Coupling Front-End Separations, Ion Mobility Spectrometry, and Mass Spectrometry For Enhanced Multidimensional Biological and Environmental Analyses

PubMed Central

Zheng, Xueyun; Wojcik, Roza; Zhang, Xing; Ibrahim, Yehia M.; Burnum-Johnson, Kristin E.; Orton, Daniel J.; Monroe, Matthew E.; Moore, Ronald J.; Smith, Richard D.; Baker, Erin S.

2017-01-01

Ion mobility spectrometry (IMS) is a widely used analytical technique for rapid molecular separations in the gas phase. Though IMS alone is useful, its coupling with mass spectrometry (MS) and front-end separations is extremely beneficial for increasing measurement sensitivity, peak capacity of complex mixtures, and the scope of molecular information available from biological and environmental sample analyses. In fact, multiple disease screening and environmental evaluations have illustrated that the IMS-based multidimensional separations extract information that cannot be acquired with each technique individually. This review highlights three-dimensional separations using IMS-MS in conjunction with a range of front-end techniques, such as gas chromatography, supercritical fluid chromatography, liquid chromatography, solid-phase extractions, capillary electrophoresis, field asymmetric ion mobility spectrometry, and microfluidic devices. The origination, current state, various applications, and future capabilities of these multidimensional approaches are described in detail to provide insight into their uses and benefits. PMID:28301728

Survey of Biochemical Separation Techniques

ERIC Educational Resources Information Center

Nilsson, Melanie R.

2007-01-01

A simple laboratory exercise is illustrated that exposes students to wide range of separation techniques in one laboratory program and provides a nice complement to a project-oriented program. Students have learned the basic principles of syringe filtration, centricon, dialysis, gel filtration and solid-phase extraction methodologies and have got…

Water-induced phase separation of miconazole-poly (vinylpyrrolidone-co-vinyl acetate) amorphous solid dispersions: Insights with confocal fluorescence microscopy.

PubMed

Saboo, Sugandha; Taylor, Lynne S

2017-08-30

The aim of this study was to evaluate the utility of confocal fluorescence microscopy (CFM) to study the water-induced phase separation of miconazole-poly (vinylpyrrolidone-co-vinyl acetate) (mico-PVPVA) amorphous solid dispersions (ASDs), induced during preparation, upon storage at high relative humidity (RH) and during dissolution. Different fluorescent dyes were added to drug-polymer films and the location of the dyes was evaluated using CFM. Orthogonal techniques, in particular atomic force microscopy (AFM) coupled with nanoscale infrared spectroscopy (AFM-nanoIR), were used to provide additional analysis of the drug-polymer blends. The initial miscibility of mico-PVPVA ASDs prepared under low humidity conditions was confirmed by AFM-nanoIR. CFM enabled rapid identification of drug-rich and polymer-rich phases in phase separated films prepared under high humidity conditions. The identity of drug- and polymer-rich domains was confirmed using AFM-nanoIR imaging and localized IR spectroscopy, together with Lorentz contact resonance (LCR) measurements. The CFM technique was then utilized successfully to further investigate phase separation in mico-PVPVA films exposed to high RH storage and to visualize phase separation dynamics following film immersion in buffer. CFM is thus a promising new approach to study the phase behavior of ASDs, utilizing drug and polymer specific dyes to visualize the evolution of heterogeneity in films exposed to water. Copyright © 2017 Elsevier B.V. All rights reserved.

Separation techniques: Chromatography

PubMed Central

Coskun, Ozlem

2016-01-01

Chromatography is an important biophysical technique that enables the separation, identification, and purification of the components of a mixture for qualitative and quantitative analysis. Proteins can be purified based on characteristics such as size and shape, total charge, hydrophobic groups present on the surface, and binding capacity with the stationary phase. Four separation techniques based on molecular characteristics and interaction type use mechanisms of ion exchange, surface adsorption, partition, and size exclusion. Other chromatography techniques are based on the stationary bed, including column, thin layer, and paper chromatography. Column chromatography is one of the most common methods of protein purification. PMID:28058406

Highly efficient peptide separations in proteomics. Part 2: bi- and multidimensional liquid-based separation techniques.

PubMed

Sandra, Koen; Moshir, Mahan; D'hondt, Filip; Tuytten, Robin; Verleysen, Katleen; Kas, Koen; François, Isabelle; Sandra, Pat

2009-04-15

Multidimensional liquid-based separation techniques are described for maximizing the resolution of the enormous number of peptides generated upon tryptic digestion of proteomes, and hence, reduce the spatial and temporal complexity of the sample to a level that allows successful mass spectrometric analysis. This review complements the previous contribution on unidimensional high performance liquid chromatography (HPLC). Both chromatography and electrophoresis will be discussed albeit with reversed-phase HPLC (RPLC) as the final separation dimension prior to MS analysis.

Green chiral HPLC enantiomeric separations using high temperature liquid chromatography and subcritical water on Chiralcel OD and Chiralpak AD.

PubMed

Droux, Serge; Félix, Guy

2011-01-01

We report here the application of subcritical water in chiral separations on two popular polysaccharide chiral stationary phases (CSPs): Chiralpak AD and Chiralcel OD. The behavior of these two CSPs was studied under reversed phase conditions at room temperature to discover the maximum percentage of water in the mobile phase, which provided the separation of enantiomers of flavanone and benzoin, respectively, in a reasonable time (i.e., less than 1 h). Then, the stability of Chiralpak AD and Chiralcel OD versus temperature was investigated and discussed. Chiralcel OD separation of flavanone racemate was obtained at 120 °C with water and 2-propanol (80/20) as the mobile phase, while benzoin racemate was separated in pure water at 160 °C. Separations of several racemates were also presented, and advantages and limitations of the technique were discussed. Copyright © 2011 Wiley Periodicals, Inc.

Improved Separations of Proteins and Sugar Derivatives Using the Small-Scale Cross-Axis Coil Planet Centrifuge with Locular Multilayer Coiled Columns

PubMed Central

Shinomiya, Kazufusa; Umezawa, Motoki; Seki, Manami; Nitta, Jun; Zaima, Kazumasa; Harikai, Naoki; Ito, Yoichiro

2016-01-01

1) Background Countercurrent chromatography (CCC) is liquid-liquid partition chromatography without using a solid support matrix. This technique requires further improvement of partition efficiency and shortening theseparation time. 2) Methods The locular multilayer coils modified with and without mixer glass beads were developed for the separation of proteins and 4-methylumbelliferyl (MU) sugar derivatives using the small-scale cross-axis coil planet centrifuge. 3) Results Proteins were well separated from each other and the separation was improved at a low flow rate of the mobile phase. On the other hand, 4-MU sugar derivatives were sufficiently resolved with short separation time at a highflow rate of the mobile phase under satisfactory stationary phase retention. 4) Conclusion Effective separations were achieved using the locular multilayer coil for proteins with aqueous-aqueous polymer phase systems and for 4-MU sugar derivatives with organic-aqueous two-phase solvent systems by inserting a glass bead into each locule. PMID:27891507

Approaches for enantioselective resolution of pharmaceuticals by miniaturised separation techniques with new chiral phases based on nanoparticles and monolithis.

PubMed

Sierra, Isabel; Marina, Maria Luisa; Pérez-Quintanilla, Damián; Morante-Zarcero, Sonia; Silva, Mariana

2016-10-01

This article discusses new developments in the preparation of nanoparticles and monoliths with emphasis upon their application as the stationary and pseudo-stationary phases for miniaturised liquid phase separation techniques, which have occurred in the last 10 years (from 2006 to the actuality). References included in this review represent current trends and state of the art in the application of these materials to the analysis, by EKC, CEC and miniaturised chromatography, of chiral compounds with environmental interest such as pharmaceuticals. Due to their extraordinary properties, columns prepared with these new chiral stationary or pseudo-stationary phases, based on materials such as gold nanoparticles, metal-organic frameworks, ordered mesoporous silicas, carbonaceous materials, polymeric-based and silica-based monoliths or molecularly imprinted materials, can usually show some improvements in the separation selectivity, column efficiency and chemical stability in comparison with conventional chiral columns available commercially. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Separation techniques. [in space experiments

NASA Technical Reports Server (NTRS)

Snyder, R. S.

1986-01-01

Progress in developing three technologies for separating proteins in a microgravity environment is reviewed. NASA research on electrophoresis, electroosmosis, and phase partitioning is summarized. Future STS missions will characterize these processes in more detail.

Systematic Comparison of Reverse Phase and Hydrophilic Interaction Liquid Chromatography Platforms for the Analysis of N-linked Glycans

PubMed Central

Walker, S. Hunter; Carlisle, Brandon C.; Muddiman, David C.

2013-01-01

Due to the hydrophilic nature of glycans, reverse phase chromatography has not been widely used as a glycomic separation technique coupled to mass spectrometry. Other approaches such as hydrophilic interaction chromatography and porous graphitized carbon chromatography are often employed, though these strategies frequently suffer from decreased chromatographic resolution, long equilibration times, indefinite retention, and column bleed. Herein, it is shown that through an efficient hydrazone formation derivatization of N-linked glycans (∼4 hr of additional sample preparation time which is carried out in parallel), numerous experimental and practical advantages are gained when analyzing the glycans by online reverse phase chromatography. These benefits include an increased number of glycans detected, increased peak capacity of the separation, and the ability to analyze glycans on the identical liquid chromatography-mass spectrometry platform commonly used for proteomic analyses. The data presented show that separation of derivatized N-linked glycans by reverse phase chromatography significantly out-performs traditional separation of native or derivatized glycans by hydrophilic interaction chromatography. Furthermore, the movement to a more ubiquitous separation technique will afford numerous research groups the opportunity to analyze both proteomic and glycomic samples on the same platform with minimal time and physical change between experiments, increasing the efficiency of ‘multi-omic’ biological approaches. PMID:22954204

STS-42 Phase Partitioning Experiment (PPE) closeup taken onboard OV-103

NASA Technical Reports Server (NTRS)

1992-01-01

STS-42 Phase Partitioning Experiment (PPE), an International Microgravity Laboratory 1 (IML-1) experiment, is documented in a closeup taken onboard Discovery, Orbiter Vehicle (OV) 103. Phase partitioning is a very effective technique used by biochemists and cell biologists to obtain fairly pure cells. Cells are separated and collected in a mixture of two immiscible liquids (fluids that tend not to mix) by their surface characteristics. In the PPE, investigators feel they will be able to separate closely related cells because cell density and convection flows are not factors in the phase partitioning process in space. They also hope to study other factors that influence the process. Phase partitioning is used to separate biological materials such as bone marrow cells for cancer treatment.

Recent progress of chiral stationary phases for separation of enantiomers in gas chromatography.

PubMed

Xie, Sheng-Ming; Yuan, Li-Ming

2017-01-01

Chromatography techniques based on chiral stationary phases are widely used for the separation of enantiomers. In particular, gas chromatography has developed rapidly in recent years due to its merits such as fast analysis speed, lower consumption of stationary phases and analytes, higher column efficiency, making it a better choice for chiral separation in diverse industries. This article summarizes recent progress of novel chiral stationary phases based on cyclofructan derivatives and chiral porous materials including chiral metal-organic frameworks, chiral porous organic frameworks, chiral inorganic mesoporous materials, and chiral porous organic cages in gas chromatography, covering original research papers published since 2010. The chiral recognition properties and mechanisms of separation toward enantiomers are also introduced. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fluid Phase Separation (FPS) experiment for flight on the shuttle in a Get Away Special (GAS) canister: Design and fabrication

NASA Technical Reports Server (NTRS)

1990-01-01

The separation of fluid phases in microgravity environments is of importance to environmental control and life support systems (ECLSS) and materials processing in space. A successful fluid phase separation experiment will demonstrate a proof of concept for the separation technique and add to the knowledge base of material behavior. The phase separation experiment will contain a premixed fluid that will be exposed to a microgravity environment. After the phase separation of the compound has occurred, small samples of each of the species will be taken for analysis on Earth. By correlating the time of separation and the temperature history of the fluid, it will be possible to characterize the process. The phase separation experiment is totally self-contained, with three levels of containment on all fluids, and provides all necessary electrical power and control. The controller regulates the temperature of the fluid and controls data logging and sampling. An astronaut-activated switch will initiate the experiment and an unmaskable interrupt is provided for shutdown. The experiment has been integrated into space available on a manifested Get Away Special (GAS) experiment, CONCAP 2, part of the Consortium for Materials Complex Autonomous Payload (CAP) Program, scheduled for STS 42 in April 1991. Presented here are the design and the production of a fluid phase separation experiment for rapid implementation at low cost.

Nanoscopy of Phase Separation in InxGa1-xN Alloys.

PubMed

Abate, Yohannes; Seidlitz, Daniel; Fali, Alireza; Gamage, Sampath; Babicheva, Viktoriia; Yakovlev, Vladislav S; Stockman, Mark I; Collazo, Ramon; Alden, Dorian; Dietz, Nikolaus

2016-09-07

Phase separations in ternary/multinary semiconductor alloys is a major challenge that limits optical and electronic internal device efficiency. We have found ubiquitous local phase separation in In1-xGaxN alloys that persists to nanoscale spatial extent by employing high-resolution nanoimaging technique. We lithographically patterned InN/sapphire substrates with nanolayers of In1-xGaxN down to few atomic layers thick that enabled us to calibrate the near-field infrared response of the semiconductor nanolayers as a function of composition and thickness. We also developed an advanced theoretical approach that considers the full geometry of the probe tip and all the sample and substrate layers. Combining experiment and theory, we identified and quantified phase separation in epitaxially grown individual nanoalloys. We found that the scale of the phase separation varies widely from particle to particle ranging from all Ga- to all In-rich regions and covering everything in between. We have found that between 20 and 25% of particles show some level of Ga-rich phase separation over the entire sample region, which is in qualitative agreement with the known phase diagram of In1-xGaxN system.

Numerical analysis of wet separation of particles by density differences

NASA Astrophysics Data System (ADS)

Markauskas, D.; Kruggel-Emden, H.

2017-07-01

Wet particle separation is widely used in mineral processing and plastic recycling to separate mixtures of particulate materials into further usable fractions due to density differences. This work presents efforts aiming to numerically analyze the wet separation of particles with different densities. In the current study the discrete element method (DEM) is used for the solid phase while the smoothed particle hydrodynamics (SPH) is used for modeling of the liquid phase. The two phases are coupled by the use of a volume averaging technique. In the current study, simulations of spherical particle separation were performed. In these simulations, a set of generated particles with two different densities is dropped into a rectangular container filled with liquid. The results of simulations with two different mixtures of particles demonstrated how separation depends on the densities of particles.

Liquid chromatographic separation of terpenoid pigments in foods and food products.

PubMed

Cserháti, T; Forgács, E

2001-11-30

The newest achievements in the use of various liquid chromatographic techniques such as adsorption and reversed-phase thin-layer chromatography and HPLC employed for the separation and quantitative determination of terpenoid-based color substances in foods and food products are reviewed. The techniques applied for the analysis of individual pigments and pigments classes are surveyed and critically evaluated. Future trends in the separation and identification of pigments in foods and food products are delineated.

SEPARATION OF HAZARDOUS ORGANICS BY LOW PRESSURE REVERSE OSMOSIS MEMBRANES - PHASE II FINAL REPORT

EPA Science Inventory

Extensive experimental studies showed that thin-film, composite membranes can be used effectively for the separation of selected hazardous organic compounds. This waste treatment technique offers definite advantages in terms of high solute separations at low pressures (<2MPa) and...

Tube radial distribution phenomenon with a two-phase separation solution of a fluorocarbon and hydrocarbon organic solvent mixture in a capillary tube and metal compounds separation.

PubMed

Kitaguchi, Koichi; Hanamura, Naoya; Murata, Masaharu; Hashimoto, Masahiko; Tsukagoshi, Kazuhiko

2014-01-01

A fluorocarbon and hydrocarbon organic solvent mixture is known as a temperature-induced phase-separation solution. When a mixed solution of tetradecafluorohexane as a fluorocarbon organic solvent and hexane as a hydrocarbon organic solvent (e.g., 71:29 volume ratio) was delivered in a capillary tube that was controlled at 10°C, the tube radial distribution phenomenon (TRDP) of the solvents was clearly observed through fluorescence images of the dye, perylene, dissolved in the mixed solution. The homogeneous mixed solution (single phase) changed to a heterogeneous solution (two phases) with inner tetradecafluorohexane and outer hexane phases in the tube under laminar flow conditions, generating the dynamic liquid-liquid interface. We also tried to apply TRDP to a separation technique for metal compounds. A model analyte mixture, copper(II) and hematin, was separated through the capillary tube, and detected with a chemiluminescence detector in this order within 4 min.

Null test fourier domain alignment technique for phase-shifting point diffraction interferometer

DOEpatents

Naulleau, Patrick; Goldberg, Kenneth Alan

2000-01-01

Alignment technique for calibrating a phase-shifting point diffraction interferometer involves three independent steps where the first two steps independently align the image points and pinholes in rotation and separation to a fixed reference coordinate system, e.g, CCD. Once the two sub-elements have been properly aligned to the reference in two parameters (separation and orientation), the third step is to align the two sub-element coordinate systems to each other in the two remaining parameters (x,y) using standard methods of locating the pinholes relative to some easy to find reference point.

Fabrication of PVDF-based blend membrane with a thin hydrophilic deposition layer and a network structure supporting layer via the thermally induced phase separation followed by non-solvent induced phase separation process

NASA Astrophysics Data System (ADS)

Wu, Zhiguo; Cui, Zhenyu; Li, Tianyu; Qin, Shuhao; He, Benqiao; Han, Na; Li, Jianxin

2017-10-01

A simple strategy of thermally induced phase separation followed by non-solvent induced phase separation (TIPS-NIPS) is reported to fabricate poly (vinylidene fluoride) (PVDF)-based blend membrane. The dissolved poly (styrene-co-maleic anhydride) (SMA) in diluent prevents the crystallization of PVDF during the cooling process and deposites on the established PVDF matrix in the later extraction. Compared with traditional coating technique, this one-step TIPS-NIPS method can not only fabricate a supporting layer with an interconnected network structure even via solid-liquid phase separation of TIPS, but also form a uniform SMA skin layer approximately as thin as 200 nm via surface deposition of NIPS. Besides the better hydrophilicity, what's interesting is that the BSA rejection ratio increases from 48% to 94% with the increase of SMA, which indicates that the separation performance has improved. This strategy can be conveniently extended to the creation of firmly thin layer, surface functionalization and structure controllability of the membrane.

Direct NMR Monitoring of Phase Separation Behavior of Highly Supersaturated Nifedipine Solution Stabilized with Hypromellose Derivatives.

PubMed

Ueda, Keisuke; Higashi, Kenjirou; Moribe, Kunikazu

2017-07-03

We investigated the phase separation behavior and maintenance mechanism of the supersaturated state of poorly water-soluble nifedipine (NIF) in hypromellose (HPMC) derivative solutions. Highly supersaturated NIF formed NIF-rich nanodroplets through phase separation from aqueous solution containing HPMC derivative. Dissolvable NIF concentration in the bulk water phase was limited by the phase separation of NIF from the aqueous solution. HPMC derivatives stabilized the NIF-rich nanodroplets and maintained the NIF supersaturation with phase-separated NIF for several hours. The size of the NIF-rich phase was different depending on the HPMC derivatives dissolved in aqueous solution, although the droplet size had no correlation with the time for which NIF supersaturation was maintained without NIF crystallization. HPMC acetate and HPMC acetate succinate (HPMC-AS) effectively maintained the NIF supersaturation containing phase-separated NIF compared with HPMC. Furthermore, HPMC-AS stabilized NIF supersaturation more effectively in acidic conditions. Solution 1 H NMR measurements of NIF-supersaturated solution revealed that HPMC derivatives distributed into the NIF-rich phase during the phase separation of NIF from the aqueous solution. The hydrophobicity of HPMC derivative strongly affected its distribution into the NIF-rich phase. Moreover, the distribution of HPMC-AS into the NIF-rich phase was promoted at lower pH due to the lower aqueous solubility of HPMC-AS. The distribution of a large amount of HPMC derivatives into NIF-rich phase induced the strong inhibition of NIF crystallization from the NIF-rich phase. Polymer distribution into the drug-rich phase directly monitored by solution NMR technique can be a useful index for the stabilization efficiency of drug-supersaturated solution containing a drug-rich phase.

Antibody enhancement of free-flow electrophoresis

NASA Technical Reports Server (NTRS)

Cohly, H. H. P.; Morrison, Dennis R.; Atassi, M. Zouhair

1988-01-01

Specific T cell clones and antibodies (ABs) were developed to study the efficiency of purifying closely associated T cells using Continuous Flow Electrophoresis System. Enhanced separation is accomplished by tagging cells first with ABs directed against the antigenic determinants on the cell surface and then with ABs against the Fc portion of the first AB. This second AB protrudes sufficiently beyond the cell membrane and glycocalyx to become the major overall cell surface potential determinant and thus causes a reduction of electrophoretic mobility. This project was divided into three phases. Phase one included development of specific T cell clones and separation of these specific clones. Phase two extends these principles to the separation of T cells from spleen cells and immunized lymph node cells. Phase three applies this double antibody technique to the separation of T cytotoxic cells from bone marrow.

Separation of Poly(styrene-block-t-butyl methacrylate) Copolymers by Various Liquid Chromatography Techniques

PubMed Central

Šmigovec Ljubič, Tina; Pahovnik, David; Žigon, Majda; Žagar, Ema

2012-01-01

The separation of a mixture of three poly(styrene-block-t-butyl methacrylate) copolymers (PS-b-PtBMA), consisting of polystyrene (PS) blocks of similar length and t-butyl methacrylate (PtBMA) blocks of different lengths, was performed using various chromatographic techniques, that is, a gradient liquid chromatography on reversed-phase (C18 and C8) and normal-phase columns, a liquid chromatography under critical conditions for polystyrene as well as a fully automated two-dimensional liquid chromatography that separates block copolymers by chemical composition in the first dimension and by molar mass in the second dimension. The results show that a partial separation of the mixture of PS-b-PtBMA copolymers can be achieved only by gradient liquid chromatography on reversed-phase columns. The coelution of the two block copolymers is ascribed to a much shorter PtBMA block length, compared to the PS block, as well as a small difference in the length of the PtBMA block in two of these copolymers, which was confirmed by SEC-MALS and NMR spectroscopy. PMID:22489207

Cell separation in immunoaffinity partition in aqueous polymer two-phase systems

NASA Technical Reports Server (NTRS)

Karr, Laurel J.; Van Alstine, James M.; Snyder, Robert S.; Shafer, Steven G.; Harris, J. Milton

1989-01-01

Two methods for immunoaffinity partitioning are described. One technique involves the covalent coupling of poly (ethylene glycol) (PEG) to immunoglobulin G antibody preparations. In the second method PEG-modified Protein A is used to complex with cells and unmodified antibody. The effects of PEG molecular weight, the degree of modification, and varying phase system composition on antibody activity and its affinity for the upper phase are studied. It is observed that both methods resulted in effective cell separation.

Molecular beam epitaxy growth and magnetic properties of Cr-Co-Ga Heusler alloy films

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

Feng, Wuwei, E-mail: wfeng@cugb.edu.cn; Wang, Weihua; Zhao, Chenglong

2015-11-15

We have re-investigated growth and magnetic properties of Cr{sub 2}CoGa films using molecular beam epitaxy technique. Phase separation and precipitate formation were observed experimentally again in agreement with observation of multiple phases separation in sputtered Cr{sub 2}CoGa films by M. Meinert et al. However, significant phase separation could be suppressed by proper control of growth conditions. We showed that Cr{sub 2}CoGa Heusler phase, rather than Co{sub 2}CrGa phase, constitutes the majority of the sample grown on GaAs(001) at 450 {sup o}C. The measured small spin moment of Cr{sub 2}CoGa is in agreement with predicted HM-FCF nature; however, its Curie temperaturemore » is not as high as expected from the theoretical prediction probably due to the off-stoichiometry of Cr{sub 2}CoGa and the existence of the disorders and phase separation.« less

Chromatographic peak deconvolution of constitutional isomers by multiple-reaction-monitoring mass spectrometry.

PubMed

Trapp, Oliver

2010-02-12

Highly efficient and sophisticated separation techniques are available to analyze complex compound mixtures with superior sensitivities and selectivities often enhanced by a 2nd dimension, e.g. a separation technique or spectroscopic and spectrometric techniques. For enantioselective separations numerous chiral stationary phases (CSPs) exist to cover a broad range of chiral compounds. Despite these advances enantioselective separations can become very challenging for mixtures of stereolabile constitutional isomers, because the on-column interconversion can lead to completely overlapping peak profiles. Typically, multidimensional separation techniques, e.g. multidimensional GC (MDGC), using an achiral 1st separation dimension and transferring selected analytes to a chiral 2nd separation are the method of choice to approach such problems. However, this procedure is very time consuming and only predefined sections of peaks can be transferred by column switching to the second dimension. Here we demonstrate for stereolabile 1,2-dialkylated diaziridines a technique to experimentally deconvolute overlapping gas chromatographic elution profiles of constitutional isomers based on multiple-reaction-monitoring MS (MRM-MS). The here presented technique takes advantage of different fragmentation probabilities and pathways to isolate the elution profile of configurational isomers. Copyright 2009 Elsevier B.V. All rights reserved.

Supercritical fluid chromatographic resolution of water soluble isomeric carboxyl/amine terminated peptides facilitated via mobile phase water and ion pair formation.

PubMed

Patel, M A; Riley, F; Ashraf-Khorassani, M; Taylor, L T

2012-04-13

Both analytical scale and preparative scale packed column supercritical fluid chromatography (SFC) have found widespread applicability for chiral separations of multiple polar pharmaceutical candidates. However, SFC is rapidly becoming an achiral technique. More specifically, ion pair SFC is finding greater utility for separation of ionic analytes such as amine salts and organic sulfonates. The key to this success is, in part, the incorporation of additives such as trifluoroacetic acid and ammonium acetate into the mobile phase in association with a wide variety of both bonded silica stationary phases and high purity bare silica. Ion pairing SFC coupled with evaporative light scattering detection and mass spectrometric detection is presented here for the separation of water soluble, uncapped, isomeric peptide pairs that differ in amino acid arrangement. The separation is best achieved on either diol-bonded silica or bare silica with 1-5% (w/w) water as a significant ingredient in the mobile phase. Nitrogenous stationary phases such as 2-ethylpyridine, which had been very successful for the separation of capped peptides failed to yield the desired separation regardless of the mobile phase composition. A HILIC type retention mechanism is postulated for the separation of both isomeric uncapped peptide pairs. Copyright © 2012 Elsevier B.V. All rights reserved.

Vacancy-mediated fcc/bcc phase separation in Fe1 -xNix ultrathin films

NASA Astrophysics Data System (ADS)

Menteş, T. O.; Stojić, N.; Vescovo, E.; Ablett, J. M.; Niño, M. A.; Locatelli, A.

2016-08-01

The phase separation occurring in Fe-Ni thin films near the Invar composition is studied by using high-resolution spectromicroscopy techniques and density functional theory calculations. Annealed at temperatures around 300 ∘C ,Fe0.70Ni0.30 films on W(110) break into micron-sized bcc and fcc domains with compositions in agreement with the bulk Fe-Ni phase diagram. Ni is found to be the diffusing species in forming the chemical heterogeneity. The experimentally determined energy barrier of 1.59 ±0.09 eV is identified as the vacancy formation energy via density functional theory calculations. Thus, the principal role of the surface in the phase separation process is attributed to vacancy creation without interstitials.

Facile preparation of an alternating copolymer-based high molecular shape-selective organic phase for reversed-phase liquid chromatography.

PubMed

Mallik, Abul K; Noguchi, Hiroki; Rahman, Mohammed Mizanur; Takafuji, Makoto; Ihara, Hirotaka

2018-06-22

The synthesis of a new alternating copolymer-grafted silica phase is described for the separation of shape-constrained isomers of polycyclic aromatic hydrocarbons (PAHs) and tocopherols in reversed-phase high-performance liquid chromatography (RP-HPLC). Telomerization of the monomers (octadecyl acrylate and N-methylmaleimide) was carried out with a silane coupling agent; 3-mercaptopropyltrimethoxysilane (MPS), and the telomer (T) was grafted onto porous silica surface to prepare the alternating copolymer-grafted silica phase (Sil-alt-T). The new hybrid material was characterized by elemental analyses, diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy, and solid-state 13 C and 29 Si cross-polarization magic-angle spinning (CP/MAS) NMR spectroscopy. The results of 13 C CP/MAS NMR demonstrated that the alkyl chains of the grafted polymers in Sil-alt-T remained disordered, amorphous, and mobile represented by gauche conformational form. Separation abilities and molecular-shape selectivities of the prepared organic phase were evaluated by the separation of PAHs isomers and Standard Reference Material 869b, Column Selectivity Test Mixture for Liquid Chromatography, respectively and compared with commercially available octadecylsilylated silica (ODS) and C 30 columns as well as previously reported alternating copolymer-based column. The effectiveness of this phase is also demonstrated by the separation of tocopherol isomers. Oriented functional groups along the polymer main chains and cavity formations are investigated to be the driving force for better separation with multiple-interactions with the solutes. One of the advantages of the Sil-alt-T phase to that of the previously reported phase is the synthesis of the telomer first and then immobilized onto silica surface. In this case, the telomer was characterized easily with simple spectroscopic techniques and the molecular mass and polydispersity index of the telomer were determined by size exclusion chromatography (SEC) before grafting onto silica surface. Moreover, both of the monomers were commercially available. Therefore, the technique of preparation was very facile and better separation was achieved with the Sil-alt-T phase compared to the ODS, C 30 and other previously reported alternating copolymer-based columns. Copyright © 2018 Elsevier B.V. All rights reserved.

Liquid-liquid phase separation in aerosol particles: Imaging at the Nanometer Scale

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

O'Brien, Rachel; Wang, Bingbing; Kelly, Stephen T.

2015-04-21

Atmospheric aerosols can undergo phase transitions including liquid-liquid phase separation (LLPS) while responding to changes in the ambient relative humidity (RH). Here, we report results of chemical imaging experiments using environmental scanning electron microscopy (ESEM) and scanning transmission x-ray microscopy (STXM) to investigate the LLPS of micron sized particles undergoing a full hydration-dehydration cycle. Internally mixed particles composed of ammonium sulfate (AS) and either: limonene secondary organic carbon (LSOC), a, 4-dihydroxy-3-methoxybenzeneaceticacid (HMMA), or polyethylene glycol (PEG-400) were studied. Events of LLPS with apparent core-shell particle morphology were observed for all samples with both techniques. Chemical imaging with STXM showed thatmore » both LSOC/AS and HMMA/AS particles were never homogeneously mixed for all measured RH’s above the deliquescence point and that the majority of the organic component was located in the shell. The shell composition was estimated as 65:35 organic: inorganic in LSOC/AS and as 50:50 organic: inorganic for HMMA/AS. PEG-400/AS particles showed fully homogeneous mixtures at high RH and phase separated below 89-92% RH with an estimated 50:50% organic to inorganic mix in the shell. These two chemical imaging techniques are well suited for in-situ analysis of the hygroscopic behavior, phase separation, and surface composition of collected ambient aerosol particles.« less

Understanding the Impact of Water on the Miscibility and Microstructure of Amorphous Solid Dispersions: An AFM-LCR and TEM-EDX Study.

PubMed

Li, Na; Gilpin, Christopher J; Taylor, Lynne S

2017-05-01

Miscibility is critical for amorphous solid dispersions (ASDs). Phase-separated ASDs are more prone to crystallization, and thus can lose their solubility advantage leading to product failure. Additionally, dissolution performance can be diminished as a result of phase separation in the ASD matrix. Water is known to induce phase separation during storage for some ASDs. However, the impact of water introduced during preparation has not been as thoroughly investigated to date. The purpose of this study was to develop a mechanistic understanding of the effect of water on the phase behavior and microstructure of ASDs. Evacetrapib and two polymers were selected as the model system. Atomic force microscopy coupled with Lorentz contact resonance, and transmission electron microscopy with energy dispersive X-ray spectroscopy were employed to evaluate the microstructure and composition of phase-separated ASDs. It was found that phase separation could be induced via two routes: solution-state phase separation during ASD formation caused by water absorption during film formation by a hydrophilic solvent, or solid-phase separation following exposure to high RH during storage. Water contents of as low as 2% in the organic solvent system used to dissolve the drug and polymer were found to result in phase separation in the resultant ASD film. These findings have profound implications on lab-scale ASD preparation and potentially also for industrial production. Additionally, these high-resolution imaging techniques combined with orthogonal analyses are powerful tools to visualize structural changes in ASDs, which in turn will enable better links to be made between ASD structure and performance.

Quantitative phase imaging using four interferograms with special phase shifts by dual-wavelength in-line phase-shifting interferometry

NASA Astrophysics Data System (ADS)

Xu, Xiaoqing; Wang, Yawei; Ji, Ying; Xu, Yuanyuan; Xie, Ming; Han, Hao

2018-05-01

A new approach of quantitative phase imaging using four interferograms with special phase shifts in dual-wavelength in-line phase-shifting interferometry is presented. In this method, positive negative 2π phase shifts are employed to easily separate the incoherent addition of two single-wavelength interferograms by combining the phase-shifting technique with the subtraction procedure, then the quantitative phase at one of both wavelengths can be achieved based on two intensities without the corresponding dc terms by the use of the character of the trigonometric function. The quantitative phase of the other wavelength can be retrieved from two dc-term suppressed intensities obtained by employing the two-step phase-shifting technique or the filtering technique in the frequency domain. The proposed method is illustrated with theory, and its effectiveness is demonstrated by simulation experiments of the spherical cap and the HeLa cell, respectively.

Phase separation kinetics in immiscible liquids

NASA Technical Reports Server (NTRS)

Ng, Lee H.; Sadoway, Donald R.

1987-01-01

The kinetics of phase separation in the succinonitrile-water system are being investigated. Experiments involve initial physical mixing of the two immiscible liquids at a temperature above the consolute, decreasing the temperature into the miscibility gap, followed by iamging of the resultant microstructure as it evolves with time. Refractive index differences allow documentation of the changing microstructures by noninvasive optical techniques without the need to quench the liquid structures for analysis.

Phase separation kinetics in immiscible liquids

NASA Technical Reports Server (NTRS)

Sadoway, D. R.

1986-01-01

The kinetics of phase separation in the succinonitrile-water system are being investigated. Experiments involve initial physical mixing of the two immiscible liquids at a temperature above the consolute, decreasing the temperature into the miscibility gap, followed by imaging of the resultant microstructure as it evolves with time. Refractive index differences allow documentation of the changing microstructures by noninvasive optical techniques without the need to quench the liquid structures for analysis.

Characterization of nanoscale spatial distribution of small molecules in amorphous polymer matrices

NASA Astrophysics Data System (ADS)

Ricarte, Ralm; Hillmyer, Marc; Lodge, Timothy

Hydroxypropyl methylcellulose acetate succinate (HPMCAS) can significantly enhance the efficacy of active pharmaceutical ingredients (APIs). Yet, the interactions between species in HPMCAS-API blends are not understood. Elucidating these interactions is difficult because the spatial distributions of HPMCAS and API in the blends are ambiguous; the polymer and drug may be molecularly mixed or the species may form phase separated domains. As these phase separated domains may be less than 100 nm in size, traditional characterization techniques may not accurately evaluate the spatial distribution. To address this challenge, we explore the use of electron energy-loss spectroscopy (EELS) for detecting the model API phenytoin in an HPMCAS-phenytoin blend. Using EELS, we directly measured with high accuracy and precision the phenytoin concentrations in several blends. We present evidence that suggests phase separation occurs in blends that have a phenytoin loading of approximately 50 wt percent. Finally, we demonstrate that this technique achieves a sub-100 nm spatial resolution and can detect several other APIs.

Sample selection and testing of separation processes

NASA Technical Reports Server (NTRS)

Karr, L. J.

1985-01-01

Phase partitioning, which has become an important tool for the separation and purification of biological materials, was studied. Instruments available for this technique were researched and a countercurrent distribution apparatus, the Biosheff MK2N, was purchased. Various proteins, polysaccharides and cells were studied as models to determine operating procedures and conditions for this piece of equipment. Results were compared with those obtained from other similar equipment, including a nonsynchronous coil planet centrifuge device. Additionally, work was done with affinity ligands attached to PEG, which can further enhance the separation capabilities of phase partitioning.

Development and characterization of polyethersulfone/TiO2 mixed matrix membranes for CO2/CH4 separation

NASA Astrophysics Data System (ADS)

Galaleldin, S.; Mannan, H. A.; Mukhtar, H.

2017-12-01

In this study, mixed matrix membranes comprised of polyethersulfone as the bulk polymer phase and titanium dioxide (TiO2) nanoparticles as the inorganic discontinuous phase were prepared for CO2/CH4 separation. Membranes were synthesized at filler loading of 0, 5, 10 and 15 wt % via dry phase inversion method. Morphology, chemical bonding and thermal characteristics of membranes were scrutinized utilizing different techniques, namely: Field Emission Scanning Electron Microscopy (FESEM), Fourier Transform InfraRed (FTIR) spectra and Thermogravimetric analysis (TGA) respectively. Membranes gas separation performance was evaluated for CO2 and CH4 gases at 4 bar feed pressure. The highest separation performance was achieved by mixed matrix membrane (MMM) at 5 % loading of TiO2.

Evaluation of comprehensive multidimensional separations using reversed-phase, reversed-phase liquid chromatography/mass spectrometry for shotgun proteomics.

PubMed

Nakamura, Tatsuji; Kuromitsu, Junro; Oda, Yoshiya

2008-03-01

Two-dimensional liquid-chromatographic (LC) separation followed by mass spectrometric (MS) analysis was examined for the identification of peptides in complex mixtures as an alternative to widely used two-dimensional gel electrophoresis followed by MS analysis for use in proteomics. The present method involves the off-line coupling of a narrow-bore, polymer-based, reversed-phase column using an acetonitrile gradient in an alkaline mobile phase in the first dimension with octadecylsilanized silica (ODS)-based nano-LC/MS in the second dimension. After the first separation, successive fractions were acidified and dried off-line, then loaded on the second dimension column. Both columns separate peptides according to hydrophobicity under different pH conditions, but more peptides were identified than with the conventional technique for shotgun proteomics, that is, the combination of a strong cation exchange column with an ODS column, and the system was robust because no salts were included in the mobile phases. The suitability of the method for proteomics measurements was evaluated.

Demulsification of water/oil/solid emulsions by hollow-fiber membranes

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

Tirmizi, N.P.; Raghuraman, B.; Wiencek, J.

1996-05-01

The demulsification techniques investigated use preferential surface wetting to allow separation of oil and water phases in ultrafiltration and microfiltration membranes. A hydrophobic membrane allows the permeation of an oil phase at almost zero pressure and retains the water phase, even though the molecular weight of the water molecule (18) is much smaller than that of the oil molecule (198 for tetradecane, used in this study). Hydrophobic membranes having pore sizes from 0.02 to 0.2 {micro}m were tested for demulsification of water-in-oil emulsions and water/oil/solid mixtures. The dispersed (aqueous)-phase drop sizes ranged from 1 to 5 {micro}m. High separation rates,more » as well as good permeate quality, were obtained with microfiltration membranes. Water content of permeating oil was 32--830 ppm depending on operating conditions and interfacial properties. For emulsions with high surfactant content, simultaneous operation of a hydrophobic and hydrophilic membrane, or simultaneous membrane separation with electric demulsification was more efficient in obtaining complete phase separation.« less

A novel technique for phase synchrony measurement from the complex motor imaginary potential of combined body and limb action

NASA Astrophysics Data System (ADS)

Zhou, Zhong-xing; Wan, Bai-kun; Ming, Dong; Qi, Hong-zhi

2010-08-01

In this study, we proposed and evaluated the use of the empirical mode decomposition (EMD) technique combined with phase synchronization analysis to investigate the human brain synchrony of the supplementary motor area (SMA) and primary motor area (M1) during complex motor imagination of combined body and limb action. We separated the EEG data of the SMA and M1 into intrinsic mode functions (IMFs) using the EMD method and determined the characteristic IMFs by power spectral density (PSD) analysis. Thereafter, the instantaneous phases of the characteristic IMFs were obtained by the Hilbert transformation, and the single-trial phase-locking value (PLV) features for brain synchrony measurement between the SMA and M1 were investigated separately. The classification performance suggests that the proposed approach is effective for phase synchronization analysis and is promising for the application of a brain-computer interface in motor nerve reconstruction of the lower limbs.

Combination of Complex-Based and Magnitude-Based Multiecho Water-Fat Separation for Accurate Quantification of Fat-Fraction

PubMed Central

Yu, Huanzhou; Shimakawa, Ann; Hines, Catherine D. G.; McKenzie, Charles A.; Hamilton, Gavin; Sirlin, Claude B.; Brittain, Jean H.; Reeder, Scott B.

2011-01-01

Multipoint water–fat separation techniques rely on different water–fat phase shifts generated at multiple echo times to decompose water and fat. Therefore, these methods require complex source images and allow unambiguous separation of water and fat signals. However, complex-based water–fat separation methods are sensitive to phase errors in the source images, which may lead to clinically important errors. An alternative approach to quantify fat is through “magnitude-based” methods that acquire multiecho magnitude images. Magnitude-based methods are insensitive to phase errors, but cannot estimate fat-fraction greater than 50%. In this work, we introduce a water–fat separation approach that combines the strengths of both complex and magnitude reconstruction algorithms. A magnitude-based reconstruction is applied after complex-based water–fat separation to removes the effect of phase errors. The results from the two reconstructions are then combined. We demonstrate that using this hybrid method, 0–100% fat-fraction can be estimated with improved accuracy at low fat-fractions. PMID:21695724

Evidence of a miscibility gap in the FeTe1-xSex polycrystalline samples prepared with a melting process

NASA Astrophysics Data System (ADS)

Sala, A.; Palenzona, A.; Bernini, C.; Caglieris, F.; Cimberle, M. R.; Ferdeghini, C.; Lamura, G.; Martinelli, A.; Pani, M.; Hecher, J.; Eisterer, M.; Putti, M.

2014-05-01

The study of overdoped FeTe1-xSex (0.5 < x < 1) polycrystalline superconductor samples is reported. The samples were prepared using a melting technique previously developed by our group. Increasing the Se content a phase separation related to the formation of FeSe inside the Fe(Se,Te) phase happens, as demonstrated by structural analysis and magnetic characterization. The proposed phase separation picture is likely the fingerprint of a miscibility gap in the Fe(Se,Te) system.

All-optical phase discrimination using SOA.

PubMed

Power, Mark J; Webb, Roderick P; Manning, Robert J

2013-11-04

We describe the first experimental demonstration of a novel all-optical phase discrimination technique, which can separate the two orthogonal phase components of a signal onto different frequencies. This method exploits nonlinear mixing in a semiconductor optical amplifier (SOA) to separate a 10.65 Gbaud QPSK signal into two 10.65 Gb/s BPSK signals which are then demodulated using a delay interferometer (DI). Eye diagrams and spectral measurements verify correct operation and a conversion efficiency greater than 9 dB is observed on both output BPSK channels when compared with the input QPSK signal.

Fluid flow in solidifying monotectic alloys

NASA Technical Reports Server (NTRS)

Ecker, A.; Frazier, D. O.; Alexander, J. Iwan D.

1989-01-01

Use of a two-wavelength holographic technique results in a simultaneous determination of temperature and composition profiles during directional solidification in a system with a miscibility gap. The relationships among fluid flow, phase separation, and mass transport during the solidification of the monotectic alloy are discussed. The primary sources of fluid motion in this system are buoyancy and thermocapillary forces. These forces act together when phase separation results in the formation of droplets (this occurs at the solid-liquid interface and in the bulk melt). In the absence of phase separation, buoyancy results from density gradients related to temperature and compositional gradients in the single-phase bulk melt. The effects of buoyancy are especially evident in association with water- or ethanol-rich volumes created at the solid-liquid growth interface.

New polymers for low-gravity purification of cells by phase partitioning

NASA Technical Reports Server (NTRS)

Harris, J. M.

1983-01-01

A potentially powerful technique for separating different biological cell types is based on the partitioning of these cells between the immiscible aqueous phases formed by solution of certain polymers in water. This process is gravity-limited because cells sediment rather than associate with the phase most favored on the basis of cell-phase interactions. In the present contract we have been involved in the synthesis of new polymers both to aid in understanding the partitioning process and to improve the quality of separations. The prime driving force behind the design of these polymers is to produce materials which will aid in space experiments to separate important cell types and to study the partitioning process in the absence of gravity (i.e., in an equilibrium state).

Cell Partition in Two Polymer Aqueous Phases

NASA Technical Reports Server (NTRS)

Harris, J. M.

1985-01-01

Partition of biological cells in two phase aqueous polymer systems is recognized as a powerful separation technique which is limited by gravity. The synthesis of new, selective polymer ligand conjugates to be used in affinity partition separations is of interest. The two most commonly used polymers in two phase partitioning are dextran and polyethylene glycol. A thorough review of the chemistry of these polymers was begun, particularly in the area of protein attachment. Preliminary studies indicate the importance in affinity partitioning of minimizing gravity induced randomizing forces in the phase separation process. The PEG-protein conjugates that were prepared appear to be ideally suited for achieving high quality purifications in a microgravity environment. An interesting spin-off of this synthetic work was the observation of catalytic activity for certain of our polymer derivatives.

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.

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.

Recent advances in liquid-phase separations for clinical metabolomics.

PubMed

Kohler, Isabelle; Giera, Martin

2017-01-01

Over the last decades, several technological improvements have been achieved in liquid-based separation techniques, notably, with the advent of fully porous sub-2 μm particles and superficially porous sub-3 μm particles, the comeback of supercritical fluid chromatography, and the development of alternative chromatographic modes such as hydrophilic interaction chromatography. Combined with mass spectrometry, these techniques have demonstrated their added value, substantially increasing separation efficiency, selectivity, and speed of analysis. These benefits are essential in modern clinical metabolomics typically involving the study of large-scale sample cohorts and the analysis of thousands of metabolites showing extensive differences in physicochemical properties. This review presents a brief overview of the recent developments in liquid-phase separation sciences in the context of clinical metabolomics, focusing on increased throughput as well as metabolite coverage. Relevant metabolomics applications highlighting the benefits of ultra-high performance liquid chromatography, core-shell technology, high-temperature liquid chromatography, capillary electrophoresis, supercritical fluid chromatography, and hydrophilic interaction chromatography are discussed. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of ambroxol hydrochloride, methylparaben and benzoic acid in pharmaceutical preparations based on sequential injection technique coupled with monolithic column.

PubMed

Satínský, Dalibor; Huclová, Jitka; Ferreira, Raquel L C; Montenegro, Maria Conceição B S M; Solich, Petr

2006-02-13

The porous monolithic columns show high performance at relatively low pressure. The coupling of short monoliths with sequential injection technique (SIA) results in a new approach to implementation of separation step to non-separation low-pressure method. In this contribution, a new separation method for simultaneous determination of ambroxol, methylparaben and benzoic acid was developed based on a novel reversed-phase sequential injection chromatography (SIC) technique with UV detection. A Chromolith SpeedROD RP-18e, 50-4.6 mm column with 10 mm precolumn and a FIAlab 3000 system with a six-port selection valve and 5 ml syringe were used for sequential injection chromatographic separations in our study. The mobile phase used was acetonitrile-tetrahydrofuran-0.05M acetic acid (10:10:90, v/v/v), pH 3.75 adjusted with triethylamine, flow rate 0.48 mlmin(-1), UV-detection was at 245 nm. The analysis time was <11 min. A new SIC method was validated and compared with HPLC. The method was found to be useful for the routine analysis of the active compounds ambroxol and preservatives (methylparaben or benzoic acid) in various pharmaceutical syrups and drops.

Fabricating fiber Bragg gratings with two phase masks based on reconstruction-equivalent-chirp technique.

PubMed

Gao, Liang; Chen, Xiangfei; Xiong, Jintian; Liu, Shengchun; Pu, Tao

2012-01-30

Based on reconstruction-equivalent-chirp (REC) technique, a novel solution for fabricating low-cost long fiber Bragg gratings (FBGs) with desired properties is proposed and initially studied. A proof-of-concept experiment is demonstrated with two conventional uniform phase masks and a submicron-precision translation stage, successfully. It is shown that the original phase shift (OPS) caused by phase mismatch of the two phase masks can be compensated by the equivalent phase shift (EPS) at the ±1st channels of sampled FBGs, separately. Furthermore, as an example, a π phase-shifted FBG of about 90 mm is fabricated by using these two 50mm-long uniform phase masks based on the presented method.

Nanopatterns by phase separation of patterned mixed polymer monolayers

DOEpatents

Huber, Dale L; Frischknecht, Amalie

2014-02-18

Micron-size and sub-micron-size patterns on a substrate can direct the self-assembly of surface-bonded mixed polymer brushes to create nanoscale patterns in the phase-separated mixed polymer brush. The larger scale features, or patterns, can be defined by a variety of lithographic techniques, as well as other physical and chemical processes including but not limited to etching, grinding, and polishing. The polymer brushes preferably comprise vinyl polymers, such as polystyrene and poly(methyl methacrylate).

Phase sensitive optical coherence microscopy for photothermal imaging of gold nanorods

NASA Astrophysics Data System (ADS)

Hu, Yong; Podoleanu, Adrian G.; Dobre, George

2018-03-01

We describe a swept source based phase sensitive optical coherence microscopy (OCM) system for photothermal imaging of gold nanorods (GNR). The phase sensitive OCM system employed in the study has a displacement sensitivity of 0.17 nm to vibrations at single frequencies below 250 Hz. We demonstrate the generation of phase maps and confocal phase images. By displaying the difference between successive confocal phase images, we perform the confocal photothermal imaging of accumulated GNRs behind a glass coverslip and behind the scattering media separately. Compared with two-photon luminescence (TPL) detection techniques reported in literature, the technique in this study has the advantage of a simplified experimental setup and provides a more efficient method for imaging the aggregation of GNR. However, the repeatability performance of this technique suffers due to jitter noise from the swept laser source.

SFC-MS/MS as an orthogonal technique for improved screening of polar analytes in anti-doping control.

PubMed

Parr, Maria Kristina; Wuest, Bernhard; Naegele, Edgar; Joseph, Jan F; Wenzel, Maxi; Schmidt, Alexander H; Stanic, Mijo; de la Torre, Xavier; Botrè, Francesco

2016-09-01

HPLC is considered the method of choice for the separation of various classes of drugs. However, some analytes are still challenging as HPLC shows limited resolution capabilities for highly polar analytes as they interact insufficiently on conventional reversed-phase (RP) columns. Especially in combination with mass spectrometric detection, limitations apply for alterations of stationary phases. Some highly polar sympathomimetic drugs and their metabolites showed almost no retention on different RP columns. Their retention remains poor even on phenylhexyl phases that show different selectivity due to π-π interactions. Supercritical fluid chromatography (SFC) as an orthogonal separation technique to HPLC may help to overcome these issues. Selected polar drugs and metabolites were analyzed utilizing SFC separation. All compounds showed sharp peaks and good retention even for the very polar analytes, such as sulfoconjugates. Retention times and elution orders in SFC are different to both RP and HILIC separations as a result of the orthogonality. Short cycle times could be realized. As temperature and pressure strongly influence the polarity of supercritical fluids, precise regulation of temperature and backpressure is required for the stability of the retention times. As CO2 is the main constituent of the mobile phase in SFC, solvent consumption and solvent waste are considerably reduced. Graphical Abstract SFC-MS/MS vs. LC-MS/MS.

Superconductivity, phase separation, and charge-transfer instability in the U = infinity limit of the three-band model of the CuO sub 2 planes

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

Grilli, M.; Raimondi, R.; Castellani, C.

1991-07-08

The {ital U}={infinity} limit of the three-band Hubbard model with nearest-neighbor repulsion {ital V} is studied using the slave-boson approach and the large-{ital N} expansion technique to order 1/{ital N}. A charge-transfer instability is found as in weak-coupling theory. The charge-transfer instability is always associated with a diverging compressibility leading to a phase separation. Near the phase-separation, charge-transfer-instability region we find superconducting instabilities in the {ital s}- and {ital d}-wave channel. The requirement for superconductivity is that {ital V} be on the scale of the Cu-O hopping as suggested by Varma, Schmitt-Rink, and Abrahams.

Demodulation techniques for the amplitude modulated laser imager

NASA Astrophysics Data System (ADS)

Mullen, Linda; Laux, Alan; Cochenour, Brandon; Zege, Eleonora P.; Katsev, Iosif L.; Prikhach, Alexander S.

2007-10-01

A new technique has been found that uses in-phase and quadrature phase (I/Q) demodulation to optimize the images produced with an amplitude-modulated laser imaging system. An I/Q demodulator was used to collect the I/Q components of the received modulation envelope. It was discovered that by adjusting the local oscillator phase and the modulation frequency, the backscatter and target signals can be analyzed separately via the I/Q components. This new approach enhances image contrast beyond what was achieved with a previous design that processed only the composite magnitude information.

[Total analysis of organic rubber additives].

PubMed

He, Wen-Xuan; Robert, Shanks; You, Ye-Ming

2010-03-01

In the present paper, after middle pressure chromatograph separation using both positive phase and reversed-phase conditions, the organic additives in ethylene-propylene rubber were identified by infrared spectrometer. At the same time, by using solid phase extraction column to maintain the main component-fuel oil in organic additves to avoid its interfering with minor compounds, other organic additves were separated and analysed by GC/Ms. In addition, the remaining active compound such as benzoyl peroxide was identified by CC/Ms, through analyzing acetone extract directly. Using the above mentioned techniques, soften agents (fuel oil, plant oil and phthalte), curing agent (benzoylperoxide), vulcanizing accelerators (2-mercaptobenzothiazole, ethyl thiuram and butyl thiuram), and antiagers (2, 6-Di-tert-butyl-4-methyl phenol and styrenated phenol) in ethylene-propylene rubber were identified. Although the technique was established in ethylene-propylene rubber system, it can be used in other rubber system.

Vibration energy harvesting with polyphase AC transducers

NASA Astrophysics Data System (ADS)

McCullagh, James J.; Scruggs, Jeffrey T.; Asai, Takehiko

2016-04-01

Three-phase transduction affords certain advantages in the efficient electromechanical conversion of energy, especially at higher power scales. This paper considers the use of a three-phase electric machine for harvesting energy from vibrations. We consider the use of vector control techniques, which are common in the area of industrial electronics, for optimizing the feedback loops in a stochastically-excited energy harvesting system. To do this, we decompose the problem into two separate feedback loops for direct and quadrature current components, and illustrate how each might be separately optimized to maximize power output. In a simple analytical example, we illustrate how these techniques might be used to gain insight into the tradeoffs in the design of the electronic hardware and the choice of bus voltage.

Methods for recovering a solvent from a fluid volume and methods of removing at least one compound from a nonpolar solvent

DOEpatents

Ginosar, Daniel M.; Wendt, Daniel S.; Petkovic, Lucia M.

2014-06-10

A method of removing a nonpolar solvent from a fluid volume that includes at least one nonpolar compound, such as a fat, an oil or a triglyceride, is provided. The method comprises contacting a fluid volume with an expanding gas to expand the nonpolar solvent and form a gas-expanded solvent. The gas-expanded solvent may have a substantially reduced density in comparison to the at least one nonpolar compound and/or a substantially reduced capacity to solubilize the nonpolar compound, causing the nonpolar compounds to separate from the gas-expanded nonpolar solvent into a separate liquid phase. The liquid phase including the at least one nonpolar compound may be separated from the gas-expanded solvent using conventional techniques. After separation of the liquid phase, at least one of the temperature and pressure may be reduced to separate the nonpolar solvent from the expanding gas such that the nonpolar solvent may be recovered and reused.

SELECTIVE TRACE ENRICHMENT BY IMMUNOAFFINITY CAPILLARY ELECTROCHROMATOGRAPHY ON-LINE WITH CAPILLARY ZONE ELECTROPHORESIS - LASER-INDUCED FLUORESCENCE

EPA Science Inventory

Limited by the lack of a sensitive, universal detector, many capillary-based liquid-phase separation techniques might benefit from techniques that overcome modest concentration sensitivity by preconcentrating large injection volumes. The work presented employs selective solid-ph...

Effects of processing parameters in thermally induced phase separation technique on porous architecture of scaffolds for bone tissue engineering.

PubMed

Akbarzadeh, Rosa; Yousefi, Azizeh-Mitra

2014-08-01

Tissue engineering makes use of 3D scaffolds to sustain three-dimensional growth of cells and guide new tissue formation. To meet the multiple requirements for regeneration of biological tissues and organs, a wide range of scaffold fabrication techniques have been developed, aiming to produce porous constructs with the desired pore size range and pore morphology. Among different scaffold fabrication techniques, thermally induced phase separation (TIPS) method has been widely used in recent years because of its potential to produce highly porous scaffolds with interconnected pore morphology. The scaffold architecture can be closely controlled by adjusting the process parameters, including polymer type and concentration, solvent composition, quenching temperature and time, coarsening process, and incorporation of inorganic particles. The objective of this review is to provide information pertaining to the effect of these parameters on the architecture and properties of the scaffolds fabricated by the TIPS technique. © 2014 Wiley Periodicals, Inc.

Model-independent analysis of the Fermilab Tevatron turn-by-turn beam position monitor measurements

NASA Astrophysics Data System (ADS)

Petrenko, A. V.; Valishev, A. A.; Lebedev, V. A.

2011-09-01

Coherent transverse beam oscillations in the Tevatron were analyzed with the model-independent analysis (MIA) technique. This allowed one to obtain the model-independent values of coupled betatron amplitudes, phase advances, and dispersion function around the ring from a single dipole kick measurement. In order to solve the MIA mode mixing problem which limits the accuracy of determination of the optical functions, we have developed a new technique of rotational MIA mode untangling. The basic idea is to treat each beam position monitor (BPM) as two BPMs separated in a ring by exactly one turn. This leads to a simple criterion of MIA mode separation: the betatron phase advance between any BPM and its counterpart shifted by one turn should be equal to the betatron tune and therefore should not depend on the BPM position in the ring. Furthermore, we describe a MIA-based technique to locate vibrating magnets in a storage ring.

An atom probe perspective on phase separation and precipitation in duplex stainless steels

NASA Astrophysics Data System (ADS)

Guo, Wei; Garfinkel, David A.; Tucker, Julie D.; Haley, Daniel; Young, George A.; Poplawsky, Jonathan D.

2016-06-01

Three-dimensional chemical imaging of Fe-Cr alloys showing Fe-rich (α)/Cr-rich (α‧) phase separation is reported using atom probe tomography techniques. The extent of phase separation, i.e., amplitude and wavelength, has been quantitatively assessed using the Langer-Bar-on-Miller, proximity histogram, and autocorrelation function methods for two separate Fe-Cr alloys, designated 2101 and 2205. Although the 2101 alloy possesses a larger wavelength and amplitude after annealing at 427 °C for 100-10 000 h, it exhibits a lower hardness than the 2205 alloy. In addition to this phase separation, ultra-fine Ni-Mn-Si-Cu-rich G-phase precipitates form at the α/α‧ interfaces in both alloys. For the 2101 alloy, Cu clusters act to form a nucleus, around which a Ni-Mn-Si shell develops during the precipitation process. For the 2205 alloy, the Ni and Cu atoms enrich simultaneously and no core-shell chemical distribution was found. This segregation phenomenon may arise from the exact Ni/Cu ratio inside the ferrite. After annealing for 10 000 h, the number density of the G-phase within the 2205 alloy was found to be roughly one order of magnitude higher than in the 2101 alloy. The G-phase precipitates have an additional deleterious effect on the thermal embrittlement, as evaluated by the Ashby-Orowan equation, which explains the discrepancy between the hardness and the rate of phase separation with respect to annealing time (Gladman T 1999 Mater. Sci. Tech. Ser. 15 30-36). ).

An atom probe perspective on phase separation and precipitation in duplex stainless steels

DOE PAGES

Garfinkel, David A.; Tucker, Julie D.; Haley, Daniel A.; ...

2016-05-16

Here, three-dimensional chemical imaging of Fe–Cr alloys showing Fe-rich (α)/Cr-rich (α') phase separation is reported using atom probe tomography techniques. The extent of phase separation, i.e., amplitude and wavelength, has been quantitatively assessed using the Langer-Bar-on-Miller, proximity histogram, and autocorrelation function methods for two separate Fe–Cr alloys, designated 2101 and 2205. Although the 2101 alloy possesses a larger wavelength and amplitude after annealing at 427 °C for 100–10 000 h, it exhibits a lower hardness than the 2205 alloy. In addition to this phase separation, ultra-fine Ni–Mn–Si–Cu-rich G-phase precipitates form at the α/α' interfaces in both alloys. For the 2101more » alloy, Cu clusters act to form a nucleus, around which a Ni–Mn–Si shell develops during the precipitation process. For the 2205 alloy, the Ni and Cu atoms enrich simultaneously and no core–shell chemical distribution was found. This segregation phenomenon may arise from the exact Ni/Cu ratio inside the ferrite. After annealing for 10 000 h, the number density of the G-phase within the 2205 alloy was found to be roughly one order of magnitude higher than in the 2101 alloy. The G-phase precipitates have an additional deleterious effect on the thermal embrittlement, as evaluated by the Ashby–Orowan equation, which explains the discrepancy between the hardness and the rate of phase separation with respect to annealing time (Gladman T 1999 Mater. Sci. Tech. Ser. 15 30–36).« less

Kernel-Phase Interferometry for Super-Resolution Detection of Faint Companions

NASA Astrophysics Data System (ADS)

Factor, Samuel M.; Kraus, Adam L.

2017-01-01

Direct detection of close in companions (exoplanets or binary systems) is notoriously difficult. While coronagraphs and point spread function (PSF) subtraction can be used to reduce contrast and dig out signals of companions under the PSF, there are still significant limitations in separation and contrast. Non-redundant aperture masking (NRM) interferometry can be used to detect companions well inside the PSF of a diffraction limited image, though the mask discards ˜95% of the light gathered by the telescope and thus the technique is severely flux limited. Kernel-phase analysis applies interferometric techniques similar to NRM to a diffraction limited image utilizing the full aperture. Instead of non-redundant closure-phases, kernel-phases are constructed from a grid of points on the full aperture, simulating a redundant interferometer. I have developed my own faint companion detection pipeline which utilizes an Bayesian analysis of kernel-phases. I have used this pipeline to search for new companions in archival images from HST/NICMOS in order to constrain planet and binary formation models at separations inaccessible to previous techniques. Using this method, it is possible to detect a companion well within the classical λ/D Rayleigh diffraction limit using a fraction of the telescope time as NRM. This technique can easily be applied to archival data as no mask is needed and will thus make the detection of close in companions cheap and simple as no additional observations are needed. Since the James Webb Space Telescope (JWST) will be able to perform NRM observations, further development and characterization of kernel-phase analysis will allow efficient use of highly competitive JWST telescope time.

Kernel-Phase Interferometry for Super-Resolution Detection of Faint Companions

NASA Astrophysics Data System (ADS)

Factor, Samuel

2016-10-01

Direct detection of close in companions (binary systems or exoplanets) is notoriously difficult. While chronagraphs and point spread function (PSF) subtraction can be used to reduce contrast and dig out signals of companions under the PSF, there are still significant limitations in separation and contrast. While non-redundant aperture masking (NRM) interferometry can be used to detect companions well inside the PSF of a diffraction limited image, the mask discards 95% of the light gathered by the telescope and thus the technique is severely flux limited. Kernel-phase analysis applies interferometric techniques similar to NRM though utilizing the full aperture. Instead of closure-phases, kernel-phases are constructed from a grid of points on the full aperture, simulating a redundant interferometer. I propose to develop my own faint companion detection pipeline which utilizes an MCMC analysis of kernel-phases. I will search for new companions in archival images from NIC1 and ACS/HRC in order to constrain binary and planet formation models at separations inaccessible to previous techniques. Using this method, it is possible to detect a companion well within the classical l/D Rayleigh diffraction limit using a fraction of the telescope time as NRM. This technique can easily be applied to archival data as no mask is needed and will thus make the detection of close in companions cheap and simple as no additional observations are needed. Since the James Webb Space Telescope (JWST) will be able to perform NRM observations, further development and characterization of kernel-phase analysis will allow efficient use of highly competitive JWST telescope time.

Industrial application of green chromatography--I. Separation and analysis of niacinamide in skincare creams using pure water as the mobile phase.

PubMed

Yang, Yu; Strickland, Zackary; Kapalavavi, Brahmam; Marple, Ronita; Gamsky, Chris

2011-03-15

In this work, chromatographic separation of niacin and niacinamide using pure water as the sole component in the mobile phase has been investigated. The separation and analysis of niacinamide have been optimized using three columns at different temperatures and various flow rates. Our results clearly demonstrate that separation and analysis of niacinamide from skincare products can be achieved using pure water as the eluent at 60°C on a Waters XTerra MS C18 column, a Waters XBridge C18 column, or at 80°C on a Hamilton PRP-1 column. The separation efficiency, quantification quality, and analysis time of this new method are at least comparable with those of the traditional HPLC methods. Compared with traditional HPLC, the major advantage of this newly developed green chromatography technique is the elimination of organic solvents required in the HPLC mobile phase. In addition, the pure water chromatography separations described in this work can be directly applied in industrial plant settings without further modification of the existing HPLC equipment. Copyright © 2011 Elsevier B.V. All rights reserved.

A new solution to emulsion liquid membrane problems by non-Newtonian conversion

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

Skelland, A.H.P.; Meng, X.

1996-02-01

Surfactant-stabilized emulsion liquid membrane processes constitute an emerging separation technology that has repeatedly been shown to be highly suited for such diverse separation processes as metal recovery or removal from dilute aqueous solutions; separations in the food industry; removal of organic bases and acids from water; and separation of hydrocarbons. Emulsion liquid membrane separation processes remain excessively vulnerable to one or more of four major problems. Difficulties lie in developing liquid membranes that combine high levels of both stability and permeability with acceptably low levels of swelling and ease of subsequent demulsification for membrane and solute recovery. This article providesmore » a new technique for simultaneously overcoming the first three problems, while identifying physical indications that the proposed solution may have little adverse effect on the fourth problem (demulsification) and may even alleviate it. Numerous benefits of optimized conversion of the membrane phase into suitable non-Newtonian form are identified, their mechanisms outlined, and experimental verifications provided. These include increased stability, retained (or enhanced) permeability, reduced swelling, increased internal phase volume, and increased stirrer speeds. The highly favorable responsiveness of both aliphatic and aromatic membranes to the new technique is demonstrated.« less

The importance of new processing techniques in tissue engineering

NASA Technical Reports Server (NTRS)

Lu, L.; Mikos, A. G.; McIntire, L. V. (Principal Investigator)

1996-01-01

The use of polymer scaffolds in tissue engineering is reviewed and processing techniques are examined. The discussion of polymer-scaffold processing explains fiber bonding, solvent casting and particulate leaching, membrane lamination, melt molding, polymer/ceramic fiber composite-foam processing, phase separation, and high-pressure processing.

SEPARATION AND CHARACTERIZATION OF TETROL METABOLITES OF BENZO[A]PYRENE-DNA ADDUCTS USING HPLC AND SOLID-MATRIX ROOM TEMPERATURE LUMINESCENCE. (R824100)

EPA Science Inventory

Abstract

Four tetrols of benzo[a]pyrene-DNA adducts were separated using reversed-phase high performance liquid chromatography. Chromatographic fractions containing a given tetrol were readily characterized with solid-matrix room temperature luminescence techniques. So...

Sol-gel technique for the preparation of beta-cyclodextrin derivative stationary phase in open-tubular capillary electrochromatography.

