Control of composition and crystallinity in hydroxyapatite films deposited by electron cyclotron resonance plasma sputtering

NASA Astrophysics Data System (ADS)

Akazawa, Housei; Ueno, Yuko

2014-01-01

Hydroxyapatite (HAp) films were deposited by electron cyclotron resonance plasma sputtering under a simultaneous flow of H2O vapor gas. Crystallization during sputter-deposition at elevated temperatures and solid-phase crystallization of amorphous films were compared in terms of film properties. When HAp films were deposited with Ar sputtering gas at temperatures above 460 °C, CaO byproducts precipitated with HAp crystallites. Using Xe instead of Ar resolved the compositional problem, yielding a single HAp phase. Preferentially c-axis-oriented HAp films were obtained at substrate temperatures between 460 and 500 °C and H2O pressures higher than 1×10-2 Pa. The absorption signal of the asymmetric stretching mode of the PO43- unit (ν3) in the Fourier-transform infrared absorption (FT-IR) spectra was the narrowest for films as-crystallized during deposition with Xe, but widest for solid-phase crystallized films. While the symmetric stretching mode of PO43- (ν1) is theoretically IR-inactive, this signal emerged in the FT-IR spectra of solid-phase crystallized films, but was absent for as-crystallized films, indicating superior crystallinity for the latter. The Raman scattering signal corresponding to ν1 PO43- sensitively reflected this crystallinity. The surface hardness of as-crystallized films evaluated by a pencil hardness test was higher than that of solid-phase crystallized films.

High-Pressure Synchrotron Infrared Absorption and Raman Spectroscopy of ζ-N_2

NASA Astrophysics Data System (ADS)

Gregoryanz, E.; Goncharov, A. F.; Mao, H. K.; Hemley, R. J.

2000-03-01

Infrared mid-IR and Raman spectra of high-pressure, low-temperature phases of solid nitrogen have been measured to above 40 GPa. The transition to the lower-symmetry ordered phase ζ at 21 GPa, reported by Schiferl et al. [1]. has been confirmed. We observe three Raman-active and two IR components of the nu2 stretching mode (disk-like molecules) and only one Raman-active component of the nu1 mode (sphere-like molecules). All the vibron modes increase frequency with pressure. The structure of ζ-N2 phase is discussed. [1] Schiferl et al., J. Phys. Chem., 89, 2324 (1985).

Fabrication of a novel hydrophobic/ion-exchange mixed-mode adsorbent for the dispersive solid-phase extraction of chlorophenols from environmental water samples.

PubMed

Gao, Li; Wei, Yinmao

2016-08-01

A novel mixed-mode adsorbent was prepared by functionalizing silica with tris(2-aminoethyl)amine and 3-phenoxybenzaldehyde as the main mixed-mode scaffold due to the presence of the plentiful amino groups and benzene rings in their molecules. The adsorption mechanism was probed with acidic, natural and basic compounds, and the mixed hydrophobic and ion-exchange interactions were found to be responsible for the adsorption of analytes. The suitability of dispersive solid-phase extraction was demonstrated in the determination of chlorophenols in environmental water. Several parameters, including sample pH, desorption solvent, ionic strength, adsorbent dose, and extraction time were optimized. Under the optimal extraction conditions, the proposed dispersive solid-phase extraction coupled with high-performance liquid chromatography showed good linearity range and acceptable limits of detection (0.22∽0.54 ng/mL) for five chlorophenols. Notably, the higher extraction recoveries (88.7∽109.7%) for five chlorophenols were obtained with smaller adsorbent dose (10 mg) and shorter extraction time (15 min) compared with the reported methods. The proposed method might be potentially applied in the determination of trace chlorophenols in real water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Rayleigh-type waves in nonlocal micropolar solid half-space.

PubMed

Khurana, Aarti; Tomar, S K

2017-01-01

Propagation of Rayleigh type surface waves in nonlocal micropolar elastic solid half-space has been investigated. Two modes of Rayleigh-type waves are found to propagate under certain approximations. Frequency equations of these Rayleigh type modes and their conditions of existence have been derived. These frequency equations are found to be dispersive in character due to the presence of micropolarity and nonlocality parameters in the medium. One of the frequency equations is a counterpart of the classical Rayleigh waves and the other is new and has appeared due to micropolarity of the medium. Phase speeds of these waves are computed numerically for Magnesium crystal and their variation against wavenumber are presented graphically. Comparisons have been made between the phase speeds of Rayleigh type waves through nonlocal micropolar, local micropolar and elastic solid half-spaces. Copyright © 2016 Elsevier B.V. All rights reserved.

Headspace and direct immersion solid phase microextraction procedures for selenite determination in urine, saliva and milk by gas chromatography mass spectrometry.

PubMed

Kapsimali, D C; Zachariadis, G A

2009-10-01

Two solid phase microextraction modes were investigated and compared for their performance on the determination of selenites in various biological liquids like human urine and saliva and various types of milk. Using sodium tetraethylborate (NaBEt(4)) as ethylating reagent, selenites are converted in situ to volatile diethylselenides (DESe) in aqueous medium. The derivative is collected in situ by solid phase microextraction (SPME) using a silica fiber coated with poly(dimethylsiloxane) (PDMS) either from the headspace (HS-SPME) or directly from the liquid phase (LP-SPME) and finally determined by capillary GC/MS. Under optimum conditions of SPME, the GC separation was also optimized. Between the two examined microextraction techniques, direct immersion of the PDMS fiber in the liquid phase was proved less satisfactory. In contrast, the headspace procedure appears to be more efficient. The quantification of selenites was achieved in SIM mode with good analytical performance. A non-fat milk powder certified reference material was analyzed to evaluate the accuracy of the method. The overall precision of the method was ranged between 6.2% and 9.7%. Detection limits achieved were 0.05microgL(-1) for human urine, 0.08microgL(-1) for saliva and 0.03-0.06microgL(-1) in various milk matrices.

Yield stress in amorphous solids: A mode-coupling-theory analysis

NASA Astrophysics Data System (ADS)

Ikeda, Atsushi; Berthier, Ludovic

2013-11-01

The yield stress is a defining feature of amorphous materials which is difficult to analyze theoretically, because it stems from the strongly nonlinear response of an arrested solid to an applied deformation. Mode-coupling theory predicts the flow curves of materials undergoing a glass transition and thus offers predictions for the yield stress of amorphous solids. We use this approach to analyze several classes of disordered solids, using simple models of hard-sphere glasses, soft glasses, and metallic glasses for which the mode-coupling predictions can be directly compared to the outcome of numerical measurements. The theory correctly describes the emergence of a yield stress of entropic nature in hard-sphere glasses, and its rapid growth as density approaches random close packing at qualitative level. By contrast, the emergence of solid behavior in soft and metallic glasses, which originates from direct particle interactions is not well described by the theory. We show that similar shortcomings arise in the description of the caging dynamics of the glass phase at rest. We discuss the range of applicability of mode-coupling theory to understand the yield stress and nonlinear rheology of amorphous materials.

Failure Mode Analysis of V-Shaped Pyrotechnically Actuated Valves

NASA Technical Reports Server (NTRS)

Sachdev, Jai S.; Hosangadi, A.; Chenoweth, James D.; Saulsberry, Regor L.; McDougle, Stephen H.

2012-01-01

Current V-shaped stainless steel pyrovalve initiators have rectified many of the deficiencies of the heritage Y-shaped aluminum design. However, a credible failure mode still exists for dual simultaneous initiator (NSI) firings in which low temperatures were detected at the booster cap and less consistent ignition was observed than when a single initiator was fired. In order to asses this issue, a numerical framework has been developed for predicting the flow through pyrotechnically actuated valves. This framework includes a fully coupled solution of the gas-phase equation with a non-equilibrium dispersed phase for solid particles as well as the capability to model conjugate gradient heat transfer to the booster cap. Through a hierarchy of increasingly complex simulations, a hypothesis for the failure mode of the nearly simultaneous dual NSI firings has been proven. The simulations indicate that the failure mode for simultaneous dual NSI firings may be caused by flow interactions between the flame channels. The shock waves from each initiator interact in the booster cavity resulting in a high pressure that prevents the gas and particulate velocity from rising in the booster cap region. This impedes the bulk of the particulate phase from impacting the booster cap and reduces the heat transfer to the booster cap since the particles do not impact it. Heat transfer calculations to the solid metal indicate that gas-phase convective heat transfer may not be adequate by itself and that energy transfer from the particulate phase may be crucial for the booster cap burn through.

Quantitative ionspray liquid chromatographic/tandem mass spectrometric determination of reserpine in equine plasma.

PubMed

Anderson, M A; Wachs, T; Henion, J D

1997-02-01

A method based on ionspray liquid chromatography/tandem mass spectrometry (LC/MS/MS) was developed for the determination of reserpine in equine plasma. A comparison was made of the isolation of reserpine from plasma by liquid-liquid extraction and by solid-phase extraction. A structural analog, rescinnamine, was used as the internal standard. The reconstituted extracts were analyzed by ionspray LC/MS/MS in the selected reaction monitoring (SRM) mode. The calibration graph for reserpine extracted from equine plasma obtained using liquid-liquid extraction was linear from 10 to 5000 pg ml-1 and that using solid-phase extraction from 100 to 5000 pg ml-1. The lower level of quantitation (LLQ) using liquid-liquid and solid-phase extraction was 50 and 200 pg ml-1, respectively. The lower level of detection for reserpine by LC/MS/MS was 10 pg ml-1. The intra-assay accuracy did not exceed 13% for liquid-liquid and 12% for solid-phase extraction. The recoveries for the LLQ were 68% for liquid-liquid and 58% for solid-phase extraction.

SPECTRAL AND MODE PROPERTIES OF SOLID-STATE LASERS AND OPTICAL DYNAMIC EFFECTS.

DTIC Science & Technology

LASERS , OPTICAL PROPERTIES), THERMAL PROPERTIES, FREQUENCY, RUBY, KERR CELLS, ELECTROMAGNETIC PULSES, PHASE LOCKED SYSTEMS, GARNET, NEODYMIUM, CAVITY RESONATORS, INTERFEROMETERS, LIGHT PULSES, PROPAGATION

Introduction to the Solid State Based Interior Lighting System for ISS

NASA Technical Reports Server (NTRS)

Maida, James C.

2014-01-01

Solid state lighting assembly (SSLA) were designed to replace general luminaire assembly (GLA) for both general interior illumination and improved circadian rhythm through melatonin control using multiple spectrums. To accomplish these goals, the light is design to operate in 3 modes with 3 distinct spectrum. The different spectrum provide control of the blue portion of the light which impacts melatonin production in humans which impacts sleep. General mode is a 4500K "neutral" light spectrum intended to the be the default mode of operation for day to day operations. Pre-sleep mode is a 2700K "warm" light spectrum intended to be used by the crew at the end of the work day. Phase-shift mode is a 6500K "cool" light spectrum intended to be used for altering the crew's sleep patterns.

Raman and infrared spectroscopic investigations of a ferroelastic phase transition in B a2ZnTe O6 double perovskite

NASA Astrophysics Data System (ADS)

Moreira, Roberto L.; Lobo, Ricardo P. S. M.; Ramos, Sérgio L. L. M.; Sebastian, Mailadil T.; Matinaga, Franklin M.; Righi, Ariete; Dias, Anderson

2018-05-01

The low-temperature vibrational properties of B a2ZnTe O6 double-perovskite ceramics obtained by the solid-state route were investigated by Raman scattering and Fourier-transform infrared reflectivity. We found that this material undergoes a reversible ferroelastic phase transition at around 140 K, well compatible with a recently proposed rhombohedral-to-monoclinic structural change that would occur below 165 K. Complementary calorimetric measurements showed that the phase transition has a first-order character, with an entropy jump compatible with a displacive mechanism. The vibrational spectra show clearly the splitting of the doubly degenerate E modes into nondegenerate representations of the low-symmetry phase. In particular, the lowest-frequency Raman mode presents soft-mode behavior and splits below the critical temperature, confirming the in-plane ferroelastic deformation in the low-temperature phase.

Solid deuterated water in space: detection constraints from laboratory experiments

NASA Astrophysics Data System (ADS)

Urso, R. G.; Palumbo, M. E.; Baratta, G. A.; Scirè, C.; Strazzulla, G.

2018-06-01

The comparison between astronomical spectra and laboratory experiments is fundamental to spread light on the structure and composition of ices found in interstellar dense molecular clouds and in Solar System bodies. Water is among the most abundant solid-phase species observed in these environments, and several attempts have been made to investigate the presence of its solid-phase isotopologues. In particular, the detection of the O-D stretching mode band at 4.1 μm due to both D2O and HDO within icy grain mantles is still under debate, and no detection have been reported about the presence of these species within icy bodies in the Solar System yet. In the near future, an important contribution could derive from the data acquired in the O-D stretching mode spectral range by the sensitive instruments on board the James Webb Space Telescope. With this in mind, we performed several laboratory experiments to study the O-D stretching mode band in solid mixtures containing water and deuterated water deposited in the temperature range between 17 and 155 K, in order to simulate astrophysical relevant conditions. Furthermore, samples have been studied at various temperature and irradiated with energetic ions (200 keV H+) in order to study the effects induced by both thermal and energetic processing. Our results provide some constraints on the detection of the 4.1 μm band in astronomical environments.

Modulated structure and molecular dissociation of solid chlorine at high pressures

NASA Astrophysics Data System (ADS)

Li, Peifang; Gao, Guoying; Ma, Yanming

2012-08-01

Among diatomic molecular halogen solids, high pressure structures of solid chlorine (Cl2) remain elusive and least studied. We here report first-principles structural search on solid Cl2 at high pressures through our developed particle-swarm optimization algorithm. We successfully reproduced the known molecular Cmca phase (phase I) at low pressure and found that it remains stable up to a high pressure 142 GPa. At 150 GPa, our structural searches identified several energetically competitive, structurally similar, and modulated structures. Analysis of the structural results and their similarity with those in solid Br2 and I2, it was suggested that solid Cl2 adopts an incommensurate modulated structure with a modulation wave close to 2/7 in a narrow pressure range 142-157 GPa. Eventually, our simulations at >157 GPa were able to predict the molecular dissociation of solid Cl2 into monatomic phases having body centered orthorhombic (bco) and face-centered cubic (fcc) structures, respectively. One unique monatomic structural feature of solid Cl2 is the absence of intermediate body centered tetragonal (bct) structure during the bco → fcc transition, which however has been observed or theoretically predicted in solid Br2 and I2. Electron-phonon coupling calculations revealed that solid Cl2 becomes superconductors within bco and fcc phases possessing a highest superconducting temperature of 13.03 K at 380 GPa. We further probed the molecular Cmca → incommensurate phase transition mechanism and found that the softening of the Ag vibrational (rotational) Raman mode in the Cmca phase might be the driving force to initiate the transition.

Research Laboratory of Electronic Progress Report Number 135.

DTIC Science & Technology

1993-06-01

78 @ 1.12 Ultrashort Pulse Generation in Solid State Lasers ...generation the use of intracavity self-phase-modulation and of ultrashort laser pulses is essential for studies of negative group velocity dispersion... pulses . Our studies focus on exploiting mode locked solid state lasers . While the dominant the short pulse durations and high peak intensity of effect of

ON SITE SOLID-PHASE EXTRACTION AND LABORATORY ANALYSIS OF ULTRA-TRACE SYNTHETIC MUSKS IN MUNICIPAL SEWAGE EFFLUENT USING GAS CHROMATOGRAPHY-MASS SPECTROMETRY. FULL-SCAN MODE

EPA Science Inventory

Fragrance materials such as synthetic musks in aqueous samples, are normally determined by gas chromatography/mass spectrometry in the selected ion monitoring (SIM) mode to provide maximum sensitivity after liquid-liquid extraction of I -L samples. Full-scan mass spectra are requ...

Laser Raman spectroscopy of some local anesthetics

NASA Astrophysics Data System (ADS)

Alcolea, M.; Sigüenza, C.; Santos, M.; Gonzalez-Diaz, P. F.

1986-03-01

The Raman spectra of benzocaine and procaine hydrochlorides in solid phase are reported. From the assigned inversion and torsion modes we have also estimated the corresponding barriers by using the harmonic approximation.

Carrier-envelope phase-controlled quantum interference of injected photocurrents in semiconductors.

PubMed

Fortier, T M; Roos, P A; Jones, D J; Cundiff, S T; Bhat, R D R; Sipe, J E

2004-04-09

We demonstrate quantum interference control of injected photocurrents in a semiconductor using the phase stabilized pulse train from a mode-locked Ti:sapphire laser. Measurement of the comb offset frequency via this technique results in a signal-to-noise ratio of 40 dB (10 Hz resolution bandwidth), enabling solid-state detection of carrier-envelope phase shifts of a Ti:sapphire oscillator.

IN SITU SOLID-PHASE EXTRACTION AND ANALYSIS OF ULTRA-TRACE SYNTHETIC MUSKS IN MUNICIPAL SEWAGE EFFLUENT USING GAS CHROMATOGRAPHY-MASS SPECTROMETRY, FULL-SCAN MODE

EPA Science Inventory

Fragrance materials, such as synthetic musks in aqueous samples, are normally analyzed by GC/MS in the selected ion monitoring (SIM) mode to provide maximum sensitivity after liquid-liquid extraction of 1-L samples. A 1-L sample, however, usually provides too little ana...

ON-SITE SOLID-PHASE EXTRACTION AND LABORATORY ANALYSIS OF ULTRA-TRACE SYNTHETIC MUSKS IN MUNICIPAL SEWAGE EFFLUENT USING GAS CHROMATOGRAPHY-MASS SPECTROMETRY IN THE FULL-SCAN MODE

EPA Science Inventory

Fragrance materials such as synthetic musks in aqueous samples, are normally determined by gas chromatography/mass spectrometry in the selected ion monitoring (SIM) mode to provide maximum sensitivity after liquid-liquid extraction of I -L samples. Full-scan mass spectra are requ...

Deuterium and carbon-13 NMR of the solid polymorphism of benzenehexoyl hexa-n-hexanoate

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

Lifshitz, E.; Goldfarb,, D.; Vega, S.

Deuterium and carbon-13 NMR of specifically labeled benzenehexoyl hexa-n-hexanoate in the various solid-state phases are reported. The spectra exhibit dynamic line shapes which change discontinuously at the phase transitions. The results are interpreted in terms of sequential melting of the side chains on going from the low-temperature solid phases IV, III, etc., toward the liquid. In phase IV the molecules are very nearly static, except for fast rotation of the methyl groups about their C/sub 3/ axes. The results in phase III were quantitatively interpreted in terms of a two-site isomerization process involving simultaneous rotation by 95/sup 0/ about C/submore » 1/-C/sub 2/ and transition from gtg to g'g't (or equivalently g'tg' to ggt) for the rest of the chain. The specific rate of this reaction at 0/sup 0/C is approx. 10/sup 5/s/sup -1/. In phase II additional chain isomerization processes set-in which were, however, not analyzed quantitatively. Further motional modes, involving reorientation of whole chains about their C/sup ar/-O bonds, appear on going to phase I. In all solid phases the benzene ring remains static.« less

[Determination of wilforine in honey using solid phase extraction purification and ultra performance liquid chromatography-tanden mas spectrometry].

PubMed

Lei, Meikang; Peng, Fang; Ding, Tao; Zhu, Zitong; Xu, Jiawen; Wu, Xiaoqin

2015-01-01

A method based on solid phase extraction and ultra performance liquid chromatography coupled with tandem mass spectrometry (SPE-UPLC-MS/MS) has been proposed for the determination of wilforine residue in honey. After the sample was dissolved with water, concentrated and purified by an HLB solid phase extraction cartridge, the UPLC separation was performed on a Hypersil GOLD C18 column (50 mm x 2.1 mm, 1.9 microm) utilizing a gradient elution program of methanol (containing 0.15% formic acid) and water as mobile phases at a flow rate of 0. 25 mL/min. The determination was carried out with electrospray ion source in the positive mode (ESI) and multiple reaction monitoring (MRM) mode. The mass concentration of wilforine in the range of 0.01-2 microg/L was linearly correlated with the peak area, and the correlation coefficients was greater than 0.998. The limit of quantification (S/N>10) for wilforine was 0.01 microg/kg. The recoveries were 76.1% to 96.2% in the spiked levels of 0.01, 0.05 and 0.5 microg/kg with the relative standard deviations (RSD, n=6) lower than 10%. The results indicate that the method is rapid, sensitive and accurate, and can be applied for the qualitative and quantitative analysis of wilforine in honey.

Static SPME sampling of VOCs emitted from indoor building materials: prediction of calibration curves of single compounds for two different emission cells.

PubMed

Mocho, Pierre; Desauziers, Valérie

2011-05-01

Solid-phase microextraction (SPME) is a powerful technique, easy to implement for on-site static sampling of indoor VOCs emitted by building materials. However, a major constraint lies in the establishment of calibration curves which requires complex generation of standard atmospheres. Thus, the purpose of this paper is to propose a model to predict adsorption kinetics (i.e., calibration curves) of four model VOCs. The model is based on Fick's laws for the gas phase and on the equilibrium or the solid diffusion model for the adsorptive phase. Two samplers (the FLEC® and a home-made cylindrical emission cell), coupled to SPME for static sampling of material emissions, were studied. A good agreement between modeling and experimental data is observed and results show the influence of sampling rate on mass transfer mode in function of sample volume. The equilibrium model is adapted to quite large volume sampler (cylindrical cell) while the solid diffusion model is dedicated to small volume sampler (FLEC®). The limiting steps of mass transfer are the diffusion in gas phase for the cylindrical cell and the pore surface diffusion for the FLEC®. In the future, this modeling approach could be a useful tool for time-saving development of SPME to study building material emission in static mode sampling.

Molecularly imprinted solid-phase extraction in the analysis of agrochemicals.

PubMed

Yi, Ling-Xiao; Fang, Rou; Chen, Guan-Hua

2013-08-01

The molecular imprinting technique is a highly predeterminative recognition technology. Molecularly imprinted polymers (MIPs) can be applied to the cleanup and preconcentration of analytes as the selective adsorbent of solid-phase extraction (SPE). In recent years, a new type of SPE has formed, molecularly imprinted polymer solid-phase extraction (MISPE), and has been widely applied to the extraction of agrochemicals. In this review, the mechanism of the molecular imprinting technique and the methodology of MIP preparations are explained. The extraction modes of MISPE, including offline and online, are discussed, and the applications of MISPE in the analysis of agrochemicals such as herbicides, fungicides and insecticides are summarized. It is concluded that MISPE is a powerful tool to selectively isolate agrochemicals from real samples with higher extraction and cleanup efficiency than commercial SPE and that it has great potential for broad applications.

Rapid and sensitive analysis of phthalate metabolites, bisphenol A, and endogenous steroid hormones in human urine by mixed-mode solid-phase extraction, dansylation, and ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry.

PubMed

Wang, He-xing; Wang, Bin; Zhou, Ying; Jiang, Qing-wu

2013-05-01

Steroid hormone levels in human urine are convenient and sensitive indicators for the impact of phthalates and/or bisphenol A (BPA) exposure on the human steroid hormone endocrine system. In this study, a rapid and sensitive method for determination of 14 phthalate metabolites, BPA, and ten endogenous steroid hormones in urine was developed and validated on the basis of ultra-performance liquid chromatography coupled with electrospray ionization triple quadrupole mass spectrometry. The optimized mixed-mode solid phase-extraction separated the weakly acidic or neutral BPA and steroid hormones from acidic phthalate metabolites in urine: the former were determined in positive ion mode with a methanol/water mobile phase containing 10 mM ammonium formate; the latter were determined in negative ion mode with a acetonitrile/water mobile phase containing 0.1 % acetic acid, which significantly alleviated matrix effects for the analysis of BPA and steroid hormones. Dansylation of estrogens and BPA realized simultaneous and sensitive analysis of the endogenous steroid hormones and BPA in a single chromatographic run. The limits of detection were less than 0.84 ng/mL for phthalate metabolites and less than 0.22 ng/mL for endogenous steroid hormones and BPA. This proposed method had satisfactory precision and accuracy, and was successfully applied to the analyses of human urine samples. This method could be valuable when investigating the associations among endocrine-disrupting chemicals, endogenous steroid hormones, and relevant adverse outcomes in epidemiological studies.

