization reaction are carried out in a single step, was adopted to investigate desulfurization of DBT at high cell densities. IGTS8 was used as the biocatalyst. Optimal condition for the bacterial growth and DBT desulfurization were also investigated. RESULTS: Optimization of fermentation conditions was necessary to obtain high cell densities including controlling accumulation of acetate. Under optimal operating conditions, the maximum OD600 was measured to be 26.6 at 118 h of cultivation. When biodesulfurization of DBT in model oil with a high cell densitymore » culture of IGTS8 was investigated, accumulation of sulfate was found to limit the extent of desulfurization. A sulfate removal step was added to obtain a single-stage integrated biodesulfurization process. Sulfate removal was achieved via an aqueous bleed stream and use of a separation unit to recycle the organic phase. CONCLUSION : A proof of principle of a complete system capable of biocatalyst growth, induction, desulfurization and by-product separation was demonstrated. This system enables simplification of the biodesulfurization process and has potential to lower the operating cost of the bioprocess.« less

Light intensity distribution optimization for tunnel lamps in different zones of a long tunnel.

PubMed

Lai, Wei; Liu, Xianming; Chen, Weimin; Lei, Xiaohua; Cheng, Xingfu

2014-09-22

The light distributions in different tunnel zones have different requirements in order to meet the driver's visual system. In this paper, the light intensity distributions of tunnel lamps in different zones of a long tunnel are optimized separately. A common nonlinear optimization approach is proposed to minimize the consuming power as well as satisfy the luminance and glare requirements both on the road surface and on the wall set by International Commission on Illumination (CIE). Compared with that of the reported linear optimization method, the optimization model can save energy from 11% to 57.6% under the same installation conditions.

Analysis of low molecular weight acids by monolithic immobilized pH gradient-based capillary isoelectric focusing coupled with mass spectrometry.

PubMed

Wang, Tingting; Fekete, Agnes; Gaspar, Andras; Ma, Junfeng; Liang, Zhen; Yuan, Huiming; Zhang, Lihua; Schmitt-Kopplin, Philippe; Zhang, Yukui

2011-02-01

A novel method for the separation and detection of low molecular weight (LMW) acids was developed using monolithic immobilized pH gradient-based capillary isoelectric focusing coupled with mass spectrometry. Two main parameters, focusing conditions and delivery buffer conditions, which might affect separation efficiency, were optimized with the focusing time of 7 min at 350 V/cm and the delivery buffer of 50% (v/v) acetonitrile in 10 mmol/L ammonium formate (pH 3.0). Under these conditions, the linear correlation between the volume of delivery solvent and the pK(a) of the model components was observed. In addition, the separation mechanism of LMW acids was proposed as well. We suppose that this method may provide a useful tool for the characterization of LMW components (e.g. natural organic matter of different origins). Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimization of entanglement witnesses

NASA Astrophysics Data System (ADS)

Lewenstein, M.; Kraus, B.; Cirac, J. I.; Horodecki, P.

2000-11-01

An entanglement witness (EW) is an operator that allows the detection of entangled states. We give necessary and sufficient conditions for such operators to be optimal, i.e., to detect entangled states in an optimal way. We show how to optimize general EW, and then we particularize our results to the nondecomposable ones; the latter are those that can detect positive partial transpose entangled states (PPTES's). We also present a method to systematically construct and optimize this last class of operators based on the existence of ``edge'' PPTES's, i.e., states that violate the range separability criterion [Phys. Lett. A 232, 333 (1997)] in an extreme manner. This method also permits a systematic construction of nondecomposable positive maps (PM's). Our results lead to a sufficient condition for entanglement in terms of nondecomposable EW's and PM's. Finally, we illustrate our results by constructing optimal EW acting on H=C2⊗C4. The corresponding PM's constitute examples of PM's with minimal ``qubit'' domains, or-equivalently-minimal Hermitian conjugate codomains.

Separation of porphyrin-based photosensitizer isomers by laser-induced fluorescence capillary electrophoresis.

PubMed

Peng, Xuejun; Sternberg, Ethan; Dolphin, David

2005-10-01

Methods for the separation of photosensitizer isomers, such as benzoporphyrin derivative monoacid, benzoporphyrin ethyl monoacid, 2-[1-hexyloxyethyl]-2-devinylpyropheophorbide-a, diethyleneglycol diester benzoporphyrin derivative, tin ethyl etiopurpurin, and phthalocyanine tetrasulfonate, have been systematically developed by CE. Detection was accomplished by UV absorption at 214 nm or by LIF with excitation at 442/488 nm and emission at 690 nm. The effects of three major experimental parameters of buffer types, organic solvents, and surfactant additives are described. The optimized separation conditions were determined so as to provide satisfactory separation efficiency and analysis time. The methods are shown to be suitable for the separation and determination of porphyrin and phthalocyanines regioisomers, diastereoisomers, and enantiomers.

Enantiomeric resolution of five chiral pesticides on a Chiralpak IB-H column by SFC.

PubMed

Jin, Lixia; Gao, Weiliang; Yang, Huayun; Lin, Chunmian; Liu, Weiping

2011-10-01

The enantiomeric separations of five chiral pesticides, diclofopmethyl, 1; benalaxy, 2; acetofenate, 3; myclobutanil, 4; and difenoconazole, 5, were conducted on a Chiralpak IB-H column by a packed-column supercritical fluid chromatography (p-SFC). All compounds, except difenoconazole and myclobutanil, were well resolved within 10 min. As the mobile phase polarity decreased through changing the percentage and the type of alcohol modifiers in the supercritical carbon dioxide (CO(2)), the retention time, the separation factors, and the resolution increased. However, based on the retention time and the resolution, the optimized separations were obtained with the mobile phase containing 10% 2-propanol for diclofop-methyl 1; benalaxy, 2; myclobutanil, 4; difenoconazole, 5; and containing 3% 2-propanol for acetofenate, 3. The optimized separation temperature was at 35°C under the supercritical fluid condition. The π-π interactions and the hydrogen bonding interactions between Chiralpak IB-H CSP and the analytes might be the main chiral discriminations on enantioseparation of these five pesticides.

[Research of the essential oil of Plumeria rubra var. actifolia from Laos by supercritical carbon dioxide extraction].

PubMed

Xiao, Xin-Yu; Cui, Long-Hai; Zhou, Xin-Xin; Wu, Yan; Ge, Fa-Huan

2011-05-01

The orthogonal test and the supercritical carbon dioxide fluid extraction were used for optimizing the extraction of the essential oil from Plumeria rubra var. actifolia for the first time. Compared with the steam distillation, the optimal operation parameter of extraction was as follows: extraction pressure 25 MPa, extraction temperature 45 degrees C; separator I pressure 12 MPa, separator I temperature 55 degrees C; separator II pressure 6 MPa, separator II temperature 30 degrees C. Under this condition the yield of the essential oil was 5.8927%. The components were separated and identified by GC-MS. 53 components of Plumeria rubra var. actifolia measured by SFE method were identified and determined by normalization method. The main components were 1, 6, 10-dodecatrien-3-ol, 3, 7, 11-trimethyl, benzoic acid, 2-hydroxy-, phenylmethyl ester, 1, 2-benzenedicarboxylic acid, bis(2-methylpropyl) ester,etc.. 1, 2-Benzenedicarboxylic acid, bis (2-methylpropyl) este. took up 66.11% of the total amount, and there was much difference of the results from SD method.

Separation of 20 coumarin derivatives using the capillary electrophoresis method optimized by a series of Doehlert experimental designs.

PubMed

Woźniakiewicz, Michał; Gładysz, Marta; Nowak, Paweł M; Kędzior, Justyna; Kościelniak, Paweł

2017-05-15

The aim of this study was to develop the first CE-based method enabling separation of 20 structurally similar coumarin derivatives. To facilitate method optimization a series of three consequent Doehlert experimental designs with the response surface methodology was employed, using number of peaks and the adjusted time of analysis as the selected responses. Initially, three variables were examined: buffer pH, ionic strength and temperature (No. 1 Doehlert design). The optimal conditions provided only partial separation, on that account, several buffer additives were examined at the next step: organic cosolvents and cyclodextrin (No. 2 Doehlert design). The optimal cyclodextrin type was also selected experimentally. The most promising results were obtained for the buffers fortified with methanol, acetonitrile and heptakis(2,3,6-tri-O-methyl)-β-cyclodextrin. Since these additives may potentially affect acid-base equilibrium and ionization state of analytes, the third Doehlert design (No. 3) was used to reconcile concentration of these additives with optimal pH. Ultimately, the total separation of all 20 compounds was achieved using the borate buffer at basic pH 9.5 in the presence of 10mM cyclodextrin, 9% (v/v) acetonitrile and 36% (v/v) methanol. Identity of all compounds was confirmed using the in-lab build UV-VIS spectra library. The developed method succeeded in identification of coumarin derivatives in three real samples. It demonstrates a huge resolving power of CE assisted by addition of cyclodextrins and organic cosolvents. Our unique optimization approach, based on the three Doehlert designs, seems to be prospective for future applications of this technique. Copyright © 2017 Elsevier B.V. All rights reserved.

How to determine an optimal threshold to classify real-time crash-prone traffic conditions?

PubMed

Yang, Kui; Yu, Rongjie; Wang, Xuesong; Quddus, Mohammed; Xue, Lifang

2018-08-01

One of the proactive approaches in reducing traffic crashes is to identify hazardous traffic conditions that may lead to a traffic crash, known as real-time crash prediction. Threshold selection is one of the essential steps of real-time crash prediction. And it provides the cut-off point for the posterior probability which is used to separate potential crash warnings against normal traffic conditions, after the outcome of the probability of a crash occurring given a specific traffic condition on the basis of crash risk evaluation models. There is however a dearth of research that focuses on how to effectively determine an optimal threshold. And only when discussing the predictive performance of the models, a few studies utilized subjective methods to choose the threshold. The subjective methods cannot automatically identify the optimal thresholds in different traffic and weather conditions in real application. Thus, a theoretical method to select the threshold value is necessary for the sake of avoiding subjective judgments. The purpose of this study is to provide a theoretical method for automatically identifying the optimal threshold. Considering the random effects of variable factors across all roadway segments, the mixed logit model was utilized to develop the crash risk evaluation model and further evaluate the crash risk. Cross-entropy, between-class variance and other theories were employed and investigated to empirically identify the optimal threshold. And K-fold cross-validation was used to validate the performance of proposed threshold selection methods with the help of several evaluation criteria. The results indicate that (i) the mixed logit model can obtain a good performance; (ii) the classification performance of the threshold selected by the minimum cross-entropy method outperforms the other methods according to the criteria. This method can be well-behaved to automatically identify thresholds in crash prediction, by minimizing the cross entropy between the original dataset with continuous probability of a crash occurring and the binarized dataset after using the thresholds to separate potential crash warnings against normal traffic conditions. Copyright © 2018 Elsevier Ltd. All rights reserved.

Experimental and Model Studies on Continuous Separation of 2-Phenylpropionic Acid Enantiomers by Enantioselective Liquid-Liquid Extraction in Centrifugal Contactor Separators.

PubMed

Feng, Xiaofeng; Tang, Kewen; Zhang, Pangliang; Yin, Shuangfeng

2016-03-01

Multistage enantioselective liquid-liquid extraction (ELLE) of 2-phenylpropionic acid (2-PPA) enantiomers using hydroxypropyl-β-cyclodextrin (HP-β-CD) as extractant was studied experimentally in a counter-current cascade of centrifugal contactor separators (CCSs). Performance of the process was evaluated by purity (enantiomeric excess, ee) and yield (Y). A multistage equilibrium model was established on the basis of single-stage model for chiral extraction of 2-PPA enantiomers and the law of mass conservation. A series of experiments on the extract phase/washing phase ratio (W/O ratio), extractant concentration, the pH value of aqueous phase, and the number of stages was conducted to verify the multistage equilibrium model. It was found that model predictions were in good agreement with the experimental results. The model was applied to predict and optimize the symmetrical separation of 2-PPA enantiomers. The optimal conditions for symmetric separation involves a W/O ratio of 0.6, pH of 2.5, and HP-β-CD concentration of 0.1 mol L(-1) at a temperature of 278 K, where eeeq (equal enantiomeric excess) can reach up to 37% and Yeq (equal yield) to 69%. By simulation and optimization, the minimum number of stages was evaluated at 98 and 106 for eeeq > 95% and eeeq > 97%. © 2016 Wiley Periodicals, Inc.

Adsorption separation of carbon dioxide from flue gas by a molecularly imprinted adsorbent.

PubMed

Zhao, Yi; Shen, Yanmei; Ma, Guoyi; Hao, Rongjie

2014-01-01

CO2 separation by molecularly imprinted adsorbent from coal-fired flue gas after desulfurization system has been studied. The adsorbent was synthesized by molecular imprinted technique, using ethanedioic acid, acrylamide, and ethylene glycol dimethacrylate as the template, functional monomer, and cross-linker, respectively. According to the conditions of coal-fired flue gas, the influencing factors, including adsorption temperature, desorption temperature, gas flow rate, and concentrations of CO2, H2O, O2, SO2, and NO, were studied by fixed bed breakthrough experiments. The experimental conditions were optimized to gain the best adsorption performance and reduce unnecessary energy consumption in future practical use. The optimized adsorption temperature, desorption temperature, concentrations of CO2, and gas flow rate are 60 °C, 80 °C, 13%, and 170 mL/min, respectively, which correspond to conditions of practical flue gases to the most extent. The CO2 adsorption performance was nearly unaffected by H2O, O2, and NO in the flue gas, and was promoted by SO2 within the emission limit stipulated in the Chinese emission standards of air pollutants for a thermal power plant. The maximum CO2 adsorption capacity, 0.57 mmol/g, was obtained under the optimized experimental conditions, and the SO2 concentration was 150 mg/m(3). The influence mechanisms of H2O, O2, SO2, and NO on CO2 adsorption capacity were investigated by infrared spectroscopic analysis.

Microwave assisted synthesis of metal-organic framework MIL-101 nanocrystals as sorbent and pseudostationary phase in capillary electrophoresis for the separation of anthraquinones in environmental water samples.

PubMed

Liu, Yue; Hu, Jia; Li, Yan; Shang, Yun-Tao; Wang, Jia-Qi; Zhang, Ye; Wang, Zhong-Liang

2017-10-01

In this work, a CE method was developed to separate five anthraquinones: aloe-emodin, rhein, emodin, chrysophanol, and physcion. The CE method used a nano-sized metal organic framework MIL-101 (nMIL-101) as pseudostationary phase (PSP) and sorbent for dispersed particle extraction (DPE). The nMIL-101 was synthesized by microwave technique and was characterized by UV-vis, TEM, Zeta potential, X-ray diffraction spectrometry and micropore physisorption. In this method, anthraquinones were adsorbed by nMIL-101 of a fast kinetics within 10 min and then separated by CE. The CE conditions were optimized considering time, pH, buffer ionic strength, and nanoparticles concentration. The optimal CE condition is using 20 mM sodium borate buffer (pH 9.1) containing 15% methanol (v/v) and 400 mg/L nMIL-101 as additives within 8 min. The LODs varied from 24 to 57 μg/L, which were lower than those previously reported. Our method has been successfully applied to determine trace anthraquinones in environmental water samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous determination of diastereoisomeric and enantiomeric impurities in SSS-octahydroindole-2-carboxylic acid by chiral high-performance liquid chromatography with pre-column derivatization.

PubMed

Wang, Jin Zhao; Zeng, Su; Hu, Gong Yun; Wang, Dan Hua

2009-04-10

SSS-Octahydroindole-2-carboxylic acid (SSS-Oic) is a key intermediate used in the synthesis of some angiotensin-converting enzyme (ACE) inhibitors. The separation of diastereoisomers and enantiomers of Oic was performed using a pre-column derivatization chiral HPLC method. Phenyl isothiocyanate (PITC) was used as the derivatization reagent. Three PITC derivatives of Oic stereoisomers were separated on an Ultron ES-OVM chiral column (150 mm x 4.6 mm, 5 microm). Derivatization conditions such as reaction temperature, reaction time and derivatization reagent concentration were investigated. The chromatographic conditions for separation of the three PITC-Oic derivatives were optimized. The method was successfully applied in the diastereoisomeric and enantiomeric purity test of SSS-Oic.

Gradient enhanced-fluidity liquid hydrophilic interaction chromatography of ribonucleic acid nucleosides and nucleotides: A "green" technique.

PubMed

Beilke, Michael C; Beres, Martin J; Olesik, Susan V

2016-03-04

A "green" hydrophilic interaction liquid chromatography (HILIC) technique for separating the components of mixtures with a broad range of polarities is illustrated using enhanced-fluidity liquid mobile phases. Enhanced-fluidity liquid chromatography (EFLC) involves the addition of liquid CO2 to conventional liquid mobile phases. Decreased mobile phase viscosity and increased analyte diffusivity results when a liquefied gas is dissolved in common liquid mobile phases. The impact of CO2 addition to a methanol:water (MeOH:H2O) mobile phase was studied to optimize HILIC gradient conditions. For the first time a fast separation of 16 ribonucleic acid (RNA) nucleosides/nucleotides was achieved (16min) with greater than 1.3 resolution for all analyte pairs. By using a gradient, the analysis time was reduced by over 100% compared to similar separations conducted under isocratic conditions. The optimal separation using MeOH:H2O:CO2 mobile phases was compared to MeOH:H2O and acetonitrile:water (ACN:H2O) mobile phases. Based on chromatographic performance parameters (efficiency, resolution and speed of analysis) and an assessment of the environmental impact of the mobile phase mixtures, MeOH:H2O:CO2 mixtures are preferred over ACN:H2O or MeOH:H2O mobile phases for the separation of mixtures of RNA nucleosides and nucleotides. Copyright © 2016 Elsevier B.V. All rights reserved.

A trust-region algorithm for the optimization of PSA processes using reduced-order modeling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Agarwal, A.; Biegler, L.; Zitney, S.

2009-01-01

The last few decades have seen a considerable increase in the applications of adsorptive gas separation technologies, such as pressure swing adsorption (PSA); the applications range from bulk separations to trace contaminant removal. PSA processes are based on solid-gas equilibrium and operate under periodic transient conditions [1]. Bed models for these processes are therefore defined by coupled nonlinear partial differential and algebraic equations (PDAEs) distributed in space and time with periodic boundary conditions that connect the processing steps together and high nonlinearities arising from non-isothermal effects and nonlinear adsorption isotherms. As a result, the optimization of such systems for eithermore » design or operation represents a significant computational challenge to current nonlinear programming algorithms. Model reduction is a powerful methodology that permits systematic generation of cost-efficient low-order representations of large-scale systems that result from discretization of such PDAEs. In particular, low-dimensional approximations can be obtained from reduced order modeling (ROM) techniques based on proper orthogonal decomposition (POD) and can be used as surrogate models in the optimization problems. In this approach, a representative ensemble of solutions of the dynamic PDAE system is constructed by solving a higher-order discretization of the model using the method of lines, followed by the application of Karhunen-Loeve expansion to derive a small set of empirical eigenfunctions (POD modes). These modes are used as basis functions within a Galerkin's projection framework to derive a low-order DAE system that accurately describes the dominant dynamics of the PDAE system. This approach leads to a DAE system of significantly lower order, thus replacing the one obtained from spatial discretization before and making optimization problem computationally efficient [2]. The ROM methodology has been successfully applied to a 2-bed 4-step PSA process used for separating a hydrogen-methane mixture in [3]. The reduced order model developed was successfully used to optimize this process to maximize hydrogen recovery within a trust-region. We extend this approach in this work to develop a rigorous trust-region algorithm for ROM-based optimization of PSA processes. The trust-region update rules and sufficient decrease condition for the objective is used to determine the size of the trust-region. Based on the decrease in the objective function and error in the ROM, a ROM updation strategy is designed [4, 5]. The inequalities and bounds are handled in the algorithm using exact penalty formulation, and a non-smooth trust-region algorithm by Conn et al. [6] is used to handle non-differentiability. To ensure that the first order consistency condition is met and the optimum obtained from ROM-based optimization corresponds to the optimum of the original problem, a scaling function, such as one proposed by Alexandrov et al. [7], is incorporated in the objective function. Such error control mechanism is also capable of handling numerical inconsistencies such as unphysical oscillations in the state variable profiles. The proposed methodology is applied to optimize a PSA process to concentrate CO{sub 2} from a nitrogen-carbon dioxide mixture. As in [3], separate ROMs are developed for each operating step with different POD modes for each state variable. Numerical results will be presented for optimization case studies which involve maximizing CO{sub 2} recovery, feed throughput or minimizing overall power consumption.« less

[Study on separation of essential oil of Caryophylli flos from oil-in-water emulsion by microfiltration].

PubMed

Han, Zhifeng; Shen, Jie; Guo, Liwei; Fan, Wenlin

2011-01-01

To separate essential oil of Caryophyllix flos from oil-in-water emulsion, and to enrich the essential oil by microfiltration (MF). Using membrane flux and removal rate of COD as the indicatrixes, the membrane material as well as the operating conditions containing pressure, surface speed, temperature were optimized. The results showed that QWLM membrane of hydrophilic is the proper membrane, and the best operating conditions was at 0.06 MPa, 60 degrees C, and 150 r min(-1) stir speed. It can be concluded that MF is a reasonable way to enrich essential oil of C. flox.

Optimising reversed-phase liquid chromatographic separation of an acidic mixture on a monolithic stationary phase with the aid of response surface methodology and experimental design.

PubMed

Wang, Y; Harrison, M; Clark, B J

2006-02-10

An optimization strategy for the separation of an acidic mixture by employing a monolithic stationary phase is presented, with the aid of experimental design and response surface methodology (RSM). An orthogonal array design (OAD) OA(16) (2(15)) was used to choose the significant parameters for the optimization. The significant factors were optimized by using a central composite design (CCD) and the quadratic models between the dependent and the independent parameters were built. The mathematical models were tested on a number of simulated data set and had a coefficient of R(2) > 0.97 (n = 16). On applying the optimization strategy, the factor effects were visualized as three-dimensional (3D) response surfaces and contour plots. The optimal condition was achieved in less than 40 min by using the monolithic packing with the mobile phase of methanol/20 mM phosphate buffer pH 2.7 (25.5/74.5, v/v). The method showed good agreement between the experimental data and predictive value throughout the studied parameter space and were suitable for optimization studies on the monolithic stationary phase for acidic compounds.

Optimization of Pulsed-DEER Measurements for Gd-Based Labels: Choice of Operational Frequencies, Pulse Durations and Positions, and Temperature

DOE Office of Scientific and Technical Information (OSTI.GOV)

Raitsimring, A.; Astashkin, A. V.; Enemark, J. H.

2012-12-29

In this work, the experimental conditions and parameters necessary to optimize the long-distance (≥ 60 Å) Double Electron-Electron Resonance (DEER) measurements of biomacromolecules labeled with Gd(III) tags are analyzed. The specific parameters discussed are the temperature, microwave band, the separation between the pumping and observation frequencies, pulse train repetition rate, pulse durations and pulse positioning in the electron paramagnetic resonance spectrum. It was found that: (i) in optimized DEER measurements, the observation pulses have to be applied at the maximum of the EPR spectrum; (ii) the optimal temperature range for Ka-band measurements is 14-17 K, while in W-band the optimalmore » temperatures are between 6-9 K; (iii) W-band is preferable to Ka-band for DEER measurements. Recent achievements and the conditions necessary for short-distance measurements (<15 Å) are also briefly discussed.« less

Low voltage electrophoresis chip with multi-segments synchronized scanning

NASA Astrophysics Data System (ADS)

Gu, Wenwen; Wen, Zhiyu; Xu, Yi

2017-03-01

For low voltage electrophoresis chip, there is always a problem that the samples are truncated and peaks are broadened, as well as longer time for separation. In this paper, a low voltage electrophoresis separation model was established, and the separation conditions were discussed. A new driving mode was proposed for applying low voltage, which was called multi-segments synchronized scanning. By using this driving mode, the reversed electric field that existed between the multi-segments can enrich samples and shorten the sample zone. The low voltage electrophoresis experiments using multi-segments synchronized scanning were carried out by home-made silicon-PDMS-based chip. The fluorescein isothiocyanate (FITC) labeled lysine and phenylalanine mixed samples with the concentration of 10-4 mol/L were successfully separated under the optimal conditions of 10 mmol/L borax buffer (pH = 10.0), 200 V/cm separation electric field and electrode switch time of 2.5 s. The separation was completed with a resolution of 2.0, and the peak time for lysine and phenylalanine was 4 min and 6 min, respectively.

Partial least squares model and design of experiments toward the analysis of the metabolome of Jatropha gossypifolia leaves: Extraction and chromatographic fingerprint optimization.

PubMed

Pilon, Alan Cesar; Carnevale Neto, Fausto; Freire, Rafael Teixeira; Cardoso, Patrícia; Carneiro, Renato Lajarim; Da Silva Bolzani, Vanderlan; Castro-Gamboa, Ian

2016-03-01

A major challenge in metabolomic studies is how to extract and analyze an entire metabolome. So far, no single method was able to clearly complete this task in an efficient and reproducible way. In this work we proposed a sequential strategy for the extraction and chromatographic separation of metabolites from leaves Jatropha gossypifolia using a design of experiments and partial least square model. The effect of 14 different solvents on extraction process was evaluated and an optimized separation condition on liquid chromatography was estimated considering mobile phase composition and analysis time. The initial conditions of extraction using methanol and separation in 30 min between 5 and 100% water/methanol (1:1 v/v) with 0.1% of acetic acid, 20 μL sample volume, 3.0 mL min(-1) flow rate and 25°C column temperature led to 107 chromatographic peaks. After the optimization strategy using i-propanol/chloroform (1:1 v/v) for extraction, linear gradient elution of 60 min between 5 and 100% water/(acetonitrile/methanol 68:32 v/v with 0.1% of acetic acid), 30 μL sample volume, 2.0 mL min(-1) flow rate, and 30°C column temperature, we detected 140 chromatographic peaks, 30.84% more peaks compared to initial method. This is a reliable strategy using a limited number of experiments for metabolomics protocols. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Analysis and separation of organic and inorganic speciations of soluble zinc in edible flowers].

PubMed

Peng, Shan-shan; Huang, Guo-qing

2005-02-01

Considering the medicinal effects of the edible flowers, the authors studied the separation of trace element zinc's soluble organic and inorganic speciations in water decoction of three edible flowers: Chrysanthemum, Cottonrose hibiscus and Honeysucker by using the 0.45 microm membrane filter and amberlite XAD-2 macroreticular resins. And trace element zinc contents were determined by atomic absorption spectrometry. The optimal conditions for separation had been established. This study verifies the economic value of developing edible flowers, and provides theoretical basis for developing edible flowers as the third functional food materials.

Barriers to success: physical separation optimizes event-file retrieval in shared workspaces.

PubMed

Klempova, Bibiana; Liepelt, Roman

2017-07-08

Sharing tasks with other persons can simplify our work and life, but seeing and hearing other people's actions may also be very distracting. The joint Simon effect (JSE) is a standard measure of referential response coding when two persons share a Simon task. Sequential modulations of the joint Simon effect (smJSE) are interpreted as a measure of event-file processing containing stimulus information, response information and information about the just relevant control-state active in a given social situation. This study tested effects of physical (Experiment 1) and virtual (Experiment 2) separation of shared workspaces on referential coding and event-file processing using a joint Simon task. In Experiment 1, participants performed this task in individual (go-nogo), joint and standard Simon task conditions with and without a transparent curtain (physical separation) placed along the imagined vertical midline of the monitor. In Experiment 2, participants performed the same tasks with and without receiving background music (virtual separation). For response times, physical separation enhanced event-file retrieval indicated by an enlarged smJSE in the joint Simon task with curtain than without curtain (Experiment1), but did not change referential response coding. In line with this, we also found evidence for enhanced event-file processing through physical separation in the joint Simon task for error rates. Virtual separation did neither impact event-file processing, nor referential coding, but generally slowed down response times in the joint Simon task. For errors, virtual separation hampered event-file processing in the joint Simon task. For the cognitively more demanding standard two-choice Simon task, we found music to have a degrading effect on event-file retrieval for response times. Our findings suggest that adding a physical separation optimizes event-file processing in shared workspaces, while music seems to lead to a more relaxed task processing mode under shared task conditions. In addition, music had an interfering impact on joint error processing and more generally when dealing with a more complex task in isolation.

Demonstration of hydrazide tagging for O-glycans and a central composite design of experiments optimization using the INLIGHT™ reagent.

PubMed

King, Samuel R; Hecht, Elizabeth S; Muddiman, David C

2018-02-01

The INLIGHT™ strategy for N-linked glycan derivatization has been shown to overcome many of the challenges associated with glycan analysis. The hydrazide tag reacts efficiently with the glycans, increasing their non-polar surface area, allowing for reversed-phase separations and increased ionization efficiency. We have taken the INLIGHT™ strategy and adopted it for use with O-linked glycans. A central composite design was utilized to find optimized tagging conditions (45% acetic acid, 0.1 μg/μL tag concentration, 37 C, 1.75 h). Derivatization at optimized conditions was much quicker than any hydrazide derivatization strategy used previously. Human immunoglobulin A (IgA) and bovine submaxillary mucin (BSM) were then deglycosylated through hydrazinolysis and the removed glycans were tagged under optimum conditions. XIC of tagged glycans and MS2 data show successful hydrazide tagging of O-linked glycans for the first time. Graphical abstract The INLIGHT™ hydrazide tag was optimized using a central composite design for derivatization of O-linked glycans. Two glycoprotein standards were deglycosylated through hydrazinolysis and tagged at the optimized conditions. MS/MS data shows INLIGHT™ derivatization of glycans demonstrating successful hydrazide tagging of O-glycans for the first time.

Optimizing a Laser Process for Making Carbon Nanotubes

NASA Technical Reports Server (NTRS)

Arepalli, Sivaram; Nikolaev, Pavel; Holmes, William

2010-01-01

A systematic experimental study has been performed to determine the effects of each of the operating conditions in a double-pulse laser ablation process that is used to produce single-wall carbon nanotubes (SWCNTs). The comprehensive data compiled in this study have been analyzed to recommend conditions for optimizing the process and scaling up the process for mass production. The double-pulse laser ablation process for making SWCNTs was developed by Rice University researchers. Of all currently known nanotube-synthesizing processes (arc and chemical vapor deposition), this process yields the greatest proportion of SWCNTs in the product material. The aforementioned process conditions are important for optimizing the production of SWCNTs and scaling up production. Reports of previous research (mostly at Rice University) toward optimization of process conditions mention effects of oven temperature and briefly mention effects of flow conditions, but no systematic, comprehensive study of the effects of process conditions was done prior to the study described here. This was a parametric study, in which several production runs were carried out, changing one operating condition for each run. The study involved variation of a total of nine parameters: the sequence of the laser pulses, pulse-separation time, laser pulse energy density, buffer gas (helium or nitrogen instead of argon), oven temperature, pressure, flow speed, inner diameter of the flow tube, and flow-tube material.

Optimization and quality assessment of the post-digestion 18O labeling based on urea for protein denaturation by HPLC/ESI-TOF mass spectrometry.

PubMed

Wang, Hongbin; Hu, Gaofei; Zhang, Yongqian; Yuan, Zheng; Zhao, Xuan; Zhu, Yong; Cai, De; Li, Yujuan; Xiao, Shengyuan; Deng, Yulin

2010-07-15

The post-digestion (18)O labeling method decouples protein digestion and peptide labeling. This method allows labeling conditions to be optimized separately and increases labeling efficiency. A common method for protein denaturation in proteomics is the use of urea. Though some previous studies have used urea-based protein denaturation before post-digestion (18)O labeling, the optimal (18)O labeling conditions in this case have not been yet reported. Present study investigated the effects of urea concentration and pH on the labeling efficiency and obtained an optimized protocol. It was demonstrated that urea inhibited (18)O incorporation depending on concentration. However, a urea concentration between 1 and 2M had minimal effects on labeling. It was also demonstrated that the use of FA to quench the digestion reaction severely affected the labeling efficiency. This study revealed the reason why previous studies gave different optimal pH for labeling. They neglect the effects of different digestion conditions on the labeling conditions. Excellent labeling quality was obtained at the optimized conditions using urea 1-2 M and pH 4.5, 98.4+/-1.9% for a standard protein mixture and 97.2+/-6.2% for a complex biological sample. For a 1:1 mixture analysis of the (16)O- and (18)O-labeled peptides from the same protein sample, the average abundance ratios reached 1.05+/-0.31, demonstrating a good quantitation quality at the optimized conditions. This work will benefit other researchers who pair urea-based protein denaturation with a post-digestion (18)O labeling method. 2010 Elsevier B.V. All rights reserved.

Blending protein separation and peptide analysis through real-time proteolytic digestion.

PubMed

Slysz, Gordon W; Schriemer, David C

2005-03-15

Typical liquid- or gel-based protein separations require enzymatic digestion as an important first step in generating protein identifications. Traditional protocols involve long-term proteolytic digestion of the separated protein, often leading to sample loss and reduced sensitivity. Previously, we presented a rapid method of proteolytic digestion that showed excellent digestion of resistant and low concentrations of protein without requiring reduction and alkylation. Here, we demonstrate on-line, real-time tryptic digestion in conjunction with reversed-phase protein separation. The studies were aimed at optimizing pH and ionic strength and the size of the digestion element, to produce maximal protein digestion with minimal effects on chromatographic integrity. Upon establishing optimal conditions, the digestion element was attached downstream from a capillary C4 reversed-phase column. A four-protein mixture was processed through the combined system, and the resulting peptides were analyzed on-line by electrospray mass spectrometry. Extracted ion chromatograms for protein chromatography based on peptide elution were generated. These were shown to emulate ion chromatograms produced in a subsequent run without the digestion element, based on protein elution. The methodology will enable rapid and sensitive analysis of liquid-based protein separations using the power of bottom-up proteomics methodologies.

Optimization and development of a SPE-HPLC-UV method to determine astaxanthin in Saccharina japonica.

PubMed

Zhou, Jun; Bi, Wentao; Row, Kyung Ho

2011-04-01

An effective and accurate method including extraction, saponification, and separation was developed to determine astaxanthin (AX) in Saccharina japonica. The optimal extraction conditions with different solvents were investigated. 29.30 μg/g of AX was extracted from dry Saccharina japonica powder by solvent. After subsequent saponification, the extracted amount of AX was increased to 37.26 μg/g. Furthermore, 3 different ionic liquid-based silicas were prepared as sorbents for the solid phase extraction of AX from the extract. By comparing the adsorption isotherms of AX on different ionic liquid-based silicas, suitable sorbent was successfully selected and applied for separation of AX from extract. Astaxanthin, in 3 main forms (free, monoesters, and diesters), can be obtained from marine plants and animals. By extraction with subsequent saponification, the astaxanthin was extracted from Saccharina japonica. And then, ionic liquid-based silicas were used to separate the astaxanthin from the extract solution. This method can be widely applied for determination, or even industrial separation and purification of astaxanthin from many other algae.

DNA analysis using an integrated microchip for multiplex PCR amplification and electrophoresis for reference samples.

PubMed

Le Roux, Delphine; Root, Brian E; Reedy, Carmen R; Hickey, Jeffrey A; Scott, Orion N; Bienvenue, Joan M; Landers, James P; Chassagne, Luc; de Mazancourt, Philippe

2014-08-19

A system that automatically performs the PCR amplification and microchip electrophoretic (ME) separation for rapid forensic short tandem repeat (STR) forensic profiling in a single disposable plastic chip is demonstrated. The microchip subassays were optimized to deliver results comparable to conventional benchtop methods. The microchip process was accomplished in sub-90 min compared with >2.5 h for the conventional approach. An infrared laser with a noncontact temperature sensing system was optimized for a 45 min PCR compared with the conventional 90 min amplification time. The separation conditions were optimized using LPA-co-dihexylacrylamide block copolymers specifically designed for microchip separations to achieve accurate DNA size calling in an effective length of 7 cm in a plastic microchip. This effective separation length is less than half of other reports for integrated STR analysis and allows a compact, inexpensive microchip design. This separation quality was maintained when integrated with microchip PCR. Thirty samples were analyzed conventionally and then compared with data generated by the microfluidic chip system. The microfluidic system allele calling was 100% concordant with the conventional process. This study also investigated allelic ladder consistency over time. The PCR-ME genetic profiles were analyzed using binning palettes generated from two sets of allelic ladders run three and six months apart. Using these binning palettes, no allele calling errors were detected in the 30 samples demonstrating that a microfluidic platform can be highly consistent over long periods of time.

An electro-amalgamation approach to isolate no-carrier-added 177Lu from neutron irradiated Yb for biomedical applications.

PubMed

Chakravarty, Rubel; Das, Tapas; Dash, Ashutosh; Venkatesh, Meera

2010-10-01

A novel two-step separation process for the production of no-carrier-added (NCA) (177)Lu from neutron irradiated Yb target through an electrochemical pathway employing mercury-pool cathode has been developed. A two-cycle electrolysis procedure was adopted for separation of (177)Lu from (177)Lu/Yb mixture in lithium citrate medium. The influence of different experimental parameters on the separation process was investigated and optimized for the quantitative deposition of Yb in presence of (177)Lu. The first electrolysis was performed for 50 min in the (177)Lu/Yb feed solution at pH 6 applying a potential of 8 V using platinum electrode as anode and mercury as the cathode. The second electrolysis was performed under the same conditions using fresh electrodes. The radionuclidic and chemical purity of (177)Lu was determined by using gamma ray spectrometry and atomic absorption spectrometry. The suitability of (177)Lu for biomedical applications was ascertained by labeling 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid D-Phe(1)-Tyr(3)-octreotate(DOTA-TATE) with (177)Lu. This process could provide NCA (177)Lu with >99.99% radionuclidic purity and an overall separation yield of ∼99% was achieved within 3-4 h. The Hg content in the product was determined to be <1 ppm. Radiolabeling yield of >98% was obtained with DOTA-TATE under the optimized reaction conditions. An efficient strategy for the separation of NCA (177)Lu, suitable for biomedical applications, has been developed. Copyright © 2010 Elsevier Inc. All rights reserved.

How Much Can We Learn from a Single Chromatographic Experiment? A Bayesian Perspective.

PubMed

Wiczling, Paweł; Kaliszan, Roman

2016-01-05

In this work, we proposed and investigated a Bayesian inference procedure to find the desired chromatographic conditions based on known analyte properties (lipophilicity, pKa, and polar surface area) using one preliminary experiment. A previously developed nonlinear mixed effect model was used to specify the prior information about a new analyte with known physicochemical properties. Further, the prior (no preliminary data) and posterior predictive distribution (prior + one experiment) were determined sequentially to search towards the desired separation. The following isocratic high-performance reversed-phase liquid chromatographic conditions were sought: (1) retention time of a single analyte within the range of 4-6 min and (2) baseline separation of two analytes with retention times within the range of 4-10 min. The empirical posterior Bayesian distribution of parameters was estimated using the "slice sampling" Markov Chain Monte Carlo (MCMC) algorithm implemented in Matlab. The simulations with artificial analytes and experimental data of ketoprofen and papaverine were used to test the proposed methodology. The simulation experiment showed that for a single and two randomly selected analytes, there is 97% and 74% probability of obtaining a successful chromatogram using none or one preliminary experiment. The desired separation for ketoprofen and papaverine was established based on a single experiment. It was confirmed that the search for a desired separation rarely requires a large number of chromatographic analyses at least for a simple optimization problem. The proposed Bayesian-based optimization scheme is a powerful method of finding a desired chromatographic separation based on a small number of preliminary experiments.

On-line identification of 3,4-methylenedioxymethamphetamine in human urine by non-aqueous capillary electrophoresis-fluorescence spectroscopy at 77 K.

PubMed

Chung, Y L; Liu, J T; Lin, C H

2001-08-15

The analytical profiles for 3,4-methylenedioxymethamphetamine (3,4-MDMA) and related amphetamines in urine samples are described for non-aqueous capillary electrophoresis-fluorescence spectroscopy. 3,4-MDMA was detected and identified on-line, using a cryogenic molecular fluorescence technique at 77 K. Under optimized conditions, baseline separation of the selected compounds was achieved in less than 12 min. Precision was evaluated by measuring the repeatability and intermediate precision of the migration times and corrected peak areas. The non-aqueous CE separation conditions and the spectral characteristics of 3,4-MDMA with respect to solvent and temperature effects are also discussed.

A novel dismantling process of waste printed circuit boards using water-soluble ionic liquid.

PubMed

Zeng, Xianlai; Li, Jinhui; Xie, Henghua; Liu, Lili

2013-10-01

Recycling processes for waste printed circuit boards (WPCBs) have been well established in terms of scientific research and field pilots. However, current dismantling procedures for WPCBs have restricted the recycling process, due to their low efficiency and negative impacts on environmental and human health. This work aimed to seek an environmental-friendly dismantling process through heating with water-soluble ionic liquid to separate electronic components and tin solder from two main types of WPCBs-cathode ray tubes and computer mainframes. The work systematically investigates the influence factors, heating mechanism, and optimal parameters for opening solder connections on WPCBs during the dismantling process, and addresses its environmental performance and economic assessment. The results obtained demonstrate that the optimal temperature, retention time, and turbulence resulting from impeller rotation during the dismantling process, were 250 °C, 12 min, and 45 rpm, respectively. Nearly 90% of the electronic components were separated from the WPCBs under the optimal experimental conditions. This novel process offers the possibility of large industrial-scale operations for separating electronic components and recovering tin solder, and for a more efficient and environmentally sound process for WPCBs recycling. Copyright © 2013 Elsevier Ltd. All rights reserved.

Dataset of working conditions and thermo-economic performances for hybrid organic Rankine plants fed by solar and low-grade energy sources.

PubMed

Scardigno, Domenico; Fanelli, Emanuele; Viggiano, Annarita; Braccio, Giacobbe; Magi, Vinicio

2016-06-01

This article provides the dataset of operating conditions of a hybrid organic Rankine plant generated by the optimization procedure employed in the research article "A genetic optimization of a hybrid organic Rankine plant for solar and low-grade energy sources" (Scardigno et al., 2015) [1]. The methodology used to obtain the data is described. The operating conditions are subdivided into two separate groups: feasible and unfeasible solutions. In both groups, the values of the design variables are given. Besides, the subset of feasible solutions is described in details, by providing the thermodynamic and economic performances, the temperatures at some characteristic sections of the thermodynamic cycle, the net power, the absorbed powers and the area of the heat exchange surfaces.

FACTORS AFFECTING THE UPTAKE OF LISSAMINE GREEN BY SERUM PROTEINS

PubMed Central

Brackenridge, C. J.

1960-01-01

Eight physicochemical factors which affect the uptake of lissamine green on filter paper impregnated with serum proteins have been examined, and their relevance to the staining of electrophoretically separated protein fractions is discussed. It is shown that grade of paper, weight of protein applied, separate and combined denaturation and staining time, temperature and concentration of staining solution, concentration of denaturant, and type of protein all influence the weight of dye absorbed per unit weight of applied protein, and must be rigidly standardized if valid quantitative results are to be obtained. Five sets of conditions are obtained for optimal staining and it is found that separation of denaturant from dye yields the best procedure. It is concluded that lissamine green is an excellent dye for the staining and quantitative estimation of separated protein fractions in paper electrophoresis, and that conditions can usually be arranged to produce a linear relation between dye uptake and protein concentration in an experimentally efficient manner. PMID:13803681

Investigation, comparison and design of chambers used in centrifugal partition chromatography on the basis of flow pattern and separation experiments.

PubMed

Schwienheer, C; Merz, J; Schembecker, G

2015-04-17

In centrifugal partition chromatography (CPC) the separation efficiency is mainly influenced by the hydrodynamic of mobile and stationary phase in the chambers. Thus, the hydrodynamic has to be investigated and understood in order to enhance a CPC separation run. Different chamber geometries have been developed in the past and the influence of several phase systems and CPC operating conditions were investigated for these chambers. However, a direct comparison between the different chamber types has not been performed yet. In order to investigate the direct influence of the chamber design on the hydrodynamic, several chamber designs - partially similar in geometry to commercial available designs - are investigated under standardized conditions in the present study. The results show the influence of geometrical aspects of the chamber design on the hydrodynamic and therewith, on the separation efficiency. As a conclusion of the present study, some ideas for an optimal chamber design for laboratory and industrial purpose are proposed. Copyright © 2015 Elsevier B.V. All rights reserved.

[Extraction of 10-Deacetyl Baccatin by Supercritical CO2 from Taxus yunnanensis Branches and Leaves].

PubMed

Tang, Yang-qin; Li, Hai-chi; Huang, Wen-jie; Xiong, Yan; Ge, Fa-huan

2015-04-01

To study the supercritical CO2 fluids extraction (SFE) method to extract the components from Taxus yunnanensis. Medicinal meterials were extracted by supercritical CO2, and then purified by industrial chromatography. Using the extraction yield of 10-DAB as the index,single factor test was carried out to investigate the effect of co-solvent, extraction time, extraction pressure, extraction temperature, pressure and temperature of separation kettle I. Then orthogonal experiment was used to optimize the best extraction condition. The suitable extraction condition was as follows: the ratio of co-solvent (80% ethanol) amount and the madicinal materials was 3: 1, Separation kettle I pressure was 14 MPa, separation kettle I temperature was 40 °C, extraction pressure was 25 MPa, extraction temperature was 60 T and extraction time was 90 min. The extract was separated by industrial chromatographic and then crystallized. The supercritical CO2 extraction and purification process of 10-DAB were simple and feasible.

Arsenic species separation by IELC-ICP/OES: Arsenocholine behavior

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rubio, R.; Peralta, I.; Alberti, J.

1993-01-01

In the literature an increasing interest is observed in developing methods to determine arsenobetaine, arsenocholine and related compounds in sea food and in reference materials. The separation conditions and quantification of As(III), As(V), monomethylarsenate (MMA), dimethylarsinate (DMA), arsenobetaine (AsBet) and arsenocholine (AsChol) are studied by Liquid Chromatography (LC) coupled directly to an Inductively Coupled Plasma Optical Emission Spectroscopy (ICP/OES) system. The separation conditions are optimized to improve the resolution of the six arsenic species. Arsenocholine shows a particular pattern of behavior when phosphate is used as eluent: two peaks are observed in the chromatogram, thus a systematic study assaying differentmore » pH and concentration of phosphate is carried out to improve resolution and analysis time when the six arsenic compounds are analyzed in a mixture. Boric acid as mobile phase avoids the splitting of the arsenocholine peak and leads to a good separation of the six arsenic compounds. Detection limits are established for the six arsenic species.« less

Separation of polyethylene glycols and amino-terminated polyethylene glycols by high-performance liquid chromatography under near critical conditions.

PubMed

Wei, Y-Z; Zhuo, R-X; Jiang, X-L

2016-05-20

The separation and characterization of polyethylene glycols (PEGs) and amino-substituted derivatives on common silica-based reversed-phase packing columns using isocratic elution is described. This separation is achieved by liquid chromatography under the near critical conditions (LCCC), based on the number of amino functional end groups without obvious effect of molar mass for PEGs. The mobile phase is acetonitrile in water with an optimal ammonium acetate buffer. The separation mechanism of PEG and amino-substituted PEG under the near LCCC on silica-based packing columns is confirmed to be ion-exchange interaction. Under the LCCC of PEG backbone, with fine tune of buffer concentration, the retention factor ratios for benzylamine and phenol in buffered mobile phases, α(benzylamine/phenol)-values, were used to assess the ion-exchange capacity on silica-based reversed-phase packing columns. To the best of our knowledge, this is the first report on separation of amino-functional PEGs independent of the molar mass by isocratic elution using common C18 or phenyl reversed-phase packing columns. Copyright © 2016 Elsevier B.V. All rights reserved.

Numerical simulation of dielectrophoretic separation of live/dead cells using a three-dimensional nonuniform AC electric field in micro-fabricated devices.

PubMed

Tada, Shigeru

2015-01-01

The analysis of cell separation has many important biological and medical applications. Dielectrophoresis (DEP) is one of the most effective and widely used techniques for separating and identifying biological species. In the present study, a DEP flow channel, a device that exploits the differences in the dielectric properties of cells in cell separation, was numerically simulated and its cell-separation performance examined. The samples of cells used in the simulation were modeled as human leukocyte (B cell) live and dead cells. The cell-separation analysis was carried out for a flow channel equipped with a planar electrode on the channel's top face and a pair of interdigitated counter electrodes on the bottom. This yielded a three-dimensional (3D) nonuniform AC electric field in the entire space of the flow channel. To investigate the optimal separation conditions for mixtures of live and dead cells, the strength of the applied electric field was varied. With appropriately selected conditions, the device was predicted to be very effective at separating dead cells from live cells. The major advantage of the proposed method is that a large volume of sample can be processed rapidly because of a large spacing of the channel height.

Separation of furostanol saponins by supercritical fluid chromatography.

PubMed

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

2017-10-25

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

Modern bioanalysis of proteins by electrophoretic techniques.

PubMed

Krizkova, Sona; Ryvolova, Marketa; Masarik, Michal; Zitka, Ondrej; Adam, Vojtech; Hubalek, Jaromir; Eckschlager, Tomas; Kizek, Rene

2014-01-01

In 1957, protein rich in cysteine able to bind cadmium was isolated from horse kidney and named as metallothionein according to its structural properties. Further, this protein and metallothionein-like proteins have been found in tissues of other animal species, yeasts, fungi and plants. MT is as a potential cancer marker in the focus of interest, and its properties, functions, and behavior under various conditions are intensively studied. Our protocol describes separation of two major mammalian isoforms of MT (MT-1 and MT-2) using capillary electrophoresis (CE) coupled with UV detector. This protocol enables separation of MT isoforms and studying of their basic behavior as well as their quantification with detection limit in units of ng per μL. Sodium borate buffer (20 mM, pH 9.5) was optimized as a background electrolyte, and the separation was carried out in fused silica capillary with internal diameter of 75 μm and electric field intensity of 350 V/cm. Optimal detection wavelength was 254 nm.

Separation of sodium chloride from the evaporated residue of the reverse osmosis reject generated in the leather industry--optimization by response surface methodology.

PubMed

Boopathy, R; Sekaran, G

2014-08-01

Reverse osmosis (RO) concentrate is being evaporated by solar/thermal evaporators to meet zero liquid discharge standards. The resulted evaporated residue (ER) is contaminated with both organic and inorganic mixture of salts. The generation of ER is exceedingly huge in the leather industry, which is being collected and stored under the shelter to avoid groundwater contamination by the leachate. In the present investigation, a novel process for the separation of sodium chloride from ER was developed, to reduce the environmental impact on RO concentrate discharge. The sodium chloride was selectively separated by the reactive precipitation method using hydrogen chloride gas. The selected process variables were optimized for maximum yield ofNaCl from the ER (optimum conditions were pH, 8.0; temperature, 35 degrees C; concentration of ER, 600 g/L and HCl purging time, 3 min). The recovered NaCl purity was verified using a cyclic voltagramm.

Spent coffee-based activated carbon: specific surface features and their importance for H2S separation process.

PubMed

Kante, Karifala; Nieto-Delgado, Cesar; Rangel-Mendez, J Rene; Bandosz, Teresa J

2012-01-30

Activated carbons were prepared from spent ground coffee. Zinc chloride was used as an activation agent. The obtained materials were used as a media for separation of hydrogen sulfide from air at ambient conditions. The materials were characterized using adsorption of nitrogen, elemental analysis, SEM, FTIR, and thermal analysis. Surface features of the carbons depend on the amount of an activation agent used. Even though the residual inorganic matter takes part in the H(2)S retention via salt formation, the porous surface of carbons governs the separation process. The chemical activation method chosen resulted in formation of large volume of pores with sizes between 10 and 30Å, optimal for water and hydrogen sulfide adsorption. Even though the activation process can be optimized/changed, the presence of nitrogen in the precursor (caffeine) is a significant asset of that specific organic waste. Nitrogen functional groups play a catalytic role in hydrogen sulfide oxidation. Copyright © 2011 Elsevier B.V. All rights reserved.

Water-Gas-Shift Membrane Reactor for High-Pressure Hydrogen Production. A comprehensive project report (FY2010 - FY2012)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Klaehn, John; Peterson, Eric; Orme, Christopher

2013-01-01

Idaho National Laboratory (INL), GE Global Research (GEGR), and Western Research Institute (WRI) have successfully produced hydrogen-selective membranes for water-gas-shift (WGS) modules that enable high-pressure hydrogen product streams. Several high performance (HP) polymer membranes were investigated for their gas separation performance under simulated (mixed gas) and actual syngas conditions. To enable optimal module performance, membranes with high hydrogen (H 2) selectivity, permeance, and stability under WGS conditions are required. The team determined that the VTEC PI 80-051 and VTEC PI 1388 (polyimide from Richard Blaine International, Inc.) are prime candidates for the H 2 gas separations at operating temperatures (~200°C).more » VTEC PI 80-051 was thoroughly analyzed for its H 2 separations under syngas processing conditions using more-complex membrane configurations, such as tube modules and hollow fibers. These membrane formats have demonstrated that the selected VTEC membrane is capable of providing highly selective H 2/CO 2 separation (α = 7-9) and H 2/CO separation (α = 40-80) in humidified syngas streams. In addition, the VTEC polymer membranes are resilient within the syngas environment (WRI coal gasification) at 200°C for over 1000 hours. The information within this report conveys current developments of VTEC PI 80-051 as an effective H 2 gas separations membrane for high-temperature syngas streams.« less

Flow range enhancement by secondary flow effect in low solidity circular cascade diffusers

NASA Astrophysics Data System (ADS)

Sakaguchi, Daisaku; Tun, Min Thaw; Mizokoshi, Kanata; Kishikawa, Daiki

2014-08-01

High-pressure ratio and wide operating range are highly required for compressors and blowers. The technical issue of the design is achievement of suppression of flow separation at small flow rate without deteriorating the efficiency at design flow rate. A numerical simulation is very effective in design procedure, however, cost of the numerical simulation is generally high during the practical design process, and it is difficult to confirm the optimal design which is combined with many parameters. A multi-objective optimization technique is the idea that has been proposed for solving the problem in practical design process. In this study, a Low Solidity circular cascade Diffuser (LSD) in a centrifugal blower is successfully designed by means of multi-objective optimization technique. An optimization code with a meta-model assisted evolutionary algorithm is used with a commercial CFD code ANSYS-CFX. The optimization is aiming at improving the static pressure coefficient at design point and at low flow rate condition while constraining the slope of the lift coefficient curve. Moreover, a small tip clearance of the LSD blade was applied in order to activate and to stabilize the secondary flow effect at small flow rate condition. The optimized LSD blade has an extended operating range of 114 % towards smaller flow rate as compared to the baseline design without deteriorating the diffuser pressure recovery at design point. The diffuser pressure rise and operating flow range of the optimized LSD blade are experimentally verified by overall performance test. The detailed flow in the diffuser is also confirmed by means of a Particle Image Velocimeter. Secondary flow is clearly captured by PIV and it spreads to the whole area of LSD blade pitch. It is found that the optimized LSD blade shows good improvement of the blade loading in the whole operating range, while at small flow rate the flow separation on the LSD blade has been successfully suppressed by the secondary flow effect.

Effect of cultivating conditions on alpha-galactosidase production by a novel Aspergillus foetidus ZU-G1 strain in solid-state fermentation.

PubMed

Liu, Cai-qin; Chen, Qi-he; Cheng, Qian-jun; Wang, Jin-ling; He, Guo-qing

2007-05-01

The work is intended to achieve optimum culture conditions of alpha-galactosidase production by a mutant strain Aspergillus foetidus ZU-G1 in solid-state fermentation (SSF). Certain fermentation parameters involving moisture content, incubation temperature, cultivation period of seed, inoculum volume, initial pH value, layers of pledget, load size of medium and period of cultivation were investigated separately. The optimal cultivating conditions of alpha-galactosidase production in SSF were 60% initial moisture of medium, 28 degrees C incubation temperature, 18 h cultivation period of seed, 10% inoculum volume, 5.0 approximately 6.0 initial pH of medium, 6 layers of pledget and 10 g dry matter loadage. Under the optimized cultivation conditions, the maximum alpha-galactosidase production was 2 037.51 U/g dry matter near the 144th hour of fermentation.

Effect of cultivating conditions on α-galactosidase production by a novel Aspergillus foetidus ZU-G1 strain in solid-state fermentation

PubMed Central

Liu, Cai-qin; Chen, Qi-he; Cheng, Qian-jun; Wang, Jin-ling; He, Guo-qing

2007-01-01

The work is intended to achieve optimum culture conditions of α-galactosidase production by a mutant strain Aspergillus foetidus ZU-G1 in solid-state fermentation (SSF). Certain fermentation parameters involving moisture content, incubation temperature, cultivation period of seed, inoculum volume, initial pH value, layers of pledget, load size of medium and period of cultivation were investigated separately. The optimal cultivating conditions of α-galactosidase production in SSF were 60% initial moisture of medium, 28 °C incubation temperature, 18 h cultivation period of seed, 10% inoculum volume, 5.0~6.0 initial pH of medium, 6 layers of pledget and 10 g dry matter loadage. Under the optimized cultivation conditions, the maximum α-galactosidase production was 2 037.51 U/g dry matter near the 144th hour of fermentation. PMID:17542067

[Optimization for supercritical CO2 extraction with response surface methodology and component analysis of Sapindus mukorossi oil].

PubMed

Wu, Yan; Xiao, Xin-yu; Ge, Fa-huan

2012-02-01

To study the extraction conditions of Sapindus mukorossi oil by Supercritical CO2 Extraction and identify its components. Optimized SFE-CO2 Extraction by response surface methodology and used GC-MS to analysie Sapindus mukorossi oil compounds. Established the model of an equation for the extraction rate of Sapindus mukorossi oil by Supercritical CO2 Extraction, and the optimal parameters for the Supercritical CO2 Extraction determined by the equation were: the extraction pressure was 30 MPa, temperature was 40 degrees C; The separation I pressure was 14 MPa, temperature was 45 degrees C; The separation II pressure was 6 MPa, temperature was 40 degrees C; The extraction time was 60 min and the extraction rate of Sapindus mukorossi oil of 17.58%. 22 main compounds of Sapindus mukorossi oil extracted by supercritical CO2 were identified by GC-MS, unsaturated fatty acids were 86.59%. This process is reliable, safe and with simple operation, and can be used for the extraction of Sapindus mukorossi oil.

Optimizing management of the condensing heat and cooling of gases compression in oxy block using of a genetic algorithm

NASA Astrophysics Data System (ADS)

Brzęczek, Mateusz; Bartela, Łukasz

2013-12-01

This paper presents the parameters of the reference oxy combustion block operating with supercritical steam parameters, equipped with an air separation unit and a carbon dioxide capture and compression installation. The possibility to recover the heat in the analyzed power plant is discussed. The decision variables and the thermodynamic functions for the optimization algorithm were identified. The principles of operation of genetic algorithm and methodology of conducted calculations are presented. The sensitivity analysis was performed for the best solutions to determine the effects of the selected variables on the power and efficiency of the unit. Optimization of the heat recovery from the air separation unit, flue gas condition and CO2 capture and compression installation using genetic algorithm was designed to replace the low-pressure section of the regenerative water heaters of steam cycle in analyzed unit. The result was to increase the power and efficiency of the entire power plant.

Global optimization of multicomponent distillation configurations: 2. Enumeration based global minimization algorithm

DOE PAGES

Nallasivam, Ulaganathan; Shah, Vishesh H.; Shenvi, Anirudh A.; ...

2016-02-10

We present a general Global Minimization Algorithm (GMA) to identify basic or thermally coupled distillation configurations that require the least vapor duty under minimum reflux conditions for separating any ideal or near-ideal multicomponent mixture into a desired number of product streams. In this algorithm, global optimality is guaranteed by modeling the system using Underwood equations and reformulating the resulting constraints to bilinear inequalities. The speed of convergence to the globally optimal solution is increased by using appropriate feasibility and optimality based variable-range reduction techniques and by developing valid inequalities. As a result, the GMA can be coupled with already developedmore » techniques that enumerate basic and thermally coupled distillation configurations, to provide for the first time, a global optimization based rank-list of distillation configurations.« less

Optimized Production of Biodiesel from Waste Cooking Oil by Lipase Immobilized on Magnetic Nanoparticles

PubMed Central

Yu, Chi-Yang; Huang, Liang-Yu; Kuan, I-Ching; Lee, Shiow-Ling

2013-01-01

Biodiesel, a non-toxic and biodegradable fuel, has recently become a major source of renewable alternative fuels. Utilization of lipase as a biocatalyst to produce biodiesel has advantages over common alkaline catalysts such as mild reaction conditions, easy product separation, and use of waste cooking oil as raw material. In this study, Pseudomonas cepacia lipase immobilized onto magnetic nanoparticles (MNP) was used for biodiesel production from waste cooking oil. The optimal dosage of lipase-bound MNP was 40% (w/w of oil) and there was little difference between stepwise addition of methanol at 12 h- and 24 h-intervals. Reaction temperature, substrate molar ratio (methanol/oil), and water content (w/w of oil) were optimized using response surface methodology (RSM). The optimal reaction conditions were 44.2 °C, substrate molar ratio of 5.2, and water content of 12.5%. The predicted and experimental molar conversions of fatty acid methyl esters (FAME) were 80% and 79%, respectively. PMID:24336109

Sustainable Separations of C4‐Hydrocarbons by Using Microporous Materials

PubMed Central

Gehre, Mascha; Guo, Zhiyong; Rothenberg, Gadi

2017-01-01

Abstract Petrochemical refineries must separate hydrocarbon mixtures on a large scale for the production of fuels and chemicals. Typically, these hydrocarbons are separated by distillation, which is extremely energy intensive. This high energy cost can be mitigated by developing materials that can enable efficient adsorptive separation. In this critical review, the principles of adsorptive separation are outlined, and then the case for C4 separations by using zeolites and metal–organic frameworks (MOFs) is examined. By analyzing both experimental and theoretical studies, the challenges and opportunities in C4 separation are outlined, with a focus on the separation mechanisms and structure–selectivity correlations. Zeolites are commonly used as adsorbents and, in some cases, can separate C4 mixtures well. The pore sizes of eight‐membered‐ring zeolites, for example, are in the order of the kinetic diameters of C4 isomers. Although zeolites have the advantage of a rigid and highly stable structure, this is often difficult to functionalize. MOFs are attractive candidates for hydrocarbon separation because their pores can be tailored to optimize the adsorbate–adsorbent interactions. MOF‐5 and ZIF‐7 show promising results in separating all C4 isomers, but breakthrough experiments under industrial conditions are needed to confirm these results. Moreover, the flexibility of the MOF structures could hamper their application under industrial conditions. Adsorptive separation is a promising viable alternative and it is likely to play an increasingly important role in tomorrow's refineries. PMID:28621064

Sustainable Separations of C4 -Hydrocarbons by Using Microporous Materials.

PubMed

Gehre, Mascha; Guo, Zhiyong; Rothenberg, Gadi; Tanase, Stefania

2017-10-23

Petrochemical refineries must separate hydrocarbon mixtures on a large scale for the production of fuels and chemicals. Typically, these hydrocarbons are separated by distillation, which is extremely energy intensive. This high energy cost can be mitigated by developing materials that can enable efficient adsorptive separation. In this critical review, the principles of adsorptive separation are outlined, and then the case for C 4 separations by using zeolites and metal-organic frameworks (MOFs) is examined. By analyzing both experimental and theoretical studies, the challenges and opportunities in C 4 separation are outlined, with a focus on the separation mechanisms and structure-selectivity correlations. Zeolites are commonly used as adsorbents and, in some cases, can separate C 4 mixtures well. The pore sizes of eight-membered-ring zeolites, for example, are in the order of the kinetic diameters of C 4 isomers. Although zeolites have the advantage of a rigid and highly stable structure, this is often difficult to functionalize. MOFs are attractive candidates for hydrocarbon separation because their pores can be tailored to optimize the adsorbate-adsorbent interactions. MOF-5 and ZIF-7 show promising results in separating all C 4 isomers, but breakthrough experiments under industrial conditions are needed to confirm these results. Moreover, the flexibility of the MOF structures could hamper their application under industrial conditions. Adsorptive separation is a promising viable alternative and it is likely to play an increasingly important role in tomorrow's refineries. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Electrokinetic dispersion in microfluidic separation systems

NASA Astrophysics Data System (ADS)

Molho, Joshua Irving

Numerous efforts have focused on engineering miniaturized chemical analysis devices that are faster, more portable and consume smaller volumes of expensive reagents than their macroscale counterparts. Many of these analysis devices employ electrokinetic effects to transport picoliter volumes of liquids and to separate chemical species from an initially mixed sample volume. In these microfluidic separation systems, dispersion must be minimized to obtain the highest resolution separation possible. This work focuses on modeling, simulation and experimental measurement of two electrokinetic dispersion mechanisms that can reduce the effectiveness of microfluidic separation systems: dispersion resulting from non-uniform wall zeta-potential, and dispersion caused by microchannel turns. When the surface of a microchannel has non-uniform zeta-potential (e.g., if the surface charge varies along the length of the microchannel), an applied electric field creates both electroosmotic and pressure-driven flow. A caged-fluorescence imaging technique was used to visualize the dispersion caused by this electrokinetically induced pressure-driven flow. A simple model for a single channel with an axially varying surface charge is presented and compared to experimental measurements. Microchannel turns have been shown to create dispersion of electrokinetically transported analyte bands. Using a method of moments analysis, a model is developed that quantifies this dispersion and identifies the conditions under which turn dispersion limits the resolution of a microfluidic separation system. Measurements using the caged-fluorescence visualization technique were used to verify this model. New turn geometries are presented and were optimized using both a reduced parameter technique as well as a more generalized, numerical shape optimization approach. These improved turn designs were manufactured using two fabrication techniques and then tested experimentally. The turn optimization approaches and resulting turn geometries described here are shown to reduce turn dispersion to less than 1% of the dispersion caused by unoptimized, constant-width turns.

Effect of dilute alkaline pretreatment on the conversion of different parts of corn stalk to fermentable sugars and its application in acetone-butanol-ethanol fermentation.

PubMed

Cai, Di; Li, Ping; Luo, Zhangfeng; Qin, Peiyong; Chen, Changjing; Wang, Yong; Wang, Zheng; Tan, Tianwei

2016-07-01

To investigate the effect of dilute alkaline pretreatment on different parts of biomass, corn stalk was separated into flower, leaf, cob, husk and stem, which were treated by NaOH in range of temperature and chemical loading. The NaOH-pretreated solid was then enzymatic hydrolysis and used as the substrate for batch acetone-butanol-ethanol (ABE) fermentation. The results demonstrated the five parts of corn stalk could be used as potential feedstock separately, with vivid performances in solvents production. Under the optimized conditions towards high product titer, 7.5g/L, 7.6g/L, 9.4g/L, 7g/L and 7.6g/L of butanol was obtained in the fermentation broth of flower, leaf, cob, husk and stem hydrolysate, respectively. Under the optimized conditions towards high product yield, 143.7g/kg, 126.3g/kg, 169.1g/kg, 107.7g/kg and 116.4g/kg of ABE solvent were generated, respectively. Copyright © 2016 Elsevier Ltd. All rights reserved.