PubMed

Wang, Y; Zeng, Z; Guan, N; Cheng, J

2001-07-01

A novel open-tubular capillary electrochromatography (OT-CEC) column coated with 2,6-dibutyl-beta-cyclodextrin (DB-beta-CD) was prepared using sol-gel technique. In the sol-gel approach, owing to the three-dimensional network of sol-gel and the strong chemical bond between the stationary phase and the surface of capillary columns, good chromatographic characteristics and unique selectivity in separating isomers were shown. We achieved high efficiencies of 5-14 x 10(4) plates/m for the isomeric nitrophenols using the sol-gel-derived DB-beta-CD columns. The migration time reproducibility of the separation of the isomeric nitrophenols was better than 2.2% over five runs and 4.5% from column to column. These sol-gel-coated DB-beta-CD columns have shown improved separations of isomeric aminophenols, isomeric dihydroxybenzenes and isomeric nitrophenols, in comparison with the sol-gel matrix capillary column. The influences of buffer pH and methanol solvent on separation were investigated. The chiral resolution of enantiomers such as ibuprofen and binaphthol was explored primarily.

Highly hydrophilic and nonionic poly(2-vinyloxazoline)-grafted silica: a novel organic phase for high-selectivity hydrophilic interaction chromatography.

PubMed

Mallik, Abul K; Cheah, Wee Keat; Shingo, Kaori; Ejzaki, Aika; Takafuji, Makoto; Ihara, Hirotaka

2014-07-01

A new hydrophilic and nonionic poly(2-vinyloxazoline)-grafted silica (Sil-VOX(n)) phase was synthesized and applied for the separation of nucleosides and nucleobases in hydrophilic interaction chromatography (HILIC). Polymerization and immobilization onto silica were confirmed by using characterization techniques including (1)H NMR spectroscopy, elemental analysis, and diffuse reflectance infrared Fourier transform spectroscopy. The hydrophilicity or wettability of Sil-VOX(n) was observed by measuring the contact angle (59.9°). The chromatographic results were compared with those obtained with a conventional HILIC silica column. The Sil-VOX(n) phase showed much better separation of polar test analytes than the silica column, and the elution order was different. Differences in selectivity between these two columns indicate that the stationary phase cannot function merely as an inert support for a water layer into which the solutes are partitioned from the bulk mobile phase. To elucidate the interaction mechanism, the separation of dihydroxybenzene isomers was performed on both columns in normal-phase liquid chromatography. Sil-VOX(n) was very sensitive to the dipole moments of the positional isomers of polycyclic aromatic compounds in normal-phase liquid chromatography. The interaction mechanism for Sil-VOX(n) in HILIC separation is also described.

Anisotropic imprint of amorphization and phase separation in manganite thin films via laser interference irradiation.

PubMed

Ding, Junfeng; Lin, Zhipeng; Wu, Jianchun; Dong, Zhili; Wu, Tom

2015-02-04

Materials with mesoscopic structural and electronic phase separation, either inherent from synthesis or created via external means, are known to exhibit functionalities absent in the homogeneous counterparts. One of the most notable examples is the colossal magnetoresistance discovered in mixed-valence manganites, where the coexistence of nano- to micrometer-sized phase-separated domains dictates the magnetotransport. However, it remains challenging to pattern and process such materials into predesigned structures and devices. In this work, a direct laser interference irradiation (LII) method is employed to produce periodic stripes in thin films of a prototypical phase-separated manganite Pr0.65 (Ca0.75 Sr0.25 )0.35 MnO3 (PCSMO). LII induces selective structural amorphization within the crystalline PCSMO matrix, forming arrays with dimensions commensurate with the laser wavelength. Furthermore, because the length scale of LII modification is compatible to that of phase separation in PCSMO, three orders of magnitude of increase in magnetoresistance and significant in-plane transport anisotropy are observed in treated PCSMO thin films. Our results show that LII is a rapid, cost-effective and contamination-free technique to tailor and improve the physical properties of manganite thin films, and it is promising to be generalized to other functional materials. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Separation and determination of eight plant hormones by reversed-phase high performance liquid chromatography].

PubMed

Fang, N; Hou, S; Shao, X; He, Y; Zhao, G

1998-09-01

In this paper, reversed-phase high performance liquid chromatographic technique was used for the separation and determination of eight plant hormones. Methanol-water-acetic acid system was chosen as the mobile phase. The effects of different separation conditions, such as the methanol and acetic acid concentrations in mobile phase, on the retention behaviours of eight plant hormones in this system were studied. The general trends in retention behaviours could be correlated to the methanol concentration in mobile phase. The experimental results showed that the optimum separation was achieved with following gradient elution condition: 0-3 minutes, 70% (water percentage in mobile phase), 3-13 minutes, 70%-20%, 13-48 minutes, 20%. Benzene was added to be as the internal standard. Under this experimental condition, the eight plant hormones could be separated completely and detected quantitatively at 260 nm within 16 minutes. The calibration curves for the eight compounds gave linearity over a wide range. The correlation coefficients of each components were r(ZT) = 0.9971, r(GAs) = 0.9999, r(K) = 0.9997, r(BA) = 0.9995, r(IAA) = 0.9998, r(IPA) = 0.9982, r(IBA) = 0.9995 and r(NAA) = 0.9995. The method is rapid, simple and efficient. It is a suitable method for the accurate determination of gibberellic acid (GA) and alpha-naphthaleneacetic acid (alpha-NAA) in products for agricultural use.

Advanced flight hardware for organic separations using aqueous two-phase partitioning

NASA Astrophysics Data System (ADS)

Deuser, Mark S.; Vellinger, John C.; Weber, John T.

1996-03-01

Separation of cells and cell components is the limiting factor in many biomedical research and pharmaceutical development processes. Aqueous Two-Phase Partitioning (ATPP) is a unique separation technique which allows purification and classification of biological materials. SHOT has employed the ATPP process in separation equipment developed for both space and ground applications. Initial equipment development and research focused on the ORganic SEParation (ORSEP) space flight experiments that were performed on suborbital rockets and the shuttle. ADvanced SEParations (ADSEP) technology was developed as the next generation of ORSEP equipment through a NASA Small Business Innovation Research (SBIR) contract. Under the SBIR contract, a marketing study was conducted, indicating a growing commercial market exists among biotechnology firms for ADSEP equipment and associated flight research and development services. SHOT is preparing to begin manufacturing and marketing laboratory versions of the ADSEP hardware for the ground-based market. In addition, through a self-financed SBIR Phase III effort, SHOT is fabricating and integrating the ADSEP flight hardware for a commercially-driven SPACEHAB 04 experiment that will be the initial step in marketing space separations services. The ADSEP ground-based and microgravity research is expected to play a vital role in developing important new biomedical and pharmaceutical products.

Saying Good-by: An Example of Using a Good-by Technique and Concomitant Psychodrama in the Resolving of Family Grief.

ERIC Educational Resources Information Center

Kaminski, Robert C.

A structured technique for saying "good-bye," or terminating a relationship, an important aspect of the therapeutic relationship, is presented. It consists of three distinct phases that are all dynamically interrelated, and can also be structured into separation caused by death. The technique is described in terms of three specific areas…

Simultaneous separation and analysis of water- and fat-soluble vitamins on multi-modal reversed-phase weak anion exchange material by HPLC-UV.

PubMed

Dabre, Romain; Azad, Nazanin; Schwämmle, Achim; Lämmerhofer, Michael; Lindner, Wolfgang

2011-04-01

Several methods for the separation of vitamins on HPLC columns were already validated in the last 20 years. However, most of the techniques focus on separating either fat- or water-soluble vitamins and only few methods are intended to separate lipophilic and hydrophilic vitamins simultaneously. A mixed-mode reversed-phase weak anion exchange (RP-WAX) stationary phase was developed in our laboratory in order to address such mixture of analytes with different chemical characteristics, which are difficult to separate on standard columns. The high versatility in usage of the RP-WAX chromatographic material allowed a baseline separation of ten vitamins within a single run, seven water-soluble and three fat-soluble, using three different chromatographic modes: some positively charged vitamins are eluted in ion exclusion and ion repulsion modes whereas the negatively charged molecules are eluted in the ion exchange mechanism. The non-charged molecules are eluted in a classical reversed-phase mode, regarding their polarities. The method was validated for the vitamin analysis in tablets, evaluating selectivity, robustness, linearity, accuracy, and precision. The validated method was finally employed for the analysis of the vitamin content of some commercially available supplement tablets. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Anomalous amplification of a homodyne signal via almost-balanced weak values.

PubMed

Liu, Wei-Tao; Martínez-Rincón, Julián; Viza, Gerardo I; Howell, John C

2017-03-01

We propose precision measurements of ultra-small angular velocities of a mirror within a modified Sagnac interferometer, where the counter-propagating beams are spatially separated, using the recently proposed technique of almost-balanced weak values amplification (ABWV) [Phys. Rev. Lett.116, 100803 (2016)PRLTAO0031-900710.1103/PhysRevLett.116.100803]. The separation between the two beams provides additional amplification with respect to using collinear beams in a Sagnac interferometer. Within the same setup, the weak-value amplification technique is also performed for comparison. Much higher amplification factors can be obtained using the almost-balanced weak values technique, with the best one achieved in our experiments being as high as 1.2×10⁷. In addition, the amplification factor monotonically increases with decreasing of the post-selection phase for the ABWV case in our experiments, which is not the case for weak-value amplification (WVA) at small post-selection phases. Both techniques consist of measuring the angular velocity. The sensitivity of the ABWV technique is ∼38  nrad/s per averaged pulse for a repetition rate of 1 Hz and ∼33  nrad/s per averaged pulse for the WVA technique.

Chembio extraction on a chip by nanoliter droplet ejection.

PubMed

Yu, Hongyu; Kwon, Jae Wan; Kim, Eun Sok

2005-03-01

This paper describes a novel liquid separation technique for chembio extraction by an ultrasonic nanoliter-liquid-droplet ejector built on a PZT sheet. This technique extracts material from an aqueous two-phase system (ATPS) in a precise amount through digital control of the number of nanoliter droplets, without any mixing between the two liquids in the ATPS. The ultrasonic droplet ejector uses an acoustic streaming effect produced by an acoustic beam focused on the liquid surface, and ejects liquid droplets only from the liquid surface without disturbing most of the liquid below the surface. This unique characteristic of the focused acoustic beam is perfect (1) for separating a top-layer liquid (from the bulk of liquid) that contains particles of interest or (2) for recovering a top-layer liquid that has different phase from a bottom-layer liquid. Three kinds of liquid extraction are demonstrated with the ultrasonic droplet ejector: (1) 16 microl of top layer in Dextran-polyethylene glycol-water ATPS (aqueous two-phase system) is recovered within 20 s; (2) micron sized particles that float on water surface are ejected out with water droplets; and (3) oil layer on top of water is separated out.

Spinodal Decomposition in Functionally Graded Super Duplex Stainless Steel and Weld Metal

NASA Astrophysics Data System (ADS)

Hosseini, Vahid A.; Thuvander, Mattias; Wessman, Sten; Karlsson, Leif

2018-07-01

Low-temperature phase separations (T < 500 °C), resulting in changes in mechanical and corrosion properties, of super duplex stainless steel (SDSS) base and weld metals were investigated for short heat treatment times (0.5 to 600 minutes). A novel heat treatment technique, where a stationary arc produces a steady state temperature gradient for selected times, was employed to fabricate functionally graded materials. Three different initial material conditions including 2507 SDSS, remelted 2507 SDSS, and 2509 SDSS weld metal were investigated. Selective etching of ferrite significantly decreased in regions heat treated at 435 °C to 480 °C already after 3 minutes due to rapid phase separations. Atom probe tomography results revealed spinodal decomposition of ferrite and precipitation of Cu particles. Microhardness mapping showed that as-welded microstructure and/or higher Ni content accelerated decomposition. The arc heat treatment technique combined with microhardness mapping and electrolytical etching was found to be a successful approach to evaluate kinetics of low-temperature phase separations in SDSS, particularly at its earlier stages. A time-temperature transformation diagram was proposed showing the kinetics of 475 °C-embrittlement in 2507 SDSS.

Spinodal Decomposition in Functionally Graded Super Duplex Stainless Steel and Weld Metal

NASA Astrophysics Data System (ADS)

Hosseini, Vahid A.; Thuvander, Mattias; Wessman, Sten; Karlsson, Leif

2018-04-01

Low-temperature phase separations (T < 500 °C), resulting in changes in mechanical and corrosion properties, of super duplex stainless steel (SDSS) base and weld metals were investigated for short heat treatment times (0.5 to 600 minutes). A novel heat treatment technique, where a stationary arc produces a steady state temperature gradient for selected times, was employed to fabricate functionally graded materials. Three different initial material conditions including 2507 SDSS, remelted 2507 SDSS, and 2509 SDSS weld metal were investigated. Selective etching of ferrite significantly decreased in regions heat treated at 435 °C to 480 °C already after 3 minutes due to rapid phase separations. Atom probe tomography results revealed spinodal decomposition of ferrite and precipitation of Cu particles. Microhardness mapping showed that as-welded microstructure and/or higher Ni content accelerated decomposition. The arc heat treatment technique combined with microhardness mapping and electrolytical etching was found to be a successful approach to evaluate kinetics of low-temperature phase separations in SDSS, particularly at its earlier stages. A time-temperature transformation diagram was proposed showing the kinetics of 475 °C-embrittlement in 2507 SDSS.

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

PubMed

Speybrouck, David; Lipka, Emmanuelle

2016-10-07

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

Multiwavelength digital holography with wavelength-multiplexed holograms and arbitrary symmetric phase shifts.

PubMed

Tahara, Tatsuki; Otani, Reo; Omae, Kaito; Gotohda, Takuya; Arai, Yasuhiko; Takaki, Yasuhiro

2017-05-15

We propose multiwavelength in-line digital holography with wavelength-multiplexed phase-shifted holograms and arbitrary symmetric phase shifts. We use phase-shifting interferometry selectively extracting wavelength information to reconstruct multiwavelength object waves separately from wavelength-multiplexed monochromatic images. The proposed technique obtains systems of equations for real and imaginary parts of multiwavelength object waves from the holograms by introducing arbitrary symmetric phase shifts. Then, the technique derives each complex amplitude distribution of each object wave selectively and analytically by solving the two systems of equations. We formulate the algorithm in the case of an arbitrary number of wavelengths and confirm its validity numerically and experimentally in the cases where the number of wavelengths is two and three.

Experimental Investigation and Thermodynamic Assessment of Phase Equilibria in the PLLA/Dioxane/Water Ternary System for Applications in the Biomedical Field.

PubMed

Ruggiero, Flavia; Netti, Paolo Antonio; Torino, Enza

2015-12-01

Fundamental understanding of thermodynamic of phase separation plays a key role in tuning the desired features of biomedical devices. In particular, phase separation of ternary solution is of remarkable interest in processes to obtain biodegradable and biocompatible architectures applied as artificial devices to repair, replace, or support damaged tissues or organs. In these perspectives, thermally induced phase separation (TIPS) is the most widely used technique to obtained porous morphologies and, in addition, among different ternary systems, polylactic acid (PLLA)/dioxane/water has given promising results and has been largely studied. However, to increase the control of TIPS-based processes and architectures, an investigation of the basic energetic phenomena occurring during phase separation is still required. Here we propose an experimental investigation of the selected ternary system by using isothermal titration calorimetric approach at different solvent/antisolvent ratio and a thermodynamic explanation related to the polymer-solvents interactions in terms of energetic contribution to the phase separation process. Furthermore, relevant information about the phase diagrams and interaction parameters of the studied systems are furnished in terms of liquid-liquid miscibility gap. Indeed, polymer-solvents interactions are responsible for the mechanism of the phase separation process and, therefore, of the final features of the morphologies; the knowledge of such data is fundamental to control processes for the production of membranes, scaffolds and several nanostructures. The behavior of the polymer at different solvent/nonsolvent ratios is discussed in terms of solvation mechanism and a preliminary contribution to the understanding of the role of the hydrogen bonding in the interface phenomena is also reported. It is the first time that thermodynamic data of a ternary system are collected by mean of nano-isothermal titration calorimetry (nano-ITC). Supporting Information is available.

On-line comprehensive two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography for preparative isolation of Peucedanum praeruptorum.

PubMed

Wang, Xin-Yuan; Li, Jia-Fu; Jian, Ya-Mei; Wu, Zhen; Fang, Mei-Juan; Qiu, Ying-Kun

2015-03-27

A new on-line comprehensive preparative two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography (2D NPLC × RPLC) system was developed for the separation of complicated natural products. It was based on the use of a silica gel packed medium-pressure column as the first dimension and an ODS preparative HPLC column as the second dimension. The two dimensions were connected with normal-phase (NP) and reversed-phase (RP) enrichment units, involving a newly developed airflow assisted adsorption (AAA) technique. The instrument operation and the performance of this NPLC × RPLC separation method were illustrated by gram-scale isolation of ethanol extract from the roots of Peucedanum praeruptorum. In total, 19 compounds with high purity were obtained via automated multi-step preparative separation in a short period of time using this system, and their structures were comprehensively characterized by ESI-MS, (1)H NMR, and (13)C NMR. Including two new compounds, five isomers in two groups with identical HPLC and TLC retention values were also obtained and identified by 1D NMR and 2D NMR. This is the first report of an NPLC × RPLC system successfully applied in an on-line preparative process. This system not only solved the interfacing problem of mobile-phase immiscibility caused by NP and RP separation, it also exhibited apparent advantages in separation efficiency and sample treatment capacity compared with conventional methods. Copyright © 2015 Elsevier B.V. All rights reserved.

Modification of Gaussian mixture models for data classification in high energy physics

NASA Astrophysics Data System (ADS)

Štěpánek, Michal; Franc, Jiří; Kůs, Václav

2015-01-01

In high energy physics, we deal with demanding task of signal separation from background. The Model Based Clustering method involves the estimation of distribution mixture parameters via the Expectation-Maximization algorithm in the training phase and application of Bayes' rule in the testing phase. Modifications of the algorithm such as weighting, missing data processing, and overtraining avoidance will be discussed. Due to the strong dependence of the algorithm on initialization, genetic optimization techniques such as mutation, elitism, parasitism, and the rank selection of individuals will be mentioned. Data pre-processing plays a significant role for the subsequent combination of final discriminants in order to improve signal separation efficiency. Moreover, the results of the top quark separation from the Tevatron collider will be compared with those of standard multivariate techniques in high energy physics. Results from this study has been used in the measurement of the inclusive top pair production cross section employing DØ Tevatron full Runll data (9.7 fb-1).

Recent advances in capillary ultrahigh pressure liquid chromatography.

PubMed

Blue, Laura E; Franklin, Edward G; Godinho, Justin M; Grinias, James P; Grinias, Kaitlin M; Lunn, Daniel B; Moore, Stephanie M

2017-11-10

In the twenty years since its initial demonstration, capillary ultrahigh pressure liquid chromatography (UHPLC) has proven to be one of most powerful separation techniques for the analysis of complex mixtures. This review focuses on the most recent advances made since 2010 towards increasing the performance of such separations. Improvements in capillary column preparation techniques that have led to columns with unprecedented performance are described. New stationary phases and phase supports that have been reported over the past decade are detailed, with a focus on their use in capillary formats. A discussion on the instrument developments that have been required to ensure that extra-column effects do not diminish the intrinsic efficiency of these columns during analysis is also included. Finally, the impact of these capillary UHPLC topics on the field of proteomics and ways in which capillary UHPLC may continue to be applied to the separation of complex samples are addressed. Copyright © 2017 Elsevier B.V. All rights reserved.

Isolation of >1 nm Diameter Single-Wall Carbon Nanotube Species Using Aqueous Two-Phase Extraction.

PubMed

Fagan, Jeffrey A; Hároz, Erik H; Ihly, Rachelle; Gui, Hui; Blackburn, Jeffrey L; Simpson, Jeffrey R; Lam, Stephanie; Hight Walker, Angela R; Doorn, Stephen K; Zheng, Ming

2015-05-26

In this contribution we demonstrate the effective separation of single-wall carbon nanotube (SWCNT) species with diameters larger than 1 nm through multistage aqueous two-phase extraction (ATPE), including isolation at the near-monochiral species level up to at least the diameter range of SWCNTs synthesized by electric arc synthesis (1.3-1.6 nm). We also demonstrate that refined species are readily obtained from both the metallic and semiconducting subpopulations of SWCNTs and that this methodology is effective for multiple SWCNT raw materials. Using these data, we report an empirical function for the necessary surfactant concentrations in the ATPE method for separating different SWCNTs into either the lower or upper phase as a function of SWCNT diameter. This empirical correlation enables predictive separation design and identifies a subset of SWCNTs that behave unusually as compared to other species. These results not only dramatically increase the range of SWCNT diameters to which species selective separation can be achieved but also demonstrate that aqueous two-phase separations can be designed across experimentally accessible ranges of surfactant concentrations to controllably separate SWCNT populations of very small (∼0.62 nm) to very large diameters (>1.7 nm). Together, the results reported here indicate that total separation of all SWCNT species is likely feasible by the ATPE method, especially given future development of multistage automated extraction techniques.

Planar particle/droplet size measurement technique using digital particle image velocimetry image data

NASA Technical Reports Server (NTRS)

Kadambi, Jaikrishnan R. (Inventor); Wernet, Mark P. (Inventor); Mielke, Amy F. (Inventor)

2005-01-01

A method for determining a mass flux of an entrained phase in a planar two-phase flow records images of particles in the two-phase flow. Respective sizes of the particles (the entrained phase) are determined as a function of a separation between spots identified on the particle images. Respective velocities of the particles are determined. The mass flux of the entrained phase is determined as a function of the size and velocity of the particles.

Candidate space processing techniques for biomaterials other than preparative electrophoresis

NASA Technical Reports Server (NTRS)

Brooks, D. E.

1976-01-01

The advantages of performing the partition and countercurrent distribution (CCD) of cells in phase separated aqueous polymer systems under reduced gravity were assessed. Other possible applications considered for the space processing program include the freezing front separation of cells, adsorption of cells at the air-water interface, and the macrophage electrophoretic mobility test for cancer.

Analysis of Phase Separation in Czochralski Grown Single Crystal Ilmenite

NASA Technical Reports Server (NTRS)

Wilkins, R.; Powell, Kirk St. A.; Loregnard, Kieron R.; Lin, Sy-Chyi; Muthusami, Jayakumar; Zhou, Feng; Pandey, R. K.; Brown, Geoff; Hawley, M. E.

1998-01-01

Ilmenite (FeTiOs) is a wide bandgap semiconductor with an energy gap of 2.58 eV. Ilmenite has properties suited for radiation tolerant applications, as well as a variety of other electronic applications. Single crystal ilmenite has been grown from the melt using the Czochralski method. Growth conditions have a profound effect on the microstructure of the samples. Here we present data from a variety of analytical techniques which indicate that some grown crystals exhibit distinct phase separation during growth. This phase separation is apparent for both post-growth annealed and unannealed samples. Under optical microscopy, there appear two distinct areas forming a matrix with an array of dots on order of 5 pm diameter. While appearing bright in the optical micrograph, atomic force microscope (AFM) shows the dots to be shallow pits on the surface. Magnetic force microscope (MFM) shows the dots to be magnetic. Phase identification via electron microprobe analysis (EMPA) indicates two major phases in the unannealed samples and four in the annealed samples, where the dots appear to be almost pure iron. This is consistent with micrographs taken with a scanning probe microscope used in the magnetic force mode. Samples that do not exhibit the phase separation have little or no discernible magnetic structure detectable by the MFM.

Kernel-Phase Interferometry for Super-Resolution Detection of Faint Companions

NASA Astrophysics Data System (ADS)

Factor, Samuel M.; Kraus, Adam L.

2017-06-01

Direct detection of close in companions (exoplanets or binary systems) is notoriously difficult. While coronagraphs and point spread function (PSF) subtraction can be used to reduce contrast and dig out signals of companions under the PSF, there are still significant limitations in separation and contrast near λ/D. Non-redundant aperture masking (NRM) interferometry can be used to detect companions well inside the PSF of a diffraction limited image, though the mask discards ˜ 95% of the light gathered by the telescope and thus the technique is severely flux limited. Kernel-phase analysis applies interferometric techniques similar to NRM to a diffraction limited image utilizing the full aperture. Instead of non-redundant closure-phases, kernel-phases are constructed from a grid of points on the full aperture, simulating a redundant interferometer. I have developed a new, easy to use, faint companion detection pipeline which analyzes kernel-phases utilizing Bayesian model comparison. I demonstrate this pipeline on archival images from HST/NICMOS, searching for new companions in order to constrain binary formation models at separations inaccessible to previous techniques. Using this method, it is possible to detect a companion well within the classical λ/D Rayleigh diffraction limit using a fraction of the telescope time as NRM. Since the James Webb Space Telescope (JWST) will be able to perform NRM observations, further development and characterization of kernel-phase analysis will allow efficient use of highly competitive JWST telescope time. As no mask is needed, this technique can easily be applied to archival data and even target acquisition images (e.g. from JWST), making the detection of close in companions cheap and simple as no additional observations are needed.

Gas chromatography on wall-coated open-tubular columns with ionic liquid stationary phases.

PubMed

Poole, Colin F; Lenca, Nicole

2014-08-29

Ionic liquids have moved from novel to practical stationary phases for gas chromatography with an increasing portfolio of applications. Ionic liquids complement conventional stationary phases because of a combination of thermophysical and solvation properties that only exist for ionic solvents. Their high thermal stability and low vapor pressure makes them suitable as polar stationary phases for separations requiring high temperatures. Ionic liquids are good solvents and can be used to expand the chemical space for separations. They are the only stationary phases with significant hydrogen-bond acidity in common use; they extend the hydrogen-bond basicity of conventional stationary phases; they are as dipolar/polarizable as the most polar conventional stationary phases; and some ionic liquids are significantly less cohesive than conventional polar stationary phases. Problems in column coating techniques and related low column performance, column activity, and stationary phase reactivity require further exploration as the reasons for these features are poorly understood at present. Copyright © 2014 Elsevier B.V. All rights reserved.

Principles of Micellar Electrokinetic Capillary Chromatography Applied in Pharmaceutical Analysis

PubMed Central

Hancu, Gabriel; Simon, Brigitta; Rusu, Aura; Mircia, Eleonora; Gyéresi, Árpád

2013-01-01

Since its introduction capillary electrophoresis has shown great potential in areas where electrophoretic techniques have rarely been used before, including here the analysis of pharmaceutical substances. The large majority of pharmaceutical substances are neutral from electrophoretic point of view, consequently separations by the classic capillary zone electrophoresis; where separation is based on the differences between the own electrophoretic mobilities of the analytes; are hard to achieve. Micellar electrokinetic capillary chromatography, a hybrid method that combines chromatographic and electrophoretic separation principles, extends the applicability of capillary electrophoretic methods to neutral analytes. In micellar electrokinetic capillary chromatography, surfactants are added to the buffer solution in concentration above their critical micellar concentrations, consequently micelles are formed; micelles that undergo electrophoretic migration like any other charged particle. The separation is based on the differential partitioning of an analyte between the two-phase system: the mobile aqueous phase and micellar pseudostationary phase. The present paper aims to summarize the basic aspects regarding separation principles and practical applications of micellar electrokinetic capillary chromatography, with particular attention to those relevant in pharmaceutical analysis. PMID:24312804

The assessment of pi-pi selective stationary phases for two-dimensional HPLC analysis of foods: application to the analysis of coffee.

PubMed

Mnatsakanyan, Mariam; Stevenson, Paul G; Shock, David; Conlan, Xavier A; Goodie, Tiffany A; Spencer, Kylie N; Barnett, Neil W; Francis, Paul S; Shalliker, R Andrew

2010-09-15

Differences between alkyl, dipole-dipole, hydrogen bonding, and pi-pi selective surfaces represented by non-resonance and resonance pi-stationary phases have been assessed for the separation of 'Ristretto' café espresso by employing 2DHPLC techniques with C18 phase selectivity detection. Geometric approach to factor analysis (GAFA) was used to measure the detected peaks (N), spreading angle (beta), correlation, practical peak capacity (n(p)) and percentage usage of the separations space, as an assessment of selectivity differences between regional quadrants of the two-dimensional separation plane. Although all tested systems were correlated to some degree to the C18 dimension, regional measurement of separation divergence revealed that performance of specific systems was better for certain sample components. The results illustrate that because of the complexity of the 'real' sample obtaining a truly orthogonal two-dimensional system for complex samples of natural origin may be practically impossible. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Solid-phase extraction and high-performance liquid chromatographic separation of pigments of red wines.

PubMed

Csiktusnádi Kiss, G A; Forgács, E; Cserháti, T; Candeias, M; Vilas-Boas, L; Bronze, R; Spranger, I

2000-08-11

The adsorption and desorption capacities of 11 different solid-phase extraction sorbents were tested for the preconcenration of pigments of various Hungarian red wines. The concentrates were evaluated by multiwavelengh spectrophotometry combined with a spectral mapping technique (SPM) and by reversed-phase high-performance liquid chromatography. The highest (10-fold) concentration of pigments was achieved on octadecylsilica sorbent. It can be used five times without losing adsorption and desorption characteristics. SPM indicated that multiwavelength spectrophotometry can be employed for the differentiation of red wines. Comparison of the chromatograms of pigments with and without preconcentration showed that preconcentration makes possible the separation and detection of pigments present in low concentration in red wines.

Trying to detect gas-phase ions? Understanding Ion Mobility Spectrometry

PubMed Central

Cumeras, R.; Figueras, E.; Davis, C.E.; Baumbach, J.I.; Gràcia, I.

2014-01-01

Ion Mobility Spectrometry (IMS) is a widely used and ‘well-known’ technique of ion separation in gaseous phase based on the differences of ion mobilities under an electric field. This technique has received increased interest over the last several decades as evidenced by the pace and advances of new IMS devices available. In this review we explore the hyphenated techniques that are used with IMS, especially mass spectrometry as identification approach and multi-capillary column as pre-separation approach. Also, we will pay special attention to the key figures of merit of the ion mobility spectrum and how data is treated, and the influences of the experimental parameters in both a conventional drift time IMS (DTIMS) and a miniaturized IMS also known as high Field Asymmetric IMS (FAIMS) in the planar configuration. The current review article is preceded by a companion review article which details the current instrumentation and to the sections that configures both a conventional DTIMS and FAIMS devices. Those reviews will give the reader an insightful view of the main characteristics and aspects of the IMS technique. PMID:25465248

Selective spectroscopic imaging of hyperpolarized pyruvate and its metabolites using a single-echo variable phase advance method in balanced SSFP

PubMed Central

Varma, Gopal; Wang, Xiaoen; Vinogradov, Elena; Bhatt, Rupal S.; Sukhatme, Vikas; Seth, Pankaj; Lenkinski, Robert E.; Alsop, David C.; Grant, Aaron K.

2015-01-01

Purpose In balanced steady state free precession (bSSFP), the signal intensity has a well-known dependence on the off-resonance frequency, or, equivalently, the phase advance between successive radiofrequency (RF) pulses. The signal profile can be used to resolve the contributions from the spectrally separated metabolites. This work describes a method based on use of a variable RF phase advance to acquire spatial and spectral data in a time-efficient manner for hyperpolarized 13C MRI. Theory and Methods The technique relies on the frequency response from a bSSFP acquisition to acquire relatively rapid, high-resolution images that may be reconstructed to separate contributions from different metabolites. The ability to produce images from spectrally separated metabolites was demonstrated in-vitro, as well as in-vivo following administration of hyperpolarized 1-13C pyruvate in mice with xenograft tumors. Results In-vivo images of pyruvate, alanine, pyruvate hydrate and lactate were reconstructed from 4 images acquired in 2 seconds with an in-plane resolution of 1.25 × 1.25mm2 and 5mm slice thickness. Conclusions The phase advance method allowed acquisition of spectroscopically selective images with high spatial and temporal resolution. This method provides an alternative approach to hyperpolarized 13C spectroscopic MRI that can be combined with other techniques such as multi-echo or fluctuating equilibrium bSSFP. PMID:26507361

Quantitative Phase Fraction Detection in Organic Photovoltaic Materials through EELS Imaging

DOE PAGES

Dyck, Ondrej; Hu, Sheng; Das, Sanjib; ...

2015-11-24

Organic photovoltaic materials have recently seen intense interest from the research community. Improvements in device performance are occurring at an impressive rate; however, visualization of the active layer phase separation still remains a challenge. Our paper outlines the application of two electron energy-loss spectroscopic (EELS) imaging techniques that can complement and enhance current phase detection techniques. Specifically, the bulk plasmon peak position, often used to produce contrast between phases in energy filtered transmission electron microscopy (EFTEM), is quantitatively mapped across a sample cross section. One complementary spectrum image capturing the carbon and sulfur core loss edges is compared with themore » plasmon peak map and found to agree quite well, indicating that carbon and sulfur density differences between the two phases also allows phase discrimination. Additionally, an analytical technique for determining absolute atomic areal density is used to produce an absolute carbon and sulfur areal density map. We also show how these maps may be re-interpreted as a phase ratio map, giving quantitative information about the purity of the phases within the junction.« less

Vacancy-mediated fcc/bcc phase separation in Fe 1-xNi x ultrathin films

DOE PAGES

Mentes, T. O.; Stojic, N.; Vescovo, E.; ...

2016-08-01

The phase separation occurring in Fe-Ni thin lms near the Invar composition is studied by using high resolution spectromicroscopy techniques and density functional theory calculations. Annealed at temperatures around 300 C, Fe 0.70Ni 0.30 lms on W(110) break into micron-sized bcc and fcc domains with compositions in agreement with the bulk Fe-Ni phase diagram. Ni is found to be the di using species in forming the chemical heterogeneity. The experimentally-determined energy barrier of 1.59 0.09 eV is identi ed as the vacancy formation energy via density functional theory calculations. Thus, the principal role of the surface in the phase separationmore » process is attributed to vacancy creation without interstitials.« less

Polymer-induced phase separation and crystallization in immunoglobulin G solutions.

PubMed

Li, Jianguo; Rajagopalan, Raj; Jiang, Jianwen

2008-05-28

We study the effects of the size of polymer additives and ionic strength on the phase behavior of a nonglobular protein-immunoglobulin G (IgG)-by using a simple four-site model to mimic the shape of IgG. The interaction potential between the protein molecules consists of a Derjaguin-Landau-Verwey-Overbeek-type colloidal potential and an Asakura-Oosawa depletion potential arising from the addition of polymer. Liquid-liquid equilibria and fluid-solid equilibria are calculated by using the Gibbs ensemble Monte Carlo technique and the Gibbs-Duhem integration (GDI) method, respectively. Absolute Helmholtz energy is also calculated to get an initial coexisting point as required by GDI. The results reveal a nonmonotonic dependence of the critical polymer concentration rho(PEG) (*) (i.e., the minimum polymer concentration needed to induce liquid-liquid phase separation) on the polymer-to-protein size ratio q (equivalently, the range of the polymer-induced depletion interaction potential). We have developed a simple equation for estimating the minimum amount of polymer needed to induce the liquid-liquid phase separation and show that rho(PEG) (*) approximately [q(1+q)(3)]. The results also show that the liquid-liquid phase separation is metastable for low-molecular weight polymers (q=0.2) but stable at large molecular weights (q=1.0), thereby indicating that small sizes of polymer are required for protein crystallization. The simulation results provide practical guidelines for the selection of polymer size and ionic strength for protein phase separation and crystallization.

Surface characterization based on optical phase shifting interferometry

DOEpatents

Mello, Michael , Rosakis; Ares, J [Altadena, CA

2011-08-02

Apparatus, techniques and systems for implementing an optical interferometer to measure surfaces, including mapping of instantaneous curvature or in-plane and out-of-plane displacement field gradients of a sample surface based on obtaining and processing four optical interferograms from a common optical reflected beam from the sample surface that are relatively separated in phase by .pi./2.

Nanoporous thermosetting polymers.

PubMed

Raman, Vijay I; Palmese, Giuseppe R

2005-02-15

Potential applications of nanoporous thermosetting polymers include polyelectrolytes in fuel cells, separation membranes, adsorption media, and sensors. Design of nanoporous polymers for such applications entails controlling permeability by tailoring pore size, structure, and interface chemistry. Nanoporous thermosetting polymers are often synthesized via free radical mechanisms using solvents that phase separate during polymerization. In this work, a novel technique for the synthesis of nanoporous thermosets is presented that is based on the reactive encapsulation of an inert solvent using step-growth cross-linking polymerization without micro/macroscopic phase separation. The criteria for selecting such a monomer-polymer-solvent system are discussed based on FTIR analysis, observed micro/macroscopic phase separation, and thermodynamics of swelling. Investigation of resulting network pore structures by scanning electron microscopy (SEM) and small-angle X-ray scattering following extraction and supercritical drying using carbon dioxide showed that nanoporous polymeric materials with pore sizes ranging from 1 to 50 nm can be synthesized by varying the solvent content. The differences in the porous morphology of these materials compared to more common free radically polymerized analogues that exhibit phase separation were evident from SEM imaging. Furthermore, it was demonstrated that the chemical activity of the nanoporous materials obtained by our method could be tailored by grafting appropriate functional groups at the pore interface.

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

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

Foltz, K.; Landsberger, S.; Srinivasan, B.

1994-12-31

A method for the separation of radionuclides with Z greater than 88, from lower-level radioactive wastes (liquid scintillation cocktail or LSC wastes), is described. The method is liquid-liquid extraction (LLX) and demulsification. The actinide elements are removed from the LSC wastes by extraction into an aqueous phase after the cocktail has been demulsified. The aqueous and organic phases are separated, then the wastes type remaining may be incinerated. Future experiments will be performed to study the effects of pH and temperature and to extend the study to wastes containing americium.

N-linked glycoprotein analysis using dual-extraction ultrahigh-performance liquid chromatography and electrospray tandem mass spectrometry.

PubMed

Siu, S O; Lam, Maggie P Y; Lau, Edward; Yeung, William S B; Cox, David M; Chu, Ivan K

2010-01-01

Although reverse-phase liquid chromatography (RP-LC) is a common technique for peptide separation in shotgun proteomics and glycoproteomics, it often provides unsatisfactory results for the analysis of glycopeptides and glycans. This bias against glycopeptides makes it difficult to study glycoproteins. By coupling mass spectrometry (MS) with a combination of RP-LC and normal-phase (NP)-LC as an integrated front-end separation system, we demonstrate that effective identification and characterization of both peptides and glycopeptides mixtures, and their constituent glycan structures, can be achieved from a single sample injection event.

Hydrophilic organic/salt-containing aqueous two-phase solvent system for counter-current chromatography: a novel technique for separation of polar compounds.

PubMed

Liu, Dan; Zou, Xiaowei; Gao, Mingzhe; Gu, Ming; Xiao, Hongbin

2014-08-22

Hydrophilic organic/salt-containing aqueous two-phase system composing of ethanol, water and ammonium sulfate for separation polar compounds was investigated on multilayer coil associated with J-type HSCCC devices. Compared to the classical polar solvent system based on 1-butanol-water or PEG1000-ammonium sulfate-water, the water content of upper phase in ethanol-ammonium sulfate-water systems was from 53.7% to 32.8% (wt%), closed to PEG1000-ammonium sulfate-water aqueous two-phase systems and higher than 1-butanol-water (22.0%, wt%). Therefore, the polarity of ethanol-ammonium sulfate-water is in the middle of 1-butanol-water and PEG-ammonium sulfate-water system, which is quite good for separating polar compounds like phenols, nucleosides and amino acids with low partition coefficient in 1-octanol-water system. The retention of stationary phase in four elution mode on type-J counter-current chromatography devices with multilayer coil column changed from 26% to 71%. Hydrodynamic trend possess both intermediate and hydrophilic solvent system property, which closely related to the composition of solvent system. The applicability of this system was demonstrated by successful separation of adenosine, uridine guanosine and cytidine. Copyright © 2014 Elsevier B.V. All rights reserved.

Sensors research and technology

NASA Technical Reports Server (NTRS)

Cutts, James A.

1988-01-01

Information on sensors research and technology is given in viewgraph form. Information is given on sensing techniques for space science, passive remote sensing techniques and applications, submillimeter coherent sensing, submillimeter mixers and local oscillator sources, non-coherent sensors, active remote sensing, solid state laser development, a low vibration cooler, separation of liquid helium and vapor phase in zero gravity, and future plans.

Opalescence in monoclonal antibody solutions and its correlation with intermolecular interactions in dilute and concentrated solutions.

PubMed

Raut, Ashlesha S; Kalonia, Devendra S

2015-04-01

Opalescence indicates physical instability of a formulation because of the presence of aggregates or liquid-liquid phase separation in solution and has been reported for monoclonal antibody (mAb) formulations. Increased solution opalescence can be attributed to attractive protein-protein interactions (PPIs). Techniques including light scattering, AUC, or membrane osmometry are routinely employed to measure PPIs in dilute solutions, whereas opalescence is seen at relatively higher concentrations, where both long- and short-range forces contribute to overall PPIs. The mAb molecule studied here shows a unique property of high opalescence because of liquid-liquid phase separation. In this study, opalescence measurements are correlated to PPIs measured in diluted and concentrated solutions using light scattering (kD ) and high-frequency rheology (G'), respectively. Charges on the molecules were calculated using zeta potential measurements. Results indicate that high opalescence and phase separation are a result of the attractive interactions in solution; however, the presence of attractive interactions do not always imply phase separation. Temperature dependence of opalescence suggests that thermodynamic contribution to opalescence is significant and Tcloud can be utilized as a potential tool to assess attractive interactions in solution. © 2014 Wiley Periodicals, Inc. and the American Pharmacists Association.

Methods for determining infrasound phase velocity direction with an array of line sensors.

PubMed

Walker, Kristoffer T; Zumberge, Mark A; Hedlin, Michael A H; Shearer, Peter M

2008-10-01

Infrasound arrays typically consist of several microbarometers separated by distances that provide predictable signal time separations, forming the basis for processing techniques that estimate the phase velocity direction. The directional resolution depends on the noise level and is proportional to the number of these point sensors; additional sensors help attenuate noise and improve direction resolution. An alternative approach is to form an array of directional line sensors, each of which emulates a line of many microphones that instantaneously integrate pressure change. The instrument response is a function of the orientation of the line with respect to the signal wavefront. Real data recorded at the Piñon Flat Observatory in southern California and synthetic data show that this spectral property can be exploited with multiple line sensors to determine the phase velocity direction with a precision comparable to a larger aperture array of microbarometers. Three types of instrument-response-dependent beamforming and an array deconvolution technique are evaluated. The results imply that an array of five radial line sensors, with equal azimuthal separation and an aperture that depends on the frequency band of interest, provides directional resolution while requiring less space compared to an equally effective array of five microbarometers with rosette wind filters.

A novel bio-safe phase separation process for preparing open-pore biodegradable polycaprolactone microparticles.

PubMed

Salerno, Aurelio; Domingo, Concepción

2014-09-01

Open-pore biodegradable microparticles are object of considerable interest for biomedical applications, particularly as cell and drug delivery carriers in tissue engineering and health care treatments. Furthermore, the engineering of microparticles with well definite size distribution and pore architecture by bio-safe fabrication routes is crucial to avoid the use of toxic compounds potentially harmful to cells and biological tissues. To achieve this important issue, in the present study a straightforward and bio-safe approach for fabricating porous biodegradable microparticles with controlled morphological and structural features down to the nanometer scale is developed. In particular, ethyl lactate is used as a non-toxic solvent for polycaprolactone particles fabrication via a thermal induced phase separation technique. The used approach allows achieving open-pore particles with mean particle size in the 150-250 μm range and a 3.5-7.9 m(2)/g specific surface area. Finally, the combination of thermal induced phase separation and porogen leaching techniques is employed for the first time to obtain multi-scaled porous microparticles with large external and internal pore sizes and potential improved characteristics for cell culture and tissue engineering. Samples were characterized to assess their thermal properties, morphology and crystalline structure features and textural properties. Copyright © 2014 Elsevier B.V. All rights reserved.

Modern separation techniques coupled to high performance mass spectrometry for glycolipid analysis.

PubMed

Sarbu, Mirela; Zamfir, Alina Diana

2018-01-21

Glycolipids (GLs), involved in biological processes and pathologies, such as viral, neurodegenerative and oncogenic transformations are in the focus of research related to method development for structural analysis. This review highlights modern separation techniques coupled to mass spectrometry (MS) for the investigation of GLs from various biological matrices. First section is dedicated to methods, which, although provide the separation in a non-liquid phase, are able to supply important data on the composition of complex mixtures. While classical thin layer chromatography (TLC) is useful for MS analyses of the fractionated samples, ultramodern ion mobility (IMS) characterized by high reproducibility facilitates to discover minor species and to apply low sample amounts, in addition to providing conformational separation with isomer discrimination. Second section highlights the advantages, applications and limitations of liquid-based separation techniques such as high performance liquid chromatography (HPLC) and hydrophilic interaction liquid chromatography (HILIC) in direct or indirect coupling to MS for glycolipidomics surveys. The on- and off-line capillary electrophoresis (CE) MS, offering a remarkable separation efficiency of GLs is also presented and critically assessed from the technical and application perspective in the final part of the review. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Molecular-level characterization of crude oil compounds combining reversed-phase high-performance liquid chromatography with off-line high-resolution mass spectrometry

USGS Publications Warehouse

Sim, Arum; Cho, Yunju; Kim, Daae; Witt, Matthias; Birdwell, Justin E.; Kim, Byung Ju; Kim, Sunghwan

2014-01-01

A reversed-phase separation technique was developed in a previous study (Loegel et al., 2012) and successfully applied to the de-asphalted fraction of crude oil. However, to the best of our knowledge, the molecular-level characterization of oil fractions obtained by reversed-phase high-performance liquid chromatography (HPLC) coupled with high-resolution mass spectrometry (MS) has not yet been reported. A detailed characterization of the oil fractions prepared by reversed-phase HPLC was performed in this study. HPLC fractionation was carried out on conventional crude oil and an oil shale pyrolysate. The analyses of the fractions showed that the carbon number of alkyl chains and the double bond equivalent (DBE) value were the major factors determining elution order. The compounds with larger DBE (presumably more condensed aromatic structures) and smaller carbon number (presumably compounds with short side chains) were eluted earlier but those compounds with lower DBE values (presumably less aromatic structures) and higher carbon number (presumably compounds with longer alkyl chains) eluted later in the chromatograms. This separation behavior is in good agreement with that expected from the principles of reversed-phase separation. The data presented in this study show that reversed-phase chromatography is effective in separating crude oil compounds and can be combined with ultrahigh-resolution MS data to better understand natural oils and oil shale pyrolysates.

Recent highlights in electro-driven separations- selected applications of alkylthiol gold nanoparticles in capillary electrophoresis and capillary electro-chromatography.

PubMed

Guihen, Elizabeth

2017-09-01

To date, alkylthiol gold nanoparticles (AuNPs) have been widely used in electro-chromatographic separation techniques as a viable alternative to traditional stationary phases. This is mainly due to their stability, chemical inertness, ease of functionality, increased phase ratio, ability to form self-assembled monolayers. They also yield versatile stationary phases with highly specific targeted functionalities. At the nanoscale region, the chemical and physical properties of a molecule display different attributes to that of the parent molecules or material, hence these features can be harnessed in electro-driven chromatographic separations. Application areas illustrating the use of AuNPs in separation science continue to grow and expand to cover many different kinds of analysis. The last decade has witnessed a successful trend in miniaturisation of chemical separation systems toward the micro and nanoscale ranges. Nanoparticle-based stationary phases fit well with performing chemical separations on microfluidic and capillary platforms. In this review the theory of the use of alkylthiol gold nanoparticles in electro-chromatographic driven separation methods will be discussed. This will be followed by details of recent and selected applications showing alkylthiol gold nanoparticles in capillary electrophoretic and open-tubular electro-chromatographic separations. This review will focus solely on alkylthiol based gold nanoparticles, therefore other kinds of chemical moieties bonded to gold nanoparticles are outside the scope of this review. Finally the future outlook of this exciting technology will be outlined in some detail in the final section. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Gradient stationary phase optimized selectivity liquid chromatography with conventional columns.

PubMed

Chen, Kai; Lynen, Frédéric; Szucs, Roman; Hanna-Brown, Melissa; Sandra, Pat

2013-05-21

Stationary phase optimized selectivity liquid chromatography (SOSLC) is a promising technique to optimize the selectivity of a given separation. By combination of different stationary phases, SOSLC offers excellent possibilities for method development under both isocratic and gradient conditions. The so far available commercial SOSLC protocol utilizes dedicated column cartridges and corresponding cartridge holders to build up the combined column of different stationary phases. The present work is aimed at developing and extending the gradient SOSLC approach towards coupling conventional columns. Generic tubing was used to connect short commercially available LC columns. Fast and base-line separation of a mixture of 12 compounds containing phenones, benzoic acids and hydroxybenzoates under both isocratic and linear gradient conditions was selected to demonstrate the potential of SOSLC. The influence of the connecting tubing on the deviation of predictions is also discussed.

Pressure-Induced Dissolution and Reentrant Formation of Condensed, Liquid-Liquid Phase-Separated Elastomeric α-Elastin.

PubMed

Cinar, Hasan; Cinar, Süleyman; Chan, Hue Sun; Winter, Roland

2018-05-08

We investigated the combined effects of temperature and pressure on liquid-liquid phase separation (LLPS) phenomena of α-elastin up to the multi-kbar regime. FT-IR spectroscopy, CD, UV/Vis absorption, phase-contrast light and fluorescence microscopy techniques were employed to reveal structural changes and mesoscopic phase states of the system. A novel pressure-induced reentrant LLPS was observed in the intermediate temperature range. A molecular-level picture, in particular on the role of hydrophobic interactions, hydration, and void volume in controlling LLPS phenomena is presented. The potential role of the LLPS phenomena in the development of early cellular compartmentalization is discussed, which might have started in the deep sea, where pressures up to the kbar level are encountered. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Characterization and compensation of the residual chirp in a Mach-Zehnder-type electro-optical intensity modulator.

PubMed

Rogers, C E; Carini, J L; Pechkis, J A; Gould, P L

2010-01-18

We utilize various techniques to characterize the residual phase modulation of a waveguide-based Mach-Zehnder electro-optical intensity modulator. A heterodyne technique is used to directly measure the phase change due to a given change in intensity, thereby determining the chirp parameter of the device. This chirp parameter is also measured by examining the ratio of sidebands for sinusoidal amplitude modulation. Finally, the frequency chirp caused by an intensity pulse on the nanosecond time scale is measured via the heterodyne signal. We show that this chirp can be largely compensated with a separate phase modulator. The various measurements of the chirp parameter are in reasonable agreement.

Characterization of Polysulfone Membranes Prepared with Thermally Induced Phase Separation Technique

NASA Astrophysics Data System (ADS)

Tiron, L. G.; Pintilie, Ș C.; Vlad, M.; Birsan, I. G.; Baltă, Ș

2017-06-01

Abstract Membrane technology is one of the most used water treatment technology because of its high removal efficiency and cost effectiveness. Preparation techniques for polymer membranes show an important aspect of membrane properties. Generally, polysulfone (PSf) and polyethersulfone (PES) are used for the preparation of ultrafiltration (UF) membranes. Polysulfone (PSf) membranes have been widely used for separation and purification of different solutions because of their excellent chemical and thermal stability. Polymeric membranes were obtained by phase inversion method. The polymer solution introduced in the nonsolvent bath (distilled water) initiate the evaporation of the solvent from the solution, this phenomenon has a strong influence on the transport properties. The effect of the coagulation bath temperature on the membrane properties is of interest for this study. Membranes are characterized by pure water flux, permeability, porosity and retention of methylene blue. The low temperature of coagulation bath improve the membrane’s rejection and its influence was most notable.

Characterising the structural properties of polymer separators for lithium-ion batteries in 3D using phase contrast X-ray microscopy

NASA Astrophysics Data System (ADS)

Finegan, Donal P.; Cooper, Samuel J.; Tjaden, Bernhard; Taiwo, Oluwadamilola O.; Gelb, Jeff; Hinds, Gareth; Brett, Dan J. L.; Shearing, Paul R.

2016-11-01

Separators are an integral component for optimising performance and safety of lithium-ion batteries; therefore, a clear understanding of how their microstructure affects cell performance and safety is crucial. Phase contrast X-ray microscopy is used here to capture the microstructures of commercial monolayer, tri-layer, and ceramic-coated lithium-ion battery polymer separators. Spatial variations in key structural parameters, including porosity, tortuosity factor and pore size distribution, are determined through the application of 3D quantification techniques and stereology. The architectures of individual layers in multi-layer membranes are characterised, revealing anisotropy in porosity, tortuosity factor and mean pore size of the three types of separator. Detailed structural properties of the individual layers of multi-layered membranes are then related with their expected effect on safety and rate capability of cells.

The design of a new concept chromatography column.

PubMed

Camenzuli, Michelle; Ritchie, Harald J; Ladine, James R; Shalliker, R Andrew

2011-12-21

Active Flow Management is a new separation technique whereby the flow of mobile phase and the injection of sample are introduced to the column in a manner that allows migration according to the principles of the infinite diameter column. A segmented flow outlet fitting allows for the separation of solvent or solute that elutes along the central radial section of the column from that of the sample or solvent that elutes along the wall region of the column. Separation efficiency on the analytical scale is increased by 25% with an increase in sensitivity by as much as 52% compared to conventional separations.

Phase Behavior of Ritonavir Amorphous Solid Dispersions during Hydration and Dissolution.

PubMed

Purohit, Hitesh S; Taylor, Lynne S

2017-12-01

The aim of this research was to study the interplay of solid and solution state phase transformations during the dissolution of ritonavir (RTV) amorphous solid dispersions (ASDs). RTV ASDs with polyvinylpyrrolidone (PVP), polyvinylpyrrolidone vinyl acetate (PVPVA) and hydroxypropyl methylcellulose acetate succinate (HPMCAS) were prepared at 10-50% drug loading by solvent evaporation. The miscibility of RTV ASDs was studied before and after exposure to 97% relative humidity (RH). Non-sink dissolution studies were performed on fresh and moisture-exposed ASDs. RTV and polymer release were monitored using ultraviolet-visible spectroscopy. Techniques including fluorescence spectroscopy, confocal imaging, scanning electron microscopy (SEM), atomic force microscopy (AFM), differential scanning calorimetry (DSC) and nanoparticle tracking analysis (NTA) were utilized to monitor solid and the solution state phase transformations. All RTV-PVP and RTV-PVPVA ASDs underwent moisture-induced amorphous-amorphous phase separation (AAPS) on high RH storage whereas RTV-HPMCAS ASDs remained miscible. Non-sink dissolution of PVP- and PVPVA-based ASDs at low drug loadings led to rapid RTV and polymer release resulting in concentrations in excess of amorphous solubility, liquid-liquid phase separation (LLPS) and amorphous nanodroplet formation. High drug loading PVP- and PVPVA-based ASDs did not exhibit LLPS upon dissolution as a consequence of extensive AAPS in the hydrated ASD matrix. All RTV-HPMCAS ASDs led to LLPS upon dissolution. RTV ASD dissolution is governed by a competition between the dissolution rate and the rate of phase separation in the hydrated ASD matrix. LLPS was observed for ASDs where the drug release was polymer controlled and only ASDs that remained miscible during the initial phase of dissolution led to LLPS. Techniques such as fluorescence spectroscopy, confocal imaging and SEM were useful in understanding the phase behavior of ASDs upon hydration and dissolution and were helpful in elucidating the mechanism of generation of amorphous nanodroplets.

Hygroscopic and phase separation properties of ammonium sulfate/organic/water ternary solutions

NASA Astrophysics Data System (ADS)

Zawadowicz, M. A.; Proud, S. R.; Seppalainen, S. S.; Cziczo, D. J.

2015-03-01

Atmospheric aerosol particles are often partially or completely composed of inorganic salts, such as ammonium sulfate and sodium chloride, and therefore exhibit hygroscopic properties. Many inorganic salts have well-defined deliquescence and efflorescence points at which they take up and lose water, respectively. Deliquescence and efflorescence of simple inorganic salt particles have been investigated by a variety of methods, such as IR spectroscopy, tandem mobility analysis and electrodynamic balance. Field measurements have shown that atmospheric aerosols are not typically pure inorganic salt, instead they often also contain organic species. There is ample evidence from laboratory studies that suggests that mixed particles exist in a phase-separated state, with an aqueous inorganic core and organic shell. Although phase separation has not been measured in situ, there is no reason it would not also take place in the atmosphere. Many recent studies have focused on microscopy techniques that require deposition of the aerosol on a glass slide, possibly changing its surface properties. Here, we investigate the deliquescence and efflorescence points, phase separation and ability to exchange gas-phase components of mixed organic and inorganic aerosol using a flow tube coupled with FTIR spectroscopy. Ammonium sulfate aerosol mixed with organic polyols with different O : C ratios, including 1,4-butanediol, glycerol, 1,2,6-hexanetriol, 1,2-hexanediol, and 1,5-pentanediol have been investigated. Those constituents correspond to materials found in the atmosphere in great abundance, and therefore, particles prepared in this study should mimic atmospheric mixed phase aerosol particles. The results of this study tend to be in agreement with previous microscopy experiments, with several key differences, which possibly reveal a size-dependent effect on phase separation in organic/inorganic aerosol particles.

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.

LC-MS/MS signal suppression effects in the analysis of pesticides in complex environmental matrices.

PubMed

Choi, B K; Hercules, D M; Gusev, A I

2001-02-01

The application of LC separation and mobile phase additives in addressing LC-MS/MS matrix signal suppression effects for the analysis of pesticides in a complex environmental matrix was investigated. It was shown that signal suppression is most significant for analytes eluting early in the LC-MS analysis. Introduction of different buffers (e.g. ammonium formate, ammonium hydroxide, formic acid) into the LC mobile phase was effective in improving signal correlation between the matrix and standard samples. The signal improvement is dependent on buffer concentration as well as LC separation of the matrix components. The application of LC separation alone was not effective in addressing suppression effects when characterizing complex matrix samples. Overloading of the LC column by matrix components was found to significantly contribute to analyte-matrix co-elution and suppression of signal. This signal suppression effect can be efficiently compensated by 2D LC (LC-LC) separation techniques. The effectiveness of buffers and LC separation in improving signal correlation between standard and matrix samples is discussed.

Phase behaviour of disordered proteins underlying low density and high permeability of liquid organelles

NASA Astrophysics Data System (ADS)

Wei, Ming-Tzo; Elbaum-Garfinkle, Shana; Holehouse, Alex S.; Chen, Carlos Chih-Hsiung; Feric, Marina; Arnold, Craig B.; Priestley, Rodney D.; Pappu, Rohit V.; Brangwynne, Clifford P.

2017-11-01

Many intracellular membraneless organelles form via phase separation of intrinsically disordered proteins (IDPs) or regions (IDRs). These include the Caenorhabditis elegans protein LAF-1, which forms P granule-like droplets in vitro. However, the role of protein disorder in phase separation and the macromolecular organization within droplets remain elusive. Here, we utilize a novel technique, ultrafast-scanning fluorescence correlation spectroscopy, to measure the molecular interactions and full coexistence curves (binodals), which quantify the protein concentration within LAF-1 droplets. The binodals of LAF-1 and its IDR display a number of unusual features, including 'high concentration' binodal arms that correspond to remarkably dilute droplets. We find that LAF-1 and other in vitro and intracellular droplets are characterized by an effective mesh size of ∼3-8 nm, which determines the size scale at which droplet properties impact molecular diffusion and permeability. These findings reveal how specific IDPs can phase separate to form permeable, low-density (semi-dilute) liquids, whose structural features are likely to strongly impact biological function.

Ground-water contamination by organic bases derived from coal-tar wastes

USGS Publications Warehouse

Pereira, Wilfred E.; Rostad, Colleen E.; Garbarino, John R.; Hult, Marc F.

1983-01-01

A fluid sample from a shallow aquifer contaminated by coal-tar wastes was analyzed for organic bases. The sample consisted of a mixture of aqueous and oily-tar phases. The phases were separated by centrifugation and filtration. Organic bases were isolated from each phase by pH adjustment and solvent extraction. Organic bases in the oily-tar phase were further purified by neutral-alumina, micro-column adsorption chromatography. Separation and identification of the organic bases in each phase were achieved by using capillary gas chromatography-mass spectrometry-computer (GC-MS-COM) and probe distillation-high resolution mass spectrometry (PD-HRMS) techniques. Organic bases present in the aqueous phase included primary aromatic amines (such as aniline, alkylated anilines, and naphthylamines) as well as azaarenes (such as alkylated pyridines, quinolines, acridine, and benzoquinolines). The oily-tar phase contained acridine, benzacridines, dibenzacridines, and numerous other azaarenes, the elemental compositions of which were determined by PD-HRMS. Azaarenes in the oily-tar phase, varying in size from 6 to 12 rings, are reported for the first time. The origin and environmental significance of these compounds are discussed.

Groundwater contamination by organic bases derived from coal-tar wastes

USGS Publications Warehouse

Pereira, W.E.; Rostad, C.E.; Garbarino, J.R.; Hult, M.F.

1983-01-01

A fluid sample from a shallow aquifer contaminated by coal-tar wastes was analyzed for organic bases. The sample consisted of a mixture of aqueous and oily-tar phases. The phases were separated by centrifugation and filtration. Organic bases were isolated from each phase by pH adjustment and solvent extraction. Organic bases in the oily-tar phase were further purified by neutral-alumina, micro-column adsorption chromatography. Separation and identification of the organic bases in each phase were achieved by using capillary gas chromatography-mass spectrometry-computer (GC-MS-COM) and probe distillation-high resolution mass spectrometry (PD-HRMS) techniques. Organic bases present in the aqueous phase included primary aromatic amines (such as aniline, alkylated anilines, and naphthylamines) as well as azaarenes (such as alkylated pyridines, quinolines, acridine, and benzoquinolines). The oily-tar phase contained acridine, benzacridines, dibenzacridines, and numerous other azaarenes, the elemental compositions of which were determined by PD-HRMS. Azaarenes in the oily-tar phase, varying in size from 6 to 12 rings, are reported for the first time. The origin and environmental significance of these compounds are discussed. ?? 1983.

Separation of lymphocytes by electrophoresis under terrestrial conditions and at zero gravity, phase 3

NASA Technical Reports Server (NTRS)

Rubin, A. L.; Stenzel, K. H.; Cheigh, J. S.; Seaman, G. V. F.; Novogrodsky, A.

1977-01-01

Electrophoretic mobilities (EPM) of peripheral lymphocytes were studied from normal subjects, chronic hemodialysis patients and kidney transplant recipients. A technique to separate B lymphocytes and null cells from non-T lymphocyte preparation was developed. The experiments were designed to determine which subpopulation of the non-T lymphocytes is primarily affected and shows a decreased EPM in chronic hemodialysis patients and kidney transplant recipients.

Using dynamic interferometric synthetic aperature radar (InSAR) to image fast-moving surface waves

DOEpatents

Vincent, Paul

2005-06-28

A new differential technique and system for imaging dynamic (fast moving) surface waves using Dynamic Interferometric Synthetic Aperture Radar (InSAR) is introduced. This differential technique and system can sample the fast-moving surface displacement waves from a plurality of moving platform positions in either a repeat-pass single-antenna or a single-pass mode having a single-antenna dual-phase receiver or having dual physically separate antennas, and reconstruct a plurality of phase differentials from a plurality of platform positions to produce a series of desired interferometric images of the fast moving waves.

On diagrammatic technique for nonlinear dynamical systems

NASA Astrophysics Data System (ADS)

Semenyakin, Mykola

2014-11-01

In this paper, we investigate phase flows over ℂn and ℝn generated by vector fields V = ∑ Pi∂i where Pi are finite degree polynomials. With the convenient diagrammatic technique, we get expressions for evolution operators ev{V|t} : x(0) ↦ x(t) through the series in powers of x(0) and t, represented as sum over all trees of a particular type. Estimates are made for the radius of convergence in some particular cases. The phase flows behavior in the neighborhood of vector field fixed points are examined. Resonance cases are considered separately.

Evaluation of Wet Chemical ICP-AES Elemental Analysis Methods usingSimulated Hanford Waste Samples-Phase I Interim Report

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

Coleman, Charles J.; Edwards, Thomas B.

2005-04-30

The wet chemistry digestion method development for providing process control elemental analyses of the Hanford Tank Waste Treatment and Immobilization Plant (WTP) Melter Feed Preparation Vessel (MFPV) samples is divided into two phases: Phase I consists of: (1) optimizing digestion methods as a precursor to elemental analyses by ICP-AES techniques; (2) selecting methods with the desired analytical reliability and speed to support the nine-hour or less turnaround time requirement of the WTP; and (3) providing baseline comparison to the laser ablation (LA) sample introduction technique for ICP-AES elemental analyses that is being developed at the Savannah River National Laboratory (SRNL).more » Phase II consists of: (1) Time-and-Motion study of the selected methods from Phase I with actual Hanford waste or waste simulants in shielded cell facilities to ensure that the methods can be performed remotely and maintain the desired characteristics; and (2) digestion of glass samples prepared from actual Hanford Waste tank sludge for providing comparative results to the LA Phase II study. Based on the Phase I testing discussed in this report, a tandem digestion approach consisting of sodium peroxide fusion digestions carried out in nickel crucibles and warm mixed-acid digestions carried out in plastic bottles has been selected for Time-and-Motion study in Phase II. SRNL experience with performing this analytical approach in laboratory hoods indicates that well-trained cell operator teams will be able to perform the tandem digestions in five hours or less. The selected approach will produce two sets of solutions for analysis by ICP-AES techniques. Four hours would then be allocated for performing the ICP-AES analyses and reporting results to meet the nine-hour or less turnaround time requirement. The tandem digestion approach will need to be performed in two separate shielded analytical cells by two separate cell operator teams in order to achieve the nine-hour or less turnaround time. Because of the simplicity of the warm mixed-acid method, a well-trained cell operator team may in time be able to perform both sets of digestions. However, having separate shielded cells for each of the methods is prudent to avoid overcrowding problems that would impede a minimal turnaround time.« less

Preparative separation and identification of novel subsidiary colors of the color additive D&C Red No. 33 (Acid Red 33) using spiral high-speed counter-current chromatography☆

PubMed Central

Weisz, Adrian; Ridge, Clark D.; Mazzola, Eugene P.; Ito, Yoichiro

2015-01-01

Three low-level subsidiary color impurities (A, B, and C) often present in batches of the color additive D&C Red No. 33 (R33, Acid Red 33, Colour Index No. 17200) were separated from a portion of R33 by spiral high-speed counter-current chromatography (HSCCC). The separation involved use of a very polar solvent system, 1-BuOH/5 mM aq. (NH4)2SO4. Addition of ammonium sulfate to the lower phase forced partition of the components into the upper phase, thereby eliminating the need to add a hydrophobic counterion as was previously required for separations of components from sulfonated dyes. The very polar solvent system used would not have been retained in a conventional multi-layer coil HSCCC instrument, but the spiral configuration enabled retention of the stationary phase, and thus, the separation was possible. A 1 g portion of R33 enriched in A, B, and C was separated using the upper phase of the solvent system as the mobile phase. The retention of the stationary phase was 38.1%, and the separation resulted in 4.8 mg of A of >90% purity, 18.3 mg of B of >85% purity, and 91 mg of C of 65–72% purity. A second separation of a portion of the C mixture resulted in 7 mg of C of >94% purity. The separated impurities were identified by high-resolution mass spectrometry and NMR spectroscopic techniques as follows: 5-amino-3-biphenyl-3-ylazo-4-hydroxy-naphthalene-2,7-disulfonic acid, A; 5-amino-4-hydroxy-6-phenyl-3-phenylazo-naphthalene-2,7-disulfonic acid, B; and 5-amino-4-hydroxy-3,6-bis-phenylazo-naphthalene-2,7-disulfonic acid, C. The isomers A and B are compounds reported for the first time. Application of the spiral HSCCC method resulted in the additional benefit of yielding 930 mg of the main component of R33, 5-amino-4-hydroxy-3-phenylazo-naphthalene-2,7-disulfonic acid, of >97% purity. PMID:25591404

Preparative separation and identification of novel subsidiary colors of the color additive D&C Red No. 33 (Acid Red 33) using spiral high-speed counter-current chromatography.