Equation of State for Solid Phase I of Carbon Dioxide Valid for Temperatures up to 800 K and Pressures up to 12 GPa

NASA Astrophysics Data System (ADS)

Martin Trusler, J. P.

2011-12-01

The available thermodynamic-property data for solid phase I of carbon dioxide ("dry ice") are reviewed and used to determine the parameters of a new fundamental equation of state constructed in the form of a Helmholtz energy function with temperature and molar volume as the independent variables. The experimental data considered include the pressure, molar volume, and isobaric heat capacity along the sublimation curve, the melting-pressure curve, and molar volume in the compressed solid at temperatures from 295 to 764 K and pressures up to 12 GPa. The equation of state is based on the quasi-harmonic approximation, incorporating a Debye oscillator distribution for the vibrons, two discrete modes for the librons and a further three distinct modes for the internal vibrations of the CO2 molecule. A small anharmonic correction term is included, which is significant mainly in the region of the triple point. The estimated relative uncertainty of molar volume at specified temperature and pressure calculated from the equation of state is 0.02% on the sublimation curve and 1.5% in the compressed solid; for isobaric heat capacity on the sublimation curve, the uncertainty varies from 5.0% to 0.5% between 2 and 195 K. Auxiliary equations for the pressure and molar volume on the sublimation and melting curves are given. The equation of state is valid at temperatures from 0 to 800 K and at pressures from the solid-fluid phase boundary to 12 GPa.

Anomalous Refraction of Acoustic Guided Waves in Solids with Geometrically Tapered Metasurfaces.

PubMed

Zhu, Hongfei; Semperlotti, Fabio

2016-07-15

The concept of a metasurface opens new exciting directions to engineer the refraction properties in both optical and acoustic media. Metasurfaces are typically designed by assembling arrays of subwavelength anisotropic scatterers able to mold incoming wave fronts in rather unconventional ways. The concept of a metasurface was pioneered in photonics and later extended to acoustics while its application to the propagation of elastic waves in solids is still relatively unexplored. We investigate the design of acoustic metasurfaces to control elastic guided waves in thin-walled structural elements. These engineered discontinuities enable the anomalous refraction of guided wave modes according to the generalized Snell's law. The metasurfaces are made out of locally resonant toruslike tapers enabling an accurate phase shift of the incoming wave, which ultimately affects the refraction properties. We show that anomalous refraction can be achieved on transmitted antisymmetric modes (A_{0}) either when using a symmetric (S_{0}) or antisymmetric (A_{0}) incident wave, the former clearly involving mode conversion. The same metasurface design also allows achieving structure embedded planar focal lenses and phase masks for nonparaxial propagation.

Amorphous SiC/c-ZnO-Based Quasi-Lamb Mode Sensor for Liquid Environments.

PubMed

Caliendo, Cinzia; Hamidullah, Muhammad; Laidoudi, Farouk

2017-05-25

The propagation of the quasi-Lamb modes along a-SiC/ZnO thin composite plates was modeled and analysed with the aim to design a sensor able to detect the changes in parameters of a liquid environment, such as added mass and viscosity changes. The modes propagation was modeled by numerically solving the system of coupled electro-mechanical field equations in three media. The mode shape, the power flow, the phase velocity, and the electroacoustic coupling efficiency (K²) of the modes were calculated, specifically addressing the design of enhanced-coupling, microwave frequency sensors for applications in probing the solid/liquid interface. Three modes were identified that have predominant longitudinal polarization, high phase velocity, and quite good K²: the fundamental quasi symmetric mode (qS₀) and two higher order quasi-longitudinal modes (qL₁ and qL₂) with a dominantly longitudinal displacement component in one plate side. The velocity and attenuation of these modes were calculated for different liquid viscosities and added mass, and the gravimetric and viscosity sensitivities of both the phase velocity and attenuation were theoretically calculated. The present study highlights the feasibility of the a-SiC/ZnO acoustic waveguides for the development of high-frequency, integrated-circuit compatible electroacoustic devices suitable for working in a liquid environment.

Evaluating the operational risks of biomedical waste using failure mode and effects analysis.

PubMed

Chen, Ying-Chu; Tsai, Pei-Yi

2017-06-01

The potential problems and risks of biomedical waste generation have become increasingly apparent in recent years. This study applied a failure mode and effects analysis to evaluate the operational problems and risks of biomedical waste. The microbiological contamination of biomedical waste seldom receives the attention of researchers. In this study, the biomedical waste lifecycle was divided into seven processes: Production, classification, packaging, sterilisation, weighing, storage, and transportation. Twenty main failure modes were identified in these phases and risks were assessed based on their risk priority numbers. The failure modes in the production phase accounted for the highest proportion of the risk priority number score (27.7%). In the packaging phase, the failure mode 'sharp articles not placed in solid containers' had the highest risk priority number score, mainly owing to its high severity rating. The sterilisation process is the main difference in the treatment of infectious and non-infectious biomedical waste. The failure modes in the sterilisation phase were mainly owing to human factors (mostly related to operators). This study increases the understanding of the potential problems and risks associated with biomedical waste, thereby increasing awareness of how to improve the management of biomedical waste to better protect workers, the public, and the environment.

Helicons in Unbounded Plasmas.

PubMed

Stenzel, R L; Urrutia, J M

2015-05-22

Helicons are whistler modes with helical phase fronts. They have been studied in solid state plasmas and in discharge tubes where boundaries and nonuniformities are ever present. The present work shows that helicons also exist in unbounded and uniform plasmas, thereby bridging the fields of laboratory and space plasma physics. First measurements of helicon field lines in three dimensional space are presented. Helicons with negative and positive mode numbers can propagate with equal amplitudes.

Hydrolysis and acidification of agricultural waste in a non-airtight system: Effect of solid content, temperature, and mixing mode.

PubMed

Yu, Jiadong; Zhao, Yubin; Zhang, Huan; Hua, Binbin; Yuan, Xufeng; Zhu, Wanbin; Wang, Xiaofen; Cui, Zongjun

2017-01-01

A two-phase digestion system for treating agricultural waste is beneficial for methane production. This study explored the effect of solid content, temperature, and mixing mode on the process of hydrolysis and acidification using rice straw and cow dung launched in non-airtight acidogenic system. The results showed that the substrate could be hydrolyzed efficiently in the initial stage, the hydrolysis coefficient (k) of maximum cellulose and hemicellulose can be increased by 217.9% and 290.5%, respectively, compared with those of middle and last stages. High solid content played a leading role in promoting hydrolysis, resulted in hydrolysate content (sCOD) that was significantly higher than in treatments with low solid content (P<0.01), and led to organic acids accumulation up to 5.8 and 6.7g/L at mesophilic and thermophilic temperatures. Thermophilic temperature stimulated the hydrolysis and acidification of low solid content (P<0.05), and improved organic acid accumulation of high solid content only during the middle stage (P<0.01). Mixing mode was not a major factor, but increasing the mixing time was necessary for organic acid accumulation during the last stage (P<0.05). In addition, the study comprehensively analyzed a series of corresponding relationships among each operating parameter during the whole treatment process using canonical correspondence analysis. Copyright © 2016 Elsevier Ltd. All rights reserved.

Review of the absorption spectra of solid O2 and N2 as they relate to contamination of a cooled infrared telescope

NASA Technical Reports Server (NTRS)

Smith, S. M.

1977-01-01

During contamination studies for the liquid helium cooled shuttle infrared telescope facility, a literature search was conducted to determine the absorption spectra of the solid state of homonuclear molecules of O2 and N2, and ascertain what laboratory measurements of the solid have been made in the infrared. With the inclusion of one unpublished spectrum, the absorption spectrum of the solid oxygen molecule has been thoroughly studied from visible to millimeter wavelengths. Only two lines appear in the solid that do not also appear in the gas or liquid. A similar result is implied for the solid nitrogen molecule because it also is homonuclear. The observed infrared absorption lines result from lattice modes of the alpha phase of the solid, and disappear at the warmer temperatures of the beta, gamma, and liquid phases. They are not observed from polycrystalline forms of O2, while strong scattering is. Scattering, rather than absorption, is considered to be the principal natural contamination problem for cooled infrared telescopes in low earth orbit.

Nucleation of the diamond phase in aluminium-solid solutions

NASA Technical Reports Server (NTRS)

Hornbogen, E.; Mukhopadhyay, A. K.; Starke, E. A., Jr.

1993-01-01

Precipitation was studied from fcc solid solutions with silicon, germanium, copper and magnesium. Of all these elements only silicon and germanium form diamond cubic (DC) precipitates in fcc Al. Nucleation of the DC structure is enhanced if both types of atom are dissolved in the fcc lattice. This is interpreted as due to atomic size effects in the prenucleation stage. There are two modes of interference of fourth elements with nucleation of the DC phase in Al + Si, Ge. The formation of the DC phase is hardly affected if the atoms (for example, copper) are rejected from the (Si, Ge)-rich clusters. If additional types of atom are attracted by silicon and/or germanium, DC nuclei are replaced by intermetallic compounds (for example Mg2Si).

All-solid-state single longitudinal mode MOPA laser system

NASA Astrophysics Data System (ADS)

Zhang, Xiang; Gu, Haidong; Hu, Wenhua; Ren, Shilong

2018-03-01

Side diode pumped electro-optical Q Switching Nd: YAG is demonstrated as master oscillator. F-P etalon and twisted-mode cavity combined configuration is introduced to select longitudinal modes. The seed light experiences a round trip through the two flash pump amplifiers, in this device, the 4f image transmission system and SBS phase conjugate mirror is adopted in order to improved beam quality, by compensating the heat depolarization effect and eliminate wave-front distortion. In the condition of 1 or 5 repetitions of the wavelength at 1064nm, it produces the pulse energy of 300mJ, pulse width of 12ns, and energy instability (RMS) below 3% in single longitudinal mode operation. With a type two-phase matched KTP crystal, 532nm green light is yielded, at 1 Hz repetition rate, the pulse energy of green light is more than 150mJ.

Emergent Optical Phononic Modes upon Nanoscale Mesogenic Phase Transitions

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

Bolmatov, Dima; Zhernenkov, Mikhail; Sharpnack, Lewis

The investigation of phononic collective excitations in soft matter systems at the molecular scale has always been challenging due to limitations of experimental techniques in resolving low-energy modes. Recent advances in inelastic X-ray scattering (IXS) enabled the study of such systems with unprecedented spectral contrast at meV excitation energies. In particular, it has become possible to shed light on the low-energy collective motions in materials whose morphology and phase behavior can easily be manipulated, such as mesogenic systems. The understanding of collective mode behavior with a Q-dependence is the key to implement heat management based on the control of amore » sample structure. The latter has great potential for a large number of energy-inspired innovations. As a first step toward this goal, we carried out high contrast IXS measurements on a liquid crystal sample, D7AOB, which exhibits solid-like dynamic features, such as the coexistence of longitudinal and transverse phononic modes. For the first time, we found that these terahertz phononic excitations persist in the crystal, smectic A, and isotropic phases. Furthermore, the intermediate smectic A phase is shown to support a van der Waals-mediated nonhydrodynamic mode with an optical-like phononic behavior. In conclusion, the tunability of the collective excitations at nanometer–terahertz scales via selection of the sample mesogenic phase represents a new opportunity to manipulate optomechanical properties of soft metamaterials.« less

Emergent Optical Phononic Modes upon Nanoscale Mesogenic Phase Transitions

DOE PAGES

Bolmatov, Dima; Zhernenkov, Mikhail; Sharpnack, Lewis; ...

2017-05-26

The investigation of phononic collective excitations in soft matter systems at the molecular scale has always been challenging due to limitations of experimental techniques in resolving low-energy modes. Recent advances in inelastic X-ray scattering (IXS) enabled the study of such systems with unprecedented spectral contrast at meV excitation energies. In particular, it has become possible to shed light on the low-energy collective motions in materials whose morphology and phase behavior can easily be manipulated, such as mesogenic systems. The understanding of collective mode behavior with a Q-dependence is the key to implement heat management based on the control of amore » sample structure. The latter has great potential for a large number of energy-inspired innovations. As a first step toward this goal, we carried out high contrast IXS measurements on a liquid crystal sample, D7AOB, which exhibits solid-like dynamic features, such as the coexistence of longitudinal and transverse phononic modes. For the first time, we found that these terahertz phononic excitations persist in the crystal, smectic A, and isotropic phases. Furthermore, the intermediate smectic A phase is shown to support a van der Waals-mediated nonhydrodynamic mode with an optical-like phononic behavior. In conclusion, the tunability of the collective excitations at nanometer–terahertz scales via selection of the sample mesogenic phase represents a new opportunity to manipulate optomechanical properties of soft metamaterials.« less

Highly selective solid-phase extraction and large volume injection for the robust gas chromatography-mass spectrometric analysis of TCA and TBA in wines.

PubMed

Insa, S; Anticó, E; Ferreira, V

2005-09-30

A reliable solid-phase extraction (SPE) method for the simultaneous determination of 2,4,6-trichloroanisole (TCA) and 2,4,6-tribromoanisole (TBA) in wines has been developed. In the proposed procedure 50 mL of wine are extracted in a 1 mL cartridge filled with 50 mg of LiChrolut EN resins. Most wine volatiles are washed up with 12.5 mL of a water:methanol solution (70%, v/v) containing 1% of NaHCO3. Analytes are further eluted with 0.6 mL of dichloromethane. A 40 microL aliquot of this extract is directly injected into a PTV injector operated in the solvent split mode, and analysed by gas chromatography (GC)-ion trap mass spectrometry using the selected ion storage mode. The solid-phase extraction, including sample volume and rinsing and elution solvents, and the large volume GC injection have been carefully evaluated and optimized. The resulting method is precise (RSD (%) < 6% at 100 ng L(-1)), sensitive (LOD were 0.2 and 0.4 ng/L for TCA and TBA, respectively), robust (the absolute recoveries of both analytes are higher than 80% and consistent wine to wine) and friendly to the GC-MS system (the extract is clean, simple and free from non-volatiles).

Density functional theory for prediction of far-infrared vibrational frequencies: molecular crystals of astrophysical interest

NASA Astrophysics Data System (ADS)

Ennis, C.; Auchettl, R.; Appadoo, D. R. T.; Robertson, E. G.

2017-11-01

Solid-state density functional theory code has been implemented for the structure optimization of crystalline methanol, acetaldehyde and acetic acid and for the calculation of infrared frequencies. The results are compared to thin film spectra obtained from low-temperature experiments performed at the Australian Synchrotron. Harmonic frequency calculations of the internal modes calculated at the B3LYP-D3/m-6-311G(d) level shows higher deviation from infrared experiment than more advanced theory applied to the gas phase. Importantly for the solid-state, the simulation of low-frequency molecular lattice modes closely resembles the observed far-infrared features after application of a 0.92 scaling factor. This allowed experimental peaks to be assigned to specific translation and libration modes, including acetaldehyde and acetic acid lattice features for the first time. These frequency calculations have been performed without the need for supercomputing resources that are required for large molecular clusters using comparable levels of theory. This new theoretical approach will find use for the rapid characterization of intermolecular interactions and bonding in crystals, and the assignment of far-infrared spectra for crystalline samples such as pharmaceuticals and molecular ices. One interesting application may be for the detection of species of prebiotic interest on the surfaces of Kuiper-Belt and Trans-Neptunian Objects. At such locations, the three small organic molecules studied here could reside in their crystalline phase. The far-infrared spectra for their low-temperature solid phases are collected under planetary conditions, allowing us to compile and assign their most intense spectral features to assist future far-infrared surveys of icy Solar system surfaces.

Analysis of n-alkanes at sub microgram per liter level after direct solid phase microextraction from aqueous samples.

PubMed

Farajzadeh, Mirali; Hatami, Mehdi

2002-11-01

This work describes the application of the previously presented solid phase microextraction (SPME) fiber in direct mode for sampling of C10-C20 n-alkanes from aqueous solution. The fiber has simple composition and is constructed from activated charcoal:PVC suspension in tetrahydrofuran. When the composition of the fiber was optimized that the optimum composition was 90:10 (activated charcoal:PVC) for direct mode, whereas it was 75:25 for sampling from the headspace of aqueous samples. This fiber is completely stable in contact with water. The extraction efficiency is improved in the presence of 0.1 M NaCl. The value is between 17.8-38.5% for the first extraction, which better than the efficiency of similar commercial fibers. After seven extractions, all analytes are removed from the aqueous samples nearly 100%. Single fiber repeatability and fiber-to-fiber reproducibility are good and both are less than 13% for all studied alkanes. Finally, direct mode SPME was used in the determination of n-alkanes in the range of sub microg L(-1) without any additional preconcentration procedure. Gas chromatography along with flame ionization detection were used for separation and detection of the studied analytes.

Impact of laser phase and amplitude noises on streak camera temporal resolution

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

Wlotzko, V., E-mail: wlotzko@optronis.com; Optronis GmbH, Ludwigstrasse 2, 77694 Kehl; Uhring, W.

2015-09-15

Streak cameras are now reaching sub-picosecond temporal resolution. In cumulative acquisition mode, this resolution does not entirely rely on the electronic or the vacuum tube performances but also on the light source characteristics. The light source, usually an actively mode-locked laser, is affected by phase and amplitude noises. In this paper, the theoretical effects of such noises on the synchronization of the streak system are studied in synchroscan and triggered modes. More precisely, the contribution of band-pass filters, delays, and time walk is ascertained. Methods to compute the resulting synchronization jitter are depicted. The results are verified by measurement withmore » a streak camera combined with a Ti:Al{sub 2}O{sub 3} solid state laser oscillator and also a fiber oscillator.« less

Fabrication and Testing of Microfluidic Optomechanical Oscillators

PubMed Central

Han, Kewen; Kim, Kyu Hyun; Kim, Junhwan; Lee, Wonsuk; Liu, Jing; Fan, Xudong; Carmon, Tal; Bahl, Gaurav

2014-01-01

Cavity optomechanics experiments that parametrically couple the phonon modes and photon modes have been investigated in various optical systems including microresonators. However, because of the increased acoustic radiative losses during direct liquid immersion of optomechanical devices, almost all published optomechanical experiments have been performed in solid phase. This paper discusses a recently introduced hollow microfluidic optomechanical resonator. Detailed methodology is provided to fabricate these ultra-high-Q microfluidic resonators, perform optomechanical testing, and measure radiation pressure-driven breathing mode and SBS-driven whispering gallery mode parametric vibrations. By confining liquids inside the capillary resonator, high mechanical- and optical- quality factors are simultaneously maintained. PMID:24962013

Dual gauge field theory of quantum liquid crystals in two dimensions

NASA Astrophysics Data System (ADS)

Beekman, Aron J.; Nissinen, Jaakko; Wu, Kai; Liu, Ke; Slager, Robert-Jan; Nussinov, Zohar; Cvetkovic, Vladimir; Zaanen, Jan

2017-04-01

We present a self-contained review of the theory of dislocation-mediated quantum melting at zero temperature in two spatial dimensions. The theory describes the liquid-crystalline phases with spatial symmetries in between a quantum crystalline solid and an isotropic superfluid: quantum nematics and smectics. It is based on an Abelian-Higgs-type duality mapping of phonons onto gauge bosons (;stress photons;), which encode for the capacity of the crystal to propagate stresses. Dislocations and disclinations, the topological defects of the crystal, are sources for the gauge fields and the melting of the crystal can be understood as the proliferation (condensation) of these defects, giving rise to the Anderson-Higgs mechanism on the dual side. For the liquid crystal phases, the shear sector of the gauge bosons becomes massive signaling that shear rigidity is lost. After providing the necessary background knowledge, including the order parameter theory of two-dimensional quantum liquid crystals and the dual theory of stress gauge bosons in bosonic crystals, the theory of melting is developed step-by-step via the disorder theory of dislocation-mediated melting. Resting on symmetry principles, we derive the phenomenological imaginary time actions of quantum nematics and smectics and analyze the full spectrum of collective modes. The quantum nematic is a superfluid having a true rotational Goldstone mode due to rotational symmetry breaking, and the origin of this 'deconfined' mode is traced back to the crystalline phase. The two-dimensional quantum smectic turns out to be a dizzyingly anisotropic phase with the collective modes interpolating between the solid and nematic in a non-trivial way. We also consider electrically charged bosonic crystals and liquid crystals, and carefully analyze the electromagnetic response of the quantum liquid crystal phases. In particular, the quantum nematic is a real superconductor and shows the Meissner effect. Their special properties inherited from spatial symmetry breaking show up mostly at finite momentum, and should be accessible by momentum-sensitive spectroscopy.

Dual gauge field theory of quantum liquid crystals in two dimensions

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

Beekman, Aron J.; Nissinen, Jaakko; Wu, Kai

We present a self-contained review of the theory of dislocation-mediated quantum melting at zero temperature in two spatial dimensions. The theory describes the liquid-crystalline phases with spatial symmetries in between a quantum crystalline solid and an isotropic superfluid: quantum nematics and smectics. It is based on an Abelian-Higgs-type duality mapping of phonons onto gauge bosons (“stress photons”), which encode for the capacity of the crystal to propagate stresses. Dislocations and disclinations, the topological defects of the crystal, are sources for the gauge fields and the melting of the crystal can be understood as the proliferation (condensation) of these defects, givingmore » rise to the Anderson–Higgs mechanism on the dual side. For the liquid crystal phases, the shear sector of the gauge bosons becomes massive signaling that shear rigidity is lost. After providing the necessary background knowledge, including the order parameter theory of two-dimensional quantum liquid crystals and the dual theory of stress gauge bosons in bosonic crystals, the theory of melting is developed step-by-step via the disorder theory of dislocation-mediated melting. Resting on symmetry principles, we derive the phenomenological imaginary time actions of quantum nematics and smectics and analyze the full spectrum of collective modes. The quantum nematic is a superfluid having a true rotational Goldstone mode due to rotational symmetry breaking, and the origin of this ‘deconfined’ mode is traced back to the crystalline phase. The two-dimensional quantum smectic turns out to be a dizzyingly anisotropic phase with the collective modes interpolating between the solid and nematic in a non-trivial way. We also consider electrically charged bosonic crystals and liquid crystals, and carefully analyze the electromagnetic response of the quantum liquid crystal phases. In particular, the quantum nematic is a real superconductor and shows the Meissner effect. Furthermore, their special properties inherited from spatial symmetry breaking show up mostly at finite momentum, and should be accessible by momentum-sensitive spectroscopy.« less

Dual gauge field theory of quantum liquid crystals in two dimensions

DOE PAGES

Beekman, Aron J.; Nissinen, Jaakko; Wu, Kai; ...