Gas-liquid flow splitting in T-junction with inclined lateral arm

NASA Astrophysics Data System (ADS)

Yang, Le-le; Liu, Shuo; Li, Hua; Zhang, Jian; Wu, Ying-xiang; Xu, Jing-yu

2018-02-01

This paper studies the gas-liquid flow splitting in T-junction with inclined lateral arm. The separation mechanism of the T-junction is related to the pressure distribution in the T-junction. It is shown that the separation efficiency strongly depends on the inclination angle, when the angle ranges from 0° to 30°, while not so strongly for angles in the range from 30° to 90° Increasing the number of connecting tubes is helpful for the gas-liquid separation, and under the present test conditions, with four connecting tubes, a good separation performance can be achieved. Accordingly, a multi-tube Y-junction separator with four connecting tubes is designed for the experimental investigation. A good agreement between the simulated and measured data shows that there is an optimal split ratio to achieve the best performance for the multi-tube Y-junction separator.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Xing; Ibrahim, Yehia M.; Chen, Tsung-Chi

We report the first evaluation of a platform coupling a high speed field asymmetric ion mobility spectrometry microchip (µFAIMS) with drift tube ion mobility and mass spectrometry (IMS-MS). The µFAIMS/IMS-MS platform was used to analyze biological samples and simultaneously acquire multidimensional information of detected features from the measured FAIMS compensation fields and IMS drift times, while also obtaining accurate ion masses. These separations thereby increase the overall separation power, resulting increased information content, and provide more complete characterization of more complex samples. The separation conditions were optimized for sensitivity and resolving power by the selection of gas compositions and pressuresmore » in the FAIMS and IMS separation stages. The resulting performance provided three dimensional separations, benefitting both broad complex mixture studies and targeted analyses by e.g. improving isomeric separations and allowing detection of species obscured by “chemical noise” and other interfering peaks.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nallasivam, Ulaganathan; Shah, Vishesh H.; Shenvi, Anirudh A.

We present a general Global Minimization Algorithm (GMA) to identify basic or thermally coupled distillation configurations that require the least vapor duty under minimum reflux conditions for separating any ideal or near-ideal multicomponent mixture into a desired number of product streams. In this algorithm, global optimality is guaranteed by modeling the system using Underwood equations and reformulating the resulting constraints to bilinear inequalities. The speed of convergence to the globally optimal solution is increased by using appropriate feasibility and optimality based variable-range reduction techniques and by developing valid inequalities. As a result, the GMA can be coupled with already developedmore » techniques that enumerate basic and thermally coupled distillation configurations, to provide for the first time, a global optimization based rank-list of distillation configurations.« less

Optimal design of tilt carrier frequency computer-generated holograms to measure aspherics.

PubMed

Peng, Jiantao; Chen, Zhe; Zhang, Xingxiang; Fu, Tianjiao; Ren, Jianyue

2015-08-20

Computer-generated holograms (CGHs) provide an approach to high-precision metrology of aspherics. A CGH is designed under the trade-off among size, mapping distortion, and line spacing. This paper describes an optimal design method based on the parametric model for tilt carrier frequency CGHs placed outside the interferometer focus points. Under the condition of retaining an admissible size and a tolerable mapping distortion, the optimal design method has two advantages: (1) separating the parasitic diffraction orders to improve the contrast of the interferograms and (2) achieving the largest line spacing to minimize sensitivity to fabrication errors. This optimal design method is applicable to common concave aspherical surfaces and illustrated with CGH design examples.

Use of an Annular Silicon Drift Detector (SDD) Versus a Conventional SDD Makes Phase Mapping a Practical Solution for Rare Earth Mineral Characterization.

PubMed

Teng, Chaoyi; Demers, Hendrix; Brodusch, Nicolas; Waters, Kristian; Gauvin, Raynald

2018-06-04

A number of techniques for the characterization of rare earth minerals (REM) have been developed and are widely applied in the mining industry. However, most of them are limited to a global analysis due to their low spatial resolution. In this work, phase map analyses were performed on REM with an annular silicon drift detector (aSDD) attached to a field emission scanning electron microscope. The optimal conditions for the aSDD were explored, and the high-resolution phase maps generated at a low accelerating voltage identify phases at the micron scale. In comparisons between an annular and a conventional SDD, the aSDD performed at optimized conditions, making the phase map a practical solution for choosing an appropriate grinding size, judging the efficiency of different separation processes, and optimizing a REM beneficiation flowsheet.

Simulation and optimization of pressure swing adsorption systmes using reduced-order modeling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Agarwal, A.; Biegler, L.; Zitney, S.

2009-01-01

Over the past three decades, pressure swing adsorption (PSA) processes have been widely used as energyefficient gas separation techniques, especially for high purity hydrogen purification from refinery gases. Models for PSA processes are multiple instances of partial differential equations (PDEs) in time and space with periodic boundary conditions that link the processing steps together. The solution of this coupled stiff PDE system is governed by steep fronts moving with time. As a result, the optimization of such systems represents a significant computational challenge to current differential algebraic equation (DAE) optimization techniques and nonlinear programming algorithms. Model reduction is one approachmore » to generate cost-efficient low-order models which can be used as surrogate models in the optimization problems. This study develops a reducedorder model (ROM) based on proper orthogonal decomposition (POD), which is a low-dimensional approximation to a dynamic PDE-based model. The proposed method leads to a DAE system of significantly lower order, thus replacing the one obtained from spatial discretization and making the optimization problem computationally efficient. The method has been applied to the dynamic coupled PDE-based model of a twobed four-step PSA process for separation of hydrogen from methane. Separate ROMs have been developed for each operating step with different POD modes for each of them. A significant reduction in the order of the number of states has been achieved. The reduced-order model has been successfully used to maximize hydrogen recovery by manipulating operating pressures, step times and feed and regeneration velocities, while meeting product purity and tight bounds on these parameters. Current results indicate the proposed ROM methodology as a promising surrogate modeling technique for cost-effective optimization purposes.« less

Perceptual attraction in tool use: evidence for a reliability-based weighting mechanism.

PubMed

Debats, Nienke B; Ernst, Marc O; Heuer, Herbert

2017-04-01

Humans are well able to operate tools whereby their hand movement is linked, via a kinematic transformation, to a spatially distant object moving in a separate plane of motion. An everyday example is controlling a cursor on a computer monitor. Despite these separate reference frames, the perceived positions of the hand and the object were found to be biased toward each other. We propose that this perceptual attraction is based on the principles by which the brain integrates redundant sensory information of single objects or events, known as optimal multisensory integration. That is, 1 ) sensory information about the hand and the tool are weighted according to their relative reliability (i.e., inverse variances), and 2 ) the unisensory reliabilities sum up in the integrated estimate. We assessed whether perceptual attraction is consistent with optimal multisensory integration model predictions. We used a cursor-control tool-use task in which we manipulated the relative reliability of the unisensory hand and cursor position estimates. The perceptual biases shifted according to these relative reliabilities, with an additional bias due to contextual factors that were present in experiment 1 but not in experiment 2 The biased position judgments' variances were, however, systematically larger than the predicted optimal variances. Our findings suggest that the perceptual attraction in tool use results from a reliability-based weighting mechanism similar to optimal multisensory integration, but that certain boundary conditions for optimality might not be satisfied. NEW & NOTEWORTHY Kinematic tool use is associated with a perceptual attraction between the spatially separated hand and the effective part of the tool. We provide a formal account for this phenomenon, thereby showing that the process behind it is similar to optimal integration of sensory information relating to single objects. Copyright © 2017 the American Physiological Society.

Silver and gold nanoparticle separation using asymmetrical flow-field flow fractionation: Influence of run conditions and of particle and membrane charges.

PubMed

Meisterjahn, Boris; Wagner, Stephan; von der Kammer, Frank; Hennecke, Dieter; Hofmann, Thilo

2016-04-01

Flow-Field Flow Fractionation (Flow-FFF), coupled with online detection systems is one of the most promising tools available for the separation and quantification of engineered nanoparticles (ENPs) in complex matrices. To correctly relate the retention of nanoparticles in the Flow-FFF-channel to the particle size, ideal separation conditions must be met. This requires optimization of the parameters that influence the separation behavior. The aim of this study was therefore to systematically investigate and evaluate the influence of parameters such as the carrier liquid, the cross flow, and the membrane material, on the separation behavior of two metallic ENPs. For this purpose the retention, recovery, and separation efficiency of sterically stabilized silver nanoparticles (AgNPs) and electrostatically stabilized gold nanoparticles (AuNPs), which represent two materials widely used in investigations on environmental fate and ecotoxicology, were investigated against a parameter matrix of three different cross-flow densities, four representative carrier solutions, and two membrane materials. The use of a complex mixture of buffers, ionic and non-ionic surfactants (FL-70 solution) together with a medium cross-flow density provided an acceptable compromise in peak quality and recovery for both types of ENPs. However, these separation conditions do not represent a perfect match for both particle types at the same time (maximized recovery at maximized retention). It could be shown that the behavior of particles within Flow-FFF channels cannot be predicted or explained purely in terms of electrostatic interactions. Particles were irreversibly lost under conditions where the measured zeta potentials suggested that there should have been sufficient electrostatic repulsion to ensure stabilization of the particles in the Flow-FFF channel resulting in good recoveries. The wide variations that we observed in ENP behavior under different conditions, together with the different behavior that has been reported in published literature for the same NPs under similar conditions, indicate a need for improvement in the membrane materials used for Flow-FFF analysis of NPs. This research has shown that careful adjustment of separation conditions can result in acceptable, but not ideal, separation conditions for two fundamentally different stabilized materials, and that it may not be possible to separate a set of different particles under ideal conditions for each particle type. This therefore needs to be taking into account in method development and when interpreting FFF results from complex samples. Copyright © 2016 Elsevier B.V. All rights reserved.

The chiral separation of triazole pesticides enantiomers by amylose-tris (3,5-dimethylphenylcarbamate) chiral stationary phase.

PubMed

Wang, Peng; Liu, Donghui; Jiang, Shuren; Xu, Yangguang; Zhou, Zhiqiang

2008-10-01

The amylose-tris(3,5-dimethylphenylcarbamate) chiral stationary phase was synthesized and used to separate the enantiomers of triazole pesticides by high-performance liquid chromatography. The mobile phase was n-hexane-isopropanol applying a flow rate of 1.0 mL/min. Six triazole pesticides were enantioselectively separated. Myclobutanil, paclobutrazol, tebuconazole, and uniconazole obtained complete separation with the resolution factors of 5.73, 2.99, 1.72, and 2.07, respectively, and imazalil and diniconazole obtained partial separation with the resolution factors of 0.79 and 0.77 under the optimized conditions. The effect of the content of isopropanol as well as column temperature on the separation was investigated. A circular dichroism detector was used to identify the enantiomers and determine the elution orders. The results showed the low temperature was good for the chiral separation except for diniconazole. The thermodynamic parameters calculated based on linear Van't Hoff plots showed the chiral separations were controlled by enthalpy.

Optimization of the method for assessment of brain perfusion in humans using contrast-enhanced reflectometry: multidistance time-resolved measurements

NASA Astrophysics Data System (ADS)

Milej, Daniel; Janusek, Dariusz; Gerega, Anna; Wojtkiewicz, Stanislaw; Sawosz, Piotr; Treszczanowicz, Joanna; Weigl, Wojciech; Liebert, Adam

2015-10-01

The aim of the study was to determine optimal measurement conditions for assessment of brain perfusion with the use of optical contrast agent and time-resolved diffuse reflectometry in the near-infrared wavelength range. The source-detector separation at which the distribution of time of flights (DTOF) of photons provided useful information on the inflow of the contrast agent to the intracerebral brain tissue compartments was determined. Series of Monte Carlo simulations was performed in which the inflow and washout of the dye in extra- and intracerebral tissue compartments was modeled and the DTOFs were obtained at different source-detector separations. Furthermore, tests on diffuse phantoms were carried out using a time-resolved setup allowing the measurement of DTOFs at 16 source-detector separations. Finally, the setup was applied in experiments carried out on the heads of adult volunteers during intravenous injection of indocyanine green. Analysis of statistical moments of the measured DTOFs showed that the source-detector separation of 6 cm is recommended for monitoring of inflow of optical contrast to the intracerebral brain tissue compartments with the use of continuous wave reflectometry, whereas the separation of 4 cm is enough when the higher-order moments of DTOFs are available.

On combining multi-normalization and ancillary measures for the optimal score level fusion of fingerprint and voice biometrics

NASA Astrophysics Data System (ADS)

Mohammed Anzar, Sharafudeen Thaha; Sathidevi, Puthumangalathu Savithri

2014-12-01

In this paper, we have considered the utility of multi-normalization and ancillary measures, for the optimal score level fusion of fingerprint and voice biometrics. An efficient matching score preprocessing technique based on multi-normalization is employed for improving the performance of the multimodal system, under various noise conditions. Ancillary measures derived from the feature space and the score space are used in addition to the matching score vectors, for weighing the modalities, based on their relative degradation. Reliability (dispersion) and the separability (inter-/intra-class distance and d-prime statistics) measures under various noise conditions are estimated from the individual modalities, during the training/validation stage. The `best integration weights' are then computed by algebraically combining these measures using the weighted sum rule. The computed integration weights are then optimized against the recognition accuracy using techniques such as grid search, genetic algorithm and particle swarm optimization. The experimental results show that, the proposed biometric solution leads to considerable improvement in the recognition performance even under low signal-to-noise ratio (SNR) conditions and reduces the false acceptance rate (FAR) and false rejection rate (FRR), making the system useful for security as well as forensic applications.

Separation of the stereoisomers of the main metabolite of a non-steroidal anti-inflammatory drug, flobufen, by chiral high-performance liquid chromatography.

PubMed

Wsól, V; Fell, A F; Kvasnicková, E; Hais, I M

1997-02-07

The major metabolite of a novel non-steroidal anti-inflammatory drug, DL-4-(2',4'-difluorobiphenyl-4-yl)-2-oxo-2-methylbutanoic acid (flobufen, I), namely 4-(2',4'-difluorobiphenyl-4-yl)-2-methyl-gamma-butyrolactone (4-dihydroflobufen lactone, III), has four stereoisomers consisting of two racemic pairs of enantiomers. Of three chiral stationary phases tested, Cyclobond I beta-RSP (Astec) (beta-cylodextrin derivatized with R,S-hydroxypropyl) was best able to separate the (+2)(--) racemate, with a liquid phase containing acetonitrile as modifier and triethylamine acetate as buffer. Using the Box-Wilson Central Composite Design for three factors, an optimum combination of pH and concentrations of the modifier and buffer was eventually obtained. A chromatographic response function based on a combination of the Kaiser peak separation function, Pi, and retention time of the second eluting enantiomer, tRL, served as a response criterion for the process of optimization. The optimum conditions developed for the (+2)(--) racemate were also found to be suitable for separating the (+-)(-+) racemate, for which earlier studies had shown the separation to be more facile. Separation of the four stereoisomers of III, for which the chiral chromatographic system optimized in this study is proposed as the second stage, is targeted at a biochemical study of the stereoisomeric metabolism of I.

Dependence of optimal separative power of the “high-speed” Iguasu centrifuge on pressure of working gas

NASA Astrophysics Data System (ADS)

Bogovalov, S. V.; Borman, V. D.; Borisevich, V. D.; Davidenko, O. V.; Tronin, I. V.; Tronin, V. N.

2016-09-01

The results of optimization calculations of the separative power of the ’’high-speed” Iguasu gas centrifuge are presented. Iguasu gas centrifuge has the rotational speed of 1000 m/s, the rotor length of 1 m. The dependence of the optimal separative power on the pressure of the working gas on the rotor wall was obtained using the numerical simulations. It is shown, that maximum of the optimal separative power corresponds to the pressure of 1100 mmHg. Maximum value of separative power is 31.9 SWU.

Analysis of antimycin A by reversed-phase liquid chromatography/nuclear magnetic-resonance spectrometry

USGS Publications Warehouse

Ha, Steven T.K.; Wilkins, Charles L.; Abidi, Sharon L.

1989-01-01

A mixture of closely related streptomyces fermentation products, antimycin A, Is separated, and the components are identified by using reversed-phase high-performance liquid chromatography with directly linked 400-MHz proton nuclear magnetic resonance detection. Analyses of mixtures of three amino acids, alanine, glycine, and valine, are used to determine optimal measurement conditions. Sensitivity increases of as much as a factor of 3 are achieved, at the expense of some loss in chromatographic resolution, by use of an 80-μL NMR cell, Instead of a smaller 14-μL cell. Analysis of the antimycin A mixture, using the optimal analytical high performance liquid chromatography/nuclear magnetic resonance conditions, reveals it to consist of at least 10 closely related components.

Optimization of the Supercritical Carbon Dioxide Separation of Bergapten from Bergamot Essential Oil.

PubMed

Sicari, Vincenzo

2018-01-01

The possibility of following traditional cold-press extraction with the post process continuous separation of bergapten from bergamot essential oil was investigated. A fractionation tower was used in an experiment in which cold-pressed bergamot oil was extracted in a continuous countercurrent process by supercritical carbon dioxide under different conditions. Bergapten is fairly soluble in CO2 in its supercritical phase, in particular at a density of 277.90 kg⋅m-3, corresponding to a pressure of 8 MPa and temperature of 40°C. Under these conditions, an extract with 0.198% bergapten was obtained, a figure slightly below the percentage of bergapten contained in cold-pressed oil (0.21%). However, at densities below 200 kg⋅m-3, the amount of bergapten in the extracted oil was negligible. Of all tested conditions for separation, the best was found to be at a pressure of 8 MPa and temperature of 70°C, conditions under which bergapten was not detected. The results of the experiment showed that bergapten, and the non-volatile fraction in general, was extracted only in small quantities and was not extracted at all with at a CO2 pressure of 8 MPa.

Optimal production of L-threo-2,3-dihydroxyphenylserine (L-threo-DOPS) on a large scale by diastereoselectivity-enhanced variant of L-threonine aldolase expressed in Escherichia coli.

PubMed

Gwon, Hui-Jeong; Yoshioka, Hideki; Song, Nho-Eul; Kim, Jong-Hui; Song, Young-Ran; Jeong, Do-Youn; Baik, Sang-Ho

2012-01-01

This study examined the efficient production and optimal separation procedures for pure L-threo-3,4-dihydroxyphenylserine (L-threo-DOPS) from a mixture of diastereomers synthesized by whole-cell aldol condensation reaction, harboring diastereoselectivity-enhanced L-threonine aldolase in Escherichia coli JM109. The addition of the reducing agent sodium sulfite was found to stimulate the production of L-threo-DOPS without affecting the diastereoselectivity ratio, especially at the 50 mM concentration. The optimal pH for diastereoselective synthesis was 6.5. The addition of Triton X-100 also strongly affected the synthesis yield, showing the highest conversion yield at a 0.75% concentration; however, the diastereoselectivity of the L-threonine aldolase was not affected. Lowering the temperature to 10°C did not significantly affect the diastereoselectiviy without affecting the synthesis rate. At the optimized conditions, a mixture of L-threo-DOPS and L-erythro-DOPS was synthesized by diastereoselectivity-enhanced L-threonine aldolase from E. coli in a continuous process for 100 hr, yielding an average of 4.0 mg/mL of L-threo-DOPS and 60% diastereoselectivity (de), and was subjected to two steps of ion exchange chromatography. The optimum separation conditions for the resin and solvent were evaluated in which it was found that a two-step process with the ion-exchange resin Dowex 50 W × 8 and activated carbon by washing with 0.5 N acetic acid was sufficient to separate the L-threo-DOPS. By using two-step ion-exchange chromatography, synthesized high-purity L-threo-DOPS of up to 100% was purified with a yield of 71%. The remaining substrates, glycine and 3,4-dihydroxybenzaldehyde, were recovered successfully with a yield of 71.2%. Our results indicate this potential procedure as an economical purification process for the synthesis and purification of important L-threo-DOPS at the pharmaceutical level.

Reduced-order model for dynamic optimization of pressure swing adsorption processes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Agarwal, A.; Biegler, L.; Zitney, S.

2007-01-01

Over the past decades, pressure swing adsorption (PSA) processes have been widely used as energy-efficient gas and liquid separation techniques, especially for high purity hydrogen purification from refinery gases. The separation processes are based on solid-gas equilibrium and operate under periodic transient conditions. Models for PSA processes are therefore multiple instances of partial differential equations (PDEs) in time and space with periodic boundary conditions that link the processing steps together. The solution of this coupled stiff PDE system is governed by steep concentrations and temperature fronts moving with time. As a result, the optimization of such systems for either designmore » or operation represents a significant computational challenge to current differential algebraic equation (DAE) optimization techniques and nonlinear programming algorithms. Model reduction is one approach to generate cost-efficient low-order models which can be used as surrogate models in the optimization problems. The study develops a reduced-order model (ROM) based on proper orthogonal decomposition (POD), which is a low-dimensional approximation to a dynamic PDE-based model. Initially, a representative ensemble of solutions of the dynamic PDE system is constructed by solving a higher-order discretization of the model using the method of lines, a two-stage approach that discretizes the PDEs in space and then integrates the resulting DAEs over time. Next, the ROM method applies the Karhunen-Loeve expansion to derive a small set of empirical eigenfunctions (POD modes) which are used as basis functions within a Galerkin's projection framework to derive a low-order DAE system that accurately describes the dominant dynamics of the PDE system. The proposed method leads to a DAE system of significantly lower order, thus replacing the one obtained from spatial discretization before and making optimization problem computationally-efficient. The method has been applied to the dynamic coupled PDE-based model of a two-bed four-step PSA process for separation of hydrogen from methane. Separate ROMs have been developed for each operating step with different POD modes for each of them. A significant reduction in the order of the number of states has been achieved. The gas-phase mole fraction, solid-state loading and temperature profiles from the low-order ROM and from the high-order simulations have been compared. Moreover, the profiles for a different set of inputs and parameter values fed to the same ROM were compared with the accurate profiles from the high-order simulations. Current results indicate the proposed ROM methodology as a promising surrogate modeling technique for cost-effective optimization purposes. Moreover, deviations from the ROM for different set of inputs and parameters suggest that a recalibration of the model is required for the optimization studies. Results for these will also be presented with the aforementioned results.« less

Imaging cell picker: A morphology-based automated cell separation system on a photodegradable hydrogel culture platform.

PubMed

Shibuta, Mayu; Tamura, Masato; Kanie, Kei; Yanagisawa, Masumi; Matsui, Hirofumi; Satoh, Taku; Takagi, Toshiyuki; Kanamori, Toshiyuki; Sugiura, Shinji; Kato, Ryuji

2018-06-09

Cellular morphology on and in a scaffold composed of extracellular matrix generally represents the cellular phenotype. Therefore, morphology-based cell separation should be interesting method that is applicable to cell separation without staining surface markers in contrast to conventional cell separation methods (e.g., fluorescence activated cell sorting and magnetic activated cell sorting). In our previous study, we have proposed a cloning technology using a photodegradable gelatin hydrogel to separate the individual cells on and in hydrogels. To further expand the applicability of this photodegradable hydrogel culture platform, we here report an image-based cell separation system imaging cell picker for the morphology-based cell separation on a photodegradable hydrogel. We have developed the platform which enables the automated workflow of image acquisition, image processing and morphology analysis, and collection of a target cells. We have shown the performance of the morphology-based cell separation through the optimization of the critical parameters that determine the system's performance, such as (i) culture conditions, (ii) imaging conditions, and (iii) the image analysis scheme, to actually clone the cells of interest. Furthermore, we demonstrated the morphology-based cloning performance of cancer cells in the mixture of cells by automated hydrogel degradation by light irradiation and pipetting. Copyright © 2018 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

Optimization and validation of the reversed-phase high-performance liquid chromatography with fluorescence detection method for the separation of tocopherol and tocotrienol isomers in cereals, employing a novel sorbent material.

PubMed

Irakli, Maria N; Samanidou, Victoria F; Papadoyannis, Ioannis N

2012-03-07

The separation and determination of tocopherols (Ts) and tocotrienols (T3s) by reversed-phase high-performance liquid chromatography with fluorescence detection has been developed and validated after optimization of various chromatographic conditions and other experimental parameters. Analytes were separated on a PerfectSil Target ODS-3 (250 × 4.6 mm, 3 μm) column filled with a novel sorbent material of ultrapure silica gel. The separation of Ts and T3s was optimized in terms of mobile-phase composition and column temperature on the basis of the best compromise among efficiency, resolution, and analysis time. Using a gradient elution of mobile phase composed of isopropanol/water and 7 °C column temperature, a satisfactory resolution was achieved within 62 min. For the quantitative determination, α-T acetate (50 μg/mL) was used as the internal standard. Detection limits ranged from 0.27 μg/mL (γ-T) to 0.76 μg/mL (γ-T3). The validation of the method was examined performing intraday (n = 5) and interday (n = 3) assays and was found to be satisfactory, with high accuracy and precision results. Solid-phase extraction provided high relative extraction recoveries from cereal samples: 87.0% for γ-T3 and 115.5% for δ-T. The method was successfully applied to cereals, such as durum wheat, bread wheat, rice, barley, oat, rye, and corn.

Enantioseparation of racemic aminoglutethimide using asynchronous simulated moving bed chromatography.

PubMed

Lin, Xiaojian; Gong, Rujin; Li, Jiaxu; Li, Ping; Yu, Jianguo; Rodrigues, Alirio E

2016-10-07

The separation of aminoglutethimide enantiomers by the continuous multicolumn chromatographic processes were investigated experimentally and theoretically, where the columns were packed with cellulose tris 3,5-dimethylphenyl-carbamate stationary phase (brand name Chiralcel OD) and mobile phase was a mixture of n-hexane and ethanol with monoethanolamine additive. The continuous enantioseparation processes included a synchronous shifting process (SMB) and an asynchronous shifting process (VARICOL), which allowed reducing the column number (here from six-column SMB to five-column VARICOL process). Transport-dispersive model with the consideration of both intraparticle mass transfer resistance and axial dispersion was adopted to design and optimize the operation conditions for the separation of aminoglutethimide enantiomers by SMB process and VARICOL process. According to the optimized operation conditions, experiments were carried out on VARICOL-Micro unit using five-column VARICOL process with 1/1.5/1.5/1 configuration and six-column SMB process with 1/2/2/1 configuration. Products of R-aminoglutethimide (R-AG) enantiomer and S-aminoglutethimide (S-AG) enantiomer with more than 99.0% purity were obtained continuously from extract stream and raffinate stream, respectively. Furthermore, the experiemntal data obtained from five-column VARICOL process were compared with that from six-column SMB process, the feasibility and efficiency for the separation of guaifenesin enantiomers by VARICOL processes were evaluated. Copyright © 2016 Elsevier B.V. All rights reserved.

Sheath-flow electrochemical detection of amino acids with a copper wire electrode in capillary electrophoresis.

PubMed

Inoue, Junji; Kaneta, Takashi; Imasaka, Totaro

2012-09-01

Here, we report the detection of native amino acids using a sheath-flow electrochemical detector with a working electrode made of copper wire. A separation capillary that was inserted into a platinum tube in the detector acted as a grounded electrode for electrophoresis and as a flow channel for sheath liquid. Sheath liquid flowed outside the capillary to support the transport of the separated analytes to the working electrode for electrochemical detection. The copper wire electrode was aligned at the outlet of the capillary in a wall-jet configuration. Amino acids injected into the capillary were separated following elution from the end of the capillary and detection by the copper electrode. Three kinds of copper electrodes with different diameters-50, 125, and 300 μm-were examined to investigate the effect of the electrode diameter on sensitivity. The peak widths of the analytes were independent of the diameter of the working electrode, while the 300-μm electrode led to a decrease in the signal-to-noise ratio compared with the 50- and 125-μm electrodes, which showed no significant difference. The flow rate of the sheath liquid was also varied to optimize the detection conditions. The limits of detection for amino acids ranged from 4.4 to 27 μM under optimal conditions. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Two-dimensional RPLC-RPLC system with different pH in two dimensions for separation of alkaloids from Corydalis yanhusuo W. T. Wang.

PubMed

Zhang, Jing; Jin, Yu; Liu, Yanfang; Xiao, Yuansheng; Feng, Jiatao; Xue, Xingya; Zhang, Xiuli; Liang, Xinmiao

2009-06-01

An effective method utilizing the same RP chromatographic column with different pH in first and second LC dimensions has been developed for separation of the basic compounds from traditional Chinese medicines (TCMs). In this work, the alkaloids in Corydalis yanhusuo which is an important TCM were selected as a model to develop the method. The additives and pH values of the mobile phase were optimized in this work. To investigate the feasibility of this method, off-line mode separation was performed in the experiments. According to the UV-absorption intensity, there were eight fractions collected in acidic conditions. All the fractions were analyzed in basic conditions. The results showed that the chromatographic selectivities were significantly different in the separations performed with acidic and alkaline elution systems. Complementary separation was achieved in this work. It is demonstrated that this method would be an effective tool for alkaloids research. Based on the different pH of the mobile phase in this method, it could also be suitable to analyze compounds which were sensible to the pH of the solution.

Recycling of waste automotive laminated glass and valorization of polyvinyl butyral through mechanochemical separation.

PubMed

Swain, Basudev; Ryang Park, Jae; Yoon Shin, Dong; Park, Kyung-Soo; Hwan Hong, Myung; Gi Lee, Chan

2015-10-01

Due to strong binding, optical clarity, adhesion to many surfaces, toughness and flexibility polyvinyl butyral (PVB) resin films are commonly used in the automotive and architectural application as a protective interlayer in the laminated glass. Worldwide million tons of PVB waste generated from end-of-life automotive associated with various environmental issues. Stringent environmental directive, higher land cost eliminates land filling option, needs a study, we have developed a mechanochemical separation process to separate PVB resins from glass and characterized the separated PVB through various techniques, i.e., scanning electron microscope (SEM), energy-dispersive X-ray spectroscopy (EDS), infrared spectroscopy (IR) and nuclear magnetic resonance spectroscopy (NMR). Commercial nonionic surfactants D201 used for the mechanochemical separation purpose. Through parameter optimization following conditions are considered to be the optimum condition; 30v ol% D201, stirring speed of 400 rpm, 35 °C temperature, operation time 1h, and dilute D201 volume to waste automotive laminated glass weight ratio of ≈25. The technology developed in our laboratory is sustainable, environmentally friendly, techno-economical feasible process, capable of mass production (recycling). Copyright © 2015 Elsevier Inc. All rights reserved.

Separation and determination of minor photosynthetic pigments by reversed-phase HPLC with minimal alteration of chlorophylls.

PubMed

Nakamura, A; Watanabe, T

2001-04-01

Reversed-phase HPLC conditions for separation of chlorophyll (Chl) a, Chl a' (the C132-epimer of Chl a), pheophytin (Pheo) a (the primary electron acceptor of photosystem (PS) II), and phylloquinone (PhQ) (the secondary electron acceptor of PS 1), have been developed. Pigment extraction conditions were optimized in terms of pigment alteration and extraction efficiency. Pigment composition analysis of light-harvesting complex II, which would not contain Chl a' nor Pheo a, showed the Chl a'/Chl a ratio of 3-4 x 10(-4) and the Pheo a/Chl a ratio of 4-5 x 10(-4), showing that the conditions developed here were sufficiently inert for Chl analysis. Preliminary analysis of thylakoid membranes with this analytical system gave the PhQ/Chl a' ratio of 0.58 +/- 0.03 (n = 4), in line with the stoichiometry of one molecule of Chl a' per PS I.

Development and numerical analysis of low specific speed mixed-flow pump

NASA Astrophysics Data System (ADS)

Li, H. F.; Huo, Y. W.; Pan, Z. B.; Zhou, W. C.; He, M. H.

2012-11-01

With the development of the city, the market of the mixed flow pump with large flux and high head is prospect. The KSB Shanghai Pump Co., LTD decided to develop low speed specific speed mixed flow pump to meet the market requirements. Based on the centrifugal pump and axial flow pump model, aiming at the characteristics of large flux and high head, a new type of guide vane mixed flow pump was designed. The computational fluid dynamics method was adopted to analyze the internal flow of the new type model and predict its performances. The time-averaged Navier-Stokes equations were closed by SST k-ω turbulent model to adapt internal flow of guide vane with larger curvatures. The multi-reference frame(MRF) method was used to deal with the coupling of rotating impeller and static guide vane, and the SIMPLEC method was adopted to achieve the coupling solution of velocity and pressure. The computational results shows that there is great flow impact on the head of vanes at different working conditions, and there is great flow separation at the tailing of the guide vanes at different working conditions, and all will affect the performance of pump. Based on the computational results, optimizations were carried out to decrease the impact on the head of vanes and flow separation at the tailing of the guide vanes. The optimized model was simulated and its performance was predicted. The computational results show that the impact on the head of vanes and the separation at the tailing of the guide vanes disappeared. The high efficiency of the optimized pump is wide, and it fit the original design destination. The newly designed mixed flow pump is now in modeling and its experimental performance will be getting soon.

Multi-objective optimization strategy based on desirability functions used for electrophoratic separation and quantification of rosiglitazone and glimepiride in plasma and formulations.

PubMed

Hefnawy, Mohamed M; Sultan, Maha A; Al-Johar, Haya I; Kassem, Mohamed G; Aboul-Enein, Hassan Y

2012-01-01

Multiple response simultaneous optimization employing Derringer's desirability function was used for the development of a capillary electrophoresis method for the simultaneous determination of rosiglitazone (RSG) and glimepiride (GLM) in plasma and formulations. Twenty experiments, taking the two resolutions, the analysis time, and the capillary current as the responses with three important factors--buffer morality, volte and column temperature--were used to design mathematical models. The experimental responses were fitted into a second order polynomial and the six responses were simultaneously optimized to predict the optimum conditions for the effective separation of the studied compounds. The separation was carried out by using capillary zone electrophoresis (CZE) with a silica capillary column and diode array detector at 210 nm. The optimum assay conditions were 52 mmol l⁻¹ phosphate buffer, pH 7, and voltage of 22 kV at 29 °C. The method showed good agreement between the experimental data and predictive value throughout the studied parameter space. The assay limit of detection was 0.02 µg ml⁻¹ and the effective working range at relative standard deviation (RSD) of ≤ 5% was 0.05-16 µg ml⁻¹ (r = 0.999) for both drugs. Analytical recoveries of the studied drugs from spiked plasma were 97.2-101.9 ± 0.31-3.0%. The precision of the assay was satisfactory; RSD was 1.07 and 1.14 for intra- and inter-assay precision, respectively. The proposed method has a great value in routine analysis of RSG and GLM for its therapeutic monitoring and pharmacokinetic studies. Copyright © 2011 John Wiley & Sons, Ltd.

Selective Detection of Peptide-Oligonucleotide Heteroconjugates Utilizing Capillary HPLC-ICPMS

NASA Astrophysics Data System (ADS)

Catron, Brittany; Caruso, Joseph A.; Limbach, Patrick A.

2012-06-01

A method for the selective detection and quantification of peptide:oligonucleotide heteroconjugates, such as those generated by protein:nucleic acid cross-links, using capillary reversed-phase high performance liquid chromatography (cap-RPHPLC) coupled with inductively coupled plasma mass spectrometry detection (ICPMS) is described. The selective detection of phosphorus as 31P+, the only natural isotope, in peptide-oligonucleotide heteroconjugates is enabled by the elemental detection capabilities of the ICPMS. Mobile phase conditions that allow separation of heteroconjugates while maintaining ICPMS compatibility were investigated. We found that trifluoroacetic acid (TFA) mobile phases, used in conventional peptide separations, and hexafluoroisopropanol/triethylamine (HFIP/TEA) mobile phases, used in conventional oligonucleotide separations, both are compatible with ICPMS and enable heteroconjugate separation. The TFA-based separations yielded limits of detection (LOD) of ~40 ppb phosphorus, which is nearly seven times lower than the LOD for HFIP/TEA-based separations. Using the TFA mobile phase, 1-2 pmol of a model heteroconjugate were routinely separated and detected by this optimized capLC-ICPMS method.

Electron beam induced strong organic/inorganic grafting for thermally stable lithium-ion battery separators

NASA Astrophysics Data System (ADS)

Choi, Yunah; Kim, Jin Il; Moon, Jungjin; Jeong, Jongyeob; Park, Jong Hyeok

2018-06-01

A tailored interface between organic and inorganic materials is of great importance to maximize the synergistic effects from hybridization. Polyethylene separators over-coated with inorganic thin films are the state-of-the art technology for preparing various secondary batteries with high safety. Unfortunately, the organic/inorganic hybrid separators have the drawback of a non-ideal interface, thus causing poor thermal/dimensional stability. Here, we report a straightforward method to resolve the drawback of the non-ideal interface between vapor deposited SiO2 and polyethylene separators, to produce a highly stable lithium-ion battery separator through strong chemical linking generated by direct electron beam irradiation. The simple treatment with an electron beam with an optimized dose generates thermally stable polymer separators, which may enhance battery safety under high-temperature conditions. Additionally, the newly formed Si-O-C or Si-CH3 chemical bonding enhances electrolyte-separator compatibility and thus may provide a better environment for ionic transport between the cathode and anode, thereby leading to better charge/discharge behaviors.

A comparative study on stress and compliance based structural topology optimization

NASA Astrophysics Data System (ADS)

Hailu Shimels, G.; Dereje Engida, W.; Fakhruldin Mohd, H.

2017-10-01

Most of structural topology optimization problems have been formulated and solved to either minimize compliance or weight of a structure under volume or stress constraints, respectively. Even if, a lot of researches are conducted on these two formulation techniques separately, there is no clear comparative study between the two approaches. This paper intends to compare these formulation techniques, so that an end user or designer can choose the best one based on the problems they have. Benchmark problems under the same boundary and loading conditions are defined, solved and results are compared based on these formulations. Simulation results shows that the two formulation techniques are dependent on the type of loading and boundary conditions defined. Maximum stress induced in the design domain is higher when the design domains are formulated using compliance based formulations. Optimal layouts from compliance minimization formulation has complex layout than stress based ones which may lead the manufacturing of the optimal layouts to be challenging. Optimal layouts from compliance based formulations are dependent on the material to be distributed. On the other hand, optimal layouts from stress based formulation are dependent on the type of material used to define the design domain. High computational time for stress based topology optimization is still a challenge because of the definition of stress constraints at element level. Results also shows that adjustment of convergence criterions can be an alternative solution to minimize the maximum stress developed in optimal layouts. Therefore, a designer or end user should choose a method of formulation based on the design domain defined and boundary conditions considered.

[Ion chromatography of L-ascorbic acid, sulfite and thiosulfate using their postcolumn reactions with cerium (IV) and fluorescence detection of cerium (III)].

PubMed

Chen, Q; Hu, K; Miura, Y

1999-09-01

An ion chromatographic method was used to separate the species of L-ascorbic acid, sulfite and thiosulfate in their mixtures. This method is based on the separation of each anion in their mixtures by using a separation column, and then on the fluorimetric measurement of cerium (III) formed by a postcolumn reaction of cerium (IV) with the species of L-ascorbic acid, sulfite and thiosulfate in the effluent. The optimal conditions for separating and determining the above three species have been established. By using a 3 mmol/L carbonate eluent, the species of L-ascorbic acid, sulfite and thiosulfate could be eluted at the proper retention times of 1.7, 2.6 and 5.0 min, respectively, and these three anions could be separated completely. The effects of the concentrations of cerium (IV) and sulfuric acid in the postcolumn reaction solution on the chromatographic peak-height were tested in order to obtain the optimal peak-height. It was found that the peak-height at first increases rapidly with an increase in the concentration of cerium (IV) and sulfuric acid respectively up to a certain concertation, then increases slowly. These critical concentrations of cerium (IV) and sulfuric acid also depend on the amount of the analyte injected. Meanwhile the baseline signals of the sepectra increase with an increase in the concentration of cerium (IV). Some concentrations above the critical concentration of sulfuric acid could be selected as the optimal concentration of sulfuric acid, but the concentration of cerium (IV) should be optimized by establishing a compromise between the higher peak-height and the lower baseline signal. The detection limit of this method was found to be 1 mumol/L for thiosulfate when an amount of 100 microL analyte was injected.

Genotyping of alpha-thalassemia deletions using multiplex polymerase chain reactions and gold nanoparticle-filled capillary electrophoresis.

PubMed

Chen, Yen-Ling; Shih, Chi-Jen; Ferrance, Jerome; Chang, Ya-Sian; Chang, Jan-Gowth; Wu, Shou-Mei

2009-02-13

A gold nanoparticle-filled capillary electrophoresis method combined with three multiplex polymerase chain reactions (PCRs) was established for simultaneous diagnosis of five common alpha-thalassemia deletions, including the -alpha(3.7) deletion, -alpha(4.2) deletion, Southeast Asian (--(SEA)), Filipino (--(FIL)) and Thai (--(THAI)) deletions. Gold nanoparticles (GNPs) were used as a pseudostationary phase to improve the resolution between DNA fragments in a low-viscosity polymer. To achieve the best CE separation, several parameters were evaluated for optimizing the separation conditions, including the capillary coating, the concentrations of polymer sieving matrix, the sizes and concentrations of GNPs, the buffer concentrations, and the pH. The final CE method for separating a 200-base pair (bp) DNA ladder and alpha-thalassemia deletions used a DB-17 capillary, 0.6% poly(ethylene oxide) (PEO) prepared in a mixture of GNP(32nm) solution and glycine buffer (25mM, pH 9.0) (80:20, v/v) as the sieving matrix with 1microM YO-PRO-1 for fluorescence detection; the applied voltage was -10kV (detector at anode side) and the separation temperature was 25 degrees C. Under these optimal conditions, 15 DNA fragments with sizes ranging from 0.2kb to 3.0kb were resolved within 11.5min. The RSDs of migration times were less than 2.81%. A total of 21 patients with alpha-thalassemia deletions were analyzed using this method, and all results showed good agreement with those obtained by gel electrophoresis.

Determination of thermodynamic values of acidic dissociation constants and complexation constants of profens and their utilization for optimization of separation conditions by Simul 5 Complex.

PubMed

Riesová, Martina; Svobodová, Jana; Ušelová, Kateřina; Tošner, Zdeněk; Zusková, Iva; Gaš, Bohuslav

2014-10-17

In this paper we determine acid dissociation constants, limiting ionic mobilities, complexation constants with β-cyclodextrin or heptakis(2,3,6-tri-O-methyl)-β-cyclodextrin, and mobilities of resulting complexes of profens, using capillary zone electrophoresis and affinity capillary electrophoresis. Complexation parameters are determined for both neutral and fully charged forms of profens and further corrected for actual ionic strength and variable viscosity in order to obtain thermodynamic values of complexation constants. The accuracy of obtained complexation parameters is verified by multidimensional nonlinear regression of affinity capillary electrophoretic data, which provides the acid dissociation and complexation parameters within one set of measurements, and by NMR technique. A good agreement among all discussed methods was obtained. Determined complexation parameters were used as input parameters for simulations of electrophoretic separation of profens by Simul 5 Complex. An excellent agreement of experimental and simulated results was achieved in terms of positions, shapes, and amplitudes of analyte peaks, confirming the applicability of Simul 5 Complex to complex systems, and accuracy of obtained physical-chemical constants. Simultaneously, we were able to demonstrate the influence of electromigration dispersion on the separation efficiency, which is not possible using the common theoretical approaches, and predict the electromigration order reversals of profen peaks. We have shown that determined acid dissociation and complexation parameters in combination with tool Simul 5 Complex software can be used for optimization of separation conditions in capillary electrophoresis. Copyright © 2014 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guney, Ali; Poyraz, M. Ibrahim; Kangal, Olgac, E-mail: kangal@itu.edu.tr

Highlights: • Both PET and PVC have nearly the same densities. • The best pH value will be 4 for optimizing pH values. • Malic acid gave the best results for selective separation of PET and PVC. - Abstract: Plastics have become the widely used materials because of their advantages, such as cheapness, endurance, lightness, and hygiene. However, they cause waste and soil pollution and they do not easily decompose. Many promising technologies are being investigated for separating mixed thermoplastics, but they are still uneconomical and unreliable. Depending on their surface characteristics, these plastics can be separated from each othermore » by flotation method which is useful mineral processing technique with its low cost and simplicity. The main objective of this study is to investigate the flotation characteristics of PET and PVC and determine the effect of plasticizer reagents on efficient plastic separation. For that purpose, various parameters such as pH, plasticizer concentration, plasticizer type, conditioning temperature and thermal conditioning were investigated. As a result, PET particles were floated with 95.1% purity and 65.3% efficiency while PVC particles were obtained with 98.1% purity and 65.3% efficiency.« less

Separation and quantification of monoclonal-antibody aggregates by hollow-fiber-flow field-flow fractionation.

PubMed

Fukuda, Jun; Iwura, Takafumi; Yanagihara, Shigehiro; Kano, Kenji

2014-10-01

Hollow-fiber-flow field-flow fractionation (HF5) separates protein molecules on the basis of the difference in the diffusion coefficient, and can evaluate the aggregation ratio of proteins. However, HF5 is still a minor technique because information on the separation conditions is limited. We examined in detail the effect of different settings, including the main-flow rate, the cross-flow rate, the focus point, the injection amount, and the ionic strength of the mobile phase, on fractographic characteristics. On the basis of the results, we proposed optimized conditions of the HF5 method for quantification of monoclonal antibody in sample solutions. The HF5 method was qualified regarding the precision, accuracy, linearity of the main peak, and quantitation limit. In addition, the HF5 method was applied to non-heated Mab A and heat-induced-antibody-aggregate-containing samples to evaluate the aggregation ratio and the distribution extent. The separation performance was comparable with or better than that of conventional methods including analytical ultracentrifugation-sedimentation velocity and asymmetric-flow field-flow fractionation.

Optimization of chromatographic conditions for determination of aflatoxin B1, B2, G1 and G2 by using liquid chromatography-mass Spectrometry

NASA Astrophysics Data System (ADS)

Ramadhaningtyas, Dillani Putri; Aryana, Nurhani; Aristiawan, Yosi; Styarini, Dyah

2017-11-01

The optimization of instrument condition and chromatographic separation for analysis of aflatoxin B1, B2, G1 and G2 using liquid chromatography tandem with mass spectrometer detector was conducted in the aim to provide more accurate and reliable analysis results. The aflatoxin known to be serious threat for human health as it is classified as the carcinogenic compounds. The aflatoxin B1, B2, G1 and G2 were selected due to its extensive contamination in various agricultural commodities. The best chromatographic separation was obtained using C-18 column with gradient elution of solvent 5 mM ammonium acetate and 0.1% formic acid in methanol at 7 minutes runtime analysis. The linearity of the detector showed satisfied results as the coefficient determination found to be 0.9994, 0.9996, 0.9998 and 0.9987 for aflatoxin B1, G1, B2, and G2 respectively in the range concentration from 1 to 20 ng/g. The quantifier ion selected for the aflatoxin B1, B2, G1 and G2 was m/z 285.1, 259, 243 and 313 respectively. The instrument precision at these quantifier ions also showed satisfied result with %RSD was around 3.4 to 6.8%. The optimized method present in this study can be used for further sample analysis.

Modelling mid-course corrections for optimality conditions along interplanetary transfers

NASA Astrophysics Data System (ADS)

Iorfida, Elisabetta; Palmer, Phil; Roberts, Mark

2014-12-01

Within the field of trajectory optimisation, Lawden developed the primer vector theory, which defines a set of necessary conditions to characterise whether a transfer trajectory, in the two-body problem context, is optimum with respect to propellant usage. If the conditions are not satisfied, a region of the transfer trajectory is identified in which one or more potential intermediate impulses are performed in order to lower the overall cost. The method is computationally complex owing to having to solve a boundary value problem. In this paper is presented a new propagator that reduces the mathematical complexity and the computational cost of the problem, in particular it exploits a separation between the in-plane and out-of-plane components of the primer vector along the transfer trajectory. Using this propagator, the optimality of the transfer arc has been investigated, varying the departure and arrival orbits. In particular, keeping fixed the transfer trajectory, the optimality has been extensively analysed varying both the initial and final positions on the orbit, together with the directions of the initial and final thrust impulses.

Boundary-Layer Separation Control under Low-Pressure Turbine Airfoil Conditions using Glow-Discharge Plasma Actuators

NASA Technical Reports Server (NTRS)

Hultgren, Lennart S.; Ashpis, David E.

2003-01-01

Modem low-pressure turbines, in general, utilize highly loaded airfoils in an effort to improve efficiency and to lower the number of airfoils needed. Typically, the airfoil boundary layers are turbulent and fully attached at takeoff conditions, whereas a substantial fraction of the boundary layers on the airfoils may be transitional at cruise conditions due to the change of density with altitude. The strong adverse pressure gradients on the suction side of these airfoils can lead to boundary-layer separation at the latter low Reynolds number conditions. Large separation bubbles, particularly those which fail to reattach, cause a significant degradation of engine efficiency. A component efficiency drop of the order 2% may occur between takeoff and cruise conditions for large commercial transport engines and could be as large as 7% for smaller engines at higher altitude. An efficient means of of separation elimination/reduction is, therefore, crucial to improved turbine design. Because the large change in the Reynolds number from takeoff to cruise leads to a distinct change in the airfoil flow physics, a separation control strategy intended for cruise conditions will need to be carefully constructed so as to incur minimum impact/penalty at takeoff. A complicating factor, but also a potential advantage in the quest for an efficient strategy, is the intricate interplay between separation and transition for the situation at hand. Volino gives a comprehensive discussion of several recent studies on transition and separation under low-pressure-turbine conditions, among them one in the present facility. Transition may begin before or after separation, depending on the Reynolds number and other flow conditions. If the transition occurs early in the boundary layer then separation may be reduced or completely eliminated. Transition in the shear layer of a separation bubble can lead to rapid reattachment. This suggests using control mechanisms to trigger and enhance early transition. Gad-el-Hak provides a review of various techniques for flow control in general and Volino discusses recent studies on separation control under low-pressure-turbine conditions utilizing passive as well as active devices. As pointed out by Volino, passive devices optimized for separation control at low Reynolds numbers tend to increase losses at high Reynolds numbers, Active devices have the attractive feature that they can be utilized only in operational regimes where they are needed and when turned off would not affect the flow. The focus in the present paper is an experimental Separation is induced on a flat plate installed in a closed-circuit wind tunnel by a shaped insert on the opposite wall. The flow conditions represent flow over the suction surface of a modem low-pressure-turbine airfoil ('Pak-B'). The Reynolds number, based on wetted plate length and nominal exit velocity, is varied from 50,000 to 300,000, covering cruise to takeoff conditions. Low (0.2%) and high (2.5%) Gee-stream turbulence intensities are set using passive grids. A spanwise-oriented phased-plasma-array actuator, fabricated on a printed circuit board, is surface- flush-mounted upstream of the separation point and can provide forcing in a wide frequency range. Static surface pressure measurements and hot-wire anemometry of the base and controlled flows are performed and indicate that the glow-discharge plasma actuator is an effective device for separation control. of active separation control using glow discharge plasma actuators.

Retention prediction and separation optimization under multilinear gradient elution in liquid chromatography with Microsoft Excel macros.

PubMed

Fasoula, S; Zisi, Ch; Gika, H; Pappa-Louisi, A; Nikitas, P

2015-05-22

A package of Excel VBA macros have been developed for modeling multilinear gradient retention data obtained in single or double gradient elution mode by changing organic modifier(s) content and/or eluent pH. For this purpose, ten chromatographic models were used and four methods were adopted for their application. The methods were based on (a) the analytical expression of the retention time, provided that this expression is available, (b) the retention times estimated using the Nikitas-Pappa approach, (c) the stepwise approximation, and (d) a simple numerical approximation involving the trapezoid rule for integration of the fundamental equation for gradient elution. For all these methods, Excel VBA macros have been written and implemented using two different platforms; the fitting and the optimization platform. The fitting platform calculates not only the adjustable parameters of the chromatographic models, but also the significance of these parameters and furthermore predicts the analyte elution times. The optimization platform determines the gradient conditions that lead to the optimum separation of a mixture of analytes by using the Solver evolutionary mode, provided that proper constraints are set in order to obtain the optimum gradient profile in the minimum gradient time. The performance of the two platforms was tested using experimental and artificial data. It was found that using the proposed spreadsheets, fitting, prediction, and optimization can be performed easily and effectively under all conditions. Overall, the best performance is exhibited by the analytical and Nikitas-Pappa's methods, although the former cannot be used under all circumstances. Copyright © 2015 Elsevier B.V. All rights reserved.

A new open tubular capillary microextraction and sweeping for the analysis of super low concentration of hydrophobic compounds.

PubMed

Xia, Zhining; Gan, Tingting; Chen, Hua; Lv, Rui; Wei, Weili; Yang, Fengqing

2010-10-01

A sample pre-concentration method based on the in-line coupling of in-tube solid-phase microextraction and electrophoretic sweeping was developed for the analysis of hydrophobic compounds. The sample pre-concentration and electrophoretic separation processes were simply and sequentially carried out with a (35%-phenyl)-methylpolysiloxane-coated capillary. The developed method was validated and applied to enrich and separate several pharmaceuticals including loratadine, indomethacin, ibuprofen and doxazosin. Several parameters of microextration were investigated such as temperature, pH and eluant. And the concentration of microemulsion that influences separation efficiency and microextraction efficiency were also studied. Central composite design was applied for the optimization of sampling flow rate and sampling time that interact in a very complex way with each other. The precision, sensitivity and recovery of the method were investigated. Under the optimal conditions, the maximum enrichment factors for loratadine, indomethacin, ibuprofen and doxazosin in aqueous solutions are 1355, 571, 523 and 318, respectively. In addition, the developed method was applied to determine loratadine in rabbit blood sample.

Feature Vector Construction Method for IRIS Recognition

NASA Astrophysics Data System (ADS)

Odinokikh, G.; Fartukov, A.; Korobkin, M.; Yoo, J.

2017-05-01

One of the basic stages of iris recognition pipeline is iris feature vector construction procedure. The procedure represents the extraction of iris texture information relevant to its subsequent comparison. Thorough investigation of feature vectors obtained from iris showed that not all the vector elements are equally relevant. There are two characteristics which determine the vector element utility: fragility and discriminability. Conventional iris feature extraction methods consider the concept of fragility as the feature vector instability without respect to the nature of such instability appearance. This work separates sources of the instability into natural and encodinginduced which helps deeply investigate each source of instability independently. According to the separation concept, a novel approach of iris feature vector construction is proposed. The approach consists of two steps: iris feature extraction using Gabor filtering with optimal parameters and quantization with separated preliminary optimized fragility thresholds. The proposed method has been tested on two different datasets of iris images captured under changing environmental conditions. The testing results show that the proposed method surpasses all the methods considered as a prior art by recognition accuracy on both datasets.

Facilitating the Hyphenation of CIEF and MALDI-MS for Two-Dimensional Separation of Proteins

PubMed Central

Cheng, Chang; Lu, Joann J.; Wang, Xiayan; Roberts, Jonathan; Liu, Shaorong

2011-01-01

Both CIEF and MALDI-MS are frequently used in protein analysis, but hyphenation of the two is not investigated proportionally. One of the major reasons is that the additives (such as carrier ampholytes and detergent) in CIEF severely suppress the MALDI-MS signal, which hampers the hyphenation of the two. In this paper, we develop a simple means to alleviate the above signal-suppressing effect. We first deposit 1 µL of water onto a MALDI-MS target, deliver a fraction of CIEF-separated protein (~0.1 µL) to the water droplet, evaporate the solvent, add 0.5 µL of MALDI matrix to the sample spot, dry the matrix, and move the target plate to a MALDI-TOF-MS for mass spectrum measurement. We optimize the droplet volume and the laser-ablation region. Under the optimized conditions, we improve the signal to noise ratio by 2–10 fold. We also apply this method for two-dimensional separations of standard proteins and Apolipoprotein A-I, a membrane protein expressed in E. Coli cells. PMID:20603827

Primary Energy Efficiency Analysis of Different Separate Sensible and Latent Cooling Techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Abdelaziz, Omar

2015-01-01

Separate Sensible and Latent cooling (SSLC) has been discussed in open literature as means to improve air conditioning system efficiency. The main benefit of SSLC is that it enables heat source optimization for the different forms of loads, sensible vs. latent, and as such maximizes the cycle efficiency. In this paper I use a thermodynamic analysis tool in order to analyse the performance of various SSLC technologies including: multi-evaporators two stage compression system, vapour compression system with heat activated desiccant dehumidification, and integrated vapour compression with desiccant dehumidification. A primary coefficient of performance is defined and used to judge themore » performance of the different SSLC technologies at the design conditions. Results showed the trade-off in performance for different sensible heat factor and regeneration temperatures.« less

Use of multiresponse statistical techniques to optimize the separation of diosmin, hesperidin, diosmetin and hesperitin in different pharmaceutical preparations by high performance liquid chromatography with UV-DAD.

PubMed

Sammani, Mohamad Subhi; Clavijo, Sabrina; Portugal, Lindomar; Suárez, Ruth; Seddik, Hassan; Cerdà, Víctor

2017-05-15

A new method for the separation and determination of four flavonoids: hesperidin (HES), diosmin (DIO), hesperitin (HTIN), and diosmetin (DTIN) in pure form and pharmaceutical formulations has been developed by using high performance liquid chromatography (HPLC) with UV-DAD detection. Multivariate statistics (2 k full factorial and Box Behnken Designs) has been used for the multiresponse optimization of the chromatographic separation, which was completed in 22min, and carried out on a symmetry® C18 column (250×3mm; 5µm) as stationary phase. Separation was conducted by gradient elution mode using a mixture of methanol, acetonitrile and water pH: 2.5 (CH 3 COOH), as mobile phase. Analytes were separated setting the column at 22°C, with a flow rate of 0.58mLmin -1 and detected at 285nm. Under the optimized conditions, the flavonoids showed retention times of: 8.62, 11.53, 18.55 and 19.94min for HES, DIO, HTIN and DTIN, respectively. Limits of detection and quantification were <0.0156µgmL -1 and <0.100µgmL -1 , respectively. Linearity was achieved with good correlation coefficients values (r 2 =0.999; n=5). Intra-day and inter-day precision were found to be less than 3.44% (n=7). Finally, the proposed method was successfully applied to determine the target flavonoids in pharmaceutical preparations with satisfactory recoveries (between 95.2% and 107.9%), demonstrating that should also find application in the quality control, as well as in the pharmacokinetic studies of these drugs. Copyright © 2017 Elsevier B.V. All rights reserved.

High-performance liquid-chromatographic separation of subcomponents of antimycin-A

USGS Publications Warehouse

Abidi, S.L.

1988-01-01

Using a reversed-phase high-performance liquid chromatographic (HPLC) technique, a mixture of antimycins A was separated into eight hitherto unreported subcomponents, Ala, Alb, A2a, A2b, A3a, A3b, A4a, and A4b. Although a base-line resolution of the known four major antimycins Al, A2, A3, and A4 was readily achieved with mobile phases containing acetate buffers, the separation of the new antibiotic subcomponents was highly sensitive to variation in mobile phase conditions. The type and composition of organic modifiers, the nature of buffer salts, and the concentration of added electrolytes had profound effects on capacity factors, separation factors, and peak resolution values. Of the numerous chromatographic systems examined, a mobile phase consisting of methanol-water (70:30) and 0.005 M tetrabutylammonium phosphate at pH 3.0 yielded the most satisfactory results for the separation of the subcomponents. Reversed-phase gradient HPLC separation of the dansylated or methylated antibiotic compounds produced superior chromatographic characteristics and the presence of added electrolytes was not a critical factor for achieving separation. Differences in the chromatographic outcome between homologous and structural isomers were interpretated based on a differential solvophobic interaction rationale. Preparative reversed-phase HPLC under optimal conditions enabled isolation of pure samples of the methylated antimycin subcomponents for use in structural studies.

Recovery of Iron from Hematite-Rich Diasporic-Type Bauxite Ore

NASA Astrophysics Data System (ADS)

Jiang, Tao; Li, Zhuoxuan; Yang, Lin; Li, Guanghui; Zhang, Yuanbo; Zeng, Jinghua

A technique has been proposed for recovering iron from hematite-rich diasporic-type bauxite ore in this study. Direct reduction roasting followed by low intensity wet magnetic separation process was carried out. The parameters including reduction temperature and time, sodium salts, grinding conditions and magnetic field intensity for separation of iron were determined. The optimum process parameters as follows: roasting temperature of 1050 °C, time of 60 min, sodium salts involving sodium sulfate, borax, sodium carbonate with dosages of 10 wt%, 2 wt%, 35 wt% respectively, and magnetic field intensity of 1000 Gs with fineness of pulp reached 92.75% passing -0.074mm. Under the optimal conditions, an iron concentrate containing 88.17% total iron grade and iron recovery of 92.51% was obtained, 4.55% total iron grade in tailings. This novel technique provide a potential route for utilizing hematiterich diasporic bauxite ore, recovering iron resource firstly, and extracting alumina from magnetic separation tailings further.

Mass analyzer ``MASHA'' high temperature target and plasma ion source

NASA Astrophysics Data System (ADS)

Semchenkov, A. G.; Rassadov, D. N.; Bekhterev, V. V.; Bystrov, V. A.; Chizov, A. Yu.; Dmitriev, S. N.; Efremov, A. A.; Guljaev, A. V.; Kozulin, E. M.; Oganessian, Yu. Ts.; Starodub, G. Ya.; Voskresensky, V. M.; Bogomolov, S. L.; Paschenko, S. V.; Zelenak, A.; Tikhonov, V. I.

2004-05-01

A new separator and mass analyzer of super heavy atoms (MASHA) has been created at the FLNR JINR Dubna to separate and measure masses of nuclei and molecules with precision better than 10-3. First experiments with the FEBIAD plasma ion source have been done and give an efficiency of ionization of up to 20% for Kr with a low flow test leak (6 particle μA). We suppose a magnetic field optimization, using the additional electrode (einzel lens type) in the extracting system, and an improving of the vacuum conditions in order to increase the ion source efficiency.

Generalized extended Lagrangian Born-Oppenheimer molecular dynamics

DOE PAGES

Niklasson, Anders M. N.; Cawkwell, Marc J.

2014-10-29

Extended Lagrangian Born-Oppenheimer molecular dynamics based on Kohn-Sham density functional theory is generalized in the limit of vanishing self-consistent field optimization prior to the force evaluations. The equations of motion are derived directly from the extended Lagrangian under the condition of an adiabatic separation between the nuclear and the electronic degrees of freedom. We show how this separation is automatically fulfilled and system independent. The generalized equations of motion require only one diagonalization per time step and are applicable to a broader range of materials with improved accuracy and stability compared to previous formulations.

Quantum design of photosynthesis for bio-inspired solar-energy conversion.

PubMed

Romero, Elisabet; Novoderezhkin, Vladimir I; van Grondelle, Rienk

2017-03-15

Photosynthesis is the natural process that converts solar photons into energy-rich products that are needed to drive the biochemistry of life. Two ultrafast processes form the basis of photosynthesis: excitation energy transfer and charge separation. Under optimal conditions, every photon that is absorbed is used by the photosynthetic organism. Fundamental quantum mechanics phenomena, including delocalization, underlie the speed, efficiency and directionality of the charge-separation process. At least four design principles are active in natural photosynthesis, and these can be applied practically to stimulate the development of bio-inspired, human-made energy conversion systems.

Large-scale dialysis of sample lipids

USGS Publications Warehouse

Meadows, Jill; Tillitt, Donald E.; Huckins, James; Schroeder, D.

1993-01-01

The use of a semipermeable membrane device (SPMD) for dialysis in an organic solvent phase is an efficient alternative approach to separation of contaminants from large amounts of lipid (up to 50 grams or more) prior to organic chemical analysis. Passive separation of contaminants can be accomplished with a minimum of equipment and a comparatively small volume of solvent. This study examines the effects of factors such as dialytic solvent, lipid type, dialytic solvent:lipid volume ratio, dialysis time, and temperature on the performance of polyethylene SPMDs during lipid-contaminant separations. The experimental conditions for maximal recoveries of organochlorine pesticides and polychlorinated biphenyls with minimal lipid carryover are determined for the examined variables. When the dialytic procedure is optimized, very satisfactory and highly reproducible analyte recoveries can be obtained in a few days while separating > 90% of the lipid material in a single operation.

Toward the optimization of control of unsteady separation

NASA Technical Reports Server (NTRS)

Shen, S. F.; Xiao, Zheng-Hua

1992-01-01

Regardless of our understanding of the complicated physical process, means can always be found to alter the occurrence and development of unsteady separation. To be able to optimize the control of separation, however, requires the identification of the critical aspects to which the intervention may be focused and achieve the desired result with minimum waste of effort. The Lagrangian analysis of unsteady boundary-layer traces the trajectories of individual fluid particles and reveals the 'bad seeds' that, through extreme deformation in the direction normal to the wall, eventually develop into a virtual barrier and cause the ejection of boundary-layer material into the main stream. It follows logically that separation can be triggered or delayed most effectively by targeting these 'bad seeds.' Since they are normally interior points of the boundary layer, attempts to influence them through the boundary conditions are necessarily indirect. Furthermore, as the strategy has to be the modification of the growing process of the 'bad seeds,' whatever may be the intervention scheme, it needs to be strong enough and early enough. In Shen and Wu, examples of how acceleration/deceleration of the two dimensional body, as well as the moving wall of a rotating cylinder, may affect the development of the bad seed toward separation are shown. In fact it was mentioned therein that the results might be the first step for a feasibility study of the control of unsteady separation. Presented are additional results of applying suction to an impulsively started circular cylinder.

Why 'Optimal' Payment for Healthcare Providers Can Never be Optimal Under Community Rating.

PubMed

Zweifel, Peter; Frech, H E

2016-02-01

This article extends the existing literature on optimal provider payment by accounting for consumer heterogeneity in preferences for health insurance and healthcare. This heterogeneity breaks down the separation of the relationship between providers and the health insurer and the relationship between consumers and the insurer. Both experimental and market evidence for a high degree of heterogeneity are presented. Given heterogeneity, a uniform policy fails to effectively control moral hazard, while incentives for risk selection created by community rating cannot be neutralized through risk adjustment. Consumer heterogeneity spills over into relationships with providers, such that a uniform contract with providers also cannot be optimal. The decisive condition for ensuring optimality of provider payment is to replace community rating (which violates the principle of marginal cost pricing) with risk rating of contributions combined with subsidization targeted at high risks with low incomes.