PubMed

Weisz, Adrian; Ridge, Clark D; Mazzola, Eugene P; Ito, Yoichiro

2015-02-06

Three low-level subsidiary color impurities (A, B, and C) often present in batches of the color additive D&C Red No. 33 (R33, Acid Red 33, Colour Index No. 17200) were separated from a portion of R33 by spiral high-speed counter-current chromatography (HSCCC). The separation involved use of a very polar solvent system, 1-BuOH/5mM aq. (NH4)2SO4. Addition of ammonium sulfate to the lower phase forced partition of the components into the upper phase, thereby eliminating the need to add a hydrophobic counterion as was previously required for separations of components from sulfonated dyes. The very polar solvent system used would not have been retained in a conventional multi-layer coil HSCCC instrument, but the spiral configuration enabled retention of the stationary phase, and thus, the separation was possible. A 1g portion of R33 enriched in A, B, and C was separated using the upper phase of the solvent system as the mobile phase. The retention of the stationary phase was 38.1%, and the separation resulted in 4.8 mg of A of >90% purity, 18.3mg of B of >85% purity, and 91 mg of C of 65-72% purity. A second separation of a portion of the C mixture resulted in 7 mg of C of >94% purity. The separated impurities were identified by high-resolution mass spectrometry and NMR spectroscopic techniques as follows: 5-amino-3-biphenyl-3-ylazo-4-hydroxy-naphthalene-2,7-disulfonic acid, A; 5-amino-4-hydroxy-6-phenyl-3-phenylazo-naphthalene-2,7-disulfonic acid, B; and 5-amino-4-hydroxy-3,6-bis-phenylazo-naphthalene-2,7-disulfonic acid, C. The isomers A and B are compounds reported for the first time. Application of the spiral HSCCC method resulted in the additional benefit of yielding 930 mg of the main component of R33, 5-amino-4-hydroxy-3-phenylazo-naphthalene-2,7-disulfonic acid, of >97% purity. Published by Elsevier B.V.

Controlling phase separation in vanadium dioxide thin films via substrate engineering

NASA Astrophysics Data System (ADS)

Gilbert Corder, Stephanie N.; Jiang, Jianjuan; Chen, Xinzhong; Kittiwatanakul, Salinporn; Tung, I.-Cheng; Zhu, Yi; Zhang, Jiawei; Bechtel, Hans A.; Martin, Michael C.; Carr, G. Lawrence; Lu, Jiwei; Wolf, Stuart A.; Wen, Haidan; Tao, Tiger H.; Liu, Mengkun

2017-10-01

The strong electron-lattice interactions in correlated electron systems provide unique opportunities for altering the material properties with relative ease and flexibility. In this Rapid Communication, we use localized strain control via a focused-ion-beam patterning of Ti O2 substrates to demonstrate that one can selectively engineer the insulator-to-metal transition temperature, the fractional component of the insulating and metallic phases, and the degree of optical anisotropy down to the length scales of the intrinsic phase separation in V O2 thin films without altering the quality of the films. The effects of localized strain control on the strongly correlated electron system are directly visualized by state-of-the-art IR near-field imaging and spectroscopy techniques and x-ray microdiffraction measurements.

Controlling phase separation in vanadium dioxide thin films via substrate engineering

DOE PAGES

Gilbert Corder, Stephanie N.; Jiang, Jianjuan; Chen, Xinzhong; ...

2017-10-23

The strong electron-lattice interactions in correlated electron systems provide unique opportunities for altering the material properties with relative ease and flexibility. Here in this Rapid Communication, we use localized strain control via a focused-ion-beam patterning of TiO 2 substrates to demonstrate that one can selectively engineer the insulator-to-metal transition temperature, the fractional component of the insulating and metallic phases, and the degree of optical anisotropy down to the length scales of the intrinsic phase separation in VO 2 thin films without altering the quality of the films. The effects of localized strain control on the strongly correlated electron system aremore » directly visualized by state-of-the-art IR near-field imaging and spectroscopy techniques and x-ray microdiffraction measurements.« less

Unweighted least squares phase unwrapping by means of multigrid techniques

NASA Astrophysics Data System (ADS)

Pritt, Mark D.

1995-11-01

We present a multigrid algorithm for unweighted least squares phase unwrapping. This algorithm applies Gauss-Seidel relaxation schemes to solve the Poisson equation on smaller, coarser grids and transfers the intermediate results to the finer grids. This approach forms the basis of our multigrid algorithm for weighted least squares phase unwrapping, which is described in a separate paper. The key idea of our multigrid approach is to maintain the partial derivatives of the phase data in separate arrays and to correct these derivatives at the boundaries of the coarser grids. This maintains the boundary conditions necessary for rapid convergence to the correct solution. Although the multigrid algorithm is an iterative algorithm, we demonstrate that it is nearly as fast as the direct Fourier-based method. We also describe how to parallelize the algorithm for execution on a distributed-memory parallel processor computer or a network-cluster of workstations.

Wire-mesh sensor, ultrasound and high-speed videometry applied for the characterization of horizontal gas-liquid slug flow

NASA Astrophysics Data System (ADS)

Ofuchi, C. Y.; Morales, R. E. M.; Arruda, L. V. R.; Neves, F., Jr.; Dorini, L.; do Amaral, C. E. F.; da Silva, M. J.

2012-03-01

Gas-liquid flows occur in a broad range of industrial applications, for instance in chemical, petrochemical and nuclear industries. Correct understating of flow behavior is crucial for safe and optimized operation of equipments and processes. Thus, measurement of gas-liquid flow plays an important role. Many techniques have been proposed and applied to analyze two-phase flows so far. In this experimental research, data from a wire-mesh sensor, an ultrasound technique and high-speed camera are used to study two-phase slug flows in horizontal pipes. The experiments were performed in an experimental two-phase flow loop which comprises a horizontal acrylic pipe of 26 mm internal diameter and 9 m length. Water and air were used to produce the two-phase flow and their flow rates are separately controlled to produce different flow conditions. As a parameter of choice, translational velocity of air bubbles was determined by each of the techniques and comparatively evaluated along with a mechanistic flow model. Results obtained show good agreement among all techniques. The visualization of flow obtained by the different techniques is also presented.

Quantitative Phase Imaging in a Volume Holographic Microscope

NASA Astrophysics Data System (ADS)

Waller, Laura; Luo, Yuan; Barbastathis, George

2010-04-01

We demonstrate a method for quantitative phase imaging in a Volume Holographic Microscope (VHM) from a single exposure, describe the properties of the system and show experimental results. The VHM system uses a multiplexed volume hologram (VH) to laterally separate images from different focal planes. This 3D intensity information is then used to solve the transport of intensity (TIE) equation and recover phase quantitatively. We discuss the modifications to the technique that were made in order to give accurate results.

Use of a Ceramic Membrane to Improve the Performance of Two-Separate-Phase Biocatalytic Membrane Reactor.

PubMed

Ranieri, Giuseppe; Mazzei, Rosalinda; Wu, Zhentao; Li, Kang; Giorno, Lidietta

2016-03-14

Biocatalytic membrane reactors (BMR) combining reaction and separation within the same unit have many advantages over conventional reactor designs. Ceramic membranes are an attractive alternative to polymeric membranes in membrane biotechnology due to their high chemical, thermal and mechanical resistance. Another important use is their potential application in a biphasic membrane system, where support solvent resistance is highly needed. In this work, the preparation of asymmetric ceramic hollow fibre membranes and their use in a two-separate-phase biocatalytic membrane reactor will be described. The asymmetric ceramic hollow fibre membranes were prepared using a combined phase inversion and sintering technique. The prepared fibres were then used as support for lipase covalent immobilization in order to develop a two-separate-phase biocatalytic membrane reactor. A functionalization method was proposed in order to increase the density of the reactive hydroxyl groups on the surface of ceramic membranes, which were then amino-activated and treated with a crosslinker. The performance and the stability of the immobilized lipase were investigated as a function of the amount of the immobilized biocatalytst. Results showed that it is possible to immobilize lipase on a ceramic membrane without altering its catalytic performance (initial residual specific activity 93%), which remains constant after 6 reaction cycles.

Incorporating an Electrode Modification Layer with a Vertical Phase Separated Photoactive Layer for Efficient and Stable Inverted Nonfullerene Polymer Solar Cells.

PubMed

Shi, Zhenzhen; Liu, Hao; Wang, Yaping; Li, Jinyan; Bai, Yiming; Wang, Fuzhi; Bian, Xingming; Hayat, Tasawar; Alsaedi, Ahmed; Tan, Zhan'ao

2017-12-20

For bulk heterojunction polymer solar cells (PSCs), the donors and acceptors featuring specific phase separation and concentration distribution within the electron donor/acceptor blends crucially affect the exciton dissociation and charge transportation. Herein, efficient and stable nonfullerene inverted PSCs incorporating a phase separated photoactive layer and a titanium chelate electrode modification layer are demonstrated. Water contact angle (WCA), scanning kelvin probe microscopy (SKPM), and atomic force microscopy (AFM) techniques are implemented to characterize the morphology of photoactive layers. Compared with the control conventional device, the short-circuit current density (J sc ) is enhanced from 14.74 to 17.45 mAcm -2 . The power conversion efficiency (PCE) for the inverted PSCs with a titanium (diisopropoxide)-bis-(2,4-pentanedionate) (TIPD) layer increases from 9.67% to 11.69% benefiting from the declined exciton recombination and fairly enhanced charge transportation. Furthermore, the nonencapsulated inverted device with a TIPD layer demonstrates the best long-term stability, 85% of initial PCE remaining and an almost undecayed open-circuit voltage (V oc ) after 1440 h. Our results reveal that the titanium chelate is an excellent electrode modification layer to incorporate with a vertical phase separated photoactive layer for producing high-efficiency and high-stability inverted nonfullerene PSCs.

Ultra-wideband microwave photonic phase shifter with configurable amplitude response.

PubMed

Pagani, M; Marpaung, D; Eggleton, B J

2014-10-15

We introduce a new principle that enables separate control of the amplitude and phase of an optical carrier, simply by controlling the power of two stimulated Brillouin scattering (SBS) pumps. This technique is used to implement a microwave photonic phase shifter with record performance, which solves the bandwidth limitation of previous gain-transparent SBS-based phase shifters, while achieving unprecedented minimum power fluctuations, as a function of phase shift. We demonstrate 360° continuously tunable phase shift, with less than 0.25 dB output power fluctuations, over a frequency band from 1.5 to 31 GHz, limited only by the measurement equipment.

Recent advances in micro-scale and nano-scale high-performance liquid-phase chromatography for proteome research.

PubMed

Tao, Dingyin; Zhang, Lihua; Shan, Yichu; Liang, Zhen; Zhang, Yukui

2011-01-01

High-performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI-MS-MS) is regarded as one of the most powerful techniques for separation and identification of proteins. Recently, much effort has been made to improve the separation capacity, detection sensitivity, and analysis throughput of micro- and nano-HPLC, by increasing column length, reducing column internal diameter, and using integrated techniques. Development of HPLC columns has also been rapid, as a result of the use of submicrometer packing materials and monolithic columns. All these innovations result in clearly improved performance of micro- and nano-HPLC for proteome research.

Studies on aqueous two phase polymer systems useful for partitioning of biological materials

NASA Technical Reports Server (NTRS)

Brooks, D. E.; Bamberger, S.

1982-01-01

The two phase systems that result when aqueous solutions of dextran and poly(ethylene glycol) (PEG) are mixed above a critical concentration of a few percent provide a useful medium for the separation of biological cell subpopulations via partition between the top, PEG-rich phase and the liquid-liquid phase boundary. Interfacial tensions of such systems have been measured by the rotating drop technique and found to range between 0.1-100 micro-N/m. The tension was found to depend on the length of the tie line describing the system on a phase diagram, via a power law relationship which differed depending on the concentration of Na phosphate buffer present. The electrokinetic properties of drops of one phase suspended in the other were studied for a variety of systems. It was found that the droplet electrophoretic mobility increased monotonically with phosphate concentration and drop diameter but exhibited the opposite sign from that anticipated from phosphate partition measurements. It was possible to take advantage of these electrokinetic properties and dramatically enhance the speed of phase separation through application of relatively small electric fields.

Homomorphic filtering textural analysis technique to reduce multiplicative noise in the 11Oba nano-doped liquid crystalline compounds

NASA Astrophysics Data System (ADS)

Madhav, B. T. P.; Pardhasaradhi, P.; Manepalli, R. K. N. R.; Pisipati, V. G. K. M.

2015-07-01

The compound undecyloxy benzoic acid (11Oba) exhibits nematic and smectic-C phases while a nano-doped undecyloxy benzoic acid with ZnO exhibits the same nematic and smectic-C phases with reduced clearing temperature as expected. The doping is done with 0.5% and 1% ZnO molecules. The clearing temperatures are reduced by approximately 4 ° and 6 °, respectively (differential scanning calorimeter data). While collecting the images from a polarizing microscope connected with hot stage and camera, the illumination and reflectance combined multiplicatively and the image quality was reduced to identify the exact phase in the compound. A novel technique of homomorphic filtering is used in this manuscript through which multiplicative noise components of the image are separated linearly in the frequency domain. This technique provides a frequency domain procedure to improve the appearance of an image by gray level range compression and contrast enhancement.

Development of Electrospun Nanomaterials and their Applications in Separation Science

NASA Astrophysics Data System (ADS)

Newsome, Toni Elwell

In separations, efficiency is inversely related to the diameter of the sorbent particles of the stationary phase. Thus, materials research in separation science has primarily been directed towards reducing the diameter of the sorbent particle used in the stationary phase. In this dissertation, innovative methods designed for the fabrication and application of electrospun sorbent nanomaterials for separation science are described. Electrospinning is a facile, cost-effective technique that relies on repulsive electrostatic forces to produce nanofibers from a viscoelastic solution. Here, electrospinning is used to generate polymer, carbon, and silica-based nanofibers which are employed as sorbent nanomaterials in extractions and separations. Electrospun carbon nanofibers have proven to be ideal extractive phases for solid-phase microextraction (SPME) when coupled to gas chromatography (GC) for headspace sampling of volatile analytes. Herein, these carbon nanofibers were employed in the direct extraction of nonvolatile analytes and coupled to liquid chromatography (LC) for the first time. The high surface area of the coatings led to enhanced extraction efficiencies; they offered a 3-33 fold increase in efficiency relative to a commercial SPME phase. Carbon nanofibers proved to be stable when immersed in liquids common to LC demonstrating the enhanced stability of these coatings in SPME coupled to LC relative to conventional SPME fibers. The enhanced chemical and mechanical stability of the carbon SPME coatings considerably expanded the range of compounds applicable to SPME and extended the lifetimes of the fibers. Electrospun nanofibers have also proven to be ideal stationary phases in ultra-thin layer chromatography (UTLC). Nanofibers provide faster separations and enhanced separation efficiencies compared to commercial particle-based stationary phases in a relatively short distance. Here, the electrospun-UTLC technology was extended for the first time to nanofibers composed of silica, the most commonly used surface for TLC. An electrospinning method was optimized to produce silica-based nanofibers with the smallest diameter possible (300-380 nm) while maintaining homogenous nanofiber morphology. Highly efficient separations were performed in 15 mm with observed plate heights as low as 8.6 mum. Silica-based nanofibers proved to be chemically stable with a wide variety of TLC reagents demonstrating the enhanced compatibility of these phases with common TLC methods relative to polymer and carbon nanofiber UTLC plates. The extension of electrospun UTLC to silica-based nanofibers vastly expanded the range of analytes and TLC methods which can be used with this technology. The main disadvantage of conventional TLC development methods is that the mobile phase velocity decreases with increasing separation distance. Here, the chromatographic performance of electrospun polymer stationary phases was further improved by using a forced-flow mobile phase in planar electrochromatography (PEC) in which mobile phase velocity does not diminish with increasing distance. Separations were performed on polymer nanofiber UTLC plates in 1-2 min. Compared to UTLC, PEC offered unique selectivity, decreased analysis times (> 4 times faster), and enhanced efficiency (2-3 times lower plate height). In addition, two-dimensional (2D) separations of a complex analyte mixture using UTLC followed by PEC required only 11 min and exhibited a significant increase in separation number (70-77).

Suppression of the antiferromagnetic order when approaching the superconducting state in a phase-separated crystal of K x Fe 2 - y Se 2

DOE PAGES

Li, Shichao; Gan, Yuan; Wang, Jinghui; ...

2017-09-06

Here, we combined elastic and inelastic neutron scattering techniques, magnetic susceptibility, and resistivity measurements to study single-crystal samples of K xFe 2-ySe 2, which contain the superconducting phase that has a transition temperature of ~31 K. In the inelastic neutron scattering measurements, we also observe both the spin-wave excitations resulting from the block antiferromagnetic ordered phase and the resonance that is associated with the superconductivity in the superconducting phase, demonstrating the coexistence of these two orders. From the temperature dependence of the intensity of the magnetic Bragg peaks, we find that well before entering the superconducting state, the development ofmore » the magnetic order is interrupted, at ~42 K. We consider this result to be evidence for the physical separation of the antiferromagnetic and superconducting phases; the suppression is possibly due to the proximity effect of the superconducting fluctuations on the antiferromagnetic order.« less

Suppression of the antiferromagnetic order when approaching the superconducting state in a phase-separated crystal of K x Fe 2 - y Se 2

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

Li, Shichao; Gan, Yuan; Wang, Jinghui

Here, we combined elastic and inelastic neutron scattering techniques, magnetic susceptibility, and resistivity measurements to study single-crystal samples of K xFe 2-ySe 2, which contain the superconducting phase that has a transition temperature of ~31 K. In the inelastic neutron scattering measurements, we also observe both the spin-wave excitations resulting from the block antiferromagnetic ordered phase and the resonance that is associated with the superconductivity in the superconducting phase, demonstrating the coexistence of these two orders. From the temperature dependence of the intensity of the magnetic Bragg peaks, we find that well before entering the superconducting state, the development ofmore » the magnetic order is interrupted, at ~42 K. We consider this result to be evidence for the physical separation of the antiferromagnetic and superconducting phases; the suppression is possibly due to the proximity effect of the superconducting fluctuations on the antiferromagnetic order.« less

WE-G-18C-07: Accelerated Water/fat Separation in MRI for Radiotherapy Planning Using Multi-Band Imaging Techniques

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

Crijns, S; Stemkens, B; Sbrizzi, A

Purpose: Dixon sequences are used to characterize disease processes, obtain good fat or water separation in cases where fat suppression fails and to obtain pseudo-CT datasets. Dixon's method uses at least two images acquired with different echo times and thus requires prolonged acquisition times. To overcome associated problems (e.g., for DCE/cine-MRI), we propose to use a method for water/fat separation based on spectrally selective RF pulses. Methods: Two alternating RF pulses were used, that imposes a fat selective phase cycling over the phase encoding lines, which results in a spatial shift for fat in the reconstructed image, identical to thatmore » in CAIPIRINHA. Associated aliasing artefacts were resolved using the encoding power of a multi-element receiver array, analogous to SENSE. In vivo measurements were performed on a 1.5T clinical MR-scanner in a healthy volunteer's legs, using a four channel receiver coil. Gradient echo images were acquired with TE/TR = 2.3/4.7ms, flip angle 20°, FOV 45×22.5cm{sup 2}, matrix 480×216, slice thickness 5mm. Dixon images were acquired with TE,1/TE,2/TR=2.2/4.6/7ms. All image reconstructions were done in Matlab using the ReconFrame toolbox (Gyrotools, Zurich, CH). Results: RF pulse alternation yields a fat image offset from the water image. Hence the water and fat images fold over, which is resolved using in-plane SENSE reconstruction. Using the proposed technique, we achieved excellent water/fat separation comparable to Dixon images, while acquiring images at only one echo time. Conclusion: The proposed technique yields both inphase water and fat images at arbitrary echo times and requires only one measurement, thereby shortening the acquisition time by a factor 2. In future work the technique may be extended to a multi-band water/fat separation sequence that is able to achieve single point water/fat separation in multiple slices at once and hence yields higher speed-up factors.« less

Paired-ion chromatography and high performance liquid chromatography of labetalol in feeds.

PubMed

Townley, E R; Ross, B

1980-11-01

A high performance liquid chromatographic (HPLC) method using reverse phase paired-ion chromatography and ultraviolet detection at 280 nm has been developed to determine labetalol, an alpha and beta adrenoceptor blocking agent, in Purina No. 5001 rodent chow. The method is simple and rapid, and demonstrates a separation technique applicable to other acidic and basic drugs. It requires only extraction of the drug with methanol--water--acetic acid (66 + 33 + 1) and separation of insoluble material by filtration before HPLC. Labetalol, is chromatographically separated from soluble feed components by means of a microBondapak C18 column and methanol--water--acetic acid (66 + 33 + 1) mobile phase, 0.005M with respect to sodium dioctylsulfosuccinate paired-ion reagent. Average recovery is 98.7% with a relative standard deviation of +/- 2.3% for the equipment described.

Pressurized capillary electrochromatographic analysis of water-soluble vitamins by combining with on-line concentration technique.

PubMed

Jia, Li; Liu, Yaling; Du, Yanyan; Xing, Da

2007-06-22

A pressurized capillary electrochromatography (pCEC) system was developed for the separation of water-soluble vitamins, in which UV absorbance was used as the detection method and a monolithic silica-ODS column as the separation column. The parameters (type and content of organic solvent in the mobile phase, type and concentration of electrolyte, pH of the electrolyte buffer, applied voltage and flow rate) affecting the separation resolution were evaluated. The combination of two on-line concentration techniques, namely, solvent gradient zone sharpening effect and field-enhanced sample stacking, was utilized to improve detection sensitivity, which proved to be beneficial to enhance the detection sensitivity by enabling the injection of large volumes of samples. Coupling electrokinetic injection with the on-line concentration techniques was much more beneficial for the concentration of positively charged vitamins. Comparing with the conventional injection mode, the enhancement in the detection sensitivities of water-soluble vitamins using the on-line concentration technique is in the range of 3 to 35-fold. The developed pCEC method was applied to evaluate water-soluble vitamins in corns.

Cellulosic Biomass-Reinforced Polyvinylidene Fluoride Separators with Enhanced Dielectric Properties and Thermal Tolerance.

PubMed

Li, Lei; Yu, Miao; Jia, Chao; Liu, Jianxin; Lv, Yanyan; Liu, Yanhua; Zhou, Yi; Liu, Chuanting; Shao, Ziqiang

2017-06-21

Safety issues are critical barriers to large-scale energy storage applications of lithium-ion batteries (LIBs). Using an ameliorated, thermally stable, shutdown separator is an effective method to overcome the safety issues. Herein, we demonstrate a novel, cellulosic biomass-material-blended polyvinylidene fluoride separator that was prepared using a simple nonsolvent-induced phase separation technique. This process formed a microporous composite separator with reduced crystallinity, uniform pore size distribution, superior thermal tolerance, and enhanced electrolyte wettability and dielectric and mechanical properties. In addition, the separator has a superior capacity retention and a better rate capability compared to the commercialized microporous polypropylene membrane. This fascinating membrane was fabricated via a relatively eco-friendly and cost-effective method and is an alternative, promising separator for high-power LIBs.

Model reduction method using variable-separation for stochastic saddle point problems

NASA Astrophysics Data System (ADS)

Jiang, Lijian; Li, Qiuqi

2018-02-01

In this paper, we consider a variable-separation (VS) method to solve the stochastic saddle point (SSP) problems. The VS method is applied to obtain the solution in tensor product structure for stochastic partial differential equations (SPDEs) in a mixed formulation. The aim of such a technique is to construct a reduced basis approximation of the solution of the SSP problems. The VS method attempts to get a low rank separated representation of the solution for SSP in a systematic enrichment manner. No iteration is performed at each enrichment step. In order to satisfy the inf-sup condition in the mixed formulation, we enrich the separated terms for the primal system variable at each enrichment step. For the SSP problems by regularization or penalty, we propose a more efficient variable-separation (VS) method, i.e., the variable-separation by penalty method. This can avoid further enrichment of the separated terms in the original mixed formulation. The computation of the variable-separation method decomposes into offline phase and online phase. Sparse low rank tensor approximation method is used to significantly improve the online computation efficiency when the number of separated terms is large. For the applications of SSP problems, we present three numerical examples to illustrate the performance of the proposed methods.

Report on Phase 1 Tests of Fairchild Automatic Vehicle Monitoring (AVM) System

DOT National Transportation Integrated Search

1977-08-01

During the winter of 1976-77 four different techniques for automatically locating land vehicles were tested in both the low and high-rise regions in Philadelphia, Pennsylvania. The tests were carried out by four different companies under separate con...

Limited Qualities Evaluation of Longitudinal Flight Control Systems Designed Using Multiobjective Control Design Techniques (HAVE INFINITY II)

DTIC Science & Technology

1998-06-01

analytical phase of this research. Finally, the mixed H2/H-Infinity method optimally tradeoff the different benefits offered by the separate H2 and H...potential benefits of the multiobjective design techniques used. Due to the HAVE INFINITY I test results, AFIT made the decision to continue the...sensitivity and complimentary sensitivity weighting, and a mixed H2/H-Infinity design that compromised the benefits of both design techniques optimally. The

Velocity Profile measurements in two-phase flow using multi-wave sensors

NASA Astrophysics Data System (ADS)

Biddinika, M. K.; Ito, D.; Takahashi, H.; Kikura, H.; Aritomi, M.

2009-02-01

Two-phase flow has been recognized as one of the most important phenomena in fluid dynamics. In addition, gas-liquid two-phase flow appears in various industrial fields such as chemical industries and power generations. In order to clarify the flow structure, some flow parameters have been measured by using many effective measurement techniques. The velocity profile as one of the important flow parameter, has been measured by using ultrasonic velocity profile (UVP) technique. This technique can measure velocity distributions along a measuring line, which is a beam formed by pulse ultrasounds. Furthermore, a multi-wave sensor can measure the velocity profiles of both gas and liquid phase using UVP method. In this study, two types of multi-wave sensors are used. A sensor has cylindrical shape, and another one has square shape. The piezoelectric elements of each sensor have basic frequencies of 8 MHz for liquid phase and 2 MHz for gas phase, separately. The velocity profiles of air-water bubbly flow in a vertical rectangular channel were measured by using these multi-wave sensors, and the validation of the measuring accuracy was performed by the comparison between the velocity profiles measured by two multi-wave sensors.

Reverse-mode thermoresponsive light attenuators produced by optical anisotropic composites of nematic liquid crystals and reactive mesogens

NASA Astrophysics Data System (ADS)

Kakiuchida, Hiroshi; Ogiwara, Akifumi

2018-04-01

Polymer network liquid crystals (PNLCs) whose optical transmittance state switches between transparence at low temperatures and haze at high temperatures were fabricated from mixtures of nematic liquid crystals (LCs) and reactive mesogens (RMs). This PNLC structure is simple but effective, namely, consists of micro-scale domains of orientation-ordered LCs and anisotropically polymerized RMs. The domains form through photopolymerization induced phase separation with inhomogeneous irradiation projected by laser speckling techniques. This irradiation method enables you to control the size and shape of phase-separation domains, and these PNLCs can be applied to novel thermoresponsive optical devices; optical isolators, thermometric sheets, and smart windows.

Phase-locked-loop interferometry applied to aspheric testing with a computer-stored compensator.

PubMed

Servin, M; Malacara, D; Rodriguez-Vera, R

1994-05-01

A recently developed technique for continuous-phase determination of interferograms with a digital phase-locked loop (PLL) is applied to the null testing of aspheres. Although this PLL demodulating scheme is also a synchronous or direct interferometric technique, the separate unwrapping process is not explicitly required. The unwrapping and the phase-detection processes are achieved simultaneously within the PLL. The proposed method uses a computer-generated holographic compensator. The holographic compensator does not need to be printed out by any means; it is calculated and used from the computer. This computer-stored compensator is used as the reference signal to phase demodulate a sample interferogram obtained from the asphere being tested. Consequently the demodulated phase contains information about the wave-front departures from the ideal computer-stored aspheric interferogram. Wave-front differences of ~ 1 λ are handled easily by the proposed PLL scheme. The maximum recorded frequency in the template's interferogram as well as in the sampled interferogram are assumed to be below the Nyquist frequency.

Generation of phase edge singularities by coplanar three-beam interference and their detection.

PubMed

Patorski, Krzysztof; Sluzewski, Lukasz; Trusiak, Maciej; Pokorski, Krzysztof

2017-02-06

In recent years singular optics has gained considerable attention in science and technology. Up to now optical vortices (phase point dislocations) have been of main interest. This paper presents the first general analysis of formation of phase edge singularities by coplanar three-beam interference. They can be generated, for example, by three-slit interference or self-imaging in the Fresnel diffraction field of a sinusoidal grating. We derive a general condition for the ratio of amplitudes of interfering beams resulting in phase edge dislocations, lateral separation of dislocations depends on this ratio as well. Analytically derived properties are corroborated by numerical and experimental studies. We develop a simple, robust, common path optical self-imaging configuration aided by a coherent tilted reference wave and spatial filtering. Finally, we propose an automatic fringe pattern analysis technique for detecting phase edge dislocations, based on the continuous wavelet transform. Presented studies open new possibilities for developing grating based sensing techniques for precision metrology of very small phase differences.

Particle separation by phase modulated surface acoustic waves.

PubMed

Simon, Gergely; Andrade, Marco A B; Reboud, Julien; Marques-Hueso, Jose; Desmulliez, Marc P Y; Cooper, Jonathan M; Riehle, Mathis O; Bernassau, Anne L

2017-09-01

High efficiency isolation of cells or particles from a heterogeneous mixture is a critical processing step in lab-on-a-chip devices. Acoustic techniques offer contactless and label-free manipulation, preserve viability of biological cells, and provide versatility as the applied electrical signal can be adapted to various scenarios. Conventional acoustic separation methods use time-of-flight and achieve separation up to distances of quarter wavelength with limited separation power due to slow gradients in the force. The method proposed here allows separation by half of the wavelength and can be extended by repeating the modulation pattern and can ensure maximum force acting on the particles. In this work, we propose an optimised phase modulation scheme for particle separation in a surface acoustic wave microfluidic device. An expression for the acoustic radiation force arising from the interaction between acoustic waves in the fluid was derived. We demonstrated, for the first time, that the expression of the acoustic radiation force differs in surface acoustic wave and bulk devices, due to the presence of a geometric scaling factor. Two phase modulation schemes are investigated theoretically and experimentally. Theoretical findings were experimentally validated for different mixtures of polystyrene particles confirming that the method offers high selectivity. A Monte-Carlo simulation enabled us to assess performance in real situations, including the effects of particle size variation and non-uniform acoustic field on sorting efficiency and purity, validating the ability to separate particles with high purity and high resolution.

Preparative enantiomer separation of dichlorprop with a cinchona-derived chiral selector employing centrifugal partition chromatography and high-performance liquid chromatography: a comparative study.

PubMed

Gavioli, Elena; Maier, Norbert M; Minguillón, Cristina; Lindner, Wolfgang

2004-10-01

A countercurrent chromatography protocol for support-free preparative enantiomer separation of the herbicidal agent 2-(2,4-dichlorphenoxy)propionic acid (dichlorprop) was developed utilizing a purposefully designed, highly enantioselective chiral stationary-phase additive (CSPA) derived from bis-1,4-(dihydroquinidinyl)phthalazine. Guided by liquid-liquid extraction experiments, a solvent system consisting of 10 mM CSPA in methyl tert-butyl ether and 100 mM sodium phosphate buffer (pH 8.0) was identified as a suitable stationary/mobile-phase combination. This solvent system provided an ideal compromise among stationary-phase retention, enantioselectivity, and well-balanced analyte distribution behavior. Using a commercial centrifugal partition chromatography instrument, complete enantiomer separations of up to 366 mg of racemic dichlorprop could be achieved, corresponding to a sample load being equivalent to the molar amount of CSPA employed. Comparison of the preparative performance characteristics of the CPC protocol with that of a HPLC separation using a silica-supported bis-1,4-(dihydroquinidinyl)phthalazine chiral stationary phase CSP revealed comparable loading capacities for both techniques but a significantly lower solvent consumption for CPC. With respect to productivity, HPLC was found to be superior, mainly due to inherent flow rate restrictions of the CPC instrument. Given that further progress in instrumental design and engineering of dedicated, highly enantioselective CSPAs can be achieved, CPC may offer a viable alternative to CSP-based HPLC for preparative-scale enantiomer separation.

Novel RF and microwave components employing ferroelectric and solid-state tunable capacitors for multi-functional wireless communication systems

NASA Astrophysics Data System (ADS)

Tombak, Ali

The recent advancement in wireless communications demands an ever increasing improvement in the system performance and functionality with a reduced size and cost. This thesis demonstrates novel RF and microwave components based on ferroelectric and solid-state based tunable capacitor (varactor) technologies for the design of low-cost, small-size and multi-functional wireless communication systems. These include tunable lumped element VHF filters based on ferroelectric varactors, a beam-steering technique which, unlike conventional systems, does not require separate power divider and phase shifters, and a predistortion linearization technique that uses a varactor based tunable R-L-C resonator. Among various ferroelectric materials, Barium Strontium Titanate (BST) is actively being studied for the fabrication of high performance varactors at RF and microwave frequencies. BST based tunable capacitors are presented with typical tunabilities of 4.2:1 with the application of 5 to 10 V DC bias voltages and typical loss tangents in the range of 0.003--0.009 at VHF frequencies. Tunable lumped element lowpass and bandpass VHF filters based on BST varactors are also demonstrated with tunabilities of 40% and 57%, respectively. A new beam-steering technique is developed based on the extended resonance power dividing technique. Phased arrays based on this technique do not require separate power divider and phase shifters. Instead, the power division and phase shifting circuits are combined into a single circuit, which utilizes tunable capacitors. This results in a substantial reduction in the circuit complexity and cost. Phased arrays based on this technique can be employed in mobile multimedia services and automotive collision avoidance radars. A 2-GHz 4-antenna and a 10-GHz 8-antenna extended resonance phased arrays are demonstrated with scan ranges of 20 degrees and 18 degrees, respectively. A new predistortion linearization technique for the linearization of RF/microwave power amplifiers is also presented. This technique utilizes a varactor based tunable R-L-C resonator in shunt configuration. Due to the small number of circuit elements required, linearizers based on this technique offer low-cost and simple circuitry, hence can be utilized in handheld and cellular applications. A 1.8 GHz power amplifier with 9 dB gain is linearized using this technique. The linearizer improves the output 1-dB compression point of the power amplifier from 21 to 22.8 dBm. Adjacent channel power ratio (ACPR) is improved approximately 11 dB at an output RF power level of 17.5 dBm. The thesis is concluded by summarizing the main achievements and discussing the future work directions.

Capillarity-Driven Bubble Separations

NASA Astrophysics Data System (ADS)

Wollman, Andrew; Weislogel, Mark; Dreyer, Michael

2013-11-01

Techniques for phase separation in the absence of gravity continue to be sought after 5 decades of space flight. This work focuses on the fundamental problem of gas bubble separation in bubbly flows through open wedge-shaped channel in a microgravity environment. The bubbles appear to rise in the channel and coalesce with the free surface. Forces acting on the bubble are the combined effects of surface tension, wetting conditions, and geometry; not buoyancy. A single dimensionless group is identified that characterizes the bubble behavior and supportive experiments are conducted in a terrestrial laboratory, in a 2.1 second drop tower, and aboard the International Space Station as part of the Capillary Channel Flow (CCF) experiments. The data is organized into regime maps that provide insight on passive phase separations for applications ranging from liquid management aboard spacecraft to lab-on-chip technologies. NASA NNX09AP66A, NASA Oregon Space Grant NNX10AK68H, NASA NNX12AO47A, DLR 50WM0535/0845/1145

Hybrid carbon nanoparticles modified core-shell silica: a high efficiency carbon-based phase for hydrophilic interaction liquid chromatography.

PubMed

Ibrahim, Mohammed E A; Wahab, M Farooq; Lucy, Charles A

2014-04-11

Hydrophilic interaction liquid chromatography (HILIC) is a fast growing separation technique for hydrophilic and polar analytes. In this work, we combine the unique selectivity of carbon surfaces with the high efficiency of core-shell silica. First, 5 μm core-shell silica is electrostatically coated with 105 nm cationic latex bearing quaternary ammonium groups. Then 50 nm anionic carbon nanoparticles are anchored onto the surface of the latex coated core-shell silica particles to produce a hybrid carbon-silica phase. The hybrid phase shows different selectivity than ten previously classified HILIC column chemistries and 36 stationary phases. The hybrid HILIC phase has shape selectivity for positional isomeric pairs (phthalic/isophthalic and 1-naphthoic/2-naphthoic acids). Fast and high efficiency HILIC separations of biologically important carboxylates, phenols and pharmaceuticals are reported with efficiencies up to 85,000 plates m(-1). Reduced plate height of 1.9 (95,000 plates m(-1)) can be achieved. The hybrid phase is stable for at least 3 months of usage and storage under typical HILIC eluents. Copyright © 2014 Elsevier B.V. All rights reserved.

Advanced flight hardware for organic separations

NASA Astrophysics Data System (ADS)

Deuser, Mark S.; Vellinger, John C.; Weber, John T.

1997-01-01

Aqueous Two-Phase Partitioning (ATPP) is a unique separation technique which allows purification and classification of biological materials. SHOT has employed the ATPP process in separation equipment developed for both space and ground applications. Initial equipment development and research focused on the ORganic SEParation (ORSEP) space flight experiments that were performed on suborbital rockets and the shuttle. ADvanced SEParations (ADSEP) technology was developed as the next generation of ORSEP equipment through a NASA Small Business Innovation Research (SBIR) contract. Under the SBIR contract, a marketing study was conducted, indicating a growing commercial market exists among biotechnology firms for ADSEP equipment and associated flight research and development services. SHOT is preparing to begin manufacturing and marketing laboratory versions of the ADSEP hardware for the ground-based market. In addition, through a self-financed SBIR Phase III effort, SHOT fabricated and integrated the ADSEP flight hardware for a commercially-driven flight experiment as the initial step in marketing space processing services. The ADSEP ground-based and microgravity research is expected to play a vital role in developing important new biomedical and pharmaceutical products.

Studying Suspended Sediment Mechanism with Two-Phase PIV

NASA Astrophysics Data System (ADS)

Matinpour, H.; Atkinson, J. F.; Bennett, S. J.; Guala, M.

2017-12-01

Suspended sediment transport affects soil erosion, agriculture and water resources quality. Turbulent diffusion is the most primary force to maintain sediments in suspension. Although extensive previous literature have been studying the interactions between turbulent motion and suspended sediment, mechanism of sediments in suspension is still poorly understood. In this study, we investigate suspension of sediments as two distinct phases: one phase of sediments and another phase of fluid with turbulent motions. We designed and deployed a state-of-the-art two-phase PIV measurement technique to discriminate these two phases and acquire velocities of each phase separately and simultaneously. The technique that we have developed is employing a computer-vision based method, which enables us to discriminate sediment particles from fluid tracer particles based on two thresholds, dissimilar particle sizes and different particle intensities. Results indicate that fluid turbulence decreases in the presence of suspended sediments. Obtaining only sediment phase consecutive images enable us to compute fluctuation sediment concentration. This result enlightens understanding of complex interaction between the fluctuation velocities and the fluctuation of associated mass and compares turbulent viscosity with turbulent eddy diffusivity experimentally.

Validation of motion correction techniques for liver CT perfusion studies

PubMed Central

Chandler, A; Wei, W; Anderson, E F; Herron, D H; Ye, Z; Ng, C S

2012-01-01

Objectives Motion in images potentially compromises the evaluation of temporally acquired CT perfusion (CTp) data; image registration should mitigate this, but first requires validation. Our objective was to compare the relative performance of manual, rigid and non-rigid registration techniques to correct anatomical misalignment in acquired liver CTp data sets. Methods 17 data sets in patients with liver tumours who had undergone a CTp protocol were evaluated. Each data set consisted of a cine acquisition during a breath-hold (Phase 1), followed by six further sets of cine scans (each containing 11 images) acquired during free breathing (Phase 2). Phase 2 images were registered to a reference image from Phase 1 cine using two semi-automated intensity-based registration techniques (rigid and non-rigid) and a manual technique (the only option available in the relevant vendor CTp software). The performance of each technique to align liver anatomy was assessed by four observers, independently and blindly, on two separate occasions, using a semi-quantitative visual validation study (employing a six-point score). The registration techniques were statistically compared using an ordinal probit regression model. Results 306 registrations (2448 observer scores) were evaluated. The three registration techniques were significantly different from each other (p=0.03). On pairwise comparison, the semi-automated techniques were significantly superior to the manual technique, with non-rigid significantly superior to rigid (p<0.0001), which in turn was significantly superior to manual registration (p=0.04). Conclusion Semi-automated registration techniques achieved superior alignment of liver anatomy compared with the manual technique. We hope this will translate into more reliable CTp analyses. PMID:22374283

Space systems engineering and risk management - joined at the hip

NASA Technical Reports Server (NTRS)

Rose, James R.

2004-01-01

This paper explores the separate skills and capabilities practiced until now, and the powerful coupling to be achieved, practically and effectively, in implementing a space mission, from inception (pre-phase A) to the end of Operations (phase E). The use of risk assessment techniques in balancing cost risk against performance risk, and the application of the systems engineering team in these trades, is the key to achieving this new implementation paradigm.

Engineering topological defect patterns of Bose condensates in shaken optical lattices

NASA Astrophysics Data System (ADS)

Feng, Lei; Clark, Logan W.; Gaj, Anita; Chin, Cheng

2017-04-01

Topological defects emerge and play an essential role in the dynamics of systems undergoing continuous, symmetry-breaking phase transitions. Here, we study the topological defects (domain walls) which form when a Bose condensate in a shaken optical lattice undergoes a quantum phase transition and separates into domains of superfluid with finite momentum. Here, we experimentally demonstrate the ability to control the pattern of domain walls using a digital micromirror device. We further explore implementations of this technique to study dynamics near the phase transition and the evolution of topological defects.

Current trends in sample preparation for cosmetic analysis.

PubMed

Zhong, Zhixiong; Li, Gongke

2017-01-01

The widespread applications of cosmetics in modern life make their analysis particularly important from a safety point of view. There is a wide variety of restricted ingredients and prohibited substances that primarily influence the safety of cosmetics. Sample preparation for cosmetic analysis is a crucial step as the complex matrices may seriously interfere with the determination of target analytes. In this review, some new developments (2010-2016) in sample preparation techniques for cosmetic analysis, including liquid-phase microextraction, solid-phase microextraction, matrix solid-phase dispersion, pressurized liquid extraction, cloud point extraction, ultrasound-assisted extraction, and microwave digestion, are presented. Furthermore, the research and progress in sample preparation techniques and their applications in the separation and purification of allowed ingredients and prohibited substances are reviewed. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Retention behavior of long chain quaternary ammonium homologues and related nitroso-alkymethylamines

USGS Publications Warehouse

Abidi, S.L.

1985-01-01

Several chromatographic methods have been utilized to study the retentionbehavior of a homologous series of n-alkylbenzyldimethylammonium chlorides (ABDAC) and the corresponding nitroso-n-alkylmethylamines (NAMA). Linear correlation of the logarithmic capacity factor (k') with the number of carbons in the alkyl chain provides useful information on both gas chromatographic (GC) and high-performance liquid chromatographich (HPLC) retention parameters of unknown components. Under all conditions empolyed, GC methodology has proved effective in achieving complete resolution of the homologous mixture of NMA despite its obvious inadequacy in the separation of E-Z configurational isomers. Conversely, normal-phase HPLC on silica demonstrates that the selectivity (a) value for an E-Z pair is much higher than that for an adjacent homologous pair. In the reversed-phase HPLC study, three different silica-based column systems were examined under various mobile phase conditions. The extent of variation in k' was found to be a function of the organic modifier, counter-ion concentration, eluent pH, nature of counter-ion, and the polarity and type of stationary phase. The k'—[NaClO4] profiles showed similar trends between the ABDAC and the NAMA series, supporting the dipolar electronic structures of the latter compounds. Mobile phase and stationary phase effects on component separation are described. The methodology presented establishes the utility of HPLC separation techniques as versatile analytical tools for practical application.

Concerted spatial-frequency and polarization-phase filtering of laser images of polycrystalline networks of blood plasma smears

NASA Astrophysics Data System (ADS)

Ushenko, Yu A.

2012-11-01

The complex technique of concerted polarization-phase and spatial-frequency filtering of blood plasma laser images is suggested. The possibility of obtaining the coordinate distributions of phases of linearly and circularly birefringent protein networks of blood plasma separately is presented. The statistical (moments of the first to fourth orders) and scale self-similar (logarithmic dependences of power spectra) structure of phase maps of different types of birefringence of blood plasma of two groups of patients-healthy people (donors) and those suffering from rectal cancer-is investigated. The diagnostically sensitive parameters of a pathological change of the birefringence of blood plasma polycrystalline networks are determined. The effectiveness of this technique for detecting change in birefringence in the smears of other biological fluids in diagnosing the appearance of cholelithiasis (bile), operative differentiation of the acute and gangrenous appendicitis (exudate), and differentiation of inflammatory diseases of joints (synovial fluid) is shown.

Mesh-based phase contrast Fourier transform imaging

NASA Astrophysics Data System (ADS)

Tahir, Sajjad; Bashir, Sajid; MacDonald, C. A.; Petruccelli, Jonathan C.

2017-04-01

Traditional x-ray radiography is limited by low attenuation contrast in materials of low electron density. Phase contrast imaging offers the potential to improve the contrast between such materials, but due to the requirements on the spatial coherence of the x-ray beam, practical implementation of such systems with tabletop (i.e. non-synchrotron) sources has been limited. One phase imaging technique employs multiple fine-pitched gratings. However, the strict manufacturing tolerances and precise alignment requirements have limited the widespread adoption of grating-based techniques. In this work, we have investigated a recently developed technique that utilizes a single grid of much coarser pitch. Our system consisted of a low power 100 μm spot Mo source, a CCD with 22 μm pixel pitch, and either a focused mammography linear grid or a stainless steel woven mesh. Phase is extracted from a single image by windowing and comparing data localized about harmonics of the mesh in the Fourier domain. The effects on the diffraction phase contrast and scattering amplitude images of varying grid types and periods, and of varying the width of the window function used to separate the harmonics were investigated. Using the wire mesh, derivatives of the phase along two orthogonal directions were obtained and combined to form improved phase contrast images.

Anodic etching of GaN based film with a strong phase-separated InGaN/GaN layer: Mechanism and properties

NASA Astrophysics Data System (ADS)

Gao, Qingxue; Liu, Rong; Xiao, Hongdi; Cao, Dezhong; Liu, Jianqiang; Ma, Jin

2016-11-01

A strong phase-separated InGaN/GaN layer, which consists of multiple quantum wells (MQW) and superlattices (SL) layers and can produce a blue wavelength spectrum, has been grown on n-GaN thin film, and then fabricated into nanoporous structures by electrochemical etching method in oxalic acid. Scanning electron microscopy (SEM) technique reveals that the etching voltage of 8 V leads to a vertically aligned nanoporous structure, whereas the films etched at 15 V show branching pores within the n-GaN layer. Due to the low doping concentration of barriers (GaN layers) in the InGaN/GaN layer, we observed a record-low rate of etching (<100 nm/min) and nanopores which are mainly originated from the V-pits in the phase-separated layer. In addition, there exists a horizontal nanoporous structure at the interface between the phase-separated layer and the n-GaN layer, presumably resulting from the high transition of electrons between the barrier and the well (InGaN layer) at the interface. As compared to the as-grown MQW structure, the etched MQW structure exhibits a photoluminescence (PL) enhancement with a partial relaxation of compressive stress due to the increased light-extracting surface area and light-guiding effect. Such a compressive stress relaxation can be further confirmed by Raman spectra.

Nano-liquid chromatography applied to enantiomers separation.

PubMed

Fanali, Salvatore

2017-02-24

This paper presents the state of the art concerning the separation of chiral compounds by means of nano-liquid chromatography (nano-LC). The enantiomers' separation and determination are a subject of fundamental importance in various application fields such as pharmaceutical industry, biomedicine, food, agrochemical etc. Nano-LC is a miniaturized chromatographic technique offering some advantages over conventional ones such as low consumption of mobile phase, sample volume and amount of chiral stationary phase, reduced costs etc. This is reported in the first part of the paper illustrating the features of the nano-LC. In addition, chiral resolution methods are briefly illustrated. Some chiral selectors, used in high-performance liquid chromatography have also been applied in nano-LC including cyclodextrins, glycopeptide antibiotics, modified polysaccharides etc. This is discussed in the second part of the review. Finally some examples of the applications available in literature are reported. Copyright © 2016 Elsevier B.V. All rights reserved.

Applications of liquid-based separation in conjunction with mass spectrometry to the analysis of forensic evidence.

PubMed

Moini, Mehdi

2018-05-01

In the past few years, there has been a significant effort by the forensic science community to develop new scientific techniques for the analysis of forensic evidence. Forensic chemists have been spearheaded to develop information-rich confirmatory technologies and techniques and apply them to a broad array of forensic challenges. The purpose of these confirmatory techniques is to provide alternatives to presumptive techniques that rely on data such as color changes, pattern matching, or retention time alone, which are prone to more false positives. To this end, the application of separation techniques in conjunction with mass spectrometry has played an important role in the analysis of forensic evidence. Moreover, in the past few years the role of liquid separation techniques, such as liquid chromatography and capillary electrophoresis in conjunction with mass spectrometry, has gained significant tractions and have been applied to a wide range of chemicals, from small molecules such as drugs and explosives, to large molecules such as proteins. For example, proteomics and peptidomics have been used for identification of humans, organs, and bodily fluids. A wide range of HPLC techniques including reversed phase, hydrophilic interaction, mixed-mode, supercritical fluid, multidimensional chromatography, and nanoLC, as well as several modes of capillary electrophoresis mass spectrometry, including capillary zone electrophoresis, partial filling, full filling, and micellar electrokenetic chromatography have been applied to the analysis drugs, explosives, and questioned documents. In this article, we review recent (2015-2017) applications of liquid separation in conjunction with mass spectrometry to the analysis of forensic evidence. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Phases, line tension and pattern formation in molecularly thin films at the air-water interface

NASA Astrophysics Data System (ADS)

Mandal, Pritam

A Langmuir film, which is a molecularly thin insoluble film on a liquid substrate, is one practical realization of a quasi-two dimensional matter. The major advantages of this system for the study of phase separation and phase co-existence are (a) it allows accurate control of the components and molecular area of the film and (b) it can be studied by various methods that require very flat films. Phase separation in molecularly thin films plays an important role in a range of systems from biomembranes to biosensors. For example, phase-separated lipid nano-domains in biomembranes are thought to play crucial roles in membrane function. I use Brewster Angel Microscopy (BAM) coupled with Fluorescence Microscopy (FM) and static Light Scattering Microscopy (LSM) to image phases and patterns within Langmuir films. The three microscopic techniques --- BAM, FM and LSM --- are complimentary to each other, providing distinct sets of information. They allow direct comparison with literature results in lipid systems. I have quantitatively validated the use of detailed hydrodynamic simulations to determine line tension in monolayers. Line tension decreases as temperature rises. This decrease gives us information on the entropy associated with the line, and thus about line structure. I carefully consider the thermodynamics of line energy and entropy to make this connection. In the longer run, LSM will be exploited to give us further information about line structure. I have also extended the technique by testing it on domains within the curved surface of a bilayer vesicle. I also note that in the same way that the presence of surface-active agents, known as surfactants, affects surface energy, the addiction of line active agents alters the inter-phase line energy. Thus my results set to stage to systematically study the influence of line active agents ---'linactants' --- on the inter-phase line energy. Hierarchal self-assembled chiral patterns were observed as a function of temperature. I found that the appearance of these domains could be explained with a simple uniaxial optical axis in the underlying structure, which is the first critical step to understanding the origin of these patterns.

Separation of metalloporphyrins from metallation reactions by liquid chromatography and electrophoresis.

PubMed

Duff, G A; Yeager, S A; Singhal, A K; Pestel, B C; Ressner, J M; Foster, N

1987-04-24

The analytical separation of the indium and manganese complexes of three synthetic, meso-substituted, water-soluble porphyrins from their respective free bases in metallation reaction mixtures is described. The ligands tetra-3N-methylpyridyl porphyrin, tetra-4N-methylpyridyl porphyrin and tetra-N,N,N-trimethylanilinium porphyrin are complexed with In (III) and Mn (III) and are separated from residual free base by high-performance liquid chromatography (HPLC) in acidic conditions with gradient elution on ODS bonded stationary phase. Electrophoretic separation is achieved on both cellulose polyacetate strips and polyacrylamide tube gels under basic conditions. Although analytical separations can be achieved by both HPLC and electrophoresis, only HPLC is suitable for the development of preparative scale separations. Column chromatography, ion-pairing and ion-suppression HPLC techniques fail to separate such highly charged and closely related aromatic compounds.

A three-image algorithm for hard x-ray grating interferometry.

PubMed

Pelliccia, Daniele; Rigon, Luigi; Arfelli, Fulvia; Menk, Ralf-Hendrik; Bukreeva, Inna; Cedola, Alessia

2013-08-12

A three-image method to extract absorption, refraction and scattering information for hard x-ray grating interferometry is presented. The method comprises a post-processing approach alternative to the conventional phase stepping procedure and is inspired by a similar three-image technique developed for analyzer-based x-ray imaging. Results obtained with this algorithm are quantitatively comparable with phase-stepping. This method can be further extended to samples with negligible scattering, where only two images are needed to separate absorption and refraction signal. Thanks to the limited number of images required, this technique is a viable route to bio-compatible imaging with x-ray grating interferometer. In addition our method elucidates and strengthens the formal and practical analogies between grating interferometry and the (non-interferometric) diffraction enhanced imaging technique.

How to Meet Water Cleanup Deadlines

ERIC Educational Resources Information Center

Schmidt, Richard K.

1976-01-01

Most waste treatment techniques conceived to meet the 1977 standards can be separated into three distinct phases: primary, secondary and tertiary treatment. An examination of the four heaviest industrial water users, pulp and paper, steel, plating, and food processing, demonstrates these treatments use proven technology to meet specific…

Solid Phase Extraction (SPE) for Biodiesel Processing and Analysis

DTIC Science & Technology

2017-12-13

1 METHODS ...sources. There are several methods than can be applied to development of separation techniques that may replace necessary water wash steps in...biodiesel refinement. Unfortunately, the most common methods are poorly suited or face high costs when applied to diesel purification. Distillation is

Fluorescence exclusion: A simple versatile technique to calculate cell volumes and local heights (Conference Presentation)

NASA Astrophysics Data System (ADS)

Thouvenin, Olivier; Fink, Mathias; Boccara, A. Claude

2017-02-01

Understanding volume regulation during mitosis is technically challenging. Indeed, a very sensitive non invasive imaging over time scales ranging from seconds to hours and over large fields is required. Therefore, Quantitative Phase Imaging (QPI) would be a perfect tool for such a project. However, because of asymmetric protein segregation during mitosis, an efficient separation of the refractive index and the height in the phase signal is required. Even though many strategies to make such a separation have been developed, they usually are difficult to implement, have poor sensitivity, or cannot be performed in living cells, or in a single shot. In this paper, we will discuss the use of a new technique called fluorescence exclusion to perform volume measurements. By coupling such technique with a simultaneous phase measurement, we were also able to recover the refractive index inside the cells. Fluorescence exclusion is a versatile and powerful technique that allows the volume measurement of many types of cells. A fluorescent dye, which cannot penetrate inside the cells, is mixed with the external medium in a confined environment. Therefore, the fluorescent signal depends on the inverse of the object's height. We could demonstrate both experimentally and theoretically that fluorescence exclusion can accurately measure cell volumes, even for cells much higher than the depth of focus of the objective. A local accurate height and RI measurement can also be obtained for smaller cells. We will also discuss the way to optimize the confinement of the observation chamber, either mechanically or optically.

Fractionation of technical octabromodiphenyl ether by countercurrent chromatography combined with gas chromatography/mass spectrometry and offline and online (1)H nuclear magnetic resonance spectroscopy.

PubMed

Hammann, Simon; Conrad, Jürgen; Vetter, Walter

2015-06-12

Countercurrent chromatography (CCC) is a technique, which uses two immiscible liquid phases for a separation process in a long and hollow tube. The technique allows the separation of high amounts of sample (50mg to several grams) with a low consumption of solvents. In this study, we fractionated 50mg technical octabromodiphenyl ether (DE-79) and analyzed the fractions by gas chromatography with mass spectrometry (GC/MS) and proton nuclear magnetic resonance ((1)H NMR) spectroscopy. CCC separations were performed with n-hexane/acetonitrile as solvent system in tail-to-head (i.e. the upper phase is mobile) mode. Twelve CCC fractions were studied for the PBDE composition. CCC elution of PBDE congeners was dependent both on the degree of bromination and substitution pattern. Higher brominated congeners eluted faster than lower brominated congeners and isomers with vicinal hydrogen atoms eluted last. In addition to several known PBDE congeners in DE-79, we were able to unequivocally identify BDE 195 in DE-79 and we could verify the presence of BDE 184. Finally, we also established the online hyphenation of CCC with (1)H NMR. The use of deuterated solvents could be avoided by using n-hexane/acetonitrile as two-phase system. By online CCC-(1)H NMR in stop-flow mode we were able to detect eight PBDE congeners in the mixture. Copyright © 2015 Elsevier B.V. All rights reserved.

Characterization of Phase Separation Propensity for Amorphous Spray Dried Dispersions.

PubMed

McNamara, Daniel; Yin, Shawn; Pan, Duohai; Crull, George; Timmins, Peter; Vig, Balvinder

2017-02-06

A generalized screening approach, applying isothermal calorimetry at 37 °C 100% RH, to formulations of spray dried dispersions (SDDs) for two active pharmaceutical ingredients (APIs) (BMS-903452 and BMS-986034) is demonstrated. APIs 452 and 034, with similar chemotypes, were synthesized and promoted during development for oral dosing. Both APIs were formulated as SDDs for animal exposure studies using the polymer hydroxypropylmethlycellulose acetyl succinate M grade (HPMCAS-M). 452 formulated at 30% (wt/wt %) was an extremely robust SDD that was able to withstand 40 °C 75% RH open storage conditions for 6 months with no physical evidence of crystallization or loss of dissolution performance. Though 034 was a chemical analogue with similar physical chemical properties to 452, a physically stable SDD of 034 could not be formulated in HPMCAS-M at any of the drug loads attempted. This study was used to develop experience with specific physical characterization laboratory techniques to evaluate the physical stability of SDDs and to characterize the propensity of SDDs to phase separate and possibly crystallize. The screening strategy adopted was to stress the formulated SDDs with a temperature humidity screen, within the calorimeter, and to apply orthogonal analytical techniques to gain a more informed understanding of why these SDDs formulated with HPMCAS-M demonstrated such different physical stability. Isothermal calorimetry (thermal activity monitor, TAM) was employed as a primary stress screen wherein the SDD formulations were monitored for 3 days at 37 °C 100% RH for signs of phase separation and possible crystallization of API. Powder X-ray diffraction (pXRD), modulated differential scanning calorimetry (mDSC), Fourier transform infrared spectroscopy (FTIR), and solid state nuclear magnetic resonance (ssNMR) were all used to examine formulated SDDs and neat amorphous drug. 452 SDDs formulated at 30% (wt/wt %) or less did not show phase separation behavior upon exposure to 37 °C 100% RH for 3 days. 034 SDD formulations from 10 through 50% (wt/wt %) all demonstrated thermal traces consistent with exothermic phase separation events over 3 days at 37 °C 100% RH in the TAM. However, only the 15, 30, and 50% containing 034 samples showed pXRD patterns consistent with crystalline material in post-TAM samples. Isothermal calorimetry is a useful screening tool to probe robust SDD physical performance and help investigate the level of drug polymer miscibility under a humid stress. Orthogonal analytical techniques such as pXRD, ssNMR, and FTIR were key in this SDD formulation screening to gain physical understanding and confirm or refute whether physical changes occur during the observed thermal events characterized by the calorimetric screening experiments.

Bioinspired phase-separated disordered nanostructures for thin photovoltaic absorbers.

PubMed

Siddique, Radwanul H; Donie, Yidenekachew J; Gomard, Guillaume; Yalamanchili, Sisir; Merdzhanova, Tsvetelina; Lemmer, Uli; Hölscher, Hendrik

2017-10-01

The wings of the black butterfly, Pachliopta aristolochiae , are covered by micro- and nanostructured scales that harvest sunlight over a wide spectral and angular range. Considering that these properties are particularly attractive for photovoltaic applications, we analyze the contribution of these micro- and nanostructures, focusing on the structural disorder observed in the wing scales. In addition to microspectroscopy experiments, we conduct three-dimensional optical simulations of the exact scale structure. On the basis of these results, we design nanostructured thin photovoltaic absorbers of disordered nanoholes, which combine efficient light in-coupling and light-trapping properties together with a high angular robustness. Finally, inspired by the phase separation mechanism of self-assembled biophotonic nanostructures, we fabricate these bioinspired absorbers using a scalable, self-assembly patterning technique based on the phase separation of binary polymer mixture. The nanopatterned absorbers achieve a relative integrated absorption increase of 90% at a normal incident angle of light to as high as 200% at large incident angles, demonstrating the potential of black butterfly structures for light-harvesting purposes in thin-film solar cells.

Bioinspired phase-separated disordered nanostructures for thin photovoltaic absorbers

PubMed Central

Siddique, Radwanul H.; Donie, Yidenekachew J.; Gomard, Guillaume; Yalamanchili, Sisir; Merdzhanova, Tsvetelina; Lemmer, Uli; Hölscher, Hendrik

2017-01-01

The wings of the black butterfly, Pachliopta aristolochiae, are covered by micro- and nanostructured scales that harvest sunlight over a wide spectral and angular range. Considering that these properties are particularly attractive for photovoltaic applications, we analyze the contribution of these micro- and nanostructures, focusing on the structural disorder observed in the wing scales. In addition to microspectroscopy experiments, we conduct three-dimensional optical simulations of the exact scale structure. On the basis of these results, we design nanostructured thin photovoltaic absorbers of disordered nanoholes, which combine efficient light in-coupling and light-trapping properties together with a high angular robustness. Finally, inspired by the phase separation mechanism of self-assembled biophotonic nanostructures, we fabricate these bioinspired absorbers using a scalable, self-assembly patterning technique based on the phase separation of binary polymer mixture. The nanopatterned absorbers achieve a relative integrated absorption increase of 90% at a normal incident angle of light to as high as 200% at large incident angles, demonstrating the potential of black butterfly structures for light-harvesting purposes in thin-film solar cells. PMID:29057320

Highly efficient organic solar cells with improved vertical donor-acceptor compositional gradient via an inverted off-center spinning method

DOE PAGES

Huang, Jiang; Carpenter, Joshua H.; Li, Chang -Zhi; ...

2015-12-02

A novel, yet simple solution fabrication technique to address the trade-off between photocurrent and fill factor in thick bulk heterojunction organic solar cells is described. Lastly, the inverted off-center spinning technique promotes a vertical gradient of the donor–acceptor phase-separated morphology, enabling devices with near 100% internal quantum efficiency and a high power conversion efficiency of 10.95%.

Separation and characterization of allergic polymerized impurities in cephalosporins by 2D-HPSEC×LC-IT-TOF MS.

PubMed

Xu, Yu; Wang, DanDan; Tang, Lan; Wang, Jian

2017-10-25

Eleven unknown allergic impurities in cefodizime, cefmenoxime and cefonicid were separated and characterized by a trap-free two-dimensional high performance size exclusion chromatography (HPSEC) and reversed phase liquid chromatography (RP-HPLC) coupled to high resolution ion trap/time-of-flight mass spectrometry (2D-HPSEC×LC-IT-TOF MS) with positive and negative modes of electrospray ionization method. Separation and characterization the allergic polymerized impurities in β-lactam antibiotics were on the basis of column-switching technique which effectively combined the advantages of HPSEC and the ability of RP-HPLC to identify the special impurities. In the first dimension HPSEC, the column was Xtimate SEC-120 analytical column (7.8mm×30cm, 5μm), and the gradient elution used pH 7.0 buffer-acetonitrile as mobile phase And the second dimension analytical column was ZORBAX SB-C18 (4.6×150mm, 3.5μm) with ammonium formate solution (10mM) and ammonium formate (8mM) in [acetonitrile-water (4:1, v/v)] solution as mobile phase. Structures of eleven unknown impurities were deduced based on the high resolution MS n data with both positive and negative modes, in which nine impurities were polymerized impurities. The forming mechanism of β-lactam antibiotic polymerization in cephalosporins was also studied. The question on incompatibility between non-volatile salt mobile phase and mass spectrometry was solved completely by multidimensional heart-cutting approaches and online demineralization technique, which was worthy of widespread use and application for the advantages of stability and repeatability. Copyright © 2017. Published by Elsevier B.V.

Prototype of an Interface for Hyphenating Distillation with Gas Chromatography and Mass Spectrometry

PubMed Central

Tang, Ya-Ru; Yang, Hui-Hsien; Urban, Pawel L.

2017-01-01

Chemical analysis of complex matrices—containing hundreds of compounds—is challenging. Two-dimensional separation techniques provide an efficient way to reduce complexity of mixtures analyzed by mass spectrometry (MS). For example, gasoline is a mixture of numerous compounds, which can be fractionated by distillation techniques. However, coupling conventional distillation with other separations as well as MS is not straightforward. We have established an automatic system for online coupling of simple microscale distillation with gas chromatography (GC) and electron ionization MS. The developed system incorporates an interface between the distillation condenser and the injector of a fused silica capillary GC column. Development of this multidimensional separation (distillation-GC-MS) was preceded by a series of preliminary off-line experiments. In the developed technique, the components with different boiling points are fractionated and instantly analyzed by GC-MS. The obtained data sets illustrate dynamics of the distillation process. An important advantage of the distillation-GC-MS technique is that raw samples can directly be analyzed without removal of the non-volatile matrix residues that could contaminate the GC injection port and the column. Distilling the samples immediately before the injection to the GC column may reduce possible matrix effects—especially in the early phase of separation, when molecules with different volatilities co-migrate. It can also reduce losses of highly volatile components (during fraction collection and transfer). The two separation steps are partly orthogonal, what can slightly increase selectivity of the entire analysis. PMID:28337400

Extraction-Separation Performance and Dynamic Modeling of Orion Test Vehicles with Adams Simulation: 2nd Edition

NASA Technical Reports Server (NTRS)

Fraire, Usbaldo, Jr.; Anderson, Keith; Varela, Jose G.; Bernatovich, Michael A.