2017-04-18

We present a self-contained review of the theory of dislocation-mediated quantum melting at zero temperature in two spatial dimensions. The theory describes the liquid-crystalline phases with spatial symmetries in between a quantum crystalline solid and an isotropic superfluid: quantum nematics and smectics. It is based on an Abelian-Higgs-type duality mapping of phonons onto gauge bosons (“stress photons”), which encode for the capacity of the crystal to propagate stresses. Dislocations and disclinations, the topological defects of the crystal, are sources for the gauge fields and the melting of the crystal can be understood as the proliferation (condensation) of these defects, givingmore » rise to the Anderson–Higgs mechanism on the dual side. For the liquid crystal phases, the shear sector of the gauge bosons becomes massive signaling that shear rigidity is lost. After providing the necessary background knowledge, including the order parameter theory of two-dimensional quantum liquid crystals and the dual theory of stress gauge bosons in bosonic crystals, the theory of melting is developed step-by-step via the disorder theory of dislocation-mediated melting. Resting on symmetry principles, we derive the phenomenological imaginary time actions of quantum nematics and smectics and analyze the full spectrum of collective modes. The quantum nematic is a superfluid having a true rotational Goldstone mode due to rotational symmetry breaking, and the origin of this ‘deconfined’ mode is traced back to the crystalline phase. The two-dimensional quantum smectic turns out to be a dizzyingly anisotropic phase with the collective modes interpolating between the solid and nematic in a non-trivial way. We also consider electrically charged bosonic crystals and liquid crystals, and carefully analyze the electromagnetic response of the quantum liquid crystal phases. In particular, the quantum nematic is a real superconductor and shows the Meissner effect. Furthermore, their special properties inherited from spatial symmetry breaking show up mostly at finite momentum, and should be accessible by momentum-sensitive spectroscopy.« less

Dual gauge field theory of quantum liquid crystals in three dimensions

NASA Astrophysics Data System (ADS)

Beekman, Aron J.; Nissinen, Jaakko; Wu, Kai; Zaanen, Jan

2017-10-01

The dislocation-mediated quantum melting of solids into quantum liquid crystals is extended from two to three spatial dimensions, using a generalization of boson-vortex or Abelian-Higgs duality. Dislocations are now Burgers-vector-valued strings that trace out worldsheets in space-time while the phonons of the solid dualize into two-form (Kalb-Ramond) gauge fields. We propose an effective dual Higgs potential that allows for restoring translational symmetry in either one, two, or three directions, leading to the quantum analogues of columnar, smectic, or nematic liquid crystals. In these phases, transverse phonons turn into gapped, propagating modes, while compressional stress remains massless. Rotational Goldstone modes emerge whenever translational symmetry is restored. We also consider the effective electromagnetic response of electrically charged quantum liquid crystals, and find among other things that as a hard principle only two out of the possible three rotational Goldstone modes are observable using propagating electromagnetic fields.

Sub-100 attosecond timing jitter from low-noise passively mode-locked solid-state laser at telecom wavelength.

PubMed

Portuondo-Campa, E; Paschotta, R; Lecomte, S

2013-08-01

We report on the ultralow timing jitter of the 100 MHz pulse trains generated by two identical passively mode-locked diode-pumped solid-state lasers (DPSSLs) emitting at 1556 nm. Ultralow timing jitter of 83 as (integrated from 10 kHz to 50 MHz) for one laser has been measured with a balanced optical cross-correlator as timing discriminator. Extremely low intensity noise has been measured as well. Several measurement techniques have been used and show similar jitter results. Different possible noise sources have been theoretically investigated and compared to the measured jitter power spectral density. It is found that although the measured integrated jitter is quite low, it is still significantly above the quantum limit in the considered frequency span. Therefore, there is a substantial potential for technical improvements that could make passively mode-locked DPSSL outperform fiber lasers as source of microwaves with low phase noise.

Carbon mass balance and microbial ecology in a laboratory scale reactor achieving simultaneous sludge reduction and nutrient removal.

PubMed

Huang, Pei; Li, Liang; Kotay, Shireen Meher; Goel, Ramesh

2014-04-15

Solids reduction in activated sludge processes (ASP) at source using process manipulation has been researched widely over the last two-decades. However, the absence of nutrient removal component, lack of understanding on the organic carbon, and limited information on key microbial community in solids minimizing ASP preclude the widespread acceptance of sludge minimizing processes. In this manuscript, we report simultaneous solids reduction through anaerobiosis along with nitrogen and phosphorus removals. The manuscript also reports carbon mass balance using stable isotope of carbon, microbial ecology of nitrifiers and polyphosphate accumulating organisms (PAOs). Two laboratory scale reactors were operated in anaerobic-aerobic-anoxic (A(2)O) mode. One reactor was run in the standard mode (hereafter called the control-SBR) simulating conventional A(2)O type of activated sludge process and the second reactor was run in the sludge minimizing mode (called the modified-SBR). Unlike other research efforts where the sludge minimizing reactor was maintained at nearly infinite solids retention time (SRT). To sustain the efficient nutrient removal, the modified-SBR in this research was operated at a very small solids yield rather than at infinite SRT. Both reactors showed consistent NH3-N, phosphorus and COD removals over a period of 263 days. Both reactors also showed active denitrification during the anoxic phase even if there was no organic carbon source available during this phase, suggesting the presence of denitrifying PAOs (DNPAOs). The observed solids yield in the modified-SBR was 60% less than the observed solids yield in the control-SBR. Specific oxygen uptake rate (SOUR) for the modified-SBR was almost 44% more than the control-SBR under identical feeding conditions, but was nearly the same for both reactors under fasting conditions. The modified-SBR showed greater diversity of ammonia oxidizing bacteria and PAOs compared to the control-SBR. The diversity of PAOs in the modified-SBR was even more interesting in which case novel clades of Candidatus Accumulibacter phosphatis (CAP), an uncultured but widely found PAOs, were found. Copyright © 2014 Elsevier Ltd. All rights reserved.

Headspace versus direct immersion solid phase microextraction in complex matrixes: investigation of analyte behavior in multicomponent mixtures.

PubMed

Gionfriddo, Emanuela; Souza-Silva, Érica A; Pawliszyn, Janusz

2015-08-18

This work aims to investigate the behavior of analytes in complex mixtures and matrixes with the use of solid-phase microextraction (SPME). Various factors that influence analyte uptake such as coating chemistry, extraction mode, the physicochemical properties of analytes, and matrix complexity were considered. At first, an aqueous system containing analytes bearing different hydrophobicities, molecular weights, and chemical functionalities was investigated by using commercially available liquid and solid porous coatings. The differences in the mass transfer mechanisms resulted in a more pronounced occurrence of coating saturation in headspace mode. Contrariwise, direct immersion extraction minimizes the occurrence of artifacts related to coating saturation and provides enhanced extraction of polar compounds. In addition, matrix-compatible PDMS-modified solid coatings, characterized by a new morphology that avoids coating fouling, were compared to their nonmodified analogues. The obtained results indicate that PDMS-modified coatings reduce artifacts associated with coating saturation, even in headspace mode. This factor, coupled to their matrix compatibility, make the use of direct SPME very practical as a quantification approach and the best choice for metabolomics studies where wide coverage is intended. To further understand the influence on analyte uptake on a system where additional interactions occur due to matrix components, ex vivo and in vivo sampling conditions were simulated using a starch matrix model, with the aim of mimicking plant-derived materials. Our results corroborate the fact that matrix handling can affect analyte/matrix equilibria, with consequent release of high concentrations of previously bound hydrophobic compounds, potentially leading to coating saturation. Direct immersion SPME limited the occurrence of the artifacts, which confirms the suitability of SPME for in vivo applications. These findings shed light into the implementation of in vivo SPME strategies in quantitative metabolomics studies of complex plant-based systems.

Generalized thermoelastic diffusive waves in heat conducting materials

NASA Astrophysics Data System (ADS)

Sharma, J. N.

2007-04-01

Keeping in view the applications of diffusion processes in geophysics and electronics industry, the aim of the present paper is to give a detail account of the plane harmonic generalized thermoelastic diffusive waves in heat conducting solids. According to the characteristic equation, three longitudinal waves namely, elastodiffusive (ED), mass diffusion (MD-mode) and thermodiffusive (TD-mode), can propagate in such solids in addition to transverse waves. The transverse waves get decoupled from rest of the fields and hence remain unaffected due to temperature change and mass diffusion effects. These waves travel without attenuation and dispersion. The other generalized thermoelastic diffusive waves are significantly influenced by the interacting fields and hence suffer both attenuation and dispersion. At low frequency mass diffusion and thermal waves do not exist but at high-frequency limits these waves propagate with infinite velocity being diffusive in character. Moreover, in the low-frequency regions, the disturbance is mainly dominant by mechanical process of transportation of energy and at high-frequency regions it is significantly dominated by a close to diffusive process (heat conduction or mass diffusion). Therefore, at low-frequency limits the waves like modes are identifiable with small amplitude waves in elastic materials that do not conduct heat. The general complex characteristic equation is solved by using irreducible case of Cardano's method with the help of DeMoivre's theorem in order to obtain phase speeds, attenuation coefficients and specific loss factor of energy dissipation of various modes. The propagation of waves in case of non-heat conducting solids is also discussed. Finally, the numerical solution is carried out for copper (solvent) and zinc (solute) materials and the obtained phase velocities, attenuation coefficients and specific loss factor of various thermoelastic diffusive waves are presented graphically.

Order-disorder phase transition in the peroxidovanadium complex NH4[VO(O2)2(NH3)].

PubMed

Schwendt, Peter; Gyepes, Róbert; Chrappová, Jana; Němec, Ivan; Vaněk, Přemysl

2018-07-05

Complex NH 4 [VO(O 2 ) 2 (NH 3 )] (1) undergoes an order-disorder phase transition at T c ~258K. This transition is accompanied by change in the space group of the orthorhombic lattice and also by significant structural rearrangements of the constituent molecules, which are pertinent mostly to their NH 4 + ions and their ammonia ligands. The low-temperature solid state IR and Raman spectra of 1 were corroborated by solid-state computations that employed Gaussian functions as the basis set. Results of these computations yielded excellent agreement with experimental data. On the curves of temperature dependence of vibrational modes, the phase transition is expressed by an abrupt change of the slope above T c . Copyright © 2018 Elsevier B.V. All rights reserved.

Two-phase thermodynamic model for efficient and accurate absolute entropy of water from molecular dynamics simulations.

PubMed

Lin, Shiang-Tai; Maiti, Prabal K; Goddard, William A

2010-06-24

Presented here is the two-phase thermodynamic (2PT) model for the calculation of energy and entropy of molecular fluids from the trajectory of molecular dynamics (MD) simulations. In this method, the density of state (DoS) functions (including the normal modes of translation, rotation, and intramolecular vibration motions) are determined from the Fourier transform of the corresponding velocity autocorrelation functions. A fluidicity parameter (f), extracted from the thermodynamic state of the system derived from the same MD, is used to partition the translation and rotation modes into a diffusive, gas-like component (with 3Nf degrees of freedom) and a nondiffusive, solid-like component. The thermodynamic properties, including the absolute value of entropy, are then obtained by applying quantum statistics to the solid component and applying hard sphere/rigid rotor thermodynamics to the gas component. The 2PT method produces exact thermodynamic properties of the system in two limiting states: the nondiffusive solid state (where the fluidicity is zero) and the ideal gas state (where the fluidicity becomes unity). We examine the 2PT entropy for various water models (F3C, SPC, SPC/E, TIP3P, and TIP4P-Ew) at ambient conditions and find good agreement with literature results obtained based on other simulation techniques. We also validate the entropy of water in the liquid and vapor phases along the vapor-liquid equilibrium curve from the triple point to the critical point. We show that this method produces converged liquid phase entropy in tens of picoseconds, making it an efficient means for extracting thermodynamic properties from MD simulations.

Microstructural Evolution and Phase Formation in 2nd-Generation Refractory-Based High Entropy Alloys

PubMed Central

Eshed, Eyal; Larianovsky, Natalya; Kovalevsky, Alexey; Popov, Vladimir; Gorbachev, Igor; Popov, Vladimir; Katz-Demyanetz, Alexander

2018-01-01

Refractory-based high entropy alloys (HEAs) of the 2nd-generation type are new intensively-studied materials with a high potential for structural high-temperature applications. This paper presents investigation results on microstructural evolution and phase formation in as-cast and subsequently heat-treated HEAs at various temperature-time regimes. Microstructural examination was performed by means of scanning electron microscopy (SEM) combined with the energy dispersive spectroscopy (EDS) mode of electron probe microanalysis (EPMA) and qualitative X-ray diffraction (XRD). The primary evolutionary trend observed was the tendency of Zr to gradually segregate as the temperature rises, while all the other elements eventually dissolve in the BCC solid solution phase once the onset of Laves phase complex decomposition is reached. The performed thermodynamic modelling was based on the Calculation of Phase Diagrams method (CALPHAD). The BCC A2 solid solution phase is predicted by the model to contain increasing amounts of Cr as the temperature rises, which is in perfect agreement with the actual results obtained by SEM. However, the model was not able to predict the existence of the Zr-rich phase or the tendency of Zr to segregate and form its own solid solution—most likely as a result of the Zr segregation trend not being an equilibrium phenomenon. PMID:29360763

The autowave modes of solid phase polymerization of metal-containing monomers in two- and three-dimensional fiberglass-filled matrices

NASA Astrophysics Data System (ADS)

Barelko, V. V.; Pomogailo, A. D.; Dzhardimalieva, G. I.; Evstratova, S. I.; Rozenberg, A. S.; Uflyand, I. E.

1999-06-01

The phenomenon of autowave (frontal) solid phase polymerization of metal-containing monomers based on metal-acrylamide complexes is considered. The comparison of the features of autowave processes realized in both the single-component matrices of the monomer and the matrices filled by the fiberglass materials is performed. The unstable regimes of the polymerization wave as well as the conditions for the stabilization of the flat front in the filled matrices are described. The peculiarities of the frontal regimes in the three- and two-dimensional media are studied. Some possibilities for using of autowave polymerization in the fabrication of the polymer-fiberglass composites and composition prepregs are discussed.

Self-induced quasistationary magnetic fields.

PubMed

Kamenetskii, E O

2006-01-01

The interaction of electromagnetic radiation with temporally dispersive magnetic solids of small dimensions may show very special resonant behaviors. The internal fields of such samples are characterized by magnetostatic-potential scalar wave functions. The oscillating modes have the energy orthogonality properties and unusual pseudoelectric (gauge) fields. Because of a phase factor, that makes the states single valued, a persistent magnetic current exists. This leads to appearance of an eigenelectric moment of a small disk sample. One of the intriguing features of the mode fields is dynamical symmetry breaking.

Direct Sampling and Analysis from Solid Phase Extraction Cards using an Automated Liquid Extraction Surface Analysis Nanoelectrospray Mass Spectrometry System

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

Walworth, Matthew J; ElNaggar, Mariam S; Stankovich, Joseph J

Direct liquid extraction based surface sampling, a technique previously demonstrated with continuous flow and autonomous pipette liquid microjunction surface sampling probes, has recently been implemented as the Liquid Extraction Surface Analysis (LESA) mode on the commercially available Advion NanoMate chip-based infusion nanoelectrospray ionization system. In the present paper, the LESA mode was applied to the analysis of 96-well format custom solid phase extraction (SPE) cards, with each well consisting of either a 1 or 2 mm diameter monolithic hydrophobic stationary phase. These substrate wells were conditioned, loaded with either single or multi-component aqueous mixtures, and read out using the LESAmore » mode of a TriVersa NanoMate or a Nanomate 100 coupled to an ABI/Sciex 4000QTRAPTM hybrid triple quadrupole/linear ion trap mass spectrometer and a Thermo LTQ XL linear ion trap mass spectrometer. Extraction conditions, including extraction/nanoESI solvent composition, volume, and dwell times, were optimized in the analysis of targeted compounds. Limit of detection and quantitation as well as analysis reproducibility figures of merit were measured. Calibration data was obtained for propranolol using a deuterated internal standard which demonstrated linearity and reproducibility. A 10x increase in signal and cleanup of micromolar Angiotensin II from a concentrated salt solution was demonstrated. Additionally, a multicomponent herbicide mixture at ppb concentration levels was analyzed using MS3 spectra for compound identification in the presence of isobaric interferences.« less

Determination of a flame retardant hydrolysis product in human urine by SPE and LC-MS. Comparison of molecularly imprinted solid-phase extraction with a mixed-mode anion exchanger.

PubMed

Möller, Kristina; Crescenzi, Carlo; Nilsson, Ulrika

2004-01-01

Diphenyl phosphate is a hydrolysis product and possible metabolite of the flame retardant and plasticiser additive triphenyl phosphate. A molecularly imprinted polymer solid-phase extraction (MISPE) method for extracting diphenyl phosphate from aqueous solutions has been developed and compared with SPE using a commercially available mixed-mode anion exchanger. The imprinted polymer was prepared using 2-vinylpyridine (2-Vpy) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker, and a structural analogue of the analyte as the template molecule. The imprinted polymer was evaluated for use as a SPE sorbent, in tests with both aqueous standards and spiked urine samples, by comparing recovery and breakthrough data obtained using the imprinted form of the polymer and a non-imprinted form (NIP). Extraction from aqueous solutions resulted in more than 80% recovery. Adsorption by the molecularly imprinted polymer (MIP) was non-selective, but selectivity was achieved by selective desorption in the wash steps. Diphenyl phosphate could also be selectively extracted from urine samples, although the urine matrix reduced the capacity of the MISPE cartridges. Recoveries from urine extraction were higher than 70%. It was important to control pH during sample loading. The MISPE method was found to yield a less complex LC-ESI-MS chromatogram of the urine extracts compared with the mixed-mode anion-exchanger method. An LC-ESI-MS method using a Hypercarb LC column with a graphitised carbon stationary phase was also evaluated for organophosphate diesters. LC-ESI-MS using negative-ion detection in selected ion monitoring (SIM) mode was shown to be linear for diphenyl phosphate in the range 0.08-20 ng microL(-1).

A Sugar-Based Gelator for Marine Oil-Spill Recovery.

PubMed

Vibhute, Amol M; Muvvala, Venkatanarayana; Sureshan, Kana M

2016-06-27

Marine oil spills constitute an environmental disaster with severe adverse effects on the economy and ecosystem. Phase-selective organogelators (PSOGs), molecules that can congeal oil selectively from oil-water mixtures, have been proposed to be useful for oil-spill recovery. However, a major drawback lies in the mode of application of the PSOG to an oil spill spread over a large area. The proposed method of using carrier solvents is impractical for various reasons. Direct application of the PSOG as a solid, although it would be ideal, is unknown, presumably owing to poor dispersion of the solid through the oil. We have designed five cheap and easy-to-make glucose-derived PSOGs that disperse in the oil phase uniformly when applied as a fine powder. These gelators were shown to selectively congeal many oils, including crude oil, from oil-water mixtures to form stable gels, which is an essential property for efficient oil-spill recovery. We have demonstrated that these PSOGs can be applied aerially as a solid powder onto a mixture of crude oil and sea water and the congealed oil can then be scooped out. Our innovative mode of application and low cost of the PSOG offers a practical solution to oil-spill recovery. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Numerical Simulation of Combustion and Extinction of a Solid Cylinder in Low-Speed Cross Flow

NASA Technical Reports Server (NTRS)

Tien, J. S.; Yang, Chin Tien

1998-01-01

The combustion and extinction behavior of a diffusion flame around a solid fuel cylinder (PMMA) in low-speed forced flow in zero gravity was studied numerically using a quasi-steady gas phase model. This model includes two-dimensional continuity, full Navier Stokes' momentum, energy, and species equations with a one-step overall chemical reaction and second-order finite-rate Arrhenius kinetics. Surface radiation and Arrhenius pyrolysis kinetics are included on the solid fuel surface description and a parameter Phi, representing the percentage of gas-phase conductive heat flux going into the solid, is introduced into the interfacial energy balance boundary condition to complete the description for the quasi-steady gas-phase system. The model was solved numerically using a body-fitted coordinate transformation and the SIMPLE algorithm. The effects of varying freestream velocity and Phi were studied. These parameters have a significant effect on the flame structure and extinction limits. Two flame modes were identified: envelope flame and wake flame. Two kinds of flammability limits were found: quenching at low-flow speeds due to radiative loss and blow-off at high flow speeds due to insufficient gas residence time. A flammability map was constructed showing the existence of maximum Phi above which the solid is not flammable at any freestream velocity.

Ultrafast Screening and Quantitation of Pesticides in Food and Environmental Matrices by Solid-Phase Microextraction-Transmission Mode (SPME-TM) and Direct Analysis in Real Time (DART).

PubMed

Gómez-Ríos, Germán Augusto; Gionfriddo, Emanuela; Poole, Justen; Pawliszyn, Janusz

2017-07-05

The direct interface of microextraction technologies to mass spectrometry (MS) has unquestionably revolutionized the speed and efficacy at which complex matrices are analyzed. Solid Phase Micro Extraction-Transmission Mode (SPME-TM) is a technology conceived as an effective synergy between sample preparation and ambient ionization. Succinctly, the device consists of a mesh coated with polymeric particles that extracts analytes of interest present in a given sample matrix. This coated mesh acts as a transmission-mode substrate for Direct Analysis in Real Time (DART), allowing for rapid and efficient thermal desorption/ionization of analytes previously concentrated on the coating, and dramatically lowering the limits of detection attained by sole DART analysis. In this study, we present SPME-TM as a novel tool for the ultrafast enrichment of pesticides present in food and environmental matrices and their quantitative determination by MS via DART ionization. Limits of quantitation in the subnanogram per milliliter range can be attained, while total analysis time does not exceed 2 min per sample. In addition to target information obtained via tandem MS, retrospective studies of the same sample via high-resolution mass spectrometry (HRMS) were accomplished by thermally desorbing a different segment of the microextraction device.

Monoclinic Cc-phase stabilization in magnetically diluted lead free Na1/2Bi1/2TiO3—Evolution of spin glass like behavior with enhanced ferroelectric and dielectric properties

NASA Astrophysics Data System (ADS)

Thangavelu, Karthik; Asthana, Saket

2015-09-01

The effect of magnetic cation substitution on the phase stabilization, ferroelectric, dielectric and magnetic properties of a lead free Na0.5Bi0.5TiO3 (NBT) system prepared by O2 atmosphere solid state sintering were studied extensively. Cobalt (Co) was chosen as the magnetic cation to substitute at the Ti-site of NBT with optimized 2.5 mol%. Rietveld analysis of x-ray diffraction data favours the monoclinic Cc phase stabilization strongly rather than the parent R3c phase. FE-SEM micrograph supports the single phase characteristics without phase segregation at the grain boundaries. The stabilized Cc space group was explained based on the collective local distortion effects due to spin-orbit stabilization at Co3+ and Co2+ functional centres. The phonon mode changes as observed in the TiO6 octahedral modes also support the Cc phase stabilization. The major Co3+-ion presence was revealed from corresponding crystal field transitions observed through solid state diffuse reflectance spectroscopy. The enhanced spontaneous polarization (Ps) from ≅38 μC cm-2 to 45 μC cm-2 could be due to the easy rotation of polarization vector along the {(1\\bar{1}0)}{{pc}} in Cc phase. An increase in static dielectric response (ɛ) from ɛ ≅ 42 to 60 along with enhanced diffusivity from γ ≅ 1.53 to 1.75 was observed. Magneto-thermal irreversibility and their magnetic field dependent ZFC/FC curves suggest the possibility of a spin glass like behaviour below 50 K. The monoclinic Cc phase stabilization as confirmed from structural studies was well correlated with the observed ferroic properties in magnetically diluted NBT.

Tetravalent chromium (Cr(4+)) as laser-active ion for tunable solid-state lasers

NASA Technical Reports Server (NTRS)

Seas, A.; Petricevic, V.; Alfano, Robert R.

1993-01-01

Major accomplishments under NASA grant NAG-1-1346 are summarized. (1) numerical modeling of the four mirror astigmatically compensated, Z-fold cavity was performed and several design parameters to be used for the construction of a femtosecond forsterite laser were revealed by simulation. (2) femtosecond pulses from a continuous wave mode-locked chromium doped forsterite laser were generated. The forsterite laser was actively mode-locked using an acousto-optic modulator operating at 78 MHz with two Brewster high dispersion glass prisms for intra-cavity chirp compensation. Transform-limited sub-100-fs pulses were routinely generated in the TEM(sub 00) mode with 85 mW of continuous power tunable over 1230-1280 nm. The shortest pulses of 60-fs pulsewidth were measured. (3) Self-mode-locked operation of the Cr:forsterite laser was achieved. Synchronous pumping was used to mode lock the forsterite laser resulting in picosecond pulses, which in turn provided the starting mechanism for self-mode-locking. The pulses generated had an FWHM of 105 fs and were tunable between 1230-1270 nm. (4) Numerical calculations indicated that the pair of SF 14 prisms used in the cavity compensated for quadratic phase but introduced a large cubic phase term. Further calculations of other optical glasses indicated that a pair of SFN 64 prisms can introduce the same amount of quadratic phase as SF 14 prisms but introduce a smaller cubic phase. When the SF 14 prisms were replaced by SFN 64 prisms the pulsewidth was reduced to 50 fs. Great improvement was observed in the stability of the self mode-locked forsterite laser and in the ease of achieving mode locking. Using the same experimental arrangement and a new forsterite crystal with improved FOM the pulse width was reduced to 36 fs.