Optimal Control Modification for Robust Adaptation of Singularly Perturbed Systems with Slow Actuators

NASA Technical Reports Server (NTRS)

Nguyen, Nhan T.; Ishihara, Abraham; Stepanyan, Vahram; Boskovic, Jovan

2009-01-01

Recently a new optimal control modification has been introduced that can achieve robust adaptation with a large adaptive gain without incurring high-frequency oscillations as with the standard model-reference adaptive control. This modification is based on an optimal control formulation to minimize the L2 norm of the tracking error. The optimal control modification adaptive law results in a stable adaptation in the presence of a large adaptive gain. This study examines the optimal control modification adaptive law in the context of a system with a time scale separation resulting from a fast plant with a slow actuator. A singular perturbation analysis is performed to derive a modification to the adaptive law by transforming the original system into a reduced-order system in slow time. The model matching conditions in the transformed time coordinate results in increase in the feedback gain and modification of the adaptive law.

Research on design method of the full form ship with minimum thrust deduction factor

NASA Astrophysics Data System (ADS)

Zhang, Bao-ji; Miao, Ai-qin; Zhang, Zhu-xin

2015-04-01

In the preliminary design stage of the full form ships, in order to obtain a hull form with low resistance and maximum propulsion efficiency, an optimization design program for a full form ship with the minimum thrust deduction factor has been developed, which combined the potential flow theory and boundary layer theory with the optimization technique. In the optimization process, the Sequential Unconstrained Minimization Technique (SUMT) interior point method of Nonlinear Programming (NLP) was proposed with the minimum thrust deduction factor as the objective function. An appropriate displacement is a basic constraint condition, and the boundary layer separation is an additional one. The parameters of the hull form modification function are used as design variables. At last, the numerical optimization example for lines of after-body of 50000 DWT product oil tanker was provided, which indicated that the propulsion efficiency was improved distinctly by this optimal design method.

A method for recovery of iron, titanium, and vanadium from vanadium-bearing titanomagnetite

NASA Astrophysics Data System (ADS)

Zhang, Yi-min; Wang, Li-na; Chen, De-sheng; Wang, Wei-jing; Liu, Ya-hui; Zhao, Hong-xin; Qi, Tao

2018-02-01

An innovative method for recovering valuable elements from vanadium-bearing titanomagnetite is proposed. This method involves two procedures: low-temperature roasting of vanadium-bearing titanomagnetite and water leaching of roasting slag. During the roasting process, the reduction of iron oxides to metallic iron, the sodium oxidation of vanadium oxides to water-soluble sodium vanadate, and the smelting separation of metallic iron and slag were accomplished simultaneously. Optimal roasting conditions for iron/slag separation were achieved with a mixture thickness of 42.5 mm, a roasting temperature of 1200°C, a residence time of 2 h, a molar ratio of C/O of 1.7, and a sodium carbonate addition of 70wt%, as well as with the use of anthracite as a reductant. Under the optimal conditions, 93.67% iron from the raw ore was recovered in the form of iron nugget with 95.44% iron grade. After a water leaching process, 85.61% of the vanadium from the roasting slag was leached, confirming the sodium oxidation of most of the vanadium oxides to water-soluble sodium vanadate during the roasting process. The total recoveries of iron, vanadium, and titanium were 93.67%, 72.68%, and 99.72%, respectively.

Detection of fraudulent addition of bovine whey in water buffalo ricotta cheese by isoelectric focusing.

PubMed

Fuselli, Fabio; Deluca, Anna; Montepeloso, Emanuela A; Ibba, Giulia; Tidona, Flavio; Longo, Lucia; Marianella, Rosa M

2015-10-01

Prevention of food fraud in the dairy field is a difficult issue for researchers, industries and policy makers, both for commercial and health reasons. Currently, no analytical method allows detection of the addition of bovine whey to water buffalo ricotta, so this fraudulent practice cannot be prevented. The authors' aim was to develop such a method. The conditions for extraction and purification of denatured ricotta whey proteins, which are unfolded and coagulated by heating during the production process, were optimized. The optimal composition of the polyacrylamide gel (pH range, type and concentration of chemical separator) was first evaluated and then the best conditions to perform the separation by isoelectric focusing were established. The performance of the method (precision, selectivity, robustness, sensibility) was determined. The method was shown to be reliable and robust for detection of the presence of bovine whey added to water buffalo Ricotta at percentages above 5% (v/v). The results suggest that the differences observed between bovine and water buffalo electrophoretic profiles are due to bovine β-lactoglobulin isoform A, which is never detected in water buffalo samples. © 2014 Society of Chemical Industry.

Large gamma-ray detector arrays and electromagnetic separators

NASA Astrophysics Data System (ADS)

Lee, I.-Yang

2013-12-01

The use of large gamma-ray detector arrays with electromagnetic separators is a powerful combination. Various types of gamma-ray detectors have been used; some provide high detector efficiency such as scintillation detector array, others use Ge detectors for good energy resolution, and recently developed Ge energy tracking arrays gives both high peak-to-background ratio and position resolution. Similarly, different types of separators were used to optimize the performance under different experimental requirements and conditions. For example, gas-filled separators were used in heavy element studies for their large efficiency and beam rejection factor. Vacuum separators with good isotope resolution were used in transfer and fragmentation reactions for the study of nuclei far from stability. This paper presents results from recent experiments using gamma-ray detector arrays in combination with electromagnetic separators, and discusses the physics opportunities provided by these instruments. In particular, we review the performance of the instruments currently in use, and discuss the requirements of instruments for future radioactive beam accelerator facilities.

Optimized ultrasound-assisted extraction procedure for the analysis of opium alkaloids in papaver plants by cyclodextrin-modified capillary electrophoresis.

PubMed

Fakhari, Ali Reza; Nojavan, Saeed; Ebrahimi, Samad Nejad; Evenhuis, Christopher John

2010-07-01

This study investigated the use of ultrasound-assisted extraction to improve the extraction efficiency of morphine, codeine and thebaine from the papaver plants. Extraction conditions such as type of solvent, temperature, duration, frequency and power level of ultrasonic were optimized and the influences of different parameters on resolution of alkaloids in CE were studied. The optimized condition for CE separation includes a sodium phosphate buffer (100 mM, pH 3.0) containing 5 mM alpha-CD. The optimized extraction conditions for ultrasound-assisted extraction was an extraction time of 1 h, an ultrasonic frequency of 60 kHz with water-methanol (80:20) at 40 degrees C as the extraction solvent. The LOD for alkaloids was found to be 0.1 microg/mL at a signal-to-noise ratio of 3:1. The RSDs for peak areas were in the range of 1.4-4.4%. The amounts of opium alkaloids (mg/100 g dried sample) in four Iranian papaver plants were found to be in the range of 7.8-8.7 (morphine), 5.5-9.5 (codeine) and 1.4-10.4 (thebaine). It should be emphasized that no cleanup of the filtered extract was required; hence, direct determination after extraction drastically simplifies the analytical process.

Steady-state configuration and tension calculations of marine cables under complex currents via separated particle swarm optimization

NASA Astrophysics Data System (ADS)

Xu, Xue-song

2014-12-01

Under complex currents, the motion governing equations of marine cables are complex and nonlinear, and the calculations of cable configuration and tension become difficult compared with those under the uniform or simple currents. To obtain the numerical results, the usual Newton-Raphson iteration is often adopted, but its stability depends on the initial guessed solution to the governing equations. To improve the stability of numerical calculation, this paper proposed separated the particle swarm optimization, in which the variables are separated into several groups, and the dimension of search space is reduced to facilitate the particle swarm optimization. Via the separated particle swarm optimization, these governing nonlinear equations can be solved successfully with any initial solution, and the process of numerical calculation is very stable. For the calculations of cable configuration and tension of marine cables under complex currents, the proposed separated swarm particle optimization is more effective than the other particle swarm optimizations.

Determination of the optimal mesh parameters for Iguassu centrifuge flow and separation calculations

NASA Astrophysics Data System (ADS)

Romanihin, S. M.; Tronin, I. V.

2016-09-01

We present the method and the results of the determination for optimal computational mesh parameters for axisymmetric modeling of flow and separation in the Iguasu gas centrifuge. The aim of this work was to determine the mesh parameters which provide relatively low computational cost whithout loss of accuracy. We use direct search optimization algorithm to calculate optimal mesh parameters. Obtained parameters were tested by the calculation of the optimal working regime of the Iguasu GC. Separative power calculated using the optimal mesh parameters differs less than 0.5% from the result obtained on the detailed mesh. Presented method can be used to determine optimal mesh parameters of the Iguasu GC with different rotor speeds.

Separation and purification of epigallocatechin-3-gallate (EGCG) from green tea using combined macroporous resin and polyamide column chromatography.

PubMed

Jin, Xin; Liu, Mingyan; Chen, Zaixing; Mao, Ruikun; Xiao, Qinghuan; Gao, Hua; Wei, Minjie

2015-10-01

Epigallocatechin-3-gallate (EGCG) is a major bioactive ingredient of green tea that produces beneficial neuroprotective effects. In this paper, to optimize the EGCG enrichment, thirteen macroporous resins with different chemical and physical properties were systemically evaluated. Among the thirteen tested resins, the H-bond resin HPD826 exhibited best adsorption/desorption capabilities and desorption ratio, as well as weakest affinity for caffeine. The absorption of EGCG on the HPD826 resin followed the pseudo-second-order kinetics and Langmuir isotherm model. The separation parameters of EGCG were optimized by dynamic adsorption/desorption experiments with the HPD826 resin column. Under the optimal condition, the content of EGCG in the 30% ethanol eluent increased by 5.8-fold from 7.7% to 44.6%, with the recovery yield of 72.1%. After further purification on a polyamide column, EGCG with 74.8% purity was obtained in the 40-50% ethanol fraction with a recovery rate of 88.4%. In addition, EGCG with 95.1% purity could be easily obtained after one-step crystallization in distilled water. Our study suggests that the combined macroporous resin and polyamide column chromatography is a simple method for large-scale separation and purification of EGCG from natural plants for food and pharmaceutical applications. Copyright © 2015 Elsevier B.V. All rights reserved.

Insights on beer volatile profile: Optimization of solid-phase microextraction procedure taking advantage of the comprehensive two-dimensional gas chromatography structured separation.

PubMed

Martins, Cátia; Brandão, Tiago; Almeida, Adelaide; Rocha, Sílvia M

2015-06-01

The aroma profile of beer is crucial for its quality and consumer acceptance, which is modu-lated by a network of variables. The main goal of this study was to optimize solid-phase microextraction experimental parameters (fiber coating, extraction temperature, and time), taking advantage of the comprehensive two-dimensional gas chromatography structured separation. As far as we know, it is the first time that this approach was used to the untargeted and comprehensive study of the beer volatile profile. Decarbonation is a critical sample preparation step, and two conditions were tested: static and under ultrasonic treatment, and the static condition was selected. Considering the conditions that promoted the highest extraction efficiency, the following parameters were selected: poly(dimethylsiloxane)/divinylbenzene fiber coating, at 40ºC, using 10 min of pre-equilibrium followed by 30 min of extraction. Around 700-800 compounds per sample were detected, corresponding to the beer volatile profile. An exploratory application was performed with commercial beers, using a set of 32 compounds with reported impact on beer aroma, in which different patterns can be observed through the structured chromatogram. In summary, the obtained results emphasize the potential of this methodology to allow an in-depth study of volatile molecular composition of beer. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High-performance liquid chromatographic analysis of as-synthesised N,N'-dimethylformamide-stabilised gold nanoclusters product

NASA Astrophysics Data System (ADS)

Xie, Shunping; Paau, Man Chin; Zhang, Yan; Shuang, Shaomin; Chan, Wan; Choi, Martin M. F.

2012-08-01

Reverse-phase high-performance liquid chromatographic (RP-HPLC) separation and analysis of polydisperse water-soluble gold nanoclusters (AuNCs) stabilised with N,N'-dimethylformamide (DMF) were investigated. Under optimal elution gradient conditions, the separation of DMF-AuNCs was monitored by absorption and fluorescence spectroscopy. The UV-vis spectral characteristics of the separated DMF-AuNCs have been captured and they do not possess distinct surface plasmon resonance bands, indicating that all DMF-AuNCs are small AuNCs. The photoluminescence emission spectra of the separated DMF-AuNCs are in the blue-light region. Moreover, cationic DMF-AuNCs are for the first time identified by ion chromatography. Our proposed RP-HPLC methodology has been successfully applied to separate AuNCs of various Au atoms as well as DMF-stabilised ligands. Finally, the composition of the separated DMF-AuNCs was confirmed by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry and electrospray ionisation mass spectrometry, proving that the as-synthesised DMF-AuNCs product consists of Au10+, Au10, Au11, Au12, Au13, and Au14 NCs stabilised with various numbers of DMF ligands.Reverse-phase high-performance liquid chromatographic (RP-HPLC) separation and analysis of polydisperse water-soluble gold nanoclusters (AuNCs) stabilised with N,N'-dimethylformamide (DMF) were investigated. Under optimal elution gradient conditions, the separation of DMF-AuNCs was monitored by absorption and fluorescence spectroscopy. The UV-vis spectral characteristics of the separated DMF-AuNCs have been captured and they do not possess distinct surface plasmon resonance bands, indicating that all DMF-AuNCs are small AuNCs. The photoluminescence emission spectra of the separated DMF-AuNCs are in the blue-light region. Moreover, cationic DMF-AuNCs are for the first time identified by ion chromatography. Our proposed RP-HPLC methodology has been successfully applied to separate AuNCs of various Au atoms as well as DMF-stabilised ligands. Finally, the composition of the separated DMF-AuNCs was confirmed by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry and electrospray ionisation mass spectrometry, proving that the as-synthesised DMF-AuNCs product consists of Au10+, Au10, Au11, Au12, Au13, and Au14 NCs stabilised with various numbers of DMF ligands. This article was submitted as part of a Themed Issue on metallic clusters. Other papers on this topic can be found in issue 14 of vol. 4 (2012). This issue can be found from the Nanoscale homepage [http://www.rsc.org/nanoscale].

Synchronized separation, concentration and determination of trace sulfadiazine and sulfamethazine in food and environment by using polyoxyethylene lauryl ether-salt aqueous two-phase system coupled to high-performance liquid chromatography.

PubMed

Lu, Yang; Cong, Biao; Tan, Zhenjiang; Yan, Yongsheng

2016-11-01

Polyoxyethylene lauryl ether (POELE10)-Na2C4H4O6 aqueous two-phase extraction system (ATPES) is a novel and green pretreatment technique to trace samples. ATPES coupled with high-performance liquid chromatography (HPLC) is used to analyze synchronously sulfadiazine (SDZ) and sulfamethazine (SMT) in animal by-products (i.e., egg and milk) and environmental water sample. It was found that the extraction efficiency (E%) and the enrichment factor (F) of SDZ and SMT were influenced by the types of salts, the concentration of salt, the concentration of POELE10 and the temperature. The orthogonal experimental design (OED) was adopted in the multi-factor experiment to determine the optimized conditions. The final optimal condition was as following: the concentration of POELE10 is 0.027gmL(-1), the concentration of Na2C4H4O6 is 0.180gmL(-1) and the temperature is 35°C. This POELE10-Na2C4H4O6 ATPS was applied to separate and enrich SDZ and SMT in real samples (i.e., water, egg and milk) under the optimal conditions, and it was found that the recovery of SDZ and SMT was 96.20-99.52% with RSD of 0.35-3.41%. The limit of detection (LOD) of this method for the SDZ and SMT in spiked samples was 2.52-3.64pgmL(-1), and the limit of quantitation (LOQ) of this method for the SDZ and SMT in spiked samples was 8.41-12.15pgmL(-1). Copyright © 2016 Elsevier Inc. All rights reserved.

Optimal mixing rate in linear solvent strength gradient liquid chromatography. Balanced mixing program.

PubMed

Blumberg, Leonid M; Desmet, Gert

2016-12-09

The mixing rate (R ϕ ) is the temporal rate of increase in the solvent strength in gradient LC. The optimal R ϕ (R ϕ ,Opt ) is the one at which a required peak capacity of gradient LC analysis is obtained in the shortest time. The balanced mixing program is a one where, for better separation of early eluting solutes, the mixing ramp is preceded by a balanced isocratic hold of the duration depending on R ϕ . The improvement in the separation of the earlier eluites due to the balanced programming has been evaluated. The value of R ϕ ,Opt depends on the solvent composition range covered by the mixing ramp and on the column pressure conditions. The R ϕ ,Opt for a column operating at maximum instrumental pressure is different from R ϕ ,Opt for a column operating below the instrumental pressure limit. On the other hand, it has been shown that the difference in the R ϕ ,Opt values under different conditions is not very large so that a single default R ϕ previously recommended for gradient analyses without the isocratic hold also yields a good approximation to the shortest analysis time for all conditions in the balanced analyses. With or without the initial balance isocratic hold, the recommended default R ϕ is about 5%/t 0 (5% increase in the solvent strength per each t 0 -long increment in time) for small-molecule samples, and about an order of magnitude slower (0.5%/t 0 ) for protein samples. A discussion illustrating the use of the optimization criteria employed here for the techniques other than LSS gradient LC is included. Copyright © 2016 Elsevier B.V. All rights reserved.

Dispersive liquid-liquid microextraction of quinolones in porcine blood: Optimization of extraction procedure and CE separation using experimental design.

PubMed

Vera-Candioti, Luciana; Teglia, Carla M; Cámara, María S

2016-10-01

A dispersive liquid-liquid microextraction procedure was developed to extract nine fluoroquinolones in porcine blood, six of which were quantified using a univariate calibration method. Extraction parameters including type and volume of extraction and dispersive solvent and pH, were optimized using a full factorial and a central composite designs. The optimum extraction parameters were a mixture of 250 μL dichloromethane (extract solvent) and 1250 μL ACN (dispersive solvent) in 500 μL of porcine blood reached to pH 6.80. After shaking and centrifugation, the upper phase was transferred in a glass tube and evaporated under N 2 steam. The residue was resuspended into 50 μL of water-ACN (70:30, v/v) and determined by CE method with DAD, under optimum separation conditions. Consequently, a tenfold enrichment factor can potentially be reached with the pretreatment, taking into account the relationship between initial sample volume and final extract volume. Optimum separation conditions were as follows: BGE solution containing equal amounts of sodium borate (Na 2 B 4 O 7 ) and di-sodium hydrogen phosphate (Na 2 HPO 4 ) with a final concentration of 23 mmol/L containing 0.2% of poly (diallyldimethylammonium chloride) and adjusted to pH 7.80. Separation was performed applying a negative potential of 25 kV, the cartridge was maintained at 25.0°C and the electropherograms were recorded at 275 nm during 4 min. The hydrodynamic injection was performed in the cathode by applying a pressure of 50 mbar for 10 s. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Reversed-phase thin-layer chromatography of homologs of Antimycin-A and related derivatives

USGS Publications Warehouse

Abidi, Sharon L.

1989-01-01

Using a reversed-phase high-performance liquid chromatographic (HPLC) technique, a mixture of antimycins A was separated into eight hitherto unreported subcomponents, Ala, Alb, A2a, A2b, A3a, A3b, A4a, and A4b. Although a base-line resolution of the known four major antimycins Al, A2, A3, and A4 was readily achieved with mobile phases containing acetate buffers, the separation of the new antibiotic subcomponents was highly sensitive to variation in mobile phase conditions. The type and composition of organic modifiers, the nature of buffer salts, and the concentration of added electrolytes had profound effects on capacity factors, separation factors, and peak resolution values. Of the numerous chromatographic systems examined, a mobile phase consisting of methanol-water (70:30) and 0.005 M tetrabutylammonium phosphate at pH 3.0 yielded the most satisfactory results for the separation of the subcomponents. Reversed-phase gradient HPLC separation of the dansylated or methylated antibiotic compounds produced superior chromatographic characteristics and the presence of added electrolytes was not a critical factor for achieving separation. Differences in the chromatographic outcome between homologous and structural isomers were interpretated based on a differential solvophobic interaction rationale. Preparative reversed-phase HPLC under optimal conditions enabled isolation of pure samples of the methylated antimycin subcomponents for use in structural studies.

Ni-H2 cell separator matrix engineering

NASA Technical Reports Server (NTRS)

Scott, W. E.

1992-01-01

This project was initiated to develop alternative separator materials to the previously used asbestos matrices which were removed from the market for health and environmental reasons. The objective of the research was to find a material or combination of materials that had the following characteristics: (1) resistant to the severe conditions encountered in Ni-H2 cells; (2) satisfactory electrical, electrolyte management, and thermal management properties to function properly; (3) environmentally benign; and (4) capable of being manufactured into a separator matrix. During the course of the research it was discovered that separators prepared from wettable polyethylene fibers along and in combination with potassium titanate pigment performed satisfactory in preliminary characterization tests. Further studies lead to the optimization of the separator composition and manufacturing process. Single ply separator sheets were manufactured with 100 percent polyethylene fibers and also with a combination of polyethylene fibers and potassium titanate pigment (PKT) in the ratio of 60 percent PKT and 40 percent fibers. A pilot paper machine was used to produce the experimental separator material by a continuous, wet laid process. Both types of matrices were produced at several different area densities (grams/sq m).

Use of RSM for the multivariate, simultaneous multiobjective optimization of the operating conditions of aliphatic carboxylic acids ion-exclusion chromatography column: Quantitative study of hydrodynamic, isotherm, and thermodynamic behavior.

PubMed

Shojaeimehr, Tahereh; Rahimpour, Farshad; Schwarze, Michael; Repke, Jens-Uwe; Godini, Hamid Reza; Wozny, Günter

2018-04-15

The present study evaluates the capability of ion exclusion chromatography (IEC) of short chain aliphatic carboxylic acids using a cation exchange column (8% sulfonated cross-linked styrene-divinylbenzene copolymer) in different experimental conditions. Since one of the prerequisites to the development of an efficient carboxylic acid separation process is to obtain the optimum operational conditions, response surface methodology (RSM) was used to develop an approach to evaluate carboxylic acids separation process in IEC columns. The effect of the operating conditions such as column temperature, sulfuric acid concentration as the mobile phase, and the flow rate was studied using Central Composite Face (CCF) design. The optimum operating conditions for the separate injection of lactic acid and acetic acid is temperature of 75 °C, sulfuric acid concentration of 0.003 N for both acids and flow rate of 0.916 (0.886) mL/min for acetic acid (lactic acid). Likewise, the optimum conditions for the simultaneous injection of acetic and lactic acid mixture are the column temperature of 68 °C, sulfuric acid concentration of 0.0003 N, and flow rate of 0.777 mL/min. In the next step, the adsorption equilibria of acetic acid and lactic acid on the stationary phase were investigated through a series of Frontal Analysis (FA), Frontal Analysis by Characteristic Points (FACP), and using Langmuir isotherm model. The results showed an excellent agreement between the model and experimental data. Finally, the results of thermodynamic studies proved that the IEC process for separation of acetic and lactic acid is a spontaneous, feasible, exothermic, and random process with a physical adsorption mechanism. The results of the current paper can be a valuable information in the stages of designing IEC columns for separation of aliphatic carboxylic acids. Copyright © 2018 Elsevier B.V. All rights reserved.

[Fast separation and analysis of water-soluble vitamins in spinach by capillary electrophoresis with high voltage].

PubMed

Hu, Xiaoqin; You, Huiyan

2009-11-01

In capillary electrophoresis, 0-40 kV (even higher) voltage can be reached by a connecting double-model high voltage power supply. In the article, water-soluble vitamins, VB1, VB2, VB6, VC, calcium D-pantothenate, D-biotin, nicotinic acid and folic acid in vegetable, were separated by using the high voltage power supply under the condition of electrolyte water solution as running buffer. The separation conditions, such as voltage, the concentration of buffer and pH value etc. , were optimized during the experiments. The results showed that eight water-soluble vitamins could be baseline separated in 2.2 min at 40 kV applied voltage, 25 mmol/L sodium tetraborate buffer solution (pH 8.8). The water-soluble vitamins in spinach were quantified and the results were satisfied. The linear correlation coefficients of the water-soluble vitamins ranged from 0.9981 to 0.9999. The detection limits ranged from 0.2 to 0.3 mg/L. The average recoveries ranged from 88.0% to 100.6% with the relative standard deviations (RSD) range of 1.15%-4.13% for the spinach samples.

A novel technology coupling extraction and foam fractionation for separating the total saponins from Achyranthes bidentata.

PubMed

Ding, Linlin; Wang, Yanji; Wu, Zhaoliang; Liu, Wei; Li, Rui; Wang, Yanyan

2016-10-02

A novel technology coupling extraction and foam fractionation was developed for separating the total saponins from Achyranthes bidentata. In the developed technology, the powder of A. bidentata was loaded in a nylon filter cloth pocket with bore diameter of 180 µm. The pocket was fixed in the bulk liquid phase for continuously releasing saponins. Under the optimal conditions, the concentration and the extraction rate of the total saponins in the foamate by the developed technology were 73.5% and 416.2% higher than those by the traditional technology, respectively. The foamates obtained by the traditional technology and the developed technology were analyzed by ultraperformance liquid chromatography-mass spectrometry to determine their ingredients, and the results appeared that the developed technology exhibited a better performance for separating saponins than the traditional technology. The study is expected to develop a novel technology for cost effectively separating plant-derived materials with surface activity.

Fundamentals and practice for ultrasensitive laser-induced fluorescence detection in microanalytical systems.

PubMed

Johnson, Mitchell E; Landers, James P

2004-11-01

Laser-induced fluorescence is an extremely sensitive method for detection in chemical separations. In addition, it is well-suited to detection in small volumes, and as such is widely used for capillary electrophoresis and microchip-based separations. This review explores the detailed instrumental conditions required for sub-zeptomole, sub-picomolar detection limits. The key to achieving the best sensitivity is to use an excitation and emission volume that is matched to the separation system and that, simultaneously, will keep scattering and luminescence background to a minimum. We discuss how this is accomplished with confocal detection, 90 degrees on-capillary detection, and sheath-flow detection. It is shown that each of these methods have their advantages and disadvantages, but that all can be used to produce extremely sensitive detectors for capillary- or microchip-based separations. Analysis of these capabilities allows prediction of the optimal means of achieving ultrasensitive detection on microchips.

State estimation bias induced by optimization under uncertainty and error cost asymmetry is likely reflected in perception.

PubMed

Shimansky, Y P

2011-05-01

It is well known from numerous studies that perception can be significantly affected by intended action in many everyday situations, indicating that perception and related decision-making is not a simple, one-way sequence, but a complex iterative cognitive process. However, the underlying functional mechanisms are yet unclear. Based on an optimality approach, a quantitative computational model of one such mechanism has been developed in this study. It is assumed in the model that significant uncertainty about task-related parameters of the environment results in parameter estimation errors and an optimal control system should minimize the cost of such errors in terms of the optimality criterion. It is demonstrated that, if the cost of a parameter estimation error is significantly asymmetrical with respect to error direction, the tendency to minimize error cost creates a systematic deviation of the optimal parameter estimate from its maximum likelihood value. Consequently, optimization of parameter estimate and optimization of control action cannot be performed separately from each other under parameter uncertainty combined with asymmetry of estimation error cost, thus making the certainty equivalence principle non-applicable under those conditions. A hypothesis that not only the action, but also perception itself is biased by the above deviation of parameter estimate is supported by ample experimental evidence. The results provide important insights into the cognitive mechanisms of interaction between sensory perception and planning an action under realistic conditions. Implications for understanding related functional mechanisms of optimal control in the CNS are discussed.

Shape optimization of pulsatile ventricular assist devices using FSI to minimize thrombotic risk

NASA Astrophysics Data System (ADS)

Long, C. C.; Marsden, A. L.; Bazilevs, Y.

2014-10-01

In this paper we perform shape optimization of a pediatric pulsatile ventricular assist device (PVAD). The device simulation is carried out using fluid-structure interaction (FSI) modeling techniques within a computational framework that combines FEM for fluid mechanics and isogeometric analysis for structural mechanics modeling. The PVAD FSI simulations are performed under realistic conditions (i.e., flow speeds, pressure levels, boundary conditions, etc.), and account for the interaction of air, blood, and a thin structural membrane separating the two fluid subdomains. The shape optimization study is designed to reduce thrombotic risk, a major clinical problem in PVADs. Thrombotic risk is quantified in terms of particle residence time in the device blood chamber. Methods to compute particle residence time in the context of moving spatial domains are presented in a companion paper published in the same issue (Comput Mech, doi: 10.1007/s00466-013-0931-y, 2013). The surrogate management framework, a derivative-free pattern search optimization method that relies on surrogates for increased efficiency, is employed in this work. For the optimization study shown here, particle residence time is used to define a suitable cost or objective function, while four adjustable design optimization parameters are used to define the device geometry. The FSI-based optimization framework is implemented in a parallel computing environment, and deployed with minimal user intervention. Using five SEARCH/ POLL steps the optimization scheme identifies a PVAD design with significantly better throughput efficiency than the original device.

Application of modern control theory to scheduling and path-stretching maneuvers of aircraft in the near terminal area

NASA Technical Reports Server (NTRS)

Athans, M.

1974-01-01

A design concept of the dynamic control of aircraft in the near terminal area is discussed. An arbitrary set of nominal air routes, with possible multiple merging points, all leading to a single runway, is considered. The system allows for the automated determination of acceleration/deceleration of aircraft along the nominal air routes, as well as for the automated determination of path-stretching delay maneuvers. In addition to normal operating conditions, the system accommodates: (1) variable commanded separations over the outer marker to allow for takeoffs and between successive landings and (2) emergency conditions under which aircraft in distress have priority. The system design is based on a combination of three distinct optimal control problems involving a standard linear-quadratic problem, a parameter optimization problem, and a minimum-time rendezvous problem.

Regenerative Life Support Systems Test Bed performance - Lettuce crop characterization

NASA Technical Reports Server (NTRS)

Barta, Daniel J.; Edeen, Marybeth A.; Eckhardt, Bradley D.

1992-01-01

System performance in terms of human life support requirements was evaluated for two crops of lettuce (Lactuca sative cv. Waldmann's Green) grown in the Regenerative Life Support Systems Test Bed. Each crop, grown in separate pots under identical environmental and cultural conditions, was irrigated with half-strength Hoagland's nutrient solution, with the frequency of irrigation being increased as the crop aged over the 30-day crop tests. Averaging over both crop tests, the test bed met the requirements of 2.1 person-days of oxygen production, 2.4 person-days of CO2 removal, and 129 person-days of potential potable water production. Gains in the mass of water and O2 produced and CO2 removed could be achieved by optimizing environmental conditions to increase plant growth rate and by optimizing cultural management methods.

Analysis of separation test for automatic brake adjuster based on linear radon transformation

NASA Astrophysics Data System (ADS)

Luo, Zai; Jiang, Wensong; Guo, Bin; Fan, Weijun; Lu, Yi

2015-01-01

The linear Radon transformation is applied to extract inflection points for online test system under the noise conditions. The linear Radon transformation has a strong ability of anti-noise and anti-interference by fitting the online test curve in several parts, which makes it easy to handle consecutive inflection points. We applied the linear Radon transformation to the separation test system to solve the separating clearance of automatic brake adjuster. The experimental results show that the feature point extraction error of the gradient maximum optimal method is approximately equal to ±0.100, while the feature point extraction error of linear Radon transformation method can reach to ±0.010, which has a lower error than the former one. In addition, the linear Radon transformation is robust.

Determination of foodborne pathogenic bacteria by multiplex PCR-microchip capillary electrophoresis with genetic algorithm-support vector regression optimization.

PubMed

Li, Yongxin; Li, Yuanqian; Zheng, Bo; Qu, Lingli; Li, Can

2009-06-08

A rapid and sensitive method based on microchip capillary electrophoresis with condition optimization of genetic algorithm-support vector regression (GA-SVR) was developed and applied to simultaneous analysis of multiplex PCR products of four foodborne pathogenic bacteria. Four pairs of oligonucleotide primers were designed to exclusively amplify the targeted gene of Vibrio parahemolyticus, Salmonella, Escherichia coli (E. coli) O157:H7, Shigella and the quadruplex PCR parameters were optimized. At the same time, GA-SVR was employed to optimize the separation conditions of DNA fragments in microchip capillary electrophoresis. The proposed method was applied to simultaneously detect the multiplex PCR products of four foodborne pathogenic bacteria under the optimal conditions within 8 min. The levels of detection were as low as 1.2 x 10(2) CFU mL(-1) of Vibrio parahemolyticus, 2.9 x 10(2) CFU mL(-1) of Salmonella, 8.7 x 10(1) CFU mL(-1) of E. coli O157:H7 and 5.2 x 10(1) CFU mL(-1) of Shigella, respectively. The relative standard deviation of migration time was in the range of 0.74-2.09%. The results demonstrated that the good resolution and less analytical time were achieved due to the application of the multivariate strategy. This study offers an efficient alternative to routine foodborne pathogenic bacteria detection in a fast, reliable, and sensitive way.

Optimization of bump and blowing to control the flow through a transonic compressor blade cascade

NASA Astrophysics Data System (ADS)

Mazaheri, K.; Khatibirad, S.

2018-03-01

Shock control bump (SCB) and blowing are two flow control methods, used here to improve the aerodynamic performance of transonic compressors. Both methods are applied to a NASA rotor 67 blade section and are optimized to minimize the total pressure loss. A continuous adjoint algorithm is used for multi-point optimization of a SCB to improve the aerodynamic performance of the rotor blade section, for a range of operational conditions around its design point. A multi-point and two single-point optimizations are performed in the design and off-design conditions. It is shown that the single-point optimized shapes have the best performance for their respective operating conditions, but the multi-point one has an overall better performance over the whole operating range. An analysis is given regarding how similarly both single- and multi-point optimized SCBs change the wave structure between blade sections resulting in a more favorable flow pattern. Interactions of the SCB with the boundary layer and the wave structure, and its effects on the separation regions are also studied. We have also introduced the concept of blowing for control of shock wave and boundary-layer interaction. A geometrical model is introduced, and the geometrical and physical parameters of blowing are optimized at the design point. The performance improvements of blowing are compared with the SCB. The physical interactions of SCB with the boundary layer and the shock wave are analyzed. The effects of SCB on the wave structure in the flow domain outside the boundary-layer region are investigated. It is shown that the effects of the blowing mechanism are very similar to the SCB.

Comprehensive Optimization of LC-MS Metabolomics Methods Using Design of Experiments (COLMeD).

PubMed

Rhoades, Seth D; Weljie, Aalim M

2016-12-01

Both reverse-phase and HILIC chemistries are deployed for liquid-chromatography mass spectrometry (LC-MS) metabolomics analyses, however HILIC methods lag behind reverse-phase methods in reproducibility and versatility. Comprehensive metabolomics analysis is additionally complicated by the physiochemical diversity of metabolites and array of tunable analytical parameters. Our aim was to rationally and efficiently design complementary HILIC-based polar metabolomics methods on multiple instruments using Design of Experiments (DoE). We iteratively tuned LC and MS conditions on ion-switching triple quadrupole (QqQ) and quadrupole-time-of-flight (qTOF) mass spectrometers through multiple rounds of a workflow we term COLMeD (Comprehensive optimization of LC-MS metabolomics methods using design of experiments). Multivariate statistical analysis guided our decision process in the method optimizations. LC-MS/MS tuning for the QqQ method on serum metabolites yielded a median response increase of 161.5% (p<0.0001) over initial conditions with a 13.3% increase in metabolite coverage. The COLMeD output was benchmarked against two widely used polar metabolomics methods, demonstrating total ion current increases of 105.8% and 57.3%, with median metabolite response increases of 106.1% and 10.3% (p<0.0001 and p<0.05 respectively). For our optimized qTOF method, 22 solvent systems were compared on a standard mix of physiochemically diverse metabolites, followed by COLMeD optimization, yielding a median 29.8% response increase (p<0.0001) over initial conditions. The COLMeD process elucidated response tradeoffs, facilitating improved chromatography and MS response without compromising separation of isobars. COLMeD is efficient, requiring no more than 20 injections in a given DoE round, and flexible, capable of class-specific optimization as demonstrated through acylcarnitine optimization within the QqQ method.

Comprehensive Optimization of LC-MS Metabolomics Methods Using Design of Experiments (COLMeD)

PubMed Central

Rhoades, Seth D.

2017-01-01

Introduction Both reverse-phase and HILIC chemistries are deployed for liquid-chromatography mass spectrometry (LC-MS) metabolomics analyses, however HILIC methods lag behind reverse-phase methods in reproducibility and versatility. Comprehensive metabolomics analysis is additionally complicated by the physiochemical diversity of metabolites and array of tunable analytical parameters. Objective Our aim was to rationally and efficiently design complementary HILIC-based polar metabolomics methods on multiple instruments using Design of Experiments (DoE). Methods We iteratively tuned LC and MS conditions on ion-switching triple quadrupole (QqQ) and quadrupole-time-of-flight (qTOF) mass spectrometers through multiple rounds of a workflow we term COLMeD (Comprehensive optimization of LC-MS metabolomics methods using design of experiments). Multivariate statistical analysis guided our decision process in the method optimizations. Results LC-MS/MS tuning for the QqQ method on serum metabolites yielded a median response increase of 161.5% (p<0.0001) over initial conditions with a 13.3% increase in metabolite coverage. The COLMeD output was benchmarked against two widely used polar metabolomics methods, demonstrating total ion current increases of 105.8% and 57.3%, with median metabolite response increases of 106.1% and 10.3% (p<0.0001 and p<0.05 respectively). For our optimized qTOF method, 22 solvent systems were compared on a standard mix of physiochemically diverse metabolites, followed by COLMeD optimization, yielding a median 29.8% response increase (p<0.0001) over initial conditions. Conclusions The COLMeD process elucidated response tradeoffs, facilitating improved chromatography and MS response without compromising separation of isobars. COLMeD is efficient, requiring no more than 20 injections in a given DoE round, and flexible, capable of class-specific optimization as demonstrated through acylcarnitine optimization within the QqQ method. PMID:28348510

Isolation, Separation, and Preconcentration of Biologically Active Compounds from Plant Matrices by Extraction Techniques.

PubMed

Raks, Victoria; Al-Suod, Hossam; Buszewski, Bogusław

2018-01-01

Development of efficient methods for isolation and separation of biologically active compounds remains an important challenge for researchers. Designing systems such as organomineral composite materials that allow extraction of a wide range of biologically active compounds, acting as broad-utility solid-phase extraction agents, remains an important and necessary task. Selective sorbents can be easily used for highly selective and reliable extraction of specific components present in complex matrices. Herein, state-of-the-art approaches for selective isolation, preconcentration, and separation of biologically active compounds from a range of matrices are discussed. Primary focus is given to novel extraction methods for some biologically active compounds including cyclic polyols, flavonoids, and oligosaccharides from plants. In addition, application of silica-, carbon-, and polymer-based solid-phase extraction adsorbents and membrane extraction for selective separation of these compounds is discussed. Potential separation process interactions are recommended; their understanding is of utmost importance for the creation of optimal conditions to extract biologically active compounds including those with estrogenic properties.

Application of phase-trafficking methods to natural products research.

PubMed

Araya, Juan J; Montenegro, Gloria; Mitscher, Lester A; Timmermann, Barbara N

2010-09-24

A novel simultaneous phase-trafficking approach using spatially separated solid-supported reagents for rapid separation of neutral, basic, and acidic compounds from organic plant extracts with minimum labor is reported. Acidic and basic ion-exchange resins were physically separated into individual sacks ("tea bags") for trapping basic and acidic compounds, respectively, leaving behind in solution neutral components of the natural mixtures. Trapped compounds were then recovered from solid phase by appropriate suspension in acidic or basic solutions. The feasibility of the proposed separation protocol was demonstrated and optimized with an "artificial mixture" of model compounds. In addition, the utility of this methodology was illustrated with the successful separation of the alkaloid skytanthine from Skytanthus acutus Meyen and the main catechins and caffeine from Camellia sinensis L. (Kuntze). This novel approach offers multiple advantages over traditional extraction methods, as it is not labor intensive, makes use of only small quantities of solvents, produces fractions in adequate quantities for biological assays, and can be easily adapted to field conditions for bioprospecting activities.

Application of Phase-Trafficking Methods to Natural Products Research

PubMed Central

Araya, Juan J.; Montenegro, Gloria; Mitscher, Lester A.; Timmermann, Barbara N.

2010-01-01

A novel simultaneous phase-trafficking approach using spatially separated solid-supported reagents (SSR) for rapid separation of neutral, basic, and acidic compounds from organic plant extracts with minimum labor is reported. Acidic and basic ion exchange resins were physically separated into individual sacks (“teabags”) for trapping basic and acidic compounds respectively, leaving behind in solution neutral components of the natural mixtures. Trapped compounds were then recovered from solid phase by appropriate suspension in acidic or basic solutions. The feasibility of the proposed separation protocol was demonstrated and optimized with an “artificial mixture” of model compounds. In addition, the utility of this methodology was illustrated with the successful separation of the alkaloid skytanthine from Skytanthus acutus Meyen and the main catechins and caffeine from Camellia sinensis L. (Kuntze). This novel approach offers multiple advantages over traditional extraction methods, as it is not labor intensive, makes use of only small quantities of solvents, produces fractions in adequate quantities for biological assays, and can be easily adapted to field conditions for bioprospecting activities. PMID:20704309

Novel beta-cyclodextrin derivative functionalized polymethacrylate-based monolithic columns for enantioselective separation of ibuprofen and naproxen enantiomers in capillary electrochromatography.

PubMed

Tian, Yun; Zhong, Cheng; Fu, Enqin; Zeng, Zhaorui

2009-02-06

A novel enantioselective polymethacrylate-based monolithic column for capillary electrochromatography was prepared by ring-opening reaction of epoxy groups from poly(glycidyl methacrylate-co-ethylene dimethacrylate) monolith with a novel beta-cyclodextrin derivative bearing 4-dimethylamino-1,8-naphthalimide functionalities. Conditions for the ring-opening reaction with respect to different reaction parameters were thoroughly optimized to obtain high electroosmotic flow, separation efficiency and enantioselectivity for the analytes. The nonaqueous mobile phase composition regarding acetonitrile-methanol ratio and the concentration of electrolyte were examined to manipulate the hydrophobic inclusion and anion-exchange interaction between the analytes and chiral stationary phase. It was observed that in addition to beta-cyclodextrin cavity, the electrostatic interaction exhibited pronounced influence on the enantioseparation of acidic analytes. Acidic enantiomers (ibuprofen and naproxen) could be separated with separation factor (alpha) values up to 1.08 and a maximum separation efficiency of 86000 plates/m could be achieved.

Planar differential mobility spectrometer as a pre-filter for atmospheric pressure ionization mass spectrometry

PubMed Central

Schneider, Bradley B.; Covey, Thomas R.; Coy, Stephen L.; Krylov, Evgeny V.

2010-01-01

Ion filters based on planar DMS can be integrated with the inlet configuration of most mass spectrometers, and are able to enhance the quality of mass analysis and quantitative accuracy by reducing chemical noise, and by pre-separating ions of similar mass. This paper is the first in a series of three papers describing the optimization of DMS / MS instrumentation. In this paper the important physical parameters of a planar DMS-MS interface including analyzer geometry, analyzer coupling to a mass spectrometer, and transport gas flow control are considered. The goal is to optimize ion transmission and transport efficiency, provide optimal and adjustable resolution, and produce stable operation under conditions of high sample contamination. We discuss the principles of DMS separations and highlight the theoretical underpinnings. The main differences between planar and cylindrical geometries are presented, including a discussion of the advantages and disadvantages of RF ion focusing. In addition, we present a description of optimization of the frequency and amplitude of the DMS fields for resolution and ion transmission, and a discussion of the influence and importance of ion residence time in DMS. We have constructed a mass spectrometer interface for planar geometries that takes advantage of atmospheric pressure gas dynamic principles, rather than ion focusing, to minimize ion losses from diffusion in the analyzer and to maximize total ion transport into the mass spectrometer. A variety of experimental results has been obtained that illustrate the performance of this type of interface, including tests of resistance to high contamination levels, and the separation of stereoisomers. In a subsequent publication the control of the chemical interactions that drive the separation process of a DMS / MS system will be considered. In a third publication we describe novel electronics designed to provide the high voltages asymmetric waveform fields (SV) required for these devices as well as the effects of different waveforms. PMID:21278836

Optimal Measurement Tasks and Their Physical Realizations

NASA Astrophysics Data System (ADS)

Yerokhin, Vadim

This thesis reflects works previously published by the author and materials hitherto unpublished on the subject of quantum information theory. Particularly, results in optimal discrimination, cloning, and separation of quantum states, and their relationships, are discussed. Our interest lies in the scenario where we are given one of two quantum states prepared with a known a-priori probability. We are given full information about the states and are assigned the task of performing an optimal measurement on the incoming state. Given that none of these tasks is in general possible to perform perfectly we must choose a figure of merit to optimize, and as we shall see there is always a trade-off between competing figures of merit, such as the likelihood of getting the desired result versus the quality of the result. For state discrimination the competing figures of merit are the success rate of the measurement, the errors involved, and the inconclusiveness. Similarly increasing the separation between states comes at a cost of less frequent successful applications of the separation protocol. For cloning, aside from successfully producing clones we are also interested in the fidelity of the clones compared to the original state, which is a measure of the quality of the clones. Because all quantum operations obey the same set of conditions for evolution one may expect similar restrictions on disparate measurement strategies, and our work shows a deep connection between all three branches, with cloning and separation asymptotically converging to state discrimination. Via Neumark's theorem, our description of these unitary processes can be implemented using single-photon interferometry with linear optical devices. Amazingly any quantum mechanical evolution may be decomposed as an experiment involving only lasers, beamsplitters, phase-shifters and mirrors. Such readily available tools allow for verification of the aforementioned protocols and we build upon existing results to derive explicit setups that the experimentalist may build.

Preparative isolation and purification of five flavonoid glycosides and one benzophenone galloyl glycoside from Psidium guajava by high-speed counter-current chromatography (HSCCC).

PubMed

Zhu, Yindi; Liu, Yue; Zhan, Ying; Liu, Lin; Xu, Yajuan; Xu, Tunhai; Liu, Tonghua

2013-12-16

Psidium guajava leaves have a diverse phytochemical composition including flavonoids, phenolics, meroterpenoids and triterpenes, responsible for the biological activities of the medicinal parts. In particular, flavonol glycosides show beneficial effects on type II diabetes mellitus. A simple and efficient HSCCC method has been developed for the preparative separation of five flavonoid glycosides and one diphenylmethane glycoside from P. guajava. A solvent system composed of n-hexane-ethyl acetate-methanol-water (0.7:4:0.8:4, v/v/v/v) was optimized for the separation. The upper phase was used as the stationary phase, and the lower phase was used as the mobile phase. Under the optimized conditions, hyperoside (15.3 mg), isoquercitrin (21.1 mg), reynoutrin (65.2 mg), quercetin-3-O-β-D-arabinopyranoside (71.7 mg), quercetin-3-O-α-L-arabinofuranoside (105.6 mg) and 2,4,6-trihydroxy-3,5-dimethylbenzophenone 4-O-(6''-O-galloyl)-β-D-glucopyranoside (98.4 mg) were separated from crude sample (19.8 g). The structures of all the isolates were identified by ESI-MS, 1H- and 13C-NMR analyses and their purities (>95%) were determined using HPLC.

Optimization of Reversed-Phase Peptide Liquid Chromatography Ultraviolet Mass Spectrometry Analyses Using an Automated Blending Methodology

PubMed Central

Chakraborty, Asish B.; Berger, Scott J.

2005-01-01

The balance between chromatographic performance and mass spectrometric response has been evaluated using an automated series of experiments where separations are produced by the real-time automated blending of water with organic and acidic modifiers. In this work, the concentration effects of two acidic modifiers (formic acid and trifluoroacetic acid) were studied on the separation selectivity, ultraviolet, and mass spectrometry detector response, using a complex peptide mixture. Peptide retention selectivity differences were apparent between the two modifiers, and under the conditions studied, trifluoroacetic acid produced slightly narrower (more concentrated) peaks, but significantly higher electrospray mass spectrometry suppression. Trifluoroacetic acid suppression of electrospray signal and influence on peptide retention and selectivity was dominant when mixtures of the two modifiers were analyzed. Our experimental results indicate that in analyses where the analyzed components are roughly equimolar (e.g., a peptide map of a recombinant protein), the selectivity of peptide separations can be optimized by choice and concentration of acidic modifier, without compromising the ability to obtain effective sequence coverage of a protein. In some cases, these selectivity differences were explored further, and a rational basis for differentiating acidic modifier effects from the underlying peptide sequences is described. PMID:16522853

Simultaneous determination of multiclass preservatives including isothiazolinones and benzophenone-type UV filters in household and personal care products by micellar electrokinetic chromatography.

PubMed

Lopez-Gazpio, Josu; Garcia-Arrona, Rosa; Millán, Esmeralda

2015-04-01

In this work, a simple and reliable micellar electrokinetic chromatography method for the separation and quantification of 14 preservatives, including isothiazolinones, and two benzophenone-type UV filters in household, cosmetic and personal care products was developed. The selected priority compounds are widely used as ingredients in many personal care products, and are included in the European Regulation concerning cosmetic products. The electrophoretic separation parameters were optimized by means of a modified chromatographic response function in combination with an experimental design, namely a central composite design. After optimization of experimental conditions, the BGE selected for the separation of the targets consisted of 60 mM SDS, 18 mM sodium tetraborate, pH 9.4 and 10% v/v methanol. The MEKC method was checked in terms of linearity, LODs and quantification, repeatability, intermediate precision, and accuracy, providing appropriate values (i.e. R(2) ≥ 0.992, repeatability RSD values ˂9%, and accuracy 90-115%). Applicability of the validated method was successfully assessed by quantifying preservatives and UV filters in commercial consumer products. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Phospholipid hydrolysis in a pharmaceutical emulsion assessed by physicochemical parameters and a new analytical method.

PubMed

Rabinovich-Guilatt, Laura; Dubernet, Catherine; Gaudin, Karen; Lambert, Gregory; Couvreur, Patrick; Chaminade, Pierre

2005-09-01

The aim of this work was to develop a simple high-performance liquid chromatography (HPLC) technique with evaporative light scattering detection (ELSD) for the separation and quantification of the major phospholipid (PL) and lysophospholipid (LPL) classes contained in a pharmaceutical phospholipid-based emulsion. In the established method, phosphatidylcholine (PC), phosphatidylethanolamine (PE), sphingomyeline (SM), lysophosphatidylcholine (LPC) and lysophosphatidylethanolamine (LPE) were separated with a PVA-Sil stationary phase and a binary gradient from pure chloroform to methanol:water (94:6 v/v) at 3.4%/min. The ELSD detection was enhanced using 0.1% triethylamine and formic acid in each gradient mobile phases. Factors such as stationary phase and ELSD drift tube temperature were optimized, concluding in optimal temperatures of 25 degrees C for separation and 50 degrees C for evaporation. This HPLC-ELSD method was then applied to a PL-emulsion exposed to autoclaving and accelerated thermal conditions at 50 degrees C. Hydrolysis of PC and PE followed first-order kinetics, representing only 45% of the total lipid mass after 3 months. The chemical stability was correlated to commonly measured formulation physical and physico-chemical parameters such as droplet size, emulsion pH and zeta-potential.

Determination of artificial sweeteners by capillary electrophoresis with contactless conductivity detection optimized by hydrodynamic pumping.

PubMed

Stojkovic, Marko; Mai, Thanh Duc; Hauser, Peter C

2013-07-17

The common sweeteners aspartame, cyclamate, saccharin and acesulfame K were determined by capillary electrophoresis with contactless conductivity detection. In order to obtain the best compromise between separation efficiency and analysis time hydrodynamic pumping was imposed during the electrophoresis run employing a sequential injection manifold based on a syringe pump. Band broadening was avoided by using capillaries of a narrow 10 μm internal diameter. The analyses were carried out in an aqueous running buffer consisting of 150 mM 2-(cyclohexylamino)ethanesulfonic acid and 400 mM tris(hydroxymethyl)aminomethane at pH 9.1 in order to render all analytes in the fully deprotonated anionic form. The use of surface modification to eliminate or reverse the electroosmotic flow was not necessary due to the superimposed bulk flow. The use of hydrodynamic pumping allowed easy optimization, either for fast separations (80s) or low detection limits (6.5 μmol L(-1), 5.0 μmol L(-1), 4.0 μmol L(-1) and 3.8 μmol L(-1) for aspartame, cyclamate, saccharin and acesulfame K respectively, at a separation time of 190 s). The conditions for fast separations not only led to higher limits of detection but also to a narrower dynamic range. However, the settings can be changed readily between separations if needed. The four compounds were determined successfully in food samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Improved HPLC method with the aid of chemometric strategy: determination of loxoprofen in pharmaceutical formulation.

PubMed

Venkatesan, P; Janardhanan, V Sree; Muralidharan, C; Valliappan, K

2012-06-01

Loxoprofen belongs to a class of Nonsteroidal anti-inflammatory drug acts by inhibiting isoforms of cyclo-oxygenase 1 and 2. In this study an improved RP-HPLC method was developed for the quantification of loxoprofen in pharmaceutical dosage form. For that purpose an experimental design approach was employed. Factors-independent variables (organic modifier, pH of the mobile phase and flow rate) were extracted from the preliminary study and as dependent variables three responses (loxoprofen retention factor, resolution between loxoprofen probenecid and retention time of probenecid) were selected. For the improvement of method development and optimization step, Derringer's desirability function was applied to simultaneously optimize the chosen three responses. The procedure allowed deduction of optimal conditions and the predicted optimum was acetonitrile: water (53:47, v/v), pH of the mobile phase adjusted at to 2.9 with ortho phosphoric acid. The separation was achieved in less than 4minutes. The method was applied in the quality control of commercial tablets. The method showed good agreement between the experimental data and predictive value throughout the studied parameter space. The optimized assay condition was validated according to International conference on harmonisation guidelines to confirm specificity, linearity, accuracy and precision.

Optimization of Crew Shielding Requirement in Reactor-Powered Lunar Surface Missions

NASA Technical Reports Server (NTRS)

Barghouty, Abdulnasser F.

2007-01-01

On the surface of the moon -and not only during heightened solar activities- the radiation environment As such that crew protection will be required for missions lasting in excess of six months. This study focuses on estimating the optimized crew shielding requirement for lunar surface missions with a nuclear option. Simple, transport-simulation based dose-depth relations of the three (galactic, solar, and fission) radiation sources am employed in a 1-dimensional optimization scheme. The scheme is developed to estimate the total required mass of lunar-regolith separating reactor from crew. The scheme was applied to both solar maximum and minimum conditions. It is shown that savings of up to 30% in regolith mass can be realized. It is argued, however, that inherent variation and uncertainty -mainly in lunar regolith attenuation properties in addition to the radiation quality factor- can easily defeat this and similar optimization schemes.

Optimization of Crew Shielding Requirement in Reactor-Powered Lunar Surface Missions

NASA Technical Reports Server (NTRS)

Barghouty, A. F.

2007-01-01

On the surface of the moon and not only during heightened solar activities the radiation environment is such that crew protection will be required for missions lasting in excess of six months. This study focuses on estimating the optimized crew shielding requirement for lunar surface missions with a nuclear option. Simple, transport-simulation based dose-depth relations of the three radiation sources (galactic, solar, and fission) are employed in a one-dimensional optimization scheme. The scheme is developed to estimate the total required mass of lunar regolith separating reactor from crew. The scheme was applied to both solar maximum and minimum conditions. It is shown that savings of up to 30% in regolith mass can be realized. It is argued, however, that inherent variation and uncertainty mainly in lunar regolith attenuation properties in addition to the radiation quality factor can easily defeat this and similar optimization schemes.

Lentil and chickpea protein-stabilized emulsions: optimization of emulsion formulation.

PubMed

Can Karaca, Asli; Nickerson, Michael T; Low, Nicholas H

2011-12-28

Chickpea and lentil protein-stabilized emulsions were optimized with regard to pH (3.0-8.0), protein concentration (1.1-4.1% w/w), and oil content (20-40%) for their ability to form and stabilize oil-in-water emulsions using response surface methodology. Specifically, creaming stability, droplet size, and droplet charge were assessed. Optimum conditions for minimal creaming (no serum separation after 24 h), small droplet size (<2 μm), and high net droplet charge (absolute value of ZP > 40 mV) were identified as 4.1% protein, 40% oil, and pH 3.0 or 8.0, regardless of the plant protein used for emulsion preparation.

Novel plasma source for safe beryllium spectral line studies in the presence of beryllium dust

NASA Astrophysics Data System (ADS)

Stankov, B. D.; Vinić, M.; Gavrilović Božović, M. R.; Ivković, M.

2018-05-01

Plasma source for beryllium spectral line studies in the presence of beryllium dust particles was realised. The guideline during construction was to prevent exposure to formed dust, considering the toxicity of beryllium. Plasma source characterization through determination of optimal working conditions is described. The necessary conditions for Be spectral line appearance and optimal conditions for line shape measurements are found. It is proven experimentally that under these conditions dust appears coincidently with the second current maximum. The electron density measured after discharge current maximum is determined from the peak separation of the hydrogen Balmer beta spectral line, and the electron temperature is determined from the ratios of the relative intensities of Be spectral lines emitted from successive ionized stages of atoms. Maximum values of electron density and temperature are measured to be 9.3 × 1022 m-3 and 16 800 K, respectively. Construction details and testing of the BeO discharge tube in comparison with SiO2 and Al2O3 discharge tubes are also presented in this paper.

Gas Chromatograph Method Optimization Trade Study for RESOLVE: 20-meter Column v. 8-meter Column

NASA Technical Reports Server (NTRS)

Huz, Kateryna

2014-01-01

RESOLVE is the payload on a Class D mission, Resource Prospector, which will prospect for water and other volatile resources at a lunar pole. The RESOLVE payload's primary scientific purpose includes determining the presence of water on the moon in the lunar regolith. In order to detect the water, a gas chromatograph (GC) will be used in conjunction with a mass spectrometer (MS). The goal of the experiment was to compare two GC column lengths and recommend which would be best for RESOLVE's purposes. Throughout the experiment, an Inficon Fusion GC and an Inficon Micro GC 3000 were used. The Fusion had a 20m long column with 0.25mm internal diameter (Id). The Micro GC 3000 had an 8m long column with a 0.32mm Id. By varying the column temperature and column pressure while holding all other parameters constant, the ideal conditions for testing with each column length in their individual instrument configurations were determined. The criteria used for determining the optimal method parameters included (in no particular order) (1) quickest run time, (2) peak sharpness, and (3) peak separation. After testing numerous combinations of temperature and pressure, the parameters for each column length that resulted in the most optimal data given my three criteria were selected. The ideal temperature and pressure for the 20m column were 95 C and 50psig. At this temperature and pressure, the peaks were separated and the retention times were shorter compared to other combinations. The Inficon Micro GC 3000 operated better at lower temperature mainly due to the shorter 8m column. The optimal column temperature and pressure were 70 C and 30psig. The Inficon Micro GC 3000 8m column had worse separation than the Inficon Fusion 20m column, but was able to separate water within a shorter run time. Therefore, the most significant tradeoff between the two column lengths was peak separation of the sample versus run time. After performing several tests, it was concluded that better detection via good peak separation with a longer run time is a better asset than moderate peak separation with a shorter run time. Even given that RESOLVE is highly interested in water and that mission timeline is of significant importance given the short seven-to-ten-day mission timeline, worse detection with an 8m column may lead to overlooking other substances existing on the moon that could advance planetary science. Thus, I recommend the 20m column. However, if mission timeline and water separation are deemed the highest priority, the 8m column should be selected due to its ability to separate water within a shorter run time than the 20m column.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wilden, Andreas; Lumetta, Gregg J.; Sadowski, Fabian

A solvent extraction system has been developed for separating trivalent actinides from lanthanides. This “Advanced TALSPEAK” system uses 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester to extract the lanthanides into a n-dodecane-based solvent phase, while the actinides are retained in a citrate-buffered aqueous phase by complexation to N-(2-hydroxyethyl)ethylenediamine-N,N',N'-triacetic acid. Batch distribution measurements indicate that the separation of americium from the light lanthanides decreases as the pH decreases. For example, the separation factor between La and Am increases from 2.5 at pH 2.0 to 19.3 at pH 3.0. However, previous investigations indicated that the extraction rates for the heavier lanthanides decrease with increasing pH.more » So, a balance between these two competing effects is required. An aqueous phase in which the pH was set at 2.6 was chosen for further process development because this offered optimal separation, with a minimum separation factor of ~8.4, based on the separation between La and Am. Centrifugal contactor single-stage efficiencies were measured to characterize the performance of the system under flow conditions.« less

Preparative HSCCC isolation of phloroglucinolysis products from grape seed polymeric proanthocyanidins as new powerful antioxidants.

PubMed

Zhang, Shuting; Cui, Yan; Li, Lingxi; Li, Yuanyuan; Zhou, Peiyu; Luo, Lanxin; Sun, Baoshan

2015-12-01

Polymeric proanthocyanidins isolated from a grape seed phenolic extract were hydrolysed in the presence of phloroglucinol into monomer catechins and their nucleophile derivatives. Each of the phloroglucinolysis products was successfully separated and isolated in large amount by semi-preparative HSCCC technique under the optimized conditions based on a selection of suitable solvent system. The optimized solvent system consisted of n-hexane-ethyl acetate-water (1:80:80, v/v/v) with a combination of head-tail and tail-head elution modes. By only one-step HSCCC separation, the purity of each obtained phloroglucinolysis product, including monomer catechins and their nucleophile derivatives was above 76%, verified by UPLC. The structures of these products were tentatively identified by UPLC based on their retention time and further confirmed by MS and (1)H NMR analysis. Furthermore, by DPPH, ABTS and FRAP assays, it was verified that all these phloroglucinolysis products possessed strong antioxidant activities, being catechin-nucleophile derivatives more powerful than free catechins. Copyright © 2015 Elsevier Ltd. All rights reserved.

Development and validation of a simple high-performance liquid chromatography analytical method for simultaneous determination of phytosterols, cholesterol and squalene in parenteral lipid emulsions.

PubMed

Novak, Ana; Gutiérrez-Zamora, Mercè; Domenech, Lluís; Suñé-Negre, Josep M; Miñarro, Montserrat; García-Montoya, Encarna; Llop, Josep M; Ticó, Josep R; Pérez-Lozano, Pilar

2018-02-01

A simple analytical method for simultaneous determination of phytosterols, cholesterol and squalene in lipid emulsions was developed owing to increased interest in their clinical effects. Method development was based on commonly used stationary (C 18 , C 8 and phenyl) and mobile phases (mixtures of acetonitrile, methanol and water) under isocratic conditions. Differences in stationary phases resulted in peak overlapping or coelution of different peaks. The best separation of all analyzed compounds was achieved on Zorbax Eclipse XDB C 8 (150 × 4.6 mm, 5 μm; Agilent) and ACN-H 2 O-MeOH, 80:19.5:0.5 (v/v/v). In order to achieve a shorter time of analysis, the method was further optimized and gradient separation was established. The optimized analytical method was validated and tested for routine use in lipid emulsion analyses. Copyright © 2017 John Wiley & Sons, Ltd.

Optimization of separation and online sample concentration of N,N-dimethyltryptamine and related compounds using MEKC.

PubMed

Wang, Man-Juing; Tsai, Chih-Hsin; Hsu, Wei-Ya; Liu, Ju-Tsung; Lin, Cheng-Huang

2009-02-01

The optimal separation conditions and online sample concentration for N,N-dimethyltryptamine (DMT) and related compounds, including alpha-methyltryptamine (AMT), 5-methoxy-AMT (5-MeO-AMT), N,N-diethyltryptamine (DET), N,N-dipropyltryptamine (DPT), N,N-dibutyltryptamine (DBT), N,N-diisopropyltryptamine (DiPT), 5-methoxy-DMT (5-MeO-DMT), and 5-methoxy-N,N-DiPT (5-MeO-DiPT), using micellar EKC (MEKC) with UV-absorbance detection are described. The LODs (S/N = 3) for MEKC ranged from 1.0 1.8 microg/mL. Use of online sample concentration methods, including sweeping-MEKC and cation-selective exhaustive injection-sweep-MEKC (CSEI-sweep-MEKC) improved the LODs to 2.2 8.0 ng/mL and 1.3 2.7 ng/mL, respectively. In addition, the order of migration of the nine tryptamines was investigated. A urine sample, obtained by spiking urine collected from a human volunteer with DMT, was also successfully examined.

Integrating uniform design and response surface methodology to optimize thiacloprid suspension

PubMed Central

Li, Bei-xing; Wang, Wei-chang; Zhang, Xian-peng; Zhang, Da-xia; Mu, Wei; Liu, Feng

2017-01-01

A model 25% suspension concentrate (SC) of thiacloprid was adopted to evaluate an integrative approach of uniform design and response surface methodology. Tersperse2700, PE1601, xanthan gum and veegum were the four experimental factors, and the aqueous separation ratio and viscosity were the two dependent variables. Linear and quadratic polynomial models of stepwise regression and partial least squares were adopted to test the fit of the experimental data. Verification tests revealed satisfactory agreement between the experimental and predicted data. The measured values for the aqueous separation ratio and viscosity were 3.45% and 278.8 mPa·s, respectively, and the relative errors of the predicted values were 9.57% and 2.65%, respectively (prepared under the proposed conditions). Comprehensive benefits could also be obtained by appropriately adjusting the amount of certain adjuvants based on practical requirements. Integrating uniform design and response surface methodology is an effective strategy for optimizing SC formulas. PMID:28383036

Core-Shell in Liquid Chromatography: Application for Determining Sulphonamides in Feed and Meat Using Conventional Chromatographic Systems

PubMed Central

Armentano, Antonio; Summa, Simona; Magro, Sonia Lo; D’Antini, Pasquale; Palermo, Carmen; Muscarella, Marilena

2016-01-01

A C18 column packed with core-shell particles was used for the chromatographic separation of sulphonamides in feed and meat by a conventional high performance liquid chromatography system coupled with a diode array detector. Two analytical methods, already used in our laboratory, have been modified without any changes in the extraction and clean-up steps and in the liquid chromatography instrumentation. Chromatographic conditions applied on a traditional 5-µm column have been optimized on a column packed with 2.6 µm core-shell particles. A binary mobile phase [acetate buffer solution at pH 4.50 and a mixture of methanol acetonitrile 50: 50 (v/v)] was employed in gradient mode at the flow rate of 1.2 mL with an injection volume of 6 µL. These chromatographic conditions allow the separation of 13 sulphonamides with an entire run of 13 minutes. Preliminary studies have been carried out comparing blanks and spiked samples of feed and meat. A good resolution and the absence of interferences were achieved in chromatograms for both matrices. Since no change was made to the sample preparation, the optimized method does not require a complete revalidation and can be used to make routine analysis faster. PMID:28217560

Separation of Lead from Crude Antimony by Pyro-Refining Process with NaPO3 Addition

NASA Astrophysics Data System (ADS)

Ye, Longgang; Hu, Yuejie; Xia, Zhimei; Chen, Yongming

2016-06-01

The main purpose of this study was to separate lead from crude antimony through an oxidation pyro-refining process and by using sodium metaphosphate as a lead elimination reagent. The process parameters that will affect the refining results were optimized experimentally under controlled conditions, such as the sodium metaphosphate charging dosage, the refining temperature and duration, and the air flow rate, to determine their effect on the lead content in refined antimony and the lead removal rate. A minimum lead content of 0.0522 wt.% and a 98.6% lead removal rate were obtained under the following optimal conditions: W_{{{NaPO}_{{3}} }} = 15% W Sb (where W represents weight), a refining temperature of 800°C, a refining time of 30 min, and an air flow rate of 3 L/min. X-ray diffractometry and scanning electron microscopy showed that high-purity antimony was obtained. The smelting operation is free from smoke or ammonia pollution when using monobasic sodium phosphate or ammonium dihydrogen phosphate as the lead elimination reagent. However, this refining process can also remove a certain amount of sulfur, cobalt, and silicon simultaneously, and smelting results also suggest that sodium metaphosphate can be used as a potential lead elimination reagent for bismuth and copper refining.