2015-01-01

NASA's Orion Capsule Parachute Assembly System (CPAS) project has advanced into the third generation of its parachute test campaign and requires technically comprehensive modeling capabilities to simulate multi-body dynamics (MBD) of test articles released from a C-17. Safely extracting a 30,000 lbm mated test article from a C-17 and performing stable mid-air separation maneuvers requires an understanding of the interaction between elements in the test configuration and how they are influenced by extraction parachute performance, aircraft dynamics, aerodynamics, separation dynamics, and kinetic energy experienced by the system. During the real-time extraction and deployment sequences, these influences can be highly unsteady and difficult to bound. An avionics logic window based on time, pitch, and pitch rate is used to account for these effects and target a favorable separation state in real time. The Adams simulation has been employed to fine-tune this window, as well as predict and reconstruct the coupled dynamics of the Parachute Test Vehicle (PTV) and Cradle Platform Separation System (CPSS) from aircraft extraction through the mid-air separation event. The test-technique for the extraction of CPAS test articles has evolved with increased complexity and requires new modeling concepts to ensure the test article is delivered to a stable test condition for the programmer phase. Prompted by unexpected dynamics and hardware malfunctions in drop tests, these modeling improvements provide a more accurate loads prediction by incorporating a spring-damper line-model derived from the material properties. The qualification phase of CPAS testing is on the horizon and modeling increasingly complex test-techniques with Adams is vital to successfully qualify the Orion parachute system for human spaceflight.

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.

Separating DDTs in edible animal fats using matrix solid-phase dispersion extraction with activated carbon filter, Toyobo-KF.

PubMed

Furusawa, Naoto

2006-09-01

A technique is presented for the economical, routine, and quantitative analysis of contamination by dichloro-diphenyl-trichloroethanes (DDTs) [pp'-DDT, pp'-dichlorodiphenyl dichloroethylene, and pp'-dichlorodiphenyl dichloreothane in beef tallow and chicken fat samples, based on their separation using matrix solid-phase dispersion (MSPD) extraction with Toyobo-KF, an activated carbon fiber. Toyobo-KF is a newly applied MSPD sorbent, and it is followed by reversed-phase high-performance liquid chromatography (HPLC) with a photodiode array detector. The resulting analytical performance parameters [recoveries of spiked DDTs (0.1, 0.2, and 0.4 microg/g) > or = 81%, with relative standard deviations of < or = 8% (n = 5), and quantitation limits < or = 0.03 microg/g], with minimal handling and cost-efficiency, indicate that the present MSPD-HPLC method may be a useful tool for routine monitoring of DDT contamination in meat.

Classification of LC columns based on the QSRR method and selectivity toward moclobemide and its metabolites.

PubMed

Plenis, Alina; Olędzka, Ilona; Bączek, Tomasz

2013-05-05

This paper focuses on a comparative study of the column classification system based on the quantitative structure-retention relationships (QSRR method) and column performance in real biomedical analysis. The assay was carried out for the LC separation of moclobemide and its metabolites in human plasma, using a set of 24 stationary phases. The QSRR models established for the studied stationary phases were compared with the column test performance results under two chemometric techniques - the principal component analysis (PCA) and the hierarchical clustering analysis (HCA). The study confirmed that the stationary phase classes found closely related by the QSRR approach yielded comparable separation for moclobemide and its metabolites. Therefore, the QSRR method could be considered supportive in the selection of a suitable column for the biomedical analysis offering the selection of similar or dissimilar columns with a relatively higher certainty. Copyright © 2013 Elsevier B.V. All rights reserved.

Application of ionic liquids in liquid chromatography and electrodriven separation.

PubMed

Huang, Yi; Yao, Shun; Song, Hang

2013-08-01

Ionic liquids (ILs) are salts in the liquid state at ambient temperature, which are nonvolatile, nonflammable with high thermal stability and dissolve easily for a wide range of inorganic and organic materials. As a kind of potential green solvent, they show high efficiency and selectivity in the field of separation research, especially in instrumental analysis. Thus far, ILs have been successfully applied by many related researchers in high-performance liquid chromatography and capillary electrophoresis as chromatographic stationary phases, mobile phase additives or electroosmotic flow modifiers. This paper provides a detailed review of these applications in the study of natural products, foods, drugs and other fine chemicals. Furthermore, the prospects of ILs in liquid chromatographic and electrodriven techniques are discussed.

Revealing hidden antiferromagnetic correlations in doped Hubbard chains via string correlators

NASA Astrophysics Data System (ADS)

Hilker, Timon A.; Salomon, Guillaume; Grusdt, Fabian; Omran, Ahmed; Boll, Martin; Demler, Eugene; Bloch, Immanuel; Gross, Christian

2017-08-01

Topological phases, like the Haldane phase in spin-1 chains, defy characterization through local order parameters. Instead, nonlocal string order parameters can be employed to reveal their hidden order. Similar diluted magnetic correlations appear in doped one-dimensional lattice systems owing to the phenomenon of spin-charge separation. Here we report on the direct observation of such hidden magnetic correlations via quantum gas microscopy of hole-doped ultracold Fermi-Hubbard chains. The measurement of nonlocal spin-density correlation functions reveals a hidden finite-range antiferromagnetic order, a direct consequence of spin-charge separation. Our technique, which measures nonlocal order directly, can be readily extended to higher dimensions to study the complex interplay between magnetic order and density fluctuations.

Automated thermal mapping techniques using chromatic image analysis

NASA Technical Reports Server (NTRS)

Buck, Gregory M.

1989-01-01

Thermal imaging techniques are introduced using a chromatic image analysis system and temperature sensitive coatings. These techniques are used for thermal mapping and surface heat transfer measurements on aerothermodynamic test models in hypersonic wind tunnels. Measurements are made on complex vehicle configurations in a timely manner and at minimal expense. The image analysis system uses separate wavelength filtered images to analyze surface spectral intensity data. The system was initially developed for quantitative surface temperature mapping using two-color thermographic phosphors but was found useful in interpreting phase change paint and liquid crystal data as well.

Tubing modifications for countercurrent chromatography (CCC): Stationary phase retention and separation efficiency.

PubMed

Englert, Michael; Vetter, Walter

2015-07-16

Countercurrent chromatography (CCC) is a separation technique in which two immiscible liquid phases are used for the preparative purification of synthetic and natural products. In CCC the number of repetitive mixing and de-mixing processes, the retention of the stationary phase and the mass transfer between the liquid phases are significant parameters that influence the resolution and separation efficiency. Limited mass transfer is the main reason for peak broadening and a low number of theoretical plates along with impaired peak resolution in CCC. Hence, technical improvements with regard to column design and tubing modifications is an important aspect to enhance mixing and mass transfer. In this study we constructed a crimping tool which allowed us to make reproducible, semi-automated modifications of conventional round-shaped tubing. Six crimped tubing modifications were prepared, mounted onto multilayer coils which were subsequently installed in the CCC system. The stationary phase retention of the tubing modifications were compared to the conventional system with unmodified tubing in a hydrophobic, an intermediate and a hydrophilic two-phase solvent system. Generally, the tubing modifications provided higher capabilities to retain the stationary phase depending on the solvent system and flow rates. In the intermediate solvent system the separation efficiency was evaluated with a mixture of six alkyl p-hydroxybenzoates. The peak resolution could be increased up to 50% with one of the tubing modifications compared to the unmodified tubing. Using the most convincing tubing modification at fixed values for the stationary phase retention, a reasonable comparison to the unmodified tubing was achieved. The peak width could be reduced up to 49% and a strong positive impact at increased flow rates regarding peak resolution and theoretical plate number was observed compared to unmodified tubing. It could be concluded that the tubing modification enhanced the interphase mixing and mass transfer of the two phases by additional and more vigorous agitation. Copyright © 2015 Elsevier B.V. All rights reserved.

SEPARATION OF TOXICOLOGICALLY RELEVANT ARSENICALS IN URINE USING A NEW SOLID PHASE EXTRACTION TECHNIQUE

EPA Science Inventory

Abstract - Metabolism and toxicity of arsenicals are critically influenced by the oxidation state of As. In human urine, inorganic and methylated arsenicals contain both As(III) and As(V). Because As(III) is easily oxidized, a method is needed to preserve the native oxidation sta...

Proceedings of the seventh international conference on high voltage electron microscopy

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

Fisher, R.M.; Gronsky, R.; Westmacott, K.H.

1983-01-01

Eight-four papers are arranged under the following headings: high resolution, techniques and instrumentation, radiation effects, in-situ and phase transformations, minerals and ceramics, and semiconductors and thin films. Twenty-three papers were abstracted separately for the data base; three of the remainder had previously been abstracted. (DLC)

Myth and Ritual in "Othello": A Technique for Teaching.

ERIC Educational Resources Information Center

Holleran, James V.

In terms of structure, the play "Othello" is a distortion of an initiation ritual. Arnold van Gennup, in his book "The Rites of Passage," reduces all initiation rituals into three definable phases: separation, transition, and incorporation. The general pattern of the initiation ritual in "Othello" is as follows:…

Enantioseparations by capillary electrochromatography.

PubMed

Fanali, S; Catarcini, P; Blaschke, G; Chankvetadze, B

2001-09-01

The review summarizes recent developments in enantioseparations by capillary electrochromatography (CEC). Selected fundamental aspects of CEC are discussed in order to stress those features which may allow the success of this technique in the competitive field of enantioseparations. In addition, the comparative characteristics of the different modes of chiral CEC and the stationary phases are presented. The effects of the characteristics of the stationary and liquid phases and operational conditions on the separation results are discussed. Finally, some future trends are briefly addressed.

Influence of gas-liquid two-phase flow on angiotensin-I converting enzyme inhibitory peptides separation by ultra-filtration.

PubMed

Charoenphun, Narin; Youravong, Wirote

2017-01-01

Membrane fouling is a major problem in ultra-filtration systems and two-phase flow is a promising technique for permeate flux enhancement. The objective of this research was to study the use of an ultra-filtration (UF) system to enrich angiotensin-I converting enzyme (ACE) inhibitory peptides from tilapia protein hydrolysate. To select the most appropriate membrane and operating condition, the effects of membrane molecular weight cut-off (MWCO), transmembrane pressure (TMP) and cross-flow velocity (CFV) on permeate flux and ACE inhibitory peptide separation were studied. Additionally, the gas-liquid two-phase flow technique was applied to investigate its effect on the process capability. The results showed that the highest ACE inhibitory activity was obtained from permeate of the 1 kDa membrane. In terms of TMP and CFV, the permeate flux tended to increase with TMP and CFV. The use of gas-liquid two-phase flow as indicated by shear stress number could reduce membrane fouling and increase the permeate flux up to 42%, depending on shear stress number. Moreover, the use of a shear stress number of 0.039 led to an augmentation in ACE inhibitory activity of permeates. Operating conditions using a shear stress number of 0.039 were recommended for enrichment of ACE inhibitory peptides. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

Review on Ion Mobility Spectrometry. Part 1: Current Instrumentation

PubMed Central

Cumeras, R.; Figueras, E.; Davis, C.E.; Baumbach, J.I.; Gràcia, I.

2014-01-01

Ion Mobility Spectrometry (IMS) is a widely used and ‘well-known’ technique of ion separation in gaseous phase based on the differences of ion mobilities under an electric field. All IMS instruments operate with an electric field that provides space separation, but some IMS instruments also operate with a drift gas flow which provides also a temporal separation. In this review we will summarize the current IMS instrumentation. IMS techniques have received an increased interest as new instrumentation has become available to be coupled with mass spectrometry (MS). For each of the eight types of IMS instruments reviewed it is mentioned whether they can be hyphenated with MS and whether they are commercially available. Finally, out of the described devices, the six most-consolidated ones are compared. The current review article is followed by a companion review article which details the IMS hyphenated techniques (mainly gas chromatography and mass spectrometry) and the factors that make the data from an IMS device change as function of device parameters and sampling conditions. These reviews will provide the reader with an insightful view of the main characteristics and aspects of the IMS technique. PMID:25465076

[The determination of molecular sulphur in Matsesta mineral water and its analog Novonukutskaya mineral water].

PubMed

Khutorianskiĭ, V A; Smirnov, A I; Matveev, D A

2014-01-01

The method of microcolumn reversed phase high performance liquid chromatography (rp-HPLC) was employed to determine the content of elemental sulphur in mineral waters. The study envisaged the analysis of the samples of sulphide-containing mineral waters Novonukutskaya and Matsesta obtained by the solid phase extraction technique. Based on these data, the authors discuss the origin and the circulation of sulphur in the hydrogen sulphide sources. The elution conditions selected in this study ensured the high-resolution separation of the octasulphur peak from the peaks of allotropic components of the extract whereas the two-wave detection technique allowed to identify the peaks of molecular sulphur.

Novel strategies for sample preparation in forensic toxicology.

PubMed

Samanidou, Victoria; Kovatsi, Leda; Fragou, Domniki; Rentifis, Konstantinos

2011-09-01

This paper provides a review of novel strategies for sample preparation in forensic toxicology. The review initially outlines the principle of each technique, followed by sections addressing each class of abused drugs separately. The novel strategies currently reviewed focus on the preparation of various biological samples for the subsequent determination of opiates, benzodiazepines, amphetamines, cocaine, hallucinogens, tricyclic antidepressants, antipsychotics and cannabinoids. According to our experience, these analytes are the most frequently responsible for intoxications in Greece. The applications of techniques such as disposable pipette extraction, microextraction by packed sorbent, matrix solid-phase dispersion, solid-phase microextraction, polymer monolith microextraction, stir bar sorptive extraction and others, which are rapidly gaining acceptance in the field of toxicology, are currently reviewed.

Solvent viscosity mismatch between the solute plug and the mobile phase: Considerations in the applications of two-dimensional HPLC

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

Shalliker, R. Andrew; Guiochon, Georges A

Understanding the nature of viscosity contrast induced flow instabilities is an important aspect in the design of two-dimensional HPLC separations. When the viscosity contrast between the sample plug and the mobile phase is sufficiently large, the phenomenon known as viscous fingering can be induced. Viscous fingering is a flow instability phenomenon that occurs at the interface between two fluids with different viscosities. In liquid chromatography, viscous fingering results in the solute band undergoing a change in form as it enters into the chromatography column. Moreover, even in the absence of viscous fingering, band shapes change shape at low viscosity contrasts.more » These changes can result in a noticeable change in separation performance, with the result depending on whether the solvent pushing the solute plug has a higher or lower viscosity than the solute plug. These viscosity induced changes become more important as the solute injection volume increases and hence understanding the process becomes critical in the implementation of multidimensional HPLC techniques, since in these techniques the sample injection plug into the second dimension is an order of magnitude greater than in one-dimensional HPLC. This review article assesses the current understanding of the viscosity contrast induced processes as they relate to liquid chromatographic separation behaviour.« less

Laser capillary spectrophotometric acquisition of bivariate drop size and concentration data for liquid-liquid dispersion

DOEpatents

Tavlarides, Lawrence L.; Bae, Jae-Heum

1991-01-01

A laser capillary spectrophotometric technique measures real time or near real time bivariate drop size and concentration distribution for a reactive liquid-liquid dispersion system. The dispersion is drawn into a precision-bore glass capillary and an appropriate light source is used to distinguish the aqueous phase from slugs of the organic phase at two points along the capillary whose separation is precisely known. The suction velocity is measured, as is the length of each slug from which the drop free diameter is calculated. For each drop, the absorptivity at a given wavelength is related to the molar concentration of a solute of interest, and the concentration of given drops of the organic phase is derived from pulse heights of the detected light. This technique permits on-line monitoring and control of liquid-liquid dispersion processes.

Solidification studies of nanocrystalline and quasicrystalline materials from the undercooled state

NASA Astrophysics Data System (ADS)

Croat, Thomas Kevin

2001-07-01

Nanocrystallization occurring during metallic glass devitrification is studied in Zr-Al-Ni-Cu bulk metallic glasses (BMGs) and Al-RE-TM (RE = rare-earth, TM = transition metal) metallic glasses. The importance of transient nucleation in BMG devitrification was established by a direct transmission electron microscopy (TEM) measurement of the grain density in two-stage annealed samples. TEM examination of low temperature annealed BMGs also suggest that amorphous phase separation is occurring prior to crystallization. Nanocrystallization of rapidly quenched Al-RE-Ni glasses was preceded by the compositional segregation of the initially homogeneous glass into Al-rich and solute-rich regions (mainly nickel-enriched) on a ≈50--100 nm length scale, suggesting amorphous phase separation. This pre-existing compositional modulation on a nanometer scale leads naturally to the development of nanocrystals. The average rare earth radius (rRE) in Al-RE-Ni alloys was altered by co-substitution of chemically similar rare earth elements. In glasses with smaller r RE, nucleation of alpha-Al occurred preferentially near the boundaries of the phase-separated regions. However, phase separation did not universally lead to alpha-Al nanocrystallization; glasses with larger rRE crystallized to metastable intermetallic phases with a 50--100 nm grain size. Kinetic analysis of the alpha-Al crystallization was performed using isothermal DSC, yielding abnormally low Avrami exponents (n = 1.0--1.5); these values were found to be consistent with the observed transformation using a model that considers the overlapping diffusion fields of the alpha-Al grains during growth within the phase separated region. Containerless solidification experiments on Ti-based quasicrystal-forming alloys have been performed using various techniques, including drop-tube solidification, electromagnetic levitation (EML) and electrostatic levitation (ESL). In Ti-Fe-Si-O, the alpha-1/1 quasicrystal approximant phase is found to nucleate directly from the liquid over the range TixFe94-xSi 4(SiO2)2 with 67 < x < 69 in EML experiments. Both the alpha-1/1 phase in Ti-Fe-Si-O and the C14 Laves phase in Ti-Zr-Ni have lower relative undercoolings than nearby crystal phases. This presumably reflects the structural similarity between these polytetrahedral phases and the undercooled liquid, which leads to smaller nucleation barriers and lower maximum undercoolings.

Highly efficient peptide separations in proteomics Part 1. Unidimensional high performance liquid chromatography.

PubMed

Sandra, Koen; Moshir, Mahan; D'hondt, Filip; Verleysen, Katleen; Kas, Koen; Sandra, Pat

2008-04-15

Sample complexity and dynamic range constitute enormous challenges in proteome analysis. The back-end technology in typical proteomics platforms, namely mass spectrometry (MS), can only tolerate a certain complexity, has a limited dynamic range per spectrum and is very sensitive towards ion suppression. Therefore, component overlap has to be minimized for successful mass spectrometric analysis and subsequent protein identification and quantification. The present review describes the advances that have been made in liquid-based separation techniques with focus on the recent developments to boost the resolving power. The review is divided in two parts; the first part deals with unidimensional liquid chromatography and the second part with bi- and multidimensional liquid-based separation techniques. Part 1 mainly focuses on reversed-phase HPLC due to the fact that it is and will, in the near future, remain the technique of choice to be hyphenated with MS. The impact of increasing the column length, decreasing the particle diameter, replacing the traditional packed beds by monolithics, amongst others, is described. The review is complemented with data obtained in the laboratories of the authors.

Characterizing plant cell wall derived oligosaccharides using hydrophilic interaction chromatography with mass spectrometry detection.

PubMed

Leijdekkers, A G M; Sanders, M G; Schols, H A; Gruppen, H

2011-12-23

Analysis of complex mixtures of plant cell wall derived oligosaccharides is still challenging and multiple analytical techniques are often required for separation and characterization of these mixtures. In this work it is demonstrated that hydrophilic interaction chromatography coupled with evaporative light scattering and mass spectrometry detection (HILIC-ELSD-MS(n)) is a valuable tool for identification of a wide range of neutral and acidic cell wall derived oligosaccharides. The separation potential for acidic oligosaccharides observed with HILIC is much better compared to other existing techniques, like capillary electrophoresis, reversed phase and porous-graphitized carbon chromatography. Important structural information, such as presence of methyl esters and acetyl groups, is retained during analysis. Separation of acidic oligosaccharides with equal charge yet with different degrees of polymerization can be obtained. The efficient coupling of HILIC with ELSD and MS(n)-detection enables characterization and quantification of many different oligosaccharide structures present in complex mixtures. This makes HILIC-ELSD-MS(n) a versatile and powerful additional technique in plant cell wall analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

Scanning measurement of Seebeck coefficient of a heated sample

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

Snyder, G. Jeffrey; Iwanaga, Shiho

2016-04-19

A novel scanning Seebeck coefficient measurement technique is disclosed utilizing a cold scanning thermocouple probe tip on heated bulk and thin film samples. The system measures variations in the Seebeck coefficient within the samples. The apparatus may be used for two dimensional mapping of the Seebeck coefficient on the bulk and thin film samples. This technique can be utilized for detection of defective regions, as well as phase separations in the sub-mm range of various thermoelectric materials.

Magneto-electronic phase separation in doped cobaltites

NASA Astrophysics Data System (ADS)

He, Chunyong

This thesis work mainly focuses on magneto-electronic phase separation (MEPS), an effect where chemically homogeneous materials display inhomogeneous magnetic and electronic properties. A model system La1-xSrxCoO3 (LSCO) is chosen for the study of MEPS. The doping evolution of MEPS in LSCO single crystals is extensively studied through complementary experimental techniques including heat capacity, small angle neutron scattering, magnetometry, and transport. It is found that there exists a finite doping range over which MEPS occurs. The doping range determined from different experimental techniques is found to be in good agreement. Also, this same doping range is reproduced by statistical simulations incorporating local compositional fluctuations. The excellent agreement between experimental data and statistical simulations leads to the conclusion that the MEPS in LSCO is driven solely by inevitable local compositional fluctuations at nanoscopic length scales. Such a conclusion indicates that nanoscopic MEPS is doping fluctuation-driven rather than electronically-driven in LSCO. The effect of microscopic magneto-electronic phase separation on electrical transport in LSCO is also examined. It is demonstrated (i) that the T = 0 metal-insulator transition can be understood within double exchange-modified percolation framework, and, (ii) that the onset of a phase-pure low T ferromagnetic state at high x has a profound effect on the high T transport. In addition, a new origin for finite spin Co ions in LaCoO3 is revealed via a Schottky Anomaly in the heat capacity, which was not previously known. Such a discovery casts a new understanding of the spin state at low temperature. Via small-angle neutron scattering and d.c. susceptibility, it is revealed that short-range ordered FM clusters exist below a well-defined temperature (T*) in highly doped LSCO. It is demonstrated that the characteristics of this clustered state appear quite unlike those of a Griffiths phase. Finally, through magenetometry and SANS, the magneto-crystalline anisotropy of highly doped LSCO is studied and the easy and hard magnetization axes are determined.

Determination of tetraalkyllead compounds in gasoline by liquid chromatography-atomic absorption spectrometry

USGS Publications Warehouse

Messman, J.D.; Rains, T.C.

1981-01-01

A liquid chromatography-atomic absorption spectrometry (LC-AAS) hybrid analytical technique is presented for metal speciation measurements on complex liquid samples. The versatility and inherent metal selectivity of the technique are Illustrated by the rapid determination of five tetraalkyllead compounds in commercial gasoline. Separation of the individual tetraalkyllead species is achieved by reversed-phase liquid chromatography using an acetonitrile/water mobile phase. The effluent from the liquid Chromatograph Is introduced directly into the aspiration uptake capillary of the nebulizer of an air/acetylene flame atomic absorption spectrometer. Spectral interferences due to coeluting hydrocarbon matrix constituents were not observed at the 283.3-nm resonance line of lead used for analysis. Detection limits of this LC-AAS hydrid analytical technique, based on a 20-??L injection, are approximately 10 ng Pb for each tetraalkyllead compound.

Accuracy of a separating foil impression using a novel polyolefin foil compared to a custom tray and a stock tray technique

PubMed Central

Pastoret, Marie-Hélène; Bühler, Julia; Weiger, Roland

2017-01-01

PURPOSE To compare the dimensional accuracy of three impression techniques- a separating foil impression, a custom tray impression, and a stock tray impression. MATERIALS AND METHODS A machined mandibular complete-arch metal model with special modifications served as a master cast. Three different impression techniques (n = 6 in each group) were performed with addition-cured silicon materials: i) putty-wash technique with a prefabricated metal tray (MET) using putty and regular body, ii) single-phase impression with custom tray (CUS) using regular body material, and iii) two-stage technique with stock metal tray (SEP) using putty with a separating foil and regular body material. All impressions were poured with epoxy resin. Six different distances (four intra-abutment and two inter-abutment distances) were gauged on the metal master model and on the casts with a microscope in combination with calibrated measuring software. The differences of the evaluated distances between the reference and the three test groups were calculated and expressed as mean (± SD). Additionally, the 95% confidence intervals were calculated and significant differences between the experimental groups were assumed when confidence intervals did not overlap. RESULTS Dimensional changes compared to reference values varied between -74.01 and 32.57 µm (MET), -78.86 and 30.84 (CUS), and between -92.20 and 30.98 (SEP). For the intra-abutment distances, no significant differences among the experimental groups were detected. CUS showed a significantly higher dimensional accuracy for the inter-abutment distances with -0.02 and -0.08 percentage deviation compared to MET and SEP. CONCLUSION The separation foil technique is a simple alternative to the custom tray technique for single tooth restorations, while limitations may exist for extended restorations with multiple abutment teeth. PMID:28874996

Phase stability, ordering tendencies, and magnetism in single-phase fcc Au-Fe nanoalloys

DOE PAGES

Zhuravlev, I. A.; Barabash, S. V.; An, J. M.; ...

2017-10-01

Bulk Au-Fe alloys separate into Au-based fcc and Fe-based bcc phases, but L1 0 and L1 2 orderings were reported in single-phase Au-Fe nanoparticles. Motivated by these observations, we study the structural and ordering energetics in this alloy by combining density functional theory (DFT) calculations with effective Hamiltonian techniques: a cluster expansion with structural filters, and the configuration-dependent lattice deformation model. The phase separation tendency in Au-Fe persists even if the fcc-bcc decomposition is suppressed. The relative stability of disordered bcc and fcc phases observed in nanoparticles is reproduced, but the fully ordered L1 0 AuFe, L1 2 Au 3Fe,more » and L1 2 AuFe 3 structures are unstable in DFT. But, a tendency to form concentration waves at the corresponding [001] ordering vector is revealed in nearly-random alloys in a certain range of concentrations. Furthermore, this incipient ordering requires enrichment by Fe relative to the equiatomic composition, which may occur in the core of a nanoparticle due to the segregation of Au to the surface. Effects of magnetism on the chemical ordering are also discussed.« less

Phase stability, ordering tendencies, and magnetism in single-phase fcc Au-Fe nanoalloys

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

Zhuravlev, I. A.; Barabash, S. V.; An, J. M.

Bulk Au-Fe alloys separate into Au-based fcc and Fe-based bcc phases, but L1 0 and L1 2 orderings were reported in single-phase Au-Fe nanoparticles. Motivated by these observations, we study the structural and ordering energetics in this alloy by combining density functional theory (DFT) calculations with effective Hamiltonian techniques: a cluster expansion with structural filters, and the configuration-dependent lattice deformation model. The phase separation tendency in Au-Fe persists even if the fcc-bcc decomposition is suppressed. The relative stability of disordered bcc and fcc phases observed in nanoparticles is reproduced, but the fully ordered L1 0 AuFe, L1 2 Au 3Fe,more » and L1 2 AuFe 3 structures are unstable in DFT. But, a tendency to form concentration waves at the corresponding [001] ordering vector is revealed in nearly-random alloys in a certain range of concentrations. Furthermore, this incipient ordering requires enrichment by Fe relative to the equiatomic composition, which may occur in the core of a nanoparticle due to the segregation of Au to the surface. Effects of magnetism on the chemical ordering are also discussed.« less

On MIMO-UFMC in the Presence of Phase Noise and Antenna Mutual Coupling

NASA Astrophysics Data System (ADS)

Chen, Xiaoming; Zhang, Shuai; Zhang, Anxue

2017-11-01

The universal filtered multicarrier (UFMC) technique has been proposed as a waveform candidate for the fifth generation (5G) communications and beyond 5G. Compared with conventional orthogonal frequency division multiplexing (OFDM), UFMC has lower out-of-band emission and is also compatible with the multiple-input multiple-output (MIMO) technique. However, like other multicarrier waveforms, it suffers from phase noise of imperfect oscillator. In contrast to the rich literature on phase noise effect on MIMO-OFDM (where the antenna mutual coupling effect is usually omitted though), there is little work investigating the phase noise effect on MIMO-UFMC. In this paper, we study the MIMO-UFMC systems in the presence of phase noise and with/without mutual coupling effect. A phase noise mitigation scheme for MIMO-UFMC systems is presented. The scheme does not require detailed knowledge of the phase noise statistics and can effectively mitigate the phase noise within each UFMC symbol. Moreover, it is shown that at small antenna separations, the performance of the MIMO-UFMC system taking the mutual coupling effect into account is better than that when the mutual coupling effect is overlooked.

Organised surfactant assemblies in analytical atomic spectrometry

NASA Astrophysics Data System (ADS)

Sanz-Medel, Alfredo; Fernandez de la Campa, Maria del Rosario; Gonzalez, Elisa Blanco; Fernandez-Sanchez, Maria Luisa

1999-02-01

The use of surfactant-based organised assemblies in analytical atomic spectroscopy is extensively and critically reviewed along three main lines: first, the ability of organised media to enhance detection of atomic spectroscopic methods by favourable manipulation of physical and chemical properties of the sample solution second, the extension of separation mechanisms by resorting to organised media and third a discussion of synergistic combinations of liquid chromatography separations and atomic detectors via the use of vesicular mobile phases. Changes in physical properties of sample solutions aspirated in atomic spectrometry by addition of surfactants can be advantageously used in at least four different ways: (i) to improve nebulisation efficiency; (ii) to enhance wettability of solid surfaces used for atomisation; (iii) to improve compatibility between aqueous and organic phases; and (iv) to achieve good dispersion of small particles in "slurry" techniques. Controversial results and statements published so far are critically discussed. The ability of surfactant-based organised assemblies, such as micelles and vesicles, to organise reactants at the molecular level has also been applied to enhance the characteristics of chemical generation of volalite species of metals and semi-metals (e.g., hydride or ethylide generation of As, Pb, Cd, Se, Sn, and cold vapour Hg generation) used in atomic methods. Enhancements in efficiency/transport of volatile species, increases in the reaction kinetics, stabilisation of some unstable species and changes in the selectivity of the reactions by surfactants are dealt with. Non-chromatographic cloud-point separations to design pre-concentration procedures with subsequent metal determination by atomic methods are addressed along with chromatographic separations of expanded scope by addition of surfactants to the conventional aqueous mobile phases of reversed-phase high-performance liquid chromatography. Finally, the synergistic effect of using vesicles to improve both the separation capabilities of reversed-phase HPLC and the detectability of atomic detectors by on-line vesicular hydride generation is described. In particular, the possible separation mechanisms responsible for micellar and vesicular mobile phases in reversed-phase chromatographies are analysed and compared. The possible effect of modification of stationary phases by monomers of the surfactants should also be taken into account. The application of such on-line couplings to develop new hybrid approaches to tackle modern problems of trace element speciation for As, Hg, Se, and Cd completes this revision of the present interface between analytical atomic spectroscopy and surfactant-based organised assemblies.

Spectral separation of gaseous fluorocarbon mixtures and measurement of diffusion constants by 19F gas phase DOSY NMR.

PubMed

Marchione, Alexander A; McCord, Elizabeth F

2009-11-01

Diffusion-ordered (DOSY) NMR techniques have for the first time been applied to the spectral separation of mixtures of fluorinated gases by diffusion rates. A mixture of linear perfluoroalkanes from methane to hexane was readily separated at 25 degrees C in an ordinary experimental setup with standard DOSY pulse sequences. Partial separation of variously fluorinated ethanes was also achieved. The constants of self-diffusion of a set of pure perfluoroalkanes were obtained at pressures from 0.25 to 1.34 atm and temperatures from 20 to 122 degrees C. Under all conditions there was agreement within 20% of experimental self-diffusion constant D and values calculated by the semiempirical Fuller method.

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

James K. Neathery; Gary Jacobs; Burtron H. Davis

In this reporting period, a fundamental filtration study was started to investigate the separation of Fischer-Tropsch Synthesis (FTS) liquids from iron-based catalyst particles. Slurry-phase FTS in slurry bubble column reactor systems is the preferred mode of production since the reaction is highly exothermic. Consequently, heavy wax products must be separated from catalyst particles before being removed from the reactor system. Achieving an efficient wax product separation from iron-based catalysts is one of the most challenging technical problems associated with slurry-phase FTS. The separation problem is further compounded by catalyst particle attrition and the formation of ultra-fine iron carbide and/or carbonmore » particles. Existing pilot-scale equipment was modified to include a filtration test apparatus. After undergoing an extensive plant shakedown period, filtration tests with cross-flow filter modules using simulant FTS wax slurry were conducted. The focus of these early tests was to find adequate mixtures of polyethylene wax to simulate FTS wax. Catalyst particle size analysis techniques were also developed. Initial analyses of the slurry and filter permeate particles will be used by the research team to design improved filter media and cleaning strategies.« less

Real-time terahertz imaging through self-mixing in a quantum-cascade laser

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

Wienold, M., E-mail: martin.wienold@dlr.de; Rothbart, N.; Hübers, H.-W.

2016-07-04

We report on a fast self-mixing approach for real-time, coherent terahertz imaging based on a quantum-cascade laser and a scanning mirror. Due to a fast deflection of the terahertz beam, images with frame rates up to several Hz are obtained, eventually limited by the mechanical inertia of the employed scanning mirror. A phase modulation technique allows for the separation of the amplitude and phase information without the necessity of parameter fitting routines. We further demonstrate the potential for transmission imaging.

DANCING IN THE DARK: NEW BROWN DWARF BINARIES FROM KERNEL PHASE INTERFEROMETRY

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

Pope, Benjamin; Tuthill, Peter; Martinache, Frantz, E-mail: bjsp@physics.usyd.edu.au, E-mail: p.tuthill@physics.usyd.edu.au, E-mail: frantz@naoj.org

2013-04-20

This paper revisits a sample of ultracool dwarfs in the solar neighborhood previously observed with the Hubble Space Telescope's NICMOS NIC1 instrument. We have applied a novel high angular resolution data analysis technique based on the extraction and fitting of kernel phases to archival data. This was found to deliver a dramatic improvement over earlier analysis methods, permitting a search for companions down to projected separations of {approx}1 AU on NIC1 snapshot images. We reveal five new close binary candidates and present revised astrometry on previously known binaries, all of which were recovered with the technique. The new candidate binariesmore » have sufficiently close separation to determine dynamical masses in a short-term observing campaign. We also present four marginal detections of objects which may be very close binaries or high-contrast companions. Including only confident detections within 19 pc, we report a binary fraction of at least #Greek Lunate Epsilon Symbol#{sub b} = 17.2{sub -3.7}{sup +5.7}%. The results reported here provide new insights into the population of nearby ultracool binaries, while also offering an incisive case study of the benefits conferred by the kernel phase approach in the recovery of companions within a few resolution elements of the point-spread function core.« less

Combination of novel coalescing oil water separator and electrocoagulation technique for treatment of petroleum compound contaminated groundwater.

PubMed

Oladzad, Sepideh; Fallah, Narges; Nasernejad, Bahram

2017-07-01

In the present study a combination of a novel coalescing oil water separator (COWS) and electrocoagulation (EC) technique was used for treatment of petroleum product contaminated groundwater. In the first phase, COWS was used as the primary treatment. Two different types of coalescing media and two levels of flow rates were examined in order to find the optimum conditions. The effluent of COWS was collected in optimum conditions and was treated using an EC process in the second phase of the research. In this phase, preliminary experiments were conducted in order to investigate the effect of EC reaction time and sedimentation time on chemical oxygen demand (COD) removal efficiency. Best conditions for EC reaction time and sedimentation time were obtained to be 5 min and 30 min, respectively. Response surface methodology was applied to evaluate the effect of initial pH, current density and aeration rate on settling velocity (V s ) and effluent COD. The optimum conditions, for achieving maximum values of V s as well as the values of effluent COD, in the range of results were obtained at conditions of 7, 34 mA·cm -2 and 1.5 L·min -1 for initial pH, current density and aeration rate, respectively.

Integrating Elemental Analysis and Chromatography Techniques by Analyzing Metal Oxide and Organic UV Absorbers in Commercial Sunscreens

ERIC Educational Resources Information Center

Quin~ones, Rosalynn; Bayline, Jennifer Logan; Polvani, Deborah A.; Neff, David; Westfall, Tamara D.; Hijazi, Abdullah

2016-01-01

A series of undergraduate laboratory experiments that utilize reversed-phase HPLC separation, inductively coupled plasma spectroscopy (ICP), and scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS) are described for the analysis of commercial sunscreens. The active ingredients of many sunscreen brands include zinc or titanium…

Separation of cucurbitane triterpenoids from bitter melon drinks and determination of partition coefficients using vortex-assisted dispersive liquid-phase microextraction followed by UHPLC analysis

USDA-ARS?s Scientific Manuscript database

A rapid, effective technique applying vortex-assisted liquid–liquid microextraction (VALLME) prior to ultra high performance liquid chromatography-evaporating light scattering detectection/ mass spectroscopy (UHPLC-ELSD/MS) determination was developed for the analysis of four cucurbitane triterpenoi...

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

PubMed

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

2016-10-07

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

Trace analysis of nitrite ions in environmental samples by using in-situ synthesized Zein biopolymeric nanoparticles as the novel green solid phase extractor.

PubMed

Hatamie, Amir; Nassiri, Mahmoud; Alivand, Meghdad Doust; Bhatnagar, Amit

2018-01-01

For the first time, a novel green method using Zein biopolymeric nanoparticles as a green dispersive solid-phase extractor is reported for the separation and preconcentration of trace amount of nitrite (NO 2 - ) ions in ppb levels. The Zein protein is a biodegradable hydrophobic plant protein that is obtained from corn and is composed of a number of hydrophobic amino acids. Zein bionanoparticles were synthesized in an anti-solvent process and used as a new biosorbent in the extraction technique. In the proposed technique, by using a standard method at first, a mixture of 1-naphthylamine and sulphanilic acid as selective regents was added to the samples, and in the presence of the nitrite ion, a red azo product was formed. After that, the ethanolic Zein solution (equal to 15mg) was injected rapidly into the sample, based on the anti-solvent process. Zein bionanoparticles (BNPs) were produced, the adsorbed colour product was separated by centrifugation, and finally samples were analysed with the spectrophotometric method. The influence of different variables such as pH, buffer and amount of buffer, amount of adsorbent and effect of time on extraction were investigated and Zein BNPs were characterized by TEM, SEM, and FT-IR techniques. The main advantages of Zein as a new solid-phase extractor are that this biopolymer is non-toxic, stable, widely available, biodegradable, very hydrophobic, and can be fabricated easily. Under optimal experimental conditions, the linear correlation coefficient (r 2 ) was found to be 0.9972 at the concentration range of 5.0-1000ngmL -1 . The limit of detection was 2.3ngmL -1 (0.05μM). This method was applied successfully for the analysis of sea and river waters as well as industrial wastewater samples. Finally, this method follows the US EPA (US Environmental Protection Agency) and WHO (World Health Organization) international standards for nitrite analysis. In addition, it has several advantages to warrant its applicability in the near future in separation science as a green biosorbent in both dispersive and normal solid-phase extraction. Copyright © 2017. Published by Elsevier B.V.

Large-scale phase separation with nano-twin domains in manganite spinel (Co,Fe,Mn){sub 3}O{sub 4}

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

Horibe, Y., E-mail: horibe@post.matsc.kyutech.ac.jp; Takeyama, S.; Mori, S.

The effect of Mn concentration on the formation of nano-domain structures in the spinel oxide (Co,Fe,Mn){sub 3}O{sub 4} was investigated by electron diffraction, bright-, and dark-field imaging technique with transmission electron microscopy. Large scale phase separation with nano-twin domains was observed in Co{sub 0.6}Fe{sub 1.0}Mn{sub 1.4}O{sub 4}, in contrast to the highly aligned checkerboard nano-domains in Co{sub 0.6}Fe{sub 0.9}Mn{sub 1.5}O{sub 4}. Diffusion of the Mn{sup 3+} ions with the Jahn-Teller distortions is suggested to play an important role in the formation of checkerboard nano-domain structure.

A unique measurement technique to study laminar-separation bubble characteristics on an airfoil

NASA Technical Reports Server (NTRS)

Stack, J. P.; Mangalam, S. M.; Berry, S. A.

1987-01-01

A 'nonintrusive', multielement heat-transfer sensor was designed to study laminar-separation bubble characteristics on a NASA LRN (1)-1010 low-Reynolds number airfoil. The sensor consists of 30 individual nickel films, vacuum-deposited on a thin substrate (0.05 mm) that was bonded to the airfoil model with the sensor array placed streamwise on the airfoil upper surface. Experiments were conducted on a 15-cm chord model in the 50,000-300,000 chord Reynolds number range. Time history as well as spectral analysis of signals from surface film gauges were simultaneously obtained to determine the location of laminar separation and the subsequent behavior of the separated shear layer. In addition to the successful determination of laminar separation, a new phenomenon involving a large phase shift in dynamic shear stresses across the separation and reattachment points was observed.

Direct Observations of a Dynamically Driven Phase Transition with in situ X-Ray Diffraction in a Simple Ionic Crystal

NASA Astrophysics Data System (ADS)

Kalita, Patricia; Specht, Paul; Root, Seth; Sinclair, Nicholas; Schuman, Adam; White, Melanie; Cornelius, Andrew L.; Smith, Jesse; Sinogeikin, Stanislav

2017-12-01

We report real-time observations of a phase transition in the ionic solid CaF2 , a model A B2 structure in high-pressure physics. Synchrotron x-ray diffraction coupled with dynamic loading to 27.7 GPa, and separately with static compression, follows, in situ, the fluorite to cotunnite structural phase transition, both on nanosecond and on minute time scales. Using Rietveld refinement techniques, we examine the kinetics and hysteresis of the transition. Our results give insight into the kinetic time scale of the fluorite-cotunnite phase transition under shock compression, which is relevant to a number of isomorphic compounds.

Direct Observations of a Dynamically Driven Phase Transition with in situ X-Ray Diffraction in a Simple Ionic Crystal

DOE PAGES

Kalita, Patricia E.; Specht, Paul Elliot; Root, Seth; ...

2017-12-21

Here, we report real-time observations of a phase transition in the ionic solid CaF 2, a model AB 2 structure in high-pressure physics. Synchrotron x-ray diffraction coupled with dynamic loading to 27.7 GPa, and separately with static compression, follows, in situ, the fluorite to cotunnite structural phase transition, both on nanosecond and on minute time scales. Using Rietveld refinement techniques, we examine the kinetics and hysteresis of the transition. Our results give insight into the kinetic time scale of the fluorite-cotunnite phase transition under shock compression, which is relevant to a number of isomorphic compounds.

Computational techniques for flows with finite-rate condensation

NASA Technical Reports Server (NTRS)

Candler, Graham V.

1993-01-01

A computational method to simulate the inviscid two-dimensional flow of a two-phase fluid was developed. This computational technique treats the gas phase and each of a prescribed number of particle sizes as separate fluids which are allowed to interact with one another. Thus, each particle-size class is allowed to move through the fluid at its own velocity at each point in the flow field. Mass, momentum, and energy are exchanged between each particle class and the gas phase. It is assumed that the particles do not collide with one another, so that there is no inter-particle exchange of momentum and energy. However, the particles are allowed to grow, and therefore, they may change from one size class to another. Appropriate rates of mass, momentum, and energy exchange between the gas and particle phases and between the different particle classes were developed. A numerical method was developed for use with this equation set. Several test cases were computed and show qualitative agreement with previous calculations.

Reduction-melting combined with a Na₂CO₃ flux recycling process for lead recovery from cathode ray tube funnel glass.

PubMed

Okada, Takashi; Yonezawa, Susumu

2014-08-01

With large quantity of flux (Na2CO3), lead can be recovered from the funnel glass of waste cathode-ray tubes via reduction-melting at 1000°C. To reduce flux cost, a technique to recover added flux from the generated oxide phase is also important in order to recycle the flux recovered from the reduction-melting process. In this study, the phase separation of sodium and the crystallization of water-soluble sodium silicates were induced after the reduction-melting process to enhance the leachability of sodium in the oxide phase and to extract the sodium from the phase for the recovery of Na2CO3 as flux. A reductive atmosphere promoted the phase separation and crystallization, and the leachability of sodium from the oxide phase was enhanced. The optimum temperature and treatment time for increasing the leachability were 700°C and 2h, respectively. After treatment, more than 90% of the sodium in the oxide phase was extracted in water. NaHCO3 can be recovered by carbonization of the solution containing sodium ions using carbon dioxide gas, decomposed to Na2CO3 at 50°C and recycled for use in the reduction-melting process. Copyright © 2014 Elsevier Ltd. All rights reserved.

Noise-Source Separation Using Internal and Far-Field Sensors for a Full-Scale Turbofan Engine

NASA Technical Reports Server (NTRS)

Hultgren, Lennart S.; Miles, Jeffrey H.

2009-01-01

Noise-source separation techniques for the extraction of the sub-dominant combustion noise from the total noise signatures obtained in static-engine tests are described. Three methods are applied to data from a static, full-scale engine test. Both 1/3-octave and narrow-band results are discussed. The results are used to assess the combustion-noise prediction capability of the Aircraft Noise Prediction Program (ANOPP). A new additional phase-angle-based discriminator for the three-signal method is also introduced.

Retention and effective diffusion of model metabolites on porous graphitic carbon.

PubMed

Lunn, Daniel B; Yun, Young J; Jorgenson, James W

2017-12-29

The study of metabolites in biological samples is of high interest for a wide range of biological and pharmaceutical applications. Reversed phase liquid chromatography is a common technique used for the separation of metabolites, but it provides little retention for polar metabolites. An alternative to C18 bonded phases, porous graphitic carbon has the ability to provide significant retention for both non-polar and polar analytes. The goal of this work is to study the retention and effective diffusion properties of porous graphitic carbon, to see if it is suitable for the wide injection bands and long run times associated with long, packed capillary-scale separations. The retention of a set of standard metabolites was studied for both stationary phases over a wide range of mobile phase conditions. This data showed that porous graphitic carbon benefits from significantly increased retention (often >100 fold) under initial gradient conditions for these metabolites, suggesting much improved ability to focus a wide injection band at the column inlet. The effective diffusion properties of these columns were studied using peak-parking experiments with the standard metabolites under a wide range of retention conditions. Under the high retention conditions, which can be associated with retention after injection loading for gradient separations, D eff /D m ∼0.1 for both the C18-bonded and porous graphitic carbon columns. As C18 bonded particles are widely, and successfully utilized for long gradient separations without issue of increasing peak width from longitudinal diffusion, this suggests that porous graphitic carbon should be amenable for long runtime gradient separations as well. Copyright © 2017 Elsevier B.V. All rights reserved.

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.

Electroencephalography and quantitative electroencephalography in mild traumatic brain injury.

PubMed

Haneef, Zulfi; Levin, Harvey S; Frost, James D; Mizrahi, Eli M

2013-04-15

Mild traumatic brain injury (mTBI) causes brain injury resulting in electrophysiologic abnormalities visible in electroencephalography (EEG) recordings. Quantitative EEG (qEEG) makes use of quantitative techniques to analyze EEG characteristics such as frequency, amplitude, coherence, power, phase, and symmetry over time independently or in combination. QEEG has been evaluated for its use in making a diagnosis of mTBI and assessing prognosis, including the likelihood of progressing to the postconcussive syndrome (PCS) phase. We review the EEG and qEEG changes of mTBI described in the literature. An attempt is made to separate the findings seen during the acute, subacute, and chronic phases after mTBI. Brief mention is also made of the neurobiological correlates of qEEG using neuroimaging techniques or in histopathology. Although the literature indicates the promise of qEEG in making a diagnosis and indicating prognosis of mTBI, further study is needed to corroborate and refine these methods.

Electroencephalography and Quantitative Electroencephalography in Mild Traumatic Brain Injury

PubMed Central

Levin, Harvey S.; Frost, James D.; Mizrahi, Eli M.

2013-01-01

Abstract Mild traumatic brain injury (mTBI) causes brain injury resulting in electrophysiologic abnormalities visible in electroencephalography (EEG) recordings. Quantitative EEG (qEEG) makes use of quantitative techniques to analyze EEG characteristics such as frequency, amplitude, coherence, power, phase, and symmetry over time independently or in combination. QEEG has been evaluated for its use in making a diagnosis of mTBI and assessing prognosis, including the likelihood of progressing to the postconcussive syndrome (PCS) phase. We review the EEG and qEEG changes of mTBI described in the literature. An attempt is made to separate the findings seen during the acute, subacute, and chronic phases after mTBI. Brief mention is also made of the neurobiological correlates of qEEG using neuroimaging techniques or in histopathology. Although the literature indicates the promise of qEEG in making a diagnosis and indicating prognosis of mTBI, further study is needed to corroborate and refine these methods. PMID:23249295

Laser capillary spectrophotometric acquisition of bivariate drop size and concentration data for liquid-liquid dispersion

DOEpatents

Tavlarides, L.L.; Bae, J.H.

1991-12-24

A laser capillary spectrophotometric technique measures real time or near real time bivariate drop size and concentration distribution for a reactive liquid-liquid dispersion system. The dispersion is drawn into a precision-bore glass capillary and an appropriate light source is used to distinguish the aqueous phase from slugs of the organic phase at two points along the capillary whose separation is precisely known. The suction velocity is measured, as is the length of each slug from which the drop free diameter is calculated. For each drop, the absorptivity at a given wavelength is related to the molar concentration of a solute of interest, and the concentration of given drops of the organic phase is derived from pulse heights of the detected light. This technique permits on-line monitoring and control of liquid-liquid dispersion processes. 17 figures.

Use of (N-1)-D expansions for N-D phase unwrapping in MRI

NASA Astrophysics Data System (ADS)

Bones, Philip J.; King, Laura J.; Millane, Rick P.

2017-09-01

In MRI the presence of metal implants causes severe artifacts in images and interferes with the usual techniques used to separate fat signals from other tissues. In the Dixon method, three images are acquired at different echo times to enable the variation in the magnetic field to be estimated. However, the estimate is represented as the phase of a complex quantity and therefore suffers from wrapping. High field gradients near the metal mean that the phase estimate is undersampled and therefore challenging to unwrap. We have developed POP, phase estimation by onion peeling, an algorithm which unwraps the phase along 1-D paths for a 2-D image obtained with the Dixon method. The unwrapping is initially performed along a closed path enclosing the implant and well separated from it. The recovered phase is expanded using a smooth periodic basis along the path. Then, path-by-path, the estimate is applied to the next path and then the expansion coefficients are estimated to best fit the wrapped measurements. We have successfully tested POP on MRI images of specially constructed phantoms and on a group of patients with hip implants. In principle, POP can be extended to 3-D imaging. In that case, POP would entail representing phase with a suitably smooth basis over a series of surfaces enclosing the implant (the "onion skins"), again beginning the phase estimation well away from the implant. An approach for this is proposed. Results are presented for fat and water separation for 2-D images of phantoms and actual patients. The practicality of the method and its employment in clinical MRI are discussed.

Problem of the thermodynamic status of the mixed-layer minerals

USGS Publications Warehouse

Zen, E.-A.

1962-01-01

Minerals that show mixed layering, particularly with the component layers in random sequence, pose problems because they may behave thermodynamically as single phases or as polyphase aggregates. Two operational criteria are proposed for their distinction. The first scheme requires two samples of mixed-layer material which differ only in the proportions of the layers. If each of these two samples are allowed to equilibrate with the same suitably chosen monitoring solution, then the intensive parameters of the solution will be invariant if the mixed-layer sample is a polyphase aggregate, but not otherwise. The second scheme makes use of the fact that portions of many titration curves of clay minerals show constancy of the chemical activities of the components in the equilibrating solutions, suggesting phase separation. If such phase separation occurs for a mixed-layer material, then, knowing the number of independent components in the system, it should be possible to decide on the number of phases the mixed-layer material represents. Knowledge of the phase status of mixed-layer material is essential to the study of the equilibrium relations of mineral assemblages involving such material, because a given mixed-layer mineral will be plotted and treated differently on a phase diagram, depending on whether it is a single phase or a polyphase aggregate. Extension of the titration technique to minerals other than the mixed-layer type is possible. In particular, this method may be used to determine if cryptoperthites and peristerites are polyphase aggregates. In general, for any high-order phase separation, the method may be used to decide just at what point in this continuous process the system must be regarded operationally as a polyphase aggregate. ?? 1962.

Evaluation of the separation performance of polyvinylpyrrolidone as a virtual stationary phase for chromatographic NMR.

PubMed

Huang, Shaohua; Wu, Rui; Bai, Zhengwu; Yang, Ying; Li, Suying; Dou, Xiaowei

2014-09-01

Polyvinylpyrrolidone (PVP) was used as a virtual stationary phase to separate p-xylene, benzyl alcohol, and p-methylphenol by the chromatographic NMR technique. The effects of concentration and weight-average molecular weight (Mw) of PVP, solvent viscosity, solvent polarity, and sample temperature on the resolution of these components were investigated. It was found that both higher PVP concentration and higher PVP Mw caused the increase of diffusion resolution for the three components. Moreover, the diffusion resolution did not change at viscosity-higher solvents. Moreover, the three components showed different resolution at different solvents. As temperature increased, the diffusion resolution between p-xylene and benzyl alcohol gradually increased, and the one between p-xylene and p-methylphenol slightly increased from 278 to 298 K and then decreased above 298 K. It was also found that the polarity of the analytes played an important role for the separation by affecting the diffusion coefficient. Copyright © 2014 John Wiley & Sons, Ltd.

Use of limonene in countercurrent chromatography: a green alkane substitute.

PubMed

Faure, Karine; Bouju, Elodie; Suchet, Pauline; Berthod, Alain

2013-05-07

Counter-current chromatography (CCC) is a preparative separation technique working with the two liquid phases of a biphasic liquid system. One phase is used as the mobile phase when the other, the stationary phase, is held in place by centrifugal fields. Limonene is a biorenewable cycloterpene solvent coming from orange peel waste. It was evaluated as a possible substitute for heptane in CCC separations. The limonene/methanol/water and heptane/methanol/water phase diagrams are very similar at room temperature. The double bonds of the limonene molecule allows for possible π-π interactions with solutes rendering limonene slightly more polar than heptane giving small differences in solute partition coefficients in the two systems. The 24% higher limonene density is a difference with heptane that has major consequences in CCC. The polar and apolar phases of the limonene/methanol/water 10/9/1 v/v have -0.025 g/cm(3) density difference (lower limonene phase) compared to +0.132 g/cm(3) with heptane (upper heptane phase). This precludes the use of this limonene system with hydrodynamic CCC columns that need significant density difference to retain a liquid stationary phase. It is an advantage with hydrostatic CCC columns because density difference is related to the working pressure drop: limonene allows one to work with high centrifugal fields and moderate pressure drop. Limonene has the capability to be a "green" alternative to petroleum-based solvents in CCC applications.

Qualitative Characterization of the Aqueous Fraction from Hydrothermal Liquefaction of Algae Using 2D Gas Chromatography with Time-of-flight Mass Spectrometry

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

Maddi, Balakrishna; Panisko, Ellen; Albrecht, Karl

Two-dimensional gas chromatography coupled with time of flight mass spectrometry is a powerful tool for identifying and quantifying components in complex mixtures. It has been used to analyze gasoline, jet fuel, diesel, bio-diesel and organic fraction of bio-crude/bio-oil. In these experiments, the first dimension of separation was non-polar, followed by a polar separation. Aqueous fractions of bio-crude and other aqueous samples have been examined with similar column combinations. However, sample preparation techniques such as derivatization, solvent extraction, and solid-phase extraction were necessary prior to analysis. In this study, aqueous fraction obtained from hydrothermal liquefaction of algae was characterized by two-dimensionalmore » gas chromatography coupled with time of flight mass spectrometry without prior sample preparation techniques using a polar separation in the first dimension followed by a non-polar separation. Two-dimensional plots from this analysis were compared with those obtained from the more traditional column combination. Results from qualitative characterization aqueous fractions of algal bio-crude are discussed in detail. The advantages of using a polar separation followed by a non-polar separation for characterization of organics in aqueous samples by two-dimensional gas chromatography coupled with time of flight mass spectrometry are highlighted.« less

Two-phase anaerobic digestion of vegetable market waste fraction of municipal solid waste and development of improved technology for phase separation in two-phase reactor.

PubMed

Majhi, Bijoy Kumar; Jash, Tushar

2016-12-01

Biogas production from vegetable market waste (VMW) fraction of municipal solid waste (MSW) by two-phase anaerobic digestion system should be preferred over the single-stage reactors. This is because VMW undergoes rapid acidification leading to accumulation of volatile fatty acids and consequent low pH resulting in frequent failure of digesters. The weakest part in the two-phase anaerobic reactors was the techniques applied for solid-liquid phase separation of digestate in the first reactor where solubilization, hydrolysis and acidogenesis of solid organic waste occur. In this study, a two-phase reactor which consisted of a solid-phase reactor and a methane reactor was designed, built and operated with VMW fraction of Indian MSW. A robust type filter, which is unique in its implementation method, was developed and incorporated in the solid-phase reactor to separate the process liquid produced in the first reactor. Experiments were carried out to assess the long term performance of the two-phase reactor with respect to biogas production, volatile solids reduction, pH and number of occurrence of clogging in the filtering system or choking in the process liquid transfer line. The system performed well and was operated successfully without the occurrence of clogging or any other disruptions throughout. Biogas production of 0.86-0.889m 3 kg -1 VS, at OLR of 1.11-1.585kgm -3 d -1 , were obtained from vegetable market waste, which were higher than the results reported for similar substrates digested in two-phase reactors. The VS reduction was 82-86%. The two-phase anaerobic digestion system was demonstrated to be stable and suitable for the treatment of VMW fraction of MSW for energy generation. Copyright © 2016 Elsevier Ltd. All rights reserved.

On the use of ionic liquids as mobile phase additives in high-performance liquid chromatography. A review.

PubMed

García-Alvarez-Coque, M C; Ruiz-Angel, M J; Berthod, A; Carda-Broch, S

2015-07-09

The popularity of ionic liquids (ILs) has grown during the last decades in several analytical separation techniques. Consequently, the number of reports devoted to the applications of ILs is still increasing. This review is focused on the use of ILs (mainly imidazolium-based associated to chloride and tetrafluoroborate) as mobile phase additives in high-performance liquid chromatography (HPLC). In this approach, ILs just function as salts, but keep several kinds of intermolecular interactions, which are useful for chromatographic separations. Both cation and anion can be adsorbed on the stationary phase, creating a bilayer. This gives rise to hydrophobic, electrostatic and other specific interactions with the stationary phase and solutes, which modify the retention behaviour and peak shape. This review updates the advances in this field, with emphasis on topics not always deeply considered in the literature, such as the mechanisms of retention, the estimation of the suppressing potency of silanols, modelling and optimisation of the chromatographic performance, and the comparison with other additives traditionally used to avoid the silanol problem. Copyright © 2015 Elsevier B.V. All rights reserved.

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

PubMed Central

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

2018-01-01

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

In situ reinforced polymers using low molecular weight compounds

NASA Astrophysics Data System (ADS)

Yordem, Onur Sinan

2011-12-01

The primary objective of this research is to generate reinforcing domains in situ during the processing of polymers by using phase separation techniques. Low molecular weight compounds were mixed with polymers where the process viscosity is reduced at process temperatures and mechanical properties are improved once the material system is cooled or reacted. Thermally induced phase separation and thermotropic phase transformation of low molar mass compounds were used in isotactic polypropylene (iPP) and poly(ether ether ketone) (PEEK) resins. Reaction induced phase separation was utilized in thermosets to generate anisotropic reinforcements. A new strategy to increase fracture toughness of materials was introduced. Simultaneously, enhancement in stiffness and reduction in process viscosity were also attained. Materials with improved rheological and mechanical properties were prepared by using thermotropic phase transformations of metal soaps in polymers (calcium stearate/iPP). Morphology and thermal properties were studied using WAXS, DSC and SEM. Mechanical and rheological investigation showed significant reduction in process viscosity and substantial improvement in fracture toughness were attained. Effects of molecular architecture of metal soaps were investigated in PEEK (calcium stearate/PEEK and sodium stearate/PEEK). The selected compounds reduced the process viscosity due to the high temperature co-continuous morphology of metal soaps. Unlike the iPP system that incorporates spherical particles, interaction between PEEK and metal soaps resulted in two discrete and co-continuous phases of PEEK and the metal stearates. DMA and melt rheology exhibited that sodium stearate/PEEK composites are stiffer. Effective moduli of secondary metal stearate phase were calculated using different composite theories, which suggested bicontinuous morphology to the metal soaps in PEEK. Use of low molecular weight crystallizable solvents was investigated in reactive systems. Formation of anisotropic reinforcements was evaluated using dimethyl sulfone (DMS) as the crystallizable diluent and diglycidyl ether of bisphenol-A (DGEBA)/m-phenylene diamine (mPDA) material system as the epoxy thermoset. Miscible blends of DMS and DGEBA/mPDA form homogenous mixtures that undergo polymerization induced phase separation, once the DGEBA oligomers react with mPDA. The effect of the competition between the crystallization and phase separation of DMS resulted in nano-wires to micro-scale fiber-like crystals that were generated by adjusting the reaction temperature and DMS concentration.

Selective filling for patterning in microfluidic channels and integration of chromatography in "lab-on-a-chip" devices using sol-gel technology

NASA Astrophysics Data System (ADS)

Jindal, Rohit

The last decade has seen tremendous advancement in the development of miniaturized chemical analysis system also known as "lab-on-a-chip". It is believed that the true potential of these devices will be achieved by integrating various functions such as separation, reaction, sensing, mixing, pumping, injection and detection onto a single chip. The ability to pattern different functionalities is indispensable for the development of highly integrated devices. In this work, a simple method based on the concept of selective filling is described for patterning in the microfluidic channels. It is based on the difference in the free energy of filling between an open and a covered part of the channel. This method was used for the integration of chromatography in the microfluidic devices. A chromatographic column was realized by utilizing sol-gel as an immobilization matrix for entrapping reversed phase chromatographic particles. Localization of the stationary phase was achieved using the selective filling technique. Channels were fabricated in quartz using photolithography and wet etching. Electroosmotic flow was used for manipulating fluid movement in the channels. Cross channel design was used for making a pulse injection of the solutes in the separation channel. An optical fiber setup was developed for carrying out on-chip UV absorbance detection. Stationary phase was created under different sol-gel synthesis conditions. It was established that the sol-gel synthesis carried out under acidic conditions provides the optimum synthesis conditions for creating separation column. Chromatographic performance of the stationary phase material was demonstrated by separating peptides present in a mixture. The sol-gel immobilization method was extended for the integration of micropump in the chip. The micropump enables pumping of the fluid in field free channels. Preliminary results, demonstrating the potential of carbon nanotubes as a support material in the microfluidic channels, were obtained using CVD (chemical vapor deposition) grown tubes in the channel. Results obtained in this work demonstrate the potential of selective filling technique along with sol-gel technology as a useful tool for the fabrication of multifunctional "lab-on-a-chip" devices.

Single-molecule dilution and multiple displacement amplification for molecular haplotyping.

PubMed

Paul, Philip; Apgar, Josh

2005-04-01

Separate haploid analysis is frequently required for heterozygous genotyping to resolve phase ambiguity or confirm allelic sequence. We demonstrate a technique of single-molecule dilution followed by multiple strand displacement amplification to haplotype polymorphic alleles. Dilution of DNA to haploid equivalency, or a single molecule, is a simple method for separating di-allelic DNA. Strand displacement amplification is a robust method for non-specific DNA expansion that employs random hexamers and phage polymerase Phi29 for double-stranded DNA displacement and primer extension, resulting in high processivity and exceptional product length. Single-molecule dilution was followed by strand displacement amplification to expand separated alleles to microgram quantities of DNA for more efficient haplotype analysis of heterozygous genes.

Facet-controlled phase separation in supersaturated Au-Ni nanoparticles upon shape equilibration

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

Herz, A., E-mail: andreas.herz@tu-ilmenau.de, E-mail: dong.wang@tu-ilmenau.de; Rossberg, D.; Hentschel, M.

2015-08-17

Solid-state dewetting is used to fabricate supersaturated, submicron-sized Au-Ni solid solution particles out of thin Au/Ni bilayers by means of a rapid thermal annealing technique. Phase separation in such particles is studied with respect to their equilibrium crystal (or Wulff) shape by subsequent annealing at elevated temperature. It is found that (100) faceting planes of the equilibrated particles are enriched with Ni and (111) faces with Au. Both phases are considered by quantum-mechanical calculations in combination with an error-reduction scheme that was developed to compensate for a missing exchange-correlation potential that would reliably describe both Au and Ni. The observedmore » phase configuration is then related to the minimization of strongly anisotropic elastic energies of Au- and Ni-rich phases and results in a rather unique nanoparticle composite state that is characterized by nearly uniform value of elastic response to epitaxial strains all over the faceted surface. The same conclusion is yielded also by evaluating bi-axial elastic moduli when employing interpolated experimental elastic constants. This work demonstrates a useful route for studying features of physical metallurgy at the mesoscale.« less

Combined operando X-ray diffraction–electrochemical impedance spectroscopy detecting solid solution reactions of LiFePO4 in batteries

PubMed Central

Hess, Michael; Sasaki, Tsuyoshi; Villevieille, Claire; Novák, Petr

2015-01-01

Lithium-ion batteries are widely used for portable applications today; however, often suffer from limited recharge rates. One reason for such limitation can be a reduced active surface area during phase separation. Here we report a technique combining high-resolution operando synchrotron X-ray diffraction coupled with electrochemical impedance spectroscopy to directly track non-equilibrium intermediate phases in lithium-ion battery materials. LiFePO4, for example, is known to undergo phase separation when cycled under low-current-density conditions. However, operando X-ray diffraction under ultra-high-rate alternating current and direct current excitation reveal a continuous but current-dependent, solid solution reaction between LiFePO4 and FePO4 which is consistent with previous experiments and calculations. In addition, the formation of a preferred phase with a composition similar to the eutectoid composition, Li0.625FePO4, is evident. Even at a low rate of 0.1C, ∼20% of the X-ray diffractogram can be attributed to non-equilibrium phases, which changes our understanding of the intercalation dynamics in LiFePO4. PMID:26345306

Combined operando X-ray diffraction-electrochemical impedance spectroscopy detecting solid solution reactions of LiFePO4 in batteries.

PubMed

Hess, Michael; Sasaki, Tsuyoshi; Villevieille, Claire; Novák, Petr

2015-09-08

Lithium-ion batteries are widely used for portable applications today; however, often suffer from limited recharge rates. One reason for such limitation can be a reduced active surface area during phase separation. Here we report a technique combining high-resolution operando synchrotron X-ray diffraction coupled with electrochemical impedance spectroscopy to directly track non-equilibrium intermediate phases in lithium-ion battery materials. LiFePO4, for example, is known to undergo phase separation when cycled under low-current-density conditions. However, operando X-ray diffraction under ultra-high-rate alternating current and direct current excitation reveal a continuous but current-dependent, solid solution reaction between LiFePO4 and FePO4 which is consistent with previous experiments and calculations. In addition, the formation of a preferred phase with a composition similar to the eutectoid composition, Li0.625FePO4, is evident. Even at a low rate of 0.1C, ∼20% of the X-ray diffractogram can be attributed to non-equilibrium phases, which changes our understanding of the intercalation dynamics in LiFePO4.

A technique for generating phase-space-based Monte Carlo beamlets in radiotherapy applications.

PubMed

Bush, K; Popescu, I A; Zavgorodni, S

2008-09-21

As radiotherapy treatment planning moves toward Monte Carlo (MC) based dose calculation methods, the MC beamlet is becoming an increasingly common optimization entity. At present, methods used to produce MC beamlets have utilized a particle source model (PSM) approach. In this work we outline the implementation of a phase-space-based approach to MC beamlet generation that is expected to provide greater accuracy in beamlet dose distributions. In this approach a standard BEAMnrc phase space is sorted and divided into beamlets with particles labeled using the inheritable particle history variable. This is achieved with the use of an efficient sorting algorithm, capable of sorting a phase space of any size into the required number of beamlets in only two passes. Sorting a phase space of five million particles can be achieved in less than 8 s on a single-core 2.2 GHz CPU. The beamlets can then be transported separately into a patient CT dataset, producing separate dose distributions (doselets). Methods for doselet normalization and conversion of dose to absolute units of Gy for use in intensity modulated radiation therapy (IMRT) plan optimization are also described.