Phase-field model of vapor-liquid-solid nanowire growth

NASA Astrophysics Data System (ADS)

Wang, Nan; Upmanyu, Moneesh; Karma, Alain

2018-03-01

We present a multiphase-field model to describe quantitatively nanowire growth by the vapor-liquid-solid (VLS) process. The free-energy functional of this model depends on three nonconserved order parameters that distinguish the vapor, liquid, and solid phases and describe the energetic properties of various interfaces, including arbitrary forms of anisotropic γ plots for the solid-vapor and solid-liquid interfaces. The evolution equations for those order parameters describe basic kinetic processes including the rapid (quasi-instantaneous) equilibration of the liquid catalyst to a droplet shape with constant mean curvature, the slow incorporation of growth atoms at the droplet surface, and crystallization within the droplet. The standard constraint that the sum of the phase fields equals unity and the conservation of the number of catalyst atoms, which relates the catalyst volume to the concentration of growth atoms inside the droplet, are handled via separate Lagrange multipliers. An analysis of the model is presented that rigorously maps the phase-field equations to a desired set of sharp-interface equations for the evolution of the phase boundaries under the constraint of force balance at three-phase junctions (triple points) given by the Young-Herring relation that includes torque term related to the anisotropy of the solid-liquid and solid-vapor interface excess free energies. Numerical examples of growth in two dimensions are presented for the simplest case of vanishing crystalline anisotropy and the more realistic case of a solid-liquid γ plot with cusped minima corresponding to two sets of (10 ) and (11 ) facets. The simulations reproduce many of the salient features of nanowire growth observed experimentally, including growth normal to the substrate with tapering of the side walls, transitions between different growth orientations, and crawling growth along the substrate. They also reproduce different observed relationships between the nanowire growth velocity and radius depending on the growth condition. For the basic normal growth mode, the steady-state solid-liquid interface tip shape consists of a main facet intersected by two truncated side facets ending at triple points. The ratio of truncated and main facet lengths are in quantitative agreement with the prediction of sharp-interface theory that is developed here for faceted nanowire growth in two dimensions.

Bound acoustic modes in the radiation continuum in isotropic layered systems without periodic structures

NASA Astrophysics Data System (ADS)

Maznev, A. A.; Every, A. G.

2018-01-01

We study the existence of guided acoustic modes in layered structures whose phase velocity is higher than that of bulk waves in a solid substrate or an adjacent fluid half space, which belong to the class of bound states in the radiation continuum (BICs). We demonstrate that in contrast to the electromagnetic case, non-symmetry-protected BICs exist in isotropic layered systems without periodic structures. Two systems supporting non-symmetry-protected sagittally polarized BICs have been identified: (i) a supported solid layer yields BICs whose phase velocity is higher than the transverse velocity of the substrate but lower than the longitudinal velocity; (ii) a supported solid layer loaded by a fluid half space supports BICs whose velocity is higher that the bulk velocity of the fluid but lower than acoustic velocities of the substrate. The latter case is a unique example of BICs in the sense that it does not involve an evanescent field in the fluid half space providing the radiation continuum. In either case, BICs are represented by isolated points in the dispersion relations located within "leaky" branches. We show that these BICs are robust with respect to small perturbations of the system parameters. Numerical results are provided for realistic materials combinations. We also show that no BICs exist in all-fluid layered structures, whereas in solid layered structures there are no shear horizontal BICs and no sagittally polarized BICs whose velocity exceeds the longitudinal velocity of the substrate.

Fabrication and characterization of solid oxide cells for energy conversion and storage

NASA Astrophysics Data System (ADS)

Yang, Chenghao

2011-12-01

There has been an increasing interest in clean and renewable energy generation for highlighted energy and environmental concerns. Solid oxide cells (SOCs) have been considered as one of the promising technologies, since they can be operated efficiently both in electrolysis mode by generating hydrogen through steam electrolysis and fuel cell mode by electrochemically combining fuel with oxidant. The present work is devoted to performing a fundamental study of SOC in both fuel cell mode for power generation and electrolysis mode for fuel production. The research work on SOCs that can be operated reversibly for power generation and fuel production has been conducted in the following six projects: (1) High performance solid oxide electrolysis cell (SOEC) Fabrication of novel structured SOEC oxygen electrode with the conventional and commercial solid oxide fuel cell materials by screen-printing and infiltration fabrication methods. The microstructure, electrochemical properties and durability of SOECs has been investigated. It was found that the LSM infiltrated cell has an area specific resistance (ASR) of 0.20 Ω cm2 at 900°C at open circuit voltage with 50% absolute humidity (AH), which is relatively lower than that of the cell with LSM-YSZ oxygen electrode made by a conventional mixing method. Electrolysis cell with LSM infiltrated oxygen electrode has demonstrated stable performance under electrolysis operation with 0.33 A/cm2 and 50 vol.% AH at 800°C. (2) Advanced performance high temperature micro-tubular solid oxide fuel cell (MT-SOFC) Phase-inversion, dip-coating, high temperature co-sintering process and impregnation method were used to fabricate micro-tubular solid oxide fuel cell. The micro-structure of the micro-tubular fuel cell will be investigated and the power output and thermal robustness has been evaluated. High performance and rapid start-up behavior have been achieved, indicates that the MT-SOFC developed in this work can be a promising technology for portable applications. (3) Promising intermediate temperature micro-tubular solid oxide fuel cells for portable power supply applications Maximum power densities of 0.5, 0.38 and 0.27 W/cm2 have been obtained using H2-15% H2O as fuel at 550, 600 and 650°C, respectively. Quick thermal cycles performed on the intermediate temperature MT-SOFC stability demonstrate that the cell has robust performance stability for portable applications. (4) Micro-tubular solid oxide cell (MT-SOC) for steam electrolysis The electrochemical properties of MT-SOC will be investigated in detail in electrolysis mode. The mechanism of the novel hydrogen electrode structure benefiting the cell performance will be demonstrated systematically. The high electrochemical performance of the MT-SOC in electrolysis mode indicates that MT-SOC can provide an efficient hydrogen generation process. (5) Micro-tubular solid oxide cell (MT-SOC) for steam and CO2 co-electrolysis The MT-SOC will be operated in co-electrolysis mode for steam and CO 2, which will provide an efficient approach to generate syngas (H2+CO) without consuming fossil fuels. This can potentially provide an alternative superior approach for carbon sequestration which has been a critical issue facing the sustainability of our society. (6) Steam and CO2 co-electrolysis using solid oxide cells fabricated by freeze-drying tape-casting Tri-layer scaffolds have been prepared by freeze-drying tape casting process and the electrode catalysts are obtained by infiltrating the porous electrode substrates. Button cells will be tested for co-electrolysis of steam and CO2. The mechanism and efficiency of steam and CO2 co-electrolysis will be systemically investigated. In conclusion, SOCs have been fabricated with conventional materials and evaluated, but their performance has been found to be limited in either SOFC or SOEC mode. The cell performance has been significantly improved by employing an infiltrated LSM-YSZ electrode, due to dramatically decreased polarization resistance. However, mass transport limitation has been observed, particularly in electrolysis mode. By utilizing micro-tubular SOCs with novel hydrogen electrode produced via a phase inversion method, mass transport limitation has been mitigated. Finally, mass transport has been further improved by using cells with electrodes fabricated through a freeze-drying tape-casting method. (Abstract shortened by UMI.)

Application of cation-exchange solid-phase extraction for the analysis of amino alcohols from water and human plasma for verification of Chemical Weapons Convention.

PubMed

Kanaujia, Pankaj K; Tak, Vijay; Pardasani, Deepak; Gupta, A K; Dubey, D K

2008-03-28

The analysis of nitrogen containing amino alcohols, which are the precursors and degradation products of nitrogen mustards and nerve agent VX, constitutes an important aspect for verifying the compliance to the CWC (Chemical Weapons Convention). This work devotes on the development of solid-phase extraction method using silica- and polymer-based SCX (strong cation-exchange) and MCX (mixed-mode strong cation-exchange) cartridges for N,N-dialkylaminoethane-2-ols and alkyl N,N-diethanolamines, from water. The extracted analytes were analyzed by GC-MS (gas chromatography-mass spectrometry) in the full scan and selected ion monitoring modes. The extraction efficiencies of SCX and MCX cartridges were compared, and results revealed that SCX performed better. Extraction parameters, such as loading capacity, extraction solvent, its volume, and washing solvent were optimized. Best recoveries were obtained using 2 mL methanol containing 10% NH(4)OH and limits of detection could be achieved up to 5 x 10(-3) microg mL(-1) in the selected ion monitoring mode and 0.01 microg mL(-1) in full scan mode. The method was successfully employed for the detection and identification of amino alcohol present in water sample sent by Organization for Prohibition of Chemical Weapons (OPCW) in the official proficiency tests. The method was also applied to extract the analytes from human plasma. The SCX cartridge showed good recoveries of amino alcohols from human plasma after protein precipitation.

Solid-phase microextraction coupled to liquid chromatography for the analysis of phenolic compounds in water.

PubMed

González-Toledo, E; Prat, M D; Alpendurada, M F

2001-07-20

Solid-phase microextraction (SPME) coupled to high-performance liquid chromatography (HPLC) has been applied to the analysis of priority pollutant phenolic compounds in water samples. Two types of polar fibers [50 microm Carbowax-templated resin (CW-TPR) and 60 microm polydimethylsiloxane-divinylbenzene (PDMS-DVB)] were evaluated. The effects of equilibration time and ionic strength of samples on the adsorption step were studied. The parameters affecting the desorption process, such as desorption mode, solvent composition and desorption time, were optimized. The developed method was used to determine the phenols in spiked river water samples collected in the Douro River, Portugal. Detection limits of 1-10 microg l(-1) were achieved under the optimized conditions.

The autowave modes of solid phase polymerization of metal-containing monomers in two- and three-dimensional fiberglass-filled matrices.

PubMed

Barelko, V. V.; Pomogailo, A. D.; Dzhardimalieva, G. I.; Evstratova, S. I.; Rozenberg, A. S.; Uflyand, I. E.

1999-06-01

The phenomenon of autowave (frontal) solid phase polymerization of metal-containing monomers based on metal-acrylamide complexes is considered. The comparison of the features of autowave processes realized in both the single-component matrices of the monomer and the matrices filled by the fiberglass materials is performed. The unstable regimes of the polymerization wave as well as the conditions for the stabilization of the flat front in the filled matrices are described. The peculiarities of the frontal regimes in the three- and two-dimensional media are studied. Some possibilities for using of autowave polymerization in the fabrication of the polymer-fiberglass composites and composition prepregs are discussed. (c) 1999 American Institute of Physics.

Dual gauge field theory of quantum liquid crystals in three dimensions

DOE PAGES

Beekman, Aron J.; Nissinen, Jaakko; Wu, Kai; ...

2017-10-09

The dislocation-mediated quantum melting of solids into quantum liquid crystals is extended from two to three spatial dimensions, using a generalization of boson-vortex or Abelian-Higgs duality. Dislocations are now Burgers-vector-valued strings that trace out worldsheets in space-time while the phonons of the solid dualize into two-form (Kalb-Ramond) gauge fields. We propose an effective dual Higgs potential that allows for restoring translational symmetry in either one, two, or three directions, leading to the quantum analogues of columnar, smectic, or nematic liquid crystals. In these phases, transverse phonons turn into gapped, propagating modes, while compressional stress remains massless. Rotational Goldstone modes emergemore » whenever translational symmetry is restored. Lastly, we also consider the effective electromagnetic response of electrically charged quantum liquid crystals, and find among other things that as a hard principle only two out of the possible three rotational Goldstone modes are observable using propagating electromagnetic fields.« less

Dual gauge field theory of quantum liquid crystals in three dimensions

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

Beekman, Aron J.; Nissinen, Jaakko; Wu, Kai

The dislocation-mediated quantum melting of solids into quantum liquid crystals is extended from two to three spatial dimensions, using a generalization of boson-vortex or Abelian-Higgs duality. Dislocations are now Burgers-vector-valued strings that trace out worldsheets in space-time while the phonons of the solid dualize into two-form (Kalb-Ramond) gauge fields. We propose an effective dual Higgs potential that allows for restoring translational symmetry in either one, two, or three directions, leading to the quantum analogues of columnar, smectic, or nematic liquid crystals. In these phases, transverse phonons turn into gapped, propagating modes, while compressional stress remains massless. Rotational Goldstone modes emergemore » whenever translational symmetry is restored. Lastly, we also consider the effective electromagnetic response of electrically charged quantum liquid crystals, and find among other things that as a hard principle only two out of the possible three rotational Goldstone modes are observable using propagating electromagnetic fields.« less

[Determination of alkylphenol and alkylphenolpolyethoxylates in brine by solid phase extraction and high performance liquid chromatography-mass spectrometry].

PubMed

Wang, Jincheng; Xiong, Li; Zhang, Haijun; Chen, Jiping

2011-12-01

A simple method based on solid phase extraction (SPE) coupled with high performance liquid chromatography-mass spectrometry (HPLC-MS) was developed for the determination of octylphenol (OP), nonylphenol (NP), octylphenol ethoxylates (OPEOs) and nonylphenol ethoxylates (NPEOs) in brine. The extraction and cleanup of brine samples were performed on C18 solid-phase extraction cartridges. The complete separation among OP, NP, OPEOs and NPEOs was achieved on a Hypersil GOLD analytical column with methanol-water as the mobile phase. The determination was achieved using HPLC-MS with electrospray ionization (ESI) in selected ion monitoring mode. The results showed that the average recoveries of target compounds were 59.6% - 104.4% and the corresponding relative standard deviations (RSDs, n = 3) were 1.0% - 13.5%. The instrumental limits of detection for the compounds were 0.08 - 3 microg/L. This method was applied to the analysis of the samples of seawater near Dalian coast. The results showed that both NP and NPEOs were detected in all samples and their concentrations in seaport and oil port were much higher than those in other sampling sites.

Application of mixed-mode, solid-phase extraction in environmental and clinical chemistry. Combining hydrogen-bonding, cation-exchange and Van der Waals interactions

USGS Publications Warehouse

Mills, M.S.; Thurman, E.M.; Pedersen, M.J.

1993-01-01

Silica- and styrene-divinylbenzene-based mixed-mode resins that contain C8, C18 and sulphonated cation-exchange groups were compared for their efficiency in isolation of neutral triazine compounds from water and of the basic drug, benzoylecgonine, from urine. The triazine compounds were isolated by a combination of Van der Waals and hydrogen-bonding interactions, and benzoylecgonine was isolated by Van der Waals interactions and cation exchange. All analytes were eluted with a polar organic solvent contaning 2% ammonium hydroxide. Larger recoveries (95%) were achieved on copolymerized mixed-mode resins where C18 and sulfonic acid are in closer proximity than on 'blended' mixed-mode resins (60-70% recovery).

Thermomechanically coupled conduction mode laser welding simulations using smoothed particle hydrodynamics

NASA Astrophysics Data System (ADS)

Hu, Haoyue; Eberhard, Peter

2017-10-01

Process simulations of conduction mode laser welding are performed using the meshless Lagrangian smoothed particle hydrodynamics (SPH) method. The solid phase is modeled based on the governing equations in thermoelasticity. For the liquid phase, surface tension effects are taken into account to simulate the melt flow in the weld pool, including the Marangoni force caused by a temperature-dependent surface tension gradient. A non-isothermal solid-liquid phase transition with the release or absorption of additional energy known as the latent heat of fusion is considered. The major heat transfer through conduction is modeled, whereas heat convection and radiation are neglected. The energy input from the laser beam is modeled as a Gaussian heat source acting on the initial material surface. The developed model is implemented in Pasimodo. Numerical results obtained with the model are presented for laser spot welding and seam welding of aluminum and iron. The change of process parameters like welding speed and laser power, and their effects on weld dimensions are investigated. Furthermore, simulations may be useful to obtain the threshold for deep penetration welding and to assess the overall welding quality. A scalability and performance analysis of the implemented SPH algorithm in Pasimodo is run in a shared memory environment. The analysis reveals the potential of large welding simulations on multi-core machines.

Determination of bisphenols in beverages by mixed-mode solid-phase extraction and liquid chromatography coupled to tandem mass spectrometry.

PubMed

Regueiro, Jorge; Wenzl, Thomas

2015-11-27

Facing growing restrictions on the use of bisphenol A in food contact materials, several bisphenol analogs are arising as major alternatives to replace this chemical in most of its applications. This work reports a simple and robust method based on mixed-mode solid-phase extraction and stable-isotope dilution liquid chromatography-tandem mass spectrometry for the analysis of bisphenol A and its main analogs - bisphenol S, 4,4'-sulfonylbis(2-methylphenol), bisphenol F, bisphenol E, bisphenol B, bisphenol Z, bisphenol AF, bisphenol AP, tetrabromobisphenol A and bisphenol P - in alcoholic and non-alcoholic beverages. Mixed-mode solid-phase extraction, combining cationic exchange and reversed-phase mechanisms, was optimized to provide a selective extraction and purification of the target analytes. Derivatization of bisphenols with pyridine-3-sulfonyl chloride allowed increasing their ionization efficiency by electrospray ionization. Validation of the proposed method was performed in terms of selectivity, matrix effects, linearity, precision, measurement uncertainty, trueness and limits of detection. Satisfactory repeatability and intermediate precision were obtained; the related relative standard deviations were ≤9% and ≤12%, respectively. The relative expanded uncertainty (k=2) was below 20% for all bisphenol analogs and the trueness of the method was demonstrated by recovery experiments. Limits of detection (LOD) ranged from 1.6ngL(-1) to 27.9ngL(-1) for all compounds. Finally, several canned and non-canned beverages were analyzed to demonstrate the applicability of the method. Only bisphenol A and three bisphenol F isomers were detected in any of the samples. Bisphenol A concentration ranged from

Soft Phonon Modes Leading to Ultralow Thermal Conductivity and High Thermoelectric Performance in AgCuTe.

PubMed

Roychowdhury, Subhajit; Jana, Manoj K; Pan, Jaysree; Guin, Satya N; Sanyal, Dirtha; Waghmare, Umesh V; Biswas, Kanishka

2018-04-03

Crystalline solids with intrinsically low lattice thermal conductivity (κ L ) are crucial to realizing high-performance thermoelectric (TE) materials. Herein, we show an ultralow κ L of 0.35 Wm -1  K -1 in AgCuTe, which has a remarkable TE figure-of-merit, zT of 1.6 at 670 K when alloyed with 10 mol % Se. First-principles DFT calculation reveals several soft phonon modes in its room-temperature hexagonal phase, which are also evident from low-temperature heat-capacity measurement. These phonon modes, dominated by Ag vibrations, soften further with temperature giving a dynamic cation disorder and driving the superionic transition. Intrinsic factors cause an ultralow κ L in the room-temperature hexagonal phase, while the dynamic disorder of Ag/Cu cations leads to reduced phonon frequencies and mean free paths in the high-temperature rocksalt phase. Despite the cation disorder at elevated temperatures, the crystalline conduits of the rigid anion sublattice give a high power factor. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Direct measurement of the glucuronide conjugate of 1-hydroxypyrene in human urine by using liquid chromatography with tandem mass spectrometry.

PubMed

Kakimoto, Kensaku; Toriba, Akira; Ohno, Takanori; Ueno, Mariko; Kameda, Takayuki; Tang, Ning; Hayakawa, Kazuichi

2008-05-15

To evaluate human exposure to polycyclic aromatic hydrocarbons (PAHs), we developed a rapid, simple and sensitive method for determining 1-hydroxypyrene-glucuronide (1-OHP-G) in human urine. To improve precision, a deuterated glucuronide was used as an internal standard. The method requires only 1 mL of urine. The urine was treated with a mixed-mode anion-exchange and reversed-phase solid-phase extraction cartridge (Oasis MAX). The analytes were analyzed with a C(18) reversed-phase column with a gradient elution, followed by tandem mass spectrometry with electrospray ionization in negative ion mode. The detection limit of 1-OHP-G (corresponding to a signal-to-noise ratio of 3) was 0.13 fmol/injection. Urinary concentrations of 1-OHP-G determined by this method were strongly correlated (r(2)=0.961) with concentrations of 1-hydroxypyrene by conventional HPLC with fluorescence detection.

Simultaneous determination of all-trans and 13-cis retinoic acids and their 4-oxo metabolites by adsorption liquid chromatography after solid-phase extraction.

PubMed

Lefebvre, P; Agadir, A; Cornic, M; Gourmel, B; Hue, B; Dreux, C; Degos, L; Chomienne, C

1995-04-07

All-trans retinoic acid (all-trans RA), the active metabolite of vitamin A, has been demonstrated to be an efficient alternative to chemotherapy in the treatment of acute promyelocytic leukemia (APL), the AML3 subtype of the FAB cytological classification. Complete remission is obtained by inducing terminal granulocytic differentiation of the leukemic cells. To study all-trans RA pharmacokinetics in patients with APL, a rapid, precise and selective high-performance liquid chromatographic (HPLC) assay was developed. This method is easy and shows good repeatability (C.V. = 8.41-12.44%), reproducibility (C.V. = 9.19-14.73%), accuracy (C.V. = 3.5-11%) and sensitivity with a detection limit of 5 pmol/ml. The analysis is performed using normal-phase HPLC in an isocratic mode with UV detection after solid-phase extraction on octadecyl (C18) columns. The mobile phase is hexane-dichloromethane-dioxane (78:18:4, v/v) containing 1% acetic acid.

[Determination of 11 anabolic hormones in fish tissue by multi-function impurity adsorption solid-phase extraction-ultrafast liquid chromatography-tandem mass spectrometry].

PubMed

Yao, Shanshan; Zhao, Yonggang; Li, Xiaoping; Chen, Xiaohong; Jin, Micong

2012-06-01

A method was developed for the determination of 11 anabolic hormones (boldenone, androstenedione, nandrolone, methandrostenolone, methyltestosterone, testosterone, testosterone acetate, trenbolone, testosterone propionate, stanozolol, fluoxymesterone) in fish by multi-function impurity adsorption solid-phase extraction-ultrafast liquid chromatography-tandem mass spectrometry. After the sample was extracted by methanol, the extract was cleaned-up quickly by C18 adsorbent, neutral alumina adsorbent and amino-functionalized nano-adsorbent. The separation was performed on a Shim-Pack XR-ODS II column (100 mm x 2.0 mm, 2.2 microm) using the mobile phases of 0.1% (v/v) formic acid in acetonitrile and 0.1% (v/v) formic acid solution in a gradient elution mode. The identification and quantification were achieved by using electrospray ionization in positive ion mode (ESI+) in multiple reaction monitoring (MRM) mode. The matrix-matched external standard calibration curves were used for quantitative determination. The results showed that the calibration curves were in good linearity for the eleven analytes with the correlation coefficients (r) more than 0.999. The limits of detection (LODs, S/N > 3) for the 11 anabolic hormones were from 0.03 microg/kg to 0.4 microg/kg and the limits of quantification (LOQs, S/N > 10) were from 0.1 microg/kg to 1.5 microg/kg. The average recoveries ranged from 80.9% to 98.1% with the relative standard deviations between 5.2% and 11.5%. The method is simple, rapid, sensitive, accurate and suitable for the quantitative determination and confirmation of the 11 anabolic hormones in fish.