[Rapid determination of trace iodate using monolithic column ion-pair chromatography coupled with direct conductivity detection].

PubMed

Liu, Yuzhen; Yu, Hong; Li, Siwen

2011-10-01

A method was developed on a monolithic column for the fast determination of trace iodate (IO(3)- ) by ion-pair chromatography with direct conductivity detection. The analytes were separated using a mobile phase of tetrabutylammonium hydroxide (TBA)-phthalic acid-acetonitrile on a reversed-phase silica-based monolithic column. The effects of eluent, flow rate and column temperature on the retention of iodate were investigated. The optimized chromatographic conditions for the determination of the anion were as follows: 0. 25 mmol/L TBA-0. 18 mmol/L phthalic acid-3% acetonitrile (pH 5.5) as mobile phase, a flow rate of 4.0 mL/min and a column temperature of 30 degrees C. Under the optimal conditions, retention time of iodate was less than 0. 5 min and the baseline separation of iodate was achieved without any interference by other anions (Cl-, NO , SO4(2)-, I- ). The detection limit (S/N= 3) was 0.36 mg/L for IO(3)- . Relative standard deviation (RSD, n = 5) of chromatographic peak area and retention time were 0. 35% and 0. 28%, respectively. The proposed method was applied to the determination of trace iodate in iodized medicine. The spiked recovery of iodate was 96. 4%. The method is rapid, simple, accurate, reliable, and practical.

Time-Frequency Analysis of Rocket Nozzle Wall Pressures During Start-up Transients

NASA Technical Reports Server (NTRS)

Baars, Woutijn J.; Tinney, Charles E.; Ruf, Joseph H.

2011-01-01

Surveys of the fluctuating wall pressure were conducted on a sub-scale, thrust- optimized parabolic nozzle in order to develop a physical intuition for its Fourier-azimuthal mode behavior during fixed and transient start-up conditions. These unsteady signatures are driven by shock wave turbulent boundary layer interactions which depend on the nozzle pressure ratio and nozzle geometry. The focus however, is on the degree of similarity between the spectral footprints of these modes obtained from transient start-ups as opposed to a sequence of fixed nozzle pressure ratio conditions. For the latter, statistically converged spectra are computed using conventional Fourier analyses techniques, whereas the former are investigated by way of time-frequency analysis. The findings suggest that at low nozzle pressure ratios -- where the flow resides in a Free Shock Separation state -- strong spectral similarities occur between fixed and transient conditions. Conversely, at higher nozzle pressure ratios -- where the flow resides in Restricted Shock Separation -- stark differences are observed between the fixed and transient conditions and depends greatly on the ramping rate of the transient period. And so, it appears that an understanding of the dynamics during transient start-up conditions cannot be furnished by a way of fixed flow analysis.

Two optimal working regimes of the ”long” Iguasu gas centrifuge

NASA Astrophysics Data System (ADS)

Borman, V. D.; Bogovalov, S. V.; Borisevich, V. D.; Tronin, I. V.; Tronin, V. N.

2016-09-01

We argue on the basis of the results of optimization calculations that the dependence of the optimal separative power of the Iguasu gas centrifuge with 2 m rotor has two local maxima,corresponding pressures of p max1 = 35 mmHg and p max2 = 350 mmHg. The optimal separative power values in these maxima differ by the value of 0.6%. Low pressure maximum is caused by the thermal drive, whereas high pressure maximum is caused by both thermal and mechanical drives. High pressure maximum is located on wide ’’plateau” from p 1 = 200 mmHg to p 2 = 500 mmHg, where the optimal separative power changes in the range of 0.7%. In this way, Iguasu gas centrifuge has two optimal working regimes with different sets of working parameters and close slightly different values of the separative power. Calculations show that high pressure regime is less sensitive to the parameters change than low pressure one.

Chiral stationary phase optimized selectivity liquid chromatography: A strategy for the separation of chiral isomers.

PubMed

Hegade, Ravindra Suryakant; De Beer, Maarten; Lynen, Frederic

2017-09-15

Chiral Stationary-Phase Optimized Selectivity Liquid Chromatography (SOSLC) is proposed as a tool to optimally separate mixtures of enantiomers on a set of commercially available coupled chiral columns. This approach allows for the prediction of the separation profiles on any possible combination of the chiral stationary phases based on a limited number of preliminary analyses, followed by automated selection of the optimal column combination. Both the isocratic and gradient SOSLC approach were implemented for prediction of the retention times for a mixture of 4 chiral pairs on all possible combinations of the 5 commercial chiral columns. Predictions in isocratic and gradient mode were performed with a commercially available and with an in-house developed Microsoft visual basic algorithm, respectively. Optimal predictions in the isocratic mode required the coupling of 4 columns whereby relative deviations between the predicted and experimental retention times ranged between 2 and 7%. Gradient predictions led to the coupling of 3 chiral columns allowing baseline separation of all solutes, whereby differences between predictions and experiments ranged between 0 and 12%. The methodology is a novel tool allowing optimizing the separation of mixtures of optical isomers. Copyright © 2017 Elsevier B.V. All rights reserved.

Incorporating perceptual decision-making training into high-intensity interval training for Australian football umpires.

PubMed

Kittel, Aden; Elsworthy, Nathan; Spittle, Michael

2018-05-30

Existing methods for developing decision-making skill for Australian football umpires separate the physical and perceptual aspects of their performance. This study aimed to determine the efficacy of incorporating video-based decision-making training during high-intensity interval training sessions, specific for Australian football umpires. 20 amateur Australian football umpires volunteered to participate in a randomised control trial. Participants completed an 8-week training intervention in a conditioning only (CON; n=7), combined video-based training and conditioning (COM; n=7), or separated conditioning and video-based training (SEP; n=6) group. Preliminary and post-testing involved a Yo-Yo Intermittent Recovery Test (Yo-YoIR1), and 10x300m run test with an Australian football specific video-based decision-making task. Overall, changes in decision-making accuracy following the intervention were unclear between groups. SEP was possibly beneficial compared to COM in Yo-YoIR1 performance, whereas CON was likely beneficial compared to COM in 10x300m sprint performance. There was no additional benefit to completing video-based training, whether combined with, or separate to physical training, suggesting that this was not an optimal training method. For video-based training to be an effective decision-making tool, detailed feedback should be incorporated into training. It is recommended that longer conditioning and video-based training interventions be implemented to determine training effectiveness.

Simulation Tool for Dielectric Barrier Discharge Plasma Actuators

NASA Technical Reports Server (NTRS)

Likhanskii, Alexander

2014-01-01

Traditional approaches for active flow separation control using dielectric barrier discharge (DBD) plasma actuators are limited to relatively low speed flows and atmospheric conditions. This results in low feasibility of the DBDs for aerospace applications. For active flow control at turbine blades, fixed wings, and rotary wings and on hypersonic vehicles, DBD plasma actuators must perform at a wide range of conditions, including rarified flows and combustion mixtures. An efficient, comprehensive, physically based DBD simulation tool can optimize DBD plasma actuators for different operation conditions. Researchers are developing a DBD plasma actuator simulation tool for a wide range of ambient gas pressures. The tool will treat DBD using either kinetic, fluid, or hybrid models, depending on the DBD operational condition.

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

PubMed

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.

An ammonium sulfate/ethanol aqueous two-phase system combined with ultrasonication for the separation and purification of lithospermic acid B from Salvia miltiorrhiza Bunge.

PubMed

Guo, Y X; Han, J; Zhang, D Y; Wang, L H; Zhou, L L

2012-07-01

We studied the effect of ultrasonication extraction technology combined with ammonium sulfate/ethanol aqueous two-phase system (ATPS) for the separation of lithospermic acid B (LAB) from Salvia miltiorrhiza Bunge. According to the literature and preliminary studies, ammonium sulfate concentration, ethanol concentration, pH, ultrasonication power, ultrasonication time and the ratio of solvent-to-solid were investigated using a single factor design to identify the factors affecting separation. Taking into consideration a simultaneous increase in LAB recovery (R (%)) and partition coefficient (K), the best performance of the ATPS was obtained at 25°C and pH 2 using ammonium sulfate 22% (w/w) and ethanol 30% (w/w). To keep the solvent-to-solid ratio at 10, response surface methodology was used to find the optimal ultrasonication power and ultrasonication time. Quadratic models were predicted for LAB yield in the upper phase. Optimal conditions of 572.1 W ultrasonication power and 42.2 min produced a maximum yield of LAB of 42.16 mg g(-1) sample. There was no obvious degradation of LAB with ultrasound under the applied conditions, and the experimental yield of LAB was 42.49 mg g(-1) sample and the purity was 55.28% (w/w), which was much higher than that obtained using conventional extraction. The present study demonstrated that ultrasound coupled with aqueous two-phase systems is very efficient tool for the extraction and purification of LAB from Salvia miltiorrhiza Bunge. Copyright © 2011 Elsevier B.V. All rights reserved.

A stepwise recovery of metals from hybrid cathodes of spent Li-ion batteries with leaching-flotation-precipitation process

NASA Astrophysics Data System (ADS)

Huang, Yanfang; Han, Guihong; Liu, Jiongtian; Chai, Wencui; Wang, Wenjuan; Yang, Shuzhen; Su, Shengpeng

2016-09-01

The recovering of valuable metals in spent lithium-ion battery cathodes brings about economic and environmental benefits. A stepwise leaching-flotation-precipitation process is adopted to separate and recover Li/Fe/Mn from the mixed types of cathode materials (hybrid wastes of LiFePO4 and LiMn2O4). The optimal operating conditions for the stepwise recovery process are determined and analyzed by factorial design, thermodynamics calculation, XRD and SEM characterization in this study. First, Li/Fe/Mn ions are released from the cathode using HCl assisted with H2O2 in the acid leaching step. The leachability of metals follows the series Li > Fe > Mn in the acidic environment. Then Fe3+ ions are selectively floated and recovered as FeCl3 from the leachate in the flotation step. Finally, Mn2+/Mn3+ and Li+ ions are sequentially precipitated and separated as MnO2/Mn2O3 and Li3PO4 using saturated KMnO4 solution and hot saturated Na3PO4 solution, respectively. Under the optimized and advisable conditions, the total recovery of Li, Fe and Mn is respectively 80.93 ± 0.16%, 85.40 ± 0.12% and 81.02 ± 0.08%. The purity for lithium, ferrum and manganese compounds is respectively 99.32 ± 0.07%, 97.91 ± 0.05% and 98.73 ± 0.05%. This stepwise process could provide an alternative way for the effective separation and recovery of metal values from spent Li-ion battery cathodes in industry.

Aptamer-functionalized Fe3 O4 magnetic nanoparticles as a solid-phase extraction adsorbent for the selective extraction of berberine from Cortex phellodendri.

PubMed

Jiang, Ling-Feng; Chen, Bo-Cheng; Chen, Ben; Li, Xue-Jian; Liao, Hai-Lin; Zhang, Wen-Yan; Wu, Lin

2017-07-01

The extraction adsorbent was fabricated by immobilizing the highly specific recognition and binding of aptamer onto the surface of Fe 3 O 4 magnetic nanoparticles, which not only acted as recognition elements to recognize and capture the target molecule berberine from the extract of Cortex phellodendri, but also could favor the rapid separation and purification of the bound berberine by using an external magnet. The developed solid-phase extraction method in this work was useful for the selective extraction and determination of berberine in Cortex phellodendri extracts. Various conditions such as the amount of aptamer-functionalized Fe 3 O 4 magnetic nanoparticles, extraction time, temperature, pH value, Mg 2+ concentration, elution time and solvent were optimized for the solid-phase extraction of berberine. Under optimal conditions, the purity of berberine extracted from Cortex phellodendri was as high as 98.7% compared with that of 4.85% in the extract, indicating that aptamer-functionalized Fe 3 O 4 magnetic nanoparticles-based solid-phase extraction method was very effective for berberine enrichment and separation from a complex herb extract. The applicability and reliability of the developed solid-phase extraction method were demonstrated by separating berberine from nine different concentrations of one Cortex phellodendri extract. The relative recoveries of the spiked solutions of all the samples were between 95.4 and 111.3%, with relative standard deviations ranging between 0.57 and 1.85%. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of underivatized amino acids to evaluate quality of beer by capillary electrophoresis with online sweeping technique.

PubMed

Luo, Tian; Ke, Jing; Xie, Yunfei; Dong, Yuming

2017-10-01

Capillary electrophoresis (CE) with ultraviolet detection was applied to determine underivatized amino acids in beer, based on the coordination interaction of copper ions and amino acids. An online sweeping technique was combined with CE to improve detection sensitivity. Using the United Nations Food Agriculture Organization/World Health Organization model of essential amino acid pattern and flavor of amino acids, the quality and taste in three kinds of beer were evaluated. It was found that Beer2 had higher quality than the other two kinds and the content of phenylalanine, proline, serine, and isoleucine was relatively large in all three kinds of beers with a great influence on beer flavor. Optimal conditions for separation were as follows: 50mM CuSO 4 at pH 4.40 as buffer; total length of fused silica capillary, 73 cm; effective length, 65 cm; separation voltage, 22.5 kV; and optimized sweeping condition, 70 seconds. In the appropriate range, linearity (r 2  > 0.9989), precision with a relative standard deviation < 8.05% (n = 5), limits of detection (0.13-0.25 μg/mL), limit of quantification (0.43-0.83 μg/mL), and recovery (80.5-115.8%) were measured. This method was shown to be applicable to the separation of amino acids in beer and to perform quantitative analysis directly without derivatization for the first time. Copyright © 2017. Published by Elsevier B.V.

Optimization of separation and detection conditions for the multiresidue analysis of pesticides in grapes by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry.

PubMed

Banerjee, Kaushik; Patil, Sangram H; Dasgupta, Soma; Oulkar, Dasharath P; Patil, Shubhangi B; Savant, Rahul; Adsule, Pandurang G

2008-05-09

A comprehensive GCxGC-TOFMS method was optimized for multiresidue analysis of pesticides using a combination of a non-polar (RTX-5MS, 10 m x 0.18 mm x 0.2 microm) and a polar capillary column (TR-50MS, 1 m x 0.1 mm x 0.1 microm), connected in series through a dual stage thermal modulator. The method resolved the co-elution problems as observed in full scan one-dimensional GC-MS analysis and allowed chromatographic separation of 51 pesticides within 24 min run time with library-searchable mass spectrometric confirmation. Four pesticides, viz. chlorpyrifos-methyl, vinclozoline, parathion-methyl and heptachlor could be baseline separated on GCxGC, which were otherwise closely eluting and interfering each other's detection in 1D GC-MS run. Similarly, it could be possible to separate myclobutanil, buprofezin, flusilazole and oxyfluorfen on GCxGC. Although in 1D GC-MS, these closely eluting compounds could be identified through deconvolution algorithm and 'peak-find' option of the Chromatof software but the spectral purity significantly improved on GCxGC analysis. Thorough optimization was accomplished for the oven temperature programming, ion source temperature and GCxGC parameters like modulation period, duration of hot pulses, modulation-offset temperature, acquisition rate, etc. to achieve best possible separation of the test compounds. The limit of detection significantly improved by 2-12 times on GCxGC-TOFMS against GC-TOFMS because of sharper and narrower peak shapes. The method was tested for grape matrix after preparing the samples using previously described method and recoveries of the entire test pesticides were within 70-110% at 10 ng/g level of fortification. GCxGC-TOFMS was found to be an excellent technique for library-based screening of pesticides with high accuracy and sensitivity.

Arsenic Speciation of Waters from the Aegean Region, Turkey by Hydride Generation: Atomic Absorption Spectrometry.

PubMed

Çiftçi, Tülin Deniz; Henden, Emur

2016-08-01

Arsenic in drinking water is a serious problem for human health. Since the toxicity of arsenic species As(III) and As(V) is different, it is important to determine the concentrations separately. Therefore, it is necessary to develop an accurate and sensitive method for the speciation of arsenic. It was intended with this work to determine the concentrations of arsenic species in water samples collected from Izmir, Manisa and nearby areas. A batch type hydride generation atomic absorption spectrometer was used. As(V) gave no signal under the optimal measurement conditions of As(III). A certified reference drinking water was analyzed by the method and the results showed excellent agreement with the reported values. The procedure was applied to 34 water samples. Eleven tap water, two spring water, 19 artesian well water and two thermal water samples were analyzed under the optimal conditions.

Arsenic removal from contaminated groundwater by membrane-integrated hybrid plant: optimization and control using Visual Basic platform.

PubMed

Chakrabortty, S; Sen, M; Pal, P

2014-03-01

A simulation software (ARRPA) has been developed in Microsoft Visual Basic platform for optimization and control of a novel membrane-integrated arsenic separation plant in the backdrop of absence of such software. The user-friendly, menu-driven software is based on a dynamic linearized mathematical model, developed for the hybrid treatment scheme. The model captures the chemical kinetics in the pre-treating chemical reactor and the separation and transport phenomena involved in nanofiltration. The software has been validated through extensive experimental investigations. The agreement between the outputs from computer simulation program and the experimental findings are excellent and consistent under varying operating conditions reflecting high degree of accuracy and reliability of the software. High values of the overall correlation coefficient (R (2) = 0.989) and Willmott d-index (0.989) are indicators of the capability of the software in analyzing performance of the plant. The software permits pre-analysis, manipulation of input data, helps in optimization and exhibits performance of an integrated plant visually on a graphical platform. Performance analysis of the whole system as well as the individual units is possible using the tool. The software first of its kind in its domain and in the well-known Microsoft Excel environment is likely to be very useful in successful design, optimization and operation of an advanced hybrid treatment plant for removal of arsenic from contaminated groundwater.

Recycling of waste automotive laminated glass and valorization of polyvinyl butyral through mechanochemical separation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Swain, Basudev, E-mail: swain@iae.re.kr; Ryang Park, Jae; Yoon Shin, Dong

Due to strong binding, optical clarity, adhesion to many surfaces, toughness and flexibility polyvinyl butyral (PVB) resin films are commonly used in the automotive and architectural application as a protective interlayer in the laminated glass. Worldwide million tons of PVB waste generated from end-of-life automotive associated with various environmental issues. Stringent environmental directive, higher land cost eliminates land filling option, needs a study, we have developed a mechanochemical separation process to separate PVB resins from glass and characterized the separated PVB through various techniques, i.e., scanning electron microscope (SEM), energy-dispersive X-ray spectroscopy (EDS), infrared spectroscopy (IR) and nuclear magnetic resonancemore » spectroscopy (NMR). Commercial nonionic surfactants D201 used for the mechanochemical separation purpose. Through parameter optimization following conditions are considered to be the optimum condition; 30 vol% D201, stirring speed of 400 rpm, 35 °C temperature, operation time 1 h, and dilute D201 volume to waste automotive laminated glass weight ratio of ≈25. The technology developed in our laboratory is sustainable, environmentally friendly, techno-economical feasible process, capable of mass production (recycling). - Highlights: • Waste automotive laminated glass and polyvinyl butyral mechanochemically separated. • An economical total recovery and environment-friendly process has been developed. • It is a global problem rather than regional environmental issue has been addressed. • Without using hazardous chemical wastes are being converted to a wealth.« less

Timing resolution and time walk in SLiK SPAD: measurement and optimization

NASA Astrophysics Data System (ADS)

Fong, Bernicy S.; Davies, Murray; Deschamps, Pierre

2017-08-01

Timing resolution (or timing jitter) and time walk are separate parameters associated with a detector's response time. Studies have been done mostly on the time resolution of various single photon detectors [1]. As the designer and manufacturer of the ultra-low noise (ƙ-factor) silicon avalanche photodiode the SLiK SPAD, which is used in many single photon counting applications, we often get inquiries from customers to better understand how this detector behaves under different operating conditions. Hence, here we will be focusing on the study of these time related parameters specifically for the SLiK SPAD, as a way to provide the most direct information for users of this detector to help with its use more efficiently and effectively. We will be providing the study data on how these parameters can be affected by temperature (both intrinsic to the detector chip and environmental input based on operating conditions), operating voltage, photon wavelength, as well as light spot size. How these parameters can be optimized and the trade-offs from optimization from the desired performance will be presented.

Simultaneous determination of carbohydrates and simmondsins in jojoba seed meal (Simmondsia chinensis) by gas chromatography.

PubMed

Lein, Sabine; Van Boven, Maurits; Holser, Ron; Decuypere, Eddy; Flo, Gerda; Lievens, Sylvia; Cokelaere, Marnix

2002-11-22

Separate methods for the analyses of soluble carbohydrates in different plants and simmondsins in jojoba seed meal are described. A reliable gas chromatographic procedure for the simultaneous quantification of D-pinitol, myo-inositoL sucrose, 5-alpha-D-galactopyranosyl-D-pinitol. 2-alpha-D-galactopyranosyl-D-pinitol, simmondsin, 4-demethylsimmondsin, 5-demethylsimmondsin and 4,5-didemethylsimmondsin as trimethylsilyl derivatives in jojoba seed meal has been developed. The study of different extraction mixtures allowed for the quantitative recovery of the 9 analytes by a mixture of methanol-water (80:20, v/v) in the concentration range between 0.1 and 4%. Comparison of the separation parameters on three different capillary stationary phases with MS detection allowed for the choice of the optimal gas chromatographic conditions for baseline separation of the analytes.

Optimizing Chromatographic Separation: An Experiment Using an HPLC Simulator

ERIC Educational Resources Information Center

Shalliker, R. A.; Kayillo, S.; Dennis, G. R.

2008-01-01

Optimization of a chromatographic separation within the time constraints of a laboratory session is practically impossible. However, by employing a HPLC simulator, experiments can be designed that allow students to develop an appreciation of the complexities involved in optimization procedures. In the present exercise, a HPLC simulator from "JCE…

Robust penalty method for structural synthesis

NASA Technical Reports Server (NTRS)

Kamat, M. P.

1983-01-01

The Sequential Unconstrained Minimization Technique (SUMT) offers an easy way of solving nonlinearly constrained problems. However, this algorithm frequently suffers from the need to minimize an ill-conditioned penalty function. An ill-conditioned minimization problem can be solved very effectively by posing the problem as one of integrating a system of stiff differential equations utilizing concepts from singular perturbation theory. This paper evaluates the robustness and the reliability of such a singular perturbation based SUMT algorithm on two different problems of structural optimization of widely separated scales. The report concludes that whereas conventional SUMT can be bogged down by frequent ill-conditioning, especially in large scale problems, the singular perturbation SUMT has no such difficulty in converging to very accurate solutions.

Real-time PCR method combined with immunomagnetic separation for detecting healthy and heat-injured Salmonella Typhimurium on raw duck wings.

PubMed

Zheng, Qianwang; Mikš-Krajnik, Marta; Yang, Yishan; Xu, Wang; Yuk, Hyun-Gyun

2014-09-01

Conventional culture detection methods are time consuming and labor-intensive. For this reason, an alternative rapid method combining real-time PCR and immunomagnetic separation (IMS) was investigated in this study to detect both healthy and heat-injured Salmonella Typhimurium on raw duck wings. Firstly, the IMS method was optimized by determining the capture efficiency of Dynabeads(®) on Salmonella cells on raw duck wings with different bead incubation (10, 30 and 60 min) and magnetic separation (3, 10 and 30 min) times. Secondly, three Taqman primer sets, Sal, invA and ttr, were evaluated to optimize the real-time PCR protocol by comparing five parameters: inclusivity, exclusivity, PCR efficiency, detection probability and limit of detection (LOD). Thirdly, the optimized real-time PCR, in combination with IMS (PCR-IMS) assay, was compared with a standard ISO and a real-time PCR (PCR) method by analyzing artificially inoculated raw duck wings with healthy and heat-injured Salmonella cells at 10(1) and 10(0) CFU/25 g. Finally, the optimized PCR-IMS assay was validated for Salmonella detection in naturally contaminated raw duck wing samples. Under optimal IMS conditions (30 min bead incubation and 3 min magnetic separation times), approximately 85 and 64% of S. Typhimurium cells were captured by Dynabeads® from pure culture and inoculated raw duck wings, respectively. Although Sal and ttr primers exhibited 100% inclusivity and exclusivity for 16 Salmonella spp. and 36 non-Salmonella strains, the Sal primer showed lower LOD (10(3) CFU/ml) and higher PCR efficiency (94.1%) than the invA and ttr primers. Moreover, for Sal and invA primers, 100% detection probability on raw duck wings suspension was observed at 10(3) and 10(4) CFU/ml with and without IMS, respectively. Thus, the Sal primer was chosen for further experiments. The optimized PCR-IMS method was significantly (P=0.0011) better at detecting healthy Salmonella cells after 7-h enrichment than traditional PCR method. However there was no significant difference between the two methods with longer enrichment time (14 h). The diagnostic accuracy of PCR-IMS was shown to be 98.3% through the validation study. These results indicate that the optimized PCR-IMS method in this study could provide a sensitive, specific and rapid detection method for Salmonella on raw duck wings, enabling 10-h detection. However, a longer enrichment time could be needed for resuscitation and reliable detection of heat-injured cells. Copyright © 2014 Elsevier B.V. All rights reserved.

A novel process for separation of polycarbonate, polyvinyl chloride and polymethyl methacrylate waste plastics by froth flotation.

PubMed

Wang, Chong-Qing; Wang, Hui; Huang, Luo-Luo

2017-07-01

A novel process was proposed for separation of ternary waste plastics by froth flotation. Pretreatment of plastics with potassium permanganate (KMnO 4 ) solution was conducted to aid flotation separation of polycarbonate (PC), polyvinyl chloride (PVC) and polymethyl methacrylate (PMMA) plastics. The effect of pretreatment parameters including KMnO 4 concentration, treatment time, temperature and stirring rate on flotation recovery were investigated by single factor experiments. Surface treatment with KMnO 4 changes selectively the flotation behavior of PC, PVC and PMMA, enabling separation of the plastics by froth flotation. Mechanism of surface treatment was studied by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and X-ray photoelectron spectrum (XPS). Effect of frother concentration and flotation time on flotation behavior of plastic mixtures was further studied for flotation separation. The optimized conditions for separation of PC are KMnO 4 concentration 2mmolL -1 , treatment time 10min, temperature 60°C, stirring rate 300rpm, flotation time 1min and frother concentration 17.5mgL -1 . Under optimum conditions, PVC and PMMA mixtures are also separated efficiently by froth flotation associated with KMnO 4 treatment. The purity of PC, PVC and PMMA is up to 100%, 98.41% and 98.68%, while the recovery reaches 96.82%, 98.71% and 98.38%, respectively. Economic analysis manifests remarkable profits of the developed process. Reusing KMnO 4 solution is feasible, enabling the process greener. Copyright © 2017 Elsevier Ltd. All rights reserved.

Evaluation of results of cell electrophoresis experiments on space shuttle STS-3 including pre-flight and post-flight laboratory experiments

NASA Technical Reports Server (NTRS)

Todd, P. W.

1985-01-01

The objectives of the red blood cell experiments were to provide a visual check on the electrophoretic process and especially electroosmotic flow in space as well as to provide test separations of non-degradable standard particles for comparison with the separations of the three viable cell types studied on the Apollo-Soyuz Test Project. Determination of the maximum concentrations of cells that can be separated in column electrophore was a significant goal. Two of the eight columns were available for red cell experiments, so two concentrations of human and rabbit RBC mixtures were used. The objectives of another experiment were to evaluate the reproducibility of microgravity electrophoretic separation of living kidney cells, to separate cells with highly viability despite two freeze-thaw cycles, and to optimize the physical conditions of cell separation. Owing to the uncertain heterogeneity of the starting material, the experimental design does not assess resolution in microgravity, but improved separability was sought in comparison to density-gradient electrophoresis or continuous-flow electrophoresis. Efforts were made to increase cell yield and cell viability and to assess reproducibility directly.

Factors affecting the separation performance of proteins in capillary electrophoresis.

PubMed

Zhu, Yueping; Li, Zhenqing; Wang, Ping; Shen, Lisong; Zhang, Dawei; Yamaguchi, Yoshinori

2018-04-15

Capillary electrophoresis (CE) is an effective tool for protein separation and analysis. Compared with capillary gel electrophoresis (CGE), non-gel sieving capillary electrophoresis (NGSCE) processes the superiority on operation, repeatability and automaticity. Herein, we investigated the effect of polymer molecular weight and concentration, electric field strength, and the effective length of the capillary on the separation performance of proteins, and find that (1) polymer with high molecular weight and concentration favors the separation of proteins, although concentrated polymer hinders its injection into the channel of the capillary due to its high viscosity. (2) The resolution between the adjacent proteins decreases with the increase of electric field strength. (3) When the effective length of the capillary is long, the separation performance improves at the cost of separation time. (4) 1.4% (w/v) hydroxyethyl cellulose (HEC), 100 V/cm voltage and 12 cm effective length offers the best separation for the proteins with molecular weight from 14,400 Da to 97,400 Da. Finally, we employed the optimal electrophoretic conditions to resolve Lysozyme, Ovalbumin, BSA and their mixtures, and found that they were baseline resolved within 15 min. Copyright © 2018 Elsevier B.V. All rights reserved.

Optimization design of multiphase pump impeller based on combined genetic algorithm and boundary vortex flux diagnosis

NASA Astrophysics Data System (ADS)

Zhang, Jin-ya; Cai, Shu-jie; Li, Yong-jiang; Li, Yong-jiang; Zhang, Yong-xue

2017-12-01

A novel optimization design method for the multiphase pump impeller is proposed through combining the quasi-3D hydraulic design (Q3DHD), the boundary vortex flux (BVF) diagnosis, and the genetic algorithm (GA). The BVF diagnosis based on the Q3DHD is used to evaluate the objection function. Numerical simulations and hydraulic performance tests are carried out to compare the impeller designed only by the Q3DHD method and that optimized by the presented method. The comparisons of both the flow fields simulated under the same condition show that (1) the pressure distribution in the optimized impeller is more reasonable and the gas-liquid separation is more efficiently inhibited, (2) the scales of the gas pocket and the vortex decrease remarkably for the optimized impeller, (3) the unevenness of the BVF distributions near the shroud of the original impeller is effectively eliminated in the optimized impeller. The experimental results show that the differential pressure and the maximum efficiency of the optimized impeller are increased by 4% and 2.5%, respectively. Overall, the study indicates that the optimization design method proposed in this paper is feasible.

Electrostatic separation for recycling waste printed circuit board: a study on external factor and a robust design for optimization.

PubMed

Hou, Shibing; Wu, Jiang; Qin, Yufei; Xu, Zhenming

2010-07-01

Electrostatic separation is an effective and environmentally friendly method for recycling waste printed circuit board (PCB) by several kinds of electrostatic separators. However, some notable problems have been detected in its applications and cannot be efficiently resolved by optimizing the separation process. Instead of the separator itself, these problems are mainly caused by some external factors such as the nonconductive powder (NP) and the superficial moisture of feeding granule mixture. These problems finally lead to an inefficient separation. In the present research, the impacts of these external factors were investigated and a robust design was built to optimize the process and to weaken the adverse impact. A most robust parameter setting (25 kv, 80 rpm) was concluded from the experimental design. In addition, some theoretical methods, including cyclone separation, were presented to eliminate these problems substantially. This will contribute to efficient electrostatic separation of waste PCB and make remarkable progress for industrial applications.

Sample preparation for the determination of 241Am in sediments utilizing gamma-spectroscopy.

PubMed

Ristic, M; Degetto, S; Ast, T; Cantallupi, C

2002-01-01

This paper describes a procedure developed to separate americium-241 from the bulk of a sample by coprecipitation followed by high sensitivity gamma-counting of the concentrate in a well-type detector. It enables the measurement of 241Am at low concentrations, e.g. fallout levels in soils and sediments, or where large sample sizes are not available. The method is much faster and more reliable than those involving separation from other alpha-emitters, electroplating and alpha-spectrometry. A number of tracer experiments was performed in order to optimize the conditions for coprecipitation of 241Am from sediment leachates. The general outline of the determination of americium is also given.

Characterization of matrix effects in developing rugged high-throughput LC-MS/MS methods for bioanalysis.

PubMed

Li, Fumin; Wang, Jun; Jenkins, Rand

2016-05-01

There is an ever-increasing demand for high-throughput LC-MS/MS bioanalytical assays to support drug discovery and development. Matrix effects of sofosbuvir (protonated) and paclitaxel (sodiated) were thoroughly evaluated using high-throughput chromatography (defined as having a run time ≤1 min) under 14 elution conditions with extracts from protein precipitation, liquid-liquid extraction and solid-phase extraction. A slight separation, in terms of retention time, between underlying matrix components and sofosbuvir/paclitaxel can greatly alleviate matrix effects. High-throughput chromatography, with proper optimization, can provide rapid and effective chromatographic separation under 1 min to alleviate matrix effects and enhance assay ruggedness for regulated bioanalysis.

Multi-objective optimization of chromatographic rare earth element separation.

PubMed

Knutson, Hans-Kristian; Holmqvist, Anders; Nilsson, Bernt

2015-10-16

The importance of rare earth elements in modern technological industry grows, and as a result the interest for developing separation processes increases. This work is a part of developing chromatography as a rare earth element processing method. Process optimization is an important step in process development, and there are several competing objectives that need to be considered in a chromatographic separation process. Most studies are limited to evaluating the two competing objectives productivity and yield, and studies of scenarios with tri-objective optimizations are scarce. Tri-objective optimizations are much needed when evaluating the chromatographic separation of rare earth elements due to the importance of product pool concentration along with productivity and yield as process objectives. In this work, a multi-objective optimization strategy considering productivity, yield and pool concentration is proposed. This was carried out in the frame of a model based optimization study on a batch chromatography separation of the rare earth elements samarium, europium and gadolinium. The findings from the multi-objective optimization were used to provide with a general strategy for achieving desirable operation points, resulting in a productivity ranging between 0.61 and 0.75 kgEu/mcolumn(3), h(-1) and a pool concentration between 0.52 and 0.79 kgEu/m(3), while maintaining a purity above 99% and never falling below an 80% yield for the main target component europium. Copyright © 2015 Elsevier B.V. All rights reserved.

Quantum-state comparison and discrimination

NASA Astrophysics Data System (ADS)

Hayashi, A.; Hashimoto, T.; Horibe, M.

2018-05-01

We investigate the performance of discrimination strategy in the comparison task of known quantum states. In the discrimination strategy, one infers whether or not two quantum systems are in the same state on the basis of the outcomes of separate discrimination measurements on each system. In some cases with more than two possible states, the optimal strategy in minimum-error comparison is that one should infer the two systems are in different states without any measurement, implying that the discrimination strategy performs worse than the trivial "no-measurement" strategy. We present a sufficient condition for this phenomenon to happen. For two pure states with equal prior probabilities, we determine the optimal comparison success probability with an error margin, which interpolates the minimum-error and unambiguous comparison. We find that the discrimination strategy is not optimal except for the minimum-error case.

Scheduling Earth Observing Satellites with Evolutionary Algorithms

NASA Technical Reports Server (NTRS)

Globus, Al; Crawford, James; Lohn, Jason; Pryor, Anna

2003-01-01

We hypothesize that evolutionary algorithms can effectively schedule coordinated fleets of Earth observing satellites. The constraints are complex and the bottlenecks are not well understood, a condition where evolutionary algorithms are often effective. This is, in part, because evolutionary algorithms require only that one can represent solutions, modify solutions, and evaluate solution fitness. To test the hypothesis we have developed a representative set of problems, produced optimization software (in Java) to solve them, and run experiments comparing techniques. This paper presents initial results of a comparison of several evolutionary and other optimization techniques; namely the genetic algorithm, simulated annealing, squeaky wheel optimization, and stochastic hill climbing. We also compare separate satellite vs. integrated scheduling of a two satellite constellation. While the results are not definitive, tests to date suggest that simulated annealing is the best search technique and integrated scheduling is superior.

Efficient optimization of the quantum relative entropy

NASA Astrophysics Data System (ADS)

Fawzi, Hamza; Fawzi, Omar

2018-04-01

Many quantum information measures can be written as an optimization of the quantum relative entropy between sets of states. For example, the relative entropy of entanglement of a state is the minimum relative entropy to the set of separable states. The various capacities of quantum channels can also be written in this way. We propose a unified framework to numerically compute these quantities using off-the-shelf semidefinite programming solvers, exploiting the approximation method proposed in Fawzi, Saunderson and Parrilo (2017 arXiv: 1705.00812). As a notable application, this method allows us to provide numerical counterexamples for a proposed lower bound on the quantum conditional mutual information in terms of the relative entropy of recovery.

Local performance optimization for a class of redundant eight-degree-of-freedom manipulators

NASA Technical Reports Server (NTRS)

Williams, Robert L., II

1994-01-01

Local performance optimization for joint limit avoidance and manipulability maximization (singularity avoidance) is obtained by using the Jacobian matrix pseudoinverse and by projecting the gradient of an objective function into the Jacobian null space. Real-time redundancy optimization control is achieved for an eight-joint redundant manipulator having a three-axis spherical shoulder, a single elbow joint, and a four-axis spherical wrist. Symbolic solutions are used for both full-Jacobian and wrist-partitioned pseudoinverses, partitioned null-space projection matrices, and all objective function gradients. A kinematic limitation of this class of manipulators and the limitation's effect on redundancy resolution are discussed. Results obtained with graphical simulation are presented to demonstrate the effectiveness of local redundant manipulator performance optimization. Actual hardware experiments performed to verify the simulated results are also discussed. A major result is that the partitioned solution is desirable because of low computation requirements. The partitioned solution is suboptimal compared with the full solution because translational and rotational terms are optimized separately; however, the results show that the difference is not significant. Singularity analysis reveals that no algorithmic singularities exist for the partitioned solution. The partitioned and full solutions share the same physical manipulator singular conditions. When compared with the full solution, the partitioned solution is shown to be ill-conditioned in smaller neighborhoods of the shared singularities.

A cross-polarization based rotating-frame separated-local-field NMR experiment under ultrafast MAS conditions

NASA Astrophysics Data System (ADS)

Zhang, Rongchun; Damron, Joshua; Vosegaard, Thomas; Ramamoorthy, Ayyalusamy

2015-01-01

Rotating-frame separated-local-field solid-state NMR experiments measure highly resolved heteronuclear dipolar couplings which, in turn, provide valuable interatomic distances for structural and dynamic studies of molecules in the solid-state. Though many different rotating-frame SLF sequences have been put forth, recent advances in ultrafast MAS technology have considerably simplified pulse sequence requirements due to the suppression of proton-proton dipolar interactions. In this study we revisit a simple two-dimensional 1H-13C dipolar coupling/chemical shift correlation experiment using 13C detected cross-polarization with a variable contact time (CPVC) and systematically study the conditions for its optimal performance at 60 kHz MAS. In addition, we demonstrate the feasibility of a proton-detected version of the CPVC experiment. The theoretical analysis of the CPVC pulse sequence under different Hartmann-Hahn matching conditions confirms that it performs optimally under the ZQ (w1H - w1C = ±wr) condition for polarization transfer. The limits of the cross polarization process are explored and precisely defined as a function of offset and Hartmann-Hahn mismatch via spin dynamics simulation and experiments on a powder sample of uniformly 13C-labeled L-isoleucine. Our results show that the performance of the CPVC sequence and subsequent determination of 1H-13C dipolar couplings are insensitive to 1H/13C frequency offset frequency when high RF fields are used on both RF channels. Conversely, the CPVC sequence is quite sensitive to the Hartmann-Hahn mismatch, particularly for systems with weak heteronuclear dipolar couplings. We demonstrate the use of the CPVC based SLF experiment as a tool to identify different carbon groups, and hope to motivate the exploration of more sophisticated 1H detected avenues for ultrafast MAS.

Population level differences in thermal sensitivity of energy assimilation in terrestrial salamanders.

PubMed

Clay, Timothy A; Gifford, Matthew E

2017-02-01

Thermal adaptation predicts that thermal sensitivity of physiological traits should be optimized to thermal conditions most frequently experienced. Furthermore, thermodynamic constraints predict that species with higher thermal optima should have higher performance maxima and narrower performance breadths. We tested these predictions by examining the thermal sensitivity of energy assimilation between populations within two species of terrestrial-lungless salamanders, Plethodon albagula and P. montanus. Within P. albagula, we examined populations that were latitudinally separated by >450km. Within P. montanus, we examined populations that were elevationally separated by >900m. Thermal sensitivity of energy assimilation varied substantially between populations of P. albagula separated latitudinally, but did not vary between populations of P. montanus separated elevationally. Specifically, in P. albagula, the lower latitude population had a higher thermal optimum, higher maximal performance, and narrower performance breadth compared to the higher latitude population. Furthermore, across all individuals as thermal optima increased, performance maxima also increased, providing support for the theory that "hotter is better". Copyright © 2016 Elsevier Ltd. All rights reserved.

Separation of Active Compounds from Food by-Product (Cocoa Shell) Using Subcritical Water Extraction.

PubMed

Jokić, Stela; Gagić, Tanja; Knez, Željko; Šubarić, Drago; Škerget, Mojca

2018-06-11

Large amounts of residues are produced in the food industries. The waste shells from cocoa processing are usually burnt for fuel or used as a mulch in gardens to add nutrients to soil and to suppress weeds. The objectives of this work were: (a) to separate valuable compounds from cocoa shell by applying sustainable green separation process—subcritical water extraction (SWE); (b) identification and quantification of active compounds, sugars and sugar degradation products in obtained extracts using HPLC; (c) characterization of the antioxidant activity of extracts; (d) optimization of separation process using response surface methodology (RSM). Depending on applied extraction conditions, different concentration of theobromine, caffeine, theophylline, epicatechin, catechin, chlorogenic acid and gallic acid were determined in the extracts obtained by subcritical water. Furthermore, mannose, glucose, xylose, arabinose, rhamnose and fucose were detected as well as their important degradation products such as 5-hydroxymethylfurfural (5-HMF), furfural, levulinic acid, lactic acid and formic acid.

A study of retention characteristics and quality control of nutraceuticals containing resveratrol and polydatin using fused-core column chromatography.

PubMed

Fibigr, Jakub; Šatínský, Dalibor; Solich, Petr

2016-02-20

A new high-performance liquid chromatography method using fused-core column for fast separation of resveratrol and polydatin has been developed and used for quality control of nutraceuticals with resveratrol and polydatin content. Retention characteristics (log k) were studied under different conditions on C-18, RP-Amide C-18, Phenyl-hexyl, Pentafluorophenyl (F5) and Cyano stationary phases for both compounds. The effect of the volume fraction of acetonitrile on a retention factors log k of resveratrol and polydatin were evaluated. The optimal separation conditions for resveratrol, polydatin and internal standard p-nitrophenol were found on the fused-core column Ascentis Express ES-Cyano (100×3.0mm), particle size 2.7μm, with mobile phase acetonitrile/water solution with 0.5% acetic acid pH 3 (20:80, v/v) at a flow rate of 1.0mL/min and at 60°C. The detection wavelength was set at 305nm. Under the optimal chromatographic conditions, good linearity with regression coefficients in the range (r=0.9992-0.9998; n=10) for both compounds was achieved. Commercial samples of nutraceuticals were extracted with methanol using ultrasound bath for 15min. A 5μL sample volume of the filtered solution was directly injected into the HPLC system. Accuracy of the method defined as a mean recovery was in the range 83.2-107.3% for both nutraceuticals. The intraday method precision was found satisfactory and relative standard deviations of sample analysis were in the range 0.8-4.7%. The developed method has shown high sample throughput during sample preparation process, modern separation approach, and short time (3min) of analysis. The results of study showed that the declared content of resveratrol and polydatin varied widely in different nutraceuticals according the producers (71.50-115.00% of declared content). Copyright © 2015 Elsevier B.V. All rights reserved.

Effects of ammonium sulfate and sodium chloride concentration on PEG/protein liquid-liquid phase separation.

PubMed

Dumetz, André C; Lewus, Rachael A; Lenhoff, Abraham M; Kaler, Eric W

2008-09-16

When added to protein solutions, poly(ethylene glycol) (PEG) creates an effective attraction between protein molecules due to depletion forces. This effect has been widely used to crystallize proteins, and PEG is among the most successful crystallization agents in current use. However, PEG is almost always used in combination with a salt at either low or relatively high concentrations. Here the effects of sodium chloride and ammonium sulfate concentration on PEG 8000/ovalbumin liquid-liquid (L-L) phase separation are investigated. At low salt the L-L phase separation occurs at decreasing protein concentration with increasing salt concentration, presumably due to repulsive electrostatic interactions between proteins. At high salt concentration, the behavior depends on the nature of the salt. Sodium chloride has little effect on the L-L phase separation, but ammonium sulfate decreases the protein concentration at which the L-L phase separation occurs. This trend is attributed to the effects of critical fluctuations on depletion forces. The implications of these results for designing solution conditions optimal for protein crystallization are discussed.

Optimization of the high-performance liquid chromatographic separation of a complex mixture containing urinary steroids, boldenone and bolasterone: application to urine samples.

PubMed

Gonzalo-Lumbreras, R; Izquierdo-Hornillos, R

2000-05-26

An HPLC separation of a complex mixture containing 13 urinary anabolics and corticoids, and boldenone and bolasterone (synthetic anabolics) has been carried out. The applied optimization method involved the use of binary, ternary and quaternary mobile phases containing acetonitrile, methanol or tetrahydrofuran as organic modifiers. The effect of different reversed-phase packings and temperature on the separation was studied. The optimum separation was achieved by using a water-acetonitrile (60:40, v/v) mobile phase in reversed-phase HPLC at 30 degrees C, allowing the separation of all the analytes in about 24 min. Calibration graphs were obtained using bolasterone or methyltestosterone as internal standards. Detection limits were in the range 0.012-0.107 microg ml(-1). The optimized separation was applied to the analysis, after liquid-liquid extraction, of human urine samples spiked with steroids.

Prediction and optimization of the recovery rate in centrifugal separation of platelet-rich plasma (PRP)

NASA Astrophysics Data System (ADS)

Piao, Linfeng; Park, Hyungmin; Jo, Chris

2016-11-01

We present a theoretical model of the recovery rate of platelet and white blood cell in the process of centrifugal separation of platelet-rich plasma (PRP). For the practically used conditions in the field, the separation process is modeled as a one-dimensional particle sedimentation; a quasi-linear partial differential equation is derived based on the kinematic-wave theory. This is solved to determine the interface positions between supernatant-suspension and suspension-sediment, used to estimate the recovery rate of the plasma. While correcting the Brown's hypothesis (1989) claiming that the platelet recovery is linearly proportional to that of plasma, we propose a new correlation model for prediction of the platelet recovery, which is a function of the volume of whole blood, centrifugal acceleration and time. For a range of practical parameters, such as hematocrit, volume of whole blood and centrifugation (time and acceleration), the predicted recovery rate shows a good agreement with available clinical data. We propose that this model is further used to optimize the preparation method of PRP that satisfies the customized case. Supported by a Grant (MPSS-CG-2016-02) through the Disaster and Safety Management Institute funded by Ministry of Public Safety and Security of Korean government.

An approach of ionic liquids/lithium salts based microwave irradiation pretreatment followed by ultrasound-microwave synergistic extraction for two coumarins preparation from Cortex fraxini.

PubMed

Liu, Zaizhi; Gu, Huiyan; Yang, Lei

2015-10-23

Ionic liquids/lithium salts solvent system was successfully introduced into the separation technique for the preparation of two coumarins (aesculin and aesculetin) from Cortex fraxini. Ionic liquids/lithium salts based microwave irradiation pretreatment followed by ultrasound-microwave synergy extraction (ILSMP-UMSE) procedure was developed and optimized for the sufficient extraction of these two analytes. Several variables which can potentially influence the extraction yields, including pretreatment time and temperature, [C4mim]Br concentration, LiAc content, ultrasound-microwave synergy extraction (UMSE) time, liquid-solid ratio, and UMSE power were optimized by Plackett-Burman design. Among seven variables, UMSE time, liquid-solid ratio, and UMSE power were the statistically significant variables and these three factors were further optimized by Box-Behnken design to predict optimal extraction conditions and find out operability ranges with maximum extraction yields. Under optimum operating conditions, ILSMP-UMSE showed higher extraction yields of two target compounds than those obtained by reference extraction solvents. Method validation studies also evidenced that ILSMP-UMSE is credible for the preparation of two coumarins from Cortex fraxini. This study is indicative of the proposed procedure that has huge application prospects for the preparation of natural products from plant materials. Copyright © 2015 Elsevier B.V. All rights reserved.

Model-based identification of optimal operating conditions for amino acid simulated moving bed enantioseparation using a macrocyclic glycopeptide stationary phase.

PubMed

Fuereder, Markus; Majeed, Imthiyas N; Panke, Sven; Bechtold, Matthias

2014-06-13

Teicoplanin aglycone columns allow efficient separation of amino acid enantiomers in aqueous mobile phases and enable robust and predictable simulated moving bed (SMB) separation of racemic methionine despite a dependency of the adsorption behavior on the column history (memory effect). In this work we systematically investigated the influence of the mobile phase (methanol content) and temperature on SMB performance using a model-based optimization approach that accounts for methionine solubility, adsorption behavior and back pressure. Adsorption isotherms became more favorable with increasing methanol content but methionine solubility was decreased and back pressure increased. Numerical optimization suggested a moderate methanol content (25-35%) for most efficient operation. Higher temperature had a positive effect on specific productivity and desorbent requirement due to higher methionine solubility, lower back pressure and virtually invariant selectivity at high loadings of racemic methionine. However, process robustness (defined as a difference in flow rate ratios) decreased strongly with increasing temperature to the extent that any significant increase in temperature over 32°C will likely result in operating points that cannot be realized technically even with the lab-scale piston pump SMB system employed in this study. Copyright © 2014. Published by Elsevier B.V.

Efficient image enhancement using sparse source separation in the Retinex theory

NASA Astrophysics Data System (ADS)

Yoon, Jongsu; Choi, Jangwon; Choe, Yoonsik

2017-11-01

Color constancy is the feature of the human vision system (HVS) that ensures the relative constancy of the perceived color of objects under varying illumination conditions. The Retinex theory of machine vision systems is based on the HVS. Among Retinex algorithms, the physics-based algorithms are efficient; however, they generally do not satisfy the local characteristics of the original Retinex theory because they eliminate global illumination from their optimization. We apply the sparse source separation technique to the Retinex theory to present a physics-based algorithm that satisfies the locality characteristic of the original Retinex theory. Previous Retinex algorithms have limited use in image enhancement because the total variation Retinex results in an overly enhanced image and the sparse source separation Retinex cannot completely restore the original image. In contrast, our proposed method preserves the image edge and can very nearly replicate the original image without any special operation.

Peptide inhibitor modified magnetic particles for pepsin separation.

PubMed

Filuszová, Michaela; Kucerová, Zdenka; Tichá, Marie

2009-06-01

Synthetic heptapeptide containing D-amino acid residues (Val-D-Leu-Pro-Phe-Phe-Val-D-Leu) was coupled to glyoxal-activated magnetic agarose particles via the free peptide amino group. The peptide-modified magnetic particles were used for the separation of pepsins. Porcine pepsin A and human pepsin A were adsorbed to the magnetic peptide-modified affinity carrier, while the rat pepsin C and human pepsin C did not interact with the immobilized ligand. Conditions of pepsin adsorption to peptide-modified magnetic particles, as well as elution buffers were optimized. Porcine pepsin A did not interact with the immobilized peptide in the presence of pepsin inhibitor pepstatin A, indicating that the enzyme binding site is involved in the studied interaction. The elaborated method represents a rapid and simple technique not only for the separation of pepsins but also, in combination with MS, for the enzyme detection and determination.

On-line concentration and determination of all-trans- and 13-cis- retinoic acids in rabbit serum by application of sweeping technique in micellar electrokinetic chromatography.

PubMed

Zhao, Yongxi; Kong, Yu; Wang, Bo; Wu, Yayan; Wu, Hong

2007-03-30

A simple and rapid micellar electrokinetic chromatography (MEKC) method with UV detection was developed for the simultaneous separation and determination of all-trans- and 13-cis-retinoic acids in rabbit serum by on-line sweeping concentration technique. The serum sample was simply deproteinized and centrifuged. Various parameters affecting sample enrichment and separation were systematically investigated. Under optimal conditions, the analytes could be well separated within 17min, and the relative standard deviations (RSD) of migration times and peak areas were less than 3.4%. Compared with the conventional MEKC injection method, the 18- and 19-fold improvements in sensitivity were achieved, respectively. The proposed method has been successfully applied to the determination of all-trans- and 13-cis-retinoic acids in serum samples from rabbits and could be feasible for the further pharmacokinetics study of all-trans-retinoic acid.

Hydrodynamic Assists Magnetophoreses Rare Cancer cells Separation in Microchannel Simulation and Experimental Verifications

NASA Astrophysics Data System (ADS)

Saeed, O.; Duru, L.; Yulin, D.

2018-05-01

A proposed microfluidic design has been fabricated and simulated using COMSOL Multiphysics software, based on two physical models included in this design. The device’s ability to create a narrow stream of the core sample by controlling the sheath flow rates Qs1 and Qs2 in both peripheral channels was investigated. The main target of this paper is to study the possibility of combing the hydrodynamic and magnetic techniques, in order to achieve a high rate of cancer cells separation from a cell mixture and/or buffer sample. The study has been conducted in two stages, firstly, the effects of the sheath flow rates (Qs1 and Qs2) on the sample stream focusing were studied, to find the proposed device effectiveness optimal conditions and its capability in cell focusing, and then the magnetic mechanism has been utilized to finalize the pre-labelled cells separation process.

Enantioseparation of thalidomide and its hydroxylated metabolites using capillary electrophoresis with various cyclodextrins and their combinations as chiral buffer additives.

PubMed

Meyring, M; Chankvetadze, B; Blaschke, G

1999-09-01

The separation of thalidomide (TD) and its hydroxylated metabolites including their simultaneous enantioseparation was studied in capillary electrophoresis (CE) using four different randomly substituted charged cyclodextrin (CD) derivatives, the combinations of some of them with each other, and beta-CD. TD, as well as two metabolites recently found in incubations of human liver microsomes and human blood, 5-hydroxythalidomide (5-OH-TD) and one of the diastereomeric 5'-hydroxythalidomides (5'-OH-TD), are neutral compounds. Therefore, they were resolved using charged chiral selectors in CE. Two different separation modes (normal polarity and carrier mode) and two different capillaries (fused-silica and polyacrylamide-coated) were tested. Based on the behavior of the individual CDs, their designed combinations were selected in order to improve the separation selectivity and enantioselectivity. Under optimized conditions all three chiral compounds and their enantiomers were resolved simultaneously.

Highly Selective and Considerable Subcritical Butane Extraction to Separate Abamectin in Green Tea.

PubMed

Zhang, Yating; Gu, Lingbiao; Wang, Fei; Kong, Lingjun; Pang, Huili; Qin, Guangyong

2017-06-01

We specially carried out the subcritical butane extraction to separate abamectin from tea leaves. Four parameters, such as extraction temperature, extraction time, number of extraction cycles, and solid-liquid ratio were studied and optimized through the response surface methodology with design matrix developed by Box-Behnken. Seventeen experiments with three various factors and three variable levels were employed to investigate the effect of these parameters on the extraction of abamectin. Besides, catechins, theanine, caffeine, and aroma components were determined by both high-performance liquid chromatography and gas chromatography-mass spectrometry to evaluate the tea quality before and after the extraction. The results showed that the extraction temperature was the uppermost parameter compared with others. The optimal extraction conditions selected as follows: extraction temperature, 42°C; number of extraction cycles and extraction time, 1 and 30 min, respectively; and solid-liquid ratio, 1:10. Based on the above study, the separation efficiency of abamectin was up to 93.95%. It is notable that there has a quite low loss rate, including the negligible damage of aroma components, the bits reduce of catechins within the range of 0.7%-13.1%, and a handful lessen of caffeine and theanine of 1.81% and 2.6%, respectively. The proposed method suggested subcritical butane possesses solubility for lipid-soluble pesticides, and since most of the pesticides are attached to the surfaces of tea, thus the as-applied method was successfully effective to separate abamectin because of the so practical and promising method.

Water and lipid diffusion MRI using chemical shift displacement-based separation of lipid tissue (SPLIT).

PubMed

Ohno, Naoki; Kan, Hirohito; Miyati, Tosiaki; Aoki, Toshitaka; Ishida, Shota; Gabata, Toshifumi

2017-06-01

To obtain water and lipid diffusion-weighted images (DWIs) simultaneously, we devised a novel method utilizing chemical shift displacement-based separation of lipid tissue (SPLIT) imaging. Single-shot diffusion echo-planar imaging without fat suppression was used and the imaging parameters were optimized to separate water and lipid DWIs by chemical shift displacement of the lipid signals along the phase-encoding direction. Using the optimized conditions, transverse DWIs at the maximum diameter of the right calf were scanned with multiple b-values in five healthy subjects. Then, apparent diffusion coefficients (ADCs) were calculated in the tibialis anterior muscle (TA), tibialis bone marrow (TB), and subcutaneous fat (SF), as well as restricted and perfusion-related diffusion coefficients (D and D*, respectively) and the fraction of the perfusion-related diffusion component (F) for TA. Water and lipid DWIs were separated adequately. The mean ADCs of the TA, TB, and SF were 1.56±0.03mm 2 /s, 0.01±0.01mm 2 /s, and 0.06±0.02mm 2 /s, respectively. The mean D*, D, and F of the TA were 13.7±4.3mm 2 /s, 1.48±0.05mm 2 /s, and 4.3±1.6%, respectively. SPLIT imaging makes it possible to simply and simultaneously obtain water and lipid DWIs without special pulse sequence and increases the amount of diffusion information of water and lipid tissue. Copyright © 2017. Published by Elsevier Inc.

Ionic liquid as a mobile phase additive in high-performance liquid chromatography for the simultaneous determination of eleven fluorescent whitening agents in paper materials.

PubMed

Wang, Qing; Chen, Xianbo; Qiu, Bin; Zhou, Liang; Zhang, Hui; Xie, Juan; Luo, Yan; Wang, Bin

2016-04-01

In the present study, 11 4,4'-diaminostilbene-2,2'-disulfonic acid based fluorescent whitening agents with different numbers of sulfonic acid groups were separated by using an ionic liquid as a mobile phase additive in high-performance liquid chromatography with fluorescence detection. The effects of ionic liquid concentration, pH of mobile phase B, and composition of mobile phase A on the separation of fluorescent whitening agents were systematically investigated. The ionic liquid tetrabutylammonium tetrafluoroborate is superior to tetrabutylammomnium bromide for the separation of the fluorescent whitening agents. The optimal separation conditions were an ionic liquid concentration at 8 mM and the pH of mobile phase B at 8.5 with methanol as mobile phase A. The established method exhibited low limits of detection (0.04-0.07 ng/mL) and wide linearity ranges (0.30-20 ng/mL) with high linear correlation coefficients from 0.9994 to 0.9998. The optimized procedure was applied to analyze target analytes in paper samples with satisfactory results. Eleven target analytes were quantified, and the recoveries of spiked paper samples were in the range of 85-105% with the relative standard deviations from 2.1 to 5.1%. The obtained results indicated that the method was efficient for detection of 11 fluorescent whitening agents. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Elasto-inertial microfluidics for bacteria separation from whole blood for sepsis diagnostics.

PubMed

Faridi, Muhammad Asim; Ramachandraiah, Harisha; Banerjee, Indradumna; Ardabili, Sahar; Zelenin, Sergey; Russom, Aman

2017-01-04

Bloodstream infections (BSI) remain a major challenge with high mortality rate, with an incidence that is increasing worldwide. Early treatment with appropriate therapy can reduce BSI-related morbidity and mortality. However, despite recent progress in molecular based assays, complex sample preparation steps have become critical roadblock for a greater expansion of molecular assays. Here, we report a size based, label-free, bacteria separation from whole blood using elasto-inertial microfluidics. In elasto-inertial microfluidics, the viscoelastic flow enables size based migration of blood cells into a non-Newtonian solution, while smaller bacteria remain in the streamline of the blood sample entrance and can be separated. We first optimized the flow conditions using particles, and show continuous separation of 5 μm particles from 2 μm at a yield of 95% for 5 µm particle and 93% for 2 µm particles at respective outlets. Next, bacteria were continuously separated at an efficiency of 76% from undiluted whole blood sample. We demonstrate separation of bacteria from undiluted while blood using elasto-inertial microfluidics. The label-free, passive bacteria preparation method has a great potential for downstream phenotypic and molecular analysis of bacteria.

Design of A Cyclone Separator Using Approximation Method

NASA Astrophysics Data System (ADS)

Sin, Bong-Su; Choi, Ji-Won; Lee, Kwon-Hee

2017-12-01

A Separator is a device installed in industrial applications to separate mixed objects. The separator of interest in this research is a cyclone type, which is used to separate a steam-brine mixture in a geothermal plant. The most important performance of the cyclone separator is the collection efficiency. The collection efficiency in this study is predicted by performing the CFD (Computational Fluid Dynamics) analysis. This research defines six shape design variables to maximize the collection efficiency. Thus, the collection efficiency is set up as the objective function in optimization process. Since the CFD analysis requires a lot of calculation time, it is impossible to obtain the optimal solution by linking the gradient-based optimization algorithm. Thus, two approximation methods are introduced to obtain an optimum design. In this process, an L18 orthogonal array is adopted as a DOE method, and kriging interpolation method is adopted to generate the metamodel for the collection efficiency. Based on the 18 analysis results, the relative importance of each variable to the collection efficiency is obtained through the ANOVA (analysis of variance). The final design is suggested considering the results obtained from two optimization methods. The fluid flow analysis of the cyclone separator is conducted by using the commercial CFD software, ANSYS-CFX.

Photosynthetic acclimation of WS and WS-gpt2 in Arabidopsis thaliana under fluctuating natural light condition

NASA Astrophysics Data System (ADS)

Pa'ee, Furzani; Johnson, Giles

2017-10-01

Photoacclimation is a process by which photosynthetic capacity is regulated in response to environmental adjustments in terms of light regime. Photoacclimation is essential in determining the photosynthetic capacity to optimize light use and to avoid potentially damaging effects. Previous work in our laboratory has identified a gene, gpt2 (At1g61800) that is essential for plants to acclimate to an increase and decrease of growth irradiance, separately. To investigate the photoacclimation ability towards fluctuating natural light condition in Arabidopsis thaliana, photosynthetic capacity was measured in plants of the accession Wassileskija (WS) and in plants lacking expression of the gene At1g61800 (WS-gpt2). The experiment was carried out over a time span from early Autumn to early Spring season in 2010-2011 and 2011-2012. The seedlings were grown in an unheated greenhouse in Manchester, UK without supplementary lighting. Gas exchange measurements and chlorophyll content estimation were performed on WS and WS-gpt2 and it showed that both sets of plants were able to acclimate to fluctuating natural light condition. Therefore, it is suggested that the mechanisms of acclimation in a separate growth light condition is mechanistically distinct than the mechanism under fluctuating natural light condition.

Supercritical Fluid Chromatography of Drugs: Parallel Factor Analysis for Column Testing in a Wide Range of Operational Conditions

PubMed Central

Al-Degs, Yahya; Andri, Bertyl; Thiébaut, Didier; Vial, Jérôme

2017-01-01

Retention mechanisms involved in supercritical fluid chromatography (SFC) are influenced by interdependent parameters (temperature, pressure, chemistry of the mobile phase, and nature of the stationary phase), a complexity which makes the selection of a proper stationary phase for a given separation a challenging step. For the first time in SFC studies, Parallel Factor Analysis (PARAFAC) was employed to evaluate the chromatographic behavior of eight different stationary phases in a wide range of chromatographic conditions (temperature, pressure, and gradient elution composition). Design of Experiment was used to optimize experiments involving 14 pharmaceutical compounds present in biological and/or environmental samples and with dissimilar physicochemical properties. The results showed the superiority of PARAFAC for the analysis of the three-way (column × drug × condition) data array over unfolding the multiway array to matrices and performing several classical principal component analyses. Thanks to the PARAFAC components, similarity in columns' function, chromatographic trend of drugs, and correlation between separation conditions could be simply depicted: columns were grouped according to their H-bonding forces, while gradient composition was dominating for condition classification. Also, the number of drugs could be efficiently reduced for columns classification as some of them exhibited a similar behavior, as shown by hierarchical clustering based on PARAFAC components. PMID:28695040

[Study on rhG-CSF modified with polyethylene glycol].

PubMed

Zhang, Lin-Lin; Zheng, Chun-Yang; Lei, Jian-Du; Ma, Guang-Hui; Su, Zhi-Guo; Wang, Li

2005-11-01

Monomethoxy Polyethylene Glycol(mPEG20000) was activated by N-hydroxysuccinimede and analyzed by infrared spectrum and hydrolysis kinetics. In order to propose the optimized reaction conditions of mono-PEGylated rhG-CSF, orthogonal design of the experiment was investigated. Ion exchange chromatography was used to separate and purify PEGylated rhG-CSF from unPEGylated rhG-CSF. The purity of mono-PEGylated rhG-CSF was analyzed by high performance liquid chromatography (HPLC) to be 97%.