Element fracture technique for hypervelocity impact simulation

NASA Astrophysics Data System (ADS)

Zhang, Xiao-tian; Li, Xiao-gang; Liu, Tao; Jia, Guang-hui

2015-05-01

Hypervelocity impact dynamics is the theoretical support of spacecraft shielding against space debris. The numerical simulation has become an important approach for obtaining the ballistic limits of the spacecraft shields. Currently, the most widely used algorithm for hypervelocity impact is the smoothed particle hydrodynamics (SPH). Although the finite element method (FEM) is widely used in fracture mechanics and low-velocity impacts, the standard FEM can hardly simulate the debris cloud generated by hypervelocity impact. This paper presents a successful application of the node-separation technique for hypervelocity impact debris cloud simulation. The node-separation technique assigns individual/coincident nodes for the adjacent elements, and it applies constraints to the coincident node sets in the modeling step. In the explicit iteration, the cracks are generated by releasing the constrained node sets that meet the fracture criterion. Additionally, the distorted elements are identified from two aspects - self-piercing and phase change - and are deleted so that the constitutive computation can continue. FEM with the node-separation technique is used for thin-wall hypervelocity impact simulations. The internal structures of the debris cloud in the simulation output are compared with that in the test X-ray graphs under different material fracture criteria. It shows that the pressure criterion is more appropriate for hypervelocity impact. The internal structures of the debris cloud are also simulated and compared under different thickness-to-diameter ratios (t/D). The simulation outputs show the same spall pattern with the tests. Finally, the triple-plate impact case is simulated with node-separation FEM.

High-aspect-ratio, silicon oxide-enclosed pillar structures in microfluidic liquid chromatography.

PubMed

Taylor, Lisa C; Lavrik, Nickolay V; Sepaniak, Michael J

2010-11-15

The present paper discusses the ability to separate chemical species using high-aspect-ratio, silicon oxide-enclosed pillar arrays. These miniaturized chromatographic systems require smaller sample volumes, experience less flow resistance, and generate superior separation efficiency over traditional packed bed liquid chromatographic columns, improvements controlled by the increased order and decreased pore size of the systems. In our distinctive fabrication sequence, plasma-enhanced chemical vapor deposition (PECVD) of silicon oxide is used to alter the surface and structural properties of the pillars for facile surface modification while improving the pillar mechanical stability and increasing surface area. The separation behavior of model compounds within our pillar systems indicated an unexpected hydrophobic-like separation mechanism. The effects of organic modifier, ionic concentration, and pressure-driven flow rate were studied. A decrease in the organic content of the mobile phase increased peak resolution while detrimentally effecting peak shape. A resolution of 4.7 (RSD = 3.7%) was obtained for nearly perfect Gaussian shaped peaks, exhibiting plate heights as low as 1.1 and 1.8 μm for fluorescein and sulforhodamine B, respectively. Contact angle measurements and DART mass spectrometry analysis indicate that our employed elastomeric soft bonding technique modifies pillar properties, creating a fortuitous stationary phase. This discovery provides evidence supporting the ability to easily functionalize PECVD oxide surfaces by gas-phase reactions.

An Eulerian time filtering technique to study large-scale transient flow phenomena

NASA Astrophysics Data System (ADS)

Vanierschot, Maarten; Persoons, Tim; van den Bulck, Eric

2009-10-01

Unsteady fluctuating velocity fields can contain large-scale periodic motions with frequencies well separated from those of turbulence. Examples are the wake behind a cylinder or the processing vortex core in a swirling jet. These turbulent flow fields contain large-scale, low-frequency oscillations, which are obscured by turbulence, making it impossible to identify them. In this paper, we present an Eulerian time filtering (ETF) technique to extract the large-scale motions from unsteady statistical non-stationary velocity fields or flow fields with multiple phenomena that have sufficiently separated spectral content. The ETF method is based on non-causal time filtering of the velocity records in each point of the flow field. It is shown that the ETF technique gives good results, similar to the ones obtained by the phase-averaging method. In this paper, not only the influence of the temporal filter is checked, but also parameters such as the cut-off frequency and sampling frequency of the data are investigated. The technique is validated on a selected set of time-resolved stereoscopic particle image velocimetry measurements such as the initial region of an annular jet and the transition between flow patterns in an annular jet. The major advantage of the ETF method in the extraction of large scales is that it is computationally less expensive and it requires less measurement time compared to other extraction methods. Therefore, the technique is suitable in the startup phase of an experiment or in a measurement campaign where several experiments are needed such as parametric studies.

Separation and Detection of Toxic Gases with a Silicon Micromachined Gas Chromatography System

NASA Technical Reports Server (NTRS)

Kolesar, Edward S.; Reston, Rocky R.

1995-01-01

A miniature gas chromatography (GC) system was designed and fabricated using silicon micromachining and integrated circuit (IC) processing techniques. The silicon micromachined gas chromatography system (SMGCS) is composed of a miniature sample injector that incorporates a 10 microliter sample loop; a 0.9 meter long, rectangular shaped (300 micrometer width and 10 micrometer height) capillary column coated with a 0.2 micrometer thick copper phthalocyanine (CuPc) stationary phase; and a dual detector scheme based upon a CuPc-coated chemiresistor and a commercially available 125 micrometer diameter thermal conductivity detector (TCD) bead. Silicon micromachining was employed to fabricate the interface between the sample injector and the GC column, the column itself, and the dual detector cavity. A novel IC thin-film processing technique was developed to sublime the CuPc stationary phase coating on the column walls that were micromachined in the host silicon wafer substrate and Pyrex (r) cover plate, which were then electrostatically bonded together. The SMGCS can separate binary gas mixtures composed of parts-per-million (ppm) concentrations of ammonia (NH3) and nitrogen dioxide (NO2) when isothermally operated (55-80 degrees C). With a helium carrier gas and nitrogen diluent, a 10 microliter sample volume containing ammonia and nitrogen dioxide injected at 40 psi ((2.8 x 10(exp 5)Pa)) can be separated in less than 30 minutes.

Fabrication of mesoporous polymer monolith: a template-free approach.

PubMed

Okada, Keisuke; Nandi, Mahasweta; Maruyama, Jun; Oka, Tatsuya; Tsujimoto, Takashi; Kondoh, Katsuyoshi; Uyama, Hiroshi

2011-07-14

Mesoporous polyacrylonitrile (PAN) monolith has been fabricated by a template-free approach using the unique affinity of PAN towards a water/dimethyl sulfoxide (DMSO) mixture. A newly developed Thermally Induced Phase Separation Technique (TIPS) has been used to obtain the polymer monoliths and their microstructures have been controlled by optimizing the concentration and cooling temperature.

Ultrafast Dynamics in Vanadium Dioxide: Separating Spatially Segregated Mixed Phase Dynamics in the Time-domain

NASA Astrophysics Data System (ADS)

Hilton, David

2011-10-01

In correlated electronic systems, observed electronic and structural behavior results from the complex interplay between multiple, sometimes competing degrees-of- freedom. One such material used to study insulator-to-metal transitions is vanadium dioxide, which undergoes a phase transition from a monoclinic-insulating phase to a rutile-metallic phase when the sample is heated to 340 K. The major open question with this material is the relative influence of this structural phase transition (Peirels transition) and the effects of electronic correlations (Mott transition) on the observed insulator-to-metal transition. Answers to these major questions are complicated by vanadium dioxide's sensitivity to perturbations in the chemical structure in VO2. For example, related VxOy oxides with nearly a 2:1 ratio do not demonstrate the insulator-to- metal transition, while recent work has demonstrated that W:VO2 has demonstrated a tunable transition temperature controllable with tungsten doping. All of these preexisting results suggest that the observed electronic properties are exquisitely sensitive to the sample disorder. Using ultrafast spectroscopic techniques, it is now possible to impulsively excite this transition and investigate the photoinduced counterpart to this thermal phase transition in a strongly nonequilibrium regime. I will discuss our recent results studying the terahertz-frequency conductivity dynamics of this photoinduced phase transition in the poorly understood near threshold temperature range. We find a dramatic softening of the transition near the critical temperature, which results primarily from the mixed phase coexistence near the transition temperature. To directly study this mixed phase behavior, we directly study the nucleation and growth rates of the metallic phase in the parent insulator using non-degenerate optical pump-probe spectroscopy. These experiments measure, in the time- domain, the coexistent phase separation in VO2 (spatially separated insulator and metal islands) and, more importantly, their dynamic evolution in response to optical excitation.

Investigating hygroscopic behavior and phase separation of organic/inorganic mixed phase aerosol particles with FTIR spectroscopy

NASA Astrophysics Data System (ADS)

Zawadowicz, M. A.; Cziczo, D. J.

2013-12-01

Atmospheric aerosol particles can be composed of inorganic salts, such as ammonium sulfate and sodium chloride, and therefore exhibit hygroscopic properties. Many inorganic salts have very well-defined deliquescence and efflorescence points at which they take up and lose water, respectively. For example, the deliquescence relative humidity of pure ammonium sulfate is about 80% and its efflorescence point is about 35%. This behavior of ammonium sulfate is important to atmospheric chemistry because some reactions, such as the hydrolysis of nitrogen pentoxide, occur on aqueous but not crystalline surfaces. Deliquescence and efflorescence of simple inorganic salt particles have been investigated by a variety of methods, such as IR spectroscopy, tandem mobility analysis and electrodynamic balance. Field measurements have shown that atmospheric aerosol are not typically a single inorganic salt, instead they often contain organic as well as inorganic species. Mixed inorganic/organic aerosol particles, while abundant in the atmosphere, have not been studied as extensively. Many recent studies have focused on microscopy techniques that require deposition of the aerosol on a glass slide, possibly changing its surface properties. This project investigates the deliquescence and efflorescence points, phase separation and ability to exchange gas-phase components of mixed organic and inorganic aerosol using a flow tube coupled with FTIR spectroscopy. Ammonium sulfate aerosol mixed with organic polyols with different O:C ratios, including glycerol, 1,2,6-hexanetriol, 1,4-butanediol and 1,5-pentanediol have been investigated. This project aims to study gas-phase exchange in these aerosol systems to determine if exchange is impacted when phase separation occurs.

Development and evaluation of a gas chromatographic method for the determination of triazine herbicides in natural water samples

USGS Publications Warehouse

Steinheimer, T.R.; Brooks, M.G.

1984-01-01

A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0.1 ??g/L in a 1-litre sample. Three different natural water samples were used for error analysis via evaluation of recovery efficiencies and estimation of overall method precision. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0. 1 mu g/L in a 1-litre sample. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.

Glass-liquid phase separation in highly supersaturated aqueous solutions of telaprevir.

PubMed

Mosquera-Giraldo, Laura I; Taylor, Lynne S

2015-02-02

Amorphous solid dispersions are of great current interest because they can improve the delivery of poorly water-soluble compounds. It has been recently noted that the highly supersaturated solutions generated by dissolution of some ASDs can undergo a phase transition to a colloidal, disordered, drug-rich phase when the concentration exceeds the "amorphous solubility" of the drug. The purpose of this study was to investigate the phase behavior of supersaturated solutions of telaprevir, which is formulated as an amorphous solid dispersion in the commercial product. Different analytical techniques including proton nuclear magnetic resonance spectroscopy (NMR), ultraviolet spectroscopy (UV), fluorescence spectroscopy and flux measurements were used to evaluate the properties of aqueous supersaturated solutions of telaprevir. It was found that highly supersaturated solutions of telaprevir underwent glass-liquid phase separation (GLPS) when the concentration exceeded 90 μg/mL, forming a water-saturated colloidal, amorphous drug-rich phase with a glass transition temperature of 52 °C. From flux measurements, it was observed that the "free" drug concentration reached a maximum at the concentration where GLPS occurred, and did not increase further as the concentration was increased. This phase behavior, which results in a precipitate and a metastable equilibrium between a supersaturated solution and a drug-rich phase, is obviously important in the context of evaluating amorphous solid dispersion formulations and their crystallization routes.

Surface-bubble-modulated liquid chromatography: a new approach for manipulation of chromatographic retention and investigation of solute distribution at water/hydrophobic interfaces.

PubMed

Nakamura, Keisuke; Nakamura, Hiroki; Saito, Shingo; Shibukawa, Masami

2015-01-20

In this paper, we present a new chromatographic method termed surface-bubble-modulated liquid chromatography (SBMLC), that has a hybrid separation medium incorporated with surface nanobubbles. Nanobubbles or nanoscale gas phases can be fixed at the interface between water and a hydrophobic material by delivering water into a dry column packed with a nanoporous material. The incorporation of a gas phase at the hydrophobic surface leads to the formation of the hybrid separation system consisting of the gas phase, hydrophobic moieties, and the water/hydrophobic interface or the interfacial water. One can change the volume of the gas phase by pressure applied to the column, which in turn alters the area of water/hydrophobic interface or the volume of the interfacial water, while the amount of the hydrophobic moiety remains constant. Therefore, this strategy provides a novel technique not only for manipulating the separation selectivity by pressure but also for elucidating the mechanism of accumulation or retention of solute compounds in aqueous solutions by a hydrophobic material. We evaluate the contributions of the interfacial water at the surface of an octadecyl bonded silica and the bonded layer itself to the retention of various solute compounds in aqueous solutions on the column packed with the material by SBMLC. The results show that the interfacial water formed at the hydrophobic surface has a key role in retention even though its volume is rather small. The manipulation of the separation selectivity of SBMLC for some organic compounds by pressure is demonstrated.

Separation of betacyanins from purple flowers of Gomphrena globosa L. by ion-pair high-speed counter-current chromatography.

PubMed

Spórna-Kucab, Aneta; Jagodzińska, Joanna; Wybraniec, Sławomir

2017-03-17

Betacyanins, known as antioxidants and chemopreventive natural compounds with colourful properties, were extracted from purple flowers of Gomphrena globosa L. belonging to the Amaranthaceae family and separated for the first time by ion-pair high-speed counter-current chromatography (HSCCC). The pigments were detected by LC-DAD-ESI-MS/MS technique. Separation of betacyanins (300mg) by HSCCC was accomplished in four solvent systems: tert-butyl methyl ether - butanol - acetonitrile - water (0.7% and 1.0% HFBA - heptafluorobutyric acid - system I and III) and tert-butyl methyl ether - butanol - methanol - water (0.7% and 1.0% HFBA - system II and IV) (2:2:1:5, v/v/v/v) in the head-to-tail mode. The mobile phase (aqueous phase) was run at 2.0ml/min and the column rotation speed was 860rpm. The applied systems enabled to study the influence of HFBA concentration as well as systems polarity on betacyanins separation. Comparison of the systems containing 0.7% HFBA (systems I-II) demonstrates that the replacement of acetonitrile by methanol increases the resolution (R s ) between all betacyanins and does not influence the retention of the stationary phase (S f =76%). Higher concentration of the acid in systems III-IV slightly decreases S f to 71% in the systems with 1.0% HFBA. Comparison of the resolution values for betacyanins in the systems with 0.7% and 1.0% HFBA demonstrates that higher concentration of the acid improves the separation effectiveness for all betacyanins as a result of increasing of the chemical affinity of the pigments to the organic stationary phase in HSCCC. The systems III-IV with 1% HFBA are the most effective for the separation of all the studied betacyanins. Copyright © 2017 Elsevier B.V. All rights reserved.

On-Chip Microfluidic Components for In Situ Analysis, Separation, and Detection of Amino Acids

NASA Technical Reports Server (NTRS)

Zheng, Yun; Getty, Stephanie; Dworkin, Jason; Balvin, Manuel; Kotecki, Carl

2013-01-01

The Astrobiology Analytical Laboratory at GSFC has identified amino acids in meteorites and returned cometary samples by using liquid chromatography-electrospray ionization time-of-flight mass spectrometry (LCMS). These organic species are key markers for life, having the property of chirality that can be used to distinguish biological from non-biological amino acids. One of the critical components in the benchtop instrument is liquid chromatography (LC) analytical column. The commercial LC analytical column is an over- 250-mm-long and 4.6-mm-diameter stainless steel tube filled with functionized microbeads as stationary phase to separate the molecular species based on their chemistry. Miniaturization of this technique for spaceflight is compelling for future payloads for landed missions targeting astrobiology objectives. A commercial liquid chromatography analytical column consists of an inert cylindrical tube filled with a stationary phase, i.e., microbeads, that has been functionalized with a targeted chemistry. When analyte is sent through the column by a pressurized carrier fluid (typically a methanol/ water mixture), compounds are separated in time due to differences in chemical interactions with the stationary phase. Different species of analyte molecules will interact more strongly with the column chemistry, and will therefore take longer to traverse the column. In this way, the column will separate molecular species based on their chemistry. A lab-on-chip liquid analysis tool was developed. The microfluidic analytical column is capable of chromatographically separating biologically relevant classes of molecules based on their chemistry. For this analytical column, fabrication, low leak rate, and stationary phase incorporation of a serpentine microchannel were demonstrated that mimic the dimensions of a commercial LC column within a 5 10 1 mm chip. The microchannel in the chip has a 75- micrometer-diameter oval-shaped cross section. The serpentine microchannel has four different lengths: 40, 60, 80, and 100 mm. Functionized microbeads were filled inside the microchannel to separate molecular species based on their chemistry.

Ionic liquids in chromatographic and electrophoretic techniques: toward additional improvements in the separation of natural compounds

PubMed Central

Freire, Carmen S. R.; Coutinho, João A. P.; Silvestre, Armando J. D.; Freire, Mara G.

2016-01-01

Due to their unique properties, in recent years, ionic liquids (ILs) have been largely investigated in the field of analytical chemistry. Particularly during the last sixteen years, they have been successfully applied in the chromatographic and electrophoretic analysis of value-added compounds extracted from biomass. Considering the growing interest in the use of ILs in this field, this critical review provides a comprehensive overview on the improvements achieved using ILs as constituents of mobile or stationary phases in analytical techniques, namely in capillary electrophoresis and its different modes, in high performance liquid chromatography, and in gas chromatography, for the separation and analysis of natural compounds. The impact of the IL chemical structure and the influence of secondary parameters, such as the IL concentration, temperature, pH, voltage and analysis time (when applied), are also critically addressed regarding the achieved separation improvements. Major conclusions on the role of ILs in the separation mechanisms and the performance of these techniques in terms of efficiency, resolution and selectivity are provided. Based on a critical analysis of all published results, some target-oriented ILs are suggested. Finally, current drawbacks and future challenges in the field are highlighted. In particular, the design and use of more benign and effective ILs as well as the development of integrated (and thus more sustainable) extraction–separation processes using IL aqueous solutions are suggested within a green chemistry perspective. PMID:27667965

Effect of the Hartmann number on phase separation controlled by magnetic field for binary mixture system with large component ratio

NASA Astrophysics Data System (ADS)

Heping, Wang; Xiaoguang, Li; Duyang, Zang; Rui, Hu; Xingguo, Geng

2017-11-01

This paper presents an exploration for phase separation in a magnetic field using a coupled lattice Boltzmann method (LBM) with magnetohydrodynamics (MHD). The left vertical wall was kept at a constant magnetic field. Simulations were conducted by the strong magnetic field to enhance phase separation and increase the size of separated phases. The focus was on the effect of magnetic intensity by defining the Hartmann number (Ha) on the phase separation properties. The numerical investigation was carried out for different governing parameters, namely Ha and the component ratio of the mixed liquid. The effective morphological evolutions of phase separation in different magnetic fields were demonstrated. The patterns showed that the slant elliptical phases were created by increasing Ha, due to the formation and increase of magnetic torque and force. The dataset was rearranged for growth kinetics of magnetic phase separation in a plot by spherically averaged structure factor and the ratio of separated phases and total system. The results indicate that the increase in Ha can increase the average size of separated phases and accelerate the spinodal decomposition and domain growth stages. Specially for the larger component ratio of mixed phases, the separation degree was also significantly improved by increasing magnetic intensity. These numerical results provide guidance for setting the optimum condition for the phase separation induced by magnetic field.

Design Techniques for Uniform-DFT, Linear Phase Filter Banks

NASA Technical Reports Server (NTRS)

Sun, Honglin; DeLeon, Phillip

1999-01-01

Uniform-DFT filter banks are an important class of filter banks and their theory is well known. One notable characteristic is their very efficient implementation when using polyphase filters and the FFT. Separately, linear phase filter banks, i.e. filter banks in which the analysis filters have a linear phase are also an important class of filter banks and desired in many applications. Unfortunately, it has been proved that one cannot design critically-sampled, uniform-DFT, linear phase filter banks and achieve perfect reconstruction. In this paper, we present a least-squares solution to this problem and in addition prove that oversampled, uniform-DFT, linear phase filter banks (which are also useful in many applications) can be constructed for perfect reconstruction. Design examples are included illustrate the methods.

Generic Health Management: A System Engineering Process Handbook Overview and Process

NASA Technical Reports Server (NTRS)

Wilson, Moses Lee; Spruill, Jim; Hong, Yin Paw

1995-01-01

Health Management, a System Engineering Process, is one of those processes-techniques-and-technologies used to define, design, analyze, build, verify, and operate a system from the viewpoint of preventing, or minimizing, the effects of failure or degradation. It supports all ground and flight elements during manufacturing, refurbishment, integration, and operation through combined use of hardware, software, and personnel. This document will integrate Health Management Processes (six phases) into five phases in such a manner that it is never a stand alone task/effort which separately defines independent work functions.

Phased array ghost elimination.

PubMed

Kellman, Peter; McVeigh, Elliot R

2006-05-01

Parallel imaging may be applied to cancel ghosts caused by a variety of distortion mechanisms, including distortions such as off-resonance or local flow, which are space variant. Phased array combining coefficients may be calculated that null ghost artifacts at known locations based on a constrained optimization, which optimizes SNR subject to the nulling constraint. The resultant phased array ghost elimination (PAGE) technique is similar to the method known as sensitivity encoding (SENSE) used for accelerated imaging; however, in this formulation is applied to full field-of-view (FOV) images. The phased array method for ghost elimination may result in greater flexibility in designing acquisition strategies. For example, in multi-shot EPI applications ghosts are typically mitigated by the use of an interleaved phase encode acquisition order. An alternative strategy is to use a sequential, non-interleaved phase encode order and cancel the resultant ghosts using PAGE parallel imaging. Cancellation of ghosts by means of phased array processing makes sequential, non-interleaved phase encode acquisition order practical, and permits a reduction in repetition time, TR, by eliminating the need for echo-shifting. Sequential, non-interleaved phase encode order has benefits of reduced distortion due to off-resonance, in-plane flow and EPI delay misalignment. Furthermore, the use of EPI with PAGE has inherent fat-water separation and has been used to provide off-resonance correction using a technique referred to as lipid elimination with an echo-shifting N/2-ghost acquisition (LEENA), and may further generalized using the multi-point Dixon method. Other applications of PAGE include cancelling ghosts which arise due to amplitude or phase variation during the approach to steady state. Parallel imaging requires estimates of the complex coil sensitivities. In vivo estimates may be derived by temporally varying the phase encode ordering to obtain a full k-space dataset in a scheme similar to the autocalibrating TSENSE method. This scheme is a generalization of the UNFOLD method used for removing aliasing in undersampled acquisitions. The more general scheme may be used to modulate each EPI ghost image to a separate temporal frequency as described in this paper. Copyright (c) 2006 John Wiley & Sons, Ltd.

Phased array ghost elimination

PubMed Central

Kellman, Peter; McVeigh, Elliot R.

2007-01-01

Parallel imaging may be applied to cancel ghosts caused by a variety of distortion mechanisms, including distortions such as off-resonance or local flow, which are space variant. Phased array combining coefficients may be calculated that null ghost artifacts at known locations based on a constrained optimization, which optimizes SNR subject to the nulling constraint. The resultant phased array ghost elimination (PAGE) technique is similar to the method known as sensitivity encoding (SENSE) used for accelerated imaging; however, in this formulation is applied to full field-of-view (FOV) images. The phased array method for ghost elimination may result in greater flexibility in designing acquisition strategies. For example, in multi-shot EPI applications ghosts are typically mitigated by the use of an interleaved phase encode acquisition order. An alternative strategy is to use a sequential, non-interleaved phase encode order and cancel the resultant ghosts using PAGE parallel imaging. Cancellation of ghosts by means of phased array processing makes sequential, non-interleaved phase encode acquisition order practical, and permits a reduction in repetition time, TR, by eliminating the need for echo-shifting. Sequential, non-interleaved phase encode order has benefits of reduced distortion due to off-resonance, in-plane flow and EPI delay misalignment. Furthermore, the use of EPI with PAGE has inherent fat-water separation and has been used to provide off-resonance correction using a technique referred to as lipid elimination with an echo-shifting N/2-ghost acquisition (LEENA), and may further generalized using the multi-point Dixon method. Other applications of PAGE include cancelling ghosts which arise due to amplitude or phase variation during the approach to steady state. Parallel imaging requires estimates of the complex coil sensitivities. In vivo estimates may be derived by temporally varying the phase encode ordering to obtain a full k-space dataset in a scheme similar to the autocalibrating TSENSE method. This scheme is a generalization of the UNFOLD method used for removing aliasing in undersampled acquisitions. The more general scheme may be used to modulate each EPI ghost image to a separate temporal frequency as described in this paper. PMID:16705636

Nanoscale Phase-Separated Structure in Core-Shell Nanoparticles of SiO2-Si1-xGexO2 Glass Revealed by Electron Microscopy.

PubMed

Kubo, Yugo; Yonezawa, Kazuhiro

2017-09-05

SiO 2 -based optical fibers are indispensable components of modern information communication technologies. It has recently become increasingly important to establish a technique for visualizing the nanoscale phase-separated structure inside SiO 2 -GeO 2 glass nanoparticles during the manufacturing of SiO 2 -GeO 2 fibers. This is because the rapidly increasing price of Ge has made it necessary to improve the Ge yield by clarifying the detailed mechanism of Ge diffusion into SiO 2 . However, direct observation of the internal nanostructure of glass particles has been extremely difficult, mainly due to electrostatic charging and the damage induced by electron and X-ray irradiation. In the present study, we used state-of-the-art scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), and energy dispersive X-ray spectroscopy (EDX) to examine cross-sectional samples of SiO 2 -GeO 2 particles embedded in an epoxy resin, which were fabricated using a broad Ar ion beam and a focused Ga ion beam. These advanced techniques enabled us to observe the internal phase-separated structure of the nanoparticles. We have for the first time clearly determined the SiO 2 -Si 1-x Ge x O 2 core-shell structure of such particles, the element distribution, the degree of crystallinity, and the quantitative chemical composition of microscopic regions, and we discuss the formation mechanism for the observed structure. The proposed imaging protocol is highly promising for studying the internal structure of various core-shell nanoparticles, which affects their catalytic, optical, and electronic properties.

Phase and group refractive indices of air calculation by fitting of phase difference measured using a combination of laser and low-coherence interferometry

NASA Astrophysics Data System (ADS)

Pikálek, Tomáš; Šarbort, Martin; Číp, Ondřej; Pham, Minh Tuan; Lešundák, Adam; Pravdová, Lenka; Buchta, Zdeněk.

2017-06-01

The air refractive index is an important parameter in interferometric length measurements, since it substantially affects the measurement accuracy. We present a refractive index of air measurement method based on monitoring the phase difference between the ambient air and vacuum inside a permanently evacuated double-spaced cell. The cell is placed in one arm of the Michelson interferometer equipped with two light sources—red LED and HeNe laser, while the low-coherence and laser interference signals are measured separately. Both phase and group refractive indices of air can be calculated from the measured signals. The method was experimentally verified by comparing the obtained refractive index values with two different techniques.

Experimental design methodologies in the optimization of chiral CE or CEC separations: an overview.

PubMed

Dejaegher, Bieke; Mangelings, Debby; Vander Heyden, Yvan

2013-01-01

In this chapter, an overview of experimental designs to develop chiral capillary electrophoresis (CE) and capillary electrochromatographic (CEC) methods is presented. Method development is generally divided into technique selection, method optimization, and method validation. In the method optimization part, often two phases can be distinguished, i.e., a screening and an optimization phase. In method validation, the method is evaluated on its fit for purpose. A validation item, also applying experimental designs, is robustness testing. In the screening phase and in robustness testing, screening designs are applied. During the optimization phase, response surface designs are used. The different design types and their application steps are discussed in this chapter and illustrated by examples of chiral CE and CEC methods.

A novel mechanical model for phase-separation in debris flows

NASA Astrophysics Data System (ADS)

Pudasaini, Shiva P.

2015-04-01

Understanding the physics of phase-separation between solid and fluid phases as a two-phase mass moves down slope is a long-standing challenge. Here, I propose a fundamentally new mechanism, called 'separation-flux', that leads to strong phase-separation in avalanche and debris flows. This new model extends the general two-phase debris flow model (Pudasaini, 2012) to include a separation-flux mechanism. The new flux separation mechanism is capable of describing and controlling the dynamically evolving phase-separation, segregation, and/or levee formation in a real two-phase, geometrically three-dimensional debris flow motion and deposition. These are often observed phenomena in natural debris flows and industrial processes that involve the transportation of particulate solid-fluid mixture material. The novel separation-flux model includes several dominant physical and mechanical aspects that result in strong phase-separation (segregation). These include pressure gradients, volume fractions of solid and fluid phases and their gradients, shear-rates, flow depth, material friction, viscosity, material densities, boundary structures, gravity and topographic constraints, grain shape, size, etc. Due to the inherent separation mechanism, as the mass moves down slope, more and more solid particles are brought to the front, resulting in a solid-rich and mechanically strong frontal surge head followed by a weak tail largely consisting of the viscous fluid. The primary frontal surge head followed by secondary surge is the consequence of the phase-separation. Such typical and dominant phase-separation phenomena are revealed here for the first time in real two-phase debris flow modeling and simulations. However, these phenomena may depend on the bulk material composition and the applied forces. Reference: Pudasaini, Shiva P. (2012): A general two-phase debris flow model. J. Geophys. Res., 117, F03010, doi: 10.1029/2011JF002186.

Microemulsion Electrokinetic Chromatography.

PubMed

Buchberger, Wolfgang

2016-01-01

Microemulsion electrokinetic chromatography (MEEKC) is a special mode of capillary electrophoresis employing a microemulsion as carrier electrolyte. Analytes may partition between the aqueous phase of the microemulsion and its oil droplets which act as a pseudostationary phase. The technique is well suited for the separation of neutral species, in which case charged oil droplets (obtained by addition of an anionic or cationic surfactant) are present. A single set of separation parameters may be sufficient for separation of a wide range of analytes belonging to quite different chemical classes. Fine-tuning of resolution and analysis time may be achieved by addition of organic solvents, by changes in the nature of the surfactants (and cosurfactants) used to stabilize the microemulsion, or by various additives that may undergo some additional interactions with the analytes. Besides the separation of neutral analytes (which may be the most important application area of MEEKC), it can also be employed for cationic and/or anionic species. In this chapter, MEEKC conditions are summarized that have proven their reliability for routine analysis. Furthermore, the mechanisms encountered in MEEKC allow an efficient on-capillary preconcentration of analytes, so that the problem of poor concentration sensitivity of ultraviolet absorbance detection is circumvented.

Multiple fuel supply system for an internal combustion engine

DOEpatents

Crothers, William T.

1977-01-01

A multiple fuel supply or an internal combustion engine wherein phase separation of components is deliberately induced. The resulting separation permits the use of a single fuel tank to supply components of either or both phases to the engine. Specifically, phase separation of a gasoline/methanol blend is induced by the addition of a minor amount of water sufficient to guarantee separation into an upper gasoline phase and a lower methanol/water phase. A single fuel tank holds the two-phase liquid with separate fuel pickups and separate level indicators for each phase. Either gasoline or methanol, or both, can be supplied to the engine as required by predetermined parameters. A fuel supply system for a phase-separated multiple fuel supply contained in a single fuel tank is described.

Phase-separation induced extraordinary toughening of magnetic hydrogels

NASA Astrophysics Data System (ADS)

Tang, Jingda; Li, Chenghai; Li, Haomin; Lv, Zengyao; Sheng, Hao; Lu, Tongqing; Wang, T. J.

2018-05-01

Phase separation markedly influences the physical properties of hydrogels. Here, we find that poly (N, N-dimethylacrylamide) (PDMA) hydrogels suffer from phase separation in aqueous sodium hydroxide solutions when the concentration is higher than 2 M. The polymer volume fraction and mechanical properties show an abrupt change around the transition point. We utilize this phase separation mechanism to synthesize tough magnetic PDMA hydrogels with the in-situ precipitation method. For comparison, we also prepared magnetic poly (2-acrylamido-2-methyl-propane sulfonic acid sodium) (PNaAMPS) magnetic hydrogels, where no phase separation occurs. The phase-separated magnetic PDMA hydrogels exhibit an extraordinarily high toughness of ˜1000 J m-2; while non-phase-separated magnetic PNaAMPS hydrogels only show a toughness of ˜1 J m-2, three orders of magnitude lower than that of PDMA hydrogels. This phase separation mechanism may become a new approach to prepare tough magnetic hydrogels and inspire more applications.

Phase-separated, epitaxial composite cap layers for electronic device applications and method of making the same

DOEpatents

Aytug, Tolga [Knoxville, TN; Paranthaman, Mariappan Parans [Knoxville, TN; Polat, Ozgur [Knoxville, TN

2012-07-17

An electronic component that includes a substrate and a phase-separated layer supported on the substrate and a method of forming the same are disclosed. The phase-separated layer includes a first phase comprising lanthanum manganate (LMO) and a second phase selected from a metal oxide (MO), metal nitride (MN), a metal (Me), and combinations thereof. The phase-separated material can be an epitaxial layer and an upper surface of the phase-separated layer can include interfaces between the first phase and the second phase. The phase-separated layer can be supported on a buffer layer comprising a composition selected from the group consisting of IBAD MgO, LMO/IBAD-MgO, homoepi-IBAD MgO and LMO/homoepi-MgO. The electronic component can also include an electronically active layer supported on the phase-separated layer. The electronically active layer can be a superconducting material, a ferroelectric material, a multiferroic material, a magnetic material, a photovoltaic material, an electrical storage material, and a semiconductor material.

Justification of rapid prototyping in the development cycle of thermoplastic-based lab-on-a-chip.

PubMed

Preywisch, Regina; Ritzi-Lehnert, Marion; Drese, Klaus S; Röser, Tina

2011-11-01

During the developmental cycle of lab-on-a-chip devices, various microstructuring techniques are required. While in the designing and assay implementation phase direct structuring or so-called rapid-prototyping methods such as milling or laser ablation are applied, replication methods like hot embossing or injection moulding are favourable for large quantity manufacturing. This work investigated the applicability of rapid-prototyping techniques for thermoplastic chip development in general, and the reproducibility of performances in dependency of the structuring technique. A previously published chip for prenatal diagnosis that preconcentrates DNA via electrokinetic trapping and field-amplified-sample-stacking and afterwards separates it in CGE was chosen as a model. The impact of structuring, sealing, and the integration of membranes on the mobility of the EOF, DNA preconcentration, and DNA separation was studied. Structuring methods were found to significantly change the location where preconcentration of DNA occurs. However, effects on the mobility of the EOF and the separation quality of DNA were not observed. Exchange of the membrane has no effect on the chip performance, whereas the sealing method impairs the separation of DNA within the chip. The overall assay performance is not significantly influenced by different structuring methods; thus, the application of rapid-prototyping methods during a chip development cycle is well justified. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A combination strategy for extraction and isolation of multi-component natural products by systematic two-phase solvent extraction-(13)C nuclear magnetic resonance pattern recognition and following conical counter-current chromatography separation: Podophyllotoxins and flavonoids from Dysosma versipellis (Hance) as examples.

PubMed

Yang, Zhi; Wu, Youqian; Wu, Shihua

2016-01-29

Despite of substantial developments of extraction and separation techniques, isolation of natural products from natural resources is still a challenging task. In this work, an efficient strategy for extraction and isolation of multi-component natural products has been successfully developed by combination of systematic two-phase liquid-liquid extraction-(13)C NMR pattern recognition and following conical counter-current chromatography separation. A small-scale crude sample was first distributed into 9 systematic hexane-ethyl acetate-methanol-water (HEMWat) two-phase solvent systems for determination of the optimum extraction solvents and partition coefficients of the prominent components. Then, the optimized solvent systems were used in succession to enrich the hydrophilic and lipophilic components from the large-scale crude sample. At last, the enriched components samples were further purified by a new conical counter-current chromatography (CCC). Due to the use of (13)C NMR pattern recognition, the kinds and structures of major components in the solvent extracts could be predicted. Therefore, the method could collect simultaneously the partition coefficients and the structural information of components in the selected two-phase solvents. As an example, a cytotoxic extract of podophyllotoxins and flavonoids from Dysosma versipellis (Hance) was selected. After the systematic HEMWat system solvent extraction and (13)C NMR pattern recognition analyses, the crude extract of D. versipellis was first degreased by the upper phase of HEMWat system (9:1:9:1, v/v), and then distributed in the two phases of the system of HEMWat (2:8:2:8, v/v) to obtain the hydrophilic lower phase extract and lipophilic upper phase extract, respectively. These extracts were further separated by conical CCC with the HEMWat systems (1:9:1:9 and 4:6:4:6, v/v). As results, total 17 cytotoxic compounds were isolated and identified. In general, whole results suggested that the strategy was very efficient for the systematic extraction and isolation of biological active components from the complex biomaterials. Copyright © 2016 Elsevier B.V. All rights reserved.

Blind separation of overlapping partials in harmonic musical notes using amplitude and phase reconstruction

NASA Astrophysics Data System (ADS)

de León, Jesús Ponce; Beltrán, José Ramón

2012-12-01

In this study, a new method of blind audio source separation (BASS) of monaural musical harmonic notes is presented. The input (mixed notes) signal is processed using a flexible analysis and synthesis algorithm (complex wavelet additive synthesis, CWAS), which is based on the complex continuous wavelet transform. When the harmonics from two or more sources overlap in a certain frequency band (or group of bands), a new technique based on amplitude similarity criteria is used to obtain an approximation to the original partial information. The aim is to show that the CWAS algorithm can be a powerful tool in BASS. Compared with other existing techniques, the main advantages of the proposed algorithm are its accuracy in the instantaneous phase estimation, its synthesis capability and that the only input information needed is the mixed signal itself. A set of synthetically mixed monaural isolated notes have been analyzed using this method, in eight different experiments: the same instrument playing two notes within the same octave and two harmonically related notes (5th and 12th intervals), two different musical instruments playing 5th and 12th intervals, two different instruments playing non-harmonic notes, major and minor chords played by the same musical instrument, three different instruments playing non-harmonically related notes and finally the mixture of a inharmonic instrument (piano) and one harmonic instrument. The results obtained show the strength of the technique.

Beam position monitor for energy recovered linac beams

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

Powers, Thomas; Evtushenko, Pavel

A method of determining the beam position in an energy recovered linac (ERL). The method makes use of in phase and quadrature (I/Q) demodulation techniques to separate the pickup signal generated by the electromagnetic fields generated by the first and second pass beam in the energy recovered linac. The method includes using analog or digital based I/Q demodulation techniques in order to measure the relative amplitude of the signals from a position sensitive beam pickup such as a button, strip line or microstripline beam position monitor.

Method for separating disparate components in a fluid stream

DOEpatents

Meikrantz, David H.

1990-01-01

The invention provides a method of separating a mixed component waste stream in a centrifugal separator. The mixed component waste stream is introduced into the separator and is centrifugally separated within a spinning rotor. A dual vortex separation occurs due to the phase density differences, with the phases exiting the rotor distinct from one another. In a preferred embodiment, aqueous solutions of organics can be separated with up to 100% efficiency. The relatively more dense water phase is centrifugally separated through a radially outer aperture in the separator, while the relatively less dense organic phase is separated through a radially inner aperture.

FAST TRACK COMMUNICATION Solving the ultradiscrete KdV equation

NASA Astrophysics Data System (ADS)

Willox, Ralph; Nakata, Yoichi; Satsuma, Junkichi; Ramani, Alfred; Grammaticos, Basile

2010-12-01

We show that a generalized cellular automaton, exhibiting solitonic interactions, can be explicitly solved by means of techniques first introduced in the context of the scattering problem for the KdV equation. We apply this method to calculate the phase-shifts caused by interactions between the solitonic and non-solitonic parts into which arbitrary initial states separate in time.

High-performance liquid chromatographic method for the determination of dansyl-polyamines

Treesearch

Subhash C. Minocha; Rakesh Minocha; Cheryl A. Robie

1990-01-01

This paper describes a fast reliable, and a sensitive technique for the separation and quantification of dansylated polyamines by high-performance liquid chromatography. Using a small 33 x 4.6 mm I.D., 3 ?m particle size, C18 reversed-phase cartridge column and a linear gradient of acetonitrile-heptanesulfonate (10 mM, pH 3.4...

Local electric field direct writing – Electron-beam lithography and mechanism

DOE PAGES

Jiang, Nan; Su, Dong; Spence, John C. H.

2017-08-24

Local electric field induced by a focused electron probe in silicate glass thin films is evaluated in this paper by the migration of cations. Extremely strong local electric fields can be obtained by the focused electron probe from a scanning transmission electron microscope. As a result, collective atomic displacements occur. This newly revised mechanism provides an efficient tool to write patterned nanostructures directly, and thus overcome the low efficiency of the conventional electron-beam lithography. Applying this technique to silicate glass thin films, as an example, a grid of rods of nanometer dimension can be efficiently produced by rapidly scanning amore » focused electron probe. This nanopatterning is achieved through swift phase separation in the sample, without any post-development processes. The controlled phase separation is induced by massive displacements of cations (glass modifiers) within the glass-former network, driven by the strong local electric fields. The electric field is induced by accumulated charge within the electron probed region, which is generated by the excitation of atomic electrons by the incident electron. Throughput is much improved compared to other scanning probe techniques. Finally, the half-pitch spatial resolution of nanostructure in this particular specimen is 2.5 nm.« less

Local electric field direct writing – Electron-beam lithography and mechanism

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

Jiang, Nan; Su, Dong; Spence, John C. H.

Local electric field induced by a focused electron probe in silicate glass thin films is evaluated in this paper by the migration of cations. Extremely strong local electric fields can be obtained by the focused electron probe from a scanning transmission electron microscope. As a result, collective atomic displacements occur. This newly revised mechanism provides an efficient tool to write patterned nanostructures directly, and thus overcome the low efficiency of the conventional electron-beam lithography. Applying this technique to silicate glass thin films, as an example, a grid of rods of nanometer dimension can be efficiently produced by rapidly scanning amore » focused electron probe. This nanopatterning is achieved through swift phase separation in the sample, without any post-development processes. The controlled phase separation is induced by massive displacements of cations (glass modifiers) within the glass-former network, driven by the strong local electric fields. The electric field is induced by accumulated charge within the electron probed region, which is generated by the excitation of atomic electrons by the incident electron. Throughput is much improved compared to other scanning probe techniques. Finally, the half-pitch spatial resolution of nanostructure in this particular specimen is 2.5 nm.« less

Multidimensional profiling of plasma lipoproteins by size exclusion chromatography followed by reverse-phase protein arrays

PubMed Central

Dernick, Gregor; Obermüller, Stefan; Mangold, Cyrill; Magg, Christine; Matile, Hugues; Gutmann, Oliver; von der Mark, Elisabeth; Handschin, Corinne; Maugeais, Cyrille; Niesor, Eric J.

2011-01-01

The composition of lipoproteins and the association of proteins with various particles are of much interest in the context of cardiovascular disease. Here, we describe a technique for the multidimensional analysis of lipoproteins and their associated apolipoproteins. Plasma is separated by size exclusion chromatography (SEC), and fractions are analyzed by reverse-phase arrays. SEC fractions are spotted on nitrocellulose slides and incubated with different antibodies against individual apolipoproteins or antibodies against various apolipoproteins. In this way, tens of analytes can be measured simultaneously in 100 μl of plasma from a single SEC separation. This methodology is particularly suited to simultaneous analysis of multiple proteins that may change their distribution to lipoproteins or alter their conformation, depending on factors that influence circulating lipoprotein size or composition. We observed changes in the distribution of exchangeable apolipoproteins following addition of recombinant apolipoproteins or interaction with exogenous compounds. While the cholesteryl ester transfer protein (CETP)-dependent formation of pre-β-HDL was inhibited by the CETP inhibitors torcetrapib and anacetrapib, it was not reduced by the CETP modulator dalcetrapib. This finding was elucidated using this technique. PMID:21971713

Fast X-ray imaging of cavitating flows

DOE PAGES

Khlifa, Ilyass; Vabre, Alexandre; Hočevar, Marko; ...

2017-10-20

A new method based on ultra-fast X-ray imaging was developed in this work for simultaneous investigations of the dynamics and the structures of complex two-phase flows. Here in this paper, cavitation was created inside a millimetric 2D Venturi-type test section, while seeding particles were injected into the flow. Thanks to the phase-contrast enhancement technique provided by the APS (Advanced Photon Source) synchrotron beam, high definition X-ray images of the complex cavitating flows were obtained. These images contain valuable information about both the liquid and the gaseous phases. By means of image processing, the two phases were separated, and velocity fieldsmore » of each phase were therefore calculated using image cross-correlations. The local vapour volume fractions were also obtained thanks to the local intensity levels within the recorded images. These simultaneous measurements, provided by this new technique, afford more insight into the structure and the dynamic of two-phase flows as well as the interactions between then, and hence enable to improve our understanding of their behavior. In the case of cavitating flows inside a Venturi-type test section, the X-ray measurements demonstrates, for the first time, the presence of significant slip velocities between the phases within sheet cavities for both steady and unsteady flow configurations.« less

Fast X-ray imaging of cavitating flows

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

Khlifa, Ilyass; Vabre, Alexandre; Hočevar, Marko

A new method based on ultra-fast X-ray imaging was developed in this work for simultaneous investigations of the dynamics and the structures of complex two-phase flows. Here in this paper, cavitation was created inside a millimetric 2D Venturi-type test section, while seeding particles were injected into the flow. Thanks to the phase-contrast enhancement technique provided by the APS (Advanced Photon Source) synchrotron beam, high definition X-ray images of the complex cavitating flows were obtained. These images contain valuable information about both the liquid and the gaseous phases. By means of image processing, the two phases were separated, and velocity fieldsmore » of each phase were therefore calculated using image cross-correlations. The local vapour volume fractions were also obtained thanks to the local intensity levels within the recorded images. These simultaneous measurements, provided by this new technique, afford more insight into the structure and the dynamic of two-phase flows as well as the interactions between then, and hence enable to improve our understanding of their behavior. In the case of cavitating flows inside a Venturi-type test section, the X-ray measurements demonstrates, for the first time, the presence of significant slip velocities between the phases within sheet cavities for both steady and unsteady flow configurations.« less

Reaction-mediated entropic effect on phase separation in a binary polymer system

NASA Astrophysics Data System (ADS)

Sun, Shujun; Guo, Miaocai; Yi, Xiaosu; Zhang, Zuoguang

2017-10-01

We present a computer simulation to study the phase separation behavior induced by polymerization in a binary system comprising polymer chains and reactive monomers. We examined the influence of interaction parameter between components and monomer concentration on the reaction-induced phase separation. The simulation results demonstrate that increasing interaction parameter (enthalpic effect) would accelerate phase separation, while entropic effect plays a key role in the process of phase separation. Furthermore, scanning electron microscopy observations illustrate identical morphologies as found in theoretical simulation. This study may enrich our comprehension of phase separation in polymer mixture.

Multifunctional picoliter droplet manipulation platform and its application in single cell analysis.

PubMed

Gu, Shu-Qing; Zhang, Yun-Xia; Zhu, Ying; Du, Wen-Bin; Yao, Bo; Fang, Qun

2011-10-01

We developed an automated and multifunctional microfluidic platform based on DropLab to perform flexible generation and complex manipulations of picoliter-scale droplets. Multiple manipulations including precise droplet generation, sequential reagent merging, and multistep solid-phase extraction for picoliter-scale droplets could be achieved in the present platform. The system precision in generating picoliter-scale droplets was significantly improved by minimizing the thermo-induced fluctuation of flow rate. A novel droplet fusion technique based on the difference of droplet interfacial tensions was developed without the need of special microchannel networks or external devices. It enabled sequential addition of reagents to droplets on demand for multistep reactions. We also developed an effective picoliter-scale droplet splitting technique with magnetic actuation. The difficulty in phase separation of magnetic beads from picoliter-scale droplets due to the high interfacial tension was overcome using ferromagnetic particles to carry the magnetic beads to pass through the phase interface. With this technique, multistep solid-phase extraction was achieved among picoliter-scale droplets. The present platform had the ability to perform complex multistep manipulations to picoliter-scale droplets, which is particularly required for single cell analysis. Its utility and potentials in single cell analysis were preliminarily demonstrated in achieving high-efficiency single-cell encapsulation, enzyme activity assay at the single cell level, and especially, single cell DNA purification based on solid-phase extraction.

Correcting for the effects of pupil discontinuities with the ACAD method

NASA Astrophysics Data System (ADS)

Mazoyer, Johan; Pueyo, Laurent; N'Diaye, Mamadou; Mawet, Dimitri; Soummer, Rémi; Norman, Colin

2016-07-01

The current generation of ground-based coronagraphic instruments uses deformable mirrors to correct for phase errors and to improve contrast levels at small angular separations. Improving these techniques, several space and ground based instruments are currently developed using two deformable mirrors to correct for both phase and amplitude errors. However, as wavefront control techniques improve, more complex telescope pupil geometries (support structures, segmentation) will soon be a limiting factor for these next generation coronagraphic instruments. The technique presented in this proceeding, the Active Correction of Aperture Discontinuities method, is taking advantage of the fact that most future coronagraphic instruments will include two deformable mirrors, and is proposing to find the shapes and actuator movements to correct for the effect introduced by these complex pupil geometries. For any coronagraph previously designed for continuous apertures, this technique allow to obtain similar performance in contrast with a complex aperture (with segmented and secondary mirror support structures), with high throughput and flexibility to adapt to changing pupil geometry (e.g. in case of segment failure or maintenance of the segments). We here present the results of the parametric analysis realized on the WFIRST pupil for which we obtained high contrast levels with several deformable mirror setups (size, separation between them), coronagraphs (Vortex charge 2, vortex charge 4, APLC) and spectral bandwidths. However, because contrast levels and separation are not the only metrics to maximize the scientific return of an instrument, we also included in this study the influence of these deformable mirror shapes on the throughput of the instrument and sensitivity to pointing jitters. Finally, we present results obtained on another potential space based telescope segmented aperture. The main result of this proceeding is that we now obtain comparable performance than the coronagraphs previously designed for WFIRST. First result from the parametric analysis strongly suggest that the 2 deformable mirror set up (size and distance between them) have a important impact on the performance in contrast and throughput of the final instrument.

Qualitative Characterization of the Aqueous Fraction from Hydrothermal Liquefaction of Algae Using 2D Gas Chromatography with Time-of-flight Mass Spectrometry

PubMed Central

Maddi, Balakrishna; Panisko, Ellen; Albrecht, Karl; Howe, Daniel

2016-01-01

Two-dimensional gas chromatography coupled with time-of-flight mass spectrometry is a powerful tool for identifying and quantifying chemical components in complex mixtures. It is often used to analyze gasoline, jet fuel, diesel, bio-diesel and the organic fraction of bio-crude/bio-oil. In most of those analyses, the first dimension of separation is non-polar, followed by a polar separation. The aqueous fractions of bio-crude and other aqueous samples from biofuels production have been examined with similar column combinations. However, sample preparation techniques such as derivatization, solvent extraction, and solid-phase extraction were necessaryprior to analysis. In this study, aqueous fractions obtained from the hydrothermal liquefaction of algae were characterized by two-dimensional gas chromatography coupled with time-of-flight mass spectrometry without prior sample preparation techniques using a polar separation in the first dimension followed by a non-polar separation in the second. Two-dimensional plots from this analysis were compared with those obtained from the more traditional column configuration. Results from qualitative characterization of the aqueous fractions of algal bio-crude are discussed in detail. The advantages of using a polar separation followed by a non-polar separation for characterization of organics in aqueous samples by two-dimensional gas chromatography coupled with time-of-flight mass spectrometry are highlighted. PMID:27022829

Qualitative Characterization of the Aqueous Fraction from Hydrothermal Liquefaction of Algae Using 2D Gas Chromatography with Time-of-flight Mass Spectrometry.

PubMed

Maddi, Balakrishna; Panisko, Ellen; Albrecht, Karl; Howe, Daniel

2016-03-06

Two-dimensional gas chromatography coupled with time-of-flight mass spectrometry is a powerful tool for identifying and quantifying chemical components in complex mixtures. It is often used to analyze gasoline, jet fuel, diesel, bio-diesel and the organic fraction of bio-crude/bio-oil. In most of those analyses, the first dimension of separation is non-polar, followed by a polar separation. The aqueous fractions of bio-crude and other aqueous samples from biofuels production have been examined with similar column combinations. However, sample preparation techniques such as derivatization, solvent extraction, and solid-phase extraction were necessary prior to analysis. In this study, aqueous fractions obtained from the hydrothermal liquefaction of algae were characterized by two-dimensional gas chromatography coupled with time-of-flight mass spectrometry without prior sample preparation techniques using a polar separation in the first dimension followed by a non-polar separation in the second. Two-dimensional plots from this analysis were compared with those obtained from the more traditional column configuration. Results from qualitative characterization of the aqueous fractions of algal bio-crude are discussed in detail. The advantages of using a polar separation followed by a non-polar separation for characterization of organics in aqueous samples by two-dimensional gas chromatography coupled with time-of-flight mass spectrometry are highlighted.

Hydrodynamic studies on two wiggling hydrofoils in an oblique arrangement

NASA Astrophysics Data System (ADS)

Lin, Xingjian; He, Guoyi; He, Xinyi; Wang, Qi; Chen, Longsheng

2018-06-01

The propulsive performance of an oblique school of fish is numerically studied using an immersed boundary technique. The effect of the spacing and wiggling phase on the hydrodynamics of the system is investigated. The hydrodynamics of the system is deeply affected by the spacing between each fish in the school. When the horizontal separation is smaller than the length of the fish body, the downstream fish exhibits a larger thrust coefficient and greater propulsive efficiency than the isolated fish. However, the corresponding values for the upstream fish are smaller. The opposite behavior occurs when the horizontal separation increases beyond the length of fish body. The propulsive performance of the entire oblique school of fish can be substantially enhanced when the separations are optimized.

Silica particles encapsulated poly(styrene-divinylbenzene) monolithic stationary phases for micro-high performance liquid chromatography.

PubMed

Bakry, R; Stöggl, W M; Hochleitner, E O; Stecher, G; Huck, C W; Bonn, G K

2006-11-03

In the paper we demonstrate a new approach for the preparation and application of continuous silica bed columns that involve encapsulation (entrapment) of functionalized silica microparticles, which can be used as packing material in micro high performance liquid chromatography (micro-HPLC) and capillary electrochromatography (CEC). Like traditional packed columns, these capillaries possess characterized silica particles that offer high phase ratio and narrow pore size distribution leading to high retention and separation efficiency, respectively. More importantly, immobilization of the microparticles stabilizes the separation bed and eliminates the need for retaining frits. The developed capillary columns were fabricated in exactly the same way as a packed capillary column (slurry packing) but with an additional entrapment step. This immobilization of the packed bed was achieved by in situ polymerization of styrene and divinylbenzene in presence of decanol as a porogen and azobisisobutyronitrile as thermal initiator. Silica particles with different particle sizes and pore sizes ranging from 60 to 4000 A were studied. In addition different modified silica was used, including C-18 reversed phase, anion exchange and chiral stationary phases. Efficient separation of polyphenolic compounds, peptides, proteins and even DNA mutation were achieved using the developed technique depending on the properties of the silica particles used (particles pore size). For example, using 3 microm ProntoSIL C-18 particles with 300 A pore size, separation efficiencies in the range of 120,000-200,000 plates/m were obtained for protein separation, in a 6 cm x 200 microm i.d. capillary column. Using encapsulated silica C-18 with 1000 A pore size, separation of DNA homo and hetero duplexes were achieved under denaturing HPLC conditions for mutation detection. In addition, nucleotides were separated using anion exchange material encapsulated with poly(styrene-divinylbenzene) (PS/DVB), which indicated that the chromatographic properties of the silica packing material were still active after polymerization. The prepared capillary columns were found to be stable and could easily be operated continuously up to a pressure of 350 bar without column damage and capillary can be cut to any desired length.

Analyzing slowly exchanging protein conformations by ion mobility mass spectrometry: study of the dynamic equilibrium of prolyl oligopeptidase.

PubMed

López, Abraham; Vilaseca, Marta; Madurga, Sergio; Varese, Monica; Tarragó, Teresa; Giralt, Ernest

2016-07-01

Ion mobility mass spectrometry (IMMS) is a biophysical technique that allows the separation of isobaric species on the basis of their size and shape. The high separation capacity, sensitivity and relatively fast time scale measurements confer IMMS great potential for the study of proteins in slow (µs-ms) conformational equilibrium in solution. However, the use of this technique for examining dynamic proteins is still not generalized. One of the major limitations is the instability of protein ions in the gas phase, which raises the question as to what extent the structures detected reflect those in solution. Here, we addressed this issue by analyzing the conformational landscape of prolyl oligopeptidase (POP) - a model of a large dynamic enzyme in the µs-ms range - by native IMMS and compared the results obtained in the gas phase with those obtained in solution. In order to interpret the experimental results, we used theoretical simulations. In addition, the stability of POP gaseous ions was explored by charge reduction and collision-induced unfolding experiments. Our experiments disclosed two species of POP in the gas phase, which correlated well with the open and closed conformations in equilibrium in solution; moreover, a gas-phase collapsed form of POP was also detected. Therefore, our findings not only support the potential of IMMS for the study of multiple co-existing conformations of large proteins in slow dynamic equilibrium in solution but also stress the need for careful data analysis to avoid artifacts. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Digitally grown AlInAsSb for high gain separate absorption, grading, charge, and multiplication avalanche photodiodes

NASA Astrophysics Data System (ADS)

Lyu, Yuexi; Han, Xi; Sun, Yaoyao; Jiang, Zhi; Guo, Chunyan; Xiang, Wei; Dong, Yinan; Cui, Jie; Yao, Yuan; Jiang, Dongwei; Wang, Guowei; Xu, Yingqiang; Niu, Zhichuan

2018-01-01

We report on the growth of high quality GaSb-based AlInAsSb quaternary alloy by molecular beam epitaxy (MBE) to fabricate avalanche photodiodes (APDs). By means of high resolution X-ray diffraction (HRXRD) and scanning transmission electron microscope (STEM), phase separation phenomenon of AlInAsSb random alloy with naturally occurring vertical superlattice configuration was demonstrated. To overcome the tendency for phase segregation while maintaining a highly crystalline film, a digital alloy technique with migration-enhanced epitaxy growth method was employed, using a shutter sequence of AlSb, AlAs, AlSb, Sb, In, InAs, In, Sb. AlInAsSb digital alloy has proved to be reproducible and consistent with single phase, showing sharp satellite peaks on HRXRD rocking curve and smooth surface morphology under atomic force microscopy (AFM). Using optimized digital alloy, AlInAsSb separate absorption, grading, charge, and multiplication (SAGCM) APD was grown and fabricated. At room temperature, the device showed high performance with low dark current density of ∼14.1 mA/cm2 at 95% breakdown and maximum stable gain before breakdown as high as ∼200, showing the potential for further applications in optoelectronic devices.

Melt Extrusion of High-Dose Co-Amorphous Drug-Drug Combinations : Theme: Formulation and Manufacturing of Solid Dosage Forms Guest Editors: Tony Zhou and Tonglei Li.

PubMed

Arnfast, Lærke; Kamruzzaman, Md; Löbmann, Korbinian; Aho, Johanna; Baldursdottir, Stefania; Rades, Thomas; Rantanen, Jukka

2017-12-01

Many future drug products will be based on innovative manufacturing solutions, which will increase the need for a thorough understanding of the interplay between drug material properties and processability. In this study, hot melt extrusion of a drug-drug mixture with minimal amount of polymeric excipient was investigated. Using indomethacin-cimetidine as a model drug-drug system, processability of physical mixtures with and without 5% (w/w) of polyethylene oxide (PEO) were studied using Differential Scanning Calorimetry (DSC) and Small Amplitude Oscillatory Shear (SAOS) rheometry. Extrudates containing a co-amorphous glass solution were produced and the solid-state composition of these was studied with DSC. Rheological analysis indicated that the studied systems display viscosities higher than expected for small molecule melts and addition of PEO decreased the viscosity of the melt. Extrudates of indomethacin-cimetidine alone displayed amorphous-amorphous phase separation after 4 weeks of storage, whereas no phase separation was observed during the 16 week storage of the indomethacin-cimetidine extrudates containing 5% (w/w) PEO. Melt extrusion of co-amorphous extrudates with low amounts of polymer was found to be a feasible manufacturing technique. Addition of 5% (w/w) polymer reduced melt viscosity and prevented phase separation.

An advanced algorithm for deformation estimation in non-urban areas

NASA Astrophysics Data System (ADS)

Goel, Kanika; Adam, Nico

2012-09-01

This paper presents an advanced differential SAR interferometry stacking algorithm for high resolution deformation monitoring in non-urban areas with a focus on distributed scatterers (DSs). Techniques such as the Small Baseline Subset Algorithm (SBAS) have been proposed for processing DSs. SBAS makes use of small baseline differential interferogram subsets. Singular value decomposition (SVD), i.e. L2 norm minimization is applied to link independent subsets separated by large baselines. However, the interferograms used in SBAS are multilooked using a rectangular window to reduce phase noise caused for instance by temporal decorrelation, resulting in a loss of resolution and the superposition of topography and deformation signals from different objects. Moreover, these have to be individually phase unwrapped and this can be especially difficult in natural terrains. An improved deformation estimation technique is presented here which exploits high resolution SAR data and is suitable for rural areas. The implemented method makes use of small baseline differential interferograms and incorporates an object adaptive spatial phase filtering and residual topography removal for an accurate phase and coherence estimation, while preserving the high resolution provided by modern satellites. This is followed by retrieval of deformation via the SBAS approach, wherein, the phase inversion is performed using an L1 norm minimization which is more robust to the typical phase unwrapping errors encountered in non-urban areas. Meter resolution TerraSAR-X data of an underground gas storage reservoir in Germany is used for demonstrating the effectiveness of this newly developed technique in rural areas.

Fluorescent probes for lipid rafts: from model membranes to living cells.

PubMed

Klymchenko, Andrey S; Kreder, Rémy

2014-01-16

Membrane microdomains (rafts) remain one of the controversial issues in biophysics. Fluorescent molecular probes, which make these lipid nanostructures visible through optical techniques, are one of the tools currently used to study lipid rafts. The most common are lipophilic fluorescent probes that partition specifically into liquid ordered or liquid disordered phase. Their partition depends on the lipid composition of a given phase, which complicates their use in cellular membranes. A second class of probes is based on environment-sensitive dyes, which partition into both phases, but stain them by different fluorescence color, intensity, or lifetime. These probes can directly address the properties of each separate phase, but their cellular applications are still limited. The present review focuses on summarizing the current state in the field of developing and applying fluorescent molecular probes to study lipid rafts. We highlight an urgent need to develop new probes, specifically adapted for cell plasma membranes and compatible with modern fluorescence microscopy techniques to push the understanding of membrane microdomains forward. Copyright © 2014 Elsevier Ltd. All rights reserved.

Separation of aqueous two-phase polymer systems in microgravity

NASA Technical Reports Server (NTRS)

Vanalstine, J. M.; Harris, J. M.; Synder, S.; Curreri, P. A.; Bamberger, S. B.; Brooks, D. E.

1984-01-01

Phase separation of polymer systems in microgravity is studied in aircraft flights to prepare shuttle experiments. Short duration (20 sec) experiments demonstrate that phase separation proceeds rapidly in low gravity despite appreciable phase viscosities and low liquid interfacial tensions (i.e., 50 cP, 10 micro N/m). Ostwald ripening does not appear to be a satisfactory model for the phase separation mechanism. Polymer coated surfaces are evaluated as a means to localize phases separated in low gravity. Contact angle measurements demonstrate that covalently coupling dextran or PEG to glass drastically alters the 1-g wall wetting behavior of the phases in dextran-PEG two phase systems.

Color image cryptosystem using Fresnel diffraction and phase modulation in an expanded fractional Fourier transform domain

NASA Astrophysics Data System (ADS)

Chen, Hang; Liu, Zhengjun; Chen, Qi; Blondel, Walter; Varis, Pierre

2018-05-01

In this letter, what we believe is a new technique for optical color image encryption by using Fresnel diffraction and a phase modulation in an extended fractional Fourier transform domain is proposed. Different from the RGB component separation based method, the color image is converted into one component by improved Chirikov mapping. The encryption system is addressed with Fresnel diffraction and phase modulation. A pair of lenses is placed into the fractional Fourier transform system for the modulation of beam propagation. The structure parameters of the optical system and parameters in Chirikov mapping serve as extra keys. Some numerical simulations are given to test the validity of the proposed cryptosystem.

RP-UHPLC-UV-ESI-MS/MS analysis of LPMO generated C4-oxidized gluco-oligosaccharides after non-reductive labeling with 2-aminobenzamide.

PubMed

Frommhagen, Matthias; van Erven, Gijs; Sanders, Mark; van Berkel, Willem J H; Kabel, Mirjam A; Gruppen, Harry

2017-08-07

Lytic polysaccharide monooxygenases (LPMOs) are able to cleave recalcitrant polysaccharides, such as cellulose, by oxidizing the C1 and/or C4 atoms. The analysis of the resulting products requires a variety of analytical techniques. Up to now, these techniques mainly focused on the identification of non-oxidized and C1-oxidized oligosaccharides. The analysis of C4-oxidized gluco-oligosaccharides is mostly performed by using high pressure anion exchange chromatography (HPAEC). However, the alkaline conditions used during HPAEC analysis lead to tautomerization of C4-oxidized gluco-oligosaccharides, which limits the use of this technique. Here, we describe the use of reverse phase-ultra high performance liquid chromatography (RP-UHPLC) in combination with non-reductive 2-aminobenzamide (2-AB) labeling. Non-reductive 2-AB labeling enabled separation of C4-oxidized gluco-oligosaccharides from their non-oxidized counterparts. Moreover, RP-UHPLC does not require buffered mobile phases, which reduce mass spectrometry (MS) sensitivity. The latter is seen as an advantage over other techniques such as hydrophilic interaction liquid chromatography and porous graphitized carbon coupled to MS. RP-UHPLC coupled to UV detection and mass spectrometry allowed the identification of both labeled non-oxidized and C4-oxidized oligosaccharides. Non-reductive labeling kept the ketone at the C4-position of LPMO oxidized oligosaccharides intact, while selective reducing agents such as sodium triacetoxyborohydride (STAB) reduced this ketone group. Our results show that RP-UHPLC-UV-ESI-MS in combination with non-reductively 2-AB labeling is a suitable technique for the separation and identification of LPMO-generated C4-oxidized gluco-oligosaccharides. Copyright © 2017 The Authors. Published by Elsevier Ltd.. All rights reserved.