High speed real-time wavefront processing system for a solid-state laser system

NASA Astrophysics Data System (ADS)

Liu, Yuan; Yang, Ping; Chen, Shanqiu; Ma, Lifang; Xu, Bing

2008-03-01

A high speed real-time wavefront processing system for a solid-state laser beam cleanup system has been built. This system consists of a core2 Industrial PC (IPC) using Linux and real-time Linux (RT-Linux) operation system (OS), a PCI image grabber, a D/A card. More often than not, the phase aberrations of the output beam from solid-state lasers vary fast with intracavity thermal effects and environmental influence. To compensate the phase aberrations of solid-state lasers successfully, a high speed real-time wavefront processing system is presented. Compared to former systems, this system can improve the speed efficiently. In the new system, the acquisition of image data, the output of control voltage data and the implementation of reconstructor control algorithm are treated as real-time tasks in kernel-space, the display of wavefront information and man-machine conversation are treated as non real-time tasks in user-space. The parallel processing of real-time tasks in Symmetric Multi Processors (SMP) mode is the main strategy of improving the speed. In this paper, the performance and efficiency of this wavefront processing system are analyzed. The opened-loop experimental results show that the sampling frequency of this system is up to 3300Hz, and this system can well deal with phase aberrations from solid-state lasers.

Analysis of Rayleigh-Lamb Modes in Soft-solids with Application to Surface Wave Elastography

NASA Astrophysics Data System (ADS)

Benech, Nicolás; Grinspan, Gustavo; Aguiar, Sofía; Brum, Javier; Negreira, Carlos; tanter, Mickäel; Gennisson, Jean-Luc

The goal of Surface Wave Elastography (SE) techniques is to estimate the shear elasticity of the sample by measuring the surface wave speed. In SE the thickness of the sample is often assumed to be infinite, in this way, the surface wave speed is directly linked to the sample's shear elasticity. However for many applications this assumption is not true. In this work, we study experimentally the Rayleigh-Lamb modes in soft solids of finite thickness to explore the optimal conditions for SWE. Experiments were carried out in three tissue mimicking phantoms of different thicknesses (10 mm, 20 mm and 60 mm) and same shear elasticity. The surface waves were generated at the surface of the phantom using piston attached to a mechanical vibrator. The central frequency of the excitation was varied between 60 Hz to 160 Hz. One component of the displacement field generated by the piston was measured at the surface and in the bulk of the sample trough a standard speckle tracking technique using a 256 element, 7.5 MHz central frequency linear array and an ultrasound ultrafast electronics. Finally, by measuring the phase velocity at each excitation frequency, velocity dispersion curves were obtained for each phantom. The results show that instead of a Rayleigh wave, zero order symmetric (S0) and antisymmetric (A0) Lamb modes are excited with this type of source. Moreover, in this study we show that due to the near field effects of the source, which are appreciable only in soft solids at low frequencies, both Lamb modes are separable in time and space. We show that while the Ao mode dominates close the source, the S0 mode dominates far away.

Superradiant phase transition with graphene embedded in one dimensional optical cavity

NASA Astrophysics Data System (ADS)

Li, Benliang; Liu, Tao; Hewak, Daniel W.; Wang, Qi Jie

2018-01-01

We theoretically investigate the cavity QED of graphene embedded in an optical cavity under perpendicular magnetic field. We consider the coupling of cyclotron transition and a multimode cavity described by a multimode Dicke model. This model exhibits a superradiant quantum phase transition, which we describe exactly in an effective Hamiltonian approach. The complete excitation spectrum in both the normal phase and superradiant phase regimes is given. In contrast to the single mode case, multimode coupling of cavity photon and cyclotron transition can greatly reduce the critical vacuum Rabi frequency required for quantum phase transition, and dramatically enhance the superradiant emission by fast modulating the Hamiltonian. Our work paves a way to experimental explorations of quantum phase transitions in solid state systems.

Determination of hydroxyaromatic compounds in water by solid-phase microextraction coupled to high-performance liquid chromatography.

PubMed

Wu, Y C; Huang, S D

1999-03-12

Solid-phase microextraction (SPME) coupled with high-performance liquid chromatography (HPLC) for the analysis of hydroxyaromatic compounds is described. Three kinds of fibers [50 microns carbowax-templated resin (CW-TPR), 60 microns polydimethylsiloxane-divinylbenzene (PDMS-DVB) and 85 microns polyacrylate (PA) fibers] were evaluated. CW-TPR and PDMS-DVB were selected for further study. The parameters of the desorption procedure (such as desorption mode, the composition of the solvent for desorption and the duration of fiber soaking) were studied and optimized. The effect of the structure and physical properties of analytes, carryover, duration of absorption, temperature of absorption, pH and ionic strength of samples were also investigated. The method was applied to environmental samples (lake water) using a simple calibration curve.

Determination of artificial sweeteners in water samples by solid-phase extraction and liquid chromatography-tandem mass spectrometry.

PubMed

Ordóñez, Edgar Y; Quintana, José Benito; Rodil, Rosario; Cela, Rafael

2012-09-21

The development and performance evaluation of an analytical method for the determination of six artificial sweeteners in environmental waters using solid-phase extraction (SPE) followed by liquid chromatography-tandem mass spectrometry are presented. To this end, different SPE alternatives have been evaluated: polymeric reversed-phase (Oasis HLB, Env+, Plexa and Strata X), and mixed-mode with either weak (Oasis WAX) or strong anionic-exchange (Oasis MAX and Plexa PAX) sorbents. Among them, reversed-phase sorbents, particularly Oasis HLB and Strata X, showed the best performance. Oasis HLB provided good trueness (recoveries: 73-112%), precision (RSD<10%) and limits of quantification (LOQ: 0.01-0.5 μg/L). Moreover, two LC separation mechanisms were evaluated: reversed-phase (RPLC) and hydrophilic interaction (HILIC), with RPLC providing better performance than HILIC. The final application of the method showed the presence of acesulfame, cyclamate, saccharin and sucralose in the wastewater and surface water samples analyzed at concentrations up to 54 μg/L. Copyright © 2012 Elsevier B.V. All rights reserved.

Phase diagram and high-pressure boundary of hydrate formation in the ethane-water system.

PubMed

Kurnosov, Alexander V; Ogienko, Andrey G; Goryainov, Sergei V; Larionov, Eduard G; Manakov, Andrey Y; Lihacheva, Anna Y; Aladko, Eugeny Y; Zhurko, Fridrikh V; Voronin, Vladimir I; Berger, Ivan F; Ancharov, Aleksei I

2006-11-02

Dissociation temperatures of gas hydrate formed in the ethane-water system were studied at pressures up to 1500 MPa. In situ neutron diffraction analysis and X-ray diffraction analysis in a diamond anvil cell showed that the gas hydrate formed in the ethane-water system at 340, 700, and 1840 MPa and room temperature belongs to the cubic structure I (CS-I). Raman spectra of C-C vibrations of ethane molecules in the hydrate phase, as well as the spectra of solid and liquid ethane under high-pressure conditions were studied at pressures up to 6900 MPa. Within 170-3600 MPa Raman shift of the C-C vibration mode of ethane in the hydrate phase did not show any discontinuities, which could be evidence of possible phase transformations. The upper pressure boundary of high-pressure hydrate existence was discovered at the pressure of 3600 MPa. This boundary corresponds to decomposition of the hydrate to solid ethane and ice VII. The type of phase diagram of ethane-water system was proposed in the pressure range of hydrate formation (0-3600 MPa).

Comparison of direct, headspace and headspace cold fiber modes in solid phase microextraction of polycyclic aromatic hydrocarbons by a new coating based on poly(3,4-ethylenedioxythiophene)/graphene oxide composite.

PubMed

Banitaba, Mohammad Hossein; Hosseiny Davarani, Saied Saeed; Kazemi Movahed, Siyavash

2014-01-17

A novel nanocomposite coating made of poly(3,4-ethylenedioxythiophene) (PEDOT) and graphene oxide was electrochemically prepared on gold wire. The prepared fiber was applied to the solid-phase microextraction (SPME) and gas chromatographic analysis of six polycyclic aromatic hydrocarbons (PAHs). Three modes of extraction i.e. direct immersion (DI), headspace (HS) and headspace cold fiber (HS-CF) in SPME were investigated. The results were compared under optimized conditions of each mode, considering the effects of the three most important parameters which are extraction temperature, extraction time and ionic strength. The comparison showed that HS-CF-SPME results in the best outcome for the extraction of PAHs from water samples. Under the optimized conditions of this mode, the calibration curves were linear within the range of 0.4-600μgL(-1) and the detection limits were between 0.05 and 0.13μgL(-1). The intra-day and inter-day relative standard deviations obtained at 10μgL(-1) (n=5), using a single fiber, were 4.1-6.8% and 4.8-8.4%, respectively. The fiber-to-fiber repeatabilities (n=4), expressed as the relative standard deviations (RSD%), were between 6.5% and 10.7% at a 10μgL(-1) concentration level. The method was successfully applied to the analysis of PAHs in seawater samples showing recoveries from 85% to 107%. Copyright © 2013 Elsevier B.V. All rights reserved.

Microphysics of liquid complex plasmas in equilibrium and non-equilibrium systems

NASA Astrophysics Data System (ADS)

Piel, Alexander; Block, Dietmar; Melzer, André; Mulsow, Matthias; Schablinski, Jan; Schella, André; Wieben, Frank; Wilms, Jochen

2018-05-01

The dynamic evolution of the microscopic structure of solid and liquid phases of complex plasmas is studied experimentally and by means of molecular dynamics (MD) simulations. In small finite systems, the cooperative motion can be described in terms of discrete modes. These modes are studied with different experimental approaches. Using diffuse scattered laser light, applying laser tweezer forces to individual particles, and periodic laser pulses, the excitation of modes is investigated. The instantaneous normal mode analysis of experimental data from two-dimensional liquid clusters gives access to the local dynamics of the liquid phase. Our investigations shed light on the role of compressional and shear modes as well as the determination of diffusion constants and melting temperatures in finite systems. Special attention is paid to hydrodynamic situations with a stationary inhomogeneous dust flow. MD simulations allow to study the collective motion in the shell of nearest neighbors, which can be linked to smooth and sudden changes of the macroscopic flow. Finally, the observed micro-motion in all situations above allows to shed light on the preference of shear-like over compressional motion in terms of a minimized potential energy and a dynamic incompressibility.

Theory of the spin-1 bosonic liquid metal - Equilibrium properties of liquid metallic deuterium

NASA Technical Reports Server (NTRS)

Oliva, J.; Ashcroft, N. W.

1984-01-01

The theory of a two-component quantum fluid comprised of spin-1/2 fermions and nonzero spin bosons is examined. This system is of interest because it embodies a possible quantum liquid metallic phase of highly compressed deuterium. Bose condensation is assumed present and the two cases of nuclear-spin-polarized and -unpolarized systems are considered. A significant feature in the unpolarized case is the presence of a nonmagnetic mode with quadratic dispersion owing its existence to nonzero boson spin. The physical character of this mode is examined in detail within a Bogoliubov approach. The specific heat, bulk modulus, spin susceptibility, and thermal expansion are all determined. Striking contrasts in the specific heats and thermal-expansion coefficients of the liquid and corresponding normal solid metallic phase are predicted.

Graphene/TiO2 nanocomposite based solid-phase extraction and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry for lipidomic profiling of avocado (Persea americana Mill.).

PubMed

Shen, Qing; Yang, Mei; Li, Linqiu; Cheung, Hon-Yeung

2014-12-10

Phospholipids possess important physiological, structural and nutritional functions in biological systems. This study described a solid-phase extraction (SPE) method, employing graphene and titanium dioxide (G/TiO2) nanocomposite as sorbent, for the selective isolation and enrichment of phospholipids from avocado (Persea americana Mill.). Based on the principal that the phosphoryl group in the phospholipid can interact with TiO2 via a bridging bidentate mode, an optimum condition was established for SPE, and was successfully applied to prepare avocado samples. The extracts were monitored by matrix-assisted laser desorption ionization time-of-flight/tandem mass spectrometry (MALDI-TOF/MS) in both positive-ion and negative-ion modes. Results showed that phospholipids could be efficiently extracted in a clean manner by G/TiO2 based SPE. In addition, the signals of phospholipids were enhanced while the noise was reduced. Some minor peaks became more obvious. In conclusion, the nanocomposite material of G/TiO2 was proved to be a promising sorbent for selective separation of phospholipids from crude lipid extract. Copyright © 2014 The Authors. Published by Elsevier B.V. All rights reserved.

[Analysis of sulfonamids and their metabolites in drinking water by high Performance liquid chromatography tandem mass spectrometry].

PubMed

Wang, Shuo; Li, Shuming; Zhang, Xiangming; Wei, Yunfang; Zhang, Meiyun; Zhang, Jing

2015-07-01

To develop a comprehensive method for simultaneous analysis of sulfonamides and their metabolites in drinking water by high performance liquid chromatography tandem mass spectrometry (LC-MS/MS). Different solid-phase extraction columns were compared with respect to the recovery of target drugs from drinking water. The drinking water samples were adjusted to 3 by HCl and purified by a mix mode cation-ion exchange solid-phase extraction (SPE), following determination using LG-MS/MS. A total of 21 sulfonamides were separated by a C15 column (2.1 mm x 100 mm, 1.7 µm) and analyzed under positive ion mode with multi-reaction monitoring. The matrix-matched external standard calibration was used for quantification. The method quantification limits for 21 analytes were 0.03-0.63 ng/L with overall recoveries of 50.1%-114.9%, and the relative standard deviations less than 20%. The method was finally used to analyze sulfonamides in drinking water in Beijing, and 5 target compounds (sulfadiazine, sulfathiazole, sulfapyridine, trimethoprim and sulfamethazine) were detected at a concentration range of 0.08-32.54 ng/L. This method could be applied in simultaneous analysis of sulfonamides and their metabolites in drinking water samples.

Validated Method for the Quantification of Baclofen in Human Plasma Using Solid-Phase Extraction and Liquid Chromatography–Tandem Mass Spectrometry

PubMed Central

Nahar, Limon Khatun; Cordero, Rosa Elena; Nutt, David; Lingford-Hughes, Anne; Turton, Samuel; Durant, Claire; Wilson, Sue; Paterson, Sue

2016-01-01

Abstract A highly sensitive and fully validated method was developed for the quantification of baclofen in human plasma. After adjusting the pH of the plasma samples using a phosphate buffer solution (pH 4), baclofen was purified using mixed mode (C8/cation exchange) solid-phase extraction (SPE) cartridges. Endogenous water-soluble compounds and lipids were removed from the cartridges before the samples were eluted and concentrated. The samples were analyzed using triple-quadrupole liquid chromatography–tandem mass spectrometry (LC–MS-MS) with triggered dynamic multiple reaction monitoring mode for simultaneous quantification and confirmation. The assay was linear from 25 to 1,000 ng/mL (r2 > 0.999; n = 6). Intraday (n = 6) and interday (n = 15) imprecisions (% relative standard deviation) were <5%, and the average recovery was 30%. The limit of detection of the method was 5 ng/mL, and the limit of quantification was 25 ng/mL. Plasma samples from healthy male volunteers (n = 9, median age: 22) given two single oral doses of baclofen (10 and 60 mg) on nonconsecutive days were analyzed to demonstrate method applicability. PMID:26538544

[Determination of paraquat and diquat in drinking water and environmental water by high performance liquid chromatography coupled with on-line clean-up and solid phase extraction].

PubMed

Chen, Jing; Liu, Zhaojin; An, Baochao; Lu, Yan; Xu, Qun

2012-10-01

An on-line solid phase extraction (SPE) system was used to eliminate the interferences sufficiently and fulfill the simple and sensitive determination of diquat and paraquat in tap and pond water. This on-line SPE system used two SPE cartridges. One was an Acclaim Mixed-Mode WAX-1 cartridge for the elimination of anionic interferences; the other one was an Acclaim Mixed-Mode WCX-1 cartridge for the enrichment of diquat and paraquat and the elimination of co-enriched cationic interferences. The baseline separation of diquat and paraquat was achieved on an Acclaim Trinity P1 column. A dual-gradient high performance liquid chromatographic (HPLC) system provided an efficient platform to fulfill the on-line SPE and separation, and the system operated under automatic control of chromatography data system software. The complete analysis only required 16 min, and the detection limits of the method were 0.12 microg/L for diquat and 0.10 microg/L for paraquat. The method is simple, rapid and sensitive, and can be applied to the determination of diquat and paraquat in drinking water and environmental water.

Developments in coupled solid-phase extraction-capillary electrophoresis 2013-2015.

PubMed

Ramautar, Rawi; Somsen, Govert W; de Jong, Gerhardus J

2016-01-01

An overview of the design and application of coupled solid-phase extraction-capillary electrophoresis (SPE-CE) systems reported in the literature between July 2013 and June 2015 is provided in this paper. The present article is a continuation of our previous review papers on this topic which covered the time period 2000-2013 (Electrophoresis 2008, 29, 108-128; Electrophoresis 2010, 31, 44-54; Electrophoresis 2012, 33, 243-250; Electrophoresis 2014, 35, 128-137). The use of in-line and on-line SPE-CE approaches is treated and outlined in this review. Recent advancements, such as, for example, the use of aptamers as affinity material for in-line SPE-CE, the use of a bead string design for in-line fritless SPE-CE, and new interfacing techniques for the on-line coupling of SPE to CE, are outlined. Selected examples demonstrate the applicability of the coupled SPE-CE systems for biomedical, pharmaceutical, environmental, and food studies. A complete overview of the recent SPE-CE studies is given in table format, providing information on sample type, SPE sorbent, coupling mode, detection mode, and LOD. Finally, some general conclusions and perspectives are provided. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analytical study of the acoustic field in a spherical resonator for single bubble sonoluminescence.

PubMed

Dellavale, Damián; Urteaga, Raúl; Bonetto, Fabián J

2010-01-01

The acoustic field in the liquid within a spherical solid shell is calculated. The proposed model takes into account Stoke's wave equation in the viscous fluid, the membrane theory to describe the solid shell motion and the energy loss through the external couplings of the system. A point source at the resonator center is included to reproduce the acoustic emission of a sonoluminescence bubble. Particular calculations of the resulting acoustic field are performed for viscous liquids of interest in single bubble sonoluminescence. The model reveals that in case of radially symmetric modes of low frequency, the quality factor is mainly determined by the acoustic energy flowing through the mechanical coupling of the resonator. Alternatively, for high frequency modes the quality factor is mainly determined by the viscous dissipation in the liquid. Furthermore, the interaction between the bubble acoustic emission and the resonator modes is analyzed. It was found that the bubble acoustic emission produces local maxima in the resonator response. The calculated amplitudes and relative phases of the harmonics constituting the bubble acoustic environment can be used to improve multi-frequency driving in sonoluminescence.

Infrared spectroscopic studies of the conformation in ethyl alpha-haloacetates in the vapor, liquid and solid phases.

PubMed

Jassem, Naserallah A; El-Bermani, Muhsin F

2010-07-01

Infrared spectra of ethyl alpha-fluoroacetate, ethyl alpha-chloroacetate, ethyl alpha-bromoacetate and ethyl alpha-iodoacetate have been measured in the solid, liquid and vapor phases in the region 4000-200 cm(-1). Vibrational frequency assignment of the observed bands to the appropriate modes of vibration was made. Calculations at DFT B3LYP/6-311+G** level, Job: conformer distribution, using Spartan program '08, release 132 was made to determine which conformers exist in which molecule. The results indicated that the first compound exists as an equilibrium mixture of cis and trans conformers and the other three compounds exist as equilibrium mixtures of cis and gauche conformers. Enthalpy differences between the conformers have been determined experimentally for each compound and for every phase. The values indicated that the trans of the first compound is more stable in the vapor phase, while the cis is the more stable in both the liquid and solid phases. In the other three compounds the gauche is more stable in the vapor and liquid phases, while the cis conformer is the more stable in the solid phase for each of the second and third compound, except for ethyl alpha-iodoacetate, the gauche conformer is the more stable over the three phases. Molar energy of activation Ea and the pseudo-thermodynamic parameters of activation DeltaH(double dagger), DeltaS(double dagger) and DeltaG(double dagger) were determined in the solid phase by applying Arrhenius equation; using bands arising from single conformers. The respective E(a) values of these compounds are 5.1+/-0.4, 6.7+/-0.1, 7.5+/-1.3 and 12.0+/-0.6 kJ mol(-1). Potential energy surface calculations were made at two levels; for ethyl alpha-fluoroacetate and ethyl alpha-chloroacetate; the calculations were established at DFT B3LYP/6-311+G** level and for ethyl alpha-bromoacetate and ethyl alpha-iodoacetate at DFT B3LYP/6-311G* level. The results showed no potential energy minimum exists for the gauche conformer in ethyl alpha-fluoroacetate. Copyright 2010 Elsevier B.V. All rights reserved.

Solid-state carrier-envelope phase stabilization via quantum interference control of injected photocurrents.

PubMed

Roos, P A; Li, Xiaoqin; Smith, R P; Pipis, Jessica A; Fortier, T M; Cundiff, S T

2005-04-01

We demonstrate carrier-envelope phase stabilization of a mode-locked Ti:sapphire laser by use of quantum interference control of injected photocurrents in a semiconductor. No harmonic generation is required for this stabilization technique. Instead, interference between coexisting single- and two-photon absorption pathways in the semiconductor provides a phase comparison between different spectral components. The phase comparison, and the detection of the photocurrent that it produces, both occur within a single low-temperature-grown gallium arsenide sample. The carrier-envelope offset beat note fidelity is 30 dB in a 10-kHz resolution bandwidth. The out-of-loop phase-noise level is essentially identical to the best previous measurements with the standard self-referencing technique.

Infrared spectra of molecules and materials of astrophysical interest

NASA Technical Reports Server (NTRS)

Durig, J. R.

1978-01-01

The Raman spectra of gaseous, liquid and solid, and infrared spectra of gaseous and solid isopropylamine-d sub 0 and -d sub 2 was investigated between 4000 and 50 cm superscript -1. Differences between the spectrum of the solid phase and that of the fluid phases were interpreted in terms of an equilibrium between low energy s-trans and high energy gauche conformers, and a complete vibrational assignment was proposed for the s-trans conformer. The far infrared spectra of the gaseous compounds contained bands due to the asymmetric amino and coupled methyl torsions; the assignment of these bands was aided by observation of a number of two quantum transitions for each vibrational mode. The asymmetric potential functions were calculated, which resulted in values for the enthalpy differences between conformers in the gaseous phase of 446 and 523 callmole for the sub 0 -d and -d sub 2 compounds, respectively. The methyl torsional potential function of isopropylamine-d sub 0 was calculated which led to a value for the barrier height to internal rotation of the methyl rotors of 4.23 + or - 0.06 kcal/mole. Values for the ideal gas thermodynamic functions were calculated over a range of temperatures.

Method of analysis and quality-assurance practices for determination of pesticides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry at the U.S. Geological Survey California District Organic Chemistry Laboratory, 1996-99

USGS Publications Warehouse

Crepeau, Kathryn L.; Baker, Lucian M.; Kuivila, Kathryn

2000-01-01

A method of analysis and quality-assurance practices were developed to study the fate and transport of pesticides in the San Francisco Bay-Estuary by the U.S. Geological Survey. Water samples were filtered to remove suspended-particulate matter and pumped through C-8 solid-phase extraction cartridges to extract the pesticides. The cartridges were dried with carbon dioxide and the pesticides were eluted with three cartridge volumes of hexane:diethyl ether (1:1) solution. The eluants were analyzed using capillary-column gas chromatography/mass spectrometry in full-scan mode. Method detection limits for pesticides ranged from 0.002 to 0.025 microgram per liter for 1-liter samples. Recoveries ranged from 44 to 140 percent for 25 pesticides in samples of organic-free reagent water and Sacramento-San Joaquin Delta and Suisun Bay water fortified at 0.05 and 0.50 microgram per liter. The estimated holding time for pesticides after extraction on C-8 solid-phase extraction cartridges ranged from 10 to 257 days.