Vortex generator design for aircraft inlet distortion as a numerical optimization problem

NASA Technical Reports Server (NTRS)

Anderson, Bernhard H.; Levy, Ralph

1991-01-01

Aerodynamic compatibility of aircraft/inlet/engine systems is a difficult design problem for aircraft that must operate in many different flight regimes. Takeoff, subsonic cruise, supersonic cruise, transonic maneuvering, and high altitude loiter each place different constraints on inlet design. Vortex generators, small wing like sections mounted on the inside surfaces of the inlet duct, are used to control flow separation and engine face distortion. The design of vortex generator installations in an inlet is defined as a problem addressable by numerical optimization techniques. A performance parameter is suggested to account for both inlet distortion and total pressure loss at a series of design flight conditions. The resulting optimization problem is difficult since some of the design parameters take on integer values. If numerical procedures could be used to reduce multimillion dollar development test programs to a small set of verification tests, numerical optimization could have a significant impact on both cost and elapsed time to design new aircraft.

Method development for speciation analysis of nanoparticle and ionic forms of gold in biological samples by high performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Malejko, Julita; Świerżewska, Natalia; Bajguz, Andrzej; Godlewska-Żyłkiewicz, Beata

2018-04-01

A new method based on coupling high performance liquid chromatography (HPLC) to inductively coupled plasma mass spectrometry (ICP MS) has been developed for the speciation analysis of gold nanoparticles (AuNPs) and dissolved gold species (Au(III)) in biological samples. The column type, the composition and the flow rate of the mobile phase were carefully investigated in order to optimize the separation conditions. The usefulness of two polymeric reversed phase columns (PLRP-S with 100 nm and 400 nm pore size) to separate gold species were investigated for the first time. Under the optimal conditions (PLRP-S400 column, 10 mmol L-1 SDS and 5% methanol as the mobile phase, 0.5 mL min-1 flow rate), detection limits of 2.2 ng L-1 for Au(III), 2.8 ng L-1 for 10 nm AuNPs and 3.7 ng L-1 for 40 nm AuNPs were achieved. The accuracy of the method was proved by analysis of reference material RM 8011 (NIST) of gold nanoparticles of nominal diameter of 10 nm. The HPLC-ICP MS method has been successfully applied to the detection and size characterization of gold species in lysates of green algae Acutodesmus obliquus, typical representative of phytoplankton flora, incubated with 10 nm AuNPs or Au(III).

CE-UV for the characterization of passion fruit juices provenance by amino acids profile with the aid of chemometric tools.

PubMed

Passos, Heloisa Moretti; Cieslarova, Zuzana; Simionato, Ana Valéria Colnaghi

2016-07-01

A separation method was developed in order to quantify free amino acids in passion fruit juices using CE-UV. A selective derivatization reaction with FMOC followed by MEKC analysis was chosen due to the highly interconnected mobilities of the analytes, enabling the separation of 22 amino acids by lipophilicity differences, as will be further discussed. To achieve such results, the method was optimized concerning BGE composition (concentrations, pH, and addition of organic modifier) and running conditions (temperature and applied voltage). The optimized running conditions were: a BGE composed by 60 mmol/L borate buffer at pH 10.1, 30 mmol/L SDS and 5 % methanol; running for 40 min at 23°C and 25 kV. The method was validated and applied on eight brands plus one fresh natural juice, detecting 12 amino acids. Quantification of six analytes combined with principal component analysis was capable to characterize different types of juices and showed potential to detect adulteration on industrial juices. Glutamic acid was found to be the most concentrated amino acid in all juices, exceeding 1 g/L in all samples and was also crucial for the correct classification of a natural juice, which presented a concentration of 22 g/L. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A Combined Independent Source Separation and Quality Index Optimization Method for Fetal ECG Extraction from Abdominal Maternal Leads

PubMed Central

Billeci, Lucia; Varanini, Maurizio

2017-01-01

The non-invasive fetal electrocardiogram (fECG) technique has recently received considerable interest in monitoring fetal health. The aim of our paper is to propose a novel fECG algorithm based on the combination of the criteria of independent source separation and of a quality index optimization (ICAQIO-based). The algorithm was compared with two methods applying the two different criteria independently—the ICA-based and the QIO-based methods—which were previously developed by our group. All three methods were tested on the recently implemented Fetal ECG Synthetic Database (FECGSYNDB). Moreover, the performance of the algorithm was tested on real data from the PhysioNet fetal ECG Challenge 2013 Database. The proposed combined method outperformed the other two algorithms on the FECGSYNDB (ICAQIO-based: 98.78%, QIO-based: 97.77%, ICA-based: 97.61%). Significant differences were obtained in particular in the conditions when uterine contractions and maternal and fetal ectopic beats occurred. On the real data, all three methods obtained very high performances, with the QIO-based method proving slightly better than the other two (ICAQIO-based: 99.38%, QIO-based: 99.76%, ICA-based: 99.37%). The findings from this study suggest that the proposed method could potentially be applied as a novel algorithm for accurate extraction of fECG, especially in critical recording conditions. PMID:28509860

Faithful Squashed Entanglement

NASA Astrophysics Data System (ADS)

Brandão, Fernando G. S. L.; Christandl, Matthias; Yard, Jon

2011-09-01

Squashed entanglement is a measure for the entanglement of bipartite quantum states. In this paper we present a lower bound for squashed entanglement in terms of a distance to the set of separable states. This implies that squashed entanglement is faithful, that is, it is strictly positive if and only if the state is entangled. We derive the lower bound on squashed entanglement from a lower bound on the quantum conditional mutual information which is used to define squashed entanglement. The quantum conditional mutual information corresponds to the amount by which strong subadditivity of von Neumann entropy fails to be saturated. Our result therefore sheds light on the structure of states that almost satisfy strong subadditivity with equality. The proof is based on two recent results from quantum information theory: the operational interpretation of the quantum mutual information as the optimal rate for state redistribution and the interpretation of the regularised relative entropy of entanglement as an error exponent in hypothesis testing. The distance to the set of separable states is measured in terms of the LOCC norm, an operationally motivated norm giving the optimal probability of distinguishing two bipartite quantum states, each shared by two parties, using any protocol formed by local quantum operations and classical communication (LOCC) between the parties. A similar result for the Frobenius or Euclidean norm follows as an immediate consequence. The result has two applications in complexity theory. The first application is a quasipolynomial-time algorithm solving the weak membership problem for the set of separable states in LOCC or Euclidean norm. The second application concerns quantum Merlin-Arthur games. Here we show that multiple provers are not more powerful than a single prover when the verifier is restricted to LOCC operations thereby providing a new characterisation of the complexity class QMA.

Development of a supercritical fluid chromatography method with ultraviolet and mass spectrometry detection for the characterization of biomass fast pyrolysis bio oils.

PubMed

Crepier, Julien; Le Masle, Agnès; Charon, Nadège; Albrieux, Florian; Heinisch, Sabine

2017-08-11

The characterization of complex mixtures is a challenging issue for the development of innovative processes dedicated to biofuels and bio-products production. The huge number of compounds present in biomass fast pyrolysis oils combined with the large diversity of chemical functions represent a bottleneck as regards analytical technique development. For the extensive characterization of complex samples, supercritical fluid chromatography (SFC) can be alternative to usual separation techniques such as gas (GC) or liquid chromatography (LC). In this study, an approach is proposed to define the best conditions for the SFC separation of a fast pyrolysis bio-oil. This approach was based on SFC data obtained directly from the bio-oil itself instead of selecting model compounds as usually done. SFC conditions were optimized by using three specific, easy-to-use and quantitative criteria aiming at maximizing the separation power. Polar stationary phases (ethylpyridine bonded silica) associated to a mix of acetonitrile and water as polarity modifier provided the best results, with more than 120 peaks detected in SFC-UV. Copyright © 2017 Elsevier B.V. All rights reserved.

Improved Flow Modulator Construction for GC × GC with Quadrupole Mass Spectrometry.

PubMed

Ston, Martin; Cabala, Radomir; Bierhanzl, Vaclav Matej; Krajicek, Jan; Bosakova, Zuzana

2016-08-18

Improvement and testing of a flow modulator for the application in comprehensive two-dimensional gas chromatography separations is the subject of the presented paper. This improved setup constructed from two independent capillary branches each consisting of a pressure regulator, a pressure sensor, a two-way solenoid valve and a microfluidic T-connector, allows an independent and easy settings of the pressures and flow velocities in the modulator and provides system flexibility in an operation without need of any component exchange. The estimated flow rates were 0.4 mL/min in the first column and 3.2 mL/min in the second column. This setup was compared with the commercial Zoex cryogenic modulator for the separation of 17 selected solvents at isothermal conditions. Modulator working conditions were optimized and its separation power was demonstrated on the analysis of a lavender extract under an application of two orthogonal capillary column sets (nonpolar-polar vs. polar-nonpolar) and temperature program. The results were evaluated by two commercial software packages and discussed with respect to the identification compliance. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Purity Determination by Capillary Electrophoresis Sodium Hexadecyl Sulfate (CE-SHS): A Novel Application For Therapeutic Protein Characterization.

PubMed

Beckman, Jeff; Song, Yuanli; Gu, Yan; Voronov, Sergey; Chennamsetty, Naresh; Krystek, Stanley; Mussa, Nesredin; Li, Zheng Jian

2018-02-20

Capillary gel electrophoresis using sodium dodecyl sulfate (CE-SDS) is used commercially to provide quantitative purity data for therapeutic protein characterization and release. In CE-SDS, proteins are denatured under reducing or nonreducing conditions in the presence of SDS and electrophoretically separated by molecular weight and hydrodynamic radius through a sieving polymer matrix. Acceptable performance of this method would yield protein peaks that are baseline resolved and symmetrical. Nominal CE-SDS conditions and parameters are not optimal for all therapeutic proteins, specifically for Recombinant Therapeutic Protein-1 (RTP-1), where acceptable resolution and peak symmetry were not achieved. The application of longer alkyl chain detergents in the running buffer matrix substantially improved assay performance. Matrix running buffer containing sodium hexadecyl sulfate (SHS) increased peak resolution and plate count 3- and 8-fold, respectively, compared to a traditional SDS-based running gel matrix. At Bristol-Myers Squibb (BMS), we developed and qualified a viable method for the characterization and release of RTP-1 using an SHS-containing running buffer matrix. This work underscores the potential of detergents other than SDS to enhance the resolution and separation power of CE-based separation methods.

Detection of the ideal resource for multiqubit teleportation

NASA Astrophysics Data System (ADS)

Zhao, Ming-Jing; Chen, Bin; Fei, Shao-Ming

2015-07-01

We give a sufficient condition for detecting the entanglement resource for perfect multiqubit teleportation. The criterion involves only local measurements on some complementary observables and can be experimentally implemented. It is also a necessary condition for full separability of multiqubit states. Moreover, by proving the optimality of teleportation witnesses, we solve the open problem in Phys. Rev. A 86, 032315 (2012). Project supported by the National Natural Science Foundation of China (Grant Nos. 11401032, 11275131, and 61473325), the Foundation of Beijing Information Science and Technology University, China (Grant No. 1425032), and the Scientific Research Foundation for the Returned Overseas Chinese Scholars, State Education Ministry of China.

Implementation of CFD modeling in the performance assessment and optimization of secondary clarifiers: the PVSC case study.

PubMed

Xanthos, S; Ramalingam, K; Lipke, S; McKenna, B; Fillos, J

2013-01-01

The water industry and especially the wastewater treatment sector has come under steadily increasing pressure to optimize their existing and new facilities to meet their discharge limits and reduce overall cost. Gravity separation of solids, producing clarified overflow and thickened solids underflow has long been one of the principal separation processes used in treating secondary effluent. Final settling tanks (FSTs) are a central link in the treatment process and often times act as the limiting step to the maximum solids handling capacity when high throughput requirements need to be met. The Passaic Valley Sewerage Commission (PVSC) is interested in using a computational fluid dynamics (CFD) modeling approach to explore any further FST retrofit alternatives to sustain significantly higher plant influent flows, especially under wet weather conditions. In detail there is an interest in modifying and/or upgrading/optimizing the existing FSTs to handle flows in the range of 280-720 million gallons per day (MGD) (12.25-31.55 m(3)/s) in compliance with the plant's effluent discharge limits for total suspended solids (TSS). The CFD model development for this specific plant will be discussed, 2D and 3D simulation results will be presented and initial results of a sensitivity study between two FST effluent weir structure designs will be reviewed at a flow of 550 MGD (∼24 m(3)/s) and 1,800 mg/L MLSS (mixed liquor suspended solids). The latter will provide useful information in determining whether the existing retrofit of one of the FSTs would enable compliance under wet weather conditions and warrants further consideration for implementing it in the remaining FSTs.

Search for evidence of life in space: analysis of enantiomeric organic molecules by N,N-dimethylformamide dimethylacetal derivative dependant Gas Chromatography-Mass Spectrometry.

PubMed

Freissinet, C; Buch, A; Sternberg, R; Szopa, C; Geffroy-Rodier, C; Jelinek, C; Stambouli, M

2010-01-29

Within the context of the future space missions to Mars (MSL 2011 and Exomars 2016), which aim at searching for traces of life at the surface, the detection and quantitation of enantiomeric organic molecules is of major importance. In this work, we have developed and optimized a method to derivatize and analyze chiral organic molecules suitable for space experiments, using N,N-dimethylformamide dimethylacetal (DMF-DMA) as the derivatization agent. The temperature, duration of the derivatization reaction, and chromatographic separation parameters have been optimized to meet instrument design constraints imposed upon space experiment devices. This work demonstrates that, in addition to its intrinsic qualities, such as production of light-weight derivatives and a great resistance to drastic operating conditions, DMF-DMA facilitates simple and fast derivatization of organic compounds (three minutes at 140 degrees C in a single-step) that is suitable for an in situ analysis in space. By using DMF-DMA as the derivatization agent, we have successfully identified 19 of the 20 proteinic amino acids and been able to enantiomerically separate ten of the potential 19 (glycine being non-chiral). Additionally, we have minimized the percentage of racemized amino acid compounds produced by optimizing the conditions of the derivatization reaction itself. Quantitative linearity studies and the determination of the limit of detection show that the proposed method is also suitable for the quantitative determination of both enantiomeric forms of most of the tested amino acids, as limits of detection obtained are lower than the ppb level of organic molecules already detected in Martian meteorites. Copyright (c) 2009 Elsevier B.V. All rights reserved.

Improved optimization of polycyclic aromatic hydrocarbons (PAHs) mixtures resolution in reversed-phase high-performance liquid chromatography by using factorial design and response surface methodology.

PubMed

Andrade-Eiroa, Auréa; Diévart, Pascal; Dagaut, Philippe

2010-04-15

A new procedure for optimizing PAHs separation in very complex mixtures by reverse phase high performance (RPLC) is proposed. It is based on changing gradually the experimental conditions all along the chromatographic procedure as a function of the physical properties of the compounds eluted. The temperature and speed flow gradients allowed obtaining the optimum resolution in large chromatographic determinations where PAHs with very different medium polarizability have to be separated. Whereas optimization procedures of RPLC methodologies had always been accomplished regardless of the physico-chemical properties of the target analytes, we found that resolution is highly dependent on the physico-chemical properties of the target analytes. Based on resolution criterion, optimization process for a 16 EPA PAHs mixture was performed on three sets of difficult-to-separate PAHs pairs: acenaphthene-fluorene (for the optimization procedure in the first part of the chromatogram where light PAHs elute), benzo[g,h,i]perylene-dibenzo[a,h]anthracene and benzo[g,h,i]perylene-indeno[1,2,3-cd]pyrene (for the optimization procedure of the second part of the chromatogram where the heavier PAHs elute). Two-level full factorial designs were applied to detect interactions among variables to be optimized: speed flow, temperature of column oven and mobile-phase gradient in the two parts of the studied chromatogram. Experimental data were fitted by multivariate nonlinear regression models and optimum values of speed flow and temperature were obtained through mathematical analysis of the constructed models. An HPLC system equipped with a reversed phase 5 microm C18, 250 mm x 4.6mm column (with acetonitrile/water mobile phase), a column oven, a binary pump, a photodiode array detector (PDA), and a fluorimetric detector were used in this work. Optimum resolution was achieved operating at 1.0 mL/min in the first part of the chromatogram (until 45 min) and 0.5 mL/min in the second one (from 45 min to the end) and by applying programmed temperature gradient (15 degrees C until 30 min and progressively increasing temperature until reaching 40 degrees C at 45 min). (c) 2009 Elsevier B.V. All rights reserved.

Application of response surface methodology (RSM) to the optimization of a post-column luminol chemiluminescence analysis of silyl peroxides.

PubMed

Baj, Stefan; Słupska, Roksana; Krawczyk, Tomasz

2013-01-15

The possibility of the utilization of chemiluminescence post-column luminol oxidation (CL) in a HPLC system for silyl peroxides analysis has been investigated. The conditions of HPLC separation for 12 silyl peroxides, representing bissilyl and alkyl-silyl peroxides, as well as their potential impurities, were established. Optimal chemiluminescent post-column reaction conditions were found using central composite design (CCD) and response surface methodology (RSM). The interaction effects of four of the most important operating variables - the concentrations of luminol, hemin, sodium hydroxide and the post-column solution flow rate - on the light intensity were evaluated. The optimized conditions for analysis were the same for bissilyl and alkyl-silyl peroxides for the base concentration (0.03 M), the luminol concentration (0.4 g L(-1)) and the hemin concentration (0.3 g L(-1)). The only differences occurred in a reagent flow rate (for bissilyl peroxide -0.3 mL min(-1) and for alkyl-silyl peroxides -0.9 mL min(-1)). Under optimal conditions, the detection limits were in the 0.07-0.16 nM range for bissilyl, and 0.53-1.01 for alkyl-silyl peroxides. The calibration curves were linear in the 0.25-3 nM range for bissilyl and the 2.5-25 range for alkyl-silyl peroxides. Intra-day and inter-day precision was lower than 5.5% for each tested concentration level. A mechanism of luminol oxidation by silyl peroxides involving a hydrolysis step with the formation of hydrogen peroxide or hydroperoxide was proposed. Copyright © 2012 Elsevier B.V. All rights reserved.

Application of mixed cloud point extraction for the analysis of six flavonoids in Apocynum venetum leaf samples by high performance liquid chromatography.

PubMed

Zhou, Jun; Sun, Jiang Bing; Xu, Xin Yu; Cheng, Zhao Hui; Zeng, Ping; Wang, Feng Qiao; Zhang, Qiong

2015-03-25

A simple, inexpensive and efficient method based on the mixed cloud point extraction (MCPE) combined with high performance liquid chromatography was developed for the simultaneous separation and determination of six flavonoids (rutin, hyperoside, quercetin-3-O-sophoroside, isoquercitrin, astragalin and quercetin) in Apocynum venetum leaf samples. The non-ionic surfactant Genapol X-080 and cetyl-trimethyl ammonium bromide (CTAB) was chosen as the mixed extracting solvent. Parameters that affect the MCPE processes, such as the content of Genapol X-080 and CTAB, pH, salt content, extraction temperature and time were investigated and optimized. Under the optimized conditions, the calibration curve for six flavonoids were all linear with the correlation coefficients greater than 0.9994. The intra-day and inter-day precision (RSD) were below 8.1% and the limits of detection (LOD) for the six flavonoids were 1.2-5.0 ng mL(-1) (S/N=3). The proposed method was successfully used to separate and determine the six flavonoids in A. venetum leaf samples. Copyright © 2015 Elsevier B.V. All rights reserved.

The use of laminar tube flow in the study of hydrodynamic and chemical influences on polymer flocculation of Escherichia coli.

PubMed

Whittington, P N; George, N

1992-08-05

The optimization of microbial flocculation for subsequent biomass separation must relate the floc properties to separation process criteria. The effects of flocculant type, dose, and hydrodynamic conditions on floc formation in laminar tube flow were determined for an Escherichia coli system. Combined with an on-line aggregation sensor, this technique allows the flocculation process to be rapidly optimized. This is important, because interbatch variation in fermentation broth has consequences for flocculation control and subsequent downstream processing. Changing tube diameter and length while maintaining a constant flow rate allowed independent study of the effects of shear and time on the flocculation rate and floc characteristics. Tube flow at higher shear rates increased the rate and completeness of flocculation, but reduced the maximum floc size attained. The mechanism for this size limitation does not appear to be fracture or erosion of existing flocs. Rearrangement of particles within the flocs appears to be most likely. The Camp number predicted the extent of flocculation obtained in terms of the reduction in primary particle number, but not in terms of floc size.

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

PubMed Central

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

2014-01-01

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

Mapping the Limitations of Breakthrough Analysis in Fixed-Bed Adsorption

NASA Technical Reports Server (NTRS)

Knox, James Clinton

2017-01-01

The separation of gases through adsorption plays an important role in the chemical processing industry, where the separation step is often the costliest part of a chemical process and thus worthy of careful study and optimization. This work developed a number of new, archival aspects on the computer simulations used for the refinement and design of these gas adsorption processes: 1. Presented a new approach to fit the undetermined heat and mass transfer coefficients in the axially dispersed plug flow equation and associated balance equations 2. Examined and described the conditions where non-physical simulation results can arise 3. Presented an approach to determine the limits of the axial dispersion and LDF mass transfer terms above which non-physical simulation results occur.

Research on technology of online gas chromatograph for SF6 decomposition products

NASA Astrophysics Data System (ADS)

Li, L.; Fan, X. P.; Zhou, Y. Y.; Tang, N.; Zou, Z. L.; Liu, M. Z.; Huang, G. J.

2017-12-01

Sulfur hexafluoride (SF6) decomposition products were qualitatively and quantitatively analyzed by several gas chromatographs in the laboratory. Test conditions and methods were selected and optimized to minimize and eliminate the SF6’ influences on detection of other trace components. The effective separation and detection of selected characteristic gases were achieved. And by comparison among different types of gas chromatograph, it was found that GPTR-S101 can effectively separate and detect SF6 decomposition products and has best the best detection limit and sensitivity. On the basis of GPTR-S101, online gas chromatograph for SF6decomposition products (GPTR-S201) was developed. It lays the foundation for further online monitoring and diagnosis of SF6.

Optimizing ultrafast illumination for multiphoton-excited fluorescence imaging

PubMed Central

Stoltzfus, Caleb R.; Rebane, Aleksander

2016-01-01

We study the optimal conditions for high throughput two-photon excited fluorescence (2PEF) and three-photon excited fluorescence (3PEF) imaging using femtosecond lasers. We derive relations that allow maximization of the rate of imaging depending on the average power, pulse repetition rate, and noise characteristics of the laser, as well as on the size and structure of the sample. We perform our analysis using ~100 MHz, ~1 MHz and 1 kHz pulse rates and using both a tightly-focused illumination beam with diffraction-limited image resolution, as well loosely focused illumination with a relatively low image resolution, where the latter utilizes separate illumination and fluorescence detection beam paths. Our theoretical estimates agree with the experiments, which makes our approach especially useful for optimizing high throughput imaging of large samples with a field-of-view up to 10x10 cm2. PMID:27231620

Analytical design and evaluation of an active control system for helicopter vibration reduction and gust response alleviation

NASA Technical Reports Server (NTRS)

Taylor, R. B.; Zwicke, P. E.; Gold, P.; Miao, W.

1980-01-01

An analytical study was conducted to define the basic configuration of an active control system for helicopter vibration and gust response alleviation. The study culminated in a control system design which has two separate systems: narrow band loop for vibration reduction and wider band loop for gust response alleviation. The narrow band vibration loop utilizes the standard swashplate control configuration to input controller for the vibration loop is based on adaptive optimal control theory and is designed to adapt to any flight condition including maneuvers and transients. The prime characteristics of the vibration control system is its real time capability. The gust alleviation control system studied consists of optimal sampled data feedback gains together with an optimal one-step-ahead prediction. The prediction permits the estimation of the gust disturbance which can then be used to minimize the gust effects on the helicopter.

Thermodynamic model effects on the design and optimization of natural gas plants

DOE Office of Scientific and Technical Information (OSTI.GOV)

Diaz, S.; Zabaloy, M.; Brignole, E.A.

1999-07-01

The design and optimization of natural gas plants is carried out on the basis of process simulators. The physical property package is generally based on cubic equations of state. By rigorous thermodynamics phase equilibrium conditions, thermodynamic functions, equilibrium phase separations, work and heat are computed. The aim of this work is to analyze the NGL turboexpansion process and identify possible process computations that are more sensitive to model predictions accuracy. Three equations of state, PR, SRK and Peneloux modification, are used to study the effect of property predictions on process calculations and plant optimization. It is shown that turboexpander plantsmore » have moderate sensitivity with respect to phase equilibrium computations, but higher accuracy is required for the prediction of enthalpy and turboexpansion work. The effect of modeling CO{sub 2} solubility is also critical in mixtures with high CO{sub 2} content in the feed.« less

Combined use of [TBA][L-ASP] and hydroxypropyl-β-cyclodextrin as selectors for separation of Cinchona alkaloids by capillary electrophoresis.

PubMed

Zhang, Yu; Yu, Haixia; Wu, Yujiao; Zhao, Wenyan; Yang, Min; Jing, Huanwang; Chen, Anjia

2014-10-01

In this paper, a new capillary electrophoresis (CE) separation and detection method was developed for the chiral separation of the four major Cinchona alkaloids (quinine/quinidine and cinchonine/cinchonidine) using hydroxypropyl-β-cyclodextrin (HP-β-CD) and chiral ionic liquid ([TBA][L-ASP]) as selectors. Separation parameters such as buffer concentrations, pH, HP-β-CD and chiral ionic liquid concentrations, capillary temperature, and separation voltage were investigated. After optimization of separation conditions, baseline separation of the three analytes (cinchonidine, quinine, cinchonine) was achieved in fewer than 7 min in ammonium acetate background electrolyte (pH 5.0) with the addition of HP-β-CD in a concentration of 40 mM and [TBA][L-ASP] of 14 mM, while the baseline separation of cinchonine and quinidine was not obtained. Therefore, the first-order derivative electropherogram was applied for resolving overlapping peaks. Regression equations revealed a good linear relationship between peak areas in first-order derivative electropherograms and concentrations of the two diastereomer pairs. The results not only indicated that the first-order derivative electropherogram was effective in determination of a low content component and of those not fully separated from adjacent ones, but also showed that the ionic liquid appeared to be a very promising chiral selector in CE. Copyright © 2014 Elsevier Inc. All rights reserved.

Cationic double-chained surfactant as pseudostationary phase in micellar electrokinetic capillary chromatography for drug separations.

PubMed

Li, Yanqing; Liu, Qian; Yao, Shouzhuo

2008-05-15

The cationic double-chained surfactant didodecyldimethylammonium bromide (DDAB) was used as pseudostationary phase (PSP) in micellar electrokinetic capillary chromatography (MEKC). Its performance on the three kinds of drugs, i.e., basic, acidic, and neutral drugs, was systematically investigated. Nicotine, cotinine, caffeine, lidocaine, and procaine were selected as the model basic drugs. Good baseline separation and high efficiency were obtained under the optimal separation condition that consisted of 50mM phosphate (pH 4.0) and 0.08 mM DDAB. Three basic phenylenediamine isomers can also be well separated with DDAB in buffer. In addition, DDAB can form cationic bilayer on the capillary wall, thus the wall adsorption of basic analytes was greatly suppressed. Compared with commonly used CTAB, the separation of basic drugs was significantly improved with a much lower amount of DDAB present in the buffer. The DDAB-involved MEKC also showed superiority to CTAB upon the separation of acidic drugs, amoxicillin and ampicillin. In the case of neutral compounds, a good separation of resorcinol, 1-naphthol and 2-naphthol was achieved with 0.1mM DDAB and 30% (v/v) acetonitrile (ACN) present in buffer. Hence, it was concluded that the double-chained cationic surfactant DDAB can be a good substitute for traditional single-chained surfactant CTAB in MEKC.

Simultaneous determination of phenylethanoid glycosides and aglycones by capillary zone electrophoresis with running buffer modifier.

PubMed

Dong, Shuqing; Gao, Ruibin; Yang, Yan; Guo, Mei; Ni, Jingman; Zhao, Liang

2014-03-15

Although the separation efficiency of capillary electrophoresis (CE) is much higher than that of other chromatographic methods, it is sometimes difficult to adequately separate the complex ingredients in biological samples. This article describes how one effective and simple way to develop the separation efficiency in CE is to add some modifiers to the running buffer. The suitable running buffer modifier β-cyclodextrin (β-CD) was explored to fast and completely separate four phenylethanoid glycosides and aglycones (homovanillyl alcohol, hydroxytyrosol, 3,4-dimethoxycinnamic acid, and caffeic acid) in Lamiophlomis rotata (Lr) and Cistanche by capillary zone electrophoresis with ultraviolet (UV) detection. It was found that when β-CD was used as running buffer modifier, a baseline separation of the four analytes could be accomplished in less than 20 min and the detection limits were as low as 10(-3) mg L(-1). Other factors affecting the CE separation, such as working potential, pH value and ionic strength of running buffer, separation voltage, and sample injection time, were investigated extensively. Under the optimal conditions, a successful practical application on the determination of Lr and Cistanche samples confirmed the validity and practicability of this method. Copyright © 2014 Elsevier Inc. All rights reserved.

Size exclusion chromatography for analyses of fibroin in silk: optimization of sampling and separation conditions

NASA Astrophysics Data System (ADS)

Pawcenis, Dominika; Koperska, Monika A.; Milczarek, Jakub M.; Łojewski, Tomasz; Łojewska, Joanna

2014-02-01

A direct goal of this paper was to improve the methods of sample preparation and separation for analyses of fibroin polypeptide with the use of size exclusion chromatography (SEC). The motivation for the study arises from our interest in natural polymers included in historic textile and paper artifacts, and is a logical response to the urgent need for developing rationale-based methods for materials conservation. The first step is to develop a reliable analytical tool which would give insight into fibroin structure and its changes caused by both natural and artificial ageing. To investigate the influence of preparation conditions, two sets of artificially aged samples were prepared (with and without NaCl in sample solution) and measured by the means of SEC with multi angle laser light scattering detector. It was shown that dialysis of fibroin dissolved in LiBr solution allows removal of the salt which destroys stacks chromatographic columns and prevents reproducible analyses. Salt rich (NaCl) water solutions of fibroin improved the quality of chromatograms.

Relaxation of microparticles exposed to hydrodynamic forces in microfluidic conduits.

PubMed

Janča, Josef; Halabalová, Věra; Polášek, Vladimír; Vašina, Martin; Menshikova, Anastasia Yu

2011-02-01

The behavior of microparticles exposed to gravitational and lift forces and to the velocity gradient in flow velocity profile formed in microfluidic conduits is studied from the viewpoint of the transient period (the relaxation) between the moment at which a particle starts to be transported by the hydrodynamic flow and the time at which it reaches an equilibrium position, characterized by a balance of all active forces. The theoretical model allowing the calculation of the relaxation time is proposed. The numerical calculus based on the proposed model is compared with the experimental data obtained under different experimental conditions, namely, for different lengths of microfluidic channels, different average linear velocities of the carrier liquid, and different sizes and densities of the particles used in the study. The results are important for the optimization of microfluidic separation units such as microthermal field-flow fractionation channels in which the separation or manipulation of the microparticles of various origin, synthetic, natural, biological, etc., is performed under similar experimental conditions but by applying an additional thermodynamic force.

Solvent microextraction-flame atomic absorption spectrometry (SME-FAAS) for determination of ultratrace amounts of cadmium in meat and fish samples.

PubMed

Goudarzi, Nasser

2009-02-11

A simple, low cost and highly sensitive method based on solvent microextraction (SME) for separation/preconcentration and flame atomic absorption spectrometry (FAAS) was proposed for the determination of ultratrace amounts of cadmium in meat and fish samples. The analytical procedure involved the formation of a hydrophobic complex by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution. In suitable conditions, the complex of cadmium-APDC entered the micro organic phase, and thus, separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, a detection limit (3 sigma) of 0.8 ng L(-1) and an enrichment factor of 93 were achieved. The relative standard deviation for the method was found to be 2.2% for Cd. The interference effects of some anions and cations were also investigated. The developed method has been applied to the determination of trace Cd in meat and fish samples.

[Application of asymmetrical flow field-flow fractionation for size characterization of low density lipoprotein in egg yolk plasma].

PubMed

Zhang, Wenhui; Cai, Chunxue; Wang, Jing; Mao, Zhen; Li, Yueqiu; Ding, Liang; Shen, Shigang; Dou, Haiyang

2017-08-08

Home-made asymmetrical flow field-flow fractionation (AF4) system, online coupled with ultraviolet/visible (UV/Vis) detector was employed for the separation and size characterization of low density lipoprotein (LDL) in egg yolk plasma. At close to natural condition of egg yolk, the effects of cross flow rate, sample loading, and type of membrane on the size distribution of LDL were investigated. Under the optimal operation conditions, AF4-UV/Vis provides the size distribution of LDL. Moreover, the precision of AF4-UV/Vis method proposed in this work for the analysis of LDL in egg yolk plasma was evaluated. The intra-day precisions were 1.3% and 1.9% ( n =7) and the inter-day precisions were 2.4% and 2.3% ( n =7) for the elution peak height and elution peak area of LDL, respectively. Results reveal that AF4-UV/Vis is a useful tool for the separation and size characterization of LDL in egg yolk plasma.

N-representability-driven reconstruction of the two-electron reduced-density matrix for a real-time time-dependent electronic structure method

NASA Astrophysics Data System (ADS)

Jeffcoat, David B.; DePrince, A. Eugene

2014-12-01

Propagating the equations of motion (EOM) for the one-electron reduced-density matrix (1-RDM) requires knowledge of the corresponding two-electron RDM (2-RDM). We show that the indeterminacy of this expression can be removed through a constrained optimization that resembles the variational optimization of the ground-state 2-RDM subject to a set of known N-representability conditions. Electronic excitation energies can then be obtained by propagating the EOM for the 1-RDM and following the dipole moment after the system interacts with an oscillating external electric field. For simple systems with well-separated excited states whose symmetry differs from that of the ground state, excitation energies obtained from this method are comparable to those obtained from full configuration interaction computations. Although the optimized 2-RDM satisfies necessary N-representability conditions, the procedure cannot guarantee a unique mapping from the 1-RDM to the 2-RDM. This deficiency is evident in the mean-field-quality description of transitions to states of the same symmetry as the ground state, as well as in the inability of the method to describe Rabi oscillations.

Signal enhancement for peptide analysis in liquid chromatography-electrospray ionization mass spectrometry with trifluoroacetic acid containing mobile phase by postcolumn electrophoretic mobility control.

PubMed

Wang, Nan-Hsuan; Lee, Wan-Li; Her, Guor-Rong

2011-08-15

A strategy based on postcolumn electrophoretic mobility control (EMC) was developed to alleviate the adverse effect of trifluoroacetic acid (TFA) on the liquid chromatography-mass spectrometry (LC-MS) analysis of peptides. The device created to achieve this goal consisted of a poly(dimethylsiloxane) (PDMS)-based junction reservoir, a short connecting capillary, and an electrospray ionization (ESI) sprayer connected to the outlet of the high-performance liquid chromatography (HPLC) column. By apply different voltages to the junction reservoir and the ESI emitter, an electric field was created across the connecting capillary. Due to the electric field, positively charged peptides migrated toward the ESI sprayer, whereas TFA anions remained in the junction reservoir and were removed from the ionization process. Because TFA did not enter the ESI source, ion suppression from TFA was alleviated. Operation of the postcolumn device was optimized using a peptide standard mixture. Under optimized conditions, signals for the peptides were enhanced 9-35-fold without a compromise in separation efficiency. The optimized conditions were also applied to the LC-MS analysis of a tryptic digest of bovine serum albumin.

Timing resolution and time walk in super low K factor single-photon avalanche diode-measurement and optimization

NASA Astrophysics Data System (ADS)

Fong, Bernicy S.; Davies, Murray; Deschamps, Pierre

2018-01-01

Timing resolution (or timing jitter) and time walk are separate parameters associated with a detector's response time. Studies have been done mostly on the time resolution of various single-photon detectors. As the designer and manufacturer of the ultra-low noise (ƙ-factor) silicon avalanche photodiode the super low K factor (SLiK) single-photon avalanche diode (SPAD), which is used in many single-photon counting applications, we often get inquiries from customers to better understand how this detector behaves under different operating conditions. Hence, here, we will be focusing on the study of these time-related parameters specifically for the SLiK SPAD, as a way to provide the most direct information for users of this detector to help with its use more efficiently and effectively. We will be providing the study data on how these parameters can be affected by temperature (both intrinsic to the detector chip and environmental input based on operating conditions), operating voltage, photon wavelength, as well as light spot size. How these parameters can be optimized and the trade-offs from optimization from the desired performance will be presented?

A facile and efficient single-step approach for the fabrication of vancomycin functionalized polymer-based monolith as chiral stationary phase for nano-liquid chromatography.

PubMed

Xu, Dongsheng; Shao, Huikai; Luo, Rongying; Wang, Qiqin; Sánchez-López, Elena; Fanali, Salvatore; Marina, Maria Luisa; Jiang, Zhengjin

2018-07-06

A facile single-step preparation strategy for fabricating vancomycin functionalized organic polymer-based monolith within 100μm fused-silica capillary was developed. The synthetic chiral functional monomer, i.e 2-isocyanatoethyl methacrylate (ICNEML) derivative of vancomycin, was co-polymerized with the cross-linker ethylene dimethacrylate (EDMA) in the presence of methanol and dimethyl sulfoxide as the selected porogens. The co-polymerization conditions were systematically optimized in order to obtain satisfactory column performance. Adequate permeability, stability and column morphology were observed for the optimized poly(ICNEML-vancomycin-co-EDMA) monolith. A series of chiral drugs were evaluated on the monolith in either polar organic-phase or reversed-phase modes. After the optimization of separation conditions, baseline or partial enantioseparation were obtained for series of drugs including thalidomide, colchicine, carteolol, salbutamol, clenbuterol and several other β-blockers. The proposed single-step approach not only resulted in a vancomycin functionalized organic polymer-based monolith with acceptable performance, but also significantly simplified the preparation procedure by reducing time and labor. Copyright © 2018 Elsevier B.V. All rights reserved.

Stratification and segregation features of pulverized electronic waste in flowing film concentration.

PubMed

Vidyadhar, A; Chalavadi, G; Das, A

2013-03-30

Gravity separation of metals from plastics in pulverized e-waste using flowing film concentration in a shaking table was investigated. Over 51% rejection of plastics in a single stage operation was achieved under optimum conditions. The shaking table was shown to be suitable for processing ground PCBs. Pulverized e-waste containing 22% metals was enriched to around 40% metals in a single pass. Statistical models for the mass yield of metal-rich stream and its grade were developed by design of experiments. Optimization was carried out to maximize the mass yield at a target product grade and preferred operating regimes were established. Experiments were designed to prevent metal loss and over 95% recovery values were obtained under all conditions. Settling distances of metals and plastics were computed and shown to be good indicators of separation performance. Particle morphology and stratification in the troughs in between the riffles were shown to influence the separation significantly. Water flow-assisted motion of the plastics was captured and its role in determining the effectiveness of separation was described. The efficacy of tabling was well established for treating ground PCBs. The wet process was shown to be environment friendly and sustainable. It is also relatively cheap and has good potential for industrial application. However, rigorous cost estimates will be required before commercial application. Copyright © 2013 Elsevier Ltd. All rights reserved.

Separation of the fatty acids in menhaden oil as methyl esters with a highly polar ionic liquid gas chromatographic column and identification by time of flight mass spectrometry.

PubMed

Fardin-Kia, Ali Reza; Delmonte, Pierluigi; Kramer, John K G; Jahreis, Gerhard; Kuhnt, Katrin; Santercole, Viviana; Rader, Jeanne I

2013-12-01

The fatty acids contained in marine oils or products are traditionally analyzed by gas chromatography using capillary columns coated with polyethylene glycol phases. Recent reports indicate that 100 % cyanopropyl siloxane phases should also be used when the analyzed samples contain trans fatty acids. We investigated the separation of the fatty acid methyl esters prepared from menhaden oil using the more polar SLB-IL111 (200 m × 0.25 mm) ionic liquid capillary column and the chromatographic conditions previously optimized for the separation of the complex mixture of fatty acid methyl esters prepared from milk fat. Identifications of fatty acids were achieved by applying Ag(+)-HPLC fractionation and GC-TOF/MS analysis in CI(+) mode with isobutane as the ionization reagent. Calculation of equivalent chain lengths confirmed the assignment of double bond positions. This methodology allowed the identification of 125 fatty acids in menhaden oil, including isoprenoid and furanoid fatty acids, and the novel 7-methyl-6-hexadecenoic and 7-methyl-6-octadecenoic fatty acids. The chromatographic conditions applied in this study showed the potential of separating in a single 90-min analysis, among others, the short chain and trans fatty acids contained in dairy products, and the polyunsaturated fatty acids contained in marine products.

Circadian clocks, feeding time, and metabolic homeostasis

PubMed Central

Paschos, Georgios K.

2015-01-01

Metabolic processes exhibit diurnal variation from cyanobacteria to humans. The circadian clock is thought to have evolved as a time keeping system for the cell to optimize the timing of metabolic events according to physiological needs and environmental conditions. Circadian rhythms temporally separate incompatible cellular processes and optimize cellular and organismal fitness. A modern 24 h lifestyle can run at odds with the circadian rhythm dictated by our molecular clocks and create desynchrony between internal and external timing. It has been suggested that this desynchrony compromises metabolic homeostasis and may promote the development of obesity (Morris et al., 2012). Here we review the evidence supporting the association between circadian misalignment and metabolic homeostasis and discuss the role of feeding time. PMID:26082718

Optimization of the Ultrasonic-Assisted Extraction of Bioactive Flavonoids from Ampelopsis grossedentata and Subsequent Separation and Purification of Two Flavonoid Aglycones by High-Speed Counter-Current Chromatography.

PubMed

Zhang, Hongbing; Xie, Guoyong; Tian, Mei; Pu, Qian; Qin, Minjian

2016-08-20

The fermented leaf of Ampelopsis grossedentata has been used as a beverage and folk medicine called "vine tea" in the southern region of China. In this paper, the optimum extraction conditions for the maximum recovery amounts of total flavonoids (TF), dihydromyricetin (DMY), myricitrin (MYG) and myricetin (MY) from natural Ampelopsis grossedentata leaves subjected to ultrasonic-assisted extraction (UAE) were determined and optimized by using response surface methodology. The method was employed by the Box-Behnken design (BBD) and Derringer's desirability function using methanol concentration, extraction time, liquid/solid ratio as factors and the contents of TF, DMY, MYG and MY as responses. The obtained optimum UAE conditions were as follows: a solvent of 80.87% methanol, an extraction time of 31.98 min and a liquid/solid ratio of 41.64:1 mL/g. Through analysis of the response surface, it implied that methanol concentration and the liquid/solid ratio had significant effects on TF, DMY, MYG and MY yields, whereas extraction time had relatively little effects. The established extraction and analytical methods were successfully applied to determine the contents of the total flavonoids and three individual flavonoids in 10 batches of the leaf samples of A. grossedentata from three counties in Fujian Province, China. The results suggested the variability in the quality of A. grossedentata leaves from different origins. In addition, high purities of dihydromyricetin and myricetin were simultaneously separated and purified from the extract subjected to optimized UAE, by high-speed counter-current chromatography using a solvent system of N-hexane-ethyl acetate-methanol-water (1:3:2:4; v/v/v/v). In a single operation, 200 mg of the extract were separated to yield 86.46 mg of dihydromyricetin and 3.61 mg of myricetin with the purity of 95.03% and 99.21%, respectively. The results would be beneficial for further exploiting the herbal products and controlling the quality of the herb and its derived products.

Empowering leaders optimize working conditions for engagement: a multilevel study.

PubMed

Tuckey, Michelle R; Bakker, Arnold B; Dollard, Maureen F

2012-01-01

Using a multilevel framework, this study examined the role of empowering leadership at the group level by fire brigade captains in facilitating the individual level motivational processes that underpin work engagement in volunteer firefighters. Anonymous mail surveys were completed by 540 volunteer firefighters from 68 fire brigades and, separately, by 68 brigade captains. As predicted on the basis of the Job Demands-Resources model, increased levels of cognitive demands and cognitive resources partially mediated the relationship between empowering leadership and work engagement. In a three-way Leadership × Demands × Resources interaction, empowering leadership also had the effect of optimizing working conditions for engagement by strengthening the positive effect of a work context in which both cognitive demands and cognitive resources were high. Our findings shed light on a process through which leaders can empower workers and enhance well-being: via their influence on and interaction with the work environment. They also underscore the need to examine work engagement from a multilevel theoretical perspective.

Development of a 5.5 m diameter vertical axis wind turbine, phase 3

NASA Astrophysics Data System (ADS)

Dekitsch, A.; Etzler, C. C.; Fritzsche, A.; Lorch, G.; Mueller, W.; Rogalla, K.; Schmelzle, J.; Schuhwerk, W.; Vollan, A.; Welte, D.

1982-06-01

In continuation of development of a 5.5 m diameter vertical axis windmill that consists in conception, building, and wind tunnel testing, a Darrieus rotor windpowered generator feeding an isolated network under different wind velocity conditions and with optimal energy conversion efficiency was designed built, and field tested. The three-bladed Darrieus rotor tested in the wind tunnel was equiped with two variable pitch Savonius rotors 2 m in diameter. By means of separate measures of the aerodynamic factors and the energy consumption, effect of revisions and optimizations on different elements was assessed. Pitch adjustement of the Savonius blades, lubrication of speed reducer, rotor speed at cut-in of generator field excitation, time constant of field excitation, stability conditions, switch points of ohmic resistors which combined with a small electric battery simulated a larger isolated network connected with a large storage battery, were investigated. Fundamentals for the economic series production of windpowered generators with Darrieus rotors for the control and the electric conversion system are presented.

Quality by Design in the development of hydrophilic interaction liquid chromatography method with gradient elution for the analysis of olanzapine.

PubMed

Tumpa, Anja; Stajić, Ana; Jančić-Stojanović, Biljana; Medenica, Mirjana

2017-02-05

This paper deals with the development of hydrophilic interaction liquid chromatography (HILIC) method with gradient elution, in accordance with Analytical Quality by Design (AQbD) methodology, for the first time. The method is developed for olanzapine and its seven related substances. Following step by step AQbD methodology, firstly as critical process parameters (CPPs) temperature, starting content of aqueous phase and duration of linear gradient are recognized, and as critical quality attributes (CQAs) separation criterion S of critical pairs of substances are investigated. Rechtschaffen design is used for the creation of models that describe the dependence between CPPs and CQAs. The design space that is obtained at the end is used for choosing the optimal conditions (set point). The method is fully validated at the end to verify the adequacy of the chosen optimal conditions and applied to real samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Enrichment and Purification of Syringin, Eleutheroside E and Isofraxidin from Acanthopanax senticosus by Macroporous Resin

PubMed Central

Yang, Fengjian; Yang, Lei; Wang, Wenjie; Liu, Yang; Zhao, Chunjian; Zu, Yuangang

2012-01-01

In order to screen a suitable resin for the preparative simultaneous separation and purification of syringin, eleutheroside E and isofraxidin from Acanthopanax senticosus, the adsorption and desorption properties of 17 widely used commercial macroporous resins were evaluated. According to our results, HPD100C, which adsorbs by the molecular tiers model, was the best macroporous resin, offering higher adsorption and desorption capacities and higher adsorption speed for syringin, eleutheroside E and isofraxidin than other resins. Dynamic adsorption and desorption tests were carried out to optimize the process parameters. The optimal conditions were as follows: for adsorption, processing volume: 24 BV, flow rate: 2 BV/h; for desorption, ethanol–water solution: 60:40 (v/v), eluent volume: 4 BV, flow rate: 3 BV/h. Under the above conditions, the contents of syringin, eleutheroside E and isofraxidin increased 174-fold, 20-fold and 5-fold and their recoveries were 80.93%, 93.97% and 93.79%, respectively. PMID:22942746

Simultaneous polarized neutron reflectometry and anisotropic magnetoresistance measurements.

PubMed

Demeter, J; Teichert, A; Kiefer, K; Wallacher, D; Ryll, H; Menéndez, E; Paramanik, D; Steitz, R; Van Haesendonck, C; Vantomme, A; Temst, K

2011-03-01

A novel experimental facility to carry out simultaneous polarized neutron reflectometry (PNR) and anisotropic magnetoresistance (AMR) measurements is presented. Performing both techniques at the same time increases their strength considerably. The proof of concept of this method is demonstrated on a CoO/Co bilayer exchange bias system. Although information on the same phenomena, such as the coercivity or the reversal mechanism, can be separately obtained from either of these techniques, the simultaneous application optimizes the consistency between both. In this way, possible differences in experimental conditions, such as applied magnetic field amplitude and orientation, sample temperature, magnetic history, etc., can be ruled out. Consequently, only differences in the fundamental sensitivities of the techniques can cause discrepancies in the interpretation between the two. The almost instantaneous information obtained from AMR can be used to reveal time-dependent effects during the PNR acquisition. Moreover, the information inferred from the AMR measurements can be used for optimizing the experimental conditions for the PNR measurements in a more efficient way than with the PNR measurements alone.

Optimal rendezvous in the neighborhood of a circular orbit

NASA Technical Reports Server (NTRS)

Jones, J. B.

1975-01-01

The minimum velocity change rendezvous solutions, when the motion may be linearized about a circular orbit, fall into two separate regions; the phase-for-free region and the general region. Phase-for-free solutions are derived from the optimum transfer solutions, require the same velocity change expenditure, but may not be unique. Analytic solutions are presented in two of the three subregions. An algorithm is presented for determining the unique solutions in the general region. Various sources of initial conditions are discussed and three examples presented.

Combined use of algorithms for peak picking, peak tracking and retention modelling to optimize the chromatographic conditions for liquid chromatography-mass spectrometry analysis of fluocinolone acetonide and its degradation products.

PubMed

Fredriksson, Mattias J; Petersson, Patrik; Axelsson, Bengt-Olof; Bylund, Dan

2011-10-17

A strategy for rapid optimization of liquid chromatography column temperature and gradient shape is presented. The optimization as such is based on the well established retention and peak width models implemented in software like e.g. DryLab and LC simulator. The novel part of the strategy is a highly automated processing algorithm for detection and tracking of chromatographic peaks in noisy liquid chromatography-mass spectrometry (LC-MS) data. The strategy is presented and visualized by the optimization of the separation of two degradants present in ultraviolet (UV) exposed fluocinolone acetonide. It should be stressed, however, that it can be utilized for LC-MS analysis of any sample and application where several runs are conducted on the same sample. In the application presented, 30 components that were difficult or impossible to detect in the UV data could be automatically detected and tracked in the MS data by using the proposed strategy. The number of correctly tracked components was above 95%. Using the parameters from the reconstructed data sets to the model gave good agreement between predicted and observed retention times at optimal conditions. The area of the smallest tracked component was estimated to 0.08% compared to the main component, a level relevant for the characterization of impurities in the pharmaceutical industry. Copyright © 2011 Elsevier B.V. All rights reserved.

Optimization of a reversed-phase-high-performance thin-layer chromatography method for the separation of isoniazid, ethambutol, rifampicin and pyrazinamide in fixed-dose combination antituberculosis tablets.

PubMed

Shewiyo, D H; Kaale, E; Risha, P G; Dejaegher, B; Smeyers-Verbeke, J; Vander Heyden, Y

2012-10-19

This paper presents the development of a new RP-HPTLC method for the separation of pyrazinamide, isoniazid, rifampicin and ethambutol in a four fixed-dose combination (4 FDC) tablet formulation. It is a single method with two steps in which after plate development pyrazinamide, isoniazid and rifampicin are detected at an UV wavelength of 280 nm. Then ethambutol is derivatized and detected at a VIS wavelength of 450 nm. Methanol, ethanol and propan-1-ol were evaluated modifiers to form alcohol-water mobile phases. Systematic optimization of the composition of each alcohol in the mobile phase was carried out using the window diagramming concept to obtain the best separation. Examination of the Rf distribution of the separated compounds showed that separation of the compounds with the mobile phase containing ethanol at the optimal fraction was almost situated within the optimal Rf-values region of 0.20-0.80. Therefore, ethanol was selected as organic modifier and the optimal mobile phase composition was found to be ethanol, water, glacial acetic acid (>99% acetic acid) and 37% ammonia solution (70/30/5/1, v/v/v/v). The method is new, quick and cheap compared to the actual method in the International Pharmacopoeia for the assay of the 4 FDC tablets, which involves the use of two separate HPLC methods. Copyright © 2012 Elsevier B.V. All rights reserved.

Quantitative analysis of pyoluteorin in anti-fungal fermentation liquor of Pseudomonas species by capillary zone electrophoresis with UV-vis detector.

PubMed

Wang, Qiu-Ling; Zhang, Xue-Hong; Fan, Liu-Yin; Zhang, Wei; Xu, Yu-Qian; Hu, Hong-Bo; Cao, Cheng-Xi

2005-11-05

This paper investigated potential utility of capillary zone electrophoresis (CZE) for very succinct but robust quantitative analysis of pyoluteorin (Plt) in anti-fungal fermentation liquor of Pseudomonas species. The experimental conditions for the separation and quantification of Plt were optimized at first. The optimized conditions are: 80 mmol/L pH 8.40 Gly-NaOH buffer, 51 cm total length (42 cm effective) and 75 microm I.D. capillary, 230 nm wavelength, 25 kV, 13 mbar 10s pressure sample injection and 24 degrees C air-cooling. Under the optimized conditions, the migration times of Plt and the internal standard phenobarbital are 2.09 and 2.49 min, respectively, the linear response of Plt concentration ranges from 5.0 to 1000 microg/mL with high correlation coefficient (r=0.99977, n=9), the limits of detection (LOD) and quantification (LOQ) for Plt are 0.66 and 2.2 microg/mL, the precision values (expressed as R.S.D.) of intra- and inter-day are 1.19-1.94% and 1.55-6.21%, respectively, the recoveries of Plt at three concentration levels of 750, 250 and 50 microg/mL range from 90.31% to 97.85% and to 98.96%, respectively. The developed method can be well used for the quantification of Plt in the fermentation liquor.

Optimization process condition for deacidification of palm oil by liquid-liquid extraction using NADES (Natural Deep Eutectic Solvent)

NASA Astrophysics Data System (ADS)

Israyandi, Zahrina, Ida; Mulia, Kamarza

2017-03-01

One of many steps in palm oil refining process is deacidification which aims to separate free fatty acids and other compounds from the oil. The deacidification process was using a green solvent, known as NADES, that consisted of betaine monohydrate and propionic acid at molar ratio of 1:8. In this study, the process conditions were optimized using the response surface method (RSM) through central composite design in order to predict the maximum distribution coefficient of palmitic acid. The obtained regression equation of the basic model for optimization was: y = 0.717 + 0.003x1 + 0.043 x2 + 0.148x3 - 0.005 x1x1 - 0.030 x2x2 + 0.047 x3x3 - 0.008 x1x2 + 0.008 x1x3 + 0.033 x2x3. The independent variables are x1 ≡ temperature (40, 60, 80 °C), x2≡ amount of palmitic acid in the palm oil (2, 5, 8 %) and x3 ≡ mass ratios of oil to NADES (1:2, 1:1, 2:1). The optimum process condition found was temperature of 62.3°C, palmitic acid content of 8%, and NADES to palm oil mass ratio of 1:2, resulting in the maximum distribution coefficient of 0.96.

Innovative high-performance liquid chromatography method development for the screening of 19 antimalarial drugs based on a generic approach, using design of experiments, independent component analysis and design space.

PubMed

Debrus, B; Lebrun, P; Kindenge, J Mbinze; Lecomte, F; Ceccato, A; Caliaro, G; Mbay, J Mavar Tayey; Boulanger, B; Marini, R D; Rozet, E; Hubert, Ph

2011-08-05

An innovative methodology based on design of experiments (DoE), independent component analysis (ICA) and design space (DS) was developed in previous works and was tested out with a mixture of 19 antimalarial drugs. This global LC method development methodology (i.e. DoE-ICA-DS) was used to optimize the separation of 19 antimalarial drugs to obtain a screening method. DoE-ICA-DS methodology is fully compliant with the current trend of quality by design. DoE was used to define the set of experiments to model the retention times at the beginning, the apex and the end of each peak. Furthermore, ICA was used to numerically separate coeluting peaks and estimate their unbiased retention times. Gradient time, temperature and pH were selected as the factors of a full factorial design. These retention times were modelled by stepwise multiple linear regressions. A recently introduced critical quality attribute, namely the separation criterion (S), was also used to assess the quality of separations rather than using the resolution. Furthermore, the resulting mathematical models were also studied from a chromatographic point of view to understand and investigate the chromatographic behaviour of each compound. Good adequacies were found between the mathematical models and the expected chromatographic behaviours predicted by chromatographic theory. Finally, focusing at quality risk management, the DS was computed as the multidimensional subspace where the probability for the separation criterion to lie in acceptance limits was higher than a defined quality level. The DS was computed propagating the prediction error from the modelled responses to the quality criterion using Monte Carlo simulations. DoE-ICA-DS allowed encountering optimal operating conditions to obtain a robust screening method for the 19 considered antimalarial drugs in the framework of the fight against counterfeit medicines. Moreover and only on the basis of the same data set, a dedicated method for the determination of three antimalarial compounds in a pharmaceutical formulation was optimized to demonstrate both the efficiency and flexibility of the methodology proposed in the present study. Copyright © 2011 Elsevier B.V. All rights reserved.

Numerical modeling and optimization of the Iguassu gas centrifuge

NASA Astrophysics Data System (ADS)

Bogovalov, S. V.; Borman, V. D.; Borisevich, V. D.; Tronin, V. N.; Tronin, I. V.

2017-07-01

The full procedure of the numerical calculation of the optimized parameters of the Iguassu gas centrifuge (GC) is under discussion. The procedure consists of a few steps. On the first step the problem of a hydrodynamical flow of the gas in the rotating rotor of the GC is solved numerically. On the second step the problem of diffusion of the binary mixture of isotopes is solved. The separation power of the gas centrifuge is calculated after that. On the last step the time consuming procedure of optimization of the GC is performed providing us the maximum of the separation power. The optimization is based on the BOBYQA method exploring the results of numerical simulations of the hydrodynamics and diffusion of the mixture of isotopes. Fast convergence of calculations is achieved due to exploring of a direct solver at the solution of the hydrodynamical and diffusion parts of the problem. Optimized separative power and optimal internal parameters of the Iguassu GC with 1 m rotor were calculated using the developed approach. Optimization procedure converges in 45 iterations taking 811 minutes.

The optimization air separation plants for combined cycle MHD-power plant applications

NASA Technical Reports Server (NTRS)

Juhasz, A. J.; Springmann, H.; Greenberg, R.

1980-01-01

Some of the design approaches being employed during a current supported study directed at developing an improved air separation process for the production of oxygen enriched air for magnetohydrodynamics (MHD) combustion are outlined. The ultimate objective is to arrive at conceptual designs of air separation plants, optimized for minimum specific power consumption and capital investment costs, for integration with MHD combined cycle power plants.

X-ray Intermolecular Structure Factor (XISF): separation of intra- and intermolecular interactions from total X-ray scattering data

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mou, Q.; Benmore, C. J.; Yarger, J. L.

2015-06-01

XISF is a MATLAB program developed to separate intermolecular structure factors from total X-ray scattering structure factors for molecular liquids and amorphous solids. The program is built on a trust-region-reflective optimization routine with the r.m.s. deviations of atoms physically constrained. XISF has been optimized for performance and can separate intermolecular structure factors of complex molecules.

X-ray Intermolecular Structure Factor ( XISF ): separation of intra- and intermolecular interactions from total X-ray scattering data

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mou, Q.; Benmore, C. J.; Yarger, J. L.

2015-05-09

XISFis a MATLAB program developed to separate intermolecular structure factors from total X-ray scattering structure factors for molecular liquids and amorphous solids. The program is built on a trust-region-reflective optimization routine with the r.m.s. deviations of atoms physically constrained.XISFhas been optimized for performance and can separate intermolecular structure factors of complex molecules.

An effective and comprehensive model for optimal rehabilitation of separate sanitary sewer systems.

PubMed

Diogo, António Freire; Barros, Luís Tiago; Santos, Joana; Temido, Jorge Santos

2018-01-15

In the field of rehabilitation of separate sanitary sewer systems, a large number of technical, environmental, and economic aspects are often relevant in the decision-making process, which may be modelled as a multi-objective optimization problem. Examples are those related with the operation and assessment of networks, optimization of structural, hydraulic, sanitary, and environmental performance, rehabilitation programmes, and execution works. In particular, the cost of investment, operation and maintenance needed to reduce or eliminate Infiltration from the underground water table and Inflows of storm water surface runoff (I/I) using rehabilitation techniques or related methods can be significantly lower than the cost of transporting and treating these flows throughout the lifespan of the systems or period studied. This paper presents a comprehensive I/I cost-benefit approach for rehabilitation that explicitly considers all elements of the systems and shows how the approximation is incorporated as an objective function in a general evolutionary multi-objective optimization model. It takes into account network performance and wastewater treatment costs, average values of several input variables, and rates that can reflect the adoption of different predictable or limiting scenarios. The approach can be used as a practical and fast tool to support decision-making in sewer network rehabilitation in any phase of a project. The fundamental aspects, modelling, implementation details and preliminary results of a two-objective optimization rehabilitation model using a genetic algorithm, with a second objective function related to the structural condition of the network and the service failure risk, are presented. The basic approach is applied to three real world cases studies of sanitary sewerage systems in Coimbra and the results show the simplicity, suitability, effectiveness, and usefulness of the approximation implemented and of the objective function proposed. Copyright © 2017 Elsevier B.V. All rights reserved.

Dispersive solid phase microextraction with magnetic graphene oxide as the sorbent for separation and preconcentration of ultra-trace amounts of gold ions.

PubMed

Kazemi, Elahe; Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad

2015-08-15

A selective, simple and rapid dispersive solid phase microextraction was developed using magnetic graphene oxide (MGO) as an efficient sorbent for the separation and preconcentration of gold ions. The MGO was synthesized by means of the simple one step chemical coprecipitation method, characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). Gold ions retained by the sorbent were eluted using 0.5mol L(-)(1) thiourea in 0.1mol L(-1) HCl solution and determined by the flow injection flame atomic absorption spectrometry (FI-FAAS). The factors affecting the separation and preconcentration of gold were investigated and optimized. Under the optimized conditions, the method exhibited a linear dynamic range of 0.02-100.0µg L(-)(1) with a detection limit of 4ng L(-1) and an enrichment factor of 500. The relative standard deviations of 3.2% and 4.7% (n=6) were obtained at 20µg L(-1) level of gold ions for the intra and the inter day analysis, respectively. The method was successfully applied to the determination of gold ions in water and waste water samples as well as a certified reference material (CCU-1b, copper flotation concentrate). Copyright © 2015 Elsevier B.V. All rights reserved.

The key to success: Gelled-electrolyte and optimized separators for stationary lead-acid batteries

NASA Astrophysics Data System (ADS)

Toniazzo, Valérie

The lead acid technology is nowadays considered one of the best suited for stationary applications. Both gel and AGM batteries are complementary technologies and can provide reliability and efficiency due to the constant optimization of the battery design and components. However, gelled-electrolyte batteries remain the preferred technology due to a better manufacturing background and show better performance mainly at low and moderate discharge rates. Especially, using the gel technology allows to get rid of the numerous problems encountered in most AGM batteries: drainage, stratification, short circuits due to dendrites, and mostly premature capacity loss due to the release of internal cell compression. These limitations are the result of the evident lack of an optimal separation system. In gel batteries, on the contrary, highly efficient polymeric separators are nowadays available. Especially, microporous separators based on PVC and silica have shown the best efficiency for nearly 30 years all over the world, and especially in Europe, where the gel technology was born. The improved performance of these separators is explained by the unique extrusion process, which leads to excellent wettability, and optimized physical properties. Because they are the key for the battery success, continuous research and development on separators have led to improved properties, which render the separator even better adapted to the more recent gel technology: the pore size distribution has been optimized to allow good oxygen transfer while avoiding dendrite growth, the pore volume has been increased, the electrical resistance and acid displacement reduced to such an extent that the electrical output of batteries has been raised both in terms of higher capacity and longer cycle life.

Optimization and modeling of reduction of wastewater sludge water content and turbidity removal using magnetic iron oxide nanoparticles (MION).

PubMed

Hwang, Jeong-Ha; Han, Dong-Woo

2015-01-01

Economic and rapid reduction of sludge water content in sewage wastewater is difficult and requires special advanced treatment technologies. This study focused on optimizing and modeling decreased sludge water content (Y1) and removing turbidity (Y2) with magnetic iron oxide nanoparticles (Fe3O4, MION) using a central composite design (CCD) and response surface methodology (RSM). CCD and RSM were applied to evaluate and optimize the interactive effects of mixing time (X1) and MION concentration (X2) on chemical flocculent performance. The results show that the optimum conditions were 14.1 min and 22.1 mg L(-1) for response Y1 and 16.8 min and 8.85 mg L(-1) for response Y2, respectively. The two responses were obtained experimentally under this optimal scheme and fit the model predictions well (R(2) = 97.2% for Y1 and R(2) = 96.9% for Y2). A 90.8% decrease in sludge water content and turbidity removal of 29.4% were demonstrated. These results confirm that the statistical models were reliable, and that the magnetic flocculation conditions for decreasing sludge water content and removing turbidity from sewage wastewater were appropriate. The results reveal that MION are efficient for rapid separation and are a suitable alterative to sediment sludge during the wastewater treatment process.

Continuous high throughput molecular adhesion based cell sorting using ridged microchannels

NASA Astrophysics Data System (ADS)

Tasadduq, Bushra; Wang, Gonghao; Alexeev, Alexander; Sarioglu, Ali Fatih; Sulchek, Todd

2016-11-01

Cell molecular interactions govern important physiological processes such as stem cell homing, inflammation and cancer metastasis. But due to a lack of effective separation technologies selective to these interactions it is challenging to specifically sort cells. Other label free separation techniques based on size, stiffness and shape do not provide enough specificity to cell type, and correlation to clinical condition. We propose a novel microfluidic device capable of high throughput molecule dependent separation of cells by flowing them through a microchannel decorated with molecule specific coated ridges. The unique aspect of this sorting design is the use of optimized gap size which is small enough to lightly squeeze the cells while flowing under the ridged part of the channel to increase the surface area for interaction between the ligand on cell surface and coated receptor molecule but large enough so that biomechanical markers, stiffness and viscoelasticity, do not dominate the cell separation mechanism. We are able to separate Jurkat cells based on its expression of PSGL-1ligand using ridged channel coated with P selectin at a flow rate of 0.045ml/min and achieve 2-fold and 5-fold enrichment of PSGL-1 positive and negative Jurkat cells respectively.