Preparation, Processing, and Characterization of Oriented Polycrystalline Zeolite and Aluminophosphate Membranes

NASA Astrophysics Data System (ADS)

Stoeger, Jared Andrew

Since the advent of zeolite membranes, speculation on their industrial applicability has been closely monitored, although widespread commercialization has been hampered by limitations in fabrication and post-synthesis processing. Economical, energy-efficient technology breakthroughs require an evaluation of a range of material candidates which show robustness and reliability. Straightforward manufacturing techniques should be devised to generate thousands of square meters of membrane area; however, this demands control of structural characteristics on the scale of nanometers. As described in this dissertation, the path forward will be forged by exploiting the intrinsic crystalline properties of zeolites or aluminophosphates for the next advancement in membrane technology. A facile method is described for the preparation of silicalite-1 (MFI zeolite type) membranes using the secondary growth technique on symmetric porous stainless steel tubes. Activation through rapid thermal processing (RTP), a lamp-based heat-treatment process used as a critical fabrication step in silicon integrated circuit manufacturing, is proven to reduce the density of non-zeolitic transport pathways which are detrimental to high-resolution molecular sieving. RTP-treated membranes are shown to have enhanced performance in the binary separation of vapor-phase isomers (p-/o-xylene), gas-phase isomers (n-/i-butane), and alcohol/water when compared to membranes activated at a much slower heating rate but otherwise similarly-prepared. The performance is discussed in the context of the market potential for industrially-attractive separations: the recovery of p-xylene from an isomeric mixture or alcohol biofuels from aqueous post-fermentation streams. Hydrothermal growth techniques for the preparation and characterization of continuous aluminophosphate (AFI zeolite type) membranes with a preferential crystallographic alignment on porous alpha-Al2O3 disc supports are demonstrated. A mechanism is proposed for flake-like crystal formation in the early stages of in-plane crystalline intergrowth between oriented columnar crystals by electric heating. It is shown that elevated temperatures induce a phase transformation to a densified aluminophosphate phase despite framework metal substitution or alternative heat-treatment conditions. Additionally, stability and membrane characteristics following in situ microwave growth using a TiO2-coated support are examined. Indications of improved quality validate the candidacy of the microwave-grown membranes with regard to the potential for carbon nanotube synthesis in the aligned one-dimensional channels for high flux, high separation factor membrane fabrication.

Correlating Resolving Power, Resolution, and Collision Cross Section: Unifying Cross-Platform Assessment of Separation Efficiency in Ion Mobility Spectrometry.

PubMed

Dodds, James N; May, Jody C; McLean, John A

2017-11-21

Here we examine the relationship among resolving power (R p ), resolution (R pp ), and collision cross section (CCS) for compounds analyzed in previous ion mobility (IM) experiments representing a wide variety of instrument platforms and IM techniques. Our previous work indicated these three variables effectively describe and predict separation efficiency for drift tube ion mobility spectrometry experiments. In this work, we seek to determine if our previous findings are a general reflection of IM behavior that can be applied to various instrument platforms and mobility techniques. Results suggest IM distributions are well characterized by a Gaussian model and separation efficiency can be predicted on the basis of the empirical difference in the gas-phase CCS and a CCS-based resolving power definition (CCS/ΔCCS). Notably traveling wave (TWIMS) was found to operate at resolutions substantially higher than a single-peak resolving power suggested. When a CCS-based R p definition was utilized, TWIMS was found to operate at a resolving power between 40 and 50, confirming the previous observations by Giles and co-workers. After the separation axis (and corresponding resolving power) is converted to cross section space, it is possible to effectively predict separation behavior for all mobility techniques evaluated (i.e., uniform field, trapped ion mobility, traveling wave, cyclic, and overtone instruments) using the equations described in this work. Finally, we are able to establish for the first time that the current state-of-the-art ion mobility separations benchmark at a CCS-based resolving power of >300 that is sufficient to differentiate analyte ions with CCS differences as small as 0.5%.

Optimizing correlation techniques for improved earthquake location

USGS Publications Warehouse

Schaff, D.P.; Bokelmann, G.H.R.; Ellsworth, W.L.; Zanzerkia, E.; Waldhauser, F.; Beroza, G.C.

2004-01-01

Earthquake location using relative arrival time measurements can lead to dramatically reduced location errors and a view of fault-zone processes with unprecedented detail. There are two principal reasons why this approach reduces location errors. The first is that the use of differenced arrival times to solve for the vector separation of earthquakes removes from the earthquake location problem much of the error due to unmodeled velocity structure. The second reason, on which we focus in this article, is that waveform cross correlation can substantially reduce measurement error. While cross correlation has long been used to determine relative arrival times with subsample precision, we extend correlation measurements to less similar waveforms, and we introduce a general quantitative means to assess when correlation data provide an improvement over catalog phase picks. We apply the technique to local earthquake data from the Calaveras Fault in northern California. Tests for an example streak of 243 earthquakes demonstrate that relative arrival times with normalized cross correlation coefficients as low as ???70%, interevent separation distances as large as to 2 km, and magnitudes up to 3.5 as recorded on the Northern California Seismic Network are more precise than relative arrival times determined from catalog phase data. Also discussed are improvements made to the correlation technique itself. We find that for large time offsets, our implementation of time-domain cross correlation is often more robust and that it recovers more observations than the cross spectral approach. Longer time windows give better results than shorter ones. Finally, we explain how thresholds and empirical weighting functions may be derived to optimize the location procedure for any given region of interest, taking advantage of the respective strengths of diverse correlation and catalog phase data on different length scales.

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

PubMed

Hartmann, Anja; Ganzera, Markus

2015-11-01

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

Detection and quantification of cocaine and benzoylecgonine in meconium using solid phase extraction and UPLC/MS/MS.

PubMed

Gunn, Josh; Kriger, Scott; Terrell, Andrea R

2010-01-01

The simultaneous determination and quantification of cocaine and its major metabolite, benzoylecgonine, in meconium using UPLC-MS/MS is described. Ultra-performance liquid chromatography (UPLC) is an emerging analytical technique which draws upon the principles of chromatography to run separations at higher flow rates for increased speed, while simultaneously achieving superior resolution and sensitivity. Extraction of cocaine and benzoylecgonine from the homogenized meconium matrix was achieved with a preliminary protein precipitation or protein 'crash' employing cold acetonitrile, followed by a mixed mode solid phase extraction (SPE). Following elution from the SPE cartridge, eluents were dried down under nitrogen, reconstituted in 200 microL of DI water:acetonitrile (ACN) (75:25), and injected onto the UPLC/MS/MS for analysis. The increased speed and separation efficiency afforded by UPLC, allowed for the separation and subsequent quantification of both analytes in less than 2 min. Analytes were quantified using multiple reaction monitoring (MRM) and six-point calibration curves constructed in negative blood. Limits of detection for both analytes were 3 ng/g and the lower limit of quantitation (LLOQ) was 30 ng/g.

Application of Extended Kalman Filter in Persistant Scatterer Interferometry to Enhace the Accuracy of Unwrapping Process

NASA Astrophysics Data System (ADS)

Tavakkoli Estahbanat, A.; Dehghani, M.

2017-09-01

In interferometry technique, phases have been modulated between 0-2π. Finding the number of integer phases missed when they were wrapped is the main goal of unwrapping algorithms. Although the density of points in conventional interferometry is high, this is not effective in some cases such as large temporal baselines or noisy interferograms. Due to existing noisy pixels, not only it does not improve results, but also it leads to some unwrapping errors during interferogram unwrapping. In PS technique, because of the sparse PS pixels, scientists are confronted with a problem to unwrap phases. Due to the irregular data separation, conventional methods are sterile. Unwrapping techniques are divided in to path-independent and path-dependent in the case of unwrapping paths. A region-growing method which is a path-dependent technique has been used to unwrap PS data. In this paper an idea of EKF has been generalized on PS data. This algorithm is applied to consider the nonlinearity of PS unwrapping problem as well as conventional unwrapping problem. A pulse-pair method enhanced with singular value decomposition (SVD) has been used to estimate spectral shift from interferometric power spectral density in 7*7 local windows. Furthermore, a hybrid cost-map is used to manage the unwrapping path. This algorithm has been implemented on simulated PS data. To form a sparse dataset, A few points from regular grid are randomly selected and the RMSE of results and true unambiguous phases in presented to validate presented approach. The results of this algorithm and true unwrapped phases were completely identical.

3D fingerprint analysis using transmission-mode multi-wavelength digital holographic topography

NASA Astrophysics Data System (ADS)

Abeywickrema, Ujitha; Banerjee, Partha; Kota, Akash; Lakhtakia, Akhlesh; Swiontek, Stephen E.

2016-03-01

The analysis of fingerprints is important for biometric identification. Two-wavelength digital holographic interferometry is used to study the topography of various types of fingerprints. This topography depends on several conditions such as the temperature, time of the day, and the proportions of eccrine and sebaceous sweat. With two-wavelength holographic interferometry, surface information can be measured with a better accuracy compared to single-wavelength phase-retrieving techniques. Latent fingerprints on transparent glass, a forensically relevant substrate are first developed by the deposition of 50-1000-nm-thick columnar thin films, and then analyzed using the transmission-mode two-wavelength digital holographic technique. In this technique, a tunable Argon-ion laser (457.9 nm to 514.5 nm) is used and holograms are recorded on a CCD camera sequentially for several sets of two wavelengths. Then the phase is reconstructed for each wavelength, and the phase difference which corresponds to the synthetic wavelength (4 μm to 48 μm) is calculated. Finally, the topography is obtained by applying proper phase-unwrapping techniques to the phase difference. Interferometric setups that utilize light reflected from the surface of interest have several disadvantages such as the effect of multiple reflections as well as the effects of the tilt of the object and its shadow (for the Mach-Zehnder configuration). To overcome these drawbacks, digital holograms of fingerprints in a transmission geometry are used. An approximately in-line geometry employing a slightly tilted reference beam to facilitate separation of various diffraction orders during holographic reconstruction is employed.

Visualizing phase transition behavior of dilute stimuli responsive polymer solutions via Mueller matrix polarimetry.

PubMed

Narayanan, Amal; Chandel, Shubham; Ghosh, Nirmalya; De, Priyadarsi

2015-09-15

Probing volume phase transition behavior of superdiluted polymer solutions both micro- and macroscopically still persists as an outstanding challenge. In this regard, we have explored 4 × 4 spectral Mueller matrix measurement and its inverse analysis for excavating the microarchitectural facts about stimuli responsiveness of "smart" polymers. Phase separation behavior of thermoresponsive poly(N-isopropylacrylamide) (PNIPAM) and pH responsive poly(N,N-(dimethylamino)ethyl methacrylate) (PDMAEMA) and their copolymers were analyzed in terms of Mueller matrix derived polarization parameters, namely, depolarization (Δ), diattenuation (d), and linear retardance (δ). The Δ, d, and δ parameters provided useful information on both macro- and microstructural alterations during the phase separation. Additionally, the two step action ((i) breakage of polymer-water hydrogen bonding and (ii) polymer-polymer aggregation) at the molecular microenvironment during the cloud point generation was successfully probed via these parameters. It is demonstrated that, in comparison to the present techniques available for assessing the hydrophobic-hydrophilic switch over of simple stimuli-responsive polymers, Mueller matrix polarimetry offers an important advantage requiring a few hundred times dilute polymer solution (0.01 mg/mL, 1.1-1.4 μM) at a low-volume format.

Self-interaction of NPM1 modulates multiple mechanisms of liquid-liquid phase separation.

PubMed

Mitrea, Diana M; Cika, Jaclyn A; Stanley, Christopher B; Nourse, Amanda; Onuchic, Paulo L; Banerjee, Priya R; Phillips, Aaron H; Park, Cheon-Gil; Deniz, Ashok A; Kriwacki, Richard W

2018-02-26

Nucleophosmin (NPM1) is an abundant, oligomeric protein in the granular component of the nucleolus with roles in ribosome biogenesis. Pentameric NPM1 undergoes liquid-liquid phase separation (LLPS) via heterotypic interactions with nucleolar components, including ribosomal RNA (rRNA) and proteins which display multivalent arginine-rich linear motifs (R-motifs), and is integral to the liquid-like nucleolar matrix. Here we show that NPM1 can also undergo LLPS via homotypic interactions between its polyampholytic intrinsically disordered regions, a mechanism that opposes LLPS via heterotypic interactions. Using a combination of biophysical techniques, including confocal microscopy, SAXS, analytical ultracentrifugation, and single-molecule fluorescence, we describe how conformational changes within NPM1 control valency and switching between the different LLPS mechanisms. We propose that this newly discovered interplay between multiple LLPS mechanisms may influence the direction of vectorial pre-ribosomal particle assembly within, and exit from the nucleolus as part of the ribosome biogenesis process.

Cross-stacked carbon nanotubes assisted self-separation of free-standing GaN substrates by hydride vapor phase epitaxy

NASA Astrophysics Data System (ADS)

Wei, Tongbo; Yang, Jiankun; Wei, Yang; Huo, Ziqiang; Ji, Xiaoli; Zhang, Yun; Wang, Junxi; Li, Jinmin; Fan, Shoushan

2016-06-01

We report a novel method to fabricate high quality 2-inch freestanding GaN substrate grown on cross-stacked carbon nanotubes (CSCNTs) coated sapphire by hydride vapor phase epitaxy (HVPE). As nanoscale masks, these CSCNTs can help weaken the interface connection and release the compressive stress by forming voids during fast coalescence and also block the propagation of threading dislocations (TDs). During the cool-down process, thermal stress-induced cracks are initiated at the CSCNTs interface with the help of air voids and propagated all over the films which leads to full self-separation of FS-GaN substrate. Raman and photoluminescence spectra further reveal the stress relief and crystalline improvement of GaN with CSCNTs. It is expected that the efficient, low cost and mass-producible technique may enable new applications for CNTs in nitride optoelectronic fields.

Recovery of biotechnological products using aqueous two phase systems.

PubMed

Phong, Win Nee; Show, Pau Loke; Chow, Yin Hui; Ling, Tau Chuan

2018-04-16

Aqueous two-phase system (ATPS) has been suggested as a promising separation tool in the biotechnological industry. This liquid-liquid extraction technique represents an interesting advance in downstream processing due to several advantages such as simplicity, rapid separation, efficiency, economy, flexibility and biocompatibility. Up to date, a range of biotechnological products have been successfully recovered from different sources with high yield using ATPS-based strategy. In view of the important potential contribution of the ATPS in downstream processing, this review article aims to provide latest information about the application of ATPS in the recovery of various biotechnological products in the past 7 years (2010-2017). Apart from that, the challenges as well as the possible future work and outlook of the ATPS-based recovery method have also been presented in this review article. Copyright © 2018 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

Cross-stacked carbon nanotubes assisted self-separation of free-standing GaN substrates by hydride vapor phase epitaxy.

PubMed

Wei, Tongbo; Yang, Jiankun; Wei, Yang; Huo, Ziqiang; Ji, Xiaoli; Zhang, Yun; Wang, Junxi; Li, Jinmin; Fan, Shoushan

2016-06-24

We report a novel method to fabricate high quality 2-inch freestanding GaN substrate grown on cross-stacked carbon nanotubes (CSCNTs) coated sapphire by hydride vapor phase epitaxy (HVPE). As nanoscale masks, these CSCNTs can help weaken the interface connection and release the compressive stress by forming voids during fast coalescence and also block the propagation of threading dislocations (TDs). During the cool-down process, thermal stress-induced cracks are initiated at the CSCNTs interface with the help of air voids and propagated all over the films which leads to full self-separation of FS-GaN substrate. Raman and photoluminescence spectra further reveal the stress relief and crystalline improvement of GaN with CSCNTs. It is expected that the efficient, low cost and mass-producible technique may enable new applications for CNTs in nitride optoelectronic fields.

Cross-stacked carbon nanotubes assisted self-separation of free-standing GaN substrates by hydride vapor phase epitaxy

PubMed Central

Wei, Tongbo; Yang, Jiankun; Wei, Yang; Huo, Ziqiang; Ji, Xiaoli; Zhang, Yun; Wang, Junxi; Li, Jinmin; Fan, Shoushan

2016-01-01

We report a novel method to fabricate high quality 2-inch freestanding GaN substrate grown on cross-stacked carbon nanotubes (CSCNTs) coated sapphire by hydride vapor phase epitaxy (HVPE). As nanoscale masks, these CSCNTs can help weaken the interface connection and release the compressive stress by forming voids during fast coalescence and also block the propagation of threading dislocations (TDs). During the cool-down process, thermal stress-induced cracks are initiated at the CSCNTs interface with the help of air voids and propagated all over the films which leads to full self-separation of FS-GaN substrate. Raman and photoluminescence spectra further reveal the stress relief and crystalline improvement of GaN with CSCNTs. It is expected that the efficient, low cost and mass-producible technique may enable new applications for CNTs in nitride optoelectronic fields. PMID:27340030

Identification of procyanidins in cocoa (Theobroma cacao) and chocolate using high-performance liquid chromatography/mass spectrometry.

PubMed

Hammerstone, J F; Lazarus, S A; Mitchell, A E; Rucker, R; Schmitz, H H

1999-02-01

Monomeric and oligomeric procyanidins present in cocoa and chocolate were separated and identified using a modified normal-phase high-performance liquid chromatography (HPLC) method coupled with on-line mass spectrometry (MS) analysis using an atmospheric pressure ionization electrospray chamber. The chromatographic separation was achieved using a silica stationary phase in combination with a gradient ascending in polarity. This qualitative report confirms the presence of a complex series of procyanidins in raw cocoa and certain chocolates using HPLC/MS techniques. Although both cocoa and chocolate contained monomeric and oligomeric procyanidin units 2-10, only use of negative mode provided MS data for the higher oligomers (i.e., >pentamer). Application of this method for qualitative analysis of proanthocyanidins in other food products and confirmation of this method as a reliable quantitative tool for determining levels of procyanidins in cocoa, chocolate, and other food products are currently being investigated.

Ultrasound-assisted analyte extraction for the determination of sulfate and elemental sulfur in zinc sulfide by different liquid chromatography techniques.

PubMed

Dash, K; Thangavel, S; Krishnamurthy, N V; Rao, S V; Karunasagar, D; Arunachalam, J

2005-04-01

The speciation and determination of sulfate (SO4(2-)) and elemental sulfur (S degree) in zinc sulfide (ZnS) using ion-chromatography (IC) and reversed-phase liquid chromatography (RPLC) respectively is described. Three sample pretreatment approaches were employed with the aim of determining sulfate: (i) conventional water extraction of the analyte; (ii) solid-liquid aqueous extraction with an ultrasonic probe; and (iii) elimination of the zinc sulfide matrix via ion-exchange dissolution (IED). The separation of sulfate was carried out by an anion-exchange column (IonPac AS17), followed by suppressed conductivity detection. Elemental sulfur was extracted ultrasonically from the acid treated sample solution into chloroform and separated on a reversed phase HPLC column equipped with a diode array detector (DAD) at 264 nm. The achievable solid detection limits for sulfate and sulfur were 35 and 10 microg g(-1) respectively.

Nanoscale phase separation of antiferromagnetic order and superconductivity in K0.75Fe1.75Se2

PubMed Central

Yuan, R. H.; Dong, T.; Song, Y. J.; Zheng, P.; Chen, G. F.; Hu, J. P.; Li, J. Q.; Wang, N. L.

2012-01-01

We report an in-plane optical spectroscopy study on the iron-selenide superconductor K0.75Fe1.75Se2. The measurement revealed the development of a sharp reflectance edge below Tc at frequency much smaller than the superconducting energy gap on a relatively incoherent electronic background, a phenomenon which was not seen in any other Fe-based superconductors so far investigated. Furthermore, the feature could be noticeably suppressed and shifted to lower frequency by a moderate magnetic field. Our analysis indicates that this edge structure arises from the development of a Josephson-coupling plasmon in the superconducting condensate. Together with the transmission electron microscopy analysis, our study yields compelling evidence for the presence of nanoscale phase separation between superconductivity and magnetism. The results also enable us to understand various seemingly controversial experimental data probed from different techniques. PMID:22355735

Portable microfluidic platform for real-time, high sensitive detection and identification of trichloroethylene and other organochloride compounds

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

Jensen, Erik

In this successful SBIR Phase II effort, HJ Science & Technology, Inc. has designed and built a novel portable instrument capable of performing automated aqueous organochloride (chlorinated solvent) speciation analysis for environmental monitoring at DoE sites. Our technique employs performing organochloride conjugation, labeling the conjugate with an efficient fluorophore, and performing on-chip capillary electrophoresis separation with laser induced fluorescence detection. The key component of the portable instrument is a novel microfluidic chip capable of complete “end-to-end” automation of sample preparation, conjugation, labeling, and μCE separation and detection. In addition, the Phase II prototype includes key supporting instrumentation such as themore » optical module, pneumatic manifold, electronics, software, etc. As such, we have achieved all of the following 4 Phase II technical objectives: 1) Further refine and optimize the “on-chip” automation of the organochloride conjugation and labeling protocol, 2) Further improve the microfluidic chip fabrication process and the pneumatic manifold design in order to address issues related to performance consistency, product yield, performance reliability, and user friendliness, 3) Design and build the supporting components of the Phase II prototype including optical module, electronics, and software, and 4) Assemble the Phase II prototype hardware.« less

Film thickness dependence of phase separation and dewetting behaviors in PMMA/SAN blend films.

PubMed

You, Jichun; Liao, Yonggui; Men, Yongfeng; Shi, Tongfei; An, Lijia

2010-09-21

Film thickness dependence of complex behaviors coupled by phase separation and dewetting in blend [poly(methyl methacrylate) (PMMA) and poly(styrene-ran-acrylonitrile) (SAN)] films on silicon oxide substrate at 175 °C was investigated by grazing incidence ultrasmall-angle X-ray scattering (GIUSAX) and in situ atomic force microscopy (AFM). It was found that the dewetting pathway was under the control of the parameter U(q0)/E, which described the initial amplitude of the surface undulation and original thickness of film, respectively. Furthermore, our results showed that interplay between phase separation and dewetting depended crucially on film thickness. Three mechanisms including dewetting-phase separation/wetting, dewetting/wetting-phase separation, and phase separation/wetting-pseudodewetting were discussed in detail. In conclusion, it is relative rates of phase separation and dewetting that dominate the interplay between them.

Frequency-domain nonlinear optics in two-dimensionally patterned quasi-phase-matching media.

PubMed

Phillips, C R; Mayer, B W; Gallmann, L; Keller, U

2016-07-11

Advances in the amplification and manipulation of ultrashort laser pulses have led to revolutions in several areas. Examples include chirped pulse amplification for generating high peak-power lasers, power-scalable amplification techniques, pulse shaping via modulation of spatially-dispersed laser pulses, and efficient frequency-mixing in quasi-phase-matched nonlinear crystals to access new spectral regions. In this work, we introduce and demonstrate a new platform for nonlinear optics which has the potential to combine these separate functionalities (pulse amplification, frequency transfer, and pulse shaping) into a single monolithic device that is bandwidth- and power-scalable. The approach is based on two-dimensional (2D) patterning of quasi-phase-matching (QPM) gratings combined with optical parametric interactions involving spatially dispersed laser pulses. Our proof of principle experiment demonstrates this technique via mid-infrared optical parametric chirped pulse amplification of few-cycle pulses. Additionally, we present a detailed theoretical and numerical analysis of such 2D-QPM devices and how they can be designed.

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

PubMed

Taguchi, Kaori; Fukusaki, Eiichiro; Bamba, Takeshi

2014-10-03

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

The Numerical Technique for the Landslide Tsunami Simulations Based on Navier-Stokes Equations

NASA Astrophysics Data System (ADS)

Kozelkov, A. S.

2017-12-01

The paper presents an integral technique simulating all phases of a landslide-driven tsunami. The technique is based on the numerical solution of the system of Navier-Stokes equations for multiphase flows. The numerical algorithm uses a fully implicit approximation method, in which the equations of continuity and momentum conservation are coupled through implicit summands of pressure gradient and mass flow. The method we propose removes severe restrictions on the time step and allows simulation of tsunami propagation to arbitrarily large distances. The landslide origin is simulated as an individual phase being a Newtonian fluid with its own density and viscosity and separated from the water and air phases by an interface. The basic formulas of equation discretization and expressions for coefficients are presented, and the main steps of the computation procedure are described in the paper. To enable simulations of tsunami propagation across wide water areas, we propose a parallel algorithm of the technique implementation, which employs an algebraic multigrid method. The implementation of the multigrid method is based on the global level and cascade collection algorithms that impose no limitations on the paralleling scale and make this technique applicable to petascale systems. We demonstrate the possibility of simulating all phases of a landslide-driven tsunami, including its generation, propagation and uprush. The technique has been verified against the problems supported by experimental data. The paper describes the mechanism of incorporating bathymetric data to simulate tsunamis in real water areas of the world ocean. Results of comparison with the nonlinear dispersion theory, which has demonstrated good agreement, are presented for the case of a historical tsunami of volcanic origin on the Montserrat Island in the Caribbean Sea.

Microextraction techniques for the determination of volatile and semivolatile organic compounds from plants: a review.

PubMed

Yang, Cui; Wang, Juan; Li, Donghao

2013-10-17

Vegetables and fruits are necessary for human health, and traditional Chinese medicine that uses plant materials can cure diseases. Thus, understanding the composition of plant matrix has gained increased attention in recent years. Since plant matrix is very complex, the extraction, separation and quantitation of these chemicals are challenging. In this review we focus on the microextraction techniques used in the determination of volatile and semivolatile organic compounds (such as esters, alcohols, aldehydes, hydrocarbons, ketones, terpenes, sesquiterpene, phenols, acids, plant secondary metabolites and pesticides) from plants (e.g., fruits, vegetables, medicinal plants, tree leaves, etc.). These microextraction techniques include: solid phase microextraction (SPME), stir-bar sorptive extraction (SBSE), single drop microextraction (SDME), hollow fiber liquid phase microextraction (HF-LPME), dispersive liquid liquid microextraction (DLLME), and gas purge microsyringe extraction (GP-MSE). We have taken into consideration papers published from 2008 to the end of January 2013, and provided critical and interpretative review on these techniques, and formulated future trends in microextraction for the determination of volatile and semivolatile compounds from plants. Copyright © 2013 Elsevier B.V. All rights reserved.

4D measurements of biological and synthetic structures using a dynamic interferometer

NASA Astrophysics Data System (ADS)

Toto-Arellano, Noel-Ivan

2017-12-01

Considering the deficiency of time elapsed for phase-stepping interferometric techniques and the need of developing non-contact and on-line measurement with high accuracy, a single-shot phase-shifting triple-interferometer (PSTI) is developed for analysis of characteristics of transparent structures and optical path difference (OPD) measurements. In the proposed PSTI, coupled three interferometers which generate four interference patterns, and a polarizer array is used as phase shifters to produce four spatially separated interferograms with π/2-phase shifts, which are recorded in a single capture by a camera. The configuration of the PSTI allows dynamic measurements (4D measurements) and does not require vibration isolation. We have applied the developed system to examine the size and OPD of cells, and the slope of thin films

Cell separation by immunoaffinity partitioning with polyethylene glycol-modified Protein A in aqueous polymer two-phase systems

NASA Technical Reports Server (NTRS)

Karr, Laurel J.; Van Alstine, James M.; Snyder, Robert S.; Shafer, Steven G.; Harris, J. Milton

1988-01-01

Previous work has shown that polyethylene glycol (PEG)-bound antibodies can be used as affinity ligands in PEG-dextran two-phase systems to provide selective partitioning of cells to the PEG-rich phase. In the present work it is shown that immunoaffinity partitioning can be simplified by use of PEG-modified Protein A which complexes with unmodified antibody and cells and shifts their partitioning into the PEG-rich phase, thus eliminating the need to prepare a PEG-modified antibody for each cell type. In addition, the paper provides a more rigorous test of the original technique with PEG-bound antibodies by showing that it is effective at shifting the partitioning of either cell type of a mixture of two cell populations.

ALMA long baseline phase calibration using phase referencing

NASA Astrophysics Data System (ADS)

Asaki, Yoshiharu; Matsushita, Satoki; Fomalont, Edward B.; Corder, Stuartt A.; Nyman, Lars-Åke; Dent, William R. F.; Philips, Neil M.; Hirota, Akihiko; Takahashi, Satoko; Vila-Vilaro, Baltasar; Nikolic, Bojan; Hunter, Todd R.; Remijan, Anthony; Vlahakis, Catherine

2016-08-01

The Atacama Large Millimeter/submillimeter Array (ALMA) is the world's largest millimeter/submillimeter telescope and provides unprecedented sensitivities and spatial resolutions. To achieve the highest imaging capabilities, interferometric phase calibration for the long baselines is one of the most important subjects: The longer the baselines, the worse the phase stability becomes because of turbulent motions of the Earth's atmosphere, especially, the water vapor in the troposphere. To overcome this subject, ALMA adopts a phase correction scheme using a Water Vapor Radiometer (WVR) to estimate the amount of water vapor content along the antenna line of sight. An additional technique is phase referencing, in which a science target and a nearby calibrator are observed by turn by quickly changing the antenna pointing. We conducted feasibility studies of the hybrid technique with the WVR phase correction and the antenna Fast Switching (FS) phase referencing (WVR+FS phase correction) for the ALMA 16 km longest baselines in cases that (1) the same observing frequency both for a target and calibrator is used, and (2) higher and lower frequencies for a target and calibrator, respectively, with a typical switching cycle time of 20 s. It was found that the phase correction performance of the hybrid technique is promising where a nearby calibrator is located within roughly 3◦ from a science target, and that the phase correction with 20 s switching cycle time significantly improves the performance with the above separation angle criterion comparing to the 120 s switching cycle time. The currently trial phase calibration method shows the same performance independent of the observing frequencies. This result is especially important for the higher frequency observations because it becomes difficult to find a bright calibrator close to an arbitrary sky position. In the series of our experiments, it is also found that phase errors affecting the image quality come from not only the water vapor content in the lower troposphere but also a large structure of the atmosphere with a typical cell scale of a few tens of kilometers.

Development of porous lamellar poly(L-lactic acid) scaffolds by conventional injection molding process.

PubMed

Ghosh, Satyabrata; Viana, Júlio C; Reis, Rui L; Mano, João F

2008-07-01

A novel fabrication technique is proposed for the preparation of unidirectionally oriented, porous scaffolds by selective polymer leaching from lamellar structures created by conventional injection molding. The proof of the concept is implemented using a 50/50 wt.% poly(L-lactic acid)/poly(ethylene oxide) (PLLA/PEO) blend. With this composition, the PLLA and PEO blend is biphasic, containing a homogeneous PLLA/PEO phase and a PEO-rich phase. The two phases were structured using injection molding into well-defined alternating layers of homogeneous PLLA/PEO phase and PEO-rich phase. Leaching of water-soluble PEO from the PEO-rich phase produces macropores, and leaching of phase-separated PEO from the initially homogeneous PLLA/PEO phase produces micropores in the lamellae. Thus, scaffolds with a macroporous lamellar architecture with microporous walls can be produced. The lamellae are continuous along the flow direction, and a continuous lamellar thickness of less than 1 microm could be achieved. Porosities of 57-74% and pore sizes of around 50-100 microm can be obtained using this process. The tensile elastic moduli of the porous constructs were between 580 and 800 MPa. We propose that this organic-solvent-free method of preparing lamellar scaffolds with good mechanical properties, and the reproducibility associated with the injection molding technique, holds promise for a wide range of guided tissue engineering applications.

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

PubMed

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

2007-11-15

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

Accommodating subject and instrument variations in spectroscopic determinations

DOEpatents

Haas, Michael J [Albuquerque, NM; Rowe, Robert K [Corrales, NM; Thomas, Edward V [Albuquerque, NM

2006-08-29

A method and apparatus for measuring a biological attribute, such as the concentration of an analyte, particularly a blood analyte in tissue such as glucose. The method utilizes spectrographic techniques in conjunction with an improved instrument-tailored or subject-tailored calibration model. In a calibration phase, calibration model data is modified to reduce or eliminate instrument-specific attributes, resulting in a calibration data set modeling intra-instrument or intra-subject variation. In a prediction phase, the prediction process is tailored for each target instrument separately using a minimal number of spectral measurements from each instrument or subject.

[Developments in preparation and experimental method of solid phase microextraction fibers].

PubMed

Yi, Xu; Fu, Yujie

2004-09-01

Solid phase microextraction (SPME) is a simple and effective adsorption and desorption technique, which concentrates volatile or nonvolatile compounds from liquid samples or headspace of samples. SPME is compatible with analyte separation and detection by gas chromatography, high performance liquid chromatography, and other instrumental methods. It can provide many advantages, such as wide linear scale, low solvent and sample consumption, short analytical times, low detection limits, simple apparatus, and so on. The theory of SPME is introduced, which includes equilibrium theory and non-equilibrium theory. The novel development of fiber preparation methods and relative experimental techniques are discussed. In addition to commercial fiber preparation, different newly developed fabrication techniques, such as sol-gel, electronic deposition, carbon-base adsorption, high-temperature epoxy immobilization, are presented. Effects of extraction modes, selection of fiber coating, optimization of operating conditions, method sensitivity and precision, and systematical automation, are taken into considerations in the analytical process of SPME. A simple perspective of SPME is proposed at last.

Bulk heterojunction thin film formation by single and dual feed ultrasonic spray method for application in organic solar cells

NASA Astrophysics Data System (ADS)

Marathe, D. M.; Tarkas, H. S.; Mahajan, M. S.; Lonkar, G. S.; Tak, S. R.; Sali, J. V.

2016-09-01

We here present a way of preparing the polymer: fullerene BHJ using dual feed method which can lead to formation of pure phases. In this report, we present results of our initial experiments in this direction. The effect of process parameters on the thickness and surface roughness of the active layer has been discussed. The structural and optical properties have been studied using the optical microscope, UV—visible spectroscopy and photoluminescence spectroscopy. Significant PL quenching indicates efficient charge separation in the BHJ formed using this technique. We have also compared the BHJ thin films prepared with this dual feed ultrasonic technique with the single feed spray method. The BHJ formed using this technique has been used as an active layer in OSC. supported by the University Grants Commission, New Delhi, under Faculty Improvement Programme (No. 33-02/12(WRO) Dt.19.03.2013) and the Special Assistance Programme (530/2/DRS/2010(SAP-I)) Phase-II.

Urban Monitoring Based on SENTINEL-1 Data Using Permanent Scatterer Interferometry and SAR Tomography

NASA Astrophysics Data System (ADS)

Crosetto, M.; Budillon, A.; Johnsy, A.; Schirinzi, G.; Devanthéry, N.; Monserrat, O.; Cuevas-González, M.

2018-04-01

A lot of research and development has been devoted to the exploitation of satellite SAR images for deformation measurement and monitoring purposes since Differential Interferometric Synthetic Apertura Radar (InSAR) was first described in 1989. In this work, we consider two main classes of advanced DInSAR techniques: Persistent Scatterer Interferometry and Tomographic SAR. Both techniques make use of multiple SAR images acquired over the same site and advanced procedures to separate the deformation component from the other phase components, such as the residual topographic component, the atmospheric component, the thermal expansion component and the phase noise. TomoSAR offers the advantage of detecting either single scatterers presenting stable proprieties over time (Persistent Scatterers) and multiple scatterers interfering within the same range-azimuth resolution cell, a significant improvement for urban areas monitoring. This paper addresses a preliminary inter-comparison of the results of both techniques, for a test site located in the metropolitan area of Barcelona (Spain), where interferometric Sentinel-1 data were analysed.

Does Deprivation Damage? A Study of the Incidence of Deprivation in Lothian and of Its Influence on Young People's Educational Attainment.

ERIC Educational Resources Information Center

Garner, Catherine L.

This report uses newly developed techniques of statistical analysis to assess the separate and joint influences of home, school, and neighborhood in Lothian (Scotland, United Kingdom) and to show that deprivation in each of these areas depresses young people's educational attainment. The results reported here come from the first phase of a…

Synthesis of a mixed-model stationary phase derived from glutamine for HPLC separation of structurally different biologically active compounds: HILIC and reversed-phase applications.

PubMed

Aral, Tarık; Aral, Hayriye; Ziyadanoğulları, Berrin; Ziyadanoğulları, Recep

2015-01-01

A novel mixed-mode stationary phase was synthesised starting from N-Boc-glutamine, aniline and spherical silica gel (4 µm, 60 Å). The prepared stationary phase was characterized by IR and elemental analysis. The new stationary phase bears an embedded amide group into phenyl ring, highly polar a terminal amide group and non-polar groups (phenyl and alkyl groups). At first, this new mixed-mode stationary phase was used for HILIC separation of four nucleotides and five nucleosides. The effects of different separation conditions, such as pH value, mobile phase and temperature, on the separation process were investigated. The optimum separation for nucleotides was achieved using HILIC isocratic elution with aqueous mobile phase and acetonitrile with 20°C column temperature. Under these conditions, the four nucleotides could be separated and detected at 265 nm within 14 min. Five nucleosides were separated under HILIC isocratic elution with aqueous mobile phase containing pH=3.25 phosphate buffer (10mM) and acetonitrile with 20°C column temperature and detected at 265 nm within 14 min. Chromatographic parameters as retention factor, selectivity, theoretical plate number and peak asymmetry factor were calculated for the effect of temperature and water content in mobile phase on the separation process. The new column was also tested for nucleotides and nucleosides mixture and six analytes were separated in 10min. The chromatographic behaviours of these polar analytes on the new mixed-model stationary phase were compared with those of HILIC columns under similar conditions. Further, phytohormones and phenolic compounds were separated in order to see influence of the new stationary phase in reverse phase conditions. Eleven plant phytohormones were separated within 13 min using RP-HPLC gradient elution with aqueous mobile phase containing pH=2.5 phosphate buffer (10mM) and acetonitrile with 20°C column temperature and detected at 230 or 278 nm. The best separation conditions for seven phenolic compounds was also achieved using reversed-phase HPLC gradient elution with aqueous mobile phase containing pH=2.5 phosphate buffer (10mM) and acetonitrile with 20°C column temperature and seven phenolic compounds could be separated and detected at 230 nm within 16 min. Copyright © 2014 Elsevier B.V. All rights reserved.

Broadband quantitative phase microscopy with extended field of view using off-axis interferometric multiplexing.

PubMed

Girshovitz, Pinhas; Frenklach, Irena; Shaked, Natan T

2015-11-01

We propose a new portable imaging configuration that can double the field of view (FOV) of existing off-axis interferometric imaging setups, including broadband off-axis interferometers. This configuration is attached at the output port of the off-axis interferometer and optically creates a multiplexed interferogram on the digital camera, which is composed of two off-axis interferograms with straight fringes at orthogonal directions. Each of these interferograms contains a different FOV of the imaged sample. Due to the separation of these two FOVs in the spatial-frequency domain, they can be fully reconstructed separately, while obtaining two complex wavefronts from the sample at once. Since the optically multiplexed off-axis interferogram is recorded by the camera in a single exposure, fast dynamics can be recorded with a doubled imaging area. We used this technique for quantitative phase microscopy of biological samples with extended FOV. We demonstrate attaching the proposed module to a diffractive phase microscopy interferometer, illuminated by a broadband light source. The biological samples used for the experimental demonstrations include microscopic diatom shells, cancer cells, and flowing blood cells.

Chromium doped nano-phase separated yttria-alumina-silica glass based optical fiber preform: fabrication and characterization

NASA Astrophysics Data System (ADS)

Dutta, Debjit; Dhar, Anirban; Das, Shyamal; Bysakh, Sandip; Kir'yanov, Alexandar; Paul, Mukul Chandra

2015-06-01

Transition metal (TM) doping in silica core optical fiber is one of the research area which has been studied for long time and Chromium (Cr) doping specially attracts a lot of research interest due to their broad emission band covering U, C and L band with many potential application such as saturable absorber or broadband amplifier etc. This paper present fabrication of Cr doped nano-phase separated silica fiber within yttria-alumina-silica core glass through conventional Modified Chemical Vapor Deposition (MCVD) process coupled with solution doping technique along with different material and optical characterization. For the first time scanning electron microscope (SEM) / energy dispersive X-ray (EDX) analysis of porous soot sample and final preform has been utilized to investigate incorporation mechanism of Crions with special emphasis on Cr-species evaporation at different stages of fabrication. We also report that optimized annealing condition of our fabricated preform exhibited enhanced fluorescence emission and a broad band within 550- 800 nm wavelength region under pumping at 532 nm wavelength due to nano-phase restructuration.

Pushing the speed limit in enantioselective supercritical fluid chromatography.

PubMed

Regalado, Erik L; Welch, Christopher J

2015-08-01

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

Bead mediated separation of microparticles in droplets.

PubMed

Wang, Sida; Sung, Ki-Joo; Lin, Xiaoxia Nina; Burns, Mark A

2017-01-01

Exchange of components such as particles and cells in droplets is important and highly desired in droplet microfluidic assays, and many current technologies use electrical or magnetic fields to accomplish this process. Bead-based microfluidic techniques offer an alternative approach that uses the bead's solid surface to immobilize targets like particles or biological material. In this paper, we demonstrate a bead-based technique for exchanging droplet content by separating fluorescent microparticles in a microfluidic device. The device uses posts to filter surface-functionalized beads from a droplet and re-capture the filtered beads in a new droplet. With post spacing of 7 μm, beads above 10 μm had 100% capture efficiency. We demonstrate the efficacy of this system using targeted particles that bind onto the functionalized beads and are, therefore, transferred from one solution to another in the device. Binding capacity tests performed in the bulk phase showed an average binding capacity of 5 particles to each bead. The microfluidic device successfully separated the targeted particles from the non-targeted particles with up to 98% purity and 100% yield.

Bead mediated separation of microparticles in droplets

PubMed Central

Sung, Ki-Joo; Lin, Xiaoxia Nina; Burns, Mark A.

2017-01-01

Exchange of components such as particles and cells in droplets is important and highly desired in droplet microfluidic assays, and many current technologies use electrical or magnetic fields to accomplish this process. Bead-based microfluidic techniques offer an alternative approach that uses the bead’s solid surface to immobilize targets like particles or biological material. In this paper, we demonstrate a bead-based technique for exchanging droplet content by separating fluorescent microparticles in a microfluidic device. The device uses posts to filter surface-functionalized beads from a droplet and re-capture the filtered beads in a new droplet. With post spacing of 7 μm, beads above 10 μm had 100% capture efficiency. We demonstrate the efficacy of this system using targeted particles that bind onto the functionalized beads and are, therefore, transferred from one solution to another in the device. Binding capacity tests performed in the bulk phase showed an average binding capacity of 5 particles to each bead. The microfluidic device successfully separated the targeted particles from the non-targeted particles with up to 98% purity and 100% yield. PMID:28282412

Capillary electrophoresis for drug analysis

NASA Astrophysics Data System (ADS)

Lurie, Ira S.

1999-02-01

Capillary electrophoresis (CE) is a high resolution separation technique which is amenable to a wide variety of solutes, including compounds which are thermally degradable, non-volatile and highly polar, and is therefore well suited for drug analysis. Techniques which have been used in our laboratory include electrokinetic chromatography (ECC), free zone electrophoresis (CZE) and capillary electrochromatography (CEC). ECC, which uses a charged run buffer additive which migrates counter to osmotic flow, is excellent for many applications, including, drug screening and analyses of heroin, cocaine and methamphetamine samples. ECC approaches include the use of micelles and charged cyclodextrins, which allow for the separation of complex mixtures. Simultaneous separation of acidic, neutral and basic solutes and the resolution of optical isomers and positional isomers are possible. CZE has been used for the analysis of small ions (cations and anions) in heroin exhibits. For the ECC and CZE experiments performed in our laboratory, uncoated capillaries were used. In contrast, CEC uses capillaries packed with high performance liquid chromatography stationary phases, and offers both high peak capacities and unique selectivities. Applications include the analysis of cannabinoids and drug screening. Although CE suffers from limited concentration sensitivity, it is still applicable to trace analysis of drug samples, especially when using injection techniques such as stacking, or detection schemes such as laser induced fluorescence and extended pathlength UV.

Molecular separations using nanostructured porous thin films fabricated by glancing angle deposition

NASA Astrophysics Data System (ADS)

Bezuidenhout, Louis Wentzel

Biomolecular separation techniques are an enabling technology that indirectly in.uence many aspects of our lives. Advances have led to faster analyses, reduced costs, higher specificity, and new analytical techniques, impacting areas such as health care, environmental monitoring, polymer sciences, agriculture, and nutrition. Further development of separations technology is anticipated to follow the path of computing technology such that miniaturization through the development of microfluidics technology, lab-on-a-chip systems, and other integrative, multi-component systems will further extend our analysis capabilities. Creation of new and improvement of existing separation technologies is an integral part of the pathway to miniaturized systems. the work of this thesis investigates molecular separations using porous nanostructured films fabricated by the thin film process glancing angle deposition (GLAD). Structural architecture, pore size and shape, and film density can be finely controlled to produce high-surface area thin films with engineered morphology. The characteristic size scales and structural control of GLAD films are well-suited to biomolecules and separation techniques, motivating investigation into the utility and performance of GLAD films for biomolecular separations. This project consisted of three phases. First, chromatographic separation of dye molecules on silica GLAD films was demonstrated by thin layer chromatography Direct control of film nanostructure altered the separation characteristics; most strikingly, anisotropic structures provided two-dimensional analyte migration. Second, nanostructures made with GLAD were integrated in PDMS microfluidic channels using a sacrificial etching process; DNA molecules (10/48 kbp and 6/10/20 kbp mixtures) were electrophoretically separated on a microfluidic chip using a porous bed of SiO2 vertical posts. Third, mass spectrometry of proteins and drugs in the mass range of 100-1300 m/z was performed using laser desorption/ionization (LDI) on silicon GLAD films, and the influence of film thickness, porosity, structure, and substrate on performance was characterized. The application of GLAD nanostructured thin films to biomolecular separations is demonstrated and validated in this thesis. Chromatographic separation of dye molecules, electrophoretic separation of DNA molecules, and mass spectrometric isolation of small proteins and drug molecules by laser desorption ionization were demonstrated using GLAD films. All three methods yielded promising results and establish GLAD as a potential technology for biomolecular separations.

High quality self-separated GaN crystal grown on a novel nanoporous template by HVPE.

PubMed

Huo, Qin; Shao, Yongliang; Wu, Yongzhong; Zhang, Baoguo; Hu, Haixiao; Hao, Xiaopeng

2018-02-16

In this study, a novel nanoporous template was obtained by a two-step etching process from MOCVD-GaN/Al 2 O 3 (MGA) with electrochemical etching sequentially followed by chemical wet etching. The twice-etched MOCVD-GaN/Al 2 O 3 (TEMGA) templates were utilized to grow GaN crystals by hydride vapor phase epitaxy (HVPE) method. The GaN crystals were separated spontaneously from the TEMGA template with the assistance of voids formed by the etched nanopores. Several techniques were utilized to characterize the quality of the free-standing GaN crystals obtained from the TEMGA template. Results showed that the quality of the as-obtained GaN crystals was improved obviously compared with those grown on the MGA. This convenient technique can be applied to grow high-quality free-standing GaN crystals.

Optical trapping for complex fluid microfluidics

NASA Astrophysics Data System (ADS)

Vestad, Tor; Oakey, John; Marr, David W. M.

2004-10-01

Many proposed applications of microfluidics involve the manipulation of complex fluid mixtures such as blood or bacterial suspensions. To sort and handle the constituent particles within these suspensions, we have developed a miniaturized automated cell sorter using optical traps. This microfluidic cell sorter offers the potential to perform chip-top microbiology more rapidly and with less associated hardware and preparation time than other techniques currently available. To realize the potential of this technology in practical clinical and consumer lab-on-a-chip devices however, microscale control of not only particulates but also the fluid phase must be achieved. To address this, we have developed a mechanical fluid control scheme that integrates well with our optical separations approach. We demonstrate here a combined technique, one that employs both mechanical actuation and optical trapping for the precise control of complex suspensions. This approach enables both cell and particle separations as well as the subsequent fluid control required for the completion of complex analyses.

New signal processing technique for density profile reconstruction using reflectometry.

PubMed

Clairet, F; Ricaud, B; Briolle, F; Heuraux, S; Bottereau, C

2011-08-01

Reflectometry profile measurement requires an accurate determination of the plasma reflected signal. Along with a good resolution and a high signal to noise ratio of the phase measurement, adequate data analysis is required. A new data processing based on time-frequency tomographic representation is used. It provides a clearer separation between multiple components and improves isolation of the relevant signals. In this paper, this data processing technique is applied to two sets of signals coming from two different reflectometer devices used on the Tore Supra tokamak. For the standard density profile reflectometry, it improves the initialization process and its reliability, providing a more accurate profile determination in the far scrape-off layer with density measurements as low as 10(16) m(-1). For a second reflectometer, which provides measurements in front of a lower hybrid launcher, this method improves the separation of the relevant plasma signal from multi-reflection processes due to the proximity of the plasma.

Headspace techniques in foods, fragrances and flavors: an overview.

PubMed

Rouseff, R; Cadwallader, K

2001-01-01

Headspace techniques have traditionally involved the collection of volatiles in the vapor state under either dynamic or static conditions as a means of determining concentrations in the product of interest. A brief overview of contemporary headspace applications and recent innovations are presented from the literature and Chapters in this book. New approaches used to concentrate volatiles under static conditions such as solid phase micro extraction, SPME, are examined. Advances in purge and trap applications and automation are also presented. Innovative methods of evaluating headspace volatiles using solid state sensor arrays (electronic noses) or mass spectrometers without prior separation are referenced. Numerous food and beverage headspace techniques are also reviewed. Advantages, limitations and alternatives to headspace analysis are presented.

Temperature-enhanced alumina HPLC method for the analysis of wax esters, sterol esters, and methyl esters.

PubMed

Moreau, Robert A; Kohout, Karen; Singh, Vijay

2002-12-01

Previous attempts at separating nonpolar lipid esters (including wax esters, sterol esters, and methyl esters) have achieved only limited success. Among the several normal-phase methods tested, a single recent report of a method employing an alumina column at 30 degrees C with a binary gradient system was the most promising. In the current study, modification of the alumina method by increasing the column temperature to 75 degrees C improved the separation of standards of wax esters and sterol esters. Elevated column temperature also enhanced the separation of FAME with differing degrees of unsaturation. Evidence was also presented to indicate that the method similarly separated phytosterol esters, based on their levels of unsaturation. With the increased interest in phytosterol- and phytostanol-ester enriched functional foods, this method should provide a technique to characterize and compare these products.

Improving chemical shift encoding‐based water–fat separation based on a detailed consideration of magnetic field contributions

PubMed Central

Ruschke, Stefan; Eggers, Holger; Meineke, Jakob; Rummeny, Ernst J.; Karampinos, Dimitrios C.

2018-01-01

Purpose To improve the robustness of existing chemical shift encoding‐based water–fat separation methods by incorporating a priori information of the magnetic field distortions in complex‐based water–fat separation. Methods Four major field contributions are considered: inhomogeneities of the scanner magnet, the shim field, an object‐based field map estimate, and a residual field. The former two are completely determined by spherical harmonic expansion coefficients directly available from the magnetic resonance (MR) scanner. The object‐based field map is forward simulated from air–tissue interfaces inside the field of view (FOV). The missing residual field originates from the object outside the FOV and is investigated by magnetic field simulations on a numerical whole body phantom. In vivo the spatially linear first‐order component of the residual field is estimated by measuring echo misalignments after demodulation of other field contributions resulting in a linear residual field. Gradient echo datasets of the cervical and the ankle region without and with shimming were acquired, where all four contributions were incorporated in the water–fat separation with two algorithms from the ISMRM water–fat toolbox and compared to water–fat separation with less incorporated field contributions. Results Incorporating all four field contributions as demodulation steps resulted in reduced temporal and spatial phase wraps leading to almost swap‐free water–fat separation results in all datasets. Conclusion Demodulating estimates of major field contributions reduces the phase evolution to be driven by only small differences in local tissue susceptibility, which supports the field smoothness assumption of existing water–fat separation techniques. PMID:29424458

Matrix product state representation of quasielectron wave functions

NASA Astrophysics Data System (ADS)

Kjäll, J.; Ardonne, E.; Dwivedi, V.; Hermanns, M.; Hansson, T. H.

2018-05-01

Matrix product state techniques provide a very efficient way to numerically evaluate certain classes of quantum Hall wave functions that can be written as correlators in two-dimensional conformal field theories. Important examples are the Laughlin and Moore-Read ground states and their quasihole excitations. In this paper, we extend the matrix product state techniques to evaluate quasielectron wave functions, a more complex task because the corresponding conformal field theory operator is not local. We use our method to obtain density profiles for states with multiple quasielectrons and quasiholes, and to calculate the (mutual) statistical phases of the excitations with high precision. The wave functions we study are subject to a known difficulty: the position of a quasielectron depends on the presence of other quasiparticles, even when their separation is large compared to the magnetic length. Quasielectron wave functions constructed using the composite fermion picture, which are topologically equivalent to the quasielectrons we study, have the same problem. This flaw is serious in that it gives wrong results for the statistical phases obtained by braiding distant quasiparticles. We analyze this problem in detail and show that it originates from an incomplete screening of the topological charges, which invalidates the plasma analogy. We demonstrate that this can be remedied in the case when the separation between the quasiparticles is large, which allows us to obtain the correct statistical phases. Finally, we propose that a modification of the Laughlin state, that allows for local quasielectron operators, should have good topological properties for arbitrary configurations of excitations.

Rapid separation of beryllium and lanthanide derivatives by capillary gas chromatography

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

Harvey, Scott D.; Lucke, Richard B.; Douglas, Matt

2012-09-04

Previous studies describe derivatization of metal ions followed by analysis using gas chromatography, usually on packed columns. In many of these studies, stable and volatile derivatives were formed using fluorinated β-diketonate reagents. This paper extends previous work by investigating separations of the derivatives on small-diameter capillary gas chromatography columns and exploring on-fiber, solid-phase microextraction derivatization techniques for beryllium. The β-diketonate used for these studies was 1,1,1,2,2,6,6,7,7,7-decafluoro-3,5-heptanedione. Derivatization of lanthanides also required addition of a neutral donor, dibutyl sulfoxide, in addition to 1,1,1,2,2,6,6,7,7,7-decafluoro-3,5-heptanedione. Unoptimized separations on a 100-μm i.d. capillary column proved capable of rapid separations (within 15 min) of lanthanidemore » derivatives that are adjacent to one another in the periodic table. Full-scan mass spectra were obtained from derivatives containing 5 ng of each lanthanide. Studies also developed a simple on-fiber solid-phase microextraction derivatization of beryllium. Beryllium could be analyzed in the presence of other alkali earth elements (Ba(II) and Sr(II)) without interference. Finally, extension of the general approach was demonstrated for several additional elements (i.e. Cu(II), Cr(III), and Ga(III)).« less

Solvent systems with n-hexane and/or cyclohexane in countercurrent chromatography--Physico-chemical parameters and their impact on the separation of alkyl hydroxybenzoates.

PubMed

Englert, Michael; Vetter, Walter

2014-05-16

Countercurrent chromatography (CCC) is an efficient preparative separation technique based on the liquid-liquid distribution of compounds between two phases of a biphasic liquid system. The crucial parameter for the successful application is the selection of the solvent system. Especially for nonpolar analytes the selection options are limited. On the search for a suitable solvent system for the separation of an alkyl hydroxybenzoate homologous series, we noted that the substitution of cyclohexane with n-hexane was accompanied with unexpected differences in partitioning coefficients of the individual analytes. In this study, we investigated the influence of the subsequent substitution of n-hexane with cyclohexane in the n-hexane/cyclohexane/tert-butylmethylether/methanol/water solvent system family. Exact phase compositions and polarity, viscosity and density differences were determined to characterize the different mixtures containing n-hexane and/or cyclohexane. Findings were confirmed by performing CCC separations with different mixtures, which led to baseline resolution for positional isomers when increasing the amount of cyclohexane while the resolution between two pairs of structural isomers decreased. With the new methodology described, structurally similar compounds could be resolved by choosing a certain ratio of n-hexane to cyclohexane. Copyright © 2014 Elsevier B.V. All rights reserved.

Phase separation and large deviations of lattice active matter

NASA Astrophysics Data System (ADS)

Whitelam, Stephen; Klymko, Katherine; Mandal, Dibyendu

2018-04-01

Off-lattice active Brownian particles form clusters and undergo phase separation even in the absence of attractions or velocity-alignment mechanisms. Arguments that explain this phenomenon appeal only to the ability of particles to move persistently in a direction that fluctuates, but existing lattice models of hard particles that account for this behavior do not exhibit phase separation. Here we present a lattice model of active matter that exhibits motility-induced phase separation in the absence of velocity alignment. Using direct and rare-event sampling of dynamical trajectories, we show that clustering and phase separation are accompanied by pronounced fluctuations of static and dynamic order parameters. This model provides a complement to off-lattice models for the study of motility-induced phase separation.

Flexible stator control on the Galileo spacecraft

NASA Technical Reports Server (NTRS)

Kopf, E. H.; Brown, T. K.; Marsh, E. L.

1979-01-01

Galileo is a dual-spin spacecraft designed to deliver a probe to Jupiter and then orbit the planet. The stator, or despun section, contains four flexible modes below 10 Hz and the despun actuator is separated from the inertial sensors by this flexibility. Control loop separation by bandwidth proved unacceptable due to performance requirements. To obtain the desired performance, a control scheme was devised which consists of three parts. First, flexibility damping and control notch filtering are accomplished by phase locked loop techniques. Second, slewing maneuvers are produced by torque profiles which are nonexcitatory to the structure. Finally, a low bandwidth perturbation controller is supplied to remove spacecraft disturbances.

Revisiting resolution in hydrodynamic countercurrent chromatography: tubing bore effect.

PubMed

Berthod, A; Faure, K

2015-04-17

A major challenge in countercurrent chromatography (CCC), the technique that works with a support-free biphasic liquid system, is to retain the liquid stationary phase inside the CCC column (Sf parameter). Two solutions are commercially available: the hydrostatic CCC columns, also called centrifugal partition chromatographs (CPC), with disks of interconnected channels and rotary seals, and the hydrodynamic CCC columns with bobbins of coiled open tube and no rotary seals. It was demonstrated that the amount of liquid stationary phase retained by a coiled tube was higher with larger bore tubing than with small bore tubes. At constant column volume, small bore tubing will be longer producing more efficiency than larger bore tube that will better retain the liquid stationary phase. Since the resolution equation in CCC is depending on both column efficiency and stationary phase retention ratio, the influence of the tubing bore should be studied. This theoretical work showed that there is an optimum tubing bore size depending on solute partition coefficient and mobile phase flow rate. The interesting result of the theoretical study is that larger tubing bores allow for dramatically reduced experiment durations for all solutes: in reversed phase CCC (polar mobile phase), hydrophobic solutes are usually highly retained. These apolar solutes can be separated by the same coil at high flow rates and reduced Sf with similar retention times as polar solutes separated at smaller flow rates and much higher Sf. Copyright © 2015 Elsevier B.V. All rights reserved.

Calorimetric analysis of cryopreservation and freeze-drying formulations.

PubMed

Sun, Wendell Q

2015-01-01

Differential scanning calorimetry (DSC) is a commonly used thermal analysis technique in cryopreservation and freeze-drying research. It has been used to investigate crystallization, eutectic formation, glass transition, devitrification, recrystallization, melting, polymorphism, molecular relaxation, phase separation, water transport, thermochemistry, and kinetics of complex reactions (e.g., protein denaturation). Such information can be used for the optimization of protective formulations and process protocols. This chapter gives an introduction to beginners who are less familiar with this technique. It covers the instrument and its basic principles, followed by a discussion of the methods as well as examples of specific applications.

Electrodeposition on nanofibrous polymer scaffolds: Rapid mineralization, tunable calcium phosphate composition and topography

PubMed Central

He, Chuanglong; Xiao, Guiyong; Jin, Xiaobing; Sun, Chenghui; Ma, Peter X.

2011-01-01

We developed a straightforward, fast, and versatile technique to fabricate mineralized nanofibrous polymer scaffolds for bone regeneration in this work. Nanofibrous poly(l-lactic acid) scaffolds were fabricated using both electrospinning and phase separation techniques. An electrodeposition process was designed to deposit calcium phosphate on the nanofibrous scaffolds. Such scaffolds contain a high quality mineral coating on the fiber surface with tunable surface topography and chemical composition by varying the processing parameters, which can mimic the composition and structure of natural bone extracellular matrix and provide a more biocompatible interface for bone regeneration. PMID:21673827

Effect of applied strain on phase separation of Fe-28 at.% Cr alloy: 3D phase-field simulation

NASA Astrophysics Data System (ADS)

Zhu, Lihui; Li, Yongsheng; Liu, Chengwei; Chen, Shi; Shi, Shujing; Jin, Shengshun

2018-04-01

A quantitative simulation of the separation of the α‧ phase in Fe-28 at.% Cr alloy under the effects of applied strain is performed by utilizing a three-dimensional phase-field model. The elongation of the Cr-enriched α‧ phase becomes obvious with the influence of applied uniaxial strain for the phase separation transforms from spinodal decomposition of 700 K to nucleation and growth of 773 K. The applied strain shows a significant influence on the early stage phase separation, and the influence is enlarged with the elevated temperature. The steady-state coarsening with the mechanism of spinodal decomposition is substantially affected by the applied strain for low-temperature aging, while the influence is reduced as the temperature increases and as the phase separation mechanism changes to nucleation and growth. The peak value of particle size distribution decreases, and the PSD for 773 K becomes more widely influenced by the applied strain. The simulation results of separation of the Cr-enriched α‧ phase with the applied strain provide a further understanding of the strain effect on the phase separation of Fe-Cr alloys from the metastable region to spinodal regions.

Seismic body wave separation in volcano-tectonic activity inferred by the Convolutive Independent Component Analysis

NASA Astrophysics Data System (ADS)

Capuano, Paolo; De Lauro, Enza; De Martino, Salvatore; Falanga, Mariarosaria; Petrosino, Simona

2015-04-01

One of the main challenge in volcano-seismological literature is to locate and characterize the source of volcano/tectonic seismic activity. This passes through the identification at least of the onset of the main phases, i.e. the body waves. Many efforts have been made to solve the problem of a clear separation of P and S phases both from a theoretical point of view and developing numerical algorithms suitable for specific cases (see, e.g., Küperkoch et al., 2012). Recently, a robust automatic procedure has been implemented for extracting the prominent seismic waveforms from continuously recorded signals and thus allowing for picking the main phases. The intuitive notion of maximum non-gaussianity is achieved adopting techniques which involve higher-order statistics in frequency domain., i.e, the Convolutive Independent Component Analysis (CICA). This technique is successful in the case of the blind source separation of convolutive mixtures. In seismological framework, indeed, seismic signals are thought as the convolution of a source function with path, site and the instrument response. In addition, time-delayed versions of the same source exist, due to multipath propagation typically caused by reverberations from some obstacle. In this work, we focus on the Volcano Tectonic (VT) activity at Campi Flegrei Caldera (Italy) during the 2006 ground uplift (Ciaramella et al., 2011). The activity was characterized approximately by 300 low-magnitude VT earthquakes (Md < 2; for the definition of duration magnitude, see Petrosino et al. 2008). Most of them were concentrated in distinct seismic sequences with hypocenters mainly clustered beneath the Solfatara-Accademia area, at depths ranging between 1 and 4 km b.s.l.. The obtained results show the clear separation of P and S phases: the technique not only allows the identification of the S-P time delay giving the timing of both phases but also provides the independent waveforms of the P and S phases. This is an enormous advantage for all the problems related to the source inversion and location In addition, the VT seismicity was accompanied by hundreds of LP events (characterized by spectral peaks in the 0.5-2-Hz frequency band) that were concentrated in a 7-day interval. The main interest is to establish whether the occurrence of LPs is only limited to the swarm that reached a climax on days 26-28 October as indicated by Saccorotti et al. (2007), or a longer period is experienced. The automatically extracted waveforms with improved signal-to-noise ratio via CICA coupled with automatic phase picking allowed to compile a more complete seismic catalog and to better quantify the seismic energy release including the presence of LP events from the beginning of October until mid of November. Finally, a further check of the volcanic nature of extracted signals is achieved by looking at the seismological properties and the content of entropy held in the traces (Falanga and Petrosino 2012; De Lauro et al., 2012). Our results allow us to move towards a full description of the complexity of the source, which can be used for hazard-model development and forecast-model testing, showing an illustrative example of the applicability of the CICA method to regions with low seismicity in high ambient noise

Preparative separation of two subsidiary colors of FD&C Yellow No. 5 (Tartrazine) using spiral high-speed counter-current chromatography◊

PubMed Central

Roque, Jose A.; Mazzola, Eugene P.; Ito, Yoichiro

2014-01-01

Specifications in the U.S. Code of Federal Regulations for the color additive FD&C Yellow No. 5 (Colour Index No. 19140) limit the level of the tetrasodium salt of 4-[(4',5-disulfo[1,1'-biphenyl]-2-yl)hydrazono]-4,5-dihydro-5-oxo-1-(4-sulfophenyl)-1H-pyrazole-3-carboxylic acid and that of the trisodium salt of 4,4'-[4,5-dihydro-5-oxo-4-[(4-sulfophenyl)hydrazono]-1H-pyrazol-1,3-diyl]bis[benzenesulfonic acid], which are subsidiary colors abbreviated as Pk5 and Pk7, respectively. Small amounts of Pk5 and Pk7 are needed by the U.S. Food and Drug Administration for confirmatory analyses and for development of analytical methods. The present study describes the use of spiral high-speed counter-current chromatography (HSCCC) with the recently introduced highly polar organic/high-ionic strength aqueous solvent systems to separate Pk5 and Pk7 from a sample of FD&C Yellow No. 5 containing ~3.5% Pk5 and ~0.7% Pk7. Multiple ~1.0 g portions of FD&C Yellow No. 5 (totaling 6.4 g dye) were separated, using the upper phase of the solvent system 1-BuOH/EtOHabs/saturated ammonium sulfate/water, 1.7:0.3:1:1, v/v/v/v, as the mobile phase. After applying a specially developed method for removing the ammonium sulfate from the HSCCC-collected fractions, these separations resulted in an enriched mixture (~160 mg) of Pk5 and Pk7 (~46% and ~21%, respectively). Separation of the enriched mixture, this time using the lower phase of that solvent system as the mobile phase, resulted in ~ 61 mg of Pk5 collected in fractions whose purity ranged from 88.0% to 92.7% (by HPLC at 254 nm). Pk7 (20.7 mg, ~83% purity) was recovered from the upper phase of the column content. Application of this procedure also resulted in purifying the major component of FD&C Yellow No. 5 to >99% purity. The separated compounds were characterized by high-resolution mass spectrometry and several 1H and 13C nuclear magnetic resonance spectroscopic techniques (COSY, NOESY, HSQC, and HMBC). PMID:24755184

Advanced Gouy phase high harmonics interferometer

NASA Astrophysics Data System (ADS)

Mustary, M. H.; Laban, D. E.; Wood, J. B. O.; Palmer, A. J.; Holdsworth, J.; Litvinyuk, I. V.; Sang, R. T.

2018-05-01

We describe an extreme ultraviolet (XUV) interferometric technique that can resolve ∼100 zeptoseconds (10‑21 s) delay between high harmonic emissions from two successive sources separated spatially along the laser propagation in a single Gaussian beam focus. Several improvements on our earlier work have been implemented in the advanced interferometer. In this paper, we report on the design, characterization and optimization of the advanced Gouy phase interferometer. Temporal coherence for both atomic argon and molecular hydrogen gases has been observed for several harmonic orders. It has been shown that phase shift of XUV pulses mainly originates from the emission time delay due to the Gouy phase in the laser focus and the observed interference is independent of the generating medium. This interferometer can be a useful tool for measuring the relative phase shift between any two gas species and for studying ultrafast dynamics of their electronic and nuclear motion.

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.