Analysis of some cytokinins in coconut (Cocos nucifera L.) water by micellar electrokinetic capillary chromatography after solid-phase extraction.

PubMed

Ge, Liya; Yong, Jean Wan Hong; Tan, Swee Ngin; Yang, Xin Hao; Ong, Eng Shi

2004-09-03

Micellar electrokinetic capillary chromatography (MECC) was developed for the separation of cytokinins including trans-zeatin, trans-zeatin-O-glucoside, dihydrozeatin, dihydrozeatin-O-glucoside, meta-topolin riboside, N6-isopentenyladenine and N6-benzylaminopurine. Under the optimum conditions, i.e. a combination of 10 mM phosphate and 10 mM borate as the running buffer containing 50 mM sodium dodecyl sulphate at pH 10.4, the separation of seven cytokinin standards was accomplished within 11 min. The C18 solid-phase extraction (SPE) method was used to pre-concentrate the putative cytokinins present in the coconut water. Following which, the eluate was further purified using mixed mode Oasis MCX SPE columns and this additional step helps to reduce matrix interference during MECC. After the two solid-phase extraction steps, the optimized MECC method was able to screen for certain cytokinins (zeatin-O-glucoside and dihydrozeatin-O-glucoside) present in coconut water. After this screening, the presence of zeatin-O-glucoside and dihydrozeatin-O-glucoside in coconut water was further confirmed by independent high-performance liquid chromatography and liquid chromatography-mass spectrometry experiments.

MSPD procedure for determining buprofezin, tetradifon, vinclozolin, and bifenthrin residues in propolis by gas chromatography-mass spectrometry.

PubMed

dos Santos, Thaíse Fernanda Santana; Aquino, Adriano; Dórea, Haroldo Silveira; Navickiene, Sandro

2008-03-01

A simple and effective extraction method based on matrix solid-phase dispersion (MSPD) was developed to determine bifenthrin, buprofezin, tetradifon, and vinclozolin in propolis using gas chromatography-mass spectrometry in selected ion monitoring mode (GC-MS, SIM). Different method conditions were evaluated, for example type of solid phase (C(18), alumina, silica, and Florisil), the amount of solid phase and eluent (n-hexane, dichloromethane, dichloromethane-n-hexane (8:2 and 1:1, v/v) and dichloromethane-ethyl acetate (9:1, 8:2 and 7:3, v/v)). The best results were obtained using 0.5 g propolis, 1.0 g silica as dispersant sorbent, 1.0 g Florisil as clean-up sorbent, and dichloromethane-ethyl acetate (9:1, v/v) as eluting solvent. The method was validated by analysis of propolis samples fortified at different concentration levels (0.25 to 1.0 mg kg(-1)). Average recoveries (four replicates) ranged from 67% to 175% with relative standard deviation between 5.6% and 12.1%. Detection and quantification limits ranged from 0.05 to 0.10 mg kg(-1) and 0.15 to 0.25 mg kg(-1) propolis, respectively.

Simple method for the determination of personal care product ingredients in lettuce by ultrasound-assisted extraction combined with solid-phase microextraction followed by GC-MS.

PubMed

Cabrera-Peralta, Jerónimo; Peña-Alvarez, Araceli

2018-05-01

A simple method for the simultaneous determination of personal care product ingredients: galaxolide, tonalide, oxybenzone, 4-methylbenzyliden camphor, padimate-o, 2-ethylhexyl methoxycinnamate, octocrylene, triclosan, and methyl triclosan in lettuce by ultrasound-assisted extraction combined with solid-phase microextraction followed by gas chromatography with mass spectrometry was developed. Lettuce was directly extracted by ultrasound-assisted extraction with methanol, this extract was combined with water, extracted by solid-phase microextraction in immersion mode, and analyzed by gas chromatography with mass spectrometry. Good linear relationships (25-250 ng/g, R 2  > 0.9702) and low detection limits (1.0-25 ng/g) were obtained for analytes along with acceptable precision for almost all analytes (RSDs < 20%). The validated method was applied for the determination of personal care product ingredients in commercial lettuce and lettuces grown in soil and irrigated with the analytes, identifying the target analytes in leaves and roots of the latter. This procedure is a miniaturized and environmentally friendly proposal which can be a useful tool for quality analysis in lettuce. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Collection-efficient, axisymmetric vacuum sublimation module for the purification of solid materials.

PubMed

May, Michael; Paul, Elizabeth; Katovic, Vladimir

2015-11-01

A vacuum sublimation module of axisymmetric geometry was developed and employed to purify solid-phase materials. The module provides certain practical advantages and it comprises: a metering valve, glass collector, glass lower body, main seal, threaded bushing, and glass internal cartridge (the latter to contain starting material). A complementary process was developed to de-solvate, sublime, weigh, and collect solid chemical materials exemplified by oxalic acid, ferrocene, pentachlorobenzene, chrysene, and urea. The oxalic acid sublimate was analyzed by titration, melting range, Fourier Transform Infrared (FT-IR) Spectroscopy, cyclic voltammetry, and its (aqueous phase) electrolytically generated gas. The analytical data were consistent with a high-purity, anhydrous oxalic acid sublimate. Cyclic voltammograms of 0.11 mol. % oxalic acid in water displayed a 2.1 V window on glassy carbon electrode beyond which electrolytic decomposition occurs. During module testing, fifteen relatively pure materials were sublimed with (energy efficient) passive cooling and the solid-phase recovery averaged 95 mass %. Key module design features include: compact vertical geometry, low-angle conical collector, uniformly compressed main seal, modest power consumption, transparency, glovebox compatibility, cooling options, and preferential conductive heat transfer. To help evaluate the structural (module) heat transfer, vertical temperature profiles along the dynamically evacuated lower body were measured versus electric heater power: for example, an input of 18.6 W generated a temperature 443-K at the bottom. Experimental results and engineering calculations indicate that during sublimation, solid conduction is the primary mode of heat transfer to the starting material.

Sensitive determination of RDX, nitroso-RDX metabolites, and other munitions in ground water by solid-phase extraction and isotope dilution liquid chromatography-atmospheric pressure electro-spray [correction of chemical] ionization mass spectrometry.

PubMed

Cassada, D A; Monson, S J; Snow, D D; Spalding, R F

1999-06-04

Recent improvements in the LC-MS interface have increased the sensitivity and selectivity of this instrument in the analysis of polar and thermally-labile aqueous constituents. Determination of RDX, nitroso-RDX metabolites, and other munitions was enhanced using LC-MS with solid-phase extraction, 15N3-RDX internal standard, and electrospray ionization (ESI) in negative ion mode. ESI produced a five-fold increase in detector response over atmospheric pressure chemical ionization (APCI) for the nitramine compounds, while the more energetic APCI produced more than twenty times the ESI response for nitroaromatics. Method detection limits in ESI for nitramines varied from 0.03 microgram l-1 for MNX to 0.05 microgram l-1 for RDX.

Lasers with intra-cavity phase elements

NASA Astrophysics Data System (ADS)

Gulses, A. Alkan; Kurtz, Russell; Islas, Gabriel; Anisimov, Igor

2018-02-01

Conventional laser resonators yield multimodal output, especially at high powers and short cavity lengths. Since highorder modes exhibit large divergence, it is desirable to suppress them to improve laser quality. Traditionally, such modal discriminations can be achieved by simple apertures that provide absorptive loss for large diameter modes, while allowing the lower orders, such as the fundamental Gaussian, to pass through. However, modal discrimination may not be sufficient for short-cavity lasers, resulting in multimodal operation as well as power loss and overheating in the absorptive part of the aperture. In research to improve laser mode control with minimal energy loss, systematic experiments have been executed using phase-only elements. These were composed of an intra-cavity step function and a diffractive out-coupler made of a computer-generated hologram. The platform was a 15-cm long solid-state laser that employs a neodymium-doped yttrium orthovanadate crystal rod, producing 1064 nm multimodal laser output. The intra-cavity phase elements (PEs) were shown to be highly effective in obtaining beams with reduced M-squared values and increased output powers, yielding improved values of radiance. The utilization of more sophisticated diffractive elements is promising for more difficult laser systems.

Simultaneous analysis of gemfibrozil, morphine, and its two active metabolites in different mouse brain structures using solid-phase extraction with ultra-high performance liquid chromatography and tandem mass spectrometry with a deuterated internal standard.

PubMed

Yang, Zizhao; Wang, Lu; Xu, Mingcheng; Gu, Jingkai; Yu, Lushan; Zeng, Su

2016-06-01

A rapid and sensitive bioassay was established and validated to simultaneously determine gemfibrozil, morphine, morphine-3β-glucuronide, and morphine-6β-glucuronide in mouse cerebrum, epencephalon, and hippocampus based on ultra-high performance liquid chromatography and tandem mass spectrometry. The deuterated internal standard, M6G-d3, was mixed with the prepared samples at 10 ng/mL as the final concentration. The samples were transferred into the C18 solid-phase extraction columns with gradient elution for solid-phase extraction. The mobile phase consisted of methanol and 0.05% formic acid (pH 3.2). Multiple reaction monitoring has been applied to analyze gemfibrozil (m/z 249.0 → 121.0) in anion mode, and M6G-d3 (m/z 465.1 → 289.1), morphine (m/z 286.0 → 200.9), and M3G and M6G (m/z 462.1 → 286.1) in the positive ion mode. The method has a linear calibration range from 0.05 to 10 ng for gemfibrozil, morphine, and M3G and M6G with correlation coefficients >0.993. The lower limit of quantitation for all four analytes was 0.05 ng/mL, relative standard deviation of intra- and interday precision was less than 10.5%, and the relative error of accuracy was from -8.2 to 8.3% at low, medium, and high concentrations for all the analytes. In conclusion, gemfibrozil can influence the morphine antinociception after coronary heart disease induced chronic angina by the change in one of morphine metabolites', M3G, distribution in mouse brain. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Lattice dynamics of solid N2 with an ab initio intermolecular potential

NASA Astrophysics Data System (ADS)

Luty, T.; van der Avoird, A.; Berns, R. M.

1980-11-01

We have performed harmonic and self-consistent phonon lattice dynamics calculations for α and γ N2 crystals using an intermolecular potential from ab initio calculations. This potential contains electrostatic (multipole) interactions, up to all R-9 terms inclusive, anisotropic dispersion interactions up to all R-10 terms inclusive, and anisotropic overlap interactions caused by charge penetration and exchange between the molecules. The lattice constants, cohesion energy, the frequencies of the translational phonon modes and the Grüneisen parameters for the librational modes are in good agreement with experimental values, confirming the quality of the potential. The frequencies of the librational modes and those of the mixed modes are less well reproduced, especially at temperatures near the α-β phase transition. Probably, the self-consistent phonon method used does not fully account for the anharmonicity in the librations.

Determination of free and deconjugated testosterone and epitestosterone in urine using SPME and LC-MS/MS.

PubMed

Zhan, Yanwei; Musteata, Florin M; Basset, Fabien A; Pawliszyn, Janusz

2011-01-01

A thin sheet of polydimethylsilosane membrane was used as an extraction phase for solid-phase microextraction. Compared with fiber or rod solid-phase microextraction geometries, the thin film exhibited much higher extraction capacity without sacrificing extraction time due to its higher area-to-volume ratio. The analytical method involved direct extraction of unconjugated testosterone (T) and epitestosterone (ET) followed by separation on a C18 column and detection by selected reaction monitoring in positive ionization mode. The limit of detection was 1 ng/l for both T and ET. After method validation, free (unconjugated) T and ET were extracted and quantified in real samples. Since T and ET are extensively metabolized, the proposed method was also applied to extract the steroids after enzymatic deconjugation of urinary-excreted steroid glucuronides. The proposed method allows quantification of both conjugated and unconjugated steroids, and revealed that there was a change in the ratio of T to ET after enzymatic deconjugation, indicating different rates of metabolism.

Transition mechanism of sH to filled-ice Ih structure of methane hydrate under fixed pressure condition

NASA Astrophysics Data System (ADS)

Kadobayashi, H.; Hirai, H.; Ohfuji, H.; Kojima, Y.; Ohishi, Y.; Hirao, N.; Ohtake, M.; Yamamoto, Y.

2017-10-01

The phase transition mechanism of methane hydrate from sH to filled-ice Ih structure was examined using a combination of time-resolved X-ray diffractometry (XRD) and Raman spectroscopy in conjunction with charge-coupled device (CCD) camera observation under fixed pressure conditions. Prior to time-resolved Raman experiments, the typical C-H vibration modes and their pressure dependence of three methane hydrate structures, fluid methane and solid methane were measured using Raman spectroscopy to distinguish the phase transitions of methane hydrates from decomposition to solid methane and ice VI or VII. Experimental results by XRD, Raman spectroscopy and CCD camera observation revealed that the structural transition of sH to filled-ice Ih occurs through a collapse of the sH framework followed by the release of fluid methane that is then gradually incorporated into the filled-ice Ih to reconstruct its structure. These observations suggest that the phase transition of sH to filled-ice Ih takes place by a typical reconstructive mechanism.

Preparation of a polymeric ionic liquid-coated solid-phase microextraction fiber by surface radical chain-transfer polymerization with stainless steel wire as support.

PubMed

Feng, Juanjuan; Sun, Min; Xu, Lili; Li, Jubai; Liu, Xia; Jiang, Shengxiang

2011-10-28

Polymeric 1-vinyl-3-octylimidazolium hexafluorophosphate was synthesized in situ on stainless steel wire by surface radical chain-transfer polymerization and used as sensitive coatings in solid-phase microextraction. The outer surface of the stainless steel wire was firstly coated with microstructured silver layer via silver mirror reaction and then functionalized with self-assembled monolayers of 1,8-octanedithiol, which acted as chain transfer agent in the polymerization. Coupled to gas chromatography, extraction performance of the fiber was studied with both headspace and direct-immersion modes using benzene, toluene, ethylbenzene and xylenes (BTEX), phenols and polycyclic aromatic hydrocarbon (PAHs) as model analytes. In combination with the microstructured silver layer, the PIL-coated fiber exhibited high extraction efficiency. Linear ranges for BTEX with headspace mode were in the range of 0.2-1000 μg L(-1) for benzene, and 0.1-1000 μg L(-1) for toluene, ethylbenzene and xylenes. Limits of detection (LODs) were from 0.02 to 0.05 μg L(-1). Wide linear ranges of direct-immersion mode for the extraction of several phenols and PAHs were also obtained with correlation coefficients (R) from 0.9943 to 0.9997. The proposed fiber showed good durability with long lifetime. RSDs of 56 times extraction were still in an acceptable range, from 8.85 to 22.8%. Copyright © 2011 Elsevier B.V. All rights reserved.

Solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for gold determination in geological samples after preconcentration onto carbon nanotubes

NASA Astrophysics Data System (ADS)

Dobrowolski, Ryszard; Mróz, Agnieszka; Dąbrowska, Marzena; Olszański, Piotr

2017-06-01

A novelty method for the determination of gold in geological samples by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry (SS HR CS GF AAS) after solid-phase extraction onto modified carbon nanotubes (CNT) was described. The methodology developed is based on solid phase extraction of Au(III) ions from digested samples to eliminate strong interference caused by iron compounds and problems related to inhomogeneities of the samples. The use of aqueous or solid standard for calibration was studied and the slope of calibration curve was the same for both of these modes. This statement indicates the possibility to perform the calibration of the method using aqueous standard solutions. Under optimum conditions the absolute detection limit for gold was equal to 2.24 · 10- 6 μg g- 1 while the adsorption capacity of modified carbon nanotubes was 264 mg g- 1. The proposed procedure was validated by the application of certified reference materials (CRMs) with different content of gold and different matrix, the results were in good agreement with certified values. The method was successfully applied for separation and determination of gold ions in complex geological samples, with precision generally better than 8%.

Design and physicochemical characterization of advanced spray-dried tacrolimus multifunctional particles for inhalation

PubMed Central

Wu, Xiao; Hayes, Don; Zwischenberger, Joseph B; Kuhn, Robert J; Mansour, Heidi M

2013-01-01

The aim of this study was to design, develop, and optimize respirable tacrolimus microparticles and nanoparticles and multifunctional tacrolimus lung surfactant mimic particles for targeted dry powder inhalation delivery as a pulmonary nanomedicine. Particles were rationally designed and produced at different pump rates by advanced spray-drying particle engineering design from organic solution in closed mode. In addition, multifunctional tacrolimus lung surfactant mimic dry powder particles were prepared by co-dissolving tacrolimus and lung surfactant mimic phospholipids in methanol, followed by advanced co-spray-drying particle engineering design technology in closed mode. The lung surfactant mimic phospholipids were 1,2-dipalmitoyl-sn-glycero-3-phosphocholine and 1,2-dipalmitoyl-sn-glycero-3-[phosphor-rac-1-glycerol]. Laser diffraction particle sizing indicated that the particle size distributions were suitable for pulmonary delivery, whereas scanning electron microscopy imaging indicated that these particles had both optimal particle morphology and surface morphology. Increasing the pump rate percent of tacrolimus solution resulted in a larger particle size. X-ray powder diffraction patterns and differential scanning calorimetry thermograms indicated that spray drying produced particles with higher amounts of amorphous phase. X-ray powder diffraction and differential scanning calorimetry also confirmed the preservation of the phospholipid bilayer structure in the solid state for all engineered respirable particles. Furthermore, it was observed in hot-stage micrographs that raw tacrolimus displayed a liquid crystal transition following the main phase transition, which is consistent with its interfacial properties. Water vapor uptake and lyotropic phase transitions in the solid state at varying levels of relative humidity were determined by gravimetric vapor sorption technique. Water content in the various powders was very low and well within the levels necessary for dry powder inhalation, as quantified by Karl Fisher coulometric titration. Conclusively, advanced spray-drying particle engineering design from organic solution in closed mode was successfully used to design and optimize solid-state particles in the respirable size range necessary for targeted pulmonary delivery, particularly for the deep lung. These particles were dry, stable, and had optimal properties for dry powder inhalation as a novel pulmonary nanomedicine. PMID:23403805

Correlation between the ripple phase and stripe domains in membranes.

PubMed

Bernchou, Uffe; Midtiby, Henrik; Ipsen, John Hjort; Simonsen, Adam Cohen

2011-12-01

We investigate the relationship between stripe domains and the ripple phase in membranes. These have previously been observed separately without being linked explicitly. Past results have demonstrated that solid and ripple phases exhibit rich textural patterns related to the orientational order of tilted lipids and the orientation of ripple corrugations. Here we reveal a highly complex network pattern of ripple and solid domains in DLPC, DPPC bilayers with structures covering length scales from 10 nm to 100 μm. Using spincoated double supported membranes we investigate domains by correlated AFM and fluorescence microscopy. Cooling experiments demonstrate the mode of nucleation and growth of stripe domains enriched in the fluorescent probe. Concurrent AFM imaging reveals that these stripe domains have a one-to-one correspondence with a rippled morphology running parallel to the stripe direction. Both thin and thick stripe domains are observed having ripple periods of 13.5±0.2 nm and 27.4±0.6 nm respectively. These are equivalent to previously observed asymmetric/equilibrium and symmetric/metastable ripple phases, respectively. Thin stripes grow from small solid domains and grow predominantly in length with a speed of ~3 times that of the thick stripes. Thick stripes grow by templating on the sides of thinner stripes or can emerge directly from the fluid phase. Bending and branching angles of stripes are in accordance with an underlying six fold lattice. We discuss mechanisms for the nucleation and growth of ripples and discuss a generic phase diagram that may partly rationalize the coexistence of metastable and stable phases. Copyright © 2011 Elsevier B.V. All rights reserved.

Ultrafast vibrational dynamics of BH{sub 4}{sup −} ions in liquid and crystalline environments

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

Tyborski, Tobias, E-mail: tyborski@mbi-berlin.de; Costard, Rene; Woerner, Michael

2014-07-21

Ultrafast vibrational dynamics of BH{sub 4}{sup −} ions, the key units in boron hydride materials for hydrogen storage, are studied in diluted polar liquid solution and in NaBH{sub 4} crystallites by femtosecond infrared spectroscopy. Two-color pump-probe experiments reveal v = 1 lifetimes of 3 ps for the asymmetric BH{sub 4}{sup −} stretching mode ν{sub 3} and of 3.6 ps for the asymmetric bending mode ν{sub 4} in the solvent isopropylamine. We provide direct evidence for the BH{sub 4}{sup −} stretching relaxation pathway via the asymmetric bending mode ν{sub 4} by probing the latter after femtosecond excitation of ν{sub 3}. Pump-probemore » traces measured in the crystalline phase show signatures of radiative coupling between the densely packed BH{sub 4}{sup −} oscillators, most clearly manifested in an accelerated subpicosecond depopulation of the v = 1 state of the ν{sub 4} mode. The radiative decay is followed by incoherent vibrational relaxation similar to the liquid phase. The excess energy released in the relaxation processes of the BH{sub 4}{sup −} intramolecular modes is transferred into the environment with thermal pump-probe signals being much more pronounced in the dense solid than in the diluted solution.« less

Development of an in-house mixed-mode solid-phase extraction for the determination of 16 basic drugs in urine by High Performance Liquid Chromatography-Ion Trap Mass Spectrometry.

PubMed

Musile, Giacomo; Cenci, Lucia; Piletska, Elena; Gottardo, Rossella; Bossi, Alessandra M; Bortolotti, Federica

2018-07-27

The aim of the present work was to develop a novel in-house mixed-mode SPE sorbent to be used for the HPLC-Ion TrapMS determination of 16 basic drugs in urine. By using a computational modelling, a virtual monomer library was screened identifying three suitable functional monomers, methacrylic acid (MAA), itaconic acid (IA) and 2-acrylamide-2-methylpropane sulfonic acid (AMPSA), respectively. Three different sorbents were then synthetized based on these monomers, and using as cross-linker trimethylolpropane trimethacrylate (TMPTMA). The sorbent characterization analyses brought to the selection of the AMPSA based phase. Using this novel in-house sorbent, a SPE-HPLC-Ion TrapMS method for drug analysis in urine was validated proving to be selective and accurate and showing a sensitivity adequate for toxicological urine analysis. The comparison of the in-house mixed-mode SPE sorbent with two analogous commercial mixed-mode SPE phases showed that the first one was better not only in terms of process efficiency, but also in terms of quality-price rate. To the best of our knowledge, this is the first time in which an in-house SPE procedure has been applied to the toxicological analysis of a complex matrix, such as urine. Copyright © 2018 Elsevier B.V. All rights reserved.

FFT analysis of sensible-heat solar-dynamic receivers

NASA Astrophysics Data System (ADS)

Lund, Kurt O.

The use of solar dynamic receivers with sensible energy storage in single-phase materials is considered. The feasibility of single-phase designs with weight and thermal performance comparable to existing two-phase designs is addressed. Linearized heat transfer equations are formulated for the receiver heat storage, representing the periodic input solar flux as the sum of steady and oscillating distributions. The steady component is solved analytically to produce the desired receiver steady outlet gas temperature, and the FFT algorithm is applied to the oscillating components to obtain the amplitudes and mode shapes of the oscillating solid and gas temperatures. The results indicate that sensible-heat receiver designs with performance comparable to state-of-the-art two-phase receivers are available.

Effect of multiphase radiation on coal combustion in a pulverized coal jet flame

NASA Astrophysics Data System (ADS)

Wu, Bifen; Roy, Somesh P.; Zhao, Xinyu; Modest, Michael F.