Synthesis and Photophysical Characterization of an Artificial Photosynthetic Reaction Center Exhibiting Acid-Responsive Regulation of Charge Separation

NASA Astrophysics Data System (ADS)

Pahk, Ian

Non-photochemical quenching (NPQ) is a photoprotective regulatory mechanism essential to the robustness of the photosynthetic apparatus of green plants. Energy flow within the low-light adapted reaction centers is dynamically optimized to match the continuously fluctuating light conditions found in nature. Activated by compartmentalized decreases in pH resulting from photosynthetic activity during periods of elevated photon flux, NPQ induces rapid thermal dissipation of excess excitation energy that would otherwise overwhelm the apparatus's ability to consume it. Consequently, the frequency of charge separation decreases and the formation of potentially deleterious, high-energy intermediates slows, thereby reducing the threat of photodamage by disallowing their accumulation. Herein is described the synthesis and photophysical analysis of a molecular triad that mimics the effects of NPQ on charge separation within the photosynthetic reaction centers. Steady-state absorption and emission, time-resolved fluorescence, and transient absorption spectroscopies were used to demonstrate reversible quenching of the first singlet excited state affecting the quantum yield of charge separation by approximately one order of magnitude. As in the natural system, the populations of unquenched and quenched states and, therefore, the overall yields of charge separation were found to be dependent upon acid concentration.

Wall effects in continuous microfluidic magneto-affinity cell separation.

PubMed

Wu, Liqun; Zhang, Yong; Palaniapan, Moorthi; Roy, Partha

2010-05-01

Continuous microfluidic magneto-affinity cell separator combines unique microscale flow phenomenon with advantageous nanobead properties, to isolate cells with high specificity. Owing to the comparable size of the cell-bead complexes and the microchannels, the walls of the microchannel exert a strong influence on the separation of cells by this method. We present a theoretical and experimental study that provides a quantitative description of hydrodynamic wall interactions and wall rolling velocity of cells. A transient convection model describes the transport of cells in two-phase microfluidic flow under the influence of an external magnetic field. Transport of cells along the microchannel walls is also considered via an additional equation. Results show the variation of cell flux in the fluid phases and the wall as a function of a dimensionless parameter arising in the equations. Our results suggest that conditions may be optimized to maximize cell separation while minimizing contact with the wall surfaces. Experimentally measured cell rolling velocities on the wall indicate the presence of other near-wall forces in addition to fluid shear forces. Separation of a human colon carcinoma cell line from a mixture of red blood cells, with folic acid conjugated 1 microm and 200 nm beads, is reported.

Separation Potential for Multicomponent Mixtures: State-of-the Art of the Problem

NASA Astrophysics Data System (ADS)

Sulaberidze, G. A.; Borisevich, V. D.; Smirnov, A. Yu.

2017-03-01

Various approaches used in introducing a separation potential (value function) for multicomponent mixtures have been analyzed. It has been shown that all known potentials do not satisfy the Dirac-Peierls axioms for a binary mixture of uranium isotopes, which makes their practical application difficult. This is mainly due to the impossibility of constructing a "standard" cascade, whose role in the case of separation of binary mixtures is played by the ideal cascade. As a result, the only universal search method for optimal parameters of the separation cascade is their numerical optimization by the criterion of the minimum number of separation elements in it.

Increased reactivity and monoamine dysregulation following stress in triploid Atlantic salmon (Salmo salar).

PubMed

Fraser, Thomas William Kenneth; Vindas, Marco Antonio; Fjelldal, Per Gunnar; Winberg, Svante; Thörnqvist, Per-Ove; Øverli, Øyvind; Skjæraasen, Jon-Egil; Hansen, Tom Jonny; Mayer, Ian

2015-07-01

Artificial triploid salmonids are sterile and therefore commercially bred to prevent genetic interactions between wild and domestic fish strains. The full biological effects of having an extra chromosome set are largely unknown, but triploids are considered to be more sensitive to sub-optimal environmental conditions and to be stressed by the presence of diploid conspecifics. Brain serotonergic and dopaminergic activity are known to regulate the stress response in vertebrates, but monoamine systems in diploid and triploid fish have yet to be compared. Here we study monoamine neurochemistry in the telencephalon and brain stem of juvenile diploid and triploid Atlantic salmon (Salmo salar) in response to stress (unstressed vs stressed individuals) and holding (separate- vs mixed-ploidy) conditions. Both diploids and triploids showed an increase in serotonergic activity following stress, but the increase was significantly greater in the telencephalon of triploids compared to diploids. Furthermore, while telencephalic dopaminergic activity was significantly increased in diploids following stress, there was no response in triploids. Holding conditions had a significant effect on dopaminergic activity in the brain stem of diploids only, with lower values in mixed- compared to separate-ploidy conditions. These results suggest artificially produced triploids experience increased reactivity and monoaminergic dysregulation following stress that may impede their welfare and performance. Copyright © 2015 Elsevier Inc. All rights reserved.

Separation of polysaccharides from rice husk and wheat bran using solvent system consisting of BMIMOAc and DMI.

PubMed

Hou, Qidong; Li, Weizun; Ju, Meiting; Liu, Le; Chen, Yu; Yang, Qian; Wang, Jingyu

2015-11-20

A solvent system consisting of 1,3-dimethyl-2-imidazolidinone (DMI), and ionic liquid 1-butyl-3-methylimidazolium acetate (BMIMOAc) was used to separate polysaccharides from rice husk and wheat bran. The effects of the DMI/BMIMOAc ratios, temperature, and time on the dissolution of rice husk and wheat bran were investigated, and the influence of anti-solvents on the regeneration of polysaccharides-rich material was evaluated. We found that the solvent system is more powerful to dissolve rice husk and wheat bran than pure BMIMOAc, and that polysaccharides-rich material can be effectively separated from the biomass solution. The polysaccharides content of regenerated material from wheat bran can reach as high as 94.4% when ethanol was used as anti-solvents. Under optimized conditions, the extraction rate of polysaccharides for wheat bran can reach as high as 71.8% at merely 50°C. The recycled solvent system exhibited constant ability to separate polysaccharides from rice husk and wheat bran. Copyright © 2015 Elsevier Ltd. All rights reserved.

Experimental design for a basic mixture on a fluorinated packing. The effect of composition of the mobile phase.

PubMed

Wang, Y; Harrison, M; Clark, B J

2006-02-10

An optimization methodology is introduced for investigating the separation and the retention behavior of analytes on a new fluorinated reversed-phase packing. Ten basic compounds were selected as test probes to study the predictive models developed by using SPSS and MATLAB software. A two-level orthogonal array design (OAD) was used to extract significant parameters. The significant factors were optimised using a central composite design to obtain the quadratic relationship between the dependent and the independent variables. Using this strategy, response surfaces were derived as the 3D and contour plots, and mathematical models were defined for the separation. The models had a satisfactory coefficient (R(2) > 0.97, n = 16). For the test compounds, the best separation condition was: MeCN/30 mM phosphate buffer pH 7.1(55.5:44.5, v/v) and 10 basic solutes were resolved in 22 min. The significant influence of the concentration of buffer shows that different mechanisms of separation for basic compounds on the fluorinated packing exist compared with a common ODS stationary phase.

Considerations in the improvement of human epidermal keratinocyte culture in vitro.

PubMed

Kaviani, Maryam; Geramizadeh, Bita; Rahsaz, Marjan; Marzban, Saeed

2015-04-01

Large-scale expansion of epidermal keratinocytes is essential in the application of these cells for severe burn treatment in patients. Therefore, this study was designed to evaluate various conditions in the expansion of human epidermal keratinocytes. The epidermis was separated from the dermis of skin samples using dispase. The epidermis was trypsinized for keratinocyte isolation. Keratinocytes were cultured in various conditions, with or without a human dermal fibroblast feeder layer, mitomycin C treatment, and different culture media. Our results suggest that keratinocytes cultured on a human dermal fibroblast feeder layer were grown for several passages. Extensive deformation and rapid deterioration were observed in the cultured cells without a feeder layer and in serum-free medium. Human dermal fibroblasts treated with mitomycin C can provide optimal conditions for proliferation of keratinocytes.

Development and Optimization of a Flocculation Procedure for Improved Solid-Liquid Separation of Digested Biomass

DOE Office of Scientific and Technical Information (OSTI.GOV)

Patton, Caroline; Lischeske, James J.; Sievers, David A.

2015-11-03

One viable treatment method for conversion of lignocellulosic biomass to biofuels begins with saccharification (thermochemical pretreatment and enzymatic hydrolysis), followed by fermentation or catalytic upgrading to fuels such as ethanol, butanol, or other hydrocarbons. The post-hydrolysis slurry is typically 4-8 percent insoluble solids, predominantly consisting of lignin. Suspended solids are known to inhibit fermentation as well as poison catalysts and obstruct flow in catalyst beds. Thus a solid-liquid separation following enzymatic hydrolysis would be highly favorable for process economics, however the material is not easily separated by filtration or gravimetric methods. Use of a polyacrylamide flocculant to bind the suspendedmore » particles in a corn stover hydrolyzate slurry into larger flocs (1-2mm diameter) has been found to be extremely helpful in improving separation. Recent and ongoing research on novel pretreatment methods yields hydrolyzate material with diverse characteristics. Therefore, we need a thorough understanding of rapid and successful flocculation design in order to quickly achieve process design goals. In this study potential indicators of flocculation performance were investigated in order to develop a rapid analysis method for flocculation procedure in the context of a novel hydrolyzate material. Flocculation conditions were optimized on flocculant type and loading, pH, and mixing time. Filtration flux of the hydrolyzate slurry was improved 170-fold using a cationic polyacrylamide flocculant with a dosing of approximately 22 mg flocculant/g insoluble solids at an approximate pH of 3. With cake washing, sugar recovery exceeded 90 percent with asymptotic yield at 15 L wash water/kg insoluble solids.« less

Optimization of a Differential Ion Mobility Spectrometry-Tandem Mass Spectrometry Method for High-Throughput Analysis of Nicotine and Related Compounds: Application to Electronic Cigarette Refill Liquids.

PubMed

Regueiro, Jorge; Giri, Anupam; Wenzl, Thomas

2016-06-21

Fast market penetration of electronic cigarettes is leading to an exponentially growing number of electronic refill liquids with different nicotine contents and an endless list of flavors. Therefore, rapid and simple methods allowing a fast screening of these products are necessary to detect harmful substances which can negatively impact the health of consumers. In this regard, the present work explores the capabilities of differential ion mobility spectrometry coupled to tandem mass spectrometry for high-throughput analysis of nicotine and 11 related compounds in commercial refill liquids for electronic cigarettes. The influence of main factors affecting the ion mobility separation, such as modifier types and concentration, separation voltage, and temperature, was systematically investigated. Despite small molecular weight differences among the studied compounds, a good separation was achieved in the ion mobility cell under the optimized conditions, which involved the use of ethanol as a polar gas-phase chemical modifier. Indeed, differential ion mobility was able to resolve (resolution >4) nicotine from its structural isomer anabasine without the use of any chromatographic separation. The quantitative performance of the proposed method was then evaluated, showing satisfactory precision (RSD ≤ 16%) and recoveries ranging from 85 to 100% for nicotine, and from 84 to 126% for the rest of the target analytes. Several commercial electronic cigarette refill liquids were analyzed to demonstrate the applicability of the method. In some cases, significant differences were found between labeled and measured levels of nicotine. Anatabine, cotinine, myosmine, and nornicotine were also found in some of the analyzed samples.

Optimal control of orientation and entanglement for two dipole-dipole coupled quantum planar rotors.

PubMed

Yu, Hongling; Ho, Tak-San; Rabitz, Herschel

2018-05-09

Optimal control simulations are performed for orientation and entanglement of two dipole-dipole coupled identical quantum rotors. The rotors at various fixed separations lie on a model non-interacting plane with an applied control field. It is shown that optimal control of orientation or entanglement represents two contrasting control scenarios. In particular, the maximally oriented state (MOS) of the two rotors has a zero entanglement entropy and is readily attainable at all rotor separations. Whereas, the contrasting maximally entangled state (MES) has a zero orientation expectation value and is most conveniently attainable at small separations where the dipole-dipole coupling is strong. It is demonstrated that the peak orientation expectation value attained by the MOS at large separations exhibits a long time revival pattern due to the small energy splittings arising form the extremely weak dipole-dipole coupling between the degenerate product states of the two free rotors. Moreover, it is found that the peak entanglement entropy value attained by the MES remains largely unchanged as the two rotors are transported to large separations after turning off the control field. Finally, optimal control simulations of transition dynamics between the MOS and the MES reveal the intricate interplay between orientation and entanglement.

CEC with new monolithic stationary phase based on a fluorinated monomer, trifluoroethyl methacrylate.

PubMed

Yurtsever, Arda; Saraçoğlu, Berna; Tuncel, Ali

2009-02-01

A new, fluorinated monolithic stationary phase for CEC was first synthesized by a single-stage, thermally initiated copolymerization of a fluorinated monomer, 2,2,2-trifluoroethyl methacrylate (TFEM) and ethylene dimethacrylate (EDMA) in the presence of a porogen mixture. In this preparation, 2-acrylamido-2-methyl-1-propanesulfonic acid was used as the charge-bearing monomer. The porogen mixture was prepared by mixing isoamylalcohol and 1,4-butanediol. A clear increase in the electroosmotic mobility was observed with increasing pH. The electroosmotic mobility decreased with increasing ACN concentration. Poly(TFEM-co-EDMA) monolith prepared under optimized polymerization conditions was successfully used in the separation of alkylbenzenes and phenols by CEC. The best chromatographic separation for alkylbenzenes was performed with lower ACN concentrations (i.e. 60% v/v) with respect to the common acrylic-based CEC monoliths. The theoretical plate numbers up to 220 000 plates/m were achieved in the reversed phase separation of phenols. Poly(TFEM-co-EDMA) monolith also allowed the simultaneous separation of aniline and benzoic acid derivatives by a single run and by using a lower ACN concentration in the mobile phase with respect to the similar electrochromatographic separations. A stable retention behaviour in reversed phase separation of alkylbenzenes was obtained with the poly(TFEM-co-EDMA) monolith.

Enantiomeric separation of non-protein amino acids by electrokinetic chromatography.

PubMed

Pérez-Míguez, Raquel; Marina, María Luisa; Castro-Puyana, María

2016-10-07

New analytical methodologies enabling the enantiomeric separation of a group of non-protein amino acids of interest in the pharmaceutical and food analysis fields were developed in this work using Electrokinetic Chromatography. The use of FMOC as derivatization reagent and the subsequent separation using acidic conditions (formate buffer at pH 2.0) and anionic cyclodextrins as chiral selectors allowed the chiral separation of eight from the ten non-protein amino acids studied. Pyroglutamic acid, norvaline, norleucine, 3,4-dihydroxyphenilalanine, 2-aminoadipic acid, and selenomethionine were enantiomericaly separated using sulfated-α-CD while sulfated-γ-CD enabled the enantiomeric separation of norvaline, 3,4-dihydroxyphenilalanine, 2-aminoadipic acid, selenomethionie, citrulline, and pipecolic acid. Moreover, the potential of the developed methodologies was demonstrated in the analysis of citrulline and its enantiomeric impurity in food supplements. For that purpose, experimental and instrumental variables were optimized and the analytical characteristics of the proposed method were evaluated. LODs of 2.1×10 -7 and 1.8×10 -7 M for d- and l-citrulline, respectively, were obtained. d-Cit was not detectable in any of the six food supplement samples analyzed showing that the effect of storage time on the racemization of citrulline was negligible. Copyright © 2016 Elsevier B.V. All rights reserved.

Comparative study of three magnetic nano-particles (FeSO4, FeSO4/SiO2, FeSO4/SiO2/TiO2) in plasmid DNA extraction.

PubMed

Rahnama, H; Sattarzadeh, A; Kazemi, F; Ahmadi, N; Sanjarian, F; Zand, Z

2016-11-15

Recent updates on Magnetic Nano-Particles (MNPs) based separation of nucleic acids have received more attention due to their easy manipulation, simplicity, ease of automation and cost-effectiveness. It has been indicated that DNA molecules absorb on solid surfaces via hydrogen-bonding, and hydrophobic and electrostatic interactions. These properties highly depend on the surface condition of the solid support. Therefore, surface modification of MNPs may enhance their functionality and specification. In the present study, we functionalized Fe3O4 nano-particle surface utilizing SiO2 and TiO2 layer as Fe3O4/SiO2 and Fe3O4/SiO2/TiO2 and then compare their functionality in the adsorption of plasmid DNA molecules with the naked Fe3O4 nano-particles. The result obtained showed that the purity and amount of DNA extracted by Fe3O4 coated by SiO2 or SiO2/TiO2 were higher than the naked Fe3O4 nano-particles. Furthermore, we obtained pH 8 and 1.5 M NaCl as an optimal condition for desorption of DNA from MNPs. The result further showed that, 0.2 mg nano-particle and 10 min at 55 °C are the optimal conditions for DNA desorption from nano-particles. In conclusion, we recommended Fe3O4/SiO2/TiO2 as a new MNP for separation of DNA molecules from biological sources. Copyright © 2016 Elsevier Inc. All rights reserved.

Membrane processes

NASA Astrophysics Data System (ADS)

Staszak, Katarzyna

2017-11-01

The membrane processes have played important role in the industrial separation process. These technologies can be found in all industrial areas such as food, beverages, metallurgy, pulp and paper, textile, pharmaceutical, automotive, biotechnology and chemical industry, as well as in water treatment for domestic and industrial application. Although these processes are known since twentieth century, there are still many studies that focus on the testing of new membranes' materials and determining of conditions for optimal selectivity, i. e. the optimum transmembrane pressure (TMP) or permeate flux to minimize fouling. Moreover the researchers proposed some calculation methods to predict the membrane processes properties. In this article, the laboratory scale experiments of membrane separation techniques, as well their validation by calculation methods are presented. Because membrane is the "heart" of the process, experimental and computational methods for its characterization are also described.

A New Cluster Analysis-Marker-Controlled Watershed Method for Separating Particles of Granular Soils.

PubMed

Alam, Md Ferdous; Haque, Asadul

2017-10-18

An accurate determination of particle-level fabric of granular soils from tomography data requires a maximum correct separation of particles. The popular marker-controlled watershed separation method is widely used to separate particles. However, the watershed method alone is not capable of producing the maximum separation of particles when subjected to boundary stresses leading to crushing of particles. In this paper, a new separation method, named as Monash Particle Separation Method (MPSM), has been introduced. The new method automatically determines the optimal contrast coefficient based on cluster evaluation framework to produce the maximum accurate separation outcomes. Finally, the particles which could not be separated by the optimal contrast coefficient were separated by integrating cuboid markers generated from the clustering by Gaussian mixture models into the routine watershed method. The MPSM was validated on a uniformly graded sand volume subjected to one-dimensional compression loading up to 32 MPa. It was demonstrated that the MPSM is capable of producing the best possible separation of particles required for the fabric analysis.

Pair-Wise and Many-Body Dispersive Interactions Coupled to an Optimally Tuned Range-Separated Hybrid Functional.

PubMed

Agrawal, Piyush; Tkatchenko, Alexandre; Kronik, Leeor

2013-08-13

We propose a nonempirical, pair-wise or many-body dispersion-corrected, optimally tuned range-separated hybrid functional. This functional retains the advantages of the optimal-tuning approach in the prediction of the electronic structure. At the same time, it gains accuracy in the prediction of binding energies for dispersively bound systems, as demonstrated on the S22 and S66 benchmark sets of weakly bound dimers.

Efficient approach for the extraction of proanthocyanidins from Cinnamomum longepaniculatum leaves using ultrasonic irradiation and an evaluation of their inhibition activity on digestive enzymes and antioxidant activity in vitro.

PubMed

Liu, Zaizhi; Mo, Kailin; Fei, Shimin; Zu, Yuangang; Yang, Lei

2017-08-01

Proanthocyanidins were separated for the first time from Cinnamomum longepaniculatum leaves. An experiment-based extraction strategy was used to research the efficiency of an ultrasound-assisted method for proanthocyanidins extraction. The Plackett-Burman design results revealed that the ultrasonication time, ultrasonic power and liquid/solid ratio were the most significant parameters among the six variables in the extraction process. Upon further optimization of the Box-Behnken design, the optimal conditions were obtained as follows: extraction temperature, 100°C; ethanol concentration, 70%; pH 5; ultrasonication power, 660 W; ultrasonication time, 44 min; liquid/solid ratio, 20 mL/g. Under the obtained conditions, the extraction yield of the proanthocyanidins using the ultrasonic-assisted method was 7.88 ± 0.21 mg/g, which is higher than that obtained using traditional methods. The phloroglucinolysis products of the proanthocyanidins, including the terminal units and derivatives from the extension units, were tentatively identified using a liquid chromatography with tandem mass spectrometry analysis. Cinnamomum longepaniculatum proanthocyanidins have promising antioxidant and anti-nutritional properties. In summary, an ultrasound-assisted method in combination with a response surface experimental design is an efficient methodology for the sufficient isolation of proanthocyanidins from Cinnamomum longepaniculatum leaves, and this method could be used for the separation of other bioactive compounds. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous determination of phenolic acids and flavonoids in rice using solid-phase extraction and RP-HPLC with photodiode array detection.

PubMed

Irakli, Maria N; Samanidou, Victoria F; Biliaderis, Costas G; Papadoyannis, Ioannis N

2012-07-01

An analytical method based on an optimized solid-phase extraction procedure and followed by high-performance liquid chromatography (HPLC) separation with diode array detection was developed and validated for the simultaneous determination of phenolic acids (gallic, protocatechuic, 4-hydroxy-benzoic, vanillic, caffeic, syringic, p-coumaric, ferulic, sinapic, and cinnamic acids), flavanols (catechin and epicatechin), flavonols (myricetin, quercetin, kaempferol, quercetin-3-O-glucoside, hyperoside, and rutin), flavones (luteolin and apigenin) and flavanones (naringenin and hesperidin) in rice flour (Oryza sativa L.). Chromatographic separation was carried out on a PerfectSil Target ODS-3 (250 mm × 4.6 mm, 3 μm) column at temperature 25°C using a mobile phase, consisting of 0.5% (v/v) acetic acid in water, methanol, and acetonitrile at a flow rate 1 mL min(-1) , under gradient elution conditions. Application of optimum extraction conditions, elaborated on both Lichrolut C(18) and Oasis HLB cartridges, have led to extraction of phenolic acids and flavonoids from rice flour with mean recoveries 84.3-113.0%. The developed method was validated in terms of linearity, accuracy, precision, stability, and sensitivity. Repeatability (n = 5) and inter-day precision (n = 4) revealed relative standard deviation (RSD) <13%. The optimized method was successfully applied to the analysis of phenolic acids and flavonoids in pigmented (red and black rice) and non-pigmented rice (brown rice) samples. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Separation of CsCl from a Ternary CsCl-LiCl-KCl Salt via a Melt Crystallization Technique for Pyroprocessing Waste Minimization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ammon Williams; Supathorn Phongikaroon; Michael Simpson

A parametric study has been conducted to identify the effects of several parameters on the separation of CsCl from molten LiCl-KCl salt via a melt crystallization process. A reverse vertical Bridgman technique was used to grow the salt crystals. The investigated parameters were: (1) the advancement rate, (2) the crucible lid configuration, (3) the amount of salt mixture, (4) the initial composition of CsCl, and (5) the temperature difference between the high and low furnace zones. From each grown crystal, samples were taken axially and analyzed using inductively coupled plasma mass spectrometry (ICP-MS). Results show that CsCl concentrations at themore » top of the crystals were low and increased to a maximum at the bottom of the salt. Salt (LiCl-KCl) recycle percentages for the experiments ranged from 50% to 75% and the CsCl composition in the waste salt was low. To increase the recycle percentage and the concentration of CsCl in the waste form, the possibility of using multiple crystallization stages was explored to further optimize the process. Results show that multiple crystallization stages are practical and the optimal experimental conditions should be operated at 5.0 mm/hr rate with a lid configuration and temperature difference of 200 °C for a total of five crystallization stages. Under these conditions, up to 88% of the salt can be recycled.« less

Antibody-immobilized column for quick cell separation based on cell rolling.

PubMed

Mahara, Atsushi; Yamaoka, Tetsuji

2010-01-01

Cell separation using methodological standards that ensure high purity is a very important step in cell transplantation for regenerative medicine and for stem cell research. A separation protocol using magnetic beads has been widely used for cell separation to isolate negative and positive cells. However, not only the surface marker pattern, e.g., negative or positive, but also the density of a cell depends on its developmental stage and differentiation ability. Rapid and label-free separation procedures based on surface marker density are the focus of our interest. In this study, we have successfully developed an antiCD34 antibody-immobilized cell-rolling column, that can separate cells depending on the CD34 density of the cell surfaces. Various conditions for the cell-rolling column were optimized including graft copolymerization, and adjustment of the column tilt angle, and medium flow rate. Using CD34-positive and -negative cell lines, the cell separation potential of the column was established. We observed a difference in the rolling velocities between CD34-positive and CD34-negative cells on antibody-immobilized microfluidic device. Cell separation was achieved by tilting the surface 20 degrees and the increasing medium flow. Surface marker characteristics of the isolated cells in each fraction were analyzed using a cell-sorting system, and it was found that populations containing high density of CD34 were eluted in the delayed fractions. These results demonstrate that cells with a given surface marker density can be continuously separated using the cell rolling column.

Separation of non-ferrous metals from ASR by corona electrostatic separation

NASA Astrophysics Data System (ADS)

Kim, Yang-soo; Choi, Jin-Young; Jeon, Ho-Seok; Han, Oh-Hyung; Park, Chul-Hyun

2016-04-01

Automotive shredder residue (ASR), the residual fraction of approximate 25% obtained after dismantling and shredding from waste car, consists of polymers (plastics and rubber), metals (ferrous and non-ferrous), wood, glass and fluff (textile and fiber). ASR cannot be effectively separated due to its heterogeneous materials and coated or laminated complexes and then largely deposited in land-fill sites as waste. Thus reducing a pollutant release before disposal, techniques that can improve the liberation of coated (or laminated) complexes and the recovery of valuable metals from the shredder residue are needed. ASR may be separated by a series of physical processing operations such as comminution, air, magnetic and electrostatic separations. The work deals with the characterization of the shredder residue coming from an industrial plant in korea and focuses on estimating the optimal conditions of corona electrostatic separation for improving the separation efficiency of valuable non-ferrous metals such as aluminum, copper and etc. From the results of test, the maximum separation achievable for non-ferrous metals using a corona electrostatic separation has been shown to be recovery of 92.5% at a grade of 75.8%. The recommended values of the process variables, particle size, electrode potential, drum speed, splitter position and relative humidity are -6mm, 50 kV, 35rpm, 20° and less 40%, respectively. Acknowledgments This study was supported by the R&D Center for Valuable Recycling (Global-Top R&BD Program) of the Ministry of Environment. (Project No. GT-11-C-01-170-0)

Extending metabolome coverage for untargeted metabolite profiling of adherent cultured hepatic cells.

PubMed

García-Cañaveras, Juan Carlos; López, Silvia; Castell, José Vicente; Donato, M Teresa; Lahoz, Agustín

2016-02-01

MS-based metabolite profiling of adherent mammalian cells comprises several challenging steps such as metabolism quenching, cell detachment, cell disruption, metabolome extraction, and metabolite measurement. In LC-MS, the final metabolome coverage is strongly determined by the separation technique and the MS conditions used. Human liver-derived cell line HepG2 was chosen as adherent mammalian cell model to evaluate the performance of several commonly used procedures in both sample processing and LC-MS analysis. In a first phase, metabolite extraction and sample analysis were optimized in a combined manner. To this end, the extraction abilities of five different solvents (or combinations) were assessed by comparing the number and the levels of the metabolites comprised in each extract. Three different chromatographic methods were selected for metabolites separation. A HILIC-based method which was set to specifically separate polar metabolites and two RP-based methods focused on lipidome and wide-ranging metabolite detection, respectively. With regard to metabolite measurement, a Q-ToF instrument operating in both ESI (+) and ESI (-) was used for unbiased extract analysis. Once metabolite extraction and analysis conditions were set up, the influence of cell harvesting on metabolome coverage was also evaluated. Therefore, different protocols for cell detachment (trypsinization or scraping) and metabolism quenching were compared. This study confirmed the inconvenience of trypsinization as a harvesting technique, and the importance of using complementary extraction solvents to extend metabolome coverage, minimizing interferences and maximizing detection, thanks to the use of dedicated analytical conditions through the combination of HILIC and RP separations. The proposed workflow allowed the detection of over 300 identified metabolites from highly polar compounds to a wide range of lipids.

Detection of caffeine in tea, instant coffee, green tea beverage, and soft drink by direct analysis in real time (DART) source coupled to single-quadrupole mass spectrometry.

PubMed

Wang, Lei; Zhao, Pengyue; Zhang, Fengzu; Bai, Aijuan; Pan, Canping

2013-01-01

Ambient ionization direct analysis in real time (DART) coupled to single-quadrupole MS (DART-MS) was evaluated for rapid detection of caffeine in commercial samples without chromatographic separation or sample preparation. Four commercial samples were examined: tea, instant coffee, green tea beverage, and soft drink. The response-related parameters were optimized for the DART temperature and MS fragmentor. Under optimal conditions, the molecular ion (M+H)+ was the major ion for identification of caffeine. The results showed that DART-MS is a promising tool for the quick analysis of important marker molecules in commercial samples. Furthermore, this system has demonstrated significant potential for high sample throughput and real-time analysis.

Transonic airfoil design for helicopter rotor applications

NASA Technical Reports Server (NTRS)

Hassan, Ahmed A.; Jackson, B.

1989-01-01

Despite the fact that the flow over a rotor blade is strongly influenced by locally three-dimensional and unsteady effects, practical experience has always demonstrated that substantial improvements in the aerodynamic performance can be gained by improving the steady two-dimensional charateristics of the airfoil(s) employed. The two phenomena known to have great impact on the overall rotor performance are: (1) retreating blade stall with the associated large pressure drag, and (2) compressibility effects on the advancing blade leading to shock formation and the associated wave drag and boundary-layer separation losses. It was concluded that: optimization routines are a powerful tool for finding solutions to multiple design point problems; the optimization process must be guided by the judicious choice of geometric and aerodynamic constraints; optimization routines should be appropriately coupled to viscous, not inviscid, transonic flow solvers; hybrid design procedures in conjunction with optimization routines represent the most efficient approach for rotor airfroil design; unsteady effects resulting in the delay of lift and moment stall should be modeled using simple empirical relations; and inflight optimization of aerodynamic loads (e.g., use of variable rate blowing, flaps, etc.) can satisfy any number of requirements at design and off-design conditions.

Temporal optimisation of image acquisition for land cover classification with Random Forest and MODIS time-series

NASA Astrophysics Data System (ADS)

Nitze, Ingmar; Barrett, Brian; Cawkwell, Fiona

2015-02-01

The analysis and classification of land cover is one of the principal applications in terrestrial remote sensing. Due to the seasonal variability of different vegetation types and land surface characteristics, the ability to discriminate land cover types changes over time. Multi-temporal classification can help to improve the classification accuracies, but different constraints, such as financial restrictions or atmospheric conditions, may impede their application. The optimisation of image acquisition timing and frequencies can help to increase the effectiveness of the classification process. For this purpose, the Feature Importance (FI) measure of the state-of-the art machine learning method Random Forest was used to determine the optimal image acquisition periods for a general (Grassland, Forest, Water, Settlement, Peatland) and Grassland specific (Improved Grassland, Semi-Improved Grassland) land cover classification in central Ireland based on a 9-year time-series of MODIS Terra 16 day composite data (MOD13Q1). Feature Importances for each acquisition period of the Enhanced Vegetation Index (EVI) and Normalised Difference Vegetation Index (NDVI) were calculated for both classification scenarios. In the general land cover classification, the months December and January showed the highest, and July and August the lowest separability for both VIs over the entire nine-year period. This temporal separability was reflected in the classification accuracies, where the optimal choice of image dates outperformed the worst image date by 13% using NDVI and 5% using EVI on a mono-temporal analysis. With the addition of the next best image periods to the data input the classification accuracies converged quickly to their limit at around 8-10 images. The binary classification schemes, using two classes only, showed a stronger seasonal dependency with a higher intra-annual, but lower inter-annual variation. Nonetheless anomalous weather conditions, such as the cold winter of 2009/2010 can alter the temporal separability pattern significantly. Due to the extensive use of the NDVI for land cover discrimination, the findings of this study should be transferrable to data from other optical sensors with a higher spatial resolution. However, the high impact of outliers from the general climatic pattern highlights the limitation of spatial transferability to locations with different climatic and land cover conditions. The use of high-temporal, moderate resolution data such as MODIS in conjunction with machine-learning techniques proved to be a good base for the prediction of image acquisition timing for optimal land cover classification results.

Systematic Review and Meta-Analysis of Psychological Therapies for Children With Chronic Pain

PubMed Central

Heathcote, Lauren; Palermo, Tonya M.; de C Williams, Amanda C; Lau, Jennifer; Eccleston, Christopher

2014-01-01

Objectives This systematic review and meta-analysis examined the effects of psychological therapies for management of chronic pain in children. Methods Randomized controlled trials of psychological interventions treating children (<18 years) with chronic pain conditions including headache, abdominal, musculoskeletal, or neuropathic pain were searched for. Pain symptoms, disability, depression, anxiety, and sleep outcomes were extracted. Risk of bias was assessed and quality of the evidence was rated using GRADE. Results 35 included studies revealed that across all chronic pain conditions, psychological interventions reduced pain symptoms and disability posttreatment. Individual pain conditions were analyzed separately. Sleep outcomes were not reported in any trials. Optimal dose of treatment was explored. For headache pain, higher treatment dose led to greater reductions in pain. No effect of dosage was found for other chronic pain conditions. Conclusions Evidence for psychological therapies treating chronic pain is promising. Recommendations for clinical practice and research are presented. PMID:24602890

Numerical modelling of the flow and isotope separation in centrifuge Iguasu for different lengths of the rotor

NASA Astrophysics Data System (ADS)

Bogovalov, S. V.; Borisevich, V. D.; Borman, V. D.; Tronin, I. V.; Tronin, V. N.

2016-06-01

Numerical modelling and optimization of the gas flow and isotope separation in the Iguasu gas centrifuge (GC) for uranium enrichment have been performed for different lengths of the rotor. The calculations show that the specific separative power of the GC reduces with the length of the rotor. We show that the reduction of the specific separative power is connected with the growth of the pressure in the optimal regime and corresponding growth of temperature to prevent the working gas sublimation. The specific separative power remains constant with the growth of the rotor length provided that the temperature of the gas is taken to be constant.

Numerical Modeling of Dependence of Separative Power of the Gas Centrifuge on the Length of Rotor

NASA Astrophysics Data System (ADS)

Bogovalov, S. V.; Borisevich, V. D.; Borman, V. D.; Tronin, I. V.; Tronin, V. N.

Numerical modelling and optimization of the gas flow and isotope separation in the Iguasu gas centrifuge (GC) for uranium enrichment have been performed for different lengths of the rotor. The calculations show that the specific separative power of the GC reduces with the length of the rotor. We show that the reduction of the specific separative power is connected with the growth of the pressure in the optimal regime and corresponding growth of temperature to prevent the working gas sublimation. The specific separative power remains constant with the growth of the rotor length provided that the temperature of the rotor is taken to be constant.

Numerical modelling of the flow and isotope separation in centrifuge Iguasu for different lengths of the rotor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bogovalov, S. V.; Borisevich, V. D.; Borman, V. D.

Numerical modelling and optimization of the gas flow and isotope separation in the Iguasu gas centrifuge (GC) for uranium enrichment have been performed for different lengths of the rotor. The calculations show that the specific separative power of the GC reduces with the length of the rotor. We show that the reduction of the specific separative power is connected with the growth of the pressure in the optimal regime and corresponding growth of temperature to prevent the working gas sublimation. The specific separative power remains constant with the growth of the rotor length provided that the temperature of the gasmore » is taken to be constant.« less

Conceptual design of distillation-based hybrid separation processes.

PubMed

Skiborowski, Mirko; Harwardt, Andreas; Marquardt, Wolfgang

2013-01-01

Hybrid separation processes combine different separation principles and constitute a promising design option for the separation of complex mixtures. Particularly, the integration of distillation with other unit operations can significantly improve the separation of close-boiling or azeotropic mixtures. Although the design of single-unit operations is well understood and supported by computational methods, the optimal design of flowsheets of hybrid separation processes is still a challenging task. The large number of operational and design degrees of freedom requires a systematic and optimization-based design approach. To this end, a structured approach, the so-called process synthesis framework, is proposed. This article reviews available computational methods for the conceptual design of distillation-based hybrid processes for the separation of liquid mixtures. Open problems are identified that must be addressed to finally establish a structured process synthesis framework for such processes.

Valence electronic structure of cobalt phthalocyanine from an optimally tuned range-separated hybrid functional.

PubMed

Brumboiu, Iulia Emilia; Prokopiou, Georgia; Kronik, Leeor; Brena, Barbara

2017-07-28

We analyse the valence electronic structure of cobalt phthalocyanine (CoPc) by means of optimally tuning a range-separated hybrid functional. The tuning is performed by modifying both the amount of short-range exact exchange (α) included in the hybrid functional and the range-separation parameter (γ), with two strategies employed for finding the optimal γ for each α. The influence of these two parameters on the structural, electronic, and magnetic properties of CoPc is thoroughly investigated. The electronic structure is found to be very sensitive to the amount and range in which the exact exchange is included. The electronic structure obtained using the optimal parameters is compared to gas-phase photo-electron data and GW calculations, with the unoccupied states additionally compared with inverse photo-electron spectroscopy measurements. The calculated spectrum with tuned γ, determined for the optimal value of α = 0.1, yields a very good agreement with both experimental results and with GW calculations that well-reproduce the experimental data.

Separated-pair independent particle model and the generalized Brillouin theorem: ab initio calculations on the dissociation of polyatomic molecules

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sundberg, Kenneth Randall

1976-01-01

A method is developed to optimize the separated-pair independent particle (SPIP) wave function; it is a special case of the separated-pair theory obtained by using two-term natural expansions of the geminals. The orbitals are optimized by a theory based on the generalized Brillouin theorem and iterative configuration interaction (CI) calculations in the space of the SPIP function and its single excitations. The geminal expansion coefficients are optimized by serial 2 x 2 CI calculations. Formulas are derived for the matrix elements. An algorithm to implement the method is presented, and the work needed to evaluate the molecular integrals is discussed.

Constraint Force Equation Methodology for Modeling Multi-Body Stage Separation Dynamics

NASA Technical Reports Server (NTRS)

Toniolo, Matthew D.; Tartabini, Paul V.; Pamadi, Bandu N.; Hotchko, Nathaniel

2008-01-01

This paper discusses a generalized approach to the multi-body separation problems in a launch vehicle staging environment based on constraint force methodology and its implementation into the Program to Optimize Simulated Trajectories II (POST2), a widely used trajectory design and optimization tool. This development facilitates the inclusion of stage separation analysis into POST2 for seamless end-to-end simulations of launch vehicle trajectories, thus simplifying the overall implementation and providing a range of modeling and optimization capabilities that are standard features in POST2. Analysis and results are presented for two test cases that validate the constraint force equation methodology in a stand-alone mode and its implementation in POST2.

Cell separation using tilted-angle standing surface acoustic waves

PubMed Central

Ding, Xiaoyun; Peng, Zhangli; Lin, Sz-Chin Steven; Geri, Michela; Li, Sixing; Li, Peng; Chen, Yuchao; Dao, Ming; Suresh, Subra; Huang, Tony Jun

2014-01-01

Separation of cells is a critical process for studying cell properties, disease diagnostics, and therapeutics. Cell sorting by acoustic waves offers a means to separate cells on the basis of their size and physical properties in a label-free, contactless, and biocompatible manner. The separation sensitivity and efficiency of currently available acoustic-based approaches, however, are limited, thereby restricting their widespread application in research and health diagnostics. In this work, we introduce a unique configuration of tilted-angle standing surface acoustic waves (taSSAW), which are oriented at an optimally designed inclination to the flow direction in the microfluidic channel. We demonstrate that this design significantly improves the efficiency and sensitivity of acoustic separation techniques. To optimize our device design, we carried out systematic simulations of cell trajectories, matching closely with experimental results. Using numerically optimized design of taSSAW, we successfully separated 2- and 10-µm-diameter polystyrene beads with a separation efficiency of ∼99%, and separated 7.3- and 9.9-µm-polystyrene beads with an efficiency of ∼97%. We illustrate that taSSAW is capable of effectively separating particles–cells of approximately the same size and density but different compressibility. Finally, we demonstrate the effectiveness of the present technique for biological–biomedical applications by sorting MCF-7 human breast cancer cells from nonmalignant leukocytes, while preserving the integrity of the separated cells. The method introduced here thus offers a unique route for separating circulating tumor cells, and for label-free cell separation with potential applications in biological research, disease diagnostics, and clinical practice. PMID:25157150

Cell separation using tilted-angle standing surface acoustic waves.

PubMed

Ding, Xiaoyun; Peng, Zhangli; Lin, Sz-Chin Steven; Geri, Michela; Li, Sixing; Li, Peng; Chen, Yuchao; Dao, Ming; Suresh, Subra; Huang, Tony Jun

2014-09-09

Separation of cells is a critical process for studying cell properties, disease diagnostics, and therapeutics. Cell sorting by acoustic waves offers a means to separate cells on the basis of their size and physical properties in a label-free, contactless, and biocompatible manner. The separation sensitivity and efficiency of currently available acoustic-based approaches, however, are limited, thereby restricting their widespread application in research and health diagnostics. In this work, we introduce a unique configuration of tilted-angle standing surface acoustic waves (taSSAW), which are oriented at an optimally designed inclination to the flow direction in the microfluidic channel. We demonstrate that this design significantly improves the efficiency and sensitivity of acoustic separation techniques. To optimize our device design, we carried out systematic simulations of cell trajectories, matching closely with experimental results. Using numerically optimized design of taSSAW, we successfully separated 2- and 10-µm-diameter polystyrene beads with a separation efficiency of ∼ 99%, and separated 7.3- and 9.9-µm-polystyrene beads with an efficiency of ∼ 97%. We illustrate that taSSAW is capable of effectively separating particles-cells of approximately the same size and density but different compressibility. Finally, we demonstrate the effectiveness of the present technique for biological-biomedical applications by sorting MCF-7 human breast cancer cells from nonmalignant leukocytes, while preserving the integrity of the separated cells. The method introduced here thus offers a unique route for separating circulating tumor cells, and for label-free cell separation with potential applications in biological research, disease diagnostics, and clinical practice.

Development of pseudo-linear gradient elution for high-throughput resin selectivity screening in RoboColumn® Format.

PubMed

Kiesewetter, André; Menstell, Peter; Peeck, Lars H; Stein, Andreas

2016-11-01

Rapid development of chromatographic processes relies on effective high-throughput screening (HTS) methods. This article describes the development of pseudo-linear gradient elution for resin selectivity screening using RoboColumns ® . It gives guidelines for the implementation of this HTS method on a Tecan Freedom EVO ® robotic platform, addressing fundamental aspects of scale down and liquid handling. The creation of a flexible script for buffer preparation and column operation plus efficient data processing provided the basis for this work. Based on the concept of discretization, linear gradient elution was transformed into multistep gradients. The impact of column size, flow rate, multistep gradient design, and fractionation scheme on separation efficiency was systematically investigated, using a ternary model protein mixture. We identified key parameters and defined optimal settings for effective column performance. For proof of concept, we examined the selectivity of several cation exchange resins using various buffer conditions. The final protocol enabled a clear differentiation of resin selectivity on miniature chromatography column (MCC) scale. Distinct differences in separation behavior of individual resins and the influence of buffer conditions could be demonstrated. Results obtained with the robotic platform were representative and consistent with data generated on a conventional chromatography system. A study on antibody monomer/high molecular weight separation comparing MCC and lab scale under higher loading conditions provided evidence of the applicability of the miniaturized approach to practically relevant feedstocks with challenging separation tasks as well as of the predictive quality for larger scale. A comparison of varying degrees of robotic method complexity with corresponding effort (analysis time and labware consumption) and output quality highlights tradeoffs to select a method appropriate for a given separation challenge or analytical constraints. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 32:1503-1519, 2016. © 2016 American Institute of Chemical Engineers.

Improvement of the performances of a tandem simulated moving bed chromatography by controlling the yield level of a key product of the first simulated moving bed unit.

PubMed

Mun, Sungyong; Wang, Nien-Hwa Linda

2017-03-10

One of the trustworthy processes for ternary separation is a tandem simulated moving bed (SMB) process, which consists of two subordinate four-zone SMB units (Ring I and Ring II). To take full advantage of a tandem SMB as a means of recovering all three products with high purities and high economical efficiency, it is important to understand how the separation condition in Ring II is affected by that in Ring I, and further to reflect such point in the stage of designing a tandem SMB. In regard to such issue, it was clarified in this study that the Ring I factors affecting the Ring II condition could be represented by the yield level of a key product of Ring I (Y key RingI ). As the Y key RingI level became higher, the amount of the Ring I key-product that was reloaded into Ring II was reduced, which affected favorably the Ring II separation condition. On the other hand, the higher Y key RingI level caused a larger dilution for the stream from Ring I to Ring II, which affected adversely the Ring II separation condition. As a result, a minimum in the desorbent usage of a tandem SMB occurred at the Y key RingI level where the two aforementioned factors could be balanced with each other. If such an optimal Y key RingI level was adopted, the desorbent usage could be reduced by up to 25%. It was also found that as the throughput of a tandem SMB became higher, the factor related to the migration of the Ring I key-product into Ring II was more influential in the performances of a tandem SMB than the factor related to the dilution of the stream from Ring I to Ring II. Copyright © 2016 Elsevier B.V. All rights reserved.

Extracting archaeal populations from iron oxidizing systems

NASA Astrophysics Data System (ADS)

Whitmore, L. M.; Hutchison, J.; Chrisler, W.; Jay, Z.; Moran, J.; Inskeep, W.; Kreuzer, H.

2013-12-01

Unique environments in Yellowstone National Park offer exceptional conditions for studying microorganisms in extreme and constrained systems. However, samples from some extreme systems often contain inorganic components that pose complications during microbial and molecular analysis. Several archaeal species are found in acidic, geothermal ferric-oxyhydroxide mats; these species have been shown to adhere to mineral surfaces in flocculated colonies. For optimal microbial analysis, (microscopy, flow cytometry, genomic extractions, proteomic analysis, stable isotope analysis, and others), improved techniques are needed to better facilitate cell detachment and separation from mineral surfaces. As a requirement, these techniques must preserve cell structure while simultaneously minimizing organic carryover to downstream analysis. Several methods have been developed for removing sediments from mixed prokaryotic populations, including ultra-centrifugation, nycodenz gradient, sucrose cushions, and cell straining. In this study we conduct a comparative analysis of mechanisms used to detach archaeal cell populations from the mineral interface. Specifically, we evaluated mechanical and chemical approaches for cell separation and homogenization. Methods were compared using confocal microscopy, flow cytometry analyses, and real-time PCR detection. The methodology and approaches identified will be used to optimize biomass collection from environmental specimens or isolates grown with solid phases.

Fabrication and investigation of electrochromatographic columns with a simplex configuration.

PubMed

Liu, Qing; Yang, Lijun; Wang, Qiuquan; Zhang, Bo

2014-07-04

Duplex capillary columns with a packed and an open section are widely used in electrochromatography (CEC). The duplex column configuration leads to non-uniform voltage drop, electrical field distribution and separation performance. It also adds to the complexity in understanding and optimizing electrochromatographic process. In this study, we introduced a simplex column configuration based on single particle fritting technology. The new column configuration has an essentially uniform packed bed through the entire column length, with only 1mm length left unpacked serving as the optical detection window. The study shows that a simplex column has higher separation efficiency than a duplex column, especially at the high voltage range, due to the consistent distribution of electrical field over the column length. In comparison to the duplex column, the simplex column presented a lower flow rate at the same applied voltage, suggesting that an open section may support a higher speed than a packed section. In practice, the long and short ends of the simplex column could be used as independent CEC columns respectively. This "two-in-one" bi-functional column configuration provided extra flexibilities in selecting and optimizing electrochromatographic conditions. Copyright © 2014 Elsevier B.V. All rights reserved.

Separation/preconcentration and determination of vanadium with dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) and electrothermal atomic absorption spectrometry.

PubMed

Asadollahi, Tahereh; Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji

2010-06-30

A novel dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) for separation/preconcentration of ultra trace amount of vanadium and its determination with the electrothermal atomic absorption spectrometry (ETAAS) was developed. The DLLME-SFO behavior of vanadium (V) using N-benzoyl-N-phenylhydroxylamine (BPHA) as complexing agent was systematically investigated. The factors influencing the complex formation and extraction by DLLME-SFO method were optimized. Under the optimized conditions: 100 microL, 200 microL and 25 mL of extraction solvent (1-undecanol), disperser solvent (acetone) and sample volume, respectively, an enrichment factor of 184, a detection limit (based on 3S(b)/m) of 7 ng L(-1) and a relative standard deviation of 4.6% (at 500 ng L(-1)) were obtained. The calibration graph using the preconcentration system for vanadium was linear from 20 to 1000 ng L(-1) with a correlation coefficient of 0.9996. The method was successfully applied for the determination of vanadium in water and parsley. Copyright 2010 Elsevier B.V. All rights reserved.

Optimization of the capillary zone electrophoresis method for Huperzine A determination using experimental design and artificial neural networks.

PubMed

Hameda, A Ben; Elosta, S; Havel, J

2005-08-19

Huperzine A, natural product from Huperzia serrata, is quite an important compound used to treat the Alzheimer's disease as a food supplement and also proposed as a prospective and prophylactic antidote against organophosphate poisoning. In this work, simple and fast capillary electrophoresis (CE) procedure with UV detection (at 230 nm) for determination of Huperzine A was developed and optimized. Capillary electrophoresis determination of Huperzine A was optimized using a combination of the experimental design (ED) and the artificial neural networks (ANN). In the first stage of optimization, the experiments were done according to the appropriate ED. Data evaluated by ANN allowed finding the optimal values of several analytical parameters (peak area, peak height, and analysis time). Optimal conditions found were 50 mM acetate buffer, pH 4.6, separation voltage 10 kV, hydrodynamic injection time 10 s and temperature 25 degrees C. The developed method shows good repeatability as relative standard division (R.S.D. = 0.9%) and it has been applied for determination of Huperzine A in various pharmaceutical products and in biological liquids. The limit of detection (LOD) in aqueous media was 0.226 ng/ml and 0.233 ng/ml for determination in the serum.

The postural control can be optimized by the first movement initiation condition encountered when submitted to muscle fatigue.

PubMed

Monjo, Florian; Forestier, Nicolas

2017-08-01

We investigated whether and how the movement initiation condition (IC) encountered during the early movements performed following focal muscle fatigue affects the postural control of discrete ballistic movements. For this purpose, subjects performed shoulder flexions in a standing posture at maximal velocity under two movement IC, i.e., in self-paced conditions and submitted to a Stroop-like task in which participants had to trigger fast shoulder flexions at the presentation of incongruent colors. Shoulder flexion kinematics, surface muscle activity of focal and postural muscles as well as center-of-pressure kinematics were recorded. The initial IC and the order in which subjects were submitted to these two conditions were varied within two separate experimental sessions. IC schedule was repeated before and after fatigue protocols involving shoulder flexors. The aim of this fatigue procedure was to affect acceleration-generating capacities of focal muscles. In such conditions, the postural muscle activity preceding and accompanying movement execution is expected to decrease. Following fatigue, when subjects initially moved in self-paced conditions, postural muscle activity decreased and scaled to the lower focal peak acceleration. This postural strategy then transferred to the Stroop-like task. In contrast, when subjects initially moved submitted to the Stroop-like task, postural muscle activity did not decrease and this transferred to self-paced movements. Regarding the center-of-pressure peak velocity, which is indicative of the efficiency of the postural actions generated in stabilizing posture, no difference appeared between the two sessions post-fatigue. This highlights an optimization of the postural actions when subjects first moved in self-paced conditions, smaller postural muscle activation levels resulting in similar postural consequences. In conclusion, the level of neuromuscular activity associated with the postural control is affected and can be optimized by the initial movement IC experienced post-fatigue. Beyond the fundamental contributions arising from these results, we point out potential applications for trainers and sports instructors. Copyright © 2017 Elsevier B.V. All rights reserved.

Optimization of Tangential Mass Injection for Minimizing Flow Separation in a Scramjet Inlet

DTIC Science & Technology

1991-12-01

34 Aerospace EnQineering, Vol. 11. No. 8, August 1991, p.23. 26. Heppenheimer , Thomas A . Lecture notes from Hypersonic Technologies seminar. University...AFIT/GAE/ENY,/9 lD-2 ( /~ AD-A243 868 "DTIC OPTIMIZATION OF TANGENTIAL MASS INJECTION FOR MINIMIZING FLOW SEPARATION IN A SC.R-.MJET INLET THESIS...OF TANGENTIAL MASS INJECTION FOR MINIMIZING FLOW SEPARATION IN A SCRAMJET INLEr THESIS Presented to the Faculty of the School of E.ngineering of the

Improving the Adaptability of Simulated Evolutionary Swarm Robots in Dynamically Changing Environments

PubMed Central

Yao, Yao; Marchal, Kathleen; Van de Peer, Yves

2014-01-01

One of the important challenges in the field of evolutionary robotics is the development of systems that can adapt to a changing environment. However, the ability to adapt to unknown and fluctuating environments is not straightforward. Here, we explore the adaptive potential of simulated swarm robots that contain a genomic encoding of a bio-inspired gene regulatory network (GRN). An artificial genome is combined with a flexible agent-based system, representing the activated part of the regulatory network that transduces environmental cues into phenotypic behaviour. Using an artificial life simulation framework that mimics a dynamically changing environment, we show that separating the static from the conditionally active part of the network contributes to a better adaptive behaviour. Furthermore, in contrast with most hitherto developed ANN-based systems that need to re-optimize their complete controller network from scratch each time they are subjected to novel conditions, our system uses its genome to store GRNs whose performance was optimized under a particular environmental condition for a sufficiently long time. When subjected to a new environment, the previous condition-specific GRN might become inactivated, but remains present. This ability to store ‘good behaviour’ and to disconnect it from the novel rewiring that is essential under a new condition allows faster re-adaptation if any of the previously observed environmental conditions is reencountered. As we show here, applying these evolutionary-based principles leads to accelerated and improved adaptive evolution in a non-stable environment. PMID:24599485

Optimal rendezvous in the neighborhood of a circular orbit

NASA Technical Reports Server (NTRS)

Jones, J. B.

1976-01-01

The minimum velocity-change rendezvous solutions, when the motion may be linearized about a circular orbit, fall into two separate regions; the phase-for-free region and the general region. Phase-for-free solutions are derived from the optimum transfer solutions, require the same velocity-change expenditure, but may not be unique. Analytic solutions are presented in two of the three subregions. An algorithm is presented for determining the unique solutions in the general region. Various sources of initial conditions are discussed and three examples are presented.

An economical state-dependent telecloning for a multiparticle GHZ state

NASA Astrophysics Data System (ADS)

Meng, Fan-Xu; Yu, Xu-Tao; Zhang, Zai-Chen

2018-03-01

The scheme for a 1-3 economical state-dependent telecloning of a multiparticle GHZ state is proposed. It shows that every one of spatially separated three receivers obtains one copy which is dependent on original state. Fidelity can hit to the optimal fidelity 5/6. Meantime, we also propose a 1-3 asymmetric economical telecloning of a particular multiparticle GHZ state by parameterizing coefficients of state in the channel. The three fidelities can reach the best match that is the same as the symmetric case. Furthermore, the above two schemes can be generalized into the case of 1-M(M=2k+1,k>0) telecloning of a multiparticle GHZ state. Satisfying some certain conditions, optimal fidelities with 1/2+(M+1)/4M can be obtained. As without ancilla in the channel, the number of entangled particles is less than one in current schemes and fidelities can be optimal if the original state is an equatorial state.

Application of genetic algorithm in integrated setup planning and operation sequencing

NASA Astrophysics Data System (ADS)

Kafashi, Sajad; Shakeri, Mohsen

2011-01-01

Process planning is an essential component for linking design and manufacturing process. Setup planning and operation sequencing is two main tasks in process planning. Many researches solved these two problems separately. Considering the fact that the two functions are complementary, it is necessary to integrate them more tightly so that performance of a manufacturing system can be improved economically and competitively. This paper present a generative system and genetic algorithm (GA) approach to process plan the given part. The proposed approach and optimization methodology analyses the TAD (tool approach direction), tolerance relation between features and feature precedence relations to generate all possible setups and operations using workshop resource database. Based on these technological constraints the GA algorithm approach, which adopts the feature-based representation, optimizes the setup plan and sequence of operations using cost indices. Case study show that the developed system can generate satisfactory results in optimizing the setup planning and operation sequencing simultaneously in feasible condition.

Method optimization for drug impurity profiling in supercritical fluid chromatography: Application to a pharmaceutical mixture.

PubMed

Muscat Galea, Charlene; Didion, David; Clicq, David; Mangelings, Debby; Vander Heyden, Yvan

2017-12-01

A supercritical chromatographic method for the separation of a drug and its impurities has been developed and optimized applying an experimental design approach and chromatogram simulations. Stationary phase screening was followed by optimization of the modifier and injection solvent composition. A design-of-experiment (DoE) approach was then used to optimize column temperature, back-pressure and the gradient slope simultaneously. Regression models for the retention times and peak widths of all mixture components were built. The factor levels for different grid points were then used to predict the retention times and peak widths of the mixture components using the regression models and the best separation for the worst separated peak pair in the experimental domain was identified. A plot of the minimal resolutions was used to help identifying the factor levels leading to the highest resolution between consecutive peaks. The effects of the DoE factors were visualized in a way that is familiar to the analytical chemist, i.e. by simulating the resulting chromatogram. The mixture of an active ingredient and seven impurities was separated in less than eight minutes. The approach discussed in this paper demonstrates how SFC methods can be developed and optimized efficiently using simple concepts and tools. Copyright © 2017 Elsevier B.V. All rights reserved.

Characteristics of Social Support Among Teenage, Optimal Age, and Advanced Age Women in Canada: An Analysis of the National Longitudinal Survey of Children and Youth.

PubMed

Kim, Theresa H M; Rotondi, Michael; Connolly, Jennifer; Tamim, Hala

2017-06-01

Background Social support is highly valued and beneficial for women, especially after childbirth. The objective was to examine the differences of social support reported among teen, optimal age, and advanced age women, and to identify the characteristics associated with social support separately for each age group. Methods This was a cross-sectional analysis of the National Longitudinal Survey of Children and Youth. Primiparous women with infants were grouped into: teen (15-19 years), optimal age (20-34 years), and advanced age (35 years and older). The outcome was social support (Social Provisions Scale), and demographic, socio-economic, health, community, and infant characteristics were considered for stepwise linear regression, separately for the groups. Results Total of 455,022 mothers was analyzed. Teens had the lowest social support (Mean = 17.56) compared to other groups (Means = 19.07 and 19.05; p < 0.001). Teens' volunteer involvement was associated with an increase in social support (Adjβ 2.77; 95%CI 0.86, 4.68), and depression was associated with a decrease (Adjβ -0.12; 95%CI -0.22, -0.02). Optimal age women's support significantly increased with maternal age (Adjβ 0.07; 95%CI 0.02,0.12), working status (Adjβ 0.60; 95%CI 0.13,1.07), and with chronic condition(s) (Adjβ 0.59; 95%CI 0.16,1.02), while it decreased with depression (Adjβ -0.05; 95%CI -0.10, -0.01) and ever-immigrants (Adjβ -1.67; 95%CI -2.29, -1.04). Use of childcare was associated with increased support among women in advanced age group (Adjβ 1.58; 95%CI 0.12, 3.04). For all groups, social support was significantly associated with neighbourhood safety. Conclusion The characteristics associated with social support varied among the three age groups. The findings may help promote awareness of the essential needs to increase support, especially for teens.

Ion-/proton-conducting apparatus and method

DOEpatents

Yates, Matthew [Penfield, NY; Liu, Dongxia [Rochester, NY

2011-05-17

A c-axis-oriented HAP thin film synthesized by seeded growth on a palladium hydrogen membrane substrate. An exemplary synthetic process includes electrochemical seeding on the substrate, and secondary and tertiary hydrothermal treatments under conditions that favor growth along c-axes and a-axes in sequence. By adjusting corresponding synthetic conditions, an HAP this film can be grown to a controllable thickness with a dense coverage on the underlying substrate. The thin films have relatively high proton conductivity under hydrogen atmosphere and high temperature conditions. The c-axis oriented films may be integrated into fuel cells for application in the intermediate temperature range of 200-600.degree. C. The electrochemical-hydrothermal deposition technique may be applied to create other oriented crystal materials having optimized properties, useful for separations and catalysis as well as electronic and electrochemical applications, electrochemical membrane reactors, and in chemical sensors.

Simple and effective label-free capillary electrophoretic analysis of sugars by complexation using quinoline boronic acids.

PubMed

Kubo, Takuya; Kanemori, Koichi; Kusumoto, Risa; Kawai, Takayuki; Sueyoshi, Kenji; Naito, Toyohiro; Otsuka, Koji

2015-01-01

An effective separation and detection procedure for sugars by capillary electrophoresis (CE) using a complexation between quinolineboronic acid (QBA) and multiple hydroxyl structure of sugar alcohol is reported. We investigated the variation of fluorescence spectra of a variety of QBAs with sorbitol at a wide range of pH conditions and then found that 5-isoQBA strongly enhanced the fluorescence intensity by the complexation at basic pH conditions. The other sugar alcohols having multiple hydroxyls also revealed the enhancement of the fluorescence intensity with 5-isoQBA, whereas the alternation of the intensity was not found in the sugars such as glucose. After optimization of the 5-isoQBA concentration and pH of the buffered solution in CE analysis, 6 sugar alcohols were successfully separated in the order based on the formation constants with 5-isoQBA, which were calculated from the variation of the fluorescence intensity with each sugar alcohol and 5-isoQBA. Furthermore, the limits of detection for sorbitol and xylitol by the CE method were estimated at 15 and 27 μM, respectively.

Capillary electrophoresis with electrochemiluminescent detection for highly sensitive assay of genetically modified organisms.

PubMed

Guo, Longhua; Yang, Huanghao; Qiu, Bin; Xiao, Xueyang; Xue, Linlin; Kim, Donghwan; Chen, Guonan

2009-12-01

A capillary electrophoresis coupled with electrochemiluminescent detection system (CE-ECL) was developed for the detection of polymerase chain reaction (PCR) amplicons. The ECL luminophore, tris(1,10-phenanthroline) ruthenium(II) (Ru(phen)(3)(2+)), was labeled to the PCR primers before amplification. Ru(phen)(3)(2+) was then introduced to PCR amplicons by PCR amplification. Eventually, the PCR amplicons were separated and detected by the homemade CE-ECL system. The detection of a typical genetically modified organism (GMO), Roundup Ready Soy (RRS), was shown as an example to demonstrate the reliability of the proposed approach. Four pairs of primers were amplified by multiple PCR (MPCR) simultaneously, three of which were targeted on the specific sequence of exogenous genes of RRS, and another was targeted on the endogenous reference gene of soybean. Both the conditions for PCR amplification and CE-ECL separation and detection were investigated in detail. Results showed that, under the optimal conditions, the proposed method can accurately identifying RRS. The corresponding limit of detection (LOD) was below 0.01% with 35 PCR cycles.

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

PubMed

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.

Synthesis and application of in-situ molecularly imprinted silica monolithic in pipette-tip solid-phase microextraction for the separation and determination of gallic acid in orange juice samples.

PubMed

Arabi, Maryam; Ghaedi, Mehrorang; Ostovan, Abbas

2017-03-24

A novel strategy was presented for the synthesis and application of functionalized silica monolithic as artificial receptor of gallic acid at micro-pipette tip. A sol-gel process was used to prepare the sorbent. In this in-situ polymerization reaction, tetraethyl orthosilicate (TEOS), 3-aminopropyl trimethoxysilane (APTMS), gallic acid and thiourea were used, respectively, as cross-linker, functionalized monomer, template and precursor to make crack-free and non-fragile structure. Such durable and inexpensive in-situ monolithic was successfully employed as useful tool for highly efficient extraction of gallic acid from orange juice samples. The effective parameters in extraction recovery were investigated and optimum conditions were obtained using experimental design methodology. Applying HPLC-UV for separation quantification at optimal conditions, the gallic acid was efficiently extracted without significant matrix interference. Good linearity for gallic acid in the range of 0.02-5.0mgL -1 with correlation coefficients of R 2 >0.999 revealed well applicability of the method for trace analysis. Copyright © 2017. Published by Elsevier B.V.

Isolation and purification of arctigenin from Fructus Arctii by enzymatic hydrolysis combined with high-speed counter-current chromatography.

PubMed

Liu, Feng; Xi, Xingjun; Wang, Mei; Fan, Li; Geng, Yanling; Wang, Xiao

2014-02-01

Enzymatic hydrolysis pretreatment combined with high-speed counter-current chromatography for the transformation and isolation of arctigenin from Fructus Arctii was successfully developed. In the first step, the extract solution of Fructus Arctii was enzymatic hydrolyzed by β-glucosidase. The optimal hydrolysis conditions were 40°C, pH 5.0, 24 h of hydrolysis time, and 1.25 mg/mL β-glucosidase concentration. Under these conditions, the content of arctigenin was transformed from 2.60 to 12.59 mg/g. In the second step, arctigenin in the hydrolysis products was separated and purified by high-speed counter-current chromatography with a two-phase solvent system composed of petroleum ether/ethyl acetate/methanol/water (10:25:15:20, v/v), and the fraction was analyzed by HPLC, ESI-MS, and (1)H NMR spectroscopy. Finally, 102 mg of arctigenin with a purity of 98.9% was obtained in a one-step separation from 200 mg of hydrolyzed sample. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A New Cluster Analysis-Marker-Controlled Watershed Method for Separating Particles of Granular Soils

PubMed Central

Alam, Md Ferdous

2017-01-01

An accurate determination of particle-level fabric of granular soils from tomography data requires a maximum correct separation of particles. The popular marker-controlled watershed separation method is widely used to separate particles. However, the watershed method alone is not capable of producing the maximum separation of particles when subjected to boundary stresses leading to crushing of particles. In this paper, a new separation method, named as Monash Particle Separation Method (MPSM), has been introduced. The new method automatically determines the optimal contrast coefficient based on cluster evaluation framework to produce the maximum accurate separation outcomes. Finally, the particles which could not be separated by the optimal contrast coefficient were separated by integrating cuboid markers generated from the clustering by Gaussian mixture models into the routine watershed method. The MPSM was validated on a uniformly graded sand volume subjected to one-dimensional compression loading up to 32 MPa. It was demonstrated that the MPSM is capable of producing the best possible separation of particles required for the fabric analysis. PMID:29057823

Cost component analysis.