A Critical Review on Clinical Application of Separation Techniques for Selective Recognition of Uracil and 5-Fluorouracil.

PubMed

Pandey, Khushaboo; Dubey, Rama Shankar; Prasad, Bhim Bali

2016-03-01

The most important objectives that are frequently found in bio-analytical chemistry involve applying tools to relevant medical/biological problems and refining these applications. Developing a reliable sample preparation step, for the medical and biological fields is another primary objective in analytical chemistry, in order to extract and isolate the analytes of interest from complex biological matrices. Since, main inborn errors of metabolism (IEM) diagnosable through uracil analysis and the therapeutic monitoring of toxic 5-fluoruracil (an important anti-cancerous drug) in dihydropyrimidine dehydrogenase deficient patients, require an ultra-sensitive, reproducible, selective, and accurate analytical techniques for their measurements. Therefore, keeping in view, the diagnostic value of uracil and 5-fluoruracil measurements, this article refines several analytical techniques involved in selective recognition and quantification of uracil and 5-fluoruracil from biological and pharmaceutical samples. The prospective study revealed that implementation of molecularly imprinted polymer as a solid-phase material for sample preparation and preconcentration of uracil and 5-fluoruracil had proven to be effective as it could obviates problems related to tedious separation techniques, owing to protein binding and drastic interferences, from the complex matrices in real samples such as blood plasma, serum samples.

Tone and Broadband Noise Separation from Acoustic Data of a Scale-Model Counter-Rotating Open Rotor

NASA Technical Reports Server (NTRS)

Sree, David; Stephens, David B.

2014-01-01

Renewed interest in contra-rotating open rotor technology for aircraft propulsion application has prompted the development of advanced diagnostic tools for better design and improved acoustical performance. In particular, the determination of tonal and broadband components of open rotor acoustic spectra is essential for properly assessing the noise control parameters and also for validating the open rotor noise simulation codes. The technique of phase averaging has been employed to separate the tone and broadband components from a single rotor, but this method does not work for the two-shaft contra-rotating open rotor. A new signal processing technique was recently developed to process the contra-rotating open rotor acoustic data. The technique was first tested using acoustic data taken of a hobby aircraft open rotor propeller, and reported previously. The intent of the present work is to verify and validate the applicability of the new technique to a realistic one-fifth scale open rotor model which has 12 forward and 10 aft contra-rotating blades operating at realistic forward flight Mach numbers and tip speeds. The results and discussions of that study are presented in this paper.

Tone and Broadband Noise Separation from Acoustic Data of a Scale-Model Contra-Rotating Open Rotor

NASA Technical Reports Server (NTRS)

Sree, Dave; Stephens, David B.

2014-01-01

Renewed interest in contra-rotating open rotor technology for aircraft propulsion application has prompted the development of advanced diagnostic tools for better design and improved acoustical performance. In particular, the determination of tonal and broadband components of open rotor acoustic spectra is essential for properly assessing the noise control parameters and also for validating the open rotor noise simulation codes. The technique of phase averaging has been employed to separate the tone and broadband components from a single rotor, but this method does not work for the two-shaft contra-rotating open rotor. A new signal processing technique was recently developed to process the contra-rotating open rotor acoustic data. The technique was first tested using acoustic data taken of a hobby aircraft open rotor propeller, and reported previously. The intent of the present work is to verify and validate the applicability of the new technique to a realistic one-fifth scale open rotor model which has 12 forward and 10 aft contra-rotating blades operating at realistic forward flight Mach numbers and tip speeds. The results and discussions of that study are presented in this paper.

Surface relief and refractive index gratings patterned in chalcogenide glasses and studied by off-axis digital holography.

PubMed

Cazac, V; Meshalkin, A; Achimova, E; Abashkin, V; Katkovnik, V; Shevkunov, I; Claus, D; Pedrini, G

2018-01-20

Surface relief gratings and refractive index gratings are formed by direct holographic recording in amorphous chalcogenide nanomultilayer structures As 2 S 3 -Se and thin films As 2 S 3 . The evolution of the grating parameters, such as the modulation of refractive index and relief depth in dependence of the holographic exposure, is investigated. Off-axis digital holographic microscopy is applied for the measurement of the photoinduced phase gratings. For the high-accuracy reconstruction of the wavefront (amplitude and phase) transmitted by the fabricated gratings, we used a computational technique based on the sparse modeling of phase and amplitude. Both topography and refractive index maps of recorded gratings are revealed. Their separated contribution in diffraction efficiency is estimated.

Optical ultra-wide-band pulse bipolar and shape modulation based on a symmetric PM-IM conversion architecture.

PubMed

Wang, Shiguang; Chen, Hongwei; Xin, Ming; Chen, Minghua; Xie, Shizhong

2009-10-15

A simple and feasible technique for ultra-wide-band (UWB) pulse bipolar modulation (PBM) and pulse shape modulation (PSM) in the optical domain is proposed and demonstrated. The PBM and PSM are performed using a symmetric phase modulation to intensity modulation conversion architecture, including a couple of phase modulators and an optical bandpass filter (OBPF). Two optical carriers, which are separately phase modulated by two appropriate electrical pulse patterns, are at the long- and short-wavelength linear slopes of the OBPF spectrum, respectively. The high-speed PBM and PSM without limit of chip length, polarity, and shape are implemented in simulation and are also verified by experiment. (c) 2009 Optical Society of America.

Stability and Oil Migration of Oil-in-Water Emulsions Emulsified by Phase-Separating Biopolymer Mixtures.

PubMed

Yang, Nan; Mao, Peng; Lv, Ruihe; Zhang, Ke; Fang, Yapeng; Nishinari, Katsuyoshi; Phillips, Glyn O

2016-08-01

Oil-in-water (O/W) emulsions with varying concentration of oil phase, medium-chain triglyceride (MCT), were prepared using phase-separating gum arabic (GA)/sugar beet pectin (SBP) mixture as an emulsifier. Stability of the emulsions including emulsion phase separation, droplet size change, and oil migration were investigated by means of visual observation, droplet size analysis, oil partition analysis, backscattering of light, and interfacial tension measurement. It was found that in the emulsions prepared with 4.0% GA/1.0% SBP, when the concentration of MCT was greater than 2.0%, emulsion phase separation was not observed and the emulsions were stable with droplet size unchanged during storage. This result proves the emulsification ability of phase-separating biopolymer mixtures and their potential usage as emulsifiers to prepare O/W emulsion. However, when the concentration of MCT was equal or less than 2.0%, emulsion phase separation occurred after preparation resulting in an upper SBP-rich phase and a lower GA-rich phase. The droplet size increased in the upper phase whereas decreased slightly in the lower phase with time, compared to the freshly prepared emulsions. During storage, the oil droplets exhibited a complex migration process: first moving to the SBP-rich phase, then to the GA-rich phase and finally gathering at the interface between the two phases. The mechanisms of the emulsion stability and oil migration in the phase-separated emulsions were discussed. © 2016 Institute of Food Technologists®

Creation of hybrid optoelectronic systems for document identification

NASA Astrophysics Data System (ADS)

Muravsky, Leonid I.; Voronyak, Taras I.; Kulynych, Yaroslav P.; Maksymenko, Olexander P.; Pogan, Ignat Y.

2001-06-01

Use of security devices based on a joint transform correlator (JTC) architecture for identification of credit cards and other products is very promising. The experimental demonstration of the random phase encoding technique for security verification shows that hybrid JTCs can be successfully utilized. The random phase encoding technique provides a very high protection level of products and things to be identified. However, the realization of this technique is connected with overcoming of the certain practical problems. To solve some of these problems and simultaneously to improve the security of documents and other products, we propose to use a transformed phase mask (TPM) as an input object in an optical correlator. This mask is synthesized from a random binary pattern (RBP), which is directly used to fabricate a reference phase mask (RPM). To obtain the TPM, we previously separate the RBP on a several parts (for example, K parts) of an arbitrary shape and further fabricate the TPM from this transformed RBP. The fabricated TPM can be bonded as the optical mark to any product or thing to be identified. If the RPM and the TPM are placed on the optical correlator input, the first diffracted order of the output correlation signal is containing the K narrow autocorrelation peaks. The distances between the peaks and the peak's intensities can be treated as the terms of the identification feature vector (FV) for the TPM identification.

Rapid Separation of Copper Phase and Iron-Rich Phase From Copper Slag at Low Temperature in a Super-Gravity Field

NASA Astrophysics Data System (ADS)

Lan, Xi; Gao, Jintao; Huang, Zili; Guo, Zhancheng

2018-03-01

A novel approach for quickly separating a metal copper phase and iron-rich phase from copper slag at low temperature is proposed based on a super-gravity method. The morphology and mineral evolution of the copper slag with increasing temperature were studied using in situ high-temperature confocal laser scanning microscopy and ex situ scanning electron microscopy and X-ray diffraction methods. Fe3O4 particles dispersed among the copper slag were transformed into FeO by adding an appropriate amount of carbon as a reducing agent, forming the slag melt with SiO2 at low temperature and assisting separation of the copper phase from the slag. Consequently, in a super-gravity field, the metallic copper and copper matte were concentrated as the copper phase along the super-gravity direction, whereas the iron-rich slag migrated in the opposite direction and was quickly separated from the copper phase. Increasing the gravity coefficient (G) significantly enhanced the separation efficiency. After super-gravity separation at G = 1000 and 1473 K (1200 °C) for 3 minutes, the mass fraction of Cu in the separated copper phase reached 86.11 wt pct, while that in the separated iron-rich phase was reduced to 0.105 wt pct. The recovery ratio of Cu in the copper phase was as high as up to 97.47 pct.

Rapid Separation of Copper Phase and Iron-Rich Phase From Copper Slag at Low Temperature in a Super-Gravity Field

NASA Astrophysics Data System (ADS)

Lan, Xi; Gao, Jintao; Huang, Zili; Guo, Zhancheng

2018-06-01

A novel approach for quickly separating a metal copper phase and iron-rich phase from copper slag at low temperature is proposed based on a super-gravity method. The morphology and mineral evolution of the copper slag with increasing temperature were studied using in situ high-temperature confocal laser scanning microscopy and ex situ scanning electron microscopy and X-ray diffraction methods. Fe3O4 particles dispersed among the copper slag were transformed into FeO by adding an appropriate amount of carbon as a reducing agent, forming the slag melt with SiO2 at low temperature and assisting separation of the copper phase from the slag. Consequently, in a super-gravity field, the metallic copper and copper matte were concentrated as the copper phase along the super-gravity direction, whereas the iron-rich slag migrated in the opposite direction and was quickly separated from the copper phase. Increasing the gravity coefficient (G) significantly enhanced the separation efficiency. After super-gravity separation at G = 1000 and 1473 K (1200 °C) for 3 minutes, the mass fraction of Cu in the separated copper phase reached 86.11 wt pct, while that in the separated iron-rich phase was reduced to 0.105 wt pct. The recovery ratio of Cu in the copper phase was as high as up to 97.47 pct.

Nanoparticle cages for enzyme catalysis in organic media.

PubMed

Wu, Changzhu; Bai, Shuo; Ansorge-Schumacher, Marion B; Wang, Dayang

2011-12-15

Encapsulation of enzymes in Pickering emulsions results in a large interfacial area of the enzyme-containing aqueous phase for biocatalysis in organic media. This immobilization technique minimizes enzyme inactivation through stabilizing immiscible liquids by particles, facilitates separation processes, and significantly increases catalytic performance of both stable and vulnerable enzymes. Thus, a broad technical applicability can be envisioned. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Archaeological Investigation at El Dorado Lake, Butler County, Kansas. Phase III.

DTIC Science & Technology

1982-01-01

time during which deep disturbance predominated is estimated to be roughly equal to the number of years surface and shallow techniques have been... during excavation, but sampled. Measurements are therefore estimated from scale drawings of feature plans. However, the drawing of Feature 3 consists... roasting features with the limestones and/or deposited as refuse during separate disposal episodes. Fauna and Flora A total of 862 bones and bone

An Extrinsic Fabry-Perot Interferometric Sensor using Intermodal Phase Shifting and Demultiplexing of the Propagating Modes in a Few-Mode Fiber

NASA Astrophysics Data System (ADS)

Chatterjee, Julius

This dissertation demonstrates a fiber-optic phase shifted Fabry-Perot interferometer (PS-FPI) as a sensor using modal demultiplexing. Single wavelength Fabry-Perot interferometers suffer from fringe ambiguity and loss of sensitivity at fringe extremes. These hindrances cause it to be a secondary choice when being selected for a measurement task at hand, and more often than not, white light based sensors are selected in favor of the single wavelength Fabry-Perot sensors. This work aims to introduce a technique involving the demultiplexing of the propagating linearly polarized (LP) modes in few mode fibers to obtain two fringe systems from the same sensing cavity. This results in a few-mode interferometer that effectively has two to three orders of magnitude higher perturbation sensitivity than a conventional few mode interferometer for the same sensing region. In this work, two different modal demultiplexing techniques (MD) are used to demodulate the propagating modes and to obtain two fringe sets. These output fringe sets are shifted in phase with respect to each other by a phase shift due to the propagation of the modes in the fiber-optic layout. A method of controlling this phase shift by straining a length of a two mode fiber located separate from the PS-FPI cavity is demonstrated and corresponding changes in phase shifts are shown. The results show a controllable phase shift for both the MD techniques, which is useful in sensing by permitting quadrature demodulation of interferometric fringes and also results in a novel few-mode sensing system having more than two orders of magnitude sensitivity than conventional few-mode devices.

Hierarchically porous materials from layer-by-layer photopolymerization of high internal phase emulsions.

PubMed

Sušec, Maja; Ligon, Samuel Clark; Stampfl, Jürgen; Liska, Robert; Krajnc, Peter

2013-06-13

A combination of high internal phase emulsion (HIPE) templating and additive manufacturing technology (AMT) is applied for creating hierarchical porosity within an acrylate and acrylate/thiol-based polymer network. The photopolymerizable formulation is optimized to produce emulsions with a volume fraction of droplet phase greater than 80 vol%. Kinetic stability of the emulsions is sufficient enough to withstand in-mold curing or computer-controlled layer-by-layer stereolithography without phase separation. By including macroscale cellular cavities within the build file, a level of controlled porosity is created simultaneous to the formation of the porous microstructure of the polyHIPE. The hybrid HIPE-AMT technique thus provides hierarchically porous materials with mechanical properties tailored by the addition of thiol chain transfer agent. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Combined urea-thin layer chromatography and silver nitrate-thin layer chromatography for micro separation and determination of hard-to-detect branched chain fatty acids in natural lipids.

PubMed

Yan, Yuanyuan; Wang, Xingguo; Liu, Yijun; Xiang, Jingying; Wang, Xiaosan; Zhang, Huijun; Yao, Yunping; Liu, Ruijie; Zou, Xiaoqiang; Huang, Jianhua; Jin, Qingzhe

2015-12-18

A simple, fast and efficient procedure was developed for micro separation and enrichment of branched chain fatty acids (BCFA) from natural products using successive thin layer chromatography (TLC) technique coupling novel urea-TLC with AgNO3-TLC, which rely on the formation of urea adduction and AgNO3 bonding in methanol. These natural lipids contain a significant amount of straight chain fatty acids (FA). Fresh and fast urea-TLC and AgNO3-TLC plate making techniques were developed with more even coating and less coating material contamination before being utilized for separation. Goat milk fat was used as a model. Various experimental parameters that affect urea-TLC and AgNO3-TLC separation of BCFA were investigated and optimized, including coating of urea, concentration of original oil sample, mobile phase and sample application format. High efficiency of removal of straight chain FA was achieved with a low amount of sample in an easy and fast way. A total BCFA mix with much higher purity than previous studies was successfully achieved. The developed method has also been applied for the concentration and analysis of BCFA in cow milk fat and Anchovy oil. Copyright © 2015 Elsevier B.V. All rights reserved.

Centrifugal partition chromatography a first dimension for biomass fast pyrolysis oil analysis.

PubMed

Le Masle, Agnès; Santin, Sandra; Marlot, Léa; Chahen, Ludovic; Charon, Nadège

2018-10-31

Biomass fast pyrolysis oils contain molecules having a large variety of chemical functions and a wide range of molecular weights (from several tens to several thousand grams per mole). The good knowledge of their complex composition is essential for optimizing the conversion of bio-oils to biofuels, thereby requiring powerful separation techniques. In this work, we investigate the interest of centrifugal partition chromatography (CPC) as a first dimension for the analysis of a bio-oil. A CPC method is proposed to separate oxygen containing compounds according to their partition coefficients in the solvent system. This approach is a powerful and easy-to-use technique that enables fractionation of a bio-oil at a semi-preparative scale, without any sample loss related to adsorption on the stationary phase. Collected fractions are then injected in liquid chromatography as a second dimension of separation. Contour plot representations of the CPC × LC separation are established to discuss the potential of this approach. These representations can be used as a veritable fingerprint in the comparison of different samples or samples at different steps of a conversion process but also as a powerful tool to identify new compounds and describe the entire composition of the bio-oil. Copyright © 2018 Elsevier B.V. All rights reserved.

A strategy for identification and structural characterization of compounds from Gardenia jasminoides by integrating macroporous resin column chromatography and liquid chromatography-tandem mass spectrometry combined with ion-mobility spectrometry.

PubMed

Wang, Lu; Liu, Shu; Zhang, Xueju; Xing, Junpeng; Liu, Zhiqiang; Song, Fengrui

2016-06-24

In this paper, an analysis strategy integrating macroporous resin (AB-8) column chromatography and high performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS/MS) combined with ion mobility spectrometry (IMS) was proposed and applied for identification and structural characterization of compounds from the fruits of Gardenia jasminoides. The extracts of G. jasminoides were separated by AB-8 resin column chromatography combined with reversed phase liquid chromatography (C18 column) and detected by electrospray ionization tandem mass spectrometry. Additionally, ion mobility spectrometry (IMS) was employed as a supplementary separation technique to discover previously undetected isomers from the fruits of G. jasminoides. A total of 71 compounds, including iridoids, flavonoids, triterpenes, monoterpenoids, carotenoids and phenolic acids were identified by the characteristic high resolution mass spectrometry and the ESI-MS/MS fragmentations. In conclusion, the IMS-MS technique achieved the separation of isomers in crocin-3 and crocin-4 according to their acquired mobility drift times differing from classical analysis by mass spectrometry. The proposed strategy can be used as a highly sensitive and efficient procedure for identification and separation isomeric components in extracts of herbal medicines. Copyright © 2016 Elsevier B.V. All rights reserved.

Wavefield iterative deconvolution to remove multiples and produce phase specific Ps receiver functions

NASA Astrophysics Data System (ADS)

Ainiwaer, A.; Gurrola, H.

2018-03-01

Common conversion point stacking or migration of receiver functions (RFs) and H-k (H is depth and k is Vp/Vs) stacking of RFs has become a common method to study the crust and upper mantle beneath broad-band three-component seismic stations. However, it can be difficult to interpret Pds RFs due to interference between the Pds, PPds and PSds phases, especially in the mantle portion of the lithosphere. We propose a phase separation method to isolate the prominent phases of the RFs and produce separate Pds, PPds and PSds `phase specific' receiver functions (referred to as PdsRFs, PPdsRFs and PSdsRFs, respectively) by deconvolution of the wavefield rather than single seismograms. One of the most important products of this deconvolution method is to produce Ps receiver functions (PdsRFs) that are free of crustal multiples. This is accomplished by using H-k analysis to identify specific phases in the wavefield from all seismograms recorded at a station which enables development of an iterative deconvolution procedure to produce the above-mentioned phase specific RFs. We refer to this method as wavefield iterative deconvolution (WID). The WID method differentiates and isolates different RF phases by exploiting their differences in moveout curves across the entire wave front. We tested the WID by applying it to synthetic seismograms produced using a modified version of the PREM velocity model. The WID effectively separates phases from each stacked RF in synthetic data. We also applied this technique to produce RFs from seismograms recorded at ARU (a broad-band station in Arti, Russia). The phase specific RFs produced using WID are easier to interpret than traditional RFs. The PdsRFs computed using WID are the most improved, owing to the distinct shape of its moveout curves as compared to the moveout curves for the PPds and PSds phases. The importance of this WID method is most significant in reducing interference between phases for depths of less than 300 km. Phases from deeper layers (i.e. P660s as compared to PP220s) are less likely to be misinterpreted because the large amount of moveout causes the appropriate phases to stack coherently if there is sufficient distribution in ray parameter. WID is most effective in producing clean PdsRFs that are relatively free of reverberations whereas PPdsRFs and PSdsRFs retain contamination from reverberations.

Electron irradiation induced phase separation in a sodium borosilicate glass

NASA Astrophysics Data System (ADS)

Sun, K.; Wang, L. M.; Ewing, R. C.; Weber, W. J.

2004-06-01

Electron irradiation induced phase separation in a sodium borosilicate glass was studied in situ by analytical electron microscopy. Distinctly separate phases that are rich in boron and silicon formed at electron doses higher than 4.0 × 10 11 Gy during irradiation. The separated phases are still in amorphous states even at a much high dose (2.1 × 10 12 Gy). It indicates that most silicon atoms remain tetrahedrally coordinated in the glass during the entire irradiation period, except some possible reduction to amorphous silicon. The particulate B-rich phase that formed at high dose was identified as amorphous boron that may contain some oxygen. Both ballistic and ionization processes may contribute to the phase separation.

Introducing causality violation for improved DPOAE component unmixing

NASA Astrophysics Data System (ADS)

Moleti, Arturo; Sisto, Renata; Shera, Christopher A.

2018-05-01

The DPOAE response consists of the linear superposition of two components, a nonlinear distortion component generated in the overlap region, and a reflection component generated by roughness in the DP resonant region. Due to approximate scaling symmetry, the DPOAE distortion component has approximately constant phase. As the reflection component may be considered as a SFOAE generated by the forward DP traveling wave, it has rapidly rotating phase, relative to that of its source, which is also equal to the phase of the DPOAE distortion component. This different phase behavior permits effective separation of the DPOAE components (unmixing), using time-domain or time-frequency domain filtering. Departures from scaling symmetry imply fluctuations around zero delay of the distortion component, which may seriously jeopardize the accuracy of these filtering techniques. The differential phase-gradient delay of the reflection component obeys causality requirements, i.e., the delay is positive only, and the fine-structure oscillations of amplitude and phase are correlated to each other, as happens for TEOAEs and SFOAEs relative to their stimulus phase. Performing the inverse Fourier (or wavelet) transform of a modified DPOAE complex spectrum, in which a constant phase function is substituted for the measured one, the time (or time-frequency) distribution shows a peak at (exactly) zero delay and long-latency specular symmetric components, with a modified (positive and negative) delay, which is that relative to that of the distortion component in the original response. Component separation, applied to this symmetrized distribution, becomes insensitive to systematic errors associated with violation of the scaling symmetry in specific frequency ranges.

Magnetic separation of general solid particles realised by a permanent magnet

PubMed Central

Hisayoshi, K.; Uyeda, C.; Terada, K.

2016-01-01

Most existing solids are categorised as diamagnetic or weak paramagnetic materials. The possibility of magnetic motion has not been intensively considered for these materials. Here, we demonstrate for the first time that ensembles of heterogeneous particles (diamagnetic bismuth, diamond and graphite particles, as well as two paramagnetic olivines) can be dynamically separated into five fractions by the low field produced by neodymium (NdFeB) magnets during short-duration microgravity (μg). This result is in contrast to the generally accepted notion that ordinary solid materials are magnetically inert. The materials of the separated particles are identified by their magnetic susceptibility (χ), which is determined from the translating velocity. The potential of this approach as an analytical technique is comparable to that of chromatography separation because the extraction of new solid phases from a heterogeneous grain ensemble will lead to important discoveries about inorganic materials. The method is applicable for the separation of the precious samples such as lunar soils and/or the Hayabusa particles recovered from the asteroids, because even micron-order grains can be thoroughly separated without sample-loss. PMID:27929081

Magnetic separation of general solid particles realised by a permanent magnet

NASA Astrophysics Data System (ADS)

Hisayoshi, K.; Uyeda, C.; Terada, K.

2016-12-01

Most existing solids are categorised as diamagnetic or weak paramagnetic materials. The possibility of magnetic motion has not been intensively considered for these materials. Here, we demonstrate for the first time that ensembles of heterogeneous particles (diamagnetic bismuth, diamond and graphite particles, as well as two paramagnetic olivines) can be dynamically separated into five fractions by the low field produced by neodymium (NdFeB) magnets during short-duration microgravity (μg). This result is in contrast to the generally accepted notion that ordinary solid materials are magnetically inert. The materials of the separated particles are identified by their magnetic susceptibility (χ), which is determined from the translating velocity. The potential of this approach as an analytical technique is comparable to that of chromatography separation because the extraction of new solid phases from a heterogeneous grain ensemble will lead to important discoveries about inorganic materials. The method is applicable for the separation of the precious samples such as lunar soils and/or the Hayabusa particles recovered from the asteroids, because even micron-order grains can be thoroughly separated without sample-loss.

Magnetic separation of general solid particles realised by a permanent magnet.

PubMed

Hisayoshi, K; Uyeda, C; Terada, K

2016-12-08

Most existing solids are categorised as diamagnetic or weak paramagnetic materials. The possibility of magnetic motion has not been intensively considered for these materials. Here, we demonstrate for the first time that ensembles of heterogeneous particles (diamagnetic bismuth, diamond and graphite particles, as well as two paramagnetic olivines) can be dynamically separated into five fractions by the low field produced by neodymium (NdFeB) magnets during short-duration microgravity (μg). This result is in contrast to the generally accepted notion that ordinary solid materials are magnetically inert. The materials of the separated particles are identified by their magnetic susceptibility (χ), which is determined from the translating velocity. The potential of this approach as an analytical technique is comparable to that of chromatography separation because the extraction of new solid phases from a heterogeneous grain ensemble will lead to important discoveries about inorganic materials. The method is applicable for the separation of the precious samples such as lunar soils and/or the Hayabusa particles recovered from the asteroids, because even micron-order grains can be thoroughly separated without sample-loss.

Trimodal low-dose X-ray tomography

PubMed Central

Zanette, I.; Bech, M.; Rack, A.; Le Duc, G.; Tafforeau, P.; David, C.; Mohr, J.; Pfeiffer, F.; Weitkamp, T.

2012-01-01

X-ray grating interferometry is a coherent imaging technique that bears tremendous potential for three-dimensional tomographic imaging of soft biological tissue and other specimens whose details exhibit very weak absorption contrast. It is intrinsically trimodal, delivering phase contrast, absorption contrast, and scattering (“dark-field”) contrast. Recently reported acquisition strategies for grating-interferometric phase tomography constitute a major improvement of dose efficiency and speed. In particular, some of these techniques eliminate the need for scanning of one of the gratings (“phase stepping”). This advantage, however, comes at the cost of other limitations. These can be a loss in spatial resolution, or the inability to fully separate the three imaging modalities. In the present paper we report a data acquisition and processing method that optimizes dose efficiency but does not share the main limitations of other recently reported methods. Although our method still relies on phase stepping, it effectively uses only down to a single detector frame per projection angle and yields images corresponding to all three contrast modalities. In particular, this means that dark-field imaging remains accessible. The method is also compliant with data acquisition over an angular range of only 180° and with a continuous rotation of the specimen. PMID:22699500

Multiphase imaging of gas flow in a nanoporous material using remote-detection NMR

NASA Astrophysics Data System (ADS)

Harel, Elad; Granwehr, Josef; Seeley, Juliette A.; Pines, Alex

2006-04-01

Pore structure and connectivity determine how microstructured materials perform in applications such as catalysis, fluid storage and transport, filtering or as reactors. We report a model study on silica aerogel using a time-of-flight magnetic resonance imaging technique to characterize the flow field and explain the effects of heterogeneities in the pore structure on gas flow and dispersion with 129Xe as the gas-phase sensor. The observed chemical shift allows the separate visualization of unrestricted xenon and xenon confined in the pores of the aerogel. The asymmetrical nature of the dispersion pattern alludes to the existence of a stationary and a flow regime in the aerogel. An exchange time constant is determined to characterize the gas transfer between them. As a general methodology, this technique provides insights into the dynamics of flow in porous media where several phases or chemical species may be present.

Kinetics of copper nanoparticle precipitation in phosphate glass: an isothermal plasmonic approach.

PubMed

Sendova, Mariana; Jiménez, José A; Smith, Robert; Rudawski, Nicholas

2015-01-14

The kinetics of copper nanoparticle (NP) precipitation in melt-quenched barium-phosphate glass has been studied by in situ isothermal optical micro-spectroscopy. A spectroscopically based approximation technique is proposed to obtain information about the activation energies of nucleation and growth in a narrow temperature range (530-570 °C). Pre-plasmonic and plasmonic NP precipitation stages are identified separated in time. The process as a whole is discussed employing classical nucleation/growth theory and the Kolmogorov-Johnson-Mehl-Avrami phase change model. Activation energies of 3.9(7) eV and 2.6(5) eV have been estimated for the pre-plasmonic and plasmonic spectroscopically assessed stages, respectively. High resolution transmission electron microscopy, differential scanning calorimetry, and Raman spectroscopy were used as complementary techniques for studying the nanoparticulate phase and glass host structure. An empirical linear dependence of the diffusion activation energy on the glass transition temperature with broad applicability is suggested.

Efficient chemical potential evaluation with kinetic Monte Carlo method and non-uniform external potential: Lennard-Jones fluid, liquid, and solid

NASA Astrophysics Data System (ADS)

Ustinov, E. A.

2017-07-01

The aim of this paper is to present a method of a direct evaluation of the chemical potential of fluid, liquid, and solid with kinetic Monte Carlo simulation. The method is illustrated with the 12-6 Lennard-Jones (LJ) system over a wide range of density and temperature. A distinctive feature of the methodology used in the present study is imposing an external potential on the elongated simulation box to split the system into two equilibrium phases, one of which is substantially diluted. This technique provides a reliable direct evaluation of the chemical potential of the whole non-uniform system (including that of the uniformly distributed dense phase in the central zone of the box), which, for example, is impossible in simulation of the uniform crystalline phase. The parameters of the vapor-liquid, liquid-solid, and fluid-solid transitions have been reliably determined. The chemical potential and the pressure are defined as thermodynamically consistent functions of density and temperature separately for the liquid and the solid (FCC) phases. It has been shown that in two-phase systems separated by a flat interface, the crystal melting always occurs at equilibrium conditions. It is also proved that in the limit of zero temperature, the specific heat capacity of an LJ crystal at constant volume is exactly 3Rg (where Rg is the gas constant) without resorting to harmonic oscillators.

Propagation path effects for rayleigh and love waves. Semi-annual technical report

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

Herrin, E.; Goforth, T.

Seismic surface waves are usually composed of overlapping wave trains representing multi-path propagation. A first task in the analysis of such waves is to identify and separate the various component wave trains so that each can be analyzed separately. Phase-matched filters are a class of linear filters in which the Fourier phase of the filter is made equal to that of a given signal. The authors previously described an iterative technique which can be used to find a phase-matched filter for a particular component of a seismic signal. Application of the filters to digital records of Rayleigh waves allowed multiplemore » arrivals to be identified and removed, and allowed recovery of the complex spectrum of the primary wave train along with its apparent group velocity dispersion curve. A comparable analysis of Love waves presents additional complications. Love waves are contaminated by both Love and Rayleigh multipathing and by primary off-axis Rayleigh energy. In the case of explosions, there is much less energy generated as Love waves than as Rayleigh waves. The applicability of phase-matched filtering to Love waves is demonstrated by its use on earthquakes occurring in the Norwegian Sea and near Iceland and on a nuclear explosion in Novaya Zemlya. Despite severe multipathing in two of the three events, the amplitude and phase of each of the primary Love waves were recovered without significant distortion.« less

Microstructure Evolution and Related Magnetic Properties of Cu-Zr-Al-Gd Phase-Separating Metallic Glasses

NASA Astrophysics Data System (ADS)

Kim, Sang Jun; Kim, Jinwoo; Park, Eun Soo

2018-04-01

We carefully investigated the correlation between microstructures and magnetic properties of Cu-Zr-Al-Gd phase-separating metallic glasses (PSMGs). The saturation magnetizations of the PSMGs were determined by total Gd contents of the alloys, while their coercivity exhibits a large deviation by the occurrence of phase separation due to the boundary pinning effect of hierarchically separated amorphous phases. Especially, the PSMGs containing Gd-rich amorphous nanoparticles show the highest coercivity which can be attributed to the size effect of the ferromagnetic amorphous phase. Furthermore, the selective crystallization of ferromagnetic amorphous phases can affect the magnetization behavior of the PSMGs. Our results could provide a novel strategy for tailoring unique soft magnetic properties of metallic glasses by introducing hierarchically separated amorphous phases and controlling their crystallinity.

Microstructure Evolution and Related Magnetic Properties of Cu-Zr-Al-Gd Phase-Separating Metallic Glasses

NASA Astrophysics Data System (ADS)

Kim, Sang Jun; Kim, Jinwoo; Park, Eun Soo

2018-06-01

We carefully investigated the correlation between microstructures and magnetic properties of Cu-Zr-Al-Gd phase-separating metallic glasses (PSMGs). The saturation magnetizations of the PSMGs were determined by total Gd contents of the alloys, while their coercivity exhibits a large deviation by the occurrence of phase separation due to the boundary pinning effect of hierarchically separated amorphous phases. Especially, the PSMGs containing Gd-rich amorphous nanoparticles show the highest coercivity which can be attributed to the size effect of the ferromagnetic amorphous phase. Furthermore, the selective crystallization of ferromagnetic amorphous phases can affect the magnetization behavior of the PSMGs. Our results could provide a novel strategy for tailoring unique soft magnetic properties of metallic glasses by introducing hierarchically separated amorphous phases and controlling their crystallinity.

Phase-sensitive techniques applied to a micromachined vacuum sensor

NASA Astrophysics Data System (ADS)

Chapman, Glenn H.; Sawadsky, N.; Juneja, P. P.

1996-09-01

Phase sensitive AC measurement techniques are particularly applicable to micromachined sensors detecting temperature changes at a sensor caused by a microheater. The small mass produces rapid thermal response to AC signals which are easily detectable with lock-in amplifiers. Phase sensitive measurements were applied to a CMOS compatible micromachined pressure sensor consisting a polysilicon sense line, 760 microns long, on an oxide microbridge separated by 6 microns on each horizontal side from similar polysilicon heaters, all over a micromachined cavity. Sinusoidal heater signals at 32 Hz induced temperature caused sense line resistance changes at 64 Hz. The lock-in detected this as a first harmonic sense resistor voltage from a DC constant sense current. By observing the first harmonic the lock-in rejects all AC coupling of noise by capacitance or inductance, by measuring only those signals at the 64 Hz frequency and with a fixed phase relationship to the heater driver signals. This sensor produces large signals near atmospheric pressure, declining to 7 (mu) V below 0.1 mTorr. Phase measurements between 760 and 100 Torr where the air's thermal conductivity changes little, combined with amplitude changes at low pressure generate a pressure measurement accurate at 5 percent from 760 Torr to 10 mTorr, sensing of induced temperature changes of 0.001 degree C.

Pi-Pi contacts are an overlooked protein feature relevant to phase separation

PubMed Central

Vernon, Robert McCoy; Chong, Paul Andrew; Tsang, Brian; Kim, Tae Hun; Bah, Alaji; Farber, Patrick; Lin, Hong

2018-01-01

Protein phase separation is implicated in formation of membraneless organelles, signaling puncta and the nuclear pore. Multivalent interactions of modular binding domains and their target motifs can drive phase separation. However, forces promoting the more common phase separation of intrinsically disordered regions are less understood, with suggested roles for multivalent cation-pi, pi-pi, and charge interactions and the hydrophobic effect. Known phase-separating proteins are enriched in pi-orbital containing residues and thus we analyzed pi-interactions in folded proteins. We found that pi-pi interactions involving non-aromatic groups are widespread, underestimated by force-fields used in structure calculations and correlated with solvation and lack of regular secondary structure, properties associated with disordered regions. We present a phase separation predictive algorithm based on pi interaction frequency, highlighting proteins involved in biomaterials and RNA processing. PMID:29424691

Superfluid helium 2 liquid-vapor phase separation: Technology assessment

NASA Technical Reports Server (NTRS)

Lee, J. M.

1984-01-01

A literature survey of helium 2 liquid vapor phase separation is presented. Currently, two types of He 2 phase separators are being investigated: porous, sintered metal plugs and the active phase separator. The permeability K(P) shows consistency in porous plug geometric characterization. Both the heat and mass fluxes increase with K(P). Downstream pressure regulation to adjust for varying heat loads and both temperatures is possible. For large dynamic heat loads, the active phase separator shows a maximum heat rejection rate of up to 2 W and bath temperature stability of 0.1 mK. Porous plug phase separation performance should be investigated for application to SIRTF and, in particular, that plugs of from 10 to the minus ninth square centimeters to 10 to the minus eighth square centimeters in conjunction with downstream pressure regulation be studied.

Facile detection of toxic ingredients in seafood using biologically enabled photonic crystal materials

NASA Astrophysics Data System (ADS)

Kong, Xianming; Squire, Kenneth; Wang, Alan X.

2018-02-01

Surface-enhanced Raman scattering (SERS) spectroscopy has attracted considerable attention recently as a powerful detection platform in biosensing because of the wealth of inherent information ascertained about the chemical and molecular composition of a sample. However, real-world samples are often composed of many components, which renders the detection of constitutes of mixed samples very challenging for SERS sensing. Accordingly, separation techniques are needed before SERS measurements. Thin layer chromatography (TLC) is a simple, fast and costeffective technique for analyte separation and can a play pivotal role for on-site sensing. However, combining TLC with SERS is only successful to detect a limited number of analytes that have large Raman scattering cross sections. As a kind of biogenic amine, histamine (2-(4-imidazolyl)-ethylamine) has a relationship with many health problems resulting from seafood consumption occurring worldwide. Diatomaceous earth consists of fossilized remains of diatoms, a type of hard-shelled algae. As a kind of natural photonic biosilica from geological deposits, it has a variety of unique properties including highly porous structure, excellent adsorption capacity, and low cost. In addition, the two dimensional periodic pores on diatomite earth with hierarchical nanoscale photonic crystal features can enhance the localized optical field. Herein, we fabricate TLC plates from diatomite as the stationary phase combining with SERS to separate and detect histamine from seafood samples. We have proved that the diatomite on the TLC plate not only functions as stationary phase, but also provides additional Raman enhancement, in which the detection limit of 2 ppm was achieved for pyrene in mixture.

Elucidating the weak protein-protein interaction mechanisms behind the liquid-liquid phase separation of a mAb solution by different types of additives.

PubMed

Wu, Guoliang; Wang, Shujing; Tian, Zhou; Zhang, Ning; Sheng, Han; Dai, Weiguo; Qian, Feng

2017-11-01

Liquid-liquid phase separation (LLPS) has long been observed during the physical stability investigation of therapeutic protein formulations. The buffer conditions and the presence of various excipients are thought to play important roles in the formulation development of monoclonal antibodies (mAbs). In this study, the effects of several small-molecule excipients (histidine, alanine, glycine, sodium phosphate, sodium chloride, sorbitol and sucrose) with diverse physical-chemical properties on LLPS of a model IgG1 (JM2) solutions were investigated by multiple techniques, including UV-vis spectroscopy, circular dichroism, differential scanning calorimetry/fluorimetry, size exclusion chromatography and dynamic light scattering. The LLPS of JM2 was confirmed to be a thermodynamic equilibrium process with no structural changes or irreversible aggregation of proteins. Phase diagrams of various JM2 formulations were constructed, suggesting that the phase behavior of JM2 was dependent on the solution pH, ionic strength and the presence of other excipients such as glycine, alanine, sorbitol and sucrose. Furthermore, we demonstrated that for this mAb, the interaction parameter (k D ) determined at low protein concentration appeared to be a good predictor for the occurrence of LLPS at high concentration. Copyright © 2017 Elsevier B.V. All rights reserved.

Moessbauer and Electron Microprobe Studies of Density Separates of Martian Nakhlite Mil03346: Implications for Interpretation of Moessbauer Spectra Acquired by the Mars Exploration Rovers

NASA Technical Reports Server (NTRS)

Morris, R. V.; McKay, G. A.; Agresti, D. G.; Li, Loan

2008-01-01

Martian meteorite MIL03346 is described as an augite-rich cumulate rock with approx.80%, approx.3%, and approx.21% modal phase proportions of augite (CPX), olivine and glassy mesostasis, respectively, and is classified as a nakhlite [1]. The Mossbauer spectrum for whole rock (WR) MIL 03346 is unusual for Martian meteorites in that it has a distinct magnetite subspectrum (7% subspectral area) [2]. The meteorite also has products of pre-terrestrial aqueous alteration ("iddingsite") that is associated primarily with the basaltic glass and olivine. The Mossbauer spectrometers on the Mars Exploration Rovers have measured the Fe oxidation state and the Fe mineralogical composition of rocks and soils on the planet s surface since their landing in Gusev Crater and Meridiani Planum in January, 2004 [3,4]. The MIL 03346 meteorite provides an opportunity to "ground truth" or refine Fe phase identifications. This is particularly the case for the so-called "nanophase ferric oxide" (npOx) component. NpOx is a generic name for a ferric rich product of oxidative alteration. On Earth, where we can take samples apart and study individual phases, examples of npOx include ferrihydrite, schwertmannite, akagaaneite, and superparamagnetic (small particle) goethite and hematite. It is also possible for ferric iron to be associated to some unknown extent with igneous phases like pyroxene. We report here an electron microprobe (EMPA) and Moessbauer (MB) study of density separates of MIL 03346. The same separates were used for isotopic studies by [5]. Experimental techniques are described by [6,7].

Astrometria diferencial de precision con VLBI el triangulo de Draco (y estudios de SN1993J)

NASA Astrophysics Data System (ADS)

Ros, E.

1997-11-01

The Very Long Baseline Interferometry (VLBI) technique provides unprecedented resolutions in astronomy. In this PhD we show progress in the study of high precision phase-delay differential astrometry through observations of the radio source triangle formed by the BL-Lac objects 1803+784 and 2007+777, and the QSO 1928+738, in the Northern constellation of Draco (the Dragon), from observations carried out on 20/21 November 1991 with an intercontinental interferometric array simultaneously at the frequencies of 2.3 and 8.4 GHz. We have determined the angular separations among the three radio sources with submilliarcsecond accuracy from a weighted least squares analysis of the differential phase delay from the three celestial bodies. Our present work introduces important advances with respect to previous astrometric studies, carried out over radio source pairs separated by smaller angular distances. We have consistently modeled the parameters involved in an astrometric VLBI observation, in order to reproduce the differential phase observed for radio sources separated by almost 7o on the sky. We have demonstrated the possibility of phase-connection over these angular distances at 8.4 GHz, even at an epoch of a maximum in the solar activity. After the phase-connection we have corrected the effects of the extended structure of the radio source and of the ionosphere. This last correction is one of the main technical achievements of this thesis: it is possible to remove the ionospheric contribution with independent measurements of the ionosphere total electron content obtained at Global Positioning Systems (GPS) sites the VLBI observing stations. The triangular geometry introduces constraints in parameter space that allow a better estimation of the angular separations among the radio sources. It is possible to test the consistency of the astrometric results through the Sky-Closure, defined as the circular sum of the angular separations of the three radio sources, determined pairwise and independently. In our case it is consistent with zero, and verifies satisfactorily the data process followed. The comparison of the measurements of the separations of the pair 1928+738/2007+777 (1991 data) with previous measurements (data from 1985 and 1988), carried out with the same technique, allows us to register adequately the absolute position of 1928+738 relative to 2007+777. We estimate the proper motion of components in 1928+738, and also identify the position of the radio source core. We confirm the superluminal motion of the components of 1928+738. The comparison of our results with those obtained by Eubanks (USNO) from group delay measurements (without structure correction) show the incorrectness of the latter. We also include succinctly in this PhD my colaboration in the work on the radio supernova SN 1993J, in galaxy M81. We have discovered a shell-like structure of the radio emission of SN 1993J which exploded on March 1993. We have also elaborated a movie of its evolution, by monitoring the shell structure for different epochs, and determined the deceleration of its expansion.

New approaches with two cyano columns to the separation of acetaminophen, phenylephrine, chlorpheniramine and related compounds.

PubMed

Olmo, B; García, A; Marín, A; Barbas, C

2005-03-25

The development of new pharmaceutical forms with classical active compounds generates new analytical problems. That is the case of sugar-free sachets of cough-cold products containing acetaminophen, phenylephrine hydrochloride and chlorpheniramine maleate. Two cyanopropyl stationary phases have been employed to tackle the problem. The Discovery cyanopropyl (SUPELCO) column permitted the separation of the three actives, maleate and excipients (mainly saccharine and orange flavour) with a constant proportion of aqueous/ organic solvent (95:5, v/v) and a pH gradient from 7.5 to 2. The run lasted 14 min. This technique avoids many problems related to baseline shifts with classical organic solvent gradients and opens great possibilities to modify selectivity not generally used in reversed phase HPLC. On the other hand, the Agilent Zorbax SB-CN column with a different retention profile permitted us to separate not only the three actives and the excipients but also the three known related compounds: 4-aminophenol, 4-chloracetanilide and 4-nitrophenol in an isocratic method with a run time under 30 min. This method was validated following ICH guidelines and validation parameters showed that it could be employed as stability-indicating method for this pharmaceutical form.

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.

On an application of Tikhonov's fixed point theorem to a nonlocal Cahn-Hilliard type system modeling phase separation

NASA Astrophysics Data System (ADS)

Colli, Pierluigi; Gilardi, Gianni; Sprekels, Jürgen

2016-06-01

This paper investigates a nonlocal version of a model for phase separation on an atomic lattice that was introduced by P. Podio-Guidugli (2006) [36]. The model consists of an initial-boundary value problem for a nonlinearly coupled system of two partial differential equations governing the evolution of an order parameter ρ and the chemical potential μ. Singular contributions to the local free energy in the form of logarithmic or double-obstacle potentials are admitted. In contrast to the local model, which was studied by P. Podio-Guidugli and the present authors in a series of recent publications, in the nonlocal case the equation governing the evolution of the order parameter contains in place of the Laplacian a nonlocal expression that originates from nonlocal contributions to the free energy and accounts for possible long-range interactions between the atoms. It is shown that just as in the local case the model equations are well posed, where the technique of proving existence is entirely different: it is based on an application of Tikhonov's fixed point theorem in a rather unusual separable and reflexive Banach space.

On the phase form of a deformation quantization with separation of variables

NASA Astrophysics Data System (ADS)

Karabegov, Alexander

2016-06-01

Given a star product with separation of variables on a pseudo-Kähler manifold, we obtain a new formal (1, 1)-form from its classifying form and call it the phase form of the star product. The cohomology class of a star product with separation of variables equals the class of its phase form. We show that the phase forms can be arbitrary and they bijectively parametrize the star products with separation of variables. We also describe the action of a change of the formal parameter on a star product with separation of variables, its formal Berezin transform, classifying form, phase form, and canonical trace density.

Rationalizing the light-induced phase separation of mixed halide organic-inorganic perovskites.

PubMed

Draguta, Sergiu; Sharia, Onise; Yoon, Seog Joon; Brennan, Michael C; Morozov, Yurii V; Manser, Joseph S; Kamat, Prashant V; Schneider, William F; Kuno, Masaru

2017-08-04

Mixed halide hybrid perovskites, CH 3 NH 3 Pb(I 1-x Br x ) 3 , represent good candidates for low-cost, high efficiency photovoltaic, and light-emitting devices. Their band gaps can be tuned from 1.6 to 2.3 eV, by changing the halide anion identity. Unfortunately, mixed halide perovskites undergo phase separation under illumination. This leads to iodide- and bromide-rich domains along with corresponding changes to the material's optical/electrical response. Here, using combined spectroscopic measurements and theoretical modeling, we quantitatively rationalize all microscopic processes that occur during phase separation. Our model suggests that the driving force behind phase separation is the bandgap reduction of iodide-rich phases. It additionally explains observed non-linear intensity dependencies, as well as self-limited growth of iodide-rich domains. Most importantly, our model reveals that mixed halide perovskites can be stabilized against phase separation by deliberately engineering carrier diffusion lengths and injected carrier densities.Mixed halide hybrid perovskites possess tunable band gaps, however, under illumination they undergo phase separation. Using spectroscopic measurements and theoretical modelling, Draguta and Sharia et al. quantitatively rationalize the microscopic processes that occur during phase separation.

In situ neutron scattering study of nanoscale phase evolution in PbTe-PbS thermoelectric material

DOE PAGES

Ren, Fei; Schmidt, Robert; Keum, Jong K.; ...

2016-08-24

Introducing nanostructural second phases has been proved to be an effective approach to reduce the lattice thermal conductivity and thus enhance the figure of merit for many thermoelectric materials. Furthermore studies of the formation and evolution of these second phases are central to understanding temperature dependent material behavior, improving thermal stabilities, as well as designing new materials. We examined powder samples of PbTe-PbS thermoelectric material using in situ neutron diffraction and small angle neutron scattering (SANS) techniques from room temperature to elevated temperature up to 663 K, to explore quantitative information on the structure, weight fraction, and size of themore » second phase. Neutron diffraction data showed the as-milled powder was primarily solid solution before heat treatment. During heating, PbS second phase precipitated out of the PbTe matrix around 480 K, while re-dissolution started around 570 K. The second phase remained separated from the matrix upon cooling. Furthermore, SANS data indicated there are two populations of nanostructures. The size of the smaller nanostructure increased from initially 5 nm to approximately 25 nm after annealing at 650 K, while the size of the larger nanostructure remained unchanged. Our study demonstrated that in situ neutron techniques are effective means to obtain quantitative information to study temperature dependent nanostructural behavior of thermoelectrics and likely other high-temperature materials.« less

Facile synthesis of flexible macroporous polypropylene sponges for separation of oil and water

PubMed Central

Wang, Guowei; Uyama, Hiroshi

2016-01-01

Oil spill disasters always occur accidentally, accompanied by the release of plenty of crude oil that could spread quickly over a wide area, creating enormous damage to the fragile marine ecological system. Therefore, the facile large-scale synthesis of hydrophobic three-dimensional (3-D) porous sorbents from low cost raw materials is in urgent demand. In this study, we report the facile template-free synthesis of polypropylene (PP) sponge by using a thermally-induced phase separation (TIPS) technique. The obtained sponge showed macroporous structure, excellent mechanical property, high hydrophobicity, and superoleophilicity. Oil could be separated from an oil/water mixture by simple immersing the sponge into the mixture and subsequent squeezing the sponge. All of these features make this sponge the most promising oil sorbent that will replace commercial non-woven PP fabrics. PMID:26880297

High-field asymmetric waveform ion mobility spectrometry for mass spectrometry-based proteomics.

PubMed

Swearingen, Kristian E; Moritz, Robert L

2012-10-01

High-field asymmetric waveform ion mobility spectrometry (FAIMS) is an atmospheric pressure ion mobility technique that separates gas-phase ions by their behavior in strong and weak electric fields. FAIMS is easily interfaced with electrospray ionization and has been implemented as an additional separation mode between liquid chromatography (LC) and mass spectrometry (MS) in proteomic studies. FAIMS separation is orthogonal to both LC and MS and is used as a means of on-line fractionation to improve the detection of peptides in complex samples. FAIMS improves dynamic range and concomitantly the detection limits of ions by filtering out chemical noise. FAIMS can also be used to remove interfering ion species and to select peptide charge states optimal for identification by tandem MS. Here, the authors review recent developments in LC-FAIMS-MS and its application to MS-based proteomics.

Counter-current motion in counter-current chromatography.

PubMed

Ito, Yoichiro

2014-12-12

After the CCC2012 meeting, I have received an e-mail regarding the terminology of "Countercurrent Chromatography". It stated that the term "Countercurrent" is a misnomer, because its stationary phase is motionless in the column and that the method should be renamed as liquid-liquid separations or centrifugal separations. However, it was found that these names are already used for various other techniques as found via Google search. The term "Countercurrent Chromatography" was originally made after two preparative methods of Countercurrent distribution and liquid Chromatography, both having no countercurrent motion in the column. However, it is surprising to find that this F1 hybrid method "Countercurrent Chromatography" can clearly exhibit countercurrent motion within the separation column in both hydrodynamic and hydrostatic equilibrium systems. This justifies that "Countercurrent Chromatography" is a proper term for this chromatographic method. Published by Elsevier B.V.

Stable Isotope Quantitative N-Glycan Analysis by Liquid Separation Techniques and Mass Spectrometry.

PubMed

Mittermayr, Stefan; Albrecht, Simone; Váradi, Csaba; Millán-Martín, Silvia; Bones, Jonathan

2017-01-01

Liquid phase separation analysis and subsequent quantitation remains a challenging task for protein-derived oligosaccharides due to their inherent structural complexity and diversity. Incomplete resolution or co-detection of multiple glycan species complicates peak area-based quantitation and associated statistical analysis when optical detection methods are used. The approach outlined herein describes the utilization of stable isotope variants of commonly used fluorescent tags that allow for mass-based glycan identification and relative quantitation following separation by liquid chromatography (LC) or capillary electrophoresis (CE). Comparability assessment of glycoprotein-derived oligosaccharides is performed by derivatization with commercially available isotope variants of 2-aminobenzoic acid or aniline and analysis by LC- and CE-mass spectrometry. Quantitative information is attained from the extracted ion chromatogram/electropherogram ratios generated from the light and heavy isotope clusters.

Nano-scale imaging and spectroscopy of plasmonic systems, thermal near-fields, and phase separation in complex oxides

NASA Astrophysics Data System (ADS)

Jones, Andrew C.

Optical spectroscopy represents a powerful characterization technique with the ability to directly interact with the electronic, spin, and lattice excitations in matter. In addition, through implementation of ultrafast techniques, further insight into the real-time dynamics of elementary interactions can be gained. However, the resolution of far-field microscopy techniques is restricted by the diffraction limit setting a spatial resolution limit in the 100s nm to micron range for visible and IR light, respectively. This resolution is too coarse for the characterization of mesoscopic phenomena in condensed matter physics. The development of experimental techniques with nanoscale resolution and sensitivity to optical fields has been a long standing obstacle to the characterization of condensed matter systems on their natural length scales. This dissertation focuses on the fundamental near-field optical properties of surfaces and nanoscale systems as well as the utilization of nano-optical techniques, specifically apertureless scattering-type Scanning Near-field Optical Microscopy (s-SNOM), to characterize said optical properties with nanometer scale resolution. First, the s-SNOM characterization of the field enhancement associated with the localized surface plasmon resonances on metallic structures is discussed. With their ability to localize light, plasmonic nano-structures are promising candidate systems to serve as molecular sensors and nano-photonic devices; however, it is well known that particle morphology and the plasmon resonance alone do not uniquely reflect the details of the local field distribution. Here, I demonstrate the use interferometric s-SNOM for imaging of the near-fields associated with plasmonic resonances of crystalline triangular silver nano-prisms in the visible spectral range. I subsequently show the extension of the concept of a localized plasmon into the mid-IR spectral range with the characterization of near-fields of silver nano-rods. Strong spatial field variation on lengths scales as short as 20 nm is observed associated with the dipolar and quadrupolar modes of both systems with details sensitively depending on the nanoparticle structure and environment. In light of recent publications predicting distinct spectral characteristics of thermal electromagnetic near-fields, I demonstrate the extension of s-SNOM techniques through the implementation of a heated atomic force microscope (AFM) tip acting as its own intrinsic light source for the characterization of thermal near-fields. Here, I detail the spectrally distinct and orders of magnitude enhanced resonant spectral near-field energy density associated with vibrational, phonon, and phonon-polariton modes. Modeling the thermal light scattering by the AFM, the scattering cross-section for thermal light may be related to the electromagnetic local density of states (EM-LDOS) above a surface. Lastly, the unique capability of s-SNOM techniques to characterize phase separation phenomena in correlated electron systems is discussed. This measurement capability provides new microscopic insight into the underlying mechanisms of the rich phase transition behavior exhibited by these materials. As a specific example, the infrared s-SNOM mapping of the metal-insulator transition and the associated nano-domain formation in individual VO2 micro-crystals subject to substrate stress is presented. Our results have important implications for the interpretation of the investigations of conventional polycrystalline thin films where the mutual interaction of constituent crystallites may affect the nature of phase separation processes.

Dynamic pH junction high-speed counter-current chromatography coupled with microwave-assisted extraction for online separation and purification of alkaloids from Stephania cepharantha.

PubMed

Yuan, Zhiquan; Xiao, Xiaohua; Li, Gongke

2013-11-22

A simple and efficient dynamic pH junction high-speed counter-current chromatography method was developed and further applied to the online extraction, separation and purification of alkaloids from Stephania cepharantha by coupling with microwave-assisted extraction. Mineral acid and organic base were added into the mobile phase and the sample solution, respectively, leading to the formation of a dynamic pH junction in the column and causing focus of alkaloids. Selective focus of analytes can be achieved on the basis of velocity changes of the pH junction through appropriate selection of solvent systems and optimization of additive concentrations. The extract can be directly introduced into the HSCCC for the online extraction, separation and purification of alkaloids from S. cepharantha. Continuous separation can be easily achieved with the same solvent system. Under the optimum conditions, 6.0 g original sample was extracted with 60 mL of the upper phase of hexane-ethyl acetate-methanol-water (1:1:1:1, v/v/v/v) containing 10% triethylamine under 50 °C and 400 W irradiation power for 10 min, the extracts were directly separated and purified by high-speed counter-current chromatography. A total of 5.7 mg sinomenine, 8.3mg 6,7-di-O-acetylsinococuline, 17.9 mg berbamine, 12.7 mg isotetrandrine and 14.6 mg cepharanthine were obtained with purities of 96.7%, 93.7%, 98.7%, 97.3% and 99.3%, respectively. The online method provides good selectivity to ionizable compounds and improves the separation and purification efficiency of the high-speed counter-current chromatography technique. It has good potential for separation and purification of effective compounds from natural products. Copyright © 2013 Elsevier B.V. All rights reserved.

Comparison of originator and biosimilar therapeutic monoclonal antibodies using comprehensive two-dimensional liquid chromatography coupled with time-of-flight mass spectrometry.

PubMed

Sorensen, Matthew; Harmes, David C; Stoll, Dwight R; Staples, Gregory O; Fekete, Szabolcs; Guillarme, Davy; Beck, Alain

2016-10-01

As research, development, and manufacturing of biosimilar protein therapeutics proliferates, there is great interest in the continued development of a portfolio of complementary analytical methods that can be used to efficiently and effectively characterize biosimilar candidate materials relative to the respective reference (i.e., originator) molecule. Liquid phase separation techniques such as liquid chromatography and capillary electrophoresis are powerful tools that can provide both qualitative and quantitative information about similarities and differences between reference and biosimilar materials, especially when coupled with mass spectrometry. However, the inherent complexity of these protein materials challenges even the most modern one-dimensional (1D) separation methods. Two-dimensional (2D) separations present a number of potential advantages over 1D methods, including increased peak capacity, 2D peak patterns that can facilitate unknown identification, and improvement in the compatibility of some separation methods with mass spectrometry. In this study, we demonstrate the use of comprehensive 2D-LC separations involving cation-exchange (CEX) and reversed-phase (RP) separations in the first and second dimensions to compare 3 reference/biosimilar pairs of monoclonal antibodies (cetuximab, trastuzumab and infliximab) that cover a range of similarity/disimilarity in a middle-up approach. The second dimension RP separations are coupled to time-of-flight mass spectrometry, which enables direct identification of features in the chromatograms obtained from mAbs digested with the IdeS enzyme, or digestion with IdeS followed by reduction with dithiothreitol. As many as 23 chemically unique mAb fragments were detected in a single sample. Our results demonstrate that these rich datasets enable facile assesment of the degree of similarity between reference and biosimilar materials.

A Preliminary Assessment of Phase Separator Ground-Based and Reduced-Gravity Testing for ALS Systems

NASA Technical Reports Server (NTRS)

Hall, Nancy Rabel

2006-01-01

A viewgraph presentation of phase separator ground-based and reduced-gravity testing for Advanced Life Support (ALS) systems is shown. The topics include: 1) Multiphase Flow Technology Program; 2) Types of Separators; 3) MOBI Phase Separators; 4) Experiment set-up; and 5) Preliminary comparison/results.

Direct mass spectrometry approaches to characterize polyphenol composition of complex samples.

PubMed

Fulcrand, Hélène; Mané, Carine; Preys, Sébastien; Mazerolles, Gérard; Bouchut, Claire; Mazauric, Jean-Paul; Souquet, Jean-Marc; Meudec, Emmanuelle; Li, Yan; Cole, Richard B; Cheynier, Véronique

2008-12-01

Lower molecular weight polyphenols including proanthocyanidin oligomers can be analyzed after HPLC separation on either reversed-phase or normal phase columns. However, these techniques are time consuming and can have poor resolution as polymer chain length and structural diversity increase. The detection of higher molecular weight compounds, as well as the determination of molecular weight distributions, remain major challenges in polyphenol analysis. Approaches based on direct mass spectrometry (MS) analysis that are proposed to help overcome these problems are reviewed. Thus, direct flow injection electrospray ionization mass spectrometry analysis can be used to establish polyphenol fingerprints of complex extracts such as in wine. This technique enabled discrimination of samples on the basis of their phenolic (i.e. anthocyanin, phenolic acid and flavan-3-ol) compositions, but larger oligomers and polymers were poorly detectable. Detection of higher molecular weight proanthocyanidins was also restricted with matrix-assisted laser desorption ionization (MALDI) MS, suggesting that they are difficult to desorb as gas-phase ions. The mass distribution of polymeric fractions could, however, be determined by analyzing the mass distributions of bovine serum albumin/proanthocyanidin complexes using MALDI-TOF-MS.

Effect of crystallographic orientations of grains on the global mechanical properties of steel sheets by depth sensing indentation

NASA Astrophysics Data System (ADS)

Burik, P.; Pesek, L.; Kejzlar, P.; Andrsova, Z.; Zubko, P.

2017-01-01

The main idea of this work is using a physical model to prepare a virtual material with required properties. The model is based on the relationship between the microstructure and mechanical properties. The macroscopic (global) mechanical properties of steel are highly dependent upon microstructure, crystallographic orientation of grains, distribution of each phase present, etc... We need to know the local mechanical properties of each phase separately in multiphase materials. The grain size is a scale, where local mechanical properties are responsible for the behavior. Nanomechanical testing using depth sensing indentation (DSI) provides a straightforward solution for quantitatively characterizing each of phases in microstructure because it is very powerful technique for characterization of materials in small volumes. The aim of this experimental investigation is: (i) to prove how the mixing rule works for local mechanical properties (indentation hardness HIT) in microstructure scale using the DSI technique on steel sheets with different microstructure; (ii) to compare measured global properties with properties achieved by mixing rule; (iii) to analyze the effect of crystallographic orientations of grains on the mixing rule.

Experimental measurement of structural power flow on an aircraft fuselage

NASA Technical Reports Server (NTRS)

Cuschieri, J. M.

1989-01-01

An experimental technique is used to measure the structural power flow through an aircraft fuselage with the excitation near the wing attachment location. Because of the large number of measurements required to analyze the whole of an aircraft fuselage, it is necessary that a balance be achieved between the number of measurement transducers, the mounting of these transducers, and the accuracy of the measurements. Using four transducers mounted on a bakelite platform, the structural intensity vectors at locations distributed throughout the fuselage are measured. To minimize the errors associated with using a four transducers technique the measurement positions are selected away from bulkheads and stiffeners. Because four separate transducers are used, with each transducer having its own drive and conditioning amplifiers, phase errors are introduced in the measurements that can be much greater than the phase differences associated with the measurements. To minimize these phase errors two sets of measurements are taken for each position with the orientation of the transducers rotated by 180 deg and an average taken between the two sets of measurements. Results are presented and discussed.

Pi-Pi contacts are an overlooked protein feature relevant to phase separation.

PubMed

Vernon, Robert McCoy; Chong, Paul Andrew; Tsang, Brian; Kim, Tae Hun; Bah, Alaji; Farber, Patrick; Lin, Hong; Forman-Kay, Julie Deborah

2018-02-09

Protein phase separation is implicated in formation of membraneless organelles, signaling puncta and the nuclear pore. Multivalent interactions of modular binding domains and their target motifs can drive phase separation. However, forces promoting the more common phase separation of intrinsically disordered regions are less understood, with suggested roles for multivalent cation-pi, pi-pi, and charge interactions and the hydrophobic effect. Known phase-separating proteins are enriched in pi-orbital containing residues and thus we analyzed pi-interactions in folded proteins. We found that pi-pi interactions involving non-aromatic groups are widespread, underestimated by force-fields used in structure calculations and correlated with solvation and lack of regular secondary structure, properties associated with disordered regions. We present a phase separation predictive algorithm based on pi interaction frequency, highlighting proteins involved in biomaterials and RNA processing. © 2018, Vernon et al.

Vertical phase separation in bulk heterojunction solar cells formed by in situ polymerization of fulleride

PubMed Central

Zhang, Lipei; Xing, Xing; Zheng, Lingling; Chen, Zhijian; Xiao, Lixin; Qu, Bo; Gong, Qihuang

2014-01-01

Vertical phase separation of the donor and the acceptor in organic bulk heterojunction solar cells is crucial to improve the exciton dissociation and charge transport efficiencies. This is because whilst the exciton diffusion length is limited, the organic film must be thick enough to absorb sufficient light. However, it is still a challenge to control the phase separation of a binary blend in a bulk heterojunction device architecture. Here we report the realization of vertical phase separation induced by in situ photo-polymerization of the acrylate-based fulleride. The power conversion efficiency of the devices with vertical phase separation increased by 20%. By optimising the device architecture, the power conversion efficiency of the single junction device reached 8.47%. We believe that in situ photo-polymerization of acrylate-based fulleride is a universal and controllable way to realise vertical phase separation in organic blends. PMID:24861168

The study of membrane formation via phase inversion method by cloud point and light scattering experiment

NASA Astrophysics Data System (ADS)

Arahman, Nasrul; Maimun, Teuku; Mukramah, Syawaliah

2017-01-01

The composition of polymer solution and the methods of membrane preparation determine the solidification process of membrane. The formation of membrane structure prepared via non-solvent induced phase separation (NIPS) method is mostly determined by phase separation process between polymer, solvent, and non-solvent. This paper discusses the phase separation process of polymer solution containing Polyethersulfone (PES), N-methylpirrolidone (NMP), and surfactant Tetronic 1307 (Tet). Cloud point experiment is conducted to determine the amount of non-solvent needed on induced phase separation. Amount of water required as a non-solvent decreases by the addition of surfactant Tet. Kinetics of phase separation for such system is studied by the light scattering measurement. With the addition of Tet., the delayed phase separation is observed and the structure growth rate decreases. Moreover, the morphology of fabricated membrane from those polymer systems is analyzed by scanning electron microscopy (SEM). The images of both systems show the formation of finger-like macrovoids through the cross-section.

Method and turbine for extracting kinetic energy from a stream of two-phase fluid

NASA Technical Reports Server (NTRS)

Elliott, D. G. (Inventor)

1979-01-01

An axial flow separator turbine is described which includes a number of nozzles for delivering streams of a two-phase fluid along linear paths. A phase separator which responsively separates the vapor and liquid is characterized by concentrically related annuli supported for rotation within the paths. The separator has endless channels for confining the liquid under the influence of centrifugal forces. A vapor turbine fan extracts kinetic energy from the liquid. Angular momentum of both the liquid phase and the vapor phase of the fluid is converted to torque.

Ionic liquid/water mixtures: from hostility to conciliation.