2017-08-01

The accurate modeling of coal combustion requires detailed radiative heat transfer models for both gaseous combustion products and solid coal particles. A multiphase Monte Carlo ray tracing (MCRT) radiation solver is developed in this work to simulate a laboratory-scale pulverized coal flame. The MCRT solver considers radiative interactions between coal particles and three major combustion products (CO2, H2O, and CO). A line-by-line spectral database for the gas phase and a size-dependent nongray correlation for the solid phase are employed to account for the nongray effects. The flame structure is significantly altered by considering nongray radiation and the lift-off height of the flame increases by approximately 35%, compared to the simulation without radiation. Radiation is also found to affect the evolution of coal particles considerably as it takes over as the dominant mode of heat transfer for medium-to-large coal particles downstream of the flame. To investigate the respective effects of spectral models for the gas and solid phases, a Planck-mean-based gray gas model and a size-independent gray particle model are applied in a frozen-field analysis of a steady-state snapshot of the flame. The gray gas approximation considerably underestimates the radiative source terms for both the gas phase and the solid phase. The gray coal approximation also leads to under-prediction of the particle emission and absorption. However, the level of under-prediction is not as significant as that resulting from the employment of the gray gas model. Finally, the effect of the spectral property of ash on radiation is also investigated and found to be insignificant for the present target flame.

Determination of Scopolamine in Human Saliva Using Solid Phase Extraction and LC/MS/MS

NASA Technical Reports Server (NTRS)

Wang, Zuwei; Vaksman, Zalman; Boyd, Jason; Putcha, Lakshmi

2007-01-01

Purpose: Scopolamine is the preferred treatment for motion sickness during space flight because of its quick onset of action, short half-life and favorable side-effect profile. The dose administered depends on the mode of administration and usually ranges between 0.1 and 0.8 mg. Such small doses make it difficult to detect concentrations of scopolamine in biological fluids by using conventional HPLC methods. To measure scopolamine in saliva and thereby to evaluate the pharmacokinetics of scopolamine, we developed an LC/MS/MS method using off-line solid phase extraction. Method: Samples (0.5mL) were loaded onto Waters Oasis HLB co-polymer cartridges (10 mg, 1 mL) and eluted with 0.5 mL methanol without evaporation and reconstitution. HPLC separation of the eluted sample was performed using an Agilent Zorbax SB-CN column (50 x 2.1 mm) at a flow rate of 0.2 mL/min for 4 minutes. The mobile phase for separation was 90:10 (v/v) methanol: ammonium acetate (2 mM) in water, pH 5.0 +/- 0.1. Concentrations of scopolamine were determined using a Micromass Quattro Micro(TM) mass spectrometer with electrospray ionization (ESI). ESI mass spectra were acquired in positive ion mode with multiple reaction monitoring for the determination of scopolamine m/z = 304.2 yields 138.1 and internal standard (IS) hyoscyamine m/z = 290.2 yields 124.1. Results: The method is rapid, reproducible, specific and has the following parameters: scopolamine and the IS are eluted at 1.7 and 3.2 min respectively. The linear range is 50-5000 pg/mL for scopolamine in saliva with correlation coefficients > 0.99 with a CV < 0.5 %. The intra-day and inter-day CVs are < 15 % for quality control samples with concentrations of 75, 300, 750 and 3000 pg/mL of scopolamine in human saliva. Conclusion: Solid phase extraction allows more rapid sample preparation and greater precision than liquid extraction. Furthermore, we increased the sensitivity and specificity by adjusting the LC mobile phase and using an MS/MS detector.

[Simultaneous determination of sixteen perfluorinated organic compounds in surface water by solid phase extraction and ultra performance liquid chromatography with electrospray ionization tandem mass spectrometry].

PubMed

Zhang, Ming; Tang, Fangliang; Yu, Yayun; Chen, Feng; Xu, Jianfen; Ye, Yonggen

2014-05-01

A high-throughput detection method has been developed for the determination of sixteen perfluorinated organic compounds (PFCs) in surface water by solid phase extraction-ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (SPE-UPLC-ESI-MS/MS). The water samples were concentrated and purified through WAX solid phase extraction cartridges. The UPLC separation was performed on an ACQUITY UPLC BEH C18 column utilizing a gradient elution program of methanol (containing 2 mmol/L ammonium acetate) and water (containing 2 mmol/L ammonium acetate) as the mobile phases at a flow rate of 0.4 mL/min. The MS/MS detection was performed under negative electrospray ionization ( ESI ) in multiple reaction monitoring (MRM) mode. Good linearities were observed in the range of 0.5-100 gg/L or 1.0 - 100 microg/L with correlation coefficients from 0.998 7 to 0.999 9. The limits of detection (LODs) for the sixteen perfluorinated organic compounds were in the range of 0.06-0.46 ng/L. The recoveries ranged from 67.6% to 103% with the relative standard deviations between 2.94% and 12.0%. This method was characterized by high sensitivity and precision, extensive range and high speed, and can be applied for the analysis of PFC contaminants in surface water.

[Simultaneous determination of nine perfluorinated compound precursors in atmospheric precipitation by solid phase extraction and ultra performance liquid chromatography with tandem mass spectrometry].

PubMed

Zhang, Ming; Tang, Fangliang; Xu, Jianfen; Yu, Bo; Zhang, Wei; Yao, Jianliang; Hu, Minhua

2017-10-08

A high-throughput detection method has been developed for the determination of nine perfluorinated compound precursors (PFCPs) in atmospheric precipitation by solid phase extraction-ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (SPE-UPLC-ESI-MS/MS). The atmospheric precipitation samples were concentrated and purified with HLB solid phase extraction cartridges. The UPLC separation was performed on an HSS T 3 column (100 mm×2.1 mm, 1.7 μm) utilizing a gradient elution program of methanol and water as the mobile phases at a flow rate of 0.2 mL/min. The MS/MS detection was performed under negative electrospray ionization (ESI - ) in multiple reaction monitoring (MRM) mode. Good linearity was observed in the range of 0.05-5.00 μg/L, 0.50-50.0 μg/L or 5.00-500 μg/L with correlation coefficients from 0.9921 to 0.9995. The limits of detection (LODs) for the nine perfluorinated compound precursors were in the ranges of 0.05-7.9 ng/L. The recoveries ranged from 76.0% to 106% with the relative standard deviations between 0.72% and 13.7%. This method is characterized by high sensitivity and precision, extensive analytical range and quick analytical rate, and can be applied for the analysis of perfluorinated compound precursors in atmospheric precipitation.

Systematic Assessment of Seven Solvent and Solid-Phase Extraction Methods for Metabolomics Analysis of Human Plasma by LC-MS

NASA Astrophysics Data System (ADS)

Sitnikov, Dmitri G.; Monnin, Cian S.; Vuckovic, Dajana

2016-12-01

The comparison of extraction methods for global metabolomics is usually executed in biofluids only and focuses on metabolite coverage and method repeatability. This limits our detailed understanding of extraction parameters such as recovery and matrix effects and prevents side-by-side comparison of different sample preparation strategies. To address this gap in knowledge, seven solvent-based and solid-phase extraction methods were systematically evaluated using standard analytes spiked into both buffer and human plasma. We compared recovery, coverage, repeatability, matrix effects, selectivity and orthogonality of all methods tested for non-lipid metabolome in combination with reversed-phased and mixed-mode liquid chromatography mass spectrometry analysis (LC-MS). Our results confirmed wide selectivity and excellent precision of solvent precipitations, but revealed their high susceptibility to matrix effects. The use of all seven methods showed high overlap and redundancy which resulted in metabolite coverage increases of 34-80% depending on LC-MS method employed as compared to the best single extraction protocol (methanol/ethanol precipitation) despite 7x increase in MS analysis time and sample consumption. The most orthogonal methods to methanol-based precipitation were ion-exchange solid-phase extraction and liquid-liquid extraction using methyl-tertbutyl ether. Our results help facilitate rational design and selection of sample preparation methods and internal standards for global metabolomics.

Systematic Assessment of Seven Solvent and Solid-Phase Extraction Methods for Metabolomics Analysis of Human Plasma by LC-MS

PubMed Central

Sitnikov, Dmitri G.; Monnin, Cian S.; Vuckovic, Dajana

2016-01-01

The comparison of extraction methods for global metabolomics is usually executed in biofluids only and focuses on metabolite coverage and method repeatability. This limits our detailed understanding of extraction parameters such as recovery and matrix effects and prevents side-by-side comparison of different sample preparation strategies. To address this gap in knowledge, seven solvent-based and solid-phase extraction methods were systematically evaluated using standard analytes spiked into both buffer and human plasma. We compared recovery, coverage, repeatability, matrix effects, selectivity and orthogonality of all methods tested for non-lipid metabolome in combination with reversed-phased and mixed-mode liquid chromatography mass spectrometry analysis (LC-MS). Our results confirmed wide selectivity and excellent precision of solvent precipitations, but revealed their high susceptibility to matrix effects. The use of all seven methods showed high overlap and redundancy which resulted in metabolite coverage increases of 34–80% depending on LC-MS method employed as compared to the best single extraction protocol (methanol/ethanol precipitation) despite 7x increase in MS analysis time and sample consumption. The most orthogonal methods to methanol-based precipitation were ion-exchange solid-phase extraction and liquid-liquid extraction using methyl-tertbutyl ether. Our results help facilitate rational design and selection of sample preparation methods and internal standards for global metabolomics. PMID:28000704

[Determination of deoxynivalenol in grain and its products by solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry].

PubMed

Huang, Juan; Chen, Guosong; Zhang, Xiaoyan; Shen, Chongyu; Lü, Chen; Wu, Bin; Liu, Yan; Chen, Huilan; Ding, Tao

2012-11-01

A method was established for the determination of deoxynivalenol (vomitoxin) in grain and its products based on solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was firstly extracted by acetonitrile-water (84:16, v/v). The extract was then cleaned-up by an HLB solid phase extraction cartridge. The separation was carried out on a Phenomenex Kinetex C18 column (100 mm x4. 6 mm, 2.6 microm) with a gradient elution using 0.3% per hundred ammonia solution-acetonitrile as mobile phases. The analysis of deoxynivalenol was performed under electrospray negative ionization mode. The limit of detection (LOD, S/N= 3) and the limit of quantification (LOQ, S/N = 10) were 20 microg/kg and 50 microg/kg, respectively. A good linearity (r > 0.99) was achieved for the target compound over the range of 20-1000 pg/L. The recoveries at the three spiked levels (50, 100, 500 microg/kg) in the blank matrices such as flour, barley, soybean, rice, cornmeal, cassava and wheat, were varied from 75.6% to 111.0% with the relative standard deviations no more than 13. 0%. The method is accurate, efficient, sensitive and practical. The cost of pretreatment is obviously reduced by replacing immunoaffinity columns and Mycosep columns with HLB columns which have the same purification effect.

A complete assignment of the vibrational spectra of 2-furoic acid based on the structures of the more stable monomer and dimer

NASA Astrophysics Data System (ADS)

Ghalla, Houcine; Issaoui, Noureddine; Castillo, María Victoria; Brandán, Silvia Antonia; Flakus, Henryk T.

2014-03-01

The structural and vibrational properties of cyclic dimer of 2-furoic acid (2FA) were predicted by combining the available experimental infrared and Raman spectra in the solid phase and ab initio calculations based on density functional theory (DFT) with Pople's basis sets. The calculations show that there are two cyclic dimers for the title molecule that have been theoretically determined in the gas phase, and that only one of them, cis conformer, is present in the solid phase. The complete assignment of the 66 normal vibrational modes for the cis cyclic dimer was performed using the Pulay's Scaled Quantum Mechanics Force Field (SQMFF) methodology. Four strong bands in the infrared spectrum at 1583, 1427, 1126 and 887 cm-1 and the group of bands in the Raman spectrum at 1464, 1452, 1147, 1030, 885, 873, 848, 715 and 590 cm-1 are characteristic of the dimeric form of 2FA in the solid phase. In this work, the calculated structural and vibrational properties of both dimeric species were analyzed and compared between them. In addition, three types of atomic charges, bond orders, possible charge transfer, topological properties of the furan rings, Natural Bond Orbital (NBO) and Atoms in Molecules (AIM) theory calculations were employed to study the stabilities and intermolecular interactions of the both dimers of 2FA.

Rapid and sensitive determination of major polyphenolic components in Euphoria longana Lam. seeds using matrix solid-phase dispersion extraction and UHPLC with hybrid linear ion trap triple quadrupole mass spectrometry.

PubMed

Rathore, Atul S; Sathiyanarayanan, L; Deshpande, Shreekant; Mahadik, Kakasaheb R

2016-11-01

A rapid and sensitive method for the extraction and determination of four major polyphenolic components in Euphoria longana Lam. seeds is presented for the first time based on matrix solid-phase dispersion extraction followed by ultra high performance liquid chromatography with hybrid triple quadrupole linear ion trap mass spectrometry. Matrix solid-phase dispersion method was designed for the extraction of Euphoria longana seed constituents and compared with microwave-assisted extraction and ultrasonic-assisted extraction methods. An Ultra high performance liquid chromatography with hybrid triple quadrupole linear ion-trap mass spectrometry method was developed for quantitative analysis in multiple-reaction monitoring mode in negative electrospray ionization. The chromatographic separation was accomplished using an ACQUITY UPLC BEH C 18 (2.1 mm × 50 mm, 1.7 μm) column with gradient elution of 0.1% aqueous formic acid and 0.1% formic acid in acetonitrile. The developed method was validated with acceptable linearity (r 2 > 0.999), precision (RSD ≤ 2.22%) and recovery (RSD ≤ 2.35%). The results indicated that matrix solid-phase dispersion produced comparable extraction efficiency compared with other methods nevertheless was more convenient and time-saving with reduced requirements on sample and solvent volumes. The proposed method is rapid and sensitive in providing a promising alternative for extraction and comprehensive determination of active components for quality control of Euphoria longana products. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Coupling solid-phase microextraction and high-performance liquid chromatography for direct and sensitive determination of halogenated fungicides in wine.

PubMed

Millán, S; Sampedro, M C; Unceta, N; Goicolea, M A; Rodríguez, E; Barrio, R J

2003-05-02

A solid-phase microextraction (SPME) method coupled to high-performance liquid chromatography with diode array detection (HPLC-DAD) for the analysis of six organochlorine fungicides (nuarimol, triadimenol, triadimefon, folpet, vinclozolin and penconazole) in wine was developed. For this purpose, polydimethylsiloxane-divinylbenzene-coated fibers were utilized and all factors affecting throughput, precision, and accuracy of the SPME method were investigated and optimized. These factors include: matrix influence, extraction and desorption time, percentage of ethanol, pH, salt effect and desorption mode. The performed analytical procedure showed detectability ranging from 4 to 27 microg l(-1) and precision from 2.4 to 14.2% (as intra-day relative standard deviation, RSD) and 4.7-25.7% (as inter-day RSD) depending on the fungicide. The results demonstrate the suitability of the SPME-HPLC-DAD method to analyze these organochlorine fungicides in red wine.

Determination of cocaine, benzoylecgonine and cocaethylene in human hair by solid-phase microextraction and gas chromatography-mass spectrometry.

PubMed

de Toledo, Fernanda Crossi Pereira; Yonamine, Mauricio; de Moraes Moreau, Regina Lucia; Silva, Ovandir Alves

2003-12-25

The present work describes a highly precise and sensitive method developed to detect cocaine (COC), benzoylecgonine (BE, its main metabolite) and cocaethylene (CE, transesterification product of the coingestion of COC with ethanol) in human head hair samples. The method was based on an alkylchloroformate derivatization of benzoylecgonine and the extraction of the analytes by solid-phase microextraction (SPME). Gas chromatography-mass spectrometry (GC-MS) was used to identify and quantify the analytes in selected ion monitoring mode (SIM). The limits of quantification and detection (LOQ and LOD) were: 0.1 ng/mg for COC and CE, and 0.5 ng/mg for BE. Good inter- and intra-assay precision was observed. The dynamic range of the assay was 0.1-50 ng/mg. The method is not time consuming and was shown to be easy to perform.

Triggering of longitudinal combustion instabilities in solid rocket motors: Nonlinear combustion response

NASA Technical Reports Server (NTRS)

Wicker, J. M.; Greene, W. D.; Kim, S. I.; Yang, V.

1995-01-01

Pulsed oscillations in solid rocket motors are investigated with emphasis on nonlinear combustion response. The study employs a wave equation governing the unsteady motions in a two-phase flow, and a solution technique based on spatial- and time-averaging. A wide class of combustion response functions is studied to second-order in fluctuation amplitude to determine if, when, and how triggered instabilities arise. Conditions for triggering are derived from analysis of limit cycles, and regions of triggering are found in parametric space. Based on the behavior of model dynamical systems, introduction of linear cross-coupling and quadratic self-coupling among the acoustic modes appears to be the manner in which the nonlinear combustion response produces triggering to a stable limit cycle. Regions of initial conditions corresponding to stable pulses were found, suggesting that stability depends on initial phase angle and harmonic content, as well as the composite amplitude, of the pulse.

Method development for the analysis of 1,4-dioxane in drinking water using solid-phase extraction and gas chromatography-mass spectrometry.

PubMed

Grimmett, Paul E; Munch, Jean W

2009-01-01

1,4-Dioxane has been identified as a probable human carcinogen and an emerging contaminant in drinking water. The United States Environmental Protection Agency's (U.S. EPA) National Exposure Research Laboratory (NERL) has developed a method for the analysis of 1,4-dioxane in drinking water at ng/L concentrations. The method consists of an activated carbon solid-phase extraction of 500-mL or 100-mL water samples using dichloromethane as the elution solvent. The extracts are analyzed by gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode. In the NERL laboratory, recovery of 1,4-dioxane ranged from 94-110% in fortified laboratory reagent water and recoveries of 96-102% were demonstrated for fortified drinking water samples. The relative standard deviations for replicate analyses were less than 6% at concentrations exceeding the minimum reporting level.

Pressure-induced polymerization of P(CN) 3

DOE PAGES

Gou, Huiyang; Yonke, Brendan L.; Epshteyn, Albert; ...

2015-05-21

Motivated to explore the formation of novel extended carbon-nitrogen solids via well-defined molecular precursor pathways, we studied the chemical reactivity of highly pure phosphorous tricyanide, P(CN) 3, under conditions of high pressure at room temperature. Raman and infrared (IR) spectroscopic measurements reveal a series of phase transformations below 10 GPa, and several low-frequency vibrational modes are reported for the first time. Synchrotron powder Xray diffraction (PXRD) measurements taken during compression show that molecular P(CN) 3 is highly compressible with a bulk modulus of 10.0±0.3 GPa and polymerizes into an amorphous solid above ~10.0 GPa. Raman and infrared (IR) spectra, togethermore » with first-principles molecular-dynamics simulations, show that the amorphization transition is associated with polymerization of the cyanide groups into CN bonds with predominantly sp 2 character, similar to known carbon nitrides, resulting in a novel PCN polymeric phase, which is recoverable to ambient pressure.« less

Two-dimensional fluid-filled closed-cell cellular solid as an acoustic metamaterial with negative index

NASA Astrophysics Data System (ADS)

Dorodnitsyn, V.; Van Damme, B.

2016-04-01

A concept for acoustic metamaterials consisting of a cellular medium with fluid-filled cells is fabricated and studied experimentally. In such a system, the fluid and solid structure explicitly interact, and elastic wave propagation is coupled to both phases. Focusing here on shear wave behavior, we confirm previous numerical studies in three steps. We first measure the material deformations pertaining to three qualitatively different shear wave modes in the frequency range below 3.5 kHz. We then measure the group velocity and demonstrate that, within a certain frequency interval, the group and phase velocity have opposite signs. This shows that the system acts as a negative-index metamaterial. Finally, we confirm the presence of band gaps due to the locally resonant behavior of the cell walls. The demonstrated concept of a closed, fluid-filled cellular material as an acoustic metamaterial opens a wide space for applications.

[Simultaneous determination of ten benzotriazole ultraviolet stabilizers in food contact plastic materials by solid phase extraction and ultra performance liquid chromatography with tandem mass spectrometry].

PubMed

Gou, Xinlei; Zhao, Xinying; Chi, Haitao; Gao, Xia; Zhou, Mingqiang; Liu, Weili

2015-06-01

A sensitive method was developed for the simultaneous determination of ten benzotriazole ultraviolet stabilizers in food contact plastic materials by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample was extracted by methanol-dichloromethane, and purified by a C18 solid-phase extraction (SPE) column. The separation was performed by using water containing 0. 1% (v/v) formic acid and methanol as the mobile phases with gradient elution at a flow rate of 0. 3 mL/min. The electrospray ionization (ESI) source in positive ion mode was used for the analysis of the ten benzotriazole ultraviolet stabilizers in multiple reaction monitoring (MRM) mode. The results showed that the standard curves were obtained with good correlation coefficients (r2 > 0.996) in their linear concentration ranges. The limits of detection (LODs, S/N = 3) for the ten benzotriazole ultraviolet stabilizers were in the range of 0.6-1.6 µg/kg. The mean recoveries for the ten benzotriazole ultraviolet stabilizers at three spiked levels (low, medium and high) were 75.2%-85.3% with relative standard deviations of 1.0%-5.7%. Ten kinds of food contact plastic materials were tested, and 2,2'-methylenebis (6-(benzotriazol-2-yl)-4-tert-octylphenol) (UV-360) was found in a sample of polyethylene (PE) material. The method is accurate, simple, rapid and feasible for the simultaneous determination of benzotriazole ultraviolet stabilizers in food plastic materials.

Determination of solid-liquid partition coefficients (Kd) for the herbicides isoproturon and trifluralin in five UK agricultural soils.

PubMed

Cooke, Cindy M; Shaw, George; Collins, Chris D

2004-12-01

Isoproturon and trifluralin are herbicides of contrasting chemical characters and modes of action. Standard batch sorption procedures were carried out to investigate the individual sorption behaviour of 14C-isoproturon and 14C-trifluralin in five agricultural soils (1.8-4.2% OC), and the soil solid-liquid partition coefficients (Kd values) were determined. Trifluralin exhibited strong partitioning to the soil solid phase (Kd range 106-294) and low desorption potential, thus should not pose a threat to sensitive waters via leaching, although particle erosion and preferential flow pathways may facilitate transport. For isoproturon, soil adsorption was low (Kd range 1.96-5.75) and desorption was high, suggesting a high leaching potential, consistent with isoproturon being the most frequently found pesticide in UK surface waters. Soil partitioning was directly related to soil organic carbon (OC) content. Accumulation isotherms were modelled using a dual-phase adsorption model to estimate adsorption and desorption rate coefficients. Associations between herbicides and soil humic substances were also shown using gel filtration chromatography.

Some experiments related to L-star instability in rocket motors

NASA Technical Reports Server (NTRS)

Kumar, R. N.; Mcnamara, R. P.

1973-01-01

The role of solid phase heterogeneity on the low-pressure L-star instability of nonmetallized AP/PBAN propellants is explored. Four particle size distributions are employed in propellants that are otherwise identical. Over one hundred test firings were conducted in the 21/2 in. diameter L-star burner. Pressure time histories in the chamber and color movies of two firings constitute the raw data. An economical firing program was used which enables the interesting range of L-star values to be covered during a single firing (at a set mean pressure), through the variations in the depleting propellant volume. Time-independent combustion, Helmholtz mode, chuff mode, and the pressure-burst phenomena are revealed as the principal signatures. Of these, the Helmholtz mode is found to be the most ordered form of instability.

Validated Method for the Quantification of Baclofen in Human Plasma Using Solid-Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry.

PubMed

Nahar, Limon Khatun; Cordero, Rosa Elena; Nutt, David; Lingford-Hughes, Anne; Turton, Samuel; Durant, Claire; Wilson, Sue; Paterson, Sue

2016-03-01

A highly sensitive and fully validated method was developed for the quantification of baclofen in human plasma. After adjusting the pH of the plasma samples using a phosphate buffer solution (pH 4), baclofen was purified using mixed mode (C8/cation exchange) solid-phase extraction (SPE) cartridges. Endogenous water-soluble compounds and lipids were removed from the cartridges before the samples were eluted and concentrated. The samples were analyzed using triple-quadrupole liquid chromatography-tandem mass spectrometry (LC-MS-MS) with triggered dynamic multiple reaction monitoring mode for simultaneous quantification and confirmation. The assay was linear from 25 to 1,000 ng/mL (r(2) > 0.999; n = 6). Intraday (n = 6) and interday (n = 15) imprecisions (% relative standard deviation) were <5%, and the average recovery was 30%. The limit of detection of the method was 5 ng/mL, and the limit of quantification was 25 ng/mL. Plasma samples from healthy male volunteers (n = 9, median age: 22) given two single oral doses of baclofen (10 and 60 mg) on nonconsecutive days were analyzed to demonstrate method applicability. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Small-scale collisions with big-scale effects: Direct numerical simulations of crystal interactions in dense suspensions and ramifications for magmatic differentiation

NASA Astrophysics Data System (ADS)

Sethian, J.; Suckale, J.; Yu, J.; Elkins-Tanton, L. T.