PubMed

Lörincz, András; Póczos, Barnabás

2003-06-01

In optimizations the dimension of the problem may severely, sometimes exponentially increase optimization time. Parametric function approximatiors (FAPPs) have been suggested to overcome this problem. Here, a novel FAPP, cost component analysis (CCA) is described. In CCA, the search space is resampled according to the Boltzmann distribution generated by the energy landscape. That is, CCA converts the optimization problem to density estimation. Structure of the induced density is searched by independent component analysis (ICA). The advantage of CCA is that each independent ICA component can be optimized separately. In turn, (i) CCA intends to partition the original problem into subproblems and (ii) separating (partitioning) the original optimization problem into subproblems may serve interpretation. Most importantly, (iii) CCA may give rise to high gains in optimization time. Numerical simulations illustrate the working of the algorithm.

Purification of complex samples: Implementation of a modular and reconfigurable droplet-based microfluidic platform with cascaded deterministic lateral displacement separation modules

PubMed Central

Pudda, Catherine; Boizot, François; Verplanck, Nicolas; Revol-Cavalier, Frédéric; Berthier, Jean; Thuaire, Aurélie

2018-01-01

Particle separation in microfluidic devices is a common problematic for sample preparation in biology. Deterministic lateral displacement (DLD) is efficiently implemented as a size-based fractionation technique to separate two populations of particles around a specific size. However, real biological samples contain components of many different sizes and a single DLD separation step is not sufficient to purify these complex samples. When connecting several DLD modules in series, pressure balancing at the DLD outlets of each step becomes critical to ensure an optimal separation efficiency. A generic microfluidic platform is presented in this paper to optimize pressure balancing, when DLD separation is connected either to another DLD module or to a different microfluidic function. This is made possible by generating droplets at T-junctions connected to the DLD outlets. Droplets act as pressure controllers, which perform at the same time the encapsulation of DLD sorted particles and the balance of output pressures. The optimized pressures to apply on DLD modules and on T-junctions are determined by a general model that ensures the equilibrium of the entire platform. The proposed separation platform is completely modular and reconfigurable since the same predictive model applies to any cascaded DLD modules of the droplet-based cartridge. PMID:29768490

Optimization of a hydrodynamic separator using a multiscale computational fluid dynamics approach.

PubMed

Schmitt, Vivien; Dufresne, Matthieu; Vazquez, Jose; Fischer, Martin; Morin, Antoine

2013-01-01

This article deals with the optimization of a hydrodynamic separator working on the tangential separation mechanism along a screen. The aim of this study is to optimize the shape of the device to avoid clogging. A multiscale approach is used. This methodology combines measurements and computational fluid dynamics (CFD). A local model enables us to observe the different phenomena occurring at the orifice scale, which shows the potential of expanded metal screens. A global model is used to simulate the flow within the device using a conceptual model of the screen (porous wall). After validation against the experimental measurements, the global model was used to investigate the influence of deflectors and disk plates in the structure.

Modeling and multi-response optimization of pervaporation of organic aqueous solutions using desirability function approach.

PubMed

Cojocaru, C; Khayet, M; Zakrzewska-Trznadel, G; Jaworska, A

2009-08-15

The factorial design of experiments and desirability function approach has been applied for multi-response optimization in pervaporation separation process. Two organic aqueous solutions were considered as model mixtures, water/acetonitrile and water/ethanol mixtures. Two responses have been employed in multi-response optimization of pervaporation, total permeate flux and organic selectivity. The effects of three experimental factors (feed temperature, initial concentration of organic compound in feed solution, and downstream pressure) on the pervaporation responses have been investigated. The experiments were performed according to a 2(3) full factorial experimental design. The factorial models have been obtained from experimental design and validated statistically by analysis of variance (ANOVA). The spatial representations of the response functions were drawn together with the corresponding contour line plots. Factorial models have been used to develop the overall desirability function. In addition, the overlap contour plots were presented to identify the desirability zone and to determine the optimum point. The optimal operating conditions were found to be, in the case of water/acetonitrile mixture, a feed temperature of 55 degrees C, an initial concentration of 6.58% and a downstream pressure of 13.99 kPa, while for water/ethanol mixture a feed temperature of 55 degrees C, an initial concentration of 4.53% and a downstream pressure of 9.57 kPa. Under such optimum conditions it was observed experimentally an improvement of both the total permeate flux and selectivity.

Electrophoretic studies of polygalacturonate oligomers and their interactions with metal ions.

PubMed

Wiedmer, S K; Cassely, A; Hong, M; Novotny, M V; Riekkola, M L

2000-09-01

Polygalacturonic acid, a linear homopolysaccharide, was investigated by capillary electrophoresis (CE) using linear polyacrylamide-coated capillaries and laser-induced fluorescence (LIF) detection. A successful separation of its fluorescently labeled oligomers was achieved through sieving in polyacrylamide entangled matrices. The reaction conditions for the derivatization of polygalacturonic acid were optimized. In studying the interactions between polygalacturonic acid and various metal ions, the end-label, free-solution electrophoretic (ELFSE) technique, developed earlier in our laboratory (Sudor, J., Novotny, M. V., Anal. Chem. 1995, 67, 4205-4209) was found preferable to the sieving method. ELFSE is fast and convenient in that no polymer solutions are needed for the separation. The investigation showed that for the moderately large oligomers, the strongest binding occurred with calcium and cadmium ions, while the smallest interaction was observed with magnesium ions.

Separation of oil from bilge water I. Bilge water characteristics and the interaction of bilge water with chemically modified surfaces. Interim report, October 1994-September 1995

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chang, E.L.; Calvert, J.M.; Koloski, T.

1997-02-01

We report on the results of a project using surface characterization and novel surface-modification techniques to address the issues of developing a minimally fouling ceramic membrane filter. We have studied the physical characteristics of a synthetic bilge water mixture, examined the surfaces of the ceramic filters for evidence of fouling, and identified several surface modifications that, under laboratory conditions, work well in prevention of foulants. These surfaces include hydrophobic as well as polar coatings. For the bilge water, it was discovered that detergent, at certain concentrations, may be useful in separating and coalescing oil droplets from the bilge water. Basedmore » on the results of the studies, several strategies for optimizing the removal of oil from water are suggested.« less

Using spatiotemporal source separation to identify prominent features in multichannel data without sinusoidal filters.

PubMed

Cohen, Michael X

2017-09-27

The number of simultaneously recorded electrodes in neuroscience is steadily increasing, providing new opportunities for understanding brain function, but also new challenges for appropriately dealing with the increase in dimensionality. Multivariate source separation analysis methods have been particularly effective at improving signal-to-noise ratio while reducing the dimensionality of the data and are widely used for cleaning, classifying and source-localizing multichannel neural time series data. Most source separation methods produce a spatial component (that is, a weighted combination of channels to produce one time series); here, this is extended to apply source separation to a time series, with the idea of obtaining a weighted combination of successive time points, such that the weights are optimized to satisfy some criteria. This is achieved via a two-stage source separation procedure, in which an optimal spatial filter is first constructed and then its optimal temporal basis function is computed. This second stage is achieved with a time-delay-embedding matrix, in which additional rows of a matrix are created from time-delayed versions of existing rows. The optimal spatial and temporal weights can be obtained by solving a generalized eigendecomposition of covariance matrices. The method is demonstrated in simulated data and in an empirical electroencephalogram study on theta-band activity during response conflict. Spatiotemporal source separation has several advantages, including defining empirical filters without the need to apply sinusoidal narrowband filters. © 2017 Federation of European Neuroscience Societies and John Wiley & Sons Ltd.

Resolution and isolation of enantiomers of (±)-isoxsuprine using thin silica gel layers impregnated with L-glutamic acid, comparison of separation of its diastereomers prepared with chiral derivatizing reagents having L-amino acids as chiral auxiliaries.

PubMed

Bhushan, Ravi; Nagar, Hariom

2015-03-01

Thin silica gel layers impregnated with optically pure l-glutamic acid were used for direct resolution of enantiomers of (±)-isoxsuprine in their native form. Three chiral derivatizing reagents, based on DFDNB moiety, were synthesized having l-alanine, l-valine and S-benzyl-l-cysteine as chiral auxiliaries. These were used to prepare diastereomers under microwave irradiation and conventional heating. The diastereomers were separated by reversed-phase high-performance liquid chromatography on a C18 column with detection at 340 nm using gradient elution with mobile phase containing aqueous trifluoroacetic acid and acetonitrile in different compositions and by thin-layer chromatography (TLC) on reversed phase (RP) C18 plates. Diastereomers prepared with enantiomerically pure (+)-isoxsuprine were used as standards for the determination of the elution order of diastereomers of (±)-isoxsuprine. The elution order in the experimental study of RP-TLC and RP-HPLC supported the developed optimized structures of diastereomers based on density functional theory. The limit of detection was 0.1-0.09 µg/mL in TLC while it was in the range of 22-23 pg/mL in HPLC and 11-13 ng/mL in RP-TLC for each enantiomer. The conditions of derivatization and chromatographic separation were optimized. The method was validated for accuracy, precision, limit of detection and limit of quantification. Copyright © 2014 John Wiley & Sons, Ltd.

Silica aerogel coated on metallic wire by phase separation of polystyrene for in-tube solid phase microextraction.

PubMed

Baktash, Mohammad Yahya; Bagheri, Habib

2017-06-02

In this research, an attempt was made toward synthesizing a sol-gel-based silica aerogel and its subsequent coating on a copper wire by phase separation of polystyrene. Adaption of this new approach enabled us to coat the metallic wire with powder materials. The use of this method for coating, led to the formation of a porous and thick structure of silica aerogel. The coated wire was placed in a needle and used as the sorbent for in-tube solid phase microextraction of chlorobenzenes (CBs). The superhydrophobicity of sorbent on extraction efficiency was investigated by using different ratios of tetraethylorthosilicate/methyltrimethoxysilane. The surface coated with the prepared silica aerogel by the phase separation of polystyrene showed high contact angle, approving the desired superhydrophobic properties. Effects of major parameters influencing the extraction efficiency including the extraction temperature, extraction time, ionic strength, desorption time were investigated and optimized. The limits of detection and quantification of the method under the optimized condition were 0.1-1.2 and 0.4-4.1ngL -1 , respectively. The relative standard deviations (RSD%) at a concentration level of 10ngL -1 were between 4 and 10% (n=3). The calibration curves of CBs showed linearity from 1 to100ngL -1 . Eventually, the method was successfully applied to the extraction of model compounds from real water samples and relative recoveries varied from 88 to 115%. Copyright © 2017 Elsevier B.V. All rights reserved.

Biorefinery of cellulosic primary sludge towards targeted Short Chain Fatty Acids, phosphorus and methane recovery.

PubMed

Crutchik, Dafne; Frison, Nicola; Eusebi, Anna Laura; Fatone, Francesco

2018-06-01

Cellulose from used toilet paper is a major untapped resource embedded in municipal wastewater which recovery and valorization to valuable products can be optimized. Cellulosic primary sludge (CPS) can be separated by upstream dynamic sieving and anaerobically digested to recover methane as much as 4.02 m 3 /capita·year. On the other hand, optimal acidogenic fermenting conditions of CPS allows the production of targeted short-chain fatty acids (SCFAs) as much as 2.92 kg COD/capita·year. Here propionate content can be more than 30% and can optimize the enhanced biological phosphorus removal (EBPR) processes or the higher valuable co-polymer of polyhydroxyalkanoates (PHAs). In this work, first a full set of batch assays were used at three different temperatures (37, 55 and 70 °C) and three different initial pH (8, 9 and 10) to identify the best conditions for optimizing both the total SCFAs and propionate content from CPS fermentation. Then, the optimal conditions were applied in long term to a Sequencing Batch Fermentation Reactor where the highest propionate production (100-120 mg COD/g TVS fed ·d) was obtained at 37 °C and adjusting the feeding pH at 8. This was attributed to the higher hydrolysis efficiency of the cellulosic materials (up to 44%), which increased the selective growth of Propionibacterium acidopropionici in the fermentation broth up to 34%. At the same time, around 88% of the phosphorus released during the acidogenic fermentation was recovered as much as 0.15 kg of struvite per capita·year. Finally, the potential market value was preliminary estimated for the recovered materials that can triple over the conventional scenario of biogas recovery in existing municipal wastewater treatment plants. Copyright © 2018 Elsevier Ltd. All rights reserved.

Optimization of the SPME parameters and its online coupling with HPLC for the analysis of tricyclic antidepressants in plasma samples.

PubMed

Alves, Claudete; Fernandes, Christian; Dos Santos Neto, Alvaro José; Rodrigues, José Carlos; Costa Queiroz, Maria Eugênia; Lanças, Fernando Mauro

2006-07-01

Solid-phase microextraction (SPME)-liquid chromatography (LC) is used to analyze tricyclic antidepressant drugs desipramine, imipramine, nortriptyline, amitriptyline, and clomipramine (internal standard) in plasma samples. Extraction conditions are optimized using a 2(3) factorial design plus a central point to evaluate the influence of the time, temperature, and matrix pH. A Polydimethylsiloxane-divinylbenzene (60-mum film thickness) fiber is selected after the assessment of different types of coating. The chromatographic separation is realized using a C(18) column (150 x 4.6 mm, 5-microm particles), ammonium acetate buffer (0.05 mol/L, pH 5.50)-acetonitrile (55:45 v/v) with 0.1% of triethylamine as mobile phase and UV-vis detection at 214 nm. Among the factorial design conditions evaluated, the best results are obtained at a pH 11.0, temperature of 30 degrees C, and extraction time of 45 min. The proposed method, using a lab-made SPME-LC interface, allowed the determination of tricyclic antidepressants in in plasma at therapeutic concentration levels.

Dual priming oligonucleotide system for the multiplex detection of respiratory viruses and SNP genotyping of CYP2C19 gene.

PubMed

Chun, Jong-Yoon; Kim, Kyoung-Joong; Hwang, In-Taek; Kim, Yun-Jee; Lee, Dae-Hoon; Lee, In-Kyoung; Kim, Jong-Kee

2007-01-01

Successful PCR starts with proper priming between an oligonucleotide primer and the template DNA. However, the inevitable risk of mismatched priming cannot be avoided in the currently used primer system, even though considerable time and effort are devoted to primer design and optimization of reaction conditions. Here, we report a novel dual priming oligonucleotide (DPO) which contains two separate priming regions joined by a polydeoxyinosine linker. The linker assumes a bubble-like structure which itself is not involved in priming, but rather delineates the boundary between the two parts of the primer. This structure results in two primer segments with distinct annealing properties: a longer 5'-segment that initiates stable priming, and a short 3'-segment that determines target-specific extension. This DPO-based system is a fundamental tool for blocking extension of non-specifically primed templates, and thereby generates consistently high PCR specificity even under less than optimal PCR conditions. The strength and utility of the DPO system are demonstrated here using multiplex PCR and SNP genotyping PCR.

Catalytic conversion of carbohydrates to 5-hydroxymethylfurfural from the waste liquid of acid hydrolysis NCC.

PubMed

Sun, Yonghui; Liu, Pengtao; Liu, Zhong

2016-05-20

The principal goal of this work was to reuse the carbohydrates and recycle sulfuric acid in the waste liquid of acid hydrolysis nanocrystalline cellulose (NCC). Therefore, in this work, the optimizations of further hydrolysis of waste liquid of acid hydrolysis NCC and catalytic conversion of L4 to 5-hydroxymethylfurfural (5-HMF) were studied. Sulfuric acid was separated by spiral wound diffusion dialysis (SWDD). The results revealed that cellulose can be hydrolyze to glucose absolutely under the condition of temperature 35 °C, 3 h, and sulfuric acid's concentration 62 wt%. And 78.3% sulfuric acid was recovered by SWDD. The yield of 5-HMF was highest in aqueous solution under the optimal condition was as follows, temperature 160 °C, 3 h, and sulfuric acid's concentration 12 wt%. Then the effect of biphasic solvent systems catalytic conversion and inorganic salt as additives were still examined. The results showed that both of them contributed to prepare 5-HMF. The yield and selectivity of 5-HMF was up to 21.0% and 31.4%, respectively. Copyright © 2016 Elsevier Ltd. All rights reserved.

Impacts analysis of car following models considering variable vehicular gap policies

NASA Astrophysics Data System (ADS)

Xin, Qi; Yang, Nan; Fu, Rui; Yu, Shaowei; Shi, Zhongke

2018-07-01

Due to the important roles playing in the vehicles' adaptive cruise control system, variable vehicular gap polices were employed to full velocity difference model (FVDM) to investigate the traffic flow properties. In this paper, two new car following models were put forward by taking constant time headway(CTH) policy and variable time headway(VTH) policy into optimal velocity function, separately. By steady state analysis of the new models, an equivalent optimal velocity function was defined. To determine the linear stable conditions of the new models, we introduce equivalent expressions of safe vehicular gap, and then apply small amplitude perturbation analysis and long terms of wave expansion techniques to obtain the new models' linear stable conditions. Additionally, the first order approximate solutions of the new models were drawn at the stable region, by transforming the models into typical Burger's partial differential equations with reductive perturbation method. The FVDM based numerical simulations indicate that the variable vehicular gap polices with proper parameters directly contribute to the improvement of the traffic flows' stability and the avoidance of the unstable traffic phenomena.

Strategies for enhanced deammonification performance and reduced nitrous oxide emissions.

PubMed

Leix, Carmen; Drewes, Jörg E; Ye, Liu; Koch, Konrad

2017-07-01

Deammonification's performance and associated nitrous oxide emissions (N 2 O) depend on operational conditions. While studies have investigated factors for high performances and low emissions separately, this study investigated optimizing deammonification performance while simultaneously reducing N 2 O emissions. Using a design of experiment (DoE) method, two models were developed for the prediction of the nitrogen removal rate and N 2 O emissions during single-stage deammonification considering three operational factors (i.e., pH value, feeding and aeration strategy). The emission factor varied between 0.7±0.5% and 4.1±1.2% at different DoE-conditions. The nitrogen removal rate was predicted to be maximized at settings of pH 7.46, intermittent feeding and aeration. Conversely, emissions were predicted to be minimized at the design edges at pH 7.80, single feeding, and continuous aeration. Results suggested a weak positive correlation between the nitrogen removal rate and N 2 O emissions, thus, a single optimizing operational set-point for maximized performance and minimized emissions did not exist. Copyright © 2017 Elsevier Ltd. All rights reserved.

Development of an analytical method for separation of phenolic acids by ultra-performance convergence chromatography (UPC2) using a column packed with a sub-2-μm particle.

PubMed

Jiang, Hai; Yang, Liu; Xing, Xudong; Yan, Meiling; Guo, Xinyue; Yang, Bingyou; Wang, Qiu-Hong; Kuang, Hai-Xue

2018-05-10

Phenolic acids are important active components of certain Traditional Chinese Medicines (TCM) and have a wide range of biological effects. Separation and purification of phenolic acids remains challenging due to difficulties with quality control using existing chromatographic methods The purpose of this study was to compare the effects of different chromatographic columns and conditions for the separation of phenolic acids. The BEH column was determined to be optimal, providing efficient separation in the shortest time (17.00 min) using gradient elution with carbon dioxide as the mobile phase, methanol/acetonitrile (70:30, v/v) with 1% TFA as the modifier, and a flow rate of 0.8 mL/min. Good peak shapes were obtained, and the peak asymmetry values were close to 1.00 for all phenolic acids. The resolution was more than 2.83 for all separated peaks. The developed method was subsequently applied to the determination of phenolic acids in Xanthii Fructus. These results are beneficial for quality control and standardization of herbal drugs using UPC 2 , providing an efficient, rapid and environmentally friendly scientific basis for future analysis of phenolic acids. Copyright © 2018. Published by Elsevier B.V.

Quantification of steviol glycosides in food products, Stevia leaves and formulations by planar chromatography, including proof of absence for steviol and isosteviol.

PubMed

Wald, Julian P; Morlock, Gertrud E

2017-07-14

Steviol glycosides may degrade in food products under certain processing and storage conditions. Hence, a method was developed that separated in the same chromatographic run seven important steviol glycosides, and additionally as a sum parameter, their reported breakdown products steviol and isosteviol. Through derivatizations with the 2-naphthol and the primuline reagent, the detection was selective and inexpensive. In case needed, the baseline separation of steviol and isosteviol was also demonstrated after a plate cut and subsequent short development (two-step method). The HPTLC method was robust with regard to varying sample matrix loads, as the stationary phase was used only once. A high sample throughput was achieved, i.e. 23 separations were performed in parallel on one plate. The total analysis time took 1h (30min application, 15min separation and 15min derivatization/densitometry) leading to a calculated analysis time of 2.6min per sample. The solvent consumption was 8mL in total (0.4mL per analysis). HPTLC-ESI-MS was employed for confirmation of the results obtained. Mass spectra were recorded only from the zones of interest, and not from matrix or background, leading to decisive advantages, such as less need for MS cleaning. The optimized HPTLC method was shown to effectively support quality control, as marketed samples may be falsified with cheaper synthetic sweeteners, which was also demonstrated in this study. The accuracy of the densitometric quantification in HPTLC was considered as high, as standards and samples were separated on fresh adsorbent and detected simultaneously under identical conditions, which minimized the influence of errors. Finally, the Aliivibrio fischeri bioassay was employed to obtain information on bioactive compounds in Stevia leaf extracts. Copyright © 2017 Elsevier B.V. All rights reserved.

Separating effective high density polyethylene segments from olefin block copolymers using high temperature liquid chromatography with a preloaded discrete adsorption promoting solvent barrier.

PubMed

Chatterjee, Tirtha; Rickard, Mark A; Pearce, Eric; Pangburn, Todd O; Li, Yongfu; Lyons, John W; Cong, Rongjuan; deGroot, A Willem; Meunier, David M

2016-09-23

Recent advances in catalyst technology have enabled the synthesis of olefin block copolymers (OBC). One type is a "hard-soft" OBC with a high density polyethylene (HDPE) block and a relatively low density polyethylene (VLDPE) block targeted as thermoplastic elastomers. Presently, one of the major challenges is to fractionate HDPE segments from the other components in an experimental OBC sample (block copolymers and VLDPE segments). Interactive high temperature liquid chromatography (HTLC) is ineffective for OBC separation as the HDPE segments and block copolymer chains experience nearly identical enthalpic interactions with the stationary phase and co-elute. In this work we have overcome this challenge by using liquid chromatography under the limiting conditions of desorption (LC LCD). A solvent plug (discrete barrier) is introduced in front of the sample which specifically promotes the adsorption of HDPE segments on the stationary phase (porous graphitic carbon). Under selected thermodynamic conditions, VLDPE segments and block copolymer chains crossed the barrier while HDPE segments followed the pore-included barrier solvent and thus enabled separation. The barrier solvent composition was optimized and the chemical composition of fractionated polymer chains was investigated as a function of barrier solvent strength using an online Fourier-transform infrared (FTIR) detector. Our study revealed that both the HDPE segments as well as asymmetric block copolymer chains (HDPE block length≫VLDPE block length) are retained in the separation and the barrier strength can be tailored to retain a particular composition. At the optimum barrier solvent composition, this method can be applied to separate effective HDPE segments from the other components, which has been demonstrated using an experimental OBC sample. Copyright © 2016 Elsevier B.V. All rights reserved.

Simultaneous separation and determination of praeruptorin A, B and C by micellar electrokinetic chromatography using sodium dodecyl sulphate and sodium cholate as mixed micelles.

PubMed

Chen, Meng; Chang, Ruimiao; Xu, Liying; Huang, Yayun; Zhang, Hongfen; Chen, Anjia

2018-02-02

Praeruptorin A, B and C are major bioactive constituents in Peucedani Radix. They display anti-inflammatory effect, anti-hypertension effect, antiplatelet aggregation, potential anti-cancer activities and so on. They are worthy of investigation as potentially novel and versatile drugs. To develop a method using micellar electrokinetic chromatography (MEKC) for the application in simultaneously separation and determination of praeruptorin A, B and C from Peucedani Radix and its medicinal preparations. Method optimisation was carried out by investigating influences of significant factors on the separation. The method was subjected to validation. The determination of praeruptorin A, B and C in Peucedani Radix and its drug formulations was accomplished by the developed method. The optimal separation condition was 20 mM borate buffer containing 40 mM sodium cholate (SC), 22 mM sodium dodecyl sulphate (SDS) and 25% (v/v) acetonitrile (pH 10.00); 15 kV of voltage; 25°C of temperature; detection at 224 nm. Under this condition, three analytes were baseline separated within 16 min. A good linearity was obtained with correlation coefficients from 0.9988 to 0.9995. The limits of detection (LODs) and limits of quantitation (LOQs) ranged from 0.50 to 0.80 μg/mL and from 1.50 to 2.50 μg/mL, respectively. The recoveries ranged between 95.3% and 103.4%. The proposed method has been successfully applied to the simultaneous determination of praeruptorin A, B and C in Peucedani Radix and its pharmaceutical preparations. Additionally, it could be a potential alternative to the quality control of Peucedani Radix. Copyright © 2018 John Wiley & Sons, Ltd.

Pareto-optimal reversed-phase chromatography separation of three insulin variants with a solubility constraint.

PubMed

Arkell, Karolina; Knutson, Hans-Kristian; Frederiksen, Søren S; Breil, Martin P; Nilsson, Bernt

2018-01-12

With the shift of focus of the regulatory bodies, from fixed process conditions towards flexible ones based on process understanding, model-based optimization is becoming an important tool for process development within the biopharmaceutical industry. In this paper, a multi-objective optimization study of separation of three insulin variants by reversed-phase chromatography (RPC) is presented. The decision variables were the load factor, the concentrations of ethanol and KCl in the eluent, and the cut points for the product pooling. In addition to the purity constraints, a solubility constraint on the total insulin concentration was applied. The insulin solubility is a function of the ethanol concentration in the mobile phase, and the main aim was to investigate the effect of this constraint on the maximal productivity. Multi-objective optimization was performed with and without the solubility constraint, and visualized as Pareto fronts, showing the optimal combinations of the two objectives productivity and yield for each case. Comparison of the constrained and unconstrained Pareto fronts showed that the former diverges when the constraint becomes active, because the increase in productivity with decreasing yield is almost halted. Consequently, we suggest the operating point at which the total outlet concentration of insulin reaches the solubility limit as the most suitable one. According to the results from the constrained optimizations, the maximal productivity on the C 4 adsorbent (0.41 kg/(m 3  column h)) is less than half of that on the C 18 adsorbent (0.87 kg/(m 3  column h)). This is partly caused by the higher selectivity between the insulin variants on the C 18 adsorbent, but the main reason is the difference in how the solubility constraint affects the processes. Since the optimal ethanol concentration for elution on the C 18 adsorbent is higher than for the C 4 one, the insulin solubility is also higher, allowing a higher pool concentration. An alternative method of finding the suggested operating point was also evaluated, and it was shown to give very satisfactory results for well-mapped Pareto fronts. Copyright © 2017 Elsevier B.V. All rights reserved.

A summary report on system effectiveness and optimization study

NASA Technical Reports Server (NTRS)

Williamson, O. L.; Rydberg, A. J.; Dorris, G.

1973-01-01

Report treats optimization and effectiveness separately. Report illustrates example of dynamic programming solution to system optimization. Computer algorithm has been developed to solve effectiveness problem and is included in report.

Hydrophilic interaction liquid chromatography in analysis of granisetron HCl and its related substances. Retention mechanisms and method development.

PubMed

Maksić, Jelena; Tumpa, Anja; Stajić, Ana; Jovanović, Marko; Rakić, Tijana; Jančić-Stojanović, Biljana

2016-05-10

In this paper separation of granisetron and its two related substances in HILIC mode is presented. Separation was done on silica column derivatized with sulfoalkylbetaine groups (ZIC-HILIC). Firstly, retention mechanisms were assessed whereby retention factors of substances were followed in wide range of acetonitrile content (80-97%), at constant concentration of aqueous buffer (10mM) as well as at constant pH value of 3.0. Further, in order to developed optimal HILIC method, Design of Experiments (DoE) methodology was applied. For optimization full factorial design 3(2) was employed. Influence of acetonitrile content and ammonium acetate concentration were investigated while pH of the water phase was kept at 3.3. Adequacy of obtained mathematical models was confirmed by ANOVA. Optimization goals (α>1.15 and minimal run time) were accomplished with 94.7% of acetonitrile in mobile phase and 70 mM of ammonium acetate in water phase. Optimal point was in the middle of defined Design Space. In the next phase, robustness was experimetally tested by Rechtschaffen design. The investigated factors and their levels were: acetonitrile content (±1%), ammonium acetate molarity in water phase (±2 mM), pH value of water phase (±0.2) and column temperature (±4 °C). The validation scope included selectivity, linearity, accuracy and precision as well as determination of limit of detection (LOD) and limit of quantification (LOQ) for the related substances. Additionally, the validation acceptance criteria were met in all cases. Finally, the proposed method could be successfully utilized for estimation of granisetron HCl and its related substances in tablets and parenteral dosage forms, as well as for monitoring degradation under various stress conditions. Copyright © 2016 Elsevier B.V. All rights reserved.

Single-Laboratory Validation for the Determination of Flavonoids in Hawthorn Leaves and Finished Products by LC-UV.

PubMed

Mudge, Elizabeth M; Liu, Ying; Lund, Jensen A; Brown, Paula N

2016-11-01

Suitably validated analytical methods that can be used to quantify medicinally active phytochemicals in natural health products are required by regulators, manufacturers, and consumers. Hawthorn ( Crataegus ) is a botanical ingredient in natural health products used for the treatment of cardiovascular disorders. A method for the quantitation of vitexin-2″- O - rhamnoside, vitexin, isovitexin, rutin, and hyperoside in hawthorn leaf and flower raw materials and finished products was optimized and validated according to AOAC International guidelines. A two-level partial factorial study was used to guide the optimization of the sample preparation. The optimal conditions were found to be a 60-minute extraction using 50 : 48 : 2 methanol : water : acetic acid followed by a 25-minute separation using a reversed-phased liquid chromatography column with ultraviolet absorbance detection. The single-laboratory validation study evaluated method selectivity, accuracy, repeatability, linearity, limit of quantitation, and limit of detection. Individual flavonoid content ranged from 0.05 mg/g to 17.5 mg/g in solid dosage forms and raw materials. Repeatability ranged from 0.7 to 11.7 % relative standard deviation corresponding to HorRat ranges from 0.2 to 1.6. Calibration curves for each flavonoid were linear within the analytical ranges with correlation coefficients greater than 99.9 %. Herein is the first report of a validated method that is fit for the purpose of quantifying five major phytochemical marker compounds in both raw materials and finished products made from North American ( Crataegus douglasii ) and European ( Crataegus monogyna and Crataegus laevigata) hawthorn species. The method includes optimized extraction of samples without a prolonged drying process and reduced liquid chromatography separation time. Georg Thieme Verlag KG Stuttgart · New York.

Quantification of Carbohydrates in Grape Tissues Using Capillary Zone Electrophoresis

PubMed Central

Zhao, Lu; Chanon, Ann M.; Chattopadhyay, Nabanita; Dami, Imed E.; Blakeslee, Joshua J.

2016-01-01

Soluble sugars play an important role in freezing tolerance in both herbaceous and woody plants, functioning in both the reduction of freezing-induced dehydration and the cryoprotection of cellular constituents. The quantification of soluble sugars in plant tissues is, therefore, essential in understanding freezing tolerance. While a number of analytical techniques and methods have been used to quantify sugars, most of these are expensive and time-consuming due to complex sample preparation procedures which require the derivatization of the carbohydrates being analyzed. Analysis of soluble sugars using capillary zone electrophoresis (CZE) under alkaline conditions with direct UV detection has previously been used to quantify simple sugars in fruit juices. However, it was unclear whether CZE-based methods could be successfully used to quantify the broader range of sugars present in complex plant extracts. Here, we present the development of an optimized CZE method capable of separating and quantifying mono-, di-, and tri-saccharides isolated from plant tissues. This optimized CZE method employs a column electrolyte buffer containing 130 mM NaOH, pH 13.0, creating a current of 185 μA when a separation voltage of 10 kV is employed. The optimized CZE method provides limits-of-detection (an average of 1.5 ng/μL) for individual carbohydrates comparable or superior to those obtained using gas chromatography–mass spectrometry, and allows resolution of non-structural sugars and cell wall components (structural sugars). The optimized CZE method was successfully used to quantify sugars from grape leaves and buds, and is a robust tool for the quantification of plant sugars found in vegetative and woody tissues. The increased analytical efficiency of this CZE method makes it ideal for use in high-throughput metabolomics studies designed to quantify plant sugars. PMID:27379118

Optimizing conditions for the extraction of pigments in cochineals (Dactylopius coccus Costa) using response surface methodology.

PubMed

González, Mónica; Méndez, Jesús; Carnero, Aurelio; Lobo, M Gloria; Afonso, Ana

2002-11-20

A simple method was developed for the extraction and determination of color pigments in cochineals (Dactylopius coccus Costa). The procedure was based on the solvent extraction of pigments in insect samples using methanol:water (65:35, v:v) as extractant. Two-level factorial design was used in order to optimize the solvent extraction parameters: temperature, time, methanol concentration in the extractant mixture, and the number of extractions. The results suggest that the number of extractions is statistically the most significant factor. The separation and determination of the pigments was carried out by high-performance liquid chromatography with UV-visible detection. Because the absorption spectra of different pigments are different in the visible region, it is convenient to use a diode array detector to obtain chromatographic profiles that allow for the characterization of the extracted pigments.

Integration of a Graphite/PMMA CompositeElectrode into a Poly(methyl methacrylate) (PMMA) Substrate for Electrochemical Detection in Microchips

PubMed Central

Regel, Anne; Lunte, Susan

2013-01-01

Traditional fabrication methods for polymer microchips, the bonding of two substrates together to form the microchip, can make the integration of carbon electrodes difficult. We have developed a simple and inexpensive method to integrate graphite/PMMA composite electrodes (GPCEs) into a PMMA substrate. These substrates can be bonded to other PMMA layers using a solvent-assisted thermal bonding method. The optimal composition of the GPCEs for electrochemical detection was determined using cyclic voltammetry with dopamine as a test analyte. Using the optimized GPCEs in an all-PMMA flow cell with flow injection analysis, it was possible to detect 50 nM dopamine under the best conditions. These electrodes were also evaluated for the detection of dopamine and catechol following separation by microchip electrophoresis (ME). PMID:23670816

Separation science is the key to successful biopharmaceuticals.

PubMed

Guiochon, Georges; Beaver, Lois Ann

2011-12-09

The impact of economic change, advances in science, therapy and production processes resulted in considerable growth in the area of biopharmaceuticals. Progress in selection of microorganisms and improvements in cell culture and bioreactors is evidenced by increased yields of the desired products in the complex fermentation mixture. At this stage the downstream process of extraction and purification of the desired biopharmaceutical requires considerable attention in the design and operation of the units used for preparative chromatography. Understanding of the process, optimization of column design and experimental conditions have become critical to the biopharmaceutical industry in order to minimize production costs while satisfying new regulatory requirements. Optimization of the purification of biopharmaceuticals by preparative liquid chromatography including an examination of column preparation and bed properties is the focus of this manuscript. Copyright © 2011 Elsevier B.V. All rights reserved.

Application of microchip CGE for the analysis of PEG-modified recombinant human granulocyte-colony stimulating factors.

PubMed

Park, Eun Ji; Lee, Kyung Soo; Lee, Kang Choon; Na, Dong Hee

2010-11-01

The purpose of this study was to evaluate the microchip CGE (MCGE) for the analysis of PEG-modified granulocyte-colony stimulating factor (PEG-G-CSF) prepared with PEG-aldehydes. The unmodified and PEG-modified G-CSFs were analyzed by Protein 80 and 230 Labchips on the Agilent 2100 Bioanalyzer. The MCGE allowed size-based separation and quantitation of PEG-G-CSF. The Protein 80 Labchip was useful for PEG-5K-G-CSF, while the Protein 230 Labchip was more suitable for PEG-20K-G-CSF. The MCGE was also used to monitor a search for optimal PEG-modification (PEGylation) conditions to produce mono-PEG-G-CSF. This study demonstrates the usefulness of MCGE for monitoring and optimizing the PEGylation of G-CSF with the advantages of speed, minimal sample consumption, and automatic quantitation.

Purification of coumarin compounds from Cortex fraxinus by adsorption chromatography.

PubMed

Yu, Minglan; Sun, Ailing; Zhang, Yongqing; Liu, Renmin

2014-10-01

In this paper, a chromatographic method for isolation and purification of coumarin compounds from Cortex fraxinus was established by using Superose 12 as the separation media for the first time. The conditions for separation were optimized. Four kinds of coumarin compounds including aesuletin, aesculin, fraxetin and fraxin were obtained. The purity of these compounds were 98.5, 99.1, 97.9 and 97.3%, respectively, which were determined by HPLC area normalization method. The chemical structures of the separated compounds were identified according to (1)H and (13)C nuclear magnetic resonance data. The retention behavior of the separated coumarin compounds on Superose 12 was also discussed. The retention is based on a mixture of hydrogen bonding and hydrophobic interactions between the coumarin compounds and the residues of the cross-linking reagents used in the manufacturing process of Superose 12. The results of this paper indicate that Superose 12 is not only suitable for size-exclusion chromatography of proteins and other biological macromolecules but also for low-molecular-weight natural products. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Entropy-based separation of yeast cells using a microfluidic system of conjoined spheres

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huang, Kai-Jian; Qin, S.-J., E-mail: shuijie.qin@gmail.com; Bai, Zhong-Chen

2013-11-21

A physical model is derived to create a biological cell separator that is based on controlling the entropy in a microfluidic system having conjoined spherical structures. A one-dimensional simplified model of this three-dimensional problem in terms of the corresponding effects of entropy on the Brownian motion of particles is presented. This dynamic mechanism is based on the Langevin equation from statistical thermodynamics and takes advantage of the characteristics of the Fokker-Planck equation. This mechanism can be applied to manipulate biological particles inside a microfluidic system with identical, conjoined, spherical compartments. This theoretical analysis is verified by performing a rapid andmore » a simple technique for separating yeast cells in these conjoined, spherical microfluidic structures. The experimental results basically match with our theoretical model and we further analyze the parameters which can be used to control this separation mechanism. Both numerical simulations and experimental results show that the motion of the particles depends on the geometrical boundary conditions of the microfluidic system and the initial concentration of the diffusing material. This theoretical model can be implemented in future biophysics devices for the optimized design of passive cell sorters.« less

[[Chiral separation of five arylpropionic acid drugs and determination of their enantiomers in pharmaceutical preparations by reversed-phase high performance liquid chromatography with cellulose-tris-(4-methylbenzoate) stationary phase

PubMed

Luo, An; Wan, Qiang; Fan, Huajun; Chen, Zhi; Wu, Xuehao; Huang, Xiaowen; Zang, Linquan

2014-09-01

Chromatographic behaviors for enantiomeric separation of arylpropionic acid drugs were systematically developed by reversed phase-high performance liquid chromatography (RP-HPLC) using cellulose-tris-(4-methylbenzoate) (CTMB) as chiral stationary phase (CSP). The effects of the composition of the mobile phase, additives and temperature on chiral separation of flurbiprofen, pranoprofen, naproxen, ibuprofen and loxoprofen were further investigated. The enantiomers had been successfully separated on CSP of CTMB by the mobile phase of methanol-0.1% (v/v) formic acid except naproxen by acetonitrile-0.1% (v/v) formic acid at 25 °C. The mechanisms of the racemic resolution for the above mentioned five drugs are discussed thermodynamically and structurally. The resolutions between respective enantiomers for arylpropionic acid drugs on CTMB had significant differences due to their chromatographic behaviors. The order of resolutions ranked pranoprofen, loxoprofen, flurbiprofen, ibuprofen and naproxen. The method established has been successfully applied to the determination of the enantiomers of the five drugs in commercial preparations under the optimized conditions. It proved that the method is simple, reliable and accurate.

Design and testing of a pilot scale magnetic separator for the treatment of textile dyeing wastewater.

PubMed

Salinas, Tobías; Durruty, Ignacio; Arciniegas, Lorena; Pasquevich, Gustavo; Lanfranconi, Matías; Orsi, Isabela; Alvarez, Vera; Bonanni, Sebastian

2018-07-15

Iron nanoparticles can be incorporated on the structure of natural clays to obtain magnetic clays, an adsorbent that be easily removed from a wastewater by magnetic means. Magnetic clays have high adsorption capacities of different contaminants such as heavy metals, fungicides, aromatic compounds and colorants and show rapid adsorption kinetics, but crucial data for achieving its full or pilot scale application is still lacking. In this work, magnetic bentonites with different amounts of magnetite (iron fractions on the clay of 0.55, 0.6 and 0.6) were used to remove color from a real textile wastewater. On a first stage the optimal conditions for the adsorption of the dye, including pH, temperature and clay dosage were determined. Also design parameters for the separation process such as residence time, distance from magnet to magnetic clay and magnet strength were obtained. Finally a pilot scale magnetic drum separator was constructed and tested. A removal of 60% of the dye from a wastewater that contained more than 250 ppm of azo dye was achieved with only 10 min of residence time inside the separator. Copyright © 2018 Elsevier Ltd. All rights reserved.

Active room compensation for sound reinforcement using sound field separation techniques.

PubMed

Heuchel, Franz M; Fernandez-Grande, Efren; Agerkvist, Finn T; Shabalina, Elena

2018-03-01

This work investigates how the sound field created by a sound reinforcement system can be controlled at low frequencies. An indoor control method is proposed which actively absorbs the sound incident on a reflecting boundary using an array of secondary sources. The sound field is separated into incident and reflected components by a microphone array close to the secondary sources, enabling the minimization of reflected components by means of optimal signals for the secondary sources. The method is purely feed-forward and assumes constant room conditions. Three different sound field separation techniques for the modeling of the reflections are investigated based on plane wave decomposition, equivalent sources, and the Spatial Fourier transform. Simulations and an experimental validation are presented, showing that the control method performs similarly well at enhancing low frequency responses with the three sound separation techniques. Resonances in the entire room are reduced, although the microphone array and secondary sources are confined to a small region close to the reflecting wall. Unlike previous control methods based on the creation of a plane wave sound field, the investigated method works in arbitrary room geometries and primary source positions.

Optimal entanglement witnesses for qubits and qutrits

NASA Astrophysics Data System (ADS)

Bertlmann, Reinhold A.; Durstberger, Katharina; Hiesmayr, Beatrix C.; Krammer, Philipp

2005-11-01

We study the connection between the Hilbert-Schmidt measure of entanglement (that is the minimal distance of an entangled state to the set of separable states) and entanglement witness in terms of a generalized Bell inequality which distinguishes between entangled and separable states. A method for checking the nearest separable state to a given entangled one is presented. We illustrate the general results by considering isotropic states, in particular two-qubit and two-qutrit states—and their generalizations to arbitrary dimensions—where we calculate the optimal entanglement witnesses explicitly.

Optimized extraction by cetyl trimethyl ammonium bromide reversed micelles of xylose reductase and xylitol dehydrogenase from Candida guilliermondii homogenate.

PubMed

Cortez, Ely Vieira; Pessoa, Adalberto; das Graças de Almeida Felipe, Maria; Roberto, Inês Conceição; Vitolo, Michele

2004-07-25

The intracellular enzymes xylose reductase (XR, EC 1.1.1.21) and xylitol dehydrogenase (XD, EC 1.1.1.9) from Candida guilliermondii, grown in sugar cane bagasse hydrolysate, were separated by reversed micelles of cetyl trimethyl ammonium bromide (CTAB) cationic surfactant. An experimental design was employed to optimize the extraction conditions of both enzymes. Under these conditions (temperature = 5 degree C, hexanol: isooctane proportion = 5% (v/v), 22 %, surfactant concentration = 0.15M, pH = 7.0 and electrical conductivity = 14 mScm(-1)) recovery values of about 100 and 80% were achieved for the enzymes XR and XD, respectively. The purity of XR and XD increased 5.6- and 1.8-fold, respectively. The extraction process caused some structural modifications in the enzymes molecules, as evidenced by the alteration of K(M) values determined before and after extraction, either in regard to the substrate (up 35% for XR and down 48% for XD) or cofactor (down 29% for XR and up 11% for XD). However, the average variation of V(max) values for both enzymes was not higher than 7%, indicating that the modified affinity of enzymes for their respective substrates and cofactors, as consequence of structural modifications suffered by them during the extraction, are compensated in some extension. This study demonstrated that liquid-liquid extraction by CTAB reversed micelles is an efficient process to separate the enzymes XR and XD present in the cell extract, and simultaneously increase the enzymatic activity and the purity of both enzymes produced by C. guilliermondii.

[Rapid Detection of Adenovirus in Fecal Samples by Capillary Electrophoresis-laser Induced Fluorescence and Microchip Capillary Electrophoresis-laser Induced Fluorescence].

PubMed

Ruan, Jia; Ren, Dong-xia; Yang, Dan-ni; Long, Pin-pin; Zhao, Hong-yue; Wang, Yi-qi; Li, Yong-xin

2015-07-01

To establish a rapid and sensitive method based on polymerase chain reaction (PCR) combined with capillary electrophoresis-laser induced fluorescence (CE-LIF) and microchip capillary electrophoresis-laser induced fluorescence (MCE-LIF) for detecting adenoviruses in fecal samples. The DNA of adenovirus in fecal samples were extracted by the commercial kits and the conserved region of hexon gene was selected as the target gene and amplified by PCR reaction. After labeling highly sensitive nucleic acid fluorescent dye SYBR Gold and SYBR Orange respectively, PCR amplification products were separated by CE and MCE under the optimized condition and detected by LIF detector. PCR amplification products could be detected within 9 min by CE-LIF and 6 min by MCE-LIF under the optimized separation condition. The sequenced PCR product showed good specificity in comparison with the prototype sequences from NCBI. The intraday and inter-day relative standard deviation (RSD) of the size (bp) of the target DNA was in the range of 1.14%-1.34% and 1.27%- 2.76%, respectively, for CE-LIF, and 1.18%-1.48% and 2.85%-4.06%, respectively, for MCE-LIF. The detection limits was 2.33 x 10(2) copies/mL for CE-LIF and 2.33 x 10(3) copies/mL for MCE-LIF. The two proposed methods were applied to detect fecal samples, both showing high accuracy. The two proposed methods of PCR-CE-LIF and PCR-MCE-LIF can detect adenovirus in fecal samples rapidly, sensitively and specifically.

Zeolites for CO2-CO-O2 Separation to Obtain CO2-Neutral Fuels.

PubMed

Perez-Carbajo, Julio; Matito-Martos, Ismael; Balestra, Salvador R G; Tsampas, Mihalis N; van de Sanden, Mauritius C M; Delgado, José A; Águeda, V Ismael; Merkling, Patrick J; Calero, Sofia

2018-06-20

Carbon dioxide release has become an important global issue due to the significant and continuous rise in atmospheric CO 2 concentrations and the depletion of carbon-based energy resources. Plasmolysis is a very energy-efficient process for reintroducing CO 2 into energy and chemical cycles by converting CO 2 into CO and O 2 utilizing renewable electricity. The bottleneck of the process is that CO remains mixed with O 2 and residual CO 2 . Therefore, efficient gas separation and recuperation are essential for obtaining pure CO, which, via water gas shift and Fischer-Tropsch reactions, can lead to the production of CO 2 -neutral fuels. The idea behind this work is to provide a separation mechanism based on zeolites to optimize the separation of carbon dioxide, carbon monoxide, and oxygen under mild operational conditions. To achieve this goal, we performed a thorough screening of available zeolites based on topology and adsorptive properties using molecular simulation and ideal adsorption solution theory. FAU, BRE, and MTW are identified as suitable topologies for these separation processes. FAU can be used for the separation of carbon dioxide from carbon monoxide and oxygen and BRE or MTW for the separation of carbon monoxide from oxygen. These results are reinforced by pressure swing adsorption simulations at room temperature combining adsorption columns with pure silica FAU zeolite and zeolite BRE at a Si/Al ratio of 3. These zeolites have the added advantage of being commercially available.

Selective extraction and separation of oxymatrine from Sophora flavescens Ait. extract by silica-confined ionic liquid.

PubMed

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

2012-01-01

This study highlighted the application of a two-stepped extraction method for extraction and separation of oxymatrine from Sophora flavescens Ait. extract by utilizing silica-confined ionic liquids as sorbent. The optimized silica-confined ionic liquid was firstly mixed with plant extract to adsorb oxymatrine. Simultaneously, some interference, such as matrine, was removed. The obtained suspension was then added to a cartridge for solid phase extraction. Through these two steps, target compound was adequately separated from interferences with 93.4% recovery. In comparison with traditional solid phase extraction, this method accelerates loading and reduces the use of organic solvents during washing. Moreover, the optimization of loading volume was simplified as optimization of solid/liquid ratio. Copyright © 2011 Elsevier B.V. All rights reserved.

Determination of D-saccharic acid-1,4-lactone from brewed kombucha broth by high-performance capillary electrophoresis.

PubMed

Wang, Kan; Gan, Xuhua; Tang, Xinyun; Wang, Shuo; Tan, Huarong

2010-02-01

Kombucha is a health tonic. D-saccharic acid-1,4-lactone (DSL), a component of kombucha, inhibits the activity of glucuronidase, an enzyme indirectly related with cancers. To date, there is no efficient method to determine the content of DSL in kombucha samples. In this paper, we report a rapid and simple method for the separation and determination of DSL in kombucha samples, using the high-performance capillary electrophoresis (HPCE) method with diode array detection (DAD). With optimized conditions, DSL can be separated in a 50 cm length capillary at a separation voltage of 20 kV in 40 mmol/L borax buffer (pH 6.5) containing 30 mmol/L SDS and 15% methanol (v/v). Quantitative evaluation of DSL was determined by ultraviolet absorption at lambda=190 nm. The relationship between the peak areas and the DSL concentrations, in a specified working range with linear response, was determined by first-order polynomial regression over the range 50-1500 microg/mL with a detection limit of 17.5 microg/mL. Our method demonstrated excellent reproducibility and accuracy with relative standard deviations (RSD) of less than 5% DSL content (n=5). This is the first report to determine DSL by HPCE. We have successfully applied this method to determine DSL in kombucha samples in various fermented conditions. 2009 Elsevier B.V. All rights reserved.

Germination behaviour of annual plants under changing climatic conditions: separating local and regional environmental effects.

PubMed

Petrů, Martina; Tielbörger, Katja

2008-04-01

The role of local adaptation and factors other than climate in determining extinction probabilities of species under climate change has not been yet explicitly studied. Here we performed a field experiment with annual plants growing along a steep climatic gradient in Israel to isolate climatic effects for local trait expression. The focus trait was seed dormancy, for which many theoretical predictions exist regarding climate-driven optimal germination behaviour. We evaluated how germination is consistent with theory, indicating local adaptation to current and changing climatic conditions, and how it varies among species and between natural and standardised soil conditions. We reciprocally sowed seeds from three or four origins for each of three annual species, Biscutella didyma, Bromus fasciculatus and Hymenocarpos circinnatus, in their home and neighbouring sowing locations along an aridity gradient. Our predictions were: lower germination fraction for seeds from more arid origins, and higher germination at wetter sowing locations for all seed origins. By sowing seeds in both local and standard soil, we separated climatic effects from local conditions. At the arid sowing location, two species supported the prediction of low germination of drier seed origins, but differences between seed origins at the other sites were not substantial. There were no clear rainfall effects on germination. Germination fractions were consistently lower on local soil than on standard soil, indicating the important role of soil type and neighbour conditions for trait expression. Local environmental conditions may override effects of climate and so should be carefully addressed in future studies testing for the potential of species to adapt or plastically respond to climate change.

The separation of Gln and Glu in STEAM: a comparison study using short and long TEs/TMs at 3 and 7 T.

PubMed

Dou, Weiqiang; Kaufmann, Jörn; Li, Meng; Zhong, Kai; Walter, Martin; Speck, Oliver

2015-08-01

This study aimed to determine the optimal echo time (TE) and mixing time (TM) for in vivo glutamine (Gln) and glutamate (Glu) separation in stimulated-echo acquisition mode at 3 and 7 T. We applied a short TE/TM (20/10 ms) for a high signal-to-noise-ratio and a field-specific long TE/TM (3 T: 72/6 ms; 7 T: 74/68 ms) for optimal Gln and Glu separation of the Carbon-4 proton resonances. Corresponding Gln and Glu spectra were simulated using VeSPA software, and measured in a phantom and human brains at 3 and 7 T. Higher spectral separation for Gln and Glu was achieved at 7 than 3 T. At 7 T, short TE/TM provided comparable spectral separation and in vitro Gln and Glu quantification compared to long TE/TM. Moreover, it showed greater reliability in in vivo Gln and Glu detection and separation than long TE/TM, with significantly lower Cramer-Rao lower bounds (Gln: 14.9 vs. 75.8; Glu: 3.8 vs. 6.5) and correlation between Gln and Glu (p = 0.004). Based on the optimal separation for Gln and Glu, a short TE/TM at 7 T is proposed for future in vivo Gln and Glu acquisition.

Analysis of flavonoids from lotus (Nelumbo nucifera) leaves using high performance liquid chromatography/photodiode array detector tandem electrospray ionization mass spectrometry and an extraction method optimized by orthogonal design.

PubMed

Chen, Sha; Wu, Ben-Hong; Fang, Jin-Bao; Liu, Yan-Ling; Zhang, Hao-Hao; Fang, Lin-Chuan; Guan, Le; Li, Shao-Hua

2012-03-02

The extraction protocol of flavonoids from lotus (Nelumbo nucifera) leaves was optimized through an orthogonal design. The solvent was the most important factor comparing solvent, solvent:tissue ratio, extraction time, and temperature. The highest yield of flavonoids was achieved with 70% methanol-water and a solvent:tissue ratio of 30:1 at 4 °C for 36 h. The optimized analytical method for HPLC was a multi-step gradient elution using 0.5% formic acid (A) and CH₃CN containing 0.1% formic acid (B), at a flow rate of 0.6 mL/min. Using this optimized method, thirteen flavonoids were simultaneously separated and identified by high performance liquid chromatography coupled with photodiode array detection/electrospray ionization mass spectrometry (HPLC/DAD/ESI-MS(n)). Five of the bioactive compounds are reported in lotus leaves for the first time. The flavonoid content of the leaves of three representative cultivars was assessed under the optimized extraction and HPLC analytical conditions, and the seed-producing cultivar 'Baijianlian' had the highest flavonoid content compared with rhizome-producing 'Zhimahuoulian' and wild floral cultivar 'Honglian'. Copyright © 2012 Elsevier B.V. All rights reserved.

A stochastic optimal feedforward and feedback control methodology for superagility

NASA Technical Reports Server (NTRS)

Halyo, Nesim; Direskeneli, Haldun; Taylor, Deborah B.

1992-01-01

A new control design methodology is developed: Stochastic Optimal Feedforward and Feedback Technology (SOFFT). Traditional design techniques optimize a single cost function (which expresses the design objectives) to obtain both the feedforward and feedback control laws. This approach places conflicting demands on the control law such as fast tracking versus noise atttenuation/disturbance rejection. In the SOFFT approach, two cost functions are defined. The feedforward control law is designed to optimize one cost function, the feedback optimizes the other. By separating the design objectives and decoupling the feedforward and feedback design processes, both objectives can be achieved fully. A new measure of command tracking performance, Z-plots, is also developed. By analyzing these plots at off-nominal conditions, the sensitivity or robustness of the system in tracking commands can be predicted. Z-plots provide an important tool for designing robust control systems. The Variable-Gain SOFFT methodology was used to design a flight control system for the F/A-18 aircraft. It is shown that SOFFT can be used to expand the operating regime and provide greater performance (flying/handling qualities) throughout the extended flight regime. This work was performed under the NASA SBIR program. ICS plans to market the software developed as a new module in its commercial CACSD software package: ACET.

A four parameter optimization and troubleshooting of a RPLC - charged aerosol detection stability indicating method for determination of S-lysophosphatidylcholines in a phospholipid formulation.

PubMed

Tam, James; Ahmad, Imad A Haidar; Blasko, Andrei

2018-06-05

A four parameter optimization of a stability indicating method for non-chromophoric degradation products of 1,2-distearoyl-sn-glycero-3-phosphocholine (DSPC), 1-stearoyl-sn-glycero-3-phosphocholine and 2-stearoyl-sn-glycero-3-phosphocholine was achieved using a reverse phase liquid chromatography-charged aerosol detection (RPLC-CAD) technique. Using the hydrophobic subtraction model of selectivity, a core-shell, polar embedded RPLC column was selected followed by gradient-temperature optimization, resulting in ideal relative peak placements for a robust, stability indicating separation. The CAD instrument parameters, power function value (PFV) and evaporator temperature were optimized for lysophosphatidylcholines to give UV absorbance detector-like linearity performance within a defined concentration range. The two lysophosphatidylcholines gave the same response factor in the selected conditions. System specific power function values needed to be set for the two RPLC-CAD instruments used. A custom flow-divert profile, sending only a portion of the column effluent to the detector, was necessary to mitigate detector response drifting effects. The importance of the PFV optimization for each instrument of identical build and how to overcome recovery issues brought on by the matrix effects from the lipid-RP stationary phase interaction is reported. Copyright © 2018 Elsevier B.V. All rights reserved.

Experimental designs for modeling retention patterns and separation efficiency in analysis of fatty acid methyl esters by gas chromatography-mass spectrometry.

PubMed

Skartland, Liv Kjersti; Mjøs, Svein A; Grung, Bjørn

2011-09-23

The retention behavior of components analyzed by chromatography varies with instrumental settings. Being able to predict how changes in these settings alter the elution pattern is useful, both with regards to component identification, as well as with regards to optimization of the chromatographic system. In this work, it is shown how experimental designs can be used for this purpose. Different experimental designs for response surface modeling of the separation of fatty acid methyl esters (FAME) as function of chromatographic conditions in GC have been evaluated. Full factorial, central composite, Doehlert and Box-Behnken designs were applied. A mixture of 38 FAMEs was separated on a polar cyanopropyl substituted polysilphenylene-siloxane phase capillary column. The temperature gradient, the start temperature of the gradient, and the carrier gas velocity were varied in the experiments. The modeled responses, as functions of chromatographic conditions, were retention time, retention indices, peak widths, separation efficiency and resolution between selected peak pairs. The designs that allowed inclusion of quadratic terms among the predictors performed significantly better than factorial design. Box-Behnken design provided the best results for prediction of retention, but the differences between the central composite, Doehlert and Box-Behnken designs were small. Retention indices could be modeled with much better accuracy than retention times. However, because the errors of predicted tR of closely eluting peaks were highly correlated, models of resolution (Rs) that were based on retention time had errors in the same range as corresponding models based on ECL. Copyright © 2011 Elsevier B.V. All rights reserved.

High-resolution, preparative purification of PEGylated protein using a laterally-fed membrane chromatography device.

PubMed

Madadkar, Pedram; Nino, Sergio Luna; Ghosh, Raja

2016-11-01

We discuss the use of a laterally-fed membrane chromatography (or LFMC) device for single-step purification of mono-PEGylated lysozyme. Recent studies have shown such LFMC devices to be suitable for high-resolution, multi-component separation of proteins in the bind-and-elute mode. The device used in this study contained a stack of rectangular cation-exchange membranes having 9.25mL bed volume. PEGylation of lysozyme was carried out in batch mode using 5kDa methoxy-polyethyleneglycol propionaldehyde (or m-PEG propionaldehyde) in the presence of sodium cyanoborohydride as reducing agent. Membrane chromatographic separation was carried out at 1.62 membrane bed volumes per minute flow rate, in the bind-and-elute mode. When a salt gradient was applied, the higher PEGylated forms of lysozyme (i.e. the byproducts) eluted earlier than mono-PEGylated lysozyme (the target product), while lysozyme eluted last. Under elution conditions optimized for resolution and speed, the separation could be carried out in less than 15 membrane bed volumes. High purity and recovery of mono-PEGylated lysozyme was obtained. The resolution of separation of mono-PEGylated lysozyme obtained under the above condition was comparable to that reported in the literature for equivalent cation-exchange resin columns while the flow rate expressed in bed volumes/min was 21.7 times higher. Also, the number of theoretical plates per meter was significantly higher with the LFMC device. Therefore the LFMC based purification process discussed in this paper combined high-productivity with high-resolution. Copyright © 2016 Elsevier B.V. All rights reserved.

Optimal glottal configuration for ease of phonation.

PubMed

Lucero, J C

1998-06-01

Recent experimental studies have shown the existence of optimal values of the glottal width and convergence angle, at which the phonation threshold pressure is minimum. These results indicate the existence of an optimal glottal configuration for ease of phonation, not predicted by the previous theory. In this paper, the origin of the optimal configuration is investigated using a low dimensional mathematical model of the vocal fold. Two phenomena of glottal aerodynamics are examined: pressure losses due to air viscosity, and air flow separation from a divergent glottis. The optimal glottal configuration seems to be a consequence of the combined effect of both factors. The results agree with the experimental data, showing that the phonation threshold pressure is minimum when the vocal folds are slightly separated in a near rectangular glottis.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cullen, David A; Koestner, Roland; Kukreja, Ratan

Improved conditions for imaging and spectroscopic mapping of thin perfluorosulfonic acid (PFSA) ionomer layers in fuel cell electrodes by scanning transmission electron microscopy (STEM) have been investigated. These conditions are first identified on model systems of Nafion ionomer-coated nanostructured thin films and nanoporous Si. The optimized conditions are then applied in a quantitative study of the ionomer through-layer loading for two typical electrode catalyst coatings using electron energy loss and energy dispersive X-ray spectroscopy in the transmission electron microscope. The e-beam induced damage to the perfluorosulfonic acid (PFSA) ionomer is quantified by following the fluorine mass loss with electron exposuremore » and is then mitigated by a few orders of magnitude using cryogenic specimen cooling and a higher incident electron voltage. Multivariate statistical analysis is also applied to the analysis of spectrum images for data denoising and unbiased separation of independent components related to the catalyst, ionomer, and support.« less

Proton transport in functionalised additives for PEM fuel cells: contributions from atomistic simulations.

PubMed

Tölle, Pia; Köhler, Christof; Marschall, Roland; Sharifi, Monir; Wark, Michael; Frauenheim, Thomas

2012-08-07

The conventional polymer electrolyte membrane (PEM) materials for fuel cell applications strongly rely on temperature and pressure conditions for optimal performance. In order to expand the range of operating conditions of these conventional PEM materials, mesoporous functionalised SiO(2) additives are developed. It has been demonstrated that these additives themselves achieve proton conductivities approaching those of conventional materials. However, the proton conduction mechanisms and especially factors influencing charge carrier mobility under different hydration conditions are not well known and difficult to separate from concentration effects in experiments. This tutorial review highlights contributions of atomistic computer simulations to the basic understanding and eventual design of these materials. Some basic introduction to the theoretical and computational framework is provided to introduce the reader to the field, the techniques are in principle applicable to a wide range of other situations as well. Simulation results are directly compared to experimental data as far as possible.

Ion-conducting ceramic apparatus, method, fabrication, and applications

DOEpatents

Yates, Matthew [Penfield, NY; Liu, Dongxia [Rochester, NY

2012-03-06

A c-axis-oriented HAP thin film synthesized by seeded growth on a palladium hydrogen membrane substrate. An exemplary synthetic process includes electrochemical seeding on the substrate, and secondary and tertiary hydrothermal treatments under conditions that favor growth along c-axes and a-axes in sequence. By adjusting corresponding synthetic conditions, an HAP this film can be grown to a controllable thickness with a dense coverage on the underlying substrate. The thin films have relatively high proton conductivity under hydrogen atmosphere and high temperature conditions. The c-axis oriented films may be integrated into fuel cells for application in the intermediate temperature range of 200-600.degree. C. The electrochemical-hydrothermal deposition technique may be applied to create other oriented crystal materials having optimized properties, useful for separations and catalysis as well as electronic and electrochemical applications, electrochemical membrane reactors, and in chemical sensors.

Shock unsteadiness in a thrust optimized parabolic nozzle

NASA Astrophysics Data System (ADS)

Verma, S. B.

2009-07-01

This paper discusses the nature of shock unsteadiness, in an overexpanded thrust optimized parabolic nozzle, prevalent in various flow separation modes experienced during start up {(δ P0 /δ t > 0)} and shut down {(δ P0/δ t < 0)} sequences. The results are based on simultaneously acquired data from real-time wall pressure measurements using Kulite pressure transducers, high-speed schlieren (2 kHz) of the exhaust flow-field and from strain-gauges installed on the nozzle bending tube. Shock unsteadiness in the separation region is seen to increase significantly just before the onset of each flow transition, even during steady nozzle operation. The intensity of this measure ( rms level) is seen to be strongly influenced by relative locations of normal and overexpansion shock, the decrease in radial size of re-circulation zone in the back-flow region, and finally, the local nozzle wall contour. During restricted shock separation, the pressure fluctuations in separation region exhibit periodic characteristics rather than the usually observed characteristics of intermittent separation. The possible physical mechanisms responsible for the generation of flow unsteadiness in various separation modes are discussed. The results are from an experimental study conducted in P6.2 cold-gas subscale test facility using a thrust optimized parabolic nozzle of area-ratio 30.

Optimization of porous microchannel heat exchanger

NASA Astrophysics Data System (ADS)

Kozhukhov, N. N.; Konovalov, D. A.

2017-11-01

The technical progress in information and communication sphere leads to a sharp increase in the use of radio electronic devices. Functioning of radio electronics is accompanied by release of thermal energy, which must be diverted from the heat-stressed element. Moreover, using of electronics at negative temperatures, on the contrary, requires supply of a certain amount of heat to start the system. There arises the task of creating a system that allows both to supply and to divert the necessary amount of thermal energy. The development of complex thermostabilization systems for radio electronic equipment is due to increasing the efficiency of each of its elements separately. For more efficient operation of a heat exchanger, which directly affects the temperature of the heat-stressed element, it is necessary to calculate the mode characteristics and to take into account the effect of its design parameters. The results of optimizing the microchannel heat exchanger are presented in the article. The target optimization functions are the mass, pressure drop and temperature. The parameters of optimization are the layout of porous fins, their geometric dimensions and coolant flow. For the given conditions, the optimum variant of porous microchannel heat exchanger is selected.