PubMed

Kohno, Yuki; Ohno, Hiroyuki

2012-07-21

Water was originally inimical to ionic liquids (ILs) especially in the analysis of their detailed properties. Various data on the properties of ILs indicate that there are two ways to design functions of ionic liquids. The first is to change the structure of component ions, to provide "task-specific ILs". The second is to mix ILs with other components, such as other ILs, organic solvents or water. Mixing makes it easy to control the properties of the solution. In this strategy, water is now a very important partner. Below, we summarise our recent results on the properties of IL/water mixtures. Stable phase separation is an effective method in some separation processes. Conversely, a dynamic phase change between a homogeneous mixture and separation of phases is important in many fields. Analysis of the relation between phase behaviour and the hydration state of the component ions indicates that the pattern of phase separation is governed by the hydrophilicity of the ions. Sufficiently hydrophilic ions yielded ILs that are miscible with water, and hydrophobic ions gave stable phase separation with water. ILs composed of hydrophobic but hydrated ions undergo a dynamic phase change between a homogeneous mixture and separate phases according to temperature. ILs having more than seven water molecules per ion pair undergo this phase transition. These dynamic phase changes are considered, with some examples, and application is made to the separation of water-soluble proteins.

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

PubMed

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

2018-02-16

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

Strong Cation Exchange Chromatography in Analysis of Posttranslational Modifications: Innovations and Perspectives

PubMed Central

Edelmann, Mariola J.

2011-01-01

Strong cation exchange (SCX) chromatography has been utilized as an excellent separation technique that can be combined with reversed-phase (RP) chromatography, which is frequently used in peptide mass spectrometry. Although SCX is valuable as the second component of such two-dimensional separation methods, its application goes far beyond efficient fractionation of complex peptide mixtures. Here I describe how SCX facilitates mapping of the protein posttranslational modifications (PTMs), specifically phosphorylation and N-terminal acetylation. The SCX chromatography has been mainly used for enrichment of these two PTMs, but it might also be beneficial for high-throughput analysis of other modifications that alter the net charge of a peptide. PMID:22174558

Sol/Gel Processing Techniques for Glass Matrix Composites.

DTIC Science & Technology

1987-11-01

silica alkoxide gels were also produced by an initial partial hydrolysis of TEOS. ,. After an aging period of 18-24 hrs. titanium (IV) isopropoxide ...preparation of these materials is the large difference in hydrolysis rate for titanium versus silica alkoxides. Thus, the tendency towards phase separation in...ethanol solution (Ref. 6-9). After an aging time, the more reactive titanium alkoxide is added. This solution gels quickly and is ready to be further

Model for a Ferromagnetic Quantum Critical Point in a 1D Kondo Lattice

NASA Astrophysics Data System (ADS)

Komijani, Yashar; Coleman, Piers

2018-04-01

Motivated by recent experiments, we study a quasi-one-dimensional model of a Kondo lattice with ferromagnetic coupling between the spins. Using bosonization and dynamical large-N techniques, we establish the presence of a Fermi liquid and a magnetic phase separated by a local quantum critical point, governed by the Kondo breakdown picture. Thermodynamic properties are studied and a gapless charged mode at the quantum critical point is highlighted.

Self-interaction of NPM1 modulates multiple mechanisms of liquid–liquid phase separation

DOE PAGES

Mitrea, Diana M.; Cika, Jaclyn A.; Stanley, Christopher B.; ...

2018-02-26

Nucleophosmin (NPM1) is an abundant, oligomeric protein in the granular component of the nucleolus with roles in ribosome biogenesis. Pentameric NPM1 undergoes liquid–liquid phase separation (LLPS) via heterotypic interactions with nucleolar components, including ribosomal RNA (rRNA) and proteins which display multivalent arginine-rich linear motifs (R-motifs), and is integral to the liquid-like nucleolar matrix. Here we show that NPM1 can also undergo LLPS via homotypic interactions between its polyampholytic intrinsically disordered regions, a mechanism that opposes LLPS via heterotypic interactions. Using a combination of biophysical techniques, including confocal microscopy, SAXS, analytical ultracentrifugation, and single-molecule fluorescence, we describe how conformational changes withinmore » NPM1 control valency and switching between the different LLPS mechanisms. We propose that this newly discovered interplay between multiple LLPS mechanisms may influence the direction of vectorial pre-ribosomal particle assembly within, and exit from the nucleolus as part of the ribosome biogenesis process.« less

Preparation of chitosan-graft-(β-cyclodextrin) based sol-gel stationary phase for open-tubular capillary electrochromatography.

PubMed

Lü, Haixia; Li, Qingyin; Yu, Xiaowei; Yi, Jiaojiao; Xie, Zenghong

2013-07-01

A novel open-tubular CEC column coated with chitosan-graft-(β-CD) (CDCS) was prepared using sol-gel technique. In the sol-gel approach, owing to the 3D network of sol-gel and the strong chemical bond between the stationary phase and the surface of capillary columns, good chromatographic characteristics and unique selectivity in separating isomers were shown. The column efficiencies of 55,000∼163,000 plates/m for the isomeric xanthopterin and phenoxy acid herbicides using the sol-gel-derived CDCS columns were achieved. Good stabilities were demonstrated that the RSD values for the retention time of thiourea and isoxanthopterin were 1.3 and 1.4% (run to run, n = 5), 1.6 and 2.0% (day to day, n = 3), 2.9 and 3.1% (column to column, n = 3), respectively. The sol-gel-coated CDCS columns have shown improved separations of isomeric xanthopterin in comparison with CDCS-bonded capillary column. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Separation processes during binary monotectic alloy production

NASA Technical Reports Server (NTRS)

Frazier, D. O.; Facemire, B. R.; Kaukler, W. F.; Witherow, W. K.; Fanning, U.

1984-01-01

Observation of microgravity solidification processes indicates that outside of sedimentation, at least two other important effects can separate the phases: critical-point wetting and spreading; and thermal migration of second-phase droplets due to interfacial tension gradients. It is difficult to study these surface tension effects while in a unit gravity field. In order to investigate the processes occurring over a temperature range, i.e., between a consolute point and the monotectic temperature, it is necessary to use a low-gravity environment. The MSFC drop tube (and tower), the ballistic trajectory KC-135 airplane, and the Space Shuttle are ideal facilities to aid formation and testing of hypotheses. Much of the early work in this area focuses on transparent materials so that process dynamics may be studied by optical techniques such as photography for viewing macro-processes; holography for studying diffusional growth; spinodal decomposition and coalescence; ellipsometry for surface wetting and spreading effects; and interferometry and spectroscopy for small-scale spatial resolution of concentration profiles.

Self-interaction of NPM1 modulates multiple mechanisms of liquid–liquid phase separation

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

Mitrea, Diana M.; Cika, Jaclyn A.; Stanley, Christopher B.

Nucleophosmin (NPM1) is an abundant, oligomeric protein in the granular component of the nucleolus with roles in ribosome biogenesis. Pentameric NPM1 undergoes liquid–liquid phase separation (LLPS) via heterotypic interactions with nucleolar components, including ribosomal RNA (rRNA) and proteins which display multivalent arginine-rich linear motifs (R-motifs), and is integral to the liquid-like nucleolar matrix. Here we show that NPM1 can also undergo LLPS via homotypic interactions between its polyampholytic intrinsically disordered regions, a mechanism that opposes LLPS via heterotypic interactions. Using a combination of biophysical techniques, including confocal microscopy, SAXS, analytical ultracentrifugation, and single-molecule fluorescence, we describe how conformational changes withinmore » NPM1 control valency and switching between the different LLPS mechanisms. We propose that this newly discovered interplay between multiple LLPS mechanisms may influence the direction of vectorial pre-ribosomal particle assembly within, and exit from the nucleolus as part of the ribosome biogenesis process.« less

Manufacturing of biodegradable polyurethane scaffolds based on polycaprolactone using a phase separation method: physical properties and in vitro assay

PubMed Central

Asefnejad, Azadeh; Khorasani, Mohammad Taghi; Behnamghader, Aliasghar; Farsadzadeh, Babak; Bonakdar, Shahin

2011-01-01

Background Biodegradable polyurethanes have found widespread use in soft tissue engineering due to their suitable mechanical properties and biocompatibility. Methods In this study, polyurethane samples were synthesized from polycaprolactone, hexamethylene diisocyanate, and a copolymer of 1,4-butanediol as a chain extender. Polyurethane scaffolds were fabricated by a combination of liquid–liquid phase separation and salt leaching techniques. The effect of the NCO:OH ratio on porosity content and pore morphology was investigated. Results Scanning electron micrographs demonstrated that the scaffolds had a regular distribution of interconnected pores, with pore diameters of 50–300 μm, and porosities of 64%–83%. It was observed that, by increasing the NCO:OH ratio, the average pore size, compressive strength, and compressive modulus increased. L929 fibroblast and chondrocytes were cultured on the scaffolds, and all samples exhibited suitable cell attachment and growth, with a high level of biocompatibility. Conclusion These biodegradable polyurethane scaffolds demonstrate potential for soft tissue engineering applications. PMID:22072874

Separation of multiphosphorylated peptide isomers by hydrophilic interaction chromatography on an aminopropyl phase.

PubMed

Singer, David; Kuhlmann, Julia; Muschket, Matthias; Hoffmann, Ralf

2010-08-01

The separation of isomeric phosphorylated peptides is challenging and often impossible for multiphosphorylated isomers using chromatographic and capillary electrophoretic methods. In this study we investigated the separation of a set of single-, double-, and triple-phosphorylated peptides (corresponding to the human tau protein) by ion-pair reversed-phase chromatography (IP-RPC) and hydrophilic interaction chromatography (HILIC). In HILIC both hydroxyl and aminopropyl stationary phases were tested with aqueous acetonitrile in order to assess their separation efficiency. The hydroxyl phase separated the phosphopeptides very well from the unphosphorylated analogue, while on the aminopropyl phase even isomeric phosphopeptides attained baseline separation. Thus, up to seven phosphorylated versions of a given tau domain were separated. Furthermore, the low concentration of an acidic ammonium formate buffer allowed an online analysis with electrospray ionization tandem mass spectrometry (ESI-MS/MS) to be conducted, enabling peptide sequencing and identification of phosphorylation sites.

Dancing in the Dark: New Brown Dwarf Binaries from Kernel Phase Interferometry

NASA Astrophysics Data System (ADS)

Pope, Benjamin; Martinache, Frantz; Tuthill, Peter

2013-04-01

This paper revisits a sample of ultracool dwarfs in the solar neighborhood previously observed with the Hubble Space Telescope's NICMOS NIC1 instrument. We have applied a novel high angular resolution data analysis technique based on the extraction and fitting of kernel phases to archival data. This was found to deliver a dramatic improvement over earlier analysis methods, permitting a search for companions down to projected separations of ~1 AU on NIC1 snapshot images. We reveal five new close binary candidates and present revised astrometry on previously known binaries, all of which were recovered with the technique. The new candidate binaries have sufficiently close separation to determine dynamical masses in a short-term observing campaign. We also present four marginal detections of objects which may be very close binaries or high-contrast companions. Including only confident detections within 19 pc, we report a binary fraction of at least \\epsilon _b = 17.2^{+5.7}_{-3.7} %. The results reported here provide new insights into the population of nearby ultracool binaries, while also offering an incisive case study of the benefits conferred by the kernel phase approach in the recovery of companions within a few resolution elements of the point-spread function core. Based on observations performed with the NASA/ESA Hubble Space Telescope. The Hubble observations are associated with proposal ID 10143 and 10879 and were obtained at the Space Telescope Science Institute, which is operated by the Association of Universities for Research in Astronomy, Inc., under NASA contract NAS 5-26555.

Broadband true time delay for microwave signal processing, using slow light based on stimulated Brillouin scattering in optical fibers.

PubMed

Chin, Sanghoon; Thévenaz, Luc; Sancho, Juan; Sales, Salvador; Capmany, José; Berger, Perrine; Bourderionnet, Jérôme; Dolfi, Daniel

2010-10-11

We experimentally demonstrate a novel technique to process broadband microwave signals, using all-optically tunable true time delay in optical fibers. The configuration to achieve true time delay basically consists of two main stages: photonic RF phase shifter and slow light, based on stimulated Brillouin scattering in fibers. Dispersion properties of fibers are controlled, separately at optical carrier frequency and in the vicinity of microwave signal bandwidth. This way time delay induced within the signal bandwidth can be manipulated to correctly act as true time delay with a proper phase compensation introduced to the optical carrier. We completely analyzed the generated true time delay as a promising solution to feed phased array antenna for radar systems and to develop dynamically reconfigurable microwave photonic filters.

Carbothermal shock synthesis of high-entropy-alloy nanoparticles

NASA Astrophysics Data System (ADS)

Yao, Yonggang; Huang, Zhennan; Xie, Pengfei; Lacey, Steven D.; Jacob, Rohit Jiji; Xie, Hua; Chen, Fengjuan; Nie, Anmin; Pu, Tiancheng; Rehwoldt, Miles; Yu, Daiwei; Zachariah, Michael R.; Wang, Chao; Shahbazian-Yassar, Reza; Li, Ju; Hu, Liangbing

2018-03-01

The controllable incorporation of multiple immiscible elements into a single nanoparticle merits untold scientific and technological potential, yet remains a challenge using conventional synthetic techniques. We present a general route for alloying up to eight dissimilar elements into single-phase solid-solution nanoparticles, referred to as high-entropy-alloy nanoparticles (HEA-NPs), by thermally shocking precursor metal salt mixtures loaded onto carbon supports [temperature ~2000 kelvin (K), 55-millisecond duration, rate of ~105 K per second]. We synthesized a wide range of multicomponent nanoparticles with a desired chemistry (composition), size, and phase (solid solution, phase-separated) by controlling the carbothermal shock (CTS) parameters (substrate, temperature, shock duration, and heating/cooling rate). To prove utility, we synthesized quinary HEA-NPs as ammonia oxidation catalysts with ~100% conversion and >99% nitrogen oxide selectivity over prolonged operations.

Evaluation of the Performance of the Distributed Phased-MIMO Sonar.

PubMed

Pan, Xiang; Jiang, Jingning; Wang, Nan

2017-01-11

A broadband signal model is proposed for a distributed multiple-input multiple-output (MIMO) sonar system consisting of two transmitters and a receiving linear array. Transmitters are widely separated to illuminate the different aspects of an extended target of interest. The beamforming technique is utilized at the reception ends for enhancement of weak target echoes. A MIMO detector is designed with the estimated target position parameters within the general likelihood rate test (GLRT) framework. For the high signal-to-noise ratio case, the detection performance of the MIMO system is better than that of the phased-array system in the numerical simulations and the tank experiments. The robustness of the distributed phased-MIMO sonar system is further demonstrated in localization of a target in at-lake experiments.

Evaluation of the Performance of the Distributed Phased-MIMO Sonar

PubMed Central

Pan, Xiang; Jiang, Jingning; Wang, Nan

2017-01-01

A broadband signal model is proposed for a distributed multiple-input multiple-output (MIMO) sonar system consisting of two transmitters and a receiving linear array. Transmitters are widely separated to illuminate the different aspects of an extended target of interest. The beamforming technique is utilized at the reception ends for enhancement of weak target echoes. A MIMO detector is designed with the estimated target position parameters within the general likelihood rate test (GLRT) framework. For the high signal-to-noise ratio case, the detection performance of the MIMO system is better than that of the phased-array system in the numerical simulations and the tank experiments. The robustness of the distributed phased-MIMO sonar system is further demonstrated in localization of a target in at-lake experiments. PMID:28085071

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

Zhao, Yong; Pan, Xuan; Bernussi, Ayrton A.

We demonstrate that catalyst-assisted hydrogen spillover doping of VO{sub 2} thin films significantly alters the metal-insulator transition characteristics and stabilizes the metallic rutile phase at room temperature. With hydrogen inserted into the VO{sub 2} lattice, high resolution X-ray diffraction reveals expansion of the V-V chain separation when compared to the VO{sub 2}(R) phase. The donated free electrons, possibly from O-H bond formation, stabilize the VO{sub 2}(R) to low temperatures. By controlling the amount of dopants to obtain mixed insulating and metallic phases, VO{sub 2} resistivity can be continuously tuned until a critical condition is achieved that suppresses Fabry-Perot resonances. Ourmore » results demonstrate that hydrogen spillover is an effective technique to tune the electrical and optical properties of VO{sub 2} thin films.« less

Legacy systems: managing evolution through integration in a distributed and object-oriented computing environment.

PubMed

Lemaitre, D; Sauquet, D; Fofol, I; Tanguy, L; Jean, F C; Degoulet, P

1995-01-01

Legacy systems are crucial for organizations since they support key functionalities. But they become obsolete with aging and the apparition of new techniques. Managing their evolution is a key issue in software engineering. This paper presents a strategy that has been developed at Broussais University Hospital in Paris to make a legacy system devoted to the management of health care units evolve towards a new up-to-date software. A two-phase evolution pathway is described. The first phase consists in separating the interface from the data storage and application control and in using a communication channel between the individualized components. The second phase proposes to use an object-oriented DBMS in place of the homegrown system. An application example for the management of hypertensive patients is described.

Chemical fractionation-enhanced structural characterization of marine dissolved organic matter

NASA Astrophysics Data System (ADS)

Arakawa, N.; Aluwihare, L.

2016-02-01

Describing the molecular fingerprint of dissolved organic matter (DOM) requires sample processing methods and separation techniques that can adequately minimize its complexity. We have employed acid hydrolysis as a way to make the subcomponents of marine solid phase-extracted (PPL) DOM more accessible to analytical techniques. Using a combination of NMR and chemical derivatization or reduction analyzed by comprehensive (GCxGC) gas chromatography, we observed chemical features strikingly similar to terrestrial DOM. In particular, we observed reduced alicylic hydrocarbons believed to be the backbone of previously identified carboxylic rich alicyclic material (CRAM). Additionally, we found carbohydrates, amino acids and small lipids and acids.

On scattered waves and lipid domains: detecting membrane rafts with X-rays and neutrons

DOE PAGES

Marquardt, Drew; Heberle, Frederick A.; Nickels, Jonathan D.; ...

2015-09-21

In order to understand the biological role of lipids in cell membranes, it is necessary to determine the mesoscopic structure of well-defined model membrane systems. Neutron and X-ray scattering are non-invasive, probe-free techniques that have been used extensively in such systems to probe length scales ranging from angstroms to microns, and dynamics occurring over picosecond to millisecond time scales. Finally, recent developments in the area of phase separated lipid systems mimicking membrane rafts will be presented, and the underlying concepts of the different scattering techniques used to study them will be discussed in detail.

X-ray imaging for studying behavior of liquids at high pressures and high temperatures using Paris-Edinburgh press.

PubMed

Kono, Yoshio; Kenney-Benson, Curtis; Shibazaki, Yuki; Park, Changyong; Wang, Yanbin; Shen, Guoyin

2015-07-01

Several X-ray techniques for studying structure, elastic properties, viscosity, and immiscibility of liquids at high pressures have been integrated using a Paris-Edinburgh press at the 16-BM-B beamline of the Advanced Photon Source. Here, we report the development of X-ray imaging techniques suitable for studying behavior of liquids at high pressures and high temperatures. White X-ray radiography allows for imaging phase separation and immiscibility of melts at high pressures, identified not only by density contrast but also by phase contrast imaging in particular for low density contrast liquids such as silicate and carbonate melts. In addition, ultrafast X-ray imaging, at frame rates up to ∼10(5) frames/second (fps) in air and up to ∼10(4) fps in Paris-Edinburgh press, enables us to investigate dynamics of liquids at high pressures. Very low viscosities of melts similar to that of water can be reliably measured. These high-pressure X-ray imaging techniques provide useful tools for understanding behavior of liquids or melts at high pressures and high temperatures.

Time-Correlated Single-Photon Counting Fluorescence Imaging of Lipid Domains In Raft-Mimicking Giant Unilamellar Vesicles

NASA Astrophysics Data System (ADS)

Clarke, James; Cheng, Kwan; Shindell, Orrin; Wang, Exing

We have designed and constructed a high-throughput electrofusion chamber and an incubator to fabricate Giant Unilamellar Vesicles (GUVs) consisting of high-melting lipids, low-melting lipids, cholesterol and both ordered and disordered phase sensitive fluorescent probes (DiIC12, dehydroergosterol and BODIPY-Cholesterol). GUVs were formed in a 3 stage pulse sequence electrofusion process with voltages ranging from 50mVpp to 2.2Vpp and frequencies from 5Hz to 10Hz. Steady state and time-correlated single-photon counting (TCSPC) fluorescence lifetime (FLIM) based confocal and/or multi-photon microscopic techniques were used to characterize phase separated lipid domains in GUVs. Confocal imaging measures the probe concentration and the chemical environment of the system. TCSPC techniques determine the chemical environment through the perturbation of fluorescent lifetimes of the probes in the system. The above techniques will be applied to investigate the protein-lipid interactions involving domain formation. Specifically, the mechanisms governing lipid domain formations in the above systems that mimic the lipid rafts in cells will be explored. Murchison Fellowship at Trinity University.

Thermal management of high power space based systems

NASA Technical Reports Server (NTRS)

Hwangbo, H.; Mcever, W. S.

1985-01-01

Conventional techniques of using a portion of the spacecraft skin for radiation of waste heat will be inadequate for high powered payloads (50 to 100 kWe) due to the lack of sufficient area. A Shuttle type system using a pumped single phase fluid loop could be scaled up to higher power but this type of system would require excessive pump power and weight. A pumped two-phase heat transfer loop has a much lower pumping requirement due to the higher latent heat of vaporization of the fluid in comparison to the sensible heat it can absorb through a temperature change. Concepts for an evaporator and a condenser for a pumped two-phase system are described. The condenser uses capillary grooves and a separate pumped condensate return line to achieve high heat transfer coefficients and stable operation due to the separation of the vapor and liquid flows. The cold plate evaporator uses wicks to contain the liquid and transport it to the heated surface. It can also function as a condenser for warming components. Control concepts for the cold plate are discussed. Concepts for deployment or erection of large space radiators are also considered.

Capture of circulating tumor cells using photoacoustic flowmetry and two phase flow

NASA Astrophysics Data System (ADS)

O'Brien, Christine M.; Rood, Kyle D.; Bhattacharyya, Kiran; DeSouza, Thiago; Sengupta, Shramik; Gupta, Sagar K.; Mosley, Jeffrey D.; Goldschmidt, Benjamin S.; Sharma, Nikhilesh; Viator, John A.

2012-06-01

Melanoma is the deadliest form of skin cancer, yet current diagnostic methods are unable to detect early onset of metastatic disease. Patients must wait until macroscopic secondary tumors form before malignancy can be diagnosed and treatment prescribed. Detection of cells that have broken off the original tumor and travel through the blood or lymph system can provide data for diagnosing and monitoring metastatic disease. By irradiating enriched blood samples spiked with cultured melanoma cells with nanosecond duration laser light, we induced photoacoustic responses in the pigmented cells. Thus, we can detect and enumerate melanoma cells in blood samples to demonstrate a paradigm for a photoacoustic flow cytometer. Furthermore, we capture the melanoma cells using microfluidic two phase flow, a technique that separates a continuous flow into alternating microslugs of air and blood cell suspension. Each slug of blood cells is tested for the presence of melanoma. Slugs that are positive for melanoma, indicated by photoacoustic waves, are separated from the cytometer for further purification and isolation of the melanoma cell. In this paper, we evaluate the two phase photoacoustic flow cytometer for its ability to detect and capture metastastic melanoma cells in blood.

Two-Point Microrheology of Phase-Separated Domains in Lipid Bilayers

PubMed Central

Hormel, Tristan T.; Reyer, Matthew A.; Parthasarathy, Raghuveer

2015-01-01

Though the importance of membrane fluidity for cellular function has been well established for decades, methods for measuring lipid bilayer viscosity remain challenging to devise and implement. Recently, approaches based on characterizing the Brownian dynamics of individual tracers such as colloidal particles or lipid domains have provided insights into bilayer viscosity. For fluids in general, however, methods based on single-particle trajectories provide a limited view of hydrodynamic response. The technique of two-point microrheology, in which correlations between the Brownian dynamics of pairs of tracers report on the properties of the intervening medium, characterizes viscosity at length-scales that are larger than that of individual tracers and has less sensitivity to tracer-induced distortions, but has never been applied to lipid membranes. We present, to our knowledge, the first two-point microrheological study of lipid bilayers, examining the correlated motion of domains in phase-separated lipid vesicles and comparing one- and two-point results. We measure two-point correlation functions in excellent agreement with the forms predicted by two-dimensional hydrodynamic models, analysis of which reveals a viscosity intermediate between those of the two lipid phases, indicative of global fluid properties rather than the viscosity of the local neighborhood of the tracer. PMID:26287625

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.

Development of a novel amide-silica stationary phase for the reversed-phase HPLC separation of different classes of phytohormones.

PubMed

Aral, Hayriye; Aral, Tarık; Ziyadanoğulları, Berrin; Ziyadanoğulları, Recep

2013-11-15

A novel amide-bonded silica stationary phase was prepared starting from N-Boc-phenylalanine, cyclohexylamine and spherical silica gel (4 µm, 60 Å). The amide ligand was synthesised with high yield. The resulting amide bonded stationary phase was characterised by SEM, IR and elemental analysis. The resulting selector bearing a polar amide group is used for the reversed-phase chromatography separation of different classes of thirteen phytohormones (plant hormones). The chromatographic behaviours of these analytes on the amide-silica stationary phase were compared with those of RP-C18 column under same conditions. The effects of different separation conditions, such as mobile phase, pH value, flow rate and temperature, on the separation and retention behaviours of the 13 phytohormones in this system were studied. The optimum separation was achieved using reversed-phase HPLC gradient elution with an aqueous mobile phase containing pH=6.85 potassium phosphate buffer (20 mM) and acetonitrile with a 22 °C column temperature. Under these experimental conditions, the 12 phytohormones could be separated and detected at 230 or 270 nm within 26 min. Copyright © 2013 Elsevier B.V. All rights reserved.

Phase behaviour of casein micelles and barley beta-glucan polymer molecules in dietary fibre-enriched dairy systems.

PubMed

Repin, Nikolay; Scanlon, Martin G; Fulcher, R Gary

2012-07-01

Enrichment of colloidal dairy systems with dietary fibre frequently causes quality defects because of phase separation. We investigate phase separation in skimmed milk enriched with Glucagel (a commercial product made from barley that is predominantly comprised of the polysaccharide β-glucan). The driving force for phase separation was depletion flocculation of casein micelles in the presence of molecules of the polysaccharide. Depending on the volume fraction of casein micelles and the concentration of Glucagel, the stable system phase separated either as a transient gel or as a sedimented system. The rate at which phase separation progressed also depended on the volume fraction of casein micelles and the concentration of Glucagel. To confirm the role of depletion flocculation in the phase separation process, enzymatic reduction in the molecular weight of β-glucan was shown to limit the range of attraction between micelles and allow the stable phase to exist at a higher β-glucan concentration for any given volume fraction of casein micelles. These phase diagrams will be useful to dairy product manufacturers striving to improve the nutrient profile of their products while avoiding product quality impairment. Copyright © 2012 Elsevier Inc. All rights reserved.

Conserved interdomain linker promotes phase separation of the multivalent adaptor protein Nck

PubMed Central

Banjade, Sudeep; Wu, Qiong; Mittal, Anuradha; Peeples, William B.; Pappu, Rohit V.; Rosen, Michael K.

2015-01-01

The organization of membranes, the cytosol, and the nucleus of eukaryotic cells can be controlled through phase separation of lipids, proteins, and nucleic acids. Collective interactions of multivalent molecules mediated by modular binding domains can induce gelation and phase separation in several cytosolic and membrane-associated systems. The adaptor protein Nck has three SRC-homology 3 (SH3) domains that bind multiple proline-rich segments in the actin regulatory protein neuronal Wiskott-Aldrich syndrome protein (N-WASP) and an SH2 domain that binds to multiple phosphotyrosine sites in the adhesion protein nephrin, leading to phase separation. Here, we show that the 50-residue linker between the first two SH3 domains of Nck enhances phase separation of Nck/N-WASP/nephrin assemblies. Two linear motifs within this element, as well as its overall positively charged character, are important for this effect. The linker increases the driving force for self-assembly of Nck, likely through weak interactions with the second SH3 domain, and this effect appears to promote phase separation. The linker sequence is highly conserved, suggesting that the sequence determinants of the driving forces for phase separation may be generally important to Nck functions. Our studies demonstrate that linker regions between modular domains can contribute to the driving forces for self-assembly and phase separation of multivalent proteins. PMID:26553976

A comparison of atmospheric effects on differential phase for a two-element antenna array and nearby site test interferometer

NASA Astrophysics Data System (ADS)

Morabito, David D.; D'Addario, Larry; Finley, Susan

2016-02-01

Phased arrays of reflector antennas can be used to obtain effective area and gain that are much larger than is practical with a single antenna. This technique is routinely used by NASA for receiving weak signals from deep space. Phase alignment of the signals can be disrupted by turbulence in the troposphere, which causes fluctuations in the differences of signal delays among the antennas. At the Deep Space Network stations, site test interferometers (STIs) are being used for long-term monitoring of these delay fluctuations using signals from geostationary satellites. In this paper, we compare the STI measurements with the phase variations seen by a nearby two-element array of 34 m diameter antennas tracking 8.4 GHz and 32 GHz signals from the Cassini spacecraft in orbit around Saturn. It is shown that the statistics of the STI delay fluctuations, after appropriate scaling for differences in antenna separation and elevation angle and conversion to phase at the spacecraft frequencies, provide reliable estimates of the phase fluctuations seen by the large antennas on the deep space signal. Techniques for adaptive compensation of the phase fluctuations are available when receiving a sufficiently strong signal, but compensation is often impractical or impossible when using the array for transmitting. These results help to validate the use of long-term STI data for assessing the feasibility of large transmitting arrays at various sites.

Separation between the digestive and the respiratory lumina during the human embryonic period: morphometric study along the tracheo-oesophageal septum

PubMed Central

NEBOT-CEGARRA, JOSEP; FÀBREGAS, PERE J.; CAMPILLO, MERCEDES; RICART, SILVIA

2001-01-01

An isolated tracheo-oesophageal fistula could be caused by close proximity of the epithelia of both organs (O'Rahilly & Müller, 1984; Kluth et al. 1987) at certain embryonic stages, the most frequent location being the tracheal bifurcation. Thus the relative position and degree of separation between the digestive and the respiratory tubes throughout their development may be relevant to the origin of this anomaly. The aim of this study was to analyse along the different segments of the tracheo-oesophageal septum (TES) where the closest relationship between both lumina occurred and what degree of separation was present at each segment. Computer imaging techniques were applied on cross sections of a graded series of normal human embryos (Carnegie stages (CS) 13–23). In addition, the differentiation of the primitive TES was also studied (from CS 12) by light microscopy. Between CS 13 and 16 both tubes tended to separate (phase of separation), principally at the proximal segments of the laryngopharyngeal and the tracheo-oesophageal portions of the TES. During this phase the separation between the trachea and oesophagus was wider than between the larynx and pharynx. From CS 17 to CS 23 the digestive and respiratory lumina reached their widest separation at different levels of the laryngopharyngeal portion. Below these levels they tended to come closer together, principally at the proximal segment of the tracheo-oesophageal portion, but also at the distal part of the laryngopharyngeal portion. During this phase of approximation they reached their closest relationship at the proximal (CS 17) and the distal (from CS 18) segments of the tracheo-oesophageal portion. When finally the distal segment of the trachea (which includes the bifurcation) comes closest to the oesophagus, the coats of both organs have already undergone an appreciable differentiation. According to these observations, the origin of the most frequent isolated tracheo-oesophageal fistula at the bifurcation region could not be explained from the normal development of the TES. PMID:11215762

Phase incremented echo train acquisition applied to magnetic resonance pore imaging

NASA Astrophysics Data System (ADS)

Hertel, S. A.; Galvosas, P.

2017-02-01

Efficient phase cycling schemes remain a challenge for NMR techniques if the pulse sequences involve a large number of rf-pulses. Especially complex is the Carr Purcell Meiboom Gill (CPMG) pulse sequence where the number of rf-pulses can range from hundreds to several thousands. Our recent implementation of Magnetic Resonance Pore Imaging (MRPI) is based on a CPMG rf-pulse sequence in order to refocus the effect of internal gradients inherent in porous media. While the spin dynamics for spin- 1 / 2 systems in CPMG like experiments are well understood it is still not straight forward to separate the desired pathway from the spectrum of unwanted coherence pathways. In this contribution we apply Phase Incremented Echo Train Acquisition (PIETA) to MRPI. We show how PIETA offers a convenient way to implement a working phase cycling scheme and how it allows one to gain deeper insights into the amplitudes of undesired pathways.

Broadband tunable microwave photonic phase shifter with low RF power variation in a high-Q AlN microring.

PubMed

Liu, Xianwen; Sun, Changzheng; Xiong, Bing; Wang, Jian; Wang, Lai; Han, Yanjun; Hao, Zhibiao; Li, Hongtao; Luo, Yi; Yan, Jianchang; Wei, Tong Bo; Zhang, Yun; Wang, Junxi

2016-08-01

An all-optically tunable microwave photonic phase shifter is demonstrated based on an epitaxial aluminum nitride (AlN) microring with an intrinsic quality factor of 3.2×10⁶. The microring adopts a pedestal structure, which allows overcoupling with 700 nm gap size and facilitates the fabrication process. A phase shift for broadband signals from 4 to 25 GHz is demonstrated by employing the thermo-optic effect and the separate carrier tuning technique. A phase tuning range of 0°-332° is recorded with a 3 dB radio frequency (RF) power variation and 48 mW optical power consumption. In addition, AlN exhibits intrinsic second-order optical nonlinearity. Thus, our work presents a novel platform with a low propagation loss and the capability of electro-optic modulation for applications in integrated microwave photonics.

Speed Measurement and Motion Analysis of Chang'E-3 Rover Based on Differential Phase Delay

NASA Astrophysics Data System (ADS)

Pan, C.; Liu, Q. H.; Zheng, X.; He, Q. B.; Wu, Y. J.

2015-07-01

On 2013 December 14, the Chang'E-3 made a successful soft landing on the lunar surface, and then carried out the tasks of separating the lander and the rover, and taking the photos of each other. With the same beam VLBI (Very long baseline interferometry) technique to observe the signals transmitted by the lander and the rover simultaneously, the differential phase delay between them is calculated, which can reflect a minor change of the rover's position on a scale of a few centimeters. Based on the high sensitivity of differential phase delay, the rover's speeds during 5 movements are obtained with an average of 0.056 m/s. The relationship between the rover's shake in moving process, and lunar terrain is analyzed by using the spectrum of the residual of the differential phase delay after the first-order polynomial fitting.

Speed Measurement and Motion Analysis of Chang'E-3 Rover Based on Differential Phase Delay

NASA Astrophysics Data System (ADS)

Chao, Pan; Qing-hui, Liu; Xin, Zheng; Qing-bao, He; Ya-jun, Wu

2016-04-01

On 14th December 2013, the Chang'E-3 made a successful soft landing on the lunar surface, and then carried out the tasks of separating the lander and the rover, and taking pictures of each other. With the same beam VLBI (Very Long Baseline Interferometry) technique to observe the signals transmitted by the lander and the rover simultaneously, the differential phase delay between them is calculated, which can reflect the minor changes of the rover's position on a scale of a few centimeters. Based on the high sensitivity of differential phase delay, the rover's speeds during 5 movements are obtained with an average of 0.056 m/s. The relationship between the rover's shake in the moving process and the lunar terrain is analyzed by using the spectrum of the residual of the differential phase delay after the first-order polynomial fitting.

Finite-temperature dynamic structure factor of the spin-1 XXZ chain with single-ion anisotropy

NASA Astrophysics Data System (ADS)

Lange, Florian; Ejima, Satoshi; Fehske, Holger

2018-02-01

Improving matrix-product state techniques based on the purification of the density matrix, we are able to accurately calculate the finite-temperature dynamic response of the infinite spin-1 XXZ chain with single-ion anisotropy in the Haldane, large-D , and antiferromagnetic phases. Distinct thermally activated scattering processes make a significant contribution to the spectral weight in all cases. In the Haldane phase, intraband magnon scattering is prominent, and the on-site anisotropy causes the magnon to split into singlet and doublet branches. In the large-D phase response, the intraband signal is separated from an exciton-antiexciton continuum. In the antiferromagnetic phase, holons are the lowest-lying excitations, with a gap that closes at the transition to the Haldane state. At finite temperatures, scattering between domain-wall excitations becomes especially important and strongly enhances the spectral weight for momentum transfer π .

Liquid-liquid two phase systems for the production of porous hydrogels and hydrogel microspheres for biomedical applications: A tutorial review

PubMed Central

Elbert, Donald L.

2010-01-01

Macroporous hydrogels may have direct applications in regenerative medicine as scaffolds to support tissue formation. Hydrogel microspheres may be used as drug delivery vehicles or as building blocks to assemble modular scaffolds. A variety of techniques exist to produce macroporous hydrogels and hydrogel microspheres. A subset of these relies on liquid-liquid two phase systems. Within this subset, vastly different types of polymerization processes are found. In this review, the history, terminology and classification of liquid-liquid two phase polymerization and crosslinking are described. Instructive examples of hydrogel microsphere and macroporous scaffold formation by precipitation/dispersion, emulsion and suspension polymerizations are used to illustrate the nature of these processes. The role of the kinetics of phase separation in determining the morphology of scaffolds and microspheres is also delineated. Brief descriptions of miniemulsion, microemulsion polymerization and ionotropic gelation are also included. PMID:20659596

Adaptive Sparse Representation for Source Localization with Gain/Phase Errors

PubMed Central

Sun, Ke; Liu, Yimin; Meng, Huadong; Wang, Xiqin

2011-01-01

Sparse representation (SR) algorithms can be implemented for high-resolution direction of arrival (DOA) estimation. Additionally, SR can effectively separate the coherent signal sources because the spectrum estimation is based on the optimization technique, such as the L1 norm minimization, but not on subspace orthogonality. However, in the actual source localization scenario, an unknown gain/phase error between the array sensors is inevitable. Due to this nonideal factor, the predefined overcomplete basis mismatches the actual array manifold so that the estimation performance is degraded in SR. In this paper, an adaptive SR algorithm is proposed to improve the robustness with respect to the gain/phase error, where the overcomplete basis is dynamically adjusted using multiple snapshots and the sparse solution is adaptively acquired to match with the actual scenario. The simulation results demonstrate the estimation robustness to the gain/phase error using the proposed method. PMID:22163875

Flow Separation Control Over a Ramp Using Sweeping Jet Actuators

NASA Technical Reports Server (NTRS)

Koklu, Mehti; Owens, Lewis R.

2014-01-01

Flow separation control on an adverse-pressure-gradient ramp model was investigated using various flow-control methods in the NASA Langley 15-Inch Wind Tunnel. The primary flow-control method studied used a sweeping jet actuator system to compare with more classic flow-control techniques such as micro-vortex generators, steady blowing, and steady- and unsteady-vortex generating jets. Surface pressure measurements and a new oilflow visualization technique were used to characterize the effects of these flow-control actuators. The sweeping jet actuators were run in three different modes to produce steady-straight, steady-angled, and unsteady-oscillating jets. It was observed that all of these flow-control methods are effective in controlling the separated flows on the ramp model. The steady-straight jet energizes the boundary layer by momentum addition and was found to be the least effective method for a fixed momentum coefficient. The steady-angled jets achieved better performance than the steady-straight jets because they generate streamwise vortices that energize the boundary layer by mixing high-momentum fluid with near wall low-momentum fluid. The unsteady-oscillating jets achieved the best performance by increasing the pressure recovery and reducing the downstream flow separation. Surface flow visualizations indicated that two out-of-phase counter-rotating vortices are generated per sweeping jet actuator, while one vortex is generated per vortex-generating jets. The extra vortex resulted in increased coverage, more pressure recovery, and reduced flow separation.

Separation of Single-Walled Carbon Nanotubes with DEP-FFF

NASA Technical Reports Server (NTRS)

Schmidt, Howard K.; Peng, Haiqing; Alvarez, Noe; Mendes, Manuel; Pasquali, Matteo

2011-01-01

A process using a modified dielectrophoresis device separates single-walled carbon nanotubes (SWNTs) according to their polarizability in electric fields. This depends on the size and dielectric constant of individual nanotubes and easily separates metallic from semiconducting nanotubes. Separation by length has also been demonstrated. Partial separation (enrichment) according to bandgap (which is linked to polarizability) has also been shown and can be improved to full separation of individual types of semiconducting SWNTs with better control over operational parameters and the length of SWNT starting material. This process and device can be scaled affordably to generate useful amounts of semiconducting SWNTs for electronic device development and production. In this study, a flow injection dielectrophoresis technique was used with a modified dielectrophoresis device. The length, width, and height of the modified chamber were 28, 2.5, and 0.025 cm, respectively. On the bottom of the chamber, there are two arrays of 50-m-wide, 2-m-thick gold electrodes, which are connected to an AC voltage generator and are alternately arranged so that every electrode is adjacent to two electrodes of the opposite polar. There is an additional plate electrode on the top of the chamber that is negatively biased. During the experiment, a syringe pump constantly pumps in the mobile phase, 1-percent sodium dodecylbenzene sulfonate (SDBS) solution, into the chamber. The frequency and voltage are set to 1 MHz and 10 V peak-to-peak, respectively. About 150 micro-L of SWNTs in 1- percent SDBS decanted solution are injected to the mobile phase through a septum near the entrance of the chamber. The flow rate of the mobile phase is set to 0.02 cu cm/min. The injected SWNTs sample flows through the chamber before it is lead into a fluorescence flow-through cell and collected for further analysis. The flow-through cell has three windows, thus allowing the fluorometer to collect fluorescence spectrum and visible absorption spectrums simultaneously. Dielectrophoresis field-flow fractionation (DEP-FFF) generally depends on interaction of a sedimentation force and DEP force for particle separation, and SWNTs are neutrally buoyant in water. In this innovation, the third electrode was added to create a sedimentation force based on DC electrophoresis. This makes this particular device applicable to separations on any neutrally buoyant particles in solution and a more general process for a broad range of nanomaterials sorting and separations.

Modification of linear prepolymers to tailor heterogeneous network formation through photo-initiated Polymerization-Induced Phase Separation

PubMed Central

Szczepanski, Caroline R.; Stansbury, Jeffrey W.

2015-01-01

Polymerization-induced phase separation (PIPS) was studied in ambient photopolymerizations of triethylene glycol dimethacrylate (TEGDMA) modified by poly(methyl methacrylate) (PMMA). The molecular weight of PMMA and the rate of network formation (through incident UV-irradiation) were varied to influence both the promotion of phase separation through increases in overall free energy, as well as the extent to which phase development occurs during polymerization through diffusion prior to network gelation. The overall free energy of the polymerizing system increases with PMMA molecular weight, such that PIPS is promoted thermodynamically at low loading levels (5 wt%) of a higher molecular weight PMMA (120 kDa), while a higher loading level (20 wt%) is needed to induce PIPS with lower PMMA molecular weight (11 kDa), and phase separation was not promoted at any loading level tested of the lowest molecular weight PMMA (1 kDa). Due to these differences in overall free energy, systems modified by PMMA (11 kDa) underwent phase separation via Nucleation and Growth, and systems modified by PMMA (120 kDa), followed the Spinodal Decomposition mechanism. Despite differences in phase structure, all materials form a continuous phase rich in TEGDMA homopolymer. At high irradiation intensity (Io=20mW/cm2), the rate of network formation prohibited significant phase separation, even when thermodynamically preferred. A staged curing approach, which utilizes low intensity irradiation (Io=300µW/cm2) for the first ~50% of reaction to allow phase separation via diffusion, followed by a high intensity flood-cure to achieve a high degree of conversion, was employed to form phase-separated networks with reduced polymerization stress yet equivalent final conversion and modulus. PMID:26190865

Phase separation and second-order phase transition in the phenomenological model for a Coulomb-frustrated two-dimensional system

NASA Astrophysics Data System (ADS)

Mamin, R. F.; Shaposhnikova, T. S.; Kabanov, V. V.

2018-03-01

We have considered the model of the phase transition of the second order for the Coulomb frustrated 2D charged system. The coupling of the order parameter with the charge was considered as the local temperature. We have found that in such a system, an appearance of the phase-separated state is possible. By numerical simulation, we have obtained different types ("stripes," "rings," "snakes") of phase-separated states and determined the parameter ranges for these states. Thus the system undergoes a series of phase transitions when the temperature decreases. First, the system moves from the homogeneous state with a zero order parameter to the phase-separated state with two phases in one of which the order parameter is zero and, in the other, it is nonzero (τ >0 ). Then a first-order transition occurs to another phase-separated state, in which both phases have different and nonzero values of the order parameter (for τ <0 ). Only a further decrease of temperature leads to a transition to a homogeneous ordered state.

Effect of temperature gradient on liquid-liquid phase separation in a polyolefin blend.

PubMed

Jiang, Hua; Dou, Nannan; Fan, Guoqiang; Yang, Zhaohui; Zhang, Xiaohua

2013-09-28

We have investigated experimentally the structure formation processes during phase separation via spinodal decomposition above and below the spinodal line in a binary polymer blend system exposed to in-plane stationary thermal gradients using phase contrast optical microscopy and temperature gradient hot stage. Below the spinodal line there is a coupling of concentration fluctuations and thermal gradient imposed by the temperature gradient hot stage. Also under the thermal gradient annealing phase-separated domains grow faster compared with the system under homogeneous temperature annealing on a zero-gradient or a conventional hot stage. We suggest that the in-plane thermal gradient accelerates phase separation through the enhancement in concentration fluctuations in the early and intermediate stages of spinodal decomposition. In a thermal gradient field, the strength of concentration fluctuation close to the critical point (above the spinodal line) is strong enough to induce phase separation even in one-phase regime of the phase diagram. In the presence of a temperature gradient the equilibrium phase diagrams are no longer valid, and the systems with an upper critical solution temperature can be quenched into phase separation by applying the stationary temperature gradient. The in-plane temperature gradient drives enhanced concentration fluctuations in a binary polymer blend system above and below the spinodal line.

Amide-induced phase separation of hexafluoroisopropanol-water mixtures depending on the hydrophobicity of amides.

PubMed

Takamuku, Toshiyuki; Wada, Hiroshi; Kawatoko, Chiemi; Shimomura, Takuya; Kanzaki, Ryo; Takeuchi, Munetaka

2012-06-21

Amide-induced phase separation of hexafluoro-2-propanol (HFIP)-water mixtures has been investigated to elucidate solvation properties of the mixtures by means of small-angle neutron scattering (SANS), (1)H and (13)C NMR, and molecular dynamics (MD) simulation. The amides included N-methylformamide (NMF), N-methylacetamide (NMA), and N-methylpropionamide (NMP). The phase diagrams of amide-HFIP-water ternary systems at 298 K showed that phase separation occurs in a closed-loop area of compositions as well as an N,N-dimethylformamide (DMF) system previously reported. The phase separation area becomes wider as the hydrophobicity of amides increases in the order of NMF < NMA < DMF < NMP. Thus, the evolution of HFIP clusters around amides due to the hydrophobic interaction gives rise to phase separation of the mixtures. In contrast, the disruption of HFIP clusters causes the recovery of the homogeneity of the ternary systems. The present results showed that HFIP clusters are evolved with increasing amide content to the lower phase separation concentration in the same mechanism among the four amide systems. However, the disruption of HFIP clusters in the NMP and DMF systems with further increasing amide content to the upper phase separation concentration occurs in a different way from those in the NMF and NMA systems.

Phase Separation and Crystallization of Hemoglobin C in Transgenic Mouse and Human Erythrocytes

PubMed Central

Canterino, Joseph E.; Galkin, Oleg; Vekilov, Peter G.; Hirsch, Rhoda Elison

2008-01-01

Individuals expressing hemoglobin C (β6 Glu→Lys) present red blood cells (RBC) with intraerythrocytic crystals that form when hemoglobin (Hb) is oxygenated. Our earlier in vitro liquid-liquid (L-L) phase separation studies demonstrated that liganded HbC exhibits a stronger net intermolecular attraction with a longer range than liganded HbS or HbA, and that L-L phase separation preceded and enhanced crystallization. We now present evidence for the role of phase separation in HbC crystallization in the RBC, and the role of the RBC membrane as a nucleation center. RBC obtained from both human homozygous HbC patients and transgenic mice expressing only human HbC were studied by bright-field and differential interference contrast video-enhanced microscopy. RBC were exposed to hypertonic NaCl solution (1.5–3%) to induce crystallization within an appropriate experimental time frame. L-L phase separation occurred inside the RBC, which in turn enhanced the formation of intraerythrocytic crystals. RBC L-L phase separation and crystallization comply with the thermodynamic and kinetics laws established through in vitro studies of phase transformations. This is the first report, to the best of our knowledge, to capture a temporal view of intraerythrocytic HbC phase separation, crystal formation, and dissolution. PMID:18621841

Phase separations in mixtures of a liquid crystal and a nanocolloidal particle.

PubMed

Matsuyama, Akihiko

2009-11-28

We present a mean field theory to describe phase separations in mixtures of a liquid crystal and a nanocolloidal particle. By taking into account a nematic, a smectic A ordering of the liquid crystal, and a crystalline ordering of the nanoparticle, we calculate the phase diagrams on the temperature-concentration plane. We predict various phase separations, such as a smectic A-crystal phase separation and a smectic A-isotropic-crystal triple point, etc., depending on the interactions between the liquid crystal and the colloidal surface. Inside binodal curves, we find new unstable and metastable regions, which are important in the phase ordering dynamics. We also find a crystalline ordering of the nanoparticles dispersed in a smectic A phase and a nematic phase. The cooperative phenomena between liquid-crystalline ordering and crystalline ordering induce a variety of phase diagrams.

Kinetics of phase separation and coarsening in dilute surfactant pentaethylene glycol monododecyl ether solutions

NASA Astrophysics Data System (ADS)

Tanaka, S.; Kubo, Y.; Yokoyama, Y.; Toda, A.; Taguchi, K.; Kajioka, H.

2011-12-01

We investigated the phase separation phenomena in dilute surfactant pentaethylene glycol monodedecyl ether (C12E5) solutions focusing on the growth law of separated domains. The solutions confined between two glass plates were found to exhibit the phase inversion, characteristic of the viscoelastic phase separation; the majority phase (water-rich phase) nucleated as droplets and the minority phase (micelle-rich phase) formed a network temporarily, then they collapsed into an usual sea-island pattern where minority phase formed islands. We found from the real-space microscopic imaging that the dynamic scaling hypothesis did not hold throughout the coarsening process. The power law growth of the domains with the exponent close to 1/3 was observed even though the coarsening was induced mainly by hydrodynamic flow, which was explained by Darcy's law of laminar flow.

Iodination and stability of somatostatin analogues: comparison of iodination techniques. A practical overview.

PubMed

de Blois, Erik; Chan, Ho Sze; Breeman, Wouter A P

2012-01-01

For iodination ((125/127)I) of tyrosine-containing peptides, chloramin-T, Pre-Coated Iodo-Gen(®) tubes and Iodo-Beads(®) (Pierce) are commonly used for in vitro radioligand investigations and there have been reliant vendors hereof for decades. However, commercial availability of these radio-iodinated peptides is decreasing. For continuation of our research in this field we investigated and optimized (radio-)iodination of somatostatin analogues. In literature, radioiodination using here described somatostatin analogues and iodination techniques are described separately. Here we present an overview, including High Performance Liquid Chromatography (HPLC) separation and characterisation by mass spectrometry, to obtain mono- and di-iodinated analogues. Reaction kinetics of (125/127)I iodinated somatostatin analogues were investigated as function of reaction time and concentration of reactants, including somatostatin analogues, iodine and oxidizing agent. To our knowledge, for the here described somatostatin analogues, no (127)I iodination and optimization are described. (Radio-)iodinated somatostatin analogues could be preserved with a >90% radiochemical purity for 1 month after reversed phase HPLC-purification.

Quantitative analysis of PEG-functionalized colloidal gold nanoparticles using charged aerosol detection.

PubMed

Smith, Mackensie C; Crist, Rachael M; Clogston, Jeffrey D; McNeil, Scott E

2015-05-01

Surface characteristics of a nanoparticle, such as functionalization with polyethylene glycol (PEG), are critical to understand and achieve optimal biocompatibility. Routine physicochemical characterization such as UV-vis spectroscopy (for gold nanoparticles), dynamic light scattering, and zeta potential are commonly used to assess the presence of PEG. However, these techniques are merely qualitative and are not sensitive enough to distinguish differences in PEG quantity, density, or presentation. As an alternative, two methods are described here which allow for quantitative measurement of PEG on PEGylated gold nanoparticles. The first, a displacement method, utilizes dithiothreitol to displace PEG from the gold surface. The dithiothreitol-coated gold nanoparticles are separated from the mixture via centrifugation, and the excess dithiothreitol and dissociated PEG are separated through reversed-phase high-performance liquid chromatography (RP-HPLC). The second, a dissolution method, utilizes potassium cyanide to dissolve the gold nanoparticles and liberate PEG. Excess CN(-), Au(CN)2 (-), and free PEG are separated using RP-HPLC. In both techniques, the free PEG can be quantified against a standard curve using charged aerosol detection. The displacement and dissolution methods are validated here using 2-, 5-, 10-, and 20-kDa PEGylated 30-nm colloidal gold nanoparticles. Further value in these techniques is demonstrated not only by quantitating the total PEG fraction but also by being able to be adapted to quantitate the free unbound PEG and the bound PEG fractions. This is an important distinction, as differences in the bound and unbound PEG fractions can affect biocompatibility, which would not be detected in techniques that only quantitate the total PEG fraction.

HPLC-Chip/MS Technology in Proteomic Profiling

NASA Astrophysics Data System (ADS)

Vollmer, Martin; van de Goor, Tom

HPLC-chip/MS is a novel nanoflow analytical technology conducted on a microfabricated chip that allows for highly efficient HPLC separation and superior sensitive MS detection of complex proteomic mixtures. This is possible through on-chip preconcentration and separation with fluidic connection made automatically in a leak-tight fashion. Minimum precolumn and postcolumn peak dispersion and uncompromised ease of use result in compounds eluting in bands of only a few nanoliters. The chip is fabricated out of bio-inert polyimide-containing channels and integrated chip structures, such as an electrospray emitter, columns, and frits manufactured by laser ablation technology. Meanwhile, a variety of HPLC-chips differing in design and stationary phase are commercially available, which provide a comprehensive solution for applications in proteomics, glycomics, biomarker, and pharmaceutical discovery. The HPLC-chip can also be easily integrated into a multidimensional separation workflow where different orthogonal separation techniques are combined to solve a highly complex separation problems. In this chapter, we describe in detail the methodological chip usage and functionality and its application in the elucidation of the protein profile of human nucleoli.

Method and apparatus for ion mobility spectrometry with alignment of dipole direction (IMS-ADD)

DOEpatents

Shvartsburg, Alexandre A [Richland, WA; Tang, Keqi [Richland, WA; Smith, Richard D [Richland, WA

2007-01-30

Techniques and instrumentation are described for analyses of substances, including complex samples/mixtures that require separation prior to characterization of individual components. A method is disclosed for separation of ion mixtures and identification of ions, including protein and other macromolecular ions and their different structural isomers. Analyte ions are not free to rotate during the separation, but are substantially oriented with respect to the drift direction. Alignment is achieved by applying, at a particular angle to the drift field, a much stronger alternating electric field that "locks" the ion dipoles with moments exceeding a certain value. That value depends on the buffer gas composition, pressure, and temperature, but may be as low as .about.3 Debye under certain conditions. The presently disclosed method measures the direction-specific cross-sections that provide the structural information complementing that obtained from known methods, and, when coupled to those methods, increases the total peak capacity and specificity of gas-phase separations. Simultaneous 2-D separations by direction-specific cross sections along and orthogonally to the ion dipole direction are also possible.

Liquid Crystals in Chromatography

NASA Astrophysics Data System (ADS)

Witkiewicz, Zygfryd

The following sections are included: * INTRODUCTION * LIQUID CRYSTALS SUITABLE FOR GAS CHROMATOGRAPHY * Monomeric Liquid Crystal Stationary Phases * Polymeric Liquid Crystal Stationary Phases * Polymeric Liquid Crystal Stationary Phases * Conventional Analytical Columns * Capillary Columns * FACTORS AFFECTING THE CHROMATOGRAPHIC SEPARATIONS ON LIQUID CRYSTAL STATIONARY PHASES * Kind of Mesophase of the Liquid Crystal * Molecular Structure of the Liquid Crystals and of the Chromatographed Substances * Substrate on which the Liquid Crystal is Deposited * ANALYTICAL APPLICATIONS OF LIQUID CRYSTAL STATIONARY PHASES IN GAS CHROMATOGRAPHY * Separation of Isomers of Benzene and Naphthalene Derivatives * Separation of Alkane and Alkene Isomers * Separation of Mixtures of Benzene and Aliphatic Hydrocarbon Derivatives Containing Heteroatoms * Separation of Polynuclear Hydrocarbons * INVESTIGATION OF THE PROPERTIES OF LIQUID CRYSTALS BY GAS CHROMATOGRAPHY * APPLICATION OF LIQUID CRYSTALS IN LIQUID CHROMATOGRAPHY * Column Chromatography * Thin-Layer Chromatography * APPLICATION OF LIQUID CRYSTAL STATIONARY PHASES IN SUPERCRITICAL FLUID CHROMATOGRAPHY * FINAL REMARKS * References

Simulations to Predict the Phase Behavior and Structure of Multipolar Colloidal Particles

NASA Astrophysics Data System (ADS)

Rutkowski, David Matthew

Colloidal particles with anisotropic charge distributions can assemble into a number of interesting structures including chains, lattices and micelles that could be useful in biotechnology, optics and electronics. The goal of this work is to understand how the properties of the colloidal particles, such as their charge distribution or shape, affect the selfassembly and phase behavior of collections of such particles. The specific aim of this work is to understand how the separation between a pair of oppositely signed charges affects the phase behavior and structure of assemblies of colloidal particles. To examine these particles, we have used both discontinuous molecular dynamics (DMD) and Monte Carlo (MC) simulation techniques. In our first study of colloidal particles with finite charge separation, we simulate systems of 2-D colloidal rods with four possible charge separations. Our simulations show that the charge separation does indeed have a large effect on the phase behavior as can be seen in the phase diagrams we construct for these four systems in the area fraction-reduced temperature plane. The phase diagrams delineate the boundaries between isotropic fluid, string-fluid and percolated fluid for all systems considered. In particular, we find that coarse gel-like structures tend to form at large charge separations while denser aggregates form at small charge separations, suggesting a route to forming low volume gels by focusing on systems with large charge separations. Next we examine systems of circular particles with four embedded charges of alternating sign fixed to a triangular lattice. This system is found to form a limit periodic structure, a theoretical structure with an infinite number of phase transitions, under specific conditions. The limit-periodic structure only forms when the rotation of the particles in the system is restricted to increments of pi/3. When the rotation is restricted to increments of th/6 or the rotation is continuous, related structures form including a striped phase and a phase with nematic order. Neither the distance from the point charges to the center of the particle nor the angle between the charges influences whether the system forms a limit-periodic structure, suggesting that point quadrupoles may also be able to form limit-periodic structures. Results from these simulations will likely aid in the quest to find an experimental realization of a limit-periodic structure. Next we examine the effect of charge separation on the self-assembly of systems of 2-D colloidal particles with off-center extended dipoles. We simulate systems with both small and large charge separations for a set of displacements of the dipole from the particle center. Upon cooling, these particles self-assemble into closed, cyclic structures at large displacements including dimers, triangular shapes and square shapes, and chain-like structures at small displacements. At extremely low temperatures, the cyclic structures form interesting lattices with particles of similar chirality grouped together. Results from this work could aid in the experimental construction of open lattice-like structures that could find use in photonic applications. Finally, we present work in collaboration with Drs. Bhuvnesh Bharti and Orlin Velev in which we investigate how the surface coverage affects the self-assembly of systems of Janus particles coated with both an iron oxide and fatty acid chain layer. We model these particles by decorating a sphere with evenly dispersed points that interact with points on other spheres through square-well interactions. The interactions are designed to mimic specific coverage values for the iron oxide/fatty acid chain layer. Structures similar to those found in experiment form readily in the simulations. The number of clusters formed as a function of surface coverage agrees well with experiment. The aggregation behavior of these novel particles can therefore, be described by a relatively simple model.

Thermal cycling effects on static and dynamic properties of a phase separated manganite

NASA Astrophysics Data System (ADS)

Sacanell, J.; Sievers, B.; Quintero, M.; Granja, L.; Ghivelder, L.; Parisi, F.

2018-06-01

In this work we address the interplay between two phenomena which are signatures of the out-of-equilibrium state in phase separated manganites: irreversibility against thermal cycling and aging/rejuvenation process. The sample investigated is La0.5Ca0.5MnO3, a prototypical manganite exhibiting phase separation. Two regimes for isothermal relaxation were observed according to the temperature range: for T > 100 K, aging/rejuvenation effects are observed, while for T < 100 K an irreversible aging was found. Our results show that thermal cycles act as a tool to unveil the dynamical behavior of the phase separated state in manganites, revealing the close interplay between static and dynamic properties of phase separated manganites.

Development of Online Spectroscopic pH Monitoring for Nuclear Fuel Reprocessing Plants: Weak Acid Schemes.

PubMed

Casella, Amanda J; Ahlers, Laura R H; Campbell, Emily L; Levitskaia, Tatiana G; Peterson, James M; Smith, Frances N; Bryan, Samuel A

2015-05-19

In nuclear fuel reprocessing, separating trivalent minor actinides and lanthanide fission products is extremely challenging and often necessitates tight pH control in TALSPEAK (Trivalent Actinide-Lanthanide Separation by Phosphorus reagent Extraction from Aqueous Komplexes) separations. In TALSPEAK and similar advanced processes, aqueous pH is one of the most important factors governing the partitioning of lanthanides and actinides between an aqueous phase containing a polyaminopolycarboxylate complexing agent and a weak carboxylic acid buffer and an organic phase containing an acidic organophosphorus extractant. Real-time pH monitoring would significantly increase confidence in the separation performance. Our research is focused on developing a general method for online determination of the pH of aqueous solutions through chemometric analysis of Raman spectra. Spectroscopic process-monitoring capabilities, incorporated in a counter-current centrifugal contactor bank, provide a pathway for online, real-time measurement of solution pH. The spectroscopic techniques are process-friendly and can be easily configured for online applications, whereas classic potentiometric pH measurements require frequent calibration/maintenance and have poor long-term stability in aggressive chemical and radiation environments. Raman spectroscopy discriminates between the protonated and deprotonated forms of the carboxylic acid buffer, and the chemometric processing of the Raman spectral data with PLS (partial least-squares) regression provides a means to quantify their respective abundances and therefore determine the solution pH. Interpretive quantitative models have been developed and validated under a range of chemical composition and pH conditions using a lactic acid/lactate buffer system. The developed model was applied to new spectra obtained from online spectral measurements during a solvent extraction experiment using a counter-current centrifugal contactor bank. The model predicted the pH of this validation data set within 11% for pH > 2, thus demonstrating that this technique could provide the capability of monitoring pH online in applications such as nuclear fuel reprocessing.

Probing the Effects of Templating on the UV and Visible Light Photocatalytic Activity of Porous Nitrogen-Modified Titania Monoliths for Dye Removal.

PubMed

Nursam, Natalita M; Wang, Xingdong; Tan, Jeannie Z Y; Caruso, Rachel A

2016-07-13

Porous nitrogen-modified titania (N-titania) monoliths with tailored morphologies were prepared using phase separation and agarose gel templating techniques. The doping and templating process were simultaneously carried out in a one-pot step using alcohol amine-assisted sol-gel chemistry. The amount of polymer used in the monoliths that were prepared using phase separation was shown to affect both the physical and optical properties: higher poly(ethylene glycol) content increased the specific surface area, porosity, and visible light absorption of the final materials. For the agarose-templated monoliths, the infiltration conditions affected the monolith morphology. A porous monolith with high surface area and the least shrinkage was obtained when the N containing alkoxide precursor was infiltrated into the agarose scaffolds at 60 °C. The effect of the diverse porous morphologies on the photocatalytic activity of N-titania was studied for the decomposition of methylene blue (MB) under visible and UV light irradiation. The highest visible light activity was achieved by the agarose-templated N-titania monolith, in part due to higher N incorporation. This sample also showed better UV activity, partly because of the higher specific surface area (up to 112 m(2) g(-1)) compared to the phase separation-induced monoliths (up to 103 m(2) g(-1)). Overall, agarose-templated, porous N-titania monoliths provided better features for effectively removing the MB contaminant.

Stress-Triggered Phase Separation Is an Adaptive, Evolutionarily Tuned Response

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

Riback, Joshua A.; Katanski, Christopher D.; Kear-Scott, Jamie L.

In eukaryotic cells, diverse stresses trigger coalescence of RNA-binding proteins into stress granules. In vitro, stress-granule-associated proteins can demix to form liquids, hydrogels, and other assemblies lacking fixed stoichiometry. Observing these phenomena has generally required conditions far removed from physiological stresses. We show that poly(A)-binding protein (Pab1 in yeast), a defining marker of stress granules, phase separates and forms hydrogels in vitro upon exposure to physiological stress conditions. Other RNA-binding proteins depend upon low-complexity regions (LCRs) or RNA for phase separation, whereas Pab1’s LCR is not required for demixing, and RNA inhibits it. Based on unique evolutionary patterns, we createmore » LCR mutations, which systematically tune its biophysical properties and Pab1 phase separation in vitro and in vivo. Mutations that impede phase separation reduce organism fitness during prolonged stress. Poly(A)-binding protein thus acts as a physiological stress sensor, exploiting phase separation to precisely mark stress onset, a broadly generalizable mechanism.« less

Method for separating water soluble organics from a process stream by aqueous biphasic extraction

DOEpatents

Chaiko, David J.; Mego, William A.

1999-01-01

A method for separating water-miscible organic species from a process stream by aqueous biphasic extraction is provided. An aqueous biphase system is generated by contacting a process stream comprised of water, salt, and organic species with an aqueous polymer solution. The organic species transfer from the salt-rich phase to the polymer-rich phase, and the phases are separated. Next, the polymer is recovered from the loaded polymer phase by selectively extracting the polymer into an organic phase at an elevated temperature, while the organic species remain in a substantially salt-free aqueous solution. Alternatively, the polymer is recovered from the loaded polymer by a temperature induced phase separation (cloud point extraction), whereby the polymer and the organic species separate into two distinct solutions. The method for separating water-miscible organic species is applicable to the treatment of industrial wastewater streams, including the extraction and recovery of complexed metal ions from salt solutions, organic contaminants from mineral processing streams, and colorants from spent dye baths.

Two-leg ladder systems with dipole–dipole Fermion interactions

NASA Astrophysics Data System (ADS)

Mosadeq, Hamid; Asgari, Reza

2018-05-01

The ground-state phase diagram of a two-leg fermionic dipolar ladder with inter-site interactions is studied using density matrix renormalization group (DMRG) techniques. We use a state-of-the-art implementation of the DMRG algorithm and finite size scaling to simulate large system sizes with high accuracy. We also consider two different model systems and explore stable phases in half and quarter filling factors. We find that in the half filling, the charge and spin gaps emerge in a finite value of the dipole–dipole and on-site interactions. In the quarter filling case, s-wave superconducting state, charge density wave, homogenous insulating and phase separation phases occur depend on the interaction values. Moreover, in the dipole–dipole interaction, the D-Mott phase emerges when the hopping terms along the chain and rung are the same, whereas, this phase has been only proposed for the anisotropic Hubbard model. In the half filling case, on the other hand, there is either charge-density wave or charged Mott order phase depends on the orientation of the dipole moments of the particles with respect to the ladder geometry.