Multi-objective optimization for an automated and simultaneous phase and baseline correction of NMR spectral data

NASA Astrophysics Data System (ADS)

Sawall, Mathias; von Harbou, Erik; Moog, Annekathrin; Behrens, Richard; Schröder, Henning; Simoneau, Joël; Steimers, Ellen; Neymeyr, Klaus

2018-04-01

Spectral data preprocessing is an integral and sometimes inevitable part of chemometric analyses. For Nuclear Magnetic Resonance (NMR) spectra a possible first preprocessing step is a phase correction which is applied to the Fourier transformed free induction decay (FID) signal. This preprocessing step can be followed by a separate baseline correction step. Especially if series of high-resolution spectra are considered, then automated and computationally fast preprocessing routines are desirable. A new method is suggested that applies the phase and the baseline corrections simultaneously in an automated form without manual input, which distinguishes this work from other approaches. The underlying multi-objective optimization or Pareto optimization provides improved results compared to consecutively applied correction steps. The optimization process uses an objective function which applies strong penalty constraints and weaker regularization conditions. The new method includes an approach for the detection of zero baseline regions. The baseline correction uses a modified Whittaker smoother. The functionality of the new method is demonstrated for experimental NMR spectra. The results are verified against gravimetric data. The method is compared to alternative preprocessing tools. Additionally, the simultaneous correction method is compared to a consecutive application of the two correction steps.

Synthetic oligonucleotide separations by mixed-mode reversed-phase/weak anion-exchange liquid chromatography.

PubMed

Zimmermann, Aleksandra; Greco, Roberto; Walker, Isabel; Horak, Jeannie; Cavazzini, Alberto; Lämmerhofer, Michael

2014-08-08

Synthetic oligonucleotides gain increasing importance in new therapeutic concepts and as probes in biological sciences. If pharmaceutical-grade purities are required, chromatographic purification using ion-pair reversed-phase chromatography is commonly carried out. However, separation selectivity for structurally closely related impurities is often insufficient, especially at high sample loads. In this study, a "mixed-mode" reversed-phase/weak anion exchanger stationary phase has been investigated as an alternative tool for chromatographic separation of synthetic oligonucleotides with minor sequence variations. The employed mixed-mode phase shows great flexibility in method development. It has been run in various gradient elution modes, viz. one, two or three parameter (mixed) gradients (altering buffer pH, buffer concentration, and organic modifier) to find optimal elution conditions and gain further insight into retention mechanisms. Compared to ion-pair reversed-phase and mere anion-exchange separation, enhanced selectivities were observed with the mixed-mode phase for 20-23 nucleotide (nt) long oligonucleotides with similar sequences. Oligonucleotides differing by 1, 2 or 3 nucleotides in length could be readily resolved and separation factors for single nucleotide replacements declined in the order Cytosine (C)/Guanine (G)>Adenine (A)/Guanine∼Guanine/Thymine (T)>Adenine/Cytosine∼Cytosine/Thymine>Adenine/Thymine. Selectivities were larger when the modification was at the 3' terminal-end, declined when it was in the middle of the sequence and was smallest when it was located at the 5' terminus. Due to the lower surface area of the 200Å pore size mixed-mode stationary phase compared to the corresponding 100Å material, lower retention times with equal selectivities under milder elution conditions were achievable. Considering high sample loading capacities of the mixed-mode anion-exchanger phase, it should have great potential for chromatographic oligonucleotide separation and purification. Copyright © 2014 Elsevier B.V. All rights reserved.

Inactivation of Aerosolized Biological Agents using Filled Nanocomposite Materials

DTIC Science & Technology

2013-02-01

developed and optimized. The dry -heat inactivation of aerosolized spores was quantified separately from chemical effects and linked to DNA repair...Bacillus spores exposed to dry heat 67 - 79 Chapter 5. Mechanically alloyed Al-I composite materials 80 - 98 Chapter 6. Iodine release...and optimized. The dry -heat inactivation of aerosolized spores was quantified separately from chemical effects and linked to DNA repair mechanisms

Optimization of capillary zone electrophoresis for charge heterogeneity testing of biopharmaceuticals using enhanced method development principles.

PubMed

Moritz, Bernd; Locatelli, Valentina; Niess, Michele; Bathke, Andrea; Kiessig, Steffen; Entler, Barbara; Finkler, Christof; Wegele, Harald; Stracke, Jan

2017-12-01

CZE is a well-established technique for charge heterogeneity testing of biopharmaceuticals. It is based on the differences between the ratios of net charge and hydrodynamic radius. In an extensive intercompany study, it was recently shown that CZE is very robust and can be easily implemented in labs that did not perform it before. However, individual characteristics of some examined proteins resulted in suboptimal resolution. Therefore, enhanced method development principles were applied here to investigate possibilities for further method optimization. For this purpose, a high number of different method parameters was evaluated with the aim to improve CZE separation. For the relevant parameters, design of experiments (DoE) models were generated and optimized in several ways for different sets of responses like resolution, peak width and number of peaks. In spite of product specific DoE optimization it was found that the resulting combination of optimized parameters did result in significant improvement of separation for 13 out of 16 different antibodies and other molecule formats. These results clearly demonstrate generic applicability of the optimized CZE method. Adaptation to individual molecular properties may sometimes still be required in order to achieve optimal separation but the set screws discussed in this study [mainly pH, identity of the polymer additive (HPC versus HPMC) and the concentrations of additives like acetonitrile, butanolamine and TETA] are expected to significantly reduce the effort for specific optimization. 2017 The Authors. Electrophoresis published by Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Selective enrichment in bioactive compound from Kniphofia uvaria by super/subcritical fluid extraction and centrifugal partition chromatography.

PubMed

Duval, Johanna; Destandau, Emilie; Pecher, Virginie; Poujol, Marion; Tranchant, Jean-François; Lesellier, Eric

2016-05-20

Nowadays, a large portion of synthetic products (active cosmetic and therapeutic ingredients) have their origin in natural products. Kniphofia uvaria is a plant from Africa which has proved in the past by in-vivo tests an antioxidant activity due to compounds present in roots. Recently, we have observed anthraquinones in K. uvaria seeds extracts. These derivatives are natural colorants which could have interesting bioactive potential. The aim of this study was to obtain an extract enriched in anthraquinones from K. uvaria seeds which mainly contains glycerides. First, the separation of the seed compounds was studied by using supercritical fluid chromatography (SFC) in the goal to provide a rapid quantification method of these bioactive compounds. A screening of numerous polar stationary phases was achieved for selecting the most suited phase to the separation of the four anthraquinones founded in the seeds. A gradient elution was optimized for improving the separation of the bioactive compounds from the numerous other families of major compounds of the extracts (fatty acids, di- and triglycerides). Besides, a non-selective and green Supercritical Fluid Extraction (SFE) with pure CO2 was applied to seeds followed by a Centrifugal Partition Chromatography (CPC). The CPC system was optimized by using the Arizona phase system, to enrich the extract in anthraquinones. Two systems were selected to isolate the bioactive compounds from the oily extract with varied purity target. The effect of the injection mode for these very viscous samples was also studied. Finally, in order to directly apply a selective process of extraction to the seeds, the super/subcritical fluid extraction was optimized to increase the anthraquinone yield in the final extract, by studying varied modifier compositions and nature, as well as different temperatures and backpressures. Conditions suited to favour an enrichment factor bases on the ratio of anthraquinone and trilycerides extracted are described. Copyright © 2016 Elsevier B.V. All rights reserved.

Microchannel gel electrophoretic separation systems and methods for preparing and using

DOEpatents

Herr, Amy E; Singh, Anup K; Throckmorton, Daniel J

2015-02-24

A micro-analytical platform for performing electrophoresis-based immunoassays was developed by integrating photopolymerized cross-linked polyacrylamide gels within a microfluidic device. The microfluidic immunoassays are performed by gel electrophoretic separation and quantifying analyte concentration based upon conventional polyacrylamide gel electrophoresis (PAGE). To retain biological activity of proteins and maintain intact immune complexes, native PAGE conditions were employed. Both direct (non-competitive) and competitive immunoassay formats are demonstrated in microchips for detecting toxins and biomarkers (cytokines, c-reactive protein) in bodily fluids (serum, saliva, oral fluids). Further, a description of gradient gels fabrication is included, in an effort to describe methods we have developed for further optimization of on-chip PAGE immunoassays. The described chip-based PAGE immunoassay method enables immunoassays that are fast (minutes) and require very small amounts of sample (less than a few microliters). Use of microfabricated chips as a platform enables integration, parallel assays, automation and development of portable devices.

Playing in parallel: the effects of multiplayer modes in active video game on motivation and physical exertion.

PubMed

Peng, Wei; Crouse, Julia

2013-06-01

Although multiplayer modes are common among contemporary video games, the bulk of game research focuses on the single-player mode. To fill the gap in the literature, the current study investigated the effects of different multiplayer modes on enjoyment, future play motivation, and the actual physical activity intensity in an active video game. One hundred sixty-two participants participated in a one-factor between-subject laboratory experiment with three conditions: (a) single player: play against self pretest score; (b) cooperation with another player in the same physical space; (c) parallel competition with another player in separated physical spaces. We found that parallel competition in separate physical spaces was the optimal mode, since it resulted in both high enjoyment and future play motivation and high physical intensity. Implications for future research on multiplayer mode and play space as well as active video game-based physical activity interventions are discussed.

Task-specific ionic liquid-assisted extraction and separation of astaxanthin from shrimp waste.

PubMed

Bi, Wentao; Tian, Minglei; Zhou, Jun; Row, Kyung Ho

2010-08-15

Astaxanthin, as an outstanding antioxidant reagent, was successfully extracted from shrimp waste by the ionic liquids based ultrasonic-assisted extraction. Seven kinds of imidazolium ionic liquids with different cations and anions were investigated in this work and one task-specific ionic liquid in ethanol with 0.50molL(-1) was selected as the solvent. At the optimized ultrasonic extraction conditions, the extraction amount of astaxanthin increased 98% (92.7microg g(-1)) compared to the conventional method (46.7microg g(-1)). Furthermore, the extracted solution was isolated through the solid-phase extraction with a molecularly imprinted polymer sorbent. After loading the samples on molecularly imprinted polymer cartridge, the different washing and elution solvents, such as water, methanol, n-hexane, acetone and dichloromethane, were evaluated, and finally, astaxanthin was separated from the shrimp waste extract. Copyright 2010 Elsevier B.V. All rights reserved.

Microchannel gel electrophoretic separation systems and methods for preparing and using

DOEpatents

Herr, Amy; Singh, Anup K; Throckmorton, Daniel J

2013-09-03

A micro-analytical platform for performing electrophoresis-based immunoassays was developed by integrating photopolymerized cross-linked polyacrylamide gels within a microfluidic device. The microfluidic immunoassays are performed by gel electrophoretic separation and quantifying analyte concentration based upon conventional polyacrylamide gel electrophoresis (PAGE). To retain biological activity of proteins and maintain intact immune complexes, native PAGE conditions were employed. Both direct (non-competitive) and competitive immunoassay formats are demonstrated in microchips for detecting toxins and biomarkers (cytokines, c-reactive protein) in bodily fluids (serum, saliva, oral fluids). Further, a description of gradient gels fabrication is included, in an effort to describe methods we have developed for further optimization of on-chip PAGE immunoassays. The described chip-based PAGE immunoassay method enables immunoassays that are fast (minutes) and require very small amounts of sample (less than a few microliters). Use of microfabricated chips as a platform enables integration, parallel assays, automation and development of portable devices.

Validation of an HPLC method for the quantification of ambroxol hydrochloride and benzoic acid in a syrup as pharmaceutical form stress test for stability evaluation.

PubMed

Heinänen, M; Barbas, C

2001-03-01

A method is described for ambroxol, trans-4-(2-amino-3,5-dibromobenzylamino) cyclohexanol hydrochloride, and benzoic acid separation by HPLC with UV detection at 247 nm in a syrup as pharmaceutical presentation. Optimal conditions were: Column Symmetry Shield RPC8, 5 microm 250 x 4.6 mm, and methanol/(H(3)PO(4) 8.5 mM/triethylamine pH=2.8) 40:60 v/v. Validation was performed using standards and the pharmaceutical preparation which contains the compounds described above. Results from both standards and samples show suitable validation parameters. The pharmaceutical grade substances were tested by factors that could influence the chemical stability. These reaction mixtures were analysed to evaluate the capability of the method to separate degradation products. Degradation products did not interfere with the determination of the substances tested by the assay.

Fast analysis of domoic acid using microchip electrophoresis with laser-induced fluorescence detection.

PubMed

Cheng, Yongqiang; Guo, Cuilian; Zhao, Bin; Yang, Li

2017-04-01

A fast and effective method was developed to detect domoic acid based upon microchip electrophoresis combined with laser-induced fluorescence detection. Through study of the gated injection process on the cross channel of the microchip, the low-voltage mode with relatively longer sample loading time was adopted to reduce the sample discrimination and improve the signal sensitivity. Fluorescein isothiocyanate was used as the derivatizing reagent for domoic acid. Under the optimized conditions, domoic acid was completely separated in 60 s with separation efficiency of 1.35 × 10 5  m -1 . The calibration curve was obtained in the range of 1.0 × 10 -9 to 1.0 × 10 -7  mol/L, and the detection limit reached 2.8 × 10 -10  mol/L. This developed method was successfully applied to analyze domoic acid in real samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Cloud point extraction thermospray flame quartz furnace atomic absorption spectrometry for determination of ultratrace cadmium in water and urine

NASA Astrophysics Data System (ADS)

Wu, Peng; Zhang, Yunchang; Lv, Yi; Hou, Xiandeng

2006-12-01

A simple, low cost and highly sensitive method based on cloud point extraction (CPE) for separation/preconcentration and thermospray flame quartz furnace atomic absorption spectrometry was proposed for the determination of ultratrace cadmium in water and urine samples. The analytical procedure involved the formation of analyte-entrapped surfactant micelles by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution and a Triton X-114 solution. When the temperature of the system was higher than the cloud point of Triton X-114, the complex of cadmium-PDC entered the surfactant-rich phase and thus separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, the limit of detection was 0.04 μg/L for cadmium with a sample volume of 10 mL. The analytical results of cadmium in water and urine samples agreed well with those by ICP-MS.

Remote NMR/MRI detection of laser polarized gases

DOEpatents

Pines, Alexander; Saxena, Sunil; Moule, Adam; Spence, Megan; Seeley, Juliette A.; Pierce, Kimberly L.; Han, Song-I; Granwehr, Josef

2006-06-13

An apparatus and method for remote NMR/MRI spectroscopy having an encoding coil with a sample chamber, a supply of signal carriers, preferably hyperpolarized xenon and a detector allowing the spatial and temporal separation of signal preparation and signal detection steps. This separation allows the physical conditions and methods of the encoding and detection steps to be optimized independently. The encoding of the carrier molecules may take place in a high or a low magnetic field and conventional NMR pulse sequences can be split between encoding and detection steps. In one embodiment, the detector is a high magnetic field NMR apparatus. In another embodiment, the detector is a superconducting quantum interference device. A further embodiment uses optical detection of Rb--Xe spin exchange. Another embodiment uses an optical magnetometer using non-linear Faraday rotation. Concentration of the signal carriers in the detector can greatly improve the signal to noise ratio.

Design of a Fission 99 Mo Recovery Process and Implications toward Mo Adsorption Mechanism on Titania and Alumina Sorbents

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stepinski, Dominique C.; Youker, Amanda J.; Krahn, Elizabeth O.

2017-03-01

Molybdenum-99 is a parent of the most widely used medical isotope technetium-99m. Proliferation concerns have prompted development of alternative Mo production methods utilizing low enriched uranium. Alumina and titania sorbents were evaluated for separation of Mo from concentrated uranyl nitrate solutions. System, mass transfer, and isotherm parameters were determined to enable design of Mo separation processes under a wide range of conditions. A model-based approach was utilized to design representative commercial-scale column processes. The designs and parameters were verified with bench-scale experiments. The results are essential for design of Mo separation processes from irradiated uranium solutions, selection of support materialmore » and process optimization. Mo uptake studies show that adsorption decreases with increasing concentration of uranyl nitrate; howeveL, examination of Mo adsorption as a function of nitrate ion concentration shows no dependency, indicating that uranium competes with Mo for adsorption sites. These results are consistent with reports indicating that Mo forms inner-sphere complexes with titania and alumina surface groups.« less

Separation of delta-, gamma- and alpha-tocopherols by CEC.

PubMed

Fanali, Salvatore; Catarcini, Paolo; Quaglia, Maria Giovanna; Camera, Emanuela; Rinaldi, Mariarosa; Picardo, Mauro

2002-08-01

In this study capillary electrochromatography (CEC) was used for the separation of three tocopherols (TOHs), namely delta-, gamma- and alpha-TOH and the antioxidant compound, butylated hydroxytoluene (BHT). The CEC experiments were carried out using an octadecylsilica (ODS) stationary phase packed, in our laboratory, in a fused-silica capillary (100 microm I.D., 365 microm O.D. x 33 cm of total length and 24.6 or 8.4 cm effective length). The mobile phase was composed by a mixture of methanol (MeOH) and acetonitrile (ACN), at different concentrations and 0.01% (w/v) of ammonium acetate. Retention time (t(R)), retention factor (k), resolution (R(s)) of the three TOHs were strongly influenced by the organic solvent composition of the run buffer and by the effective length of the capillary. Optimum experimental conditions were found even employing the short effective length of the capillary achieving the baseline separation of the studied analytes in a relatively short time (less than 5 min). The optimized method was applied to the qualitative analysis of vitamin E (alpha-TOH) present in a human serum extract.

Preparative separation of grape skin polyphenols by high-speed counter-current chromatography.

PubMed

Luo, Lanxin; Cui, Yan; Zhang, Shuting; Li, Lingxi; Li, Yuanyuan; Zhou, Peiyu; Sun, Baoshan

2016-12-01

To develop an efficient method for large preparation of various individual polyphenols from white grape skins (Fernão Pires; Vitis vinifera) by preparative high-speed counter-current chromatography (HSCCC) and preparative-HPLC, an optimized preparative HSCCC condition with two-phase solvent system composed of Hex-EtOAc-H2O (1:50:50, v/v) was used to separate grape skin polyphenols into various fractions. Both the tail-head and head-tail elution modes were used with a flow rate of 3.0ml/min and a rotary speed of 950rpm. Afterwards, a preparative-HPLC separation was applied to isolate individual polyphenols in each of the fractions from HSCCC. Total of 7 fractions (Fraction A to G) were obtained from grape skin extract by HSCCC. After preparative-HPLC isolation, fifteen individual compounds were obtained, most of which presented high yields and purity (all over 90%). The HSCCC method followed with preparative-HPLC appeared to be convenient and economical, constituting an efficient strategy for the isolation of grape skin polyphenols. Copyright © 2016 Elsevier Ltd. All rights reserved.

Use of a polystyrene-divinylbenzene-based weakly acidic cation-exchange resin column and propionic acid as an eluent in ion-exclusion/adsorption chromatography of aliphatic carboxylic acids and ethanol in food samples.

PubMed

Mori, Masanobu; Hironaga, Takahiro; Kajiwara, Hiroe; Nakatani, Nobutake; Kozaki, Daisuke; Itabashi, Hideyuki; Tanaka, Kazuhiko

2011-01-01

We developed an ion-exclusion/adsorption chromatography (IEAC) method employing a polystyrene-divinylbenzene-based weakly acidic cation-exchange resin (PS-WCX) column with propionic acid as the eluent for the simultaneous determination of multivalent aliphatic carboxylic acids and ethanol in food samples. The PS-WCX column well resolved mono-, di-, and trivalent carboxylic acids in the acidic eluent. Propionic acid as the eluent gave a higher signal-to-noise ratio, and enabled sensitive conductimetric detection of analyte acids. We found the optimal separation condition to be the combination of a PS-WCX column and 20-mM propionic acid. Practical applicability of the developed method was confirmed by using a short precolumn with a strongly acidic cation-exchange resin in the H(+)-form connected before the separation column; this was to remove cations from food samples by converting them to hydrogen ions. Consequently, common carboxylic acids and ethanol in beer, wine, and soy sauce were successfully separated by the developed method.

Pitch-informed solo and accompaniment separation towards its use in music education applications

NASA Astrophysics Data System (ADS)

Cano, Estefanía; Schuller, Gerald; Dittmar, Christian

2014-12-01

We present a system for the automatic separation of solo instruments and music accompaniment in polyphonic music recordings. Our approach is based on a pitch detection front-end and a tone-based spectral estimation. We assess the plausibility of using sound separation technologies to create practice material in a music education context. To better understand the sound separation quality requirements in music education, a listening test was conducted to determine the most perceptually relevant signal distortions that need to be improved. Results from the listening test show that solo and accompaniment tracks pose different quality requirements and should be optimized differently. We propose and evaluate algorithm modifications to better understand their effects on objective perceptual quality measures. Finally, we outline possible ways of optimizing our separation approach to better suit the requirements of music education applications.

Separation, concentration and determination of trace chloramphenicol in shrimp from different waters by using polyoxyethylene lauryl ether-salt aqueous two-phase system coupled with high-performance liquid chromatography.

PubMed

Lu, Yang; Yao, Hui; Li, Chuang; Han, Juan; Tan, Zhenjiang; Yan, Yongsheng

2016-02-01

Polyoxyethylene lauryl ether (POELE10)-NaH2PO4 aqueous two-phase extraction system (ATPES) is coupled with HPLC to analyze chloramphenicol (CAP) in aquatic product. Response surface methodology (RSM) was adopted in the multi-factor experiment to determine the optimized conditions. The extraction efficiency of CAP (E%) is up to 99.42% under the optimal conditions, namely, the concentration of NaH2PO4, the concentration of POELE10, pH and temperature were 0.186 g · mL(-1), 0.033 g · mL(-1), 3.8 and 25 °C respectively. The optimal value of enrichment factor of CAP (F) was 22.56 when the concentration of NaH2PO4 was 0.192 g · mL(-1), the concentration of POELE10 was 0.024 g/ml, pH was 4.2 and temperature was 30 °C. The limit of detection (LOD) and limit of quantification (LOQ) of this method are 0.8 μg · kg(-1) and 1 μg · kg(-1), which meet the needs of determining trace or ultratrace CAP in food. The E% and F of this technique are much better than other extraction methods. Copyright © 2015 Elsevier Ltd. All rights reserved.

Camptothecine production by mixed fermentation of two endophytic fungi from Nothapodytes nimmoniana.

PubMed

Bhalkar, Bhumika N; Patil, Swapnil M; Govindwar, Sanjay P

2016-01-01

Two endophytic fungi isolated from the endangered plant Nothapodytes nimmoniana (Grah.) Mabb. were found to effectively synthesize CPT independent of their host plant under submerged fermentation conditions. Molecular characterization of fungi revealed their identity as Colletotrichum fructicola SUK1 (F1) and Corynespora cassiicola SUK2 (F2). Mixed fermentation experiments were carried out to study the effect of microbial signalling between the two fungal species on camptothecine production. Effect of culture parameters on CPT production was studied for both mono-cultures (F1 and F2) separately as well as for the mixed fermentation (F1 + F2). Further the most influencing ones were optimized statistically using response surface methodology. Statistical model based optimized parameters were whey (70 %), agitation rate (110 rpm), temperature (30 °C), and incubation period (7 d) for the mixed fermentation. Monocultures of the two fungal species F1 and F2 yielded CPT up to 33 ± 1.1 mg l(-1)and 69 ± 1.1 mg l(-1), respectively; while their mixed fermentation under the optimized conditions yielded up to 146 ± 0.2 mg l(-1). HPLC and LC-MS/MS techniques were used to analyze the products obtained. Copyright © 2016 British Mycological Society. Published by Elsevier Ltd. All rights reserved.

Study on the synthesis and physicochemical properties of starch acetate with low substitution under microwave assistance.

PubMed

Lin, Derong; Zhou, Wei; Zhao, Jingjing; Lan, Weijie; Chen, Rongming; Li, Yutong; Xing, Baoshan; Li, Zhuohao; Xiao, Mengshi; Wu, Zhijun; Li, Xindan; Chen, Rongna; Zhang, Xingwen; Chen, Hong; Zhang, Qing; Qin, Wen; Li, Suqing

2017-10-01

In this study, synthesis and physicochemical properties of starch acetate with low substitution under microwave were studied. A three-level-three-factorial Central Composite Design using Response Surface Methodology (RSM) was employed to optimize the reaction conditions. The optimal parameters are as follows: amount of acetic anhydride of 12%, radiation time of 11min, and microwave power of 100W. These optimal conditions predicted by RSM were confirmed that the degree of substitution (DS) of acetate starch is 0.0691mg/g and the physical and chemical properties of natural corn starch (NCS) and corn starch acetate (ACS) were further studied.The transparency, water separation, water absorption, expansion force, and solubility of ACS low substitution are better than NCS, while the NCS's hydrolysis percentage is higher than ACS, which indicate that the modified corn starch has better performance than native corn starch. The surface morphology of the corn starch acetate was examined by scanning electron microscope (SEM), which showed that it had a smooth surface and a spherical and polygonal shape. However, samples' shape is irregular. Crystal structure was observed by X-ray diffraction, and the ACS can determine the level of microwave technology that can destroy the extent of the crystal and amorphous regions. Fourier transform infrared (FTIR) spectroscopy shows that around 1750cm -1 carbonyl signal determines acetylation bonding successfully. Copyright © 2017 Elsevier B.V. All rights reserved.

Theory of microemulsions in a gravitational field

NASA Technical Reports Server (NTRS)

Jeng, J. F.; Miller, Clarence A.

1989-01-01

A theory of microemulsions developed previously is extended to include the effect of a gravitational field. It predicts variation with position of drop size, drop volume fraction, and area per molecule in the surfactant films within a microemulsion phase. Variation in volume fraction is greatest and occurs in such a way that oil content increases with increasing elevation, as has been found experimentally. Large composition variations are predicted within a middle phase microemulsion near optimal conditions because inversion from the water-continuous to the oil-continuous arrangement occurs with increasing elevation. Generally speaking, gravity reduces solubilization within microemulsions and promotes separation of excess phases.

Development of MMC Gamma Detectors for Nuclear Analysis

NASA Astrophysics Data System (ADS)

Bates, C. R.; Pies, C.; Kempf, S.; Gastaldo, L.; Fleischmann, A.; Enss, C.; Friedrich, S.

2014-09-01

Non-destructive assay (NDA) of nuclear materials would benefit from gamma detectors with improved energy resolution in cases where line overlap in current Ge detectors limits NDA accuracy. We are developing metallic magnetic calorimeter gamma-detectors for this purpose by electroplating 150 m thick Au absorbers into microfabricated molds on top of Au:Er sensors. Initial tests under non-optimized conditions show an energy resolution of 200 eV FWHM at 60 keV. Monte Carlo simulations illustrate that this resolution is starting to be sufficient for direct detection of Pu in plutonium separated from spent nuclear fuel.

Optimization of ultra-high pressure liquid chromatography - tandem mass spectrometry determination in plasma and red blood cells of four sphingolipids and their evaluation as biomarker candidates of Gaucher's disease.

PubMed

Chipeaux, Caroline; de Person, Marine; Burguet, Nathalie; Billette de Villemeur, Thierry; Rose, Christian; Belmatoug, Nadia; Héron, Sylvie; Le Van Kim, Caroline; Franco, Mélanie; Moussa, Fathi

2017-11-24

While important advances have been recently achieved in the optimization of lipid classes' separation, information on the specific determination of medium polarity lipids such as sphingolipids (SLs) in highly complex matrices remains fragmentary. In human, disorders of SL metabolism known as sphingolipidoses are a heterogeneous group of inherited disorders affecting primarily the central nervous. Early diagnosis of these conditions is of importance notably when a corrective therapy is available. The diagnosis is generally based on the determination of specific SLs in plasma and red blood cells (RBCs). For instance, glucosylceramide (GL1), glucosylsphingosine (Lyso-GL1), sphingosine (Sph), and sphingosine-1-phosphate (S1P) are proposed as relevant biomarkers for Gaucher disease (GD). Our main objective was to evaluate these biomarker candidates in a cohort of GD patients. However, most of current methods of GL1, Lyso-GL1, Sph, and S1P determination in plasma of GD patients require at least two liquid chromatographic runs. On the other hand, except for GL1 nothing is known concerning the RBC sphingolipid content. Yet, several reversed phase LC-MS methods of SLs separation and/or determination in various media with different sample preparation approaches have been proposed since 2010. Here we focused on stationary phase selection and mobile phase composition as well as on the sample preparation step to optimize and validate an UHPLC-MS/MS method for the simultaneous quantification of the four sphingolipids in both plasma and RBCs. A comparison between seven stationary phases including two RP18, two polar embedded RP18, and three HILIC phases shows that under our conditions polar embedded RP18 phases are the most appropriate for the separation of the four SLs, in terms of efficiency, peak symmetry, and separation time. In the same way, a comparison between a single step extraction with methanol and a liquid-liquid extraction with a mixture of methanol/methyl tert-butyl ether, shows that the latter mixture is the most appropriate for the extraction of SLs in terms of recovery and absence of matrix effect. After validation, this method was applied to the evaluation of the targeted SLs in a cohort of 15 known GD patients. The obtained results show that Lyso-GL1 is the only relevant biomarker in both plasma and RBCs for GD diagnosis. As the proposed method is applicable to the determination in such a highly complex matrices of four SLs with a large difference in polarity, and as the sample preparation procedure is freedom of matrix effects, this method can be easily adapted to a large diversity of samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Voltage sweep ion mobility spectrometry.

PubMed

Davis, Eric J; Williams, Michael D; Siems, William F; Hill, Herbert H

2011-02-15

Ion mobility spectrometry (IMS) is a rapid, gas-phase separation technique that exhibits excellent separation of ions as a standalone instrument. However, IMS cannot achieve optimal separation power with both small and large ions simultaneously. Similar to the general elution problem in chromatography, fast ions are well resolved using a low electric field (50-150 V/cm), whereas slow drifting molecules are best separated using a higher electric field (250-500 V/cm). While using a low electric field, IMS systems tend to suffer from low ion transmission and low signal-to-noise ratios. Through the use a novel voltage algorithm, some of these effects can be alleviated. The electric field was swept from low to high while monitoring a specific drift time, and the resulting data were processed to create a 'voltage-sweep' spectrum. If an optimal drift time is calculated for each voltage and scanned simultaneously, a spectrum may be obtained with optimal separation throughout the mobility range. This increased the resolving power up to the theoretical maximum for every peak in the spectrum and extended the peak capacity of the IMS system, while maintaining accurate drift time measurements. These advantages may be extended to any IMS, requiring only a change in software.

Design and simulation of 532nm Rayleigh-Mie Doppler wind Lidar system

NASA Astrophysics Data System (ADS)

Peng, Zhuang; Xie, Chenbo; Wang, Bangxin; Shen, Fahua; Tan, Min; Li, Lu; Zhang, Zhanye

2018-02-01

Wind is one of the most significant parameter in weather forecast and the research of climate.It is essential for the weather forecast seasonally to yearly ,atmospheric dynamics,study of thermodynamics and go into the water, chemistry and aerosol which are have to do with global climate statusto measure three-dimensional troposphericwind field accurately.Structure of the doppler wind lidar system which based on Fabry-Perot etalon is introduced detailedly. In this section,the key parameters of the triple Fabry-Perot etalon are optimized and this is the key point.The results of optimizing etalon are as follows:the FSR is 8GHz,the FWHM is1GHz,3.48 GHz is the separation distance between two edge channels,and the separation distance between locking channel and the left edge channel is 1.16 GHz. In this condition,the sensitivity of wind velocity of Mie scattering and Rayleigh scattering is both 0.70%/(m/s) when the temperature is 255K in the height of 5Km and there is no wind. The simulation to this system states that in+/-50m/s radial wind speed range, the wind speed bias induced by Mie signal is less than 0.15m/s from 5 to 50km altitude.

Speciation of antimony in airborne particulate matter using ultrasound probe fast extraction and analysis by HPLC-HG-AFS.

PubMed

Bellido-Martín, A; Gómez-Ariza, J L; Smichowsky, P; Sánchez-Rodas, D

2009-09-07

A fast extraction procedure has been developed for Sb(III) and Sb(V) oxoanions speciation in airborne particulate matter samples. Different extraction media (diammonium tartrate, hidroxilammonium clorhidrate, citric acid+ascorbic acid, phosphoric acid and citrate solutions) were tried, with assistance of an ultrasonic probe. The operation power and time of extraction were also optimized. The higher extraction recoveries were obtained with a 100 mmol L(-1) hidroxilammonium clorhidrate aqueous solution assisted by the ultrasound probe operated at 50 W during 3 min. The extracts were analyzed by HPLC-HG-AFS. The chromatographic separation of Sb(III) and Sb(V) was also optimized using diammonium tartrate and phthalic acid as mobile phases. The separation of both Sb species was performed in less than 3 min under isocratic conditions, using a 200 mmol L(-1) diammonium tartrate solution. The proposed extraction procedure and the HPLC-HG-AFS instrumental coupling have been successfully applied to airborne particulate matter samples, with high Sb content, collected in heavy traffic streets from Buenos Aires (Argentina). The results showed the presence of both Sb species at similar concentrations in the ng m(-3) level. The extraction yield was higher than 90% for all the analyzed samples.

A novel process for recovering valuable metals from waste nickel-cadmium batteries.

PubMed

Huang, Kui; Li, Jia; Xu, Zhenming

2009-12-01

The environment is seriously polluted due to improper and inefficient recycling of waste nickel-cadmium (Ni-Cd) batteries in China. The aim of this work is aimed to seek an environmentally friendly recycling process for resolving the negative impacts on environmental and human health resulting from waste Ni-Cd batteries. This work investigates the fundamentals of waste Ni-Cd batteries recycling through vacuum metallurgy separation (VMS) and magnetic separation (MS). The results obtained demonstrate that the optimal temperature, the addition of carbon powder, and heating time in VMS are 1023 K, 1 wt %, 1.5 h, respectively. More than 99.2 wt % Cd is recovered under the optimal experimental condition, and the Cd purity is 99.98%. Around 98.0 wt % ferromagnetic materials are recovered through MS under 60 rpm rotational speed and the recovery ratios of Fe, Ni and Co are 99.2 wt %, 96.1 wt %, and 86.4 wt %, respectively. The composition of ferromagnetic fractions in the residue after VMS increases from 82.3 to 99.6%. Based on these results, a process (including dismantling and crushing, VMS and MS) for recycling of waste Ni-Cd batteries is proposed. This novel process provides a possibility for recycling waste Ni-Cd batteries in a large industrial scale.

Solid phase extraction and trace monitoring of cadmium ions in environmental water and food samples based on modified magnetic nanoporous silica

NASA Astrophysics Data System (ADS)

Omidi, Fariborz; Behbahani, Mohammad; Kalate Bojdi, Majid; Shahtaheri, Seyed Jamaleddin

2015-12-01

A new method has been developed for trace separation/preconcentration of cadmium ions using pyridine-functionalized magnetic nanoporous silica material (called Py-Fe3O4@MCM-41) as a new magnetic sorbent and their determination by flame atomic absorption spectrometry (FAAS). The Py-Fe3O4@MCM-41 sorbent was characterized by thermogravimetric analysis, differential thermal analysis, transmission electron microscopy, Fourier transform infrared spectrometry and X-ray diffraction. The modified Fe3O4@MCM-41 can be easily separated from an aqueous solution by applying an external magnetic field. Effects of pH, amount of functionalized Fe3O4@MCM-41, extraction time, type and quantity of eluent, desorption time, and interfering ions on the extraction efficiency were evaluated and optimized. Under the optimized conditions, the detection limit and relative standard deviation was 0.04 μg L-1 and 2.9%, respectively and the maximum adsorption capacity of the synthesized sorbent for cadmium ions was 154 mg g-1. The proposed method has been applied to the determination of Cd ions at trace levels in real samples such as, rice, onion, carrot, lettuce, parsley, basil, tap water, river water and seawater with satisfactory results.

Microengineered open tubular columns for GC analysis

NASA Astrophysics Data System (ADS)

Wiranto, Goib; Haskard, Malcolm R.; Mulcahy, Dennis E.; Davey, David E.; Dawes, Ernest F.

1999-09-01

Microengineered open tubular (MOT) columns with semi rectangular cross-sections have been designed and fabricated using microengineering techniques. The creation of 100-micrometers wide, 20-micrometers deep, and 125-cm long columns employed isotropic etching on (100) silicon and anodic bonding with a Pyrex 7740 glass cover plate. Column geometry has been optimized to achieve maximum efficiency and allow extreme operating conditions. The walls of the microcolumns were coated with a non-polar liquid stationary phase. Performances of the MOT columns have been demonstrated by their ability to completely separate a series of hydrocarbon mixture in less than 1.25 min under isothermal condition of 150 degrees C. The achievable column efficiencies as measured in terms of theoretical plate height ranged from 0.57 to 1.45 mm, which agreed well with theoretical predictions.

Sodium-sulfur Cell Technology Flight Experiment (SSCT)

NASA Technical Reports Server (NTRS)

Halbach, Carl R.

1992-01-01

The sodium-sulfur battery is emerging as a prime high-temperature energy storage technology for space flight applications. A Na-S cell demonstration is planned for a 1995-96 NASA Space Shuttle flight which focuses on the microgravity effects on individual cells. The experiment is not optimized for battery performance as such. Rather, it maximizes the variety of operating conditions which the Na-S cell is capable of in a relatively short 5-day flight. The demonstration is designed to reveal the effects of microgravity by comparison with ground test control cells experiencing identical test conditions but with gravity. Specifically, limitations of transport dynamics and associated cell performance characteristics should be revealed. The Na-S Cell Technology Flight Experiment consists of three separate experiments designed to determine cell operating characteristics, detailed electrode kinetics and reactant distributions.

20 CFR 404.1325 - Separation from active service under conditions other than dishonorable.

Code of Federal Regulations, 2013 CFR

2013-04-01

... 20 Employees' Benefits 2 2013-04-01 2013-04-01 false Separation from active service under... of the Uniformed Services Separation from Active Service § 404.1325 Separation from active service under conditions other than dishonorable. Separation from active service under conditions other than...

20 CFR 404.1325 - Separation from active service under conditions other than dishonorable.

Code of Federal Regulations, 2014 CFR

2014-04-01

... 20 Employees' Benefits 2 2014-04-01 2014-04-01 false Separation from active service under... of the Uniformed Services Separation from Active Service § 404.1325 Separation from active service under conditions other than dishonorable. Separation from active service under conditions other than...

20 CFR 404.1325 - Separation from active service under conditions other than dishonorable.

Code of Federal Regulations, 2012 CFR

2012-04-01

... 20 Employees' Benefits 2 2012-04-01 2012-04-01 false Separation from active service under... of the Uniformed Services Separation from Active Service § 404.1325 Separation from active service under conditions other than dishonorable. Separation from active service under conditions other than...

20 CFR 404.1325 - Separation from active service under conditions other than dishonorable.

Code of Federal Regulations, 2011 CFR

2011-04-01

... 20 Employees' Benefits 2 2011-04-01 2011-04-01 false Separation from active service under... of the Uniformed Services Separation from Active Service § 404.1325 Separation from active service under conditions other than dishonorable. Separation from active service under conditions other than...

20 CFR 404.1325 - Separation from active service under conditions other than dishonorable.

Code of Federal Regulations, 2010 CFR

2010-04-01

... 20 Employees' Benefits 2 2010-04-01 2010-04-01 false Separation from active service under... of the Uniformed Services Separation from Active Service § 404.1325 Separation from active service under conditions other than dishonorable. Separation from active service under conditions other than...

Optimizing integrated airport surface and terminal airspace operations under uncertainty

NASA Astrophysics Data System (ADS)

Bosson, Christabelle S.

In airports and surrounding terminal airspaces, the integration of surface, arrival and departure scheduling and routing have the potential to improve the operations efficiency. Moreover, because both the airport surface and the terminal airspace are often altered by random perturbations, the consideration of uncertainty in flight schedules is crucial to improve the design of robust flight schedules. Previous research mainly focused on independently solving arrival scheduling problems, departure scheduling problems and surface management scheduling problems and most of the developed models are deterministic. This dissertation presents an alternate method to model the integrated operations by using a machine job-shop scheduling formulation. A multistage stochastic programming approach is chosen to formulate the problem in the presence of uncertainty and candidate solutions are obtained by solving sample average approximation problems with finite sample size. The developed mixed-integer-linear-programming algorithm-based scheduler is capable of computing optimal aircraft schedules and routings that reflect the integration of air and ground operations. The assembled methodology is applied to a Los Angeles case study. To show the benefits of integrated operations over First-Come-First-Served, a preliminary proof-of-concept is conducted for a set of fourteen aircraft evolving under deterministic conditions in a model of the Los Angeles International Airport surface and surrounding terminal areas. Using historical data, a representative 30-minute traffic schedule and aircraft mix scenario is constructed. The results of the Los Angeles application show that the integration of air and ground operations and the use of a time-based separation strategy enable both significant surface and air time savings. The solution computed by the optimization provides a more efficient routing and scheduling than the First-Come-First-Served solution. Additionally, a data driven analysis is performed for the Los Angeles environment and probabilistic distributions of pertinent uncertainty sources are obtained. A sensitivity analysis is then carried out to assess the methodology performance and find optimal sampling parameters. Finally, simulations of increasing traffic density in the presence of uncertainty are conducted first for integrated arrivals and departures, then for integrated surface and air operations. To compare the optimization results and show the benefits of integrated operations, two aircraft separation methods are implemented that offer different routing options. The simulations of integrated air operations and the simulations of integrated air and surface operations demonstrate that significant traveling time savings, both total and individual surface and air times, can be obtained when more direct routes are allowed to be traveled even in the presence of uncertainty. The resulting routings induce however extra take off delay for departing flights. As a consequence, some flights cannot meet their initial assigned runway slot which engenders runway position shifting when comparing resulting runway sequences computed under both deterministic and stochastic conditions. The optimization is able to compute an optimal runway schedule that represents an optimal balance between total schedule delays and total travel times.

Vertical Isolation for Photodiodes in CMOS Imagers

NASA Technical Reports Server (NTRS)

Pain, Bedabrata

2008-01-01

In a proposed improvement in complementary metal oxide/semi conduct - or (CMOS) image detectors, two additional implants in each pixel would effect vertical isolation between the metal oxide/semiconductor field-effect transistors (MOSFETs) and the photodiode of the pixel. This improvement is expected to enable separate optimization of the designs of the photodiode and the MOSFETs so as to optimize their performances independently of each other. The purpose to be served by enabling this separate optimization is to eliminate or vastly reduce diffusion cross-talk, thereby increasing sensitivity, effective spatial resolution, and color fidelity while reducing noise.

Batch technique to evaluate the efficiency of different natural adsorbents for defluoridation from groundwater

NASA Astrophysics Data System (ADS)

Kumar, Pankaj; Saraswat, Chitresh; Mishra, Binaya Kumar; Avtar, Ram; Patel, Hiral; Patel, Asha; Sharma, Tejal; Patel, Roshni

2017-09-01

Fluoride pollution (with concentration >1.0 mg/L) in groundwater has become a global threat in the recent past due to the lesser availability of potable groundwater resource. In between several defluoridation techniques discovered so far, the adsorption process proved to be most economic and efficient. This study is an effort to evaluate defluoridation efficiency of powdered rice husk, fine chopped rice husk and sawdust by the batch adsorption process. Optimum defluoridation capacity is achieved by optimizing various parameters, viz. dose of adsorbent, pH, contact time and initial concentration. It was found that all three materials can be employed for the defluoridation technique, but powdered rice husk is the best adsorbent in the midst of all three. Powdered rice husk showed fluoride removal efficiency ranging between 85 and 90 % in the contact period of 7 h only in conditions of all optimized parameter. Following this parameter optimization, adsorption efficiency was also evaluated at natural pH of groundwater to minimize the cost of defluoridation. No significant difference was found between fluoride adsorption at optimized pH (pH = 4) and natural one (pH = 7), which concludes that powdered rice husk can be efficiently used for the defluoridation technique at field scale. The adsorption isotherm using this adsorbent perfectly followed Langmuir isotherms. The value of calculated separation factor also suggests the favourable adsorption of fluoride onto this adsorbent under the conditions used for the experiments. The field application for defluoridation of groundwater using this adsorbent (based on pH of natural groundwater there and seasonal variation of temperature) showed the high success rate.

Multivariate Approaches for Simultaneous Determination of Avanafil and Dapoxetine by UV Chemometrics and HPLC-QbD in Binary Mixtures and Pharmaceutical Product.

PubMed

2016-04-07

Multivariate UV-spectrophotometric methods and Quality by Design (QbD) HPLC are described for concurrent estimation of avanafil (AV) and dapoxetine (DP) in the binary mixture and in the dosage form. Chemometric methods have been developed, including classical least-squares, principal component regression, partial least-squares, and multiway partial least-squares. Analytical figures of merit, such as sensitivity, selectivity, analytical sensitivity, LOD, and LOQ were determined. QbD consists of three steps, starting with the screening approach to determine the critical process parameter and response variables. This is followed by understanding of factors and levels, and lastly the application of a Box-Behnken design containing four critical factors that affect the method. From an Ishikawa diagram and a risk assessment tool, four main factors were selected for optimization. Design optimization, statistical calculation, and final-condition optimization of all the reactions were Carried out. Twenty-five experiments were done, and a quadratic model was used for all response variables. Desirability plot, surface plot, design space, and three-dimensional plots were calculated. In the optimized condition, HPLC separation was achieved on Phenomenex Gemini C18 column (250 × 4.6 mm, 5 μm) using acetonitrile-buffer (ammonium acetate buffer at pH 3.7 with acetic acid) as a mobile phase at flow rate of 0.7 mL/min. Quantification was done at 239 nm, and temperature was set at 20°C. The developed methods were validated and successfully applied for simultaneous determination of AV and DP in the dosage form.

Evolved phase separation toward balanced charge transport and high efficiency in polymer solar cells.

PubMed

Fan, Haijun; Zhang, Maojie; Guo, Xia; Li, Yongfang; Zhan, Xiaowei

2011-09-01

Understanding effect of morphology on charge carrier transport within polymer/fullerene bulk heterojunction is necessary to develop high-performance polymer solar cells. In this work, we synthesized a new benzodithiophene-based polymer with good self-organization behavior as well as favorable morphology evolution of its blend films with PC(71)BM under improved processing conditions. Charge carrier transport behavior of blend films was characterized by space charge limited current method. Evolved blend film morphology by controlling blend composition and additive content gradually reaches an optimized state, featured with nanoscale fibrilla polymer phase in moderate size and balanced mobility ratio close to 1:1 for hole and electron. This optimized morphology toward more balanced charge carrier transport accounts for the best power conversion efficiency of 3.2%, measured under simulated AM 1.5 solar irradiation 100 mW/cm(2), through enhancing short circuit current and reducing geminate recombination loss.

Validation of a method for the quantitation of ghrelin and unacylated ghrelin by HPLC.

PubMed

Staes, Edith; Rozet, Eric; Ucakar, Bernard; Hubert, Philippe; Préat, Véronique

2010-02-05

An HPLC/UV method was first optimized for the separation and quantitation of human acylated and unacylated (or des-acyl) ghrelin from aqueous solutions. This method was validated by an original approach using accuracy profiles based on tolerance intervals for the total error measurement. The concentration range that achieved adequate accuracy extended from 1.85 to 59.30microM and 1.93 to 61.60microM for acylated and unacylated ghrelin, respectively. Then, optimal temperature, pH and buffer for sample storage were determined. Unacylated ghrelin was found to be stable in all conditions tested. At 37 degrees C acylated ghrelin was stable at pH 4 but unstable at pH 7.4, the main degradation product was unacylated ghrelin. Finally, this validated HPLC/UV method was used to evaluate the binding of acylated and unacylated ghrelin to liposomes.

Optimization of constellation jettisoning regards to short term collision risks

NASA Astrophysics Data System (ADS)

Handschuh, D.-DA.-A.; Bourgeois, E.

2018-04-01

The space debris problematic is directly linked to the in-orbit collision risk between artificial satellites. With the increase of the space constellation projects, a multiplication of multi-payload launches should occur. In the specific cases where many satellites are injected into orbit with the same launcher upper stage, all these objects will be placed on similar orbits, very close one from each other, at a specific moment where their control capabilities will be very limited. Under this hypothesis, it is up to the launcher operator to ensure that the simultaneous in-orbit injection is safe enough to guarantee the non-collision risk between all the objects under a ballistic hypothesis eventually considering appropriate uncertainties. The purpose of the present study is to find optimized safe separation conditions to limit the in-orbit collision risk following the injection of many objects on very close orbits in a short-delay mission.

Cloud point extraction and flame atomic absorption spectrometric determination of cadmium and nickel in drinking and wastewater samples.

PubMed

Naeemullah; Kazi, Tasneem G; Shah, Faheem; Afridi, Hassan I; Baig, Jameel Ahmed; Soomro, Abdul Sattar

2013-01-01

A simple method for the preconcentration of cadmium (Cd) and nickel (Ni) in drinking and wastewater samples was developed. Cloud point extraction has been used for the preconcentration of both metals, after formation of complexes with 8-hydroxyquinoline (8-HQ) and extraction with the surfactant octylphenoxypolyethoxyethanol (Triton X-114). Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation, and the Cd and Ni contents were measured by flame atomic absorption spectrometry. The experimental variables, such as pH, amounts of reagents (8-HQ and Triton X-114), temperature, incubation time, and sample volume, were optimized. After optimization of the complexation and extraction conditions, enhancement factors of 80 and 61, with LOD values of 0.22 and 0.52 microg/L, were obtained for Cd and Ni, respectively. The proposed method was applied satisfactorily for the determination of both elements in drinking and wastewater samples.

Optimization of L(+)-Lactic Acid Fermentation Without Neutralisation of Rhizopus Oryzae Mutant RK02 by Low-Energy Ion Implantation

NASA Astrophysics Data System (ADS)

Li, Wen; Wang, Tao; Yang, Yingge; Liu, Dan; Fan, Yonghong; Wang, Dongmei; Yang, Qian; Yao, Jianming; Zheng, Zhiming; Yu, Zengliang

2008-04-01

In order to get an industrial strain which can yield a high concentration of lactic acid for ISPR (in situ product removal), the original strain Rhizopus oryzae RE3303 was mutated by low-energy ion beam implantation. A mutant RK02 was screened, and the factors such as the substrate concentration, nitrogen source concentration, inoculum size, seed age, aeration and temperature that affect the production of lactic acid were studied in detail. Under optimal conditions, the maximum concentration of L(+)-lactic acid reached 34.85 g/L after 30 h shake-flask cultivation without adding any neutralisation (5% Glucose added), which was a 146% increase in lactic acid production after ion implantation compared with the original strain. It was also shown that RK02 can be used in ISPR to reduce the number of times of separation.

Comparative study of thermochemical processes for hydrogen production from biomass fuels.

PubMed

Biagini, Enrico; Masoni, Lorenzo; Tognotti, Leonardo

2010-08-01

Different thermochemical configurations (gasification, combustion, electrolysis and syngas separation) are studied for producing hydrogen from biomass fuels. The aim is to provide data for the production unit and the following optimization of the "hydrogen chain" (from energy source selection to hydrogen utilization) in the frame of the Italian project "Filiera Idrogeno". The project focuses on a regional scale (Tuscany, Italy), renewable energies and automotive hydrogen. Decentred and small production plants are required to solve the logistic problems of biomass supply and meet the limited hydrogen infrastructures. Different options (gasification with air, oxygen or steam/oxygen mixtures, combustion, electrolysis) and conditions (varying the ratios of biomass and gas input) are studied by developing process models with uniform hypothesis to compare the results. Results obtained in this work concern the operating parameters, process efficiencies, material and energetic needs and are fundamental to optimize the entire hydrogen chain. Copyright 2010 Elsevier Ltd. All rights reserved.

Optimal operation of turbo blowers serially connected using inlet vanes

NASA Astrophysics Data System (ADS)

Jang, Choon-Man

2011-03-01

Optimal operation of the turbo blowers having an inlet vane has been studied to understand the blowers' operating performance. To analyze three-dimensional flow field in the turbo blowers serially connected, general analysis code, CFX, is introduced in the present work. SST turbulence model is employed to estimate the eddy viscosity. Throughout the numerical analysis, it is found that the flow rates of the turbo blowers can be controlled at the vane angle between 90 (full open condition) degrees and 60 degrees effectively, because pressure loss rapidly increases below 60 degree of a vane angle. Efficiency also has almost the same values from 90 degrees to 60 degrees of a vane angle. It is noted that the distorted inlet velocity generated in the small vane angle makes performance deterioration of the turbo blowers due to the local leading edge separation and the following non-uniform blade loading.

The efficacy of a restart break for recycling with optimal performance depends critically on circadian timing.

PubMed

Van Dongen, Hans P A; Belenky, Gregory; Vila, Bryan J

2011-07-01

Under simulated shift-work conditions, we investigated the efficacy of a restart break for maintaining neurobehavioral functioning across consecutive duty cycles, as a function of the circadian timing of the duty periods. As part of a 14-day experiment, subjects underwent two cycles of five simulated daytime or nighttime duty days, separated by a 34-hour restart break. Cognitive functioning and high-fidelity driving simulator performance were tested 4 times per day during the two duty cycles. Lapses on a psychomotor vigilance test (PVT) served as the primary outcome variable. Selected sleep periods were recorded polysomnographically. The experiment was conducted under standardized, controlled laboratory conditions with continuous monitoring. Twenty-seven healthy adults (13 men, 14 women; aged 22-39 years) participated in the study. Subjects were randomly assigned to a nighttime duty (experimental) condition or a daytime duty (control) condition. The efficacy of the 34-hour restart break for maintaining neurobehavioral functioning from the pre-restart duty cycle to the post-restart duty cycle was compared between these two conditions. Relative to the daytime duty condition, the nighttime duty condition was associated with reduced amounts of sleep, whereas sleep latencies were shortened and slow-wave sleep appeared to be conserved. Neurobehavioral performance measures ranging from lapses of attention on the PVT to calculated fuel consumption on the driving simulators remained optimal across time of day in the daytime duty schedule, but degraded across time of night in the nighttime duty schedule. The 34-hour restart break was efficacious for maintaining PVT performance and other objective neurobehavioral functioning profiles from one duty cycle to the next in the daytime duty condition, but not in the nighttime duty condition. Subjective sleepiness did not reliably track objective neurobehavioral deficits. The 34-hour restart break was adequate for maintaining performance in the case of optimal circadian placement of sleep and duty periods (control condition) but was inadequate (and perhaps even detrimental) for maintaining performance in a simulated nighttime duty schedule (experimental condition). Current US transportation hours-of-service regulations mandate time off duty but do not consider the circadian aspects of shift scheduling. Reinforcing a recent trend of applying sleep science to inform policymaking for duty and rest times, our findings indicate that restart provisions in hours-of-service regulations could be improved by taking the circadian timing of the duty schedules into account.

Inter-Population Movements of Steller Sea Lions in Alaska with Implications for Population Separation

PubMed Central

Jemison, Lauri A.; Pendleton, Grey W.; Fritz, Lowell W.; Hastings, Kelly K.; Maniscalco, John M.; Trites, Andrew W.; Gelatt, Tom S.

2013-01-01

Genetic studies and differing population trends support the separation of Steller sea lions (Eumetopias jubatus) into a western distinct population segment (WDPS) and an eastern DPS (EDPS) with the dividing line between populations at 144° W. Despite little exchange for thousands of years, the gap between the breeding ranges narrowed during the past 15–30 years with the formation of new rookeries near the DPS boundary. We analyzed >22,000 sightings of 4,172 sea lions branded as pups in each DPS from 2000–2010 to estimate probabilities of a sea lion born in one DPS being seen within the range of the other DPS (either ‘West’ or ‘East’). Males from both populations regularly traveled across the DPS boundary; probabilities were highest at ages 2–5 and for males born in Prince William Sound and southern Southeast Alaska. The probability of WDPS females being in the East at age 5 was 0.067 but 0 for EDPS females which rarely traveled to the West. Prince William Sound-born females had high probabilities of being in the East during breeding and non-breeding seasons. We present strong evidence that WDPS females have permanently emigrated to the East, reproducing at two ‘mixing zone’ rookeries. We documented breeding bulls that traveled >6,500 km round trip from their natal rookery in southern Alaska to the northern Bering Sea and central Aleutian Islands and back within one year. WDPS animals began moving East in the 1990s, following steep population declines in the central Gulf of Alaska. Results of our study, and others documenting high survival and rapid population growth in northern Southeast Alaska suggest that conditions in this mixing zone region have been optimal for sea lions. It is unclear whether eastward movement across the DPS boundary is due to less-optimal conditions in the West or a reflection of favorable conditions in the East. PMID:23940543

Inter-population movements of steller sea lions in Alaska with implications for population separation.

PubMed

Jemison, Lauri A; Pendleton, Grey W; Fritz, Lowell W; Hastings, Kelly K; Maniscalco, John M; Trites, Andrew W; Gelatt, Tom S

2013-01-01

Genetic studies and differing population trends support the separation of Steller sea lions (Eumetopias jubatus) into a western distinct population segment (WDPS) and an eastern DPS (EDPS) with the dividing line between populations at 144° W. Despite little exchange for thousands of years, the gap between the breeding ranges narrowed during the past 15-30 years with the formation of new rookeries near the DPS boundary. We analyzed >22,000 sightings of 4,172 sea lions branded as pups in each DPS from 2000-2010 to estimate probabilities of a sea lion born in one DPS being seen within the range of the other DPS (either 'West' or 'East'). Males from both populations regularly traveled across the DPS boundary; probabilities were highest at ages 2-5 and for males born in Prince William Sound and southern Southeast Alaska. The probability of WDPS females being in the East at age 5 was 0.067 but 0 for EDPS females which rarely traveled to the West. Prince William Sound-born females had high probabilities of being in the East during breeding and non-breeding seasons. We present strong evidence that WDPS females have permanently emigrated to the East, reproducing at two 'mixing zone' rookeries. We documented breeding bulls that traveled >6,500 km round trip from their natal rookery in southern Alaska to the northern Bering Sea and central Aleutian Islands and back within one year. WDPS animals began moving East in the 1990s, following steep population declines in the central Gulf of Alaska. Results of our study, and others documenting high survival and rapid population growth in northern Southeast Alaska suggest that conditions in this mixing zone region have been optimal for sea lions. It is unclear whether eastward movement across the DPS boundary is due to less-optimal conditions in the West or a reflection of favorable conditions in the East.

Stationary-phase optimized selectivity liquid chromatography: development of a linear gradient prediction algorithm.

PubMed

De Beer, Maarten; Lynen, Fréderic; Chen, Kai; Ferguson, Paul; Hanna-Brown, Melissa; Sandra, Pat

2010-03-01

Stationary-phase optimized selectivity liquid chromatography (SOS-LC) is a tool in reversed-phase LC (RP-LC) to optimize the selectivity for a given separation by combining stationary phases in a multisegment column. The presently (commercially) available SOS-LC optimization procedure and algorithm are only applicable to isocratic analyses. Step gradient SOS-LC has been developed, but this is still not very elegant for the analysis of complex mixtures composed of components covering a broad hydrophobicity range. A linear gradient prediction algorithm has been developed allowing one to apply SOS-LC as a generic RP-LC optimization method. The algorithm allows operation in isocratic, stepwise, and linear gradient run modes. The features of SOS-LC in the linear gradient mode are demonstrated by means of a mixture of 13 steroids, whereby baseline separation is predicted and experimentally demonstrated.

Determination of absorption changes from moments of distributions of times of flight of photons: optimization of measurement conditions for a two-layered tissue model.

PubMed

Liebert, Adam; Wabnitz, Heidrun; Elster, Clemens

2012-05-01

Time-resolved near-infrared spectroscopy allows for depth-selective determination of absorption changes in the adult human head that facilitates separation between cerebral and extra-cerebral responses to brain activation. The aim of the present work is to analyze which combinations of moments of measured distributions of times of flight (DTOF) of photons and source-detector separations are optimal for the reconstruction of absorption changes in a two-layered tissue model corresponding to extra- and intra-cerebral compartments. To this end we calculated the standard deviations of the derived absorption changes in both layers by considering photon noise and a linear relation between the absorption changes and the DTOF moments. The results show that the standard deviation of the absorption change in the deeper (superficial) layer increases (decreases) with the thickness of the superficial layer. It is confirmed that for the deeper layer the use of higher moments, in particular the variance of the DTOF, leads to an improvement. For example, when measurements at four different source-detector separations between 8 and 35 mm are available and a realistic thickness of the upper layer of 12 mm is assumed, the inclusion of the change in mean time of flight, in addition to the change in attenuation, leads to a reduction of the standard deviation of the absorption change in the deeper tissue layer by a factor of 2.5. A reduction by another 4% can be achieved by additionally including the change in variance.

Demand driven salt clean-up in a molten salt fast reactor - Defining a priority list.

PubMed

Merk, B; Litskevich, D; Gregg, R; Mount, A R

2018-01-01

The PUREX technology based on aqueous processes is currently the leading reprocessing technology in nuclear energy systems. It seems to be the most developed and established process for light water reactor fuel and the use of solid fuel. However, demand driven development of the nuclear system opens the way to liquid fuelled reactors, and disruptive technology development through the application of an integrated fuel cycle with a direct link to reactor operation. The possibilities of this new concept for innovative reprocessing technology development are analysed, the boundary conditions are discussed, and the economic as well as the neutron physical optimization parameters of the process are elucidated. Reactor physical knowledge of the influence of different elements on the neutron economy of the reactor is required. Using an innovative study approach, an element priority list for the salt clean-up is developed, which indicates that separation of Neodymium and Caesium is desirable, as they contribute almost 50% to the loss of criticality. Separating Zirconium and Samarium in addition from the fuel salt would remove nearly 80% of the loss of criticality due to fission products. The theoretical study is followed by a qualitative discussion of the different, demand driven optimization strategies which could satisfy the conflicting interests of sustainable reactor operation, efficient chemical processing for the salt clean-up, and the related economic as well as chemical engineering consequences. A new, innovative approach of balancing the throughput through salt processing based on a low number of separation process steps is developed. Next steps for the development of an economically viable salt clean-up process are identified.

Gas chromatography-mass spectrometry of hexafluoroacetone derivatives: First time utilization of a gaseous phase derivatizing agent for analysis of extraterrestrial amino acids.

PubMed

Geffroy-Rodier, C; Buch, A; Sternberg, R; Papot, S

2012-07-06

Within the perspective of the current and next space missions to Mars (MSL 2011 and Exomars 2016-2018), the detection and enantioselective separation of building blocks such as the amino acids are important subjects which are becoming fundamental for the search for traces of life on the surface and subsurface of Mars. In this work, we have developed and optimized a method adapted to space experimentation to derivatize and analyze amino acids, using hexafluoroacetone as the derivatizing agent. The temperature, duration of the derivative transfer to the analyser, and chromatographic separation parameters have been optimized to meet the instrument design constraints imposed on devices for extraterrestrial experiments. The work presented in this rationale has established that hexafluoroacetone, in addition to its intrinsic qualities, such as the production of light-weight derivatives (no racemization) and great resistance to the drastic operating conditions, has indeed facilitated simple and fast derivatization that appears to be suitable for in situ analysis in space. By using hexafluoroacetone as the derivatizing agent, we successfully identified, 21 amino acids including 12 of the 20 proteinic amino acids without stirring or extraction steps. Ten of these derivatized amino acids were enantioselectively separated. The precision and accuracy measurements for the D/L ratio showed that the proposed method was also suitable for the determination of both enantioselective forms of most of the tested amino acids. The limits of detection obtained were lower than the ppb level of organic molecules detected in Martian meteorites. Copyright © 2012 Elsevier B.V. All rights reserved.

PVC removal from mixed plastics by triboelectrostatic separation.

PubMed

Park, Chul-Hyun; Jeon, Ho-Seok; Park, Jai-Koo

2007-06-01

Ever increasing oil price and the constant growth in generation of waste plastics stimulate a research on material separation for recycling of waste plastics. At present, most waste plastics cause serious environmental problems due to the disposal by reclamation and incineration. Particularly, polyvinyl chloride (PVC) materials among waste plastics generates hazardous HCl gas, dioxins containing Cl, and so on, which lead to air pollution and shorten the life of incinerator, and it makes difficultly recycling of other plastics. Therefore, we designed a bench scale triboelectrostatic separator for PVC removal from mixed plastics (polyvinyl chloride/polyethylene terephthalate), and then carried out material separation tests. In triboelectrostatic separation, PVC and PET particles are charged negatively and positively, respectively, due to the difference of the work function of plastics in tribo charger of the fluidized-bed, and are separated by means of splitter through an opposite electric field. In this study, the charge efficiency of PVC and PET was strongly dependent on the tribo charger material (polypropylene), relative humidity (below 30%), air velocity (over 10 m/s), and mixture ratio (PET:PVC=1:1). At the optimum conditions (electrode potential of 20 kV and splitter position of -2 cm), PVC rejection and PET recovery in PET products were 99.60 and 98.10%, respectively, and the reproducibility of optimal test was very good (+/-1%). In addition, as a change of splitter position, we developed the technique to recover high purity PET (over 99.99%) although PET recovery decreases by degrees.

The Effect of Column and Eluent Fluorination on the Retention and Separation of non-Fluorinated Amino Acids and Proteins by HPLC

PubMed Central

Joyner, Katherine; Wang, Weizhen; Yu, Yihua Bruce

2011-01-01

The effect of column and eluent fluorination on the retention and separation of non-fluorinated amino acids and proteins in HPLC is investigated. A side-by-side comparison of fluorocarbon column and eluents (F-column and F-eluents) with their hydrocarbon counterparts (H-column and H-eluents) in the separation of a group of 33 analytes, including 30 amino acids and 3 proteins, is conducted. The H-column and the F-column contain the n-C8H17 group and n-C8F17 group, respectively, in their stationary phases. The H-eluents include ethanol (EtOH) and isopropanol (ISP) while the F-eluents include trifluoroethanol (TFE) and hexafluorosopropanol (HFIP). The 2 columns and 4 eluents generated 8 (column, eluent) pairs that produce 264 retention time data points for the 33 analytes. A statistical analysis of the retention time data reveals that although the H-column is better than the F-column in analyte separation and H-eluents are better than F-eluents in analyte retention, the more critical factor is the proper pairing of column with eluent. Among the conditions explored in this project, optimal retention and separation is achieved when the fluorocarbon column is paired with ethanol, even though TFE is the most polar one among the 4 eluents. This result shows fluorocarbon columns have much potential in chromatographic analysis and separation of non-fluorinated amino acids and proteins. PMID:21318121