2011-12-01

Numerous problems in the Earth sciences involve the dynamic interaction between solid bodies and viscous flow. The goal of this contribution is to develop and validate a computational methodology for modeling complex solid-fluid interactions with minimal simplifying assumptions. The approach we develop is general enough to be applicable in a wide range of geophysical systems ranging from crystal-bearing lava flows to sediment-rich rivers and aerosol transport. Our algorithm relies on a two-step projection scheme: In the first step, we solve the multiple-phase Navier-Stokes or Stokes equation, respectively, in both domains. In the second step, we project the velocity field in the solid domain onto a rigid-body motion by enforcing that the deformation tensor in the respective domain is zero. An important component of the numerical scheme is the accurate treatment of collisions between an arbitrary number of suspended solid bodies based on the impact Stokes number and the elasticity parameters of the solid phase. We perform several benchmark computations to validate our computations including wake formation behind fixed and mobile cylinders and cuboids, the settling speed of particles, and laboratory experiments of collision modes. Finally, we apply our method to investigate the competing effect of entrainment and fractionation in crystalline suspensions - an important question in the context of magma differentiation processes in magma chambers and magma oceans. We find that the properties and volume fraction of the crystalline phase play an important role for evaluating differentiation efficiency.

Confining standing waves in optical corrals.

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

Babayan, Y.; McMahon, J. M.; Li, S.

2009-03-01

Near-field scanning optical microscopy images of solid wall, circular, and elliptical microscale corrals show standing wave patterns confined inside the structures with a wavelength close to that of the incident light. The patterns inside the corrals can be tuned by changing the size and material of the walls, the wavelength of incident light, and polarization direction for elliptical corrals. Finite-difference time-domain calculations of the corral structures agree with the experimental observations and reveal that the electric and magnetic field intensities are out of phase inside the corral. A theoretical modal analysis indicates that the fields inside the corrals can bemore » attributed to p- and s-polarized waveguide modes, and that the superposition of the propagating and evanescent modes can explain the phase differences between the fields. These experimental and theoretical results demonstrate that electromagnetic fields on a dielectric surface can be controlled in a predictable manner.« less

Enhancing radiation tolerance by controlling defect mobility and migration pathways in multicomponent single-phase alloys

NASA Astrophysics Data System (ADS)

Lu, Chenyang; Niu, Liangliang; Chen, Nanjun; Jin, Ke; Yang, Taini; Xiu, Pengyuan; Zhang, Yanwen; Gao, Fei; Bei, Hongbin; Shi, Shi; He, Mo-Rigen; Robertson, Ian M.; Weber, William J.; Wang, Lumin

2016-12-01

A grand challenge in material science is to understand the correlation between intrinsic properties and defect dynamics. Radiation tolerant materials are in great demand for safe operation and advancement of nuclear and aerospace systems. Unlike traditional approaches that rely on microstructural and nanoscale features to mitigate radiation damage, this study demonstrates enhancement of radiation tolerance with the suppression of void formation by two orders magnitude at elevated temperatures in equiatomic single-phase concentrated solid solution alloys, and more importantly, reveals its controlling mechanism through a detailed analysis of the depth distribution of defect clusters and an atomistic computer simulation. The enhanced swelling resistance is attributed to the tailored interstitial defect cluster motion in the alloys from a long-range one-dimensional mode to a short-range three-dimensional mode, which leads to enhanced point defect recombination. The results suggest design criteria for next generation radiation tolerant structural alloys.

Advanced Orion Optimized Laser System Analysis

NASA Technical Reports Server (NTRS)

1996-01-01

Contractor shall perform a complete analysis of the potential of the solid state laser in the very long pulse mode (100 ns pulse width, 10-30 hz rep-rate) and in the very short pulse mode (100 ps pulse width 10-30 hz rep rate) concentrating on the operation of the device in the 'hot-rod' mode, where no active cooling the laser operation is attempted. Contractor's calculations shall be made of the phase aberrations which develop during the repped-pulse train, and the results shall feed into the adaptive optics analyses. The contractor shall devise solutions to work around ORION track issues. A final report shall be furnished to the MSFC COTR including all calculations and analysis of estimates of bulk phase and intensity aberration distribution in the laser output beam as a function of time during the repped-pulse train for both wave forms (high-energy/long-pulse, as well as low-energy/short-pulse). Recommendations shall be made for mitigating the aberrations by laser re-design and/or changes in operating parameters of optical pump sources and/or designs.

Therapeutic drug monitoring of seven psychotropic drugs and four metabolites in human plasma by HPLC-MS.

PubMed

Choong, Eva; Rudaz, Serge; Kottelat, Astrid; Guillarme, Davy; Veuthey, Jean-Luc; Eap, Chin B

2009-12-05

A simple and sensitive LC-MS method was developed and validated for the simultaneous quantification of aripiprazole (ARI), atomoxetine (ATO), duloxetine (DUL), clozapine (CLO), olanzapine (OLA), sertindole (STN), venlafaxine (VEN) and their active metabolites dehydroaripiprazole (DARI), norclozapine (NCLO), dehydrosertindole (DSTN) and O-desmethylvenlafaxine (OVEN) in human plasma. The above mentioned compounds and the internal standard (remoxipride) were extracted from 0.5 mL plasma by solid-phase extraction (mix mode support). The analytical separation was carried out on a reverse phase liquid chromatography at basic pH (pH 8.1) in gradient mode. All analytes were monitored by MS detection in the single ion monitoring mode and the method was validated covering the corresponding therapeutic range: 2-200 ng/mL for DUL, OLA, and STN, 4-200 ng/mL for DSTN, 5-1000 ng/mL for ARI, DARI and finally 2-1000 ng/mL for ATO, CLO, NCLO, VEN, OVEN. For all investigated compounds, good performance in terms of recoveries, selectivity, stability, repeatability, intermediate precision, trueness and accuracy, was obtained. Real patient plasma samples were then successfully analysed.

Open-mode delamination stress concentrations in horseshoe and elliptic composite curved bars subjected to end forces

NASA Technical Reports Server (NTRS)

Ko, William L.; Jackson, Raymond H.

1990-01-01

The multilayer theory of anisotropic elasticity and a finite element method were used to analyze the open-mode delamination stress concentrations in horseshoe and elliptic laminated composite curved bars. Two types of laminations, solid laminations and sandwich laminations, were analyzed. It was found that the open-mode delamination stress concentration could be greatly increased in these two types of curved bars by decreasing their aspect ratios. The open-mode delamination stress concentration generated in the solid laminations was found to be far more severe than that generated in the sandwich laminations. The horseshoe curved bar may be used to determine both the open-mode delamination strength of solidly laminated composites and the open-mode debonding strength of sandwiched laminated composites. However, the elliptic curved bar is only good for determining the open-mode delamination strength of solidly laminated composites.

Graphene oxide decorated with silver nanoparticles as a coating on a stainless-steel fiber for solid-phase microextraction.

PubMed

Wang, Licheng; Hou, Xiudan; Li, Jubai; Liu, Shujuan; Guo, Yong

2015-07-01

A novel graphene oxide decorated with silver nanoparticles coating on a stainless-steel fiber for solid-phase microextraction was prepared. Scanning electron microscopy and X-ray photoelectron spectroscopy were used to characterize the coating surface and showed that silver nanoparticles were dispersed on the wrinkled graphene oxide surface. Coupled to gas chromatography with flame ionization detection, the extraction abilities of the fiber for polycyclic aromatic hydrocarbons were examined in the headspace solid-phase microextraction mode. The extraction parameters including adsorption time, adsorption temperature, salt concentration, desorption time and desorption temperature were investigated. Under the optimized condition, wide linearity with low limits of detection from 2 to 10 ng/L was obtained. The relative standard deviations for single-fiber repeatability and fiber-to-fiber reproducibility were less than 10.6 and 17.5%, respectively. The enrichment factors were from 1712.5 to 4503.7, showing the fiber has good extraction abilities. Moreover, the fiber exhibited a good stability and could be reused for more than 120 times. The established method was also applied for determination of polycyclic aromatic hydrocarbons in two real water samples and the recoveries of analytes ranged from 84.4-116.3% with relative standard deviations less than 16.2%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ascent abort capability for the HL-20

NASA Technical Reports Server (NTRS)

Naftel, J. C.; Talay, T. A.

1993-01-01

The HL-20 has been designed with the capability for rescue of the crew during all phases of powered ascent from on the launch pad until orbital injection. A launch-escape system, consisting of solid rocket motors located on the adapter between the HL-20 and the launch vehicle, provides the thrust that propels the HL-20 to a safe distance from a malfunctioning launch vehicle. After these launch-escape motors have burned out, the adapter is jettisoned and the HL-20 executes one of four abort modes. In three abort modes - return-to-launch-site, transatlantic-abort-landing, and abort-to-orbit - not only is the crew rescued, but the HL-20 is recovered intact. In the ocean-landing-by-parachute abort mode, which occurs in between the return-to-launch-site and the transatlantic-abort-landing modes, the crew is rescued, but the HL-20 would likely sustain damage from the ocean landing. This paper describes the launch-escape system and the four abort modes for an ascent on a Titan III launch vehicle.

A mode matching method for modeling dissipative silencers lined with poroelastic materials and containing mean flow.

PubMed

Nennig, Benoit; Perrey-Debain, Emmanuel; Ben Tahar, Mabrouk

2010-12-01

A mode matching method for predicting the transmission loss of a cylindrical shaped dissipative silencer partially filled with a poroelastic foam is developed. The model takes into account the solid phase elasticity of the sound-absorbing material, the mounting conditions of the foam, and the presence of a uniform mean flow in the central airway. The novelty of the proposed approach lies in the fact that guided modes of the silencer have a composite nature containing both compressional and shear waves as opposed to classical mode matching methods in which only acoustic pressure waves are present. Results presented demonstrate good agreement with finite element calculations provided a sufficient number of modes are retained. In practice, it is found that the time for computing the transmission loss over a large frequency range takes a few minutes on a personal computer. This makes the present method a reliable tool for tackling dissipative silencers lined with poroelastic materials.

Rayleigh scattering in an emitter-nanofiber-coupling system

NASA Astrophysics Data System (ADS)

Tang, Shui-Jing; Gao, Fei; Xu, Da; Li, Yan; Gong, Qihuang; Xiao, Yun-Feng

2017-04-01

Scattering is a general process in both fundamental and applied physics. In this paper, we investigate Rayleigh scattering of a solid-state-emitter coupled to a nanofiber, by S -matrix-like theory in k -space description. Under this model, both Rayleigh scattering and dipole interaction are studied between a two-level artificial atom embedded in a nanocrystal and fiber modes (guided and radiation modes). It is found that Rayleigh scattering plays a critical role in the transport properties and quantum statistics of photons. On the one hand, Rayleigh scattering produces the transparency in the optical transmitted field of the nanofiber, accompanied by the change of atomic phase, population, and frequency shift. On the other hand, the interference between two kinds of scattering fields by Rayleigh scattering and dipole transition modifies the photon statistics (second-order autocorrelation function) of output fields, showing a strong wavelength dependence. This study provides guidance for the solid-state emitter acting as a single-photon source and can be extended to explore the scattering effect in many-body physics.

Hot-water and solid-phase extraction of fluorescent whitening agents in paper materials and infant clothes followed by unequivocal determination with ion-pair chromatography-tandem mass spectrometry.

PubMed

Chen, Hsin-Chang; Ding, Wang-Hsien

2006-03-10

A comprehensive method for the determination of four stilbene-type disulfonate and one distyrylbiphenyl-type fluorescent whitening agents (FWAs) in paper materials (napkin and paper tissue) and infant clothes was developed. FWAs were extracted from paper material and cloth samples using a hot-water extraction, and the aqueous extracts were then preconcentrated with the newly developed Oasis WAX (mixed-mode of weak anion exchange and reversed-phase sorbent) solid-phase extraction cartridge. The analytes were unequivocal determined by ion pair chromatography coupled with negative electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS-MS), applying a di-n-hexyl-ammonium acetate (DHAA) as the ion-pairing reagent in mobile phase. Limits of quantitation (LOQ) were established between 0.2 and 0.9 ng/g in 2 g of samples. Recovery of five FWAs in spiked commercial samples was between 42 and 95% and RSD (n = 3) ranging from 2 to 11%. The method was finally applied to commercial samples, showing that two stilbene-type disulfonates were predominant FWAs detected in napkin and infant cloth samples.

Structural and ferroelectric phase evolution in [KNbO3]1-x[BaNi1/2Nb1/2O3-δ]x (x = 0, 0.1)

NASA Astrophysics Data System (ADS)

Hawley, Christopher; Wu, Liyan; Xiao, Geoffrey; Grinberg, Ilya; Rappe, Andrew; Davies, Peter; Spanier, Jonathan

The phase transition evolution for [KNbO3]1-x[BaNi1/2Nb1/2O3-δ]x (x=0, 0.1) is determined via complementary dielectric constant and Raman scattering measurements. Raman scattering by optical phonons over the range of 100-1000 cm-1 for -190°C < T < 600°C reveals six discernible zone-center optical phonon modes. They are assigned to structural and ferroelectric phases in the solid solution x = 0.1 and compared with those for end member x = 0 and with the results of temperature-dependent dielectric permittivity. Rigorous peak fitting analyses of spectra collected from the solid solution and end member indicate structural and ferroelectric phase transition temperatures that are quite close to those for the KNbO3 end member. Remarkably, despite the inclusion of 5 atomic Work supported by US ARO under W911NF-14-1-0500, NSF 1123696, and DoE BES under DE-FG02-07ER46431. Equipment acquisitions and computational support under DURIP and DoE NERSCC.

Ultrasound shear wave imaging

NASA Astrophysics Data System (ADS)

Ye, Shigong; Wu, Junru

2000-05-01

Shear wave propagation properties including phase velocity and attenuation coefficient are indispensable information in materials characterization and nondestructive evaluation. A computer controlled scanning shear-wave ultrasonic imaging system has been developed. It consists of a pair of focusing broadband pvdf transducers of central frequency of 50 MHz immersed in distilled water. Shear waves in a solid specimen are generated by mode-conversion. When ultrasonic waves generated by one of the pvdf transducers impinge upon a solid specimen from water with angle of incidence of θ that is greater than θcr, the critical angle of the longitudinal wave in the solid, only shear waves can propagate in the solid and longitudinal waves become evanescent waves. The shear waves pass through the specimen and received by the other pvdf transducer. Meanwhile, the specimen was scanned by a stepped motor of a step of 10 μm. The system was used to generated shear waves amplitude and phase velocity images of bone specimen of 1280 μm and they are compared with their longitudinal wave counterparts. The results have shown shear wave images can provide additional shear modulus and shear viscous information that longitudinal waves can't provide. The lateral resolution of 60 μm was achieved using shear wave imaging technique applied in bone sample.

Determination of flubendiamide in honey at trace levels by using solid phase extraction and liquid chromatography coupled to quadrupole time-of-flight mass spectrometry.

PubMed

Ares, Ana M; Valverde, Silvia; Bernal, José L; Toribio, Laura; Nozal, María J; Bernal, José

2017-10-01

In this study, a new method has been developed to determine flubendiamide in honey using liquid chromatography coupled to a selective mass spectrometry detector (quadrupole-time-of-flight). An efficient sample treatment involving a solid phase extraction with a C 18 sorbent was proposed (average analyte recoveries were between 94 and 104%). Chromatographic analysis (9min) was performed on a C 18 column (Gemini C 18 , 50×2.0mm, 3µm, 110Å). The mobile phase consisted of water and acetonitrile, with a flow rate of 0.5mL/min in gradient elution mode. The method was fully validated in terms of selectivity, limits of detection and quantification, matrix effect, linearity, trueness and precision. Low limits of detection and quantification were obtained, ranging from 0.1 to 0.2µg/kg and 0.4 to 0.6µg/kg, respectively. The method was applied to analyze flubendiamide in honey from different botanic origins (multifloral, rosemary and heather). Copyright © 2017 Elsevier Ltd. All rights reserved.

Intraseasonal oscillation associated with the Indian winter monsoon

NASA Astrophysics Data System (ADS)

Dimri, A. P.

2013-02-01

The Indian winter (December-February) monsoon (IWM) contributes almost one third of the annual precipitation over the western Himalayas (WH). In winter, eastward moving synoptic weather systems, or "western disturbances" (WDs), yield precipitation in either liquid or solid form. Although previous studies have examined the interannual variation (IAV) of the IWM, little is known of the intraseasonal oscillation (ISO) associated with the IWM. The present study examines the ISO and its plausible effects on the IWM using 28 years (1980-2007) of precipitation, height, wind, and outgoing longwave radiation (OLR) fields. The dominant ISO mode is found during the active IWM phase with well-defined cyclonic circulation in the midtroposphere over the WH. The relationship between OLR and circulation indicates that this ISO mode is driven by moisture convergence. During the peak phase, a strong moisture influx from the Arabian Sea dominates. This moisture incursion adds to the precipitation over the WH. Successive growth and decay of anomalous cyclonic and anticyclonic circulation takes place within ISO periodicity. Strong convection always seems to precede anomalous cyclonic circulation. In addition, in-phase wind and convection (over the WH region) are associated with the ISO phase.

The effect of the London-van der Waals dispersion force on interline heat transfer

NASA Technical Reports Server (NTRS)

Wayner, P. C., Jr.

1978-01-01

A theoretical procedure to determine the heat transfer characteristics of the interline region (junction of liquid-solid-vapor) from the macroscopic optical and thermophysical properties of the system is outlined. The analysis is based on the premise that the interline transport processes are controlled by the London-van der Waals dispersion force between condensed phases (solid and liquid). Numerical values of the dispersion constant are presented. The procedure is used to compare the relative size of the interline heat sink of various systems using a constant heat flux mode. This solution demonstrates the importance of the interline heat flow number, which is evaluated for various systems.

Manipulation and control of instabilities for surfactant-laden liquid film flowing down an inclined plane using a deformable solid layer

NASA Astrophysics Data System (ADS)

Tomar, Dharmendra S.; Sharma, Gaurav

2018-01-01

We analyzed the linear stability of surfactant-laden liquid film with a free surface flowing down an inclined plane under the action of gravity when the inclined plane is coated with a deformable solid layer. For a flow past a rigid incline and in the presence of inertia, the gas-liquid (GL) interface is prone to the free surface instability and the presence of surfactant is known to stabilize the free surface mode when the Marangoni number increases above a critical value. The rigid surface configuration also admits a surfactant induced Marangoni mode which remains stable for film flows with a free surface. This Marangoni mode was observed to become unstable for a surfactant covered film flow past a flexible inclined plane in a creeping flow limit when the wall is made sufficiently deformable. In view of these observations, we investigate the following two aspects. First, what is the effect of inertia on Marangoni mode instability induced by wall deformability? Second, and more importantly, whether it is possible to use a deformable solid coating to obtain stable flow for the surfactant covered film for cases when the Marangoni number is below the critical value required for stabilization of free surface instability. In order to explore the first question, we continued the growth rates for the Marangoni mode from the creeping flow limit to finite Reynolds numbers (Re) and observed that while the increase in Reynolds number has a small stabilizing effect on growth rates, the Marangoni mode still remains unstable for finite Reynolds numbers as long as the wall is sufficiently deformable. The Marangoni mode remains the dominant mode for zero and small Reynolds numbers until the GL mode also becomes unstable with the increase in Re. Thus, for a given set of parameters and beyond a critical Re, there is an exchange of dominant mode of instability from the Marangoni to free surface GL mode. With respect to the second important aspect, our results clearly demonstrate that for cases when the stabilizing contribution of surfactant is not sufficient for suppressing GL mode instability, a deformable solid coating could be employed to suppress free surface instability without triggering Marangoni or liquid-solid interfacial modes. Specifically, we have shown that for a given solid thickness, as the shear modulus of the solid layer decreases (i.e., the solid becomes more deformable) the GL mode instability is suppressed. With further decrease in shear modulus, the Marangoni and liquid-solid interfacial modes become unstable. Thus, there exists a stability window in terms of shear modulus where the surfactant-laden film flow remains stable even when the Marangoni number is below the critical value required for free surface instability suppression. Further, when the Marangoni number is greater than the critical value so that the GL mode remains stable in the rigid limit or with the deformable wall, the increase in wall deformability or solid thickness triggers Marangoni mode instability and, thus, renders a stable flow configuration into an unstable one. Thus, we show that the soft solid layer can be used to manipulate and control the stability of surfactant-laden film flows.

A new laboratory approach to shale analysis using NMR relaxometry

USGS Publications Warehouse

Washburn, Kathryn E.; Birdwell, Justin E.; Baez, Luis; Beeney, Ken; Sonnenberg, Steve

2013-01-01

Low-field nuclear magnetic resonance (LF-NMR) relaxometry is a non-invasive technique commonly used to assess hydrogen-bearing fluids in petroleum reservoir rocks. Measurements made using LF-NMR provide information on rock porosity, pore-size distributions, and in some cases, fluid types and saturations (Timur, 1967; Kenyon et al., 1986; Straley et al., 1994; Brown, 2001; Jackson, 2001; Kleinberg, 2001; Hurlimann et al., 2002). Recent improvements in LF-NMR instrument electronics have made it possible to apply methods used to measure pore fluids to assess highly viscous and even solid organic phases within reservoir rocks. T1 and T2 relaxation responses behave very differently in solids and liquids; therefore the relationship between these two modes of relaxation can be used to differentiate organic phases in rock samples or to characterize extracted organic materials. Using T1-T2 correlation data, organic components present in shales, such as kerogen and bitumen, can be examined in laboratory relaxometry measurements. In addition, implementation of a solid-echo pulse sequence to refocus T2 relaxation caused by homonuclear dipolar coupling during correlation measurements allows for improved resolution of solid-phase protons. LF-NMR measurements of T1 and T2 relaxation time distributions were carried out on raw oil shale samples from the Eocene Green River Formation and pyrolyzed samples of these shales processed by hydrous pyrolysis and techniques meant to mimic surface and in-situ retorting. Samples processed using the In Situ Simulator approach ranged from bitumen and early oil generation through to depletion of petroleum generating potential. The standard T1-T2 correlation plots revealed distinct peaks representative of solid- and liquid-like organic phases; results on the pyrolyzed shales reflect changes that occurred during thermal processing. The solid-echo T1 and T2 measurements were used to improve assessment of the solid organic phases, specifically kerogen, thermally degraded kerogen, and char. Integrated peak areas from the LF-NMR results representative of kerogen and bitumen were found to be well correlated with S1 and S2 parameters from Rock-Eval programmed pyrolysis. This study demonstrates that LFNMR relaxometry can provide a wide range of information on shales and other reservoir rocks that goes well beyond porosity and pore-fluid analysis.

Dancing drops over vibrating substrates

NASA Astrophysics Data System (ADS)

Borcia, Rodica; Borcia, Ion Dan; Helbig, Markus; Meier, Martin; Egbers, Christoph; Bestehorn, Michael

2017-04-01

We study the motion of a liquid drop on a solid plate simultaneously submitted to horizontal and vertical harmonic vibrations. The investigation is done via a phase field model earlier developed for describing static and dynamic contact angles. The density field is nearly constant in every bulk region (ρ = 1 in the liquid phase, ρ ≈ 0 in the vapor phase) and varies continuously from one phase to the other with a rapid but smooth variation across the interfaces. Complicated explicit boundary conditions along the interface are avoided and captured implicitly by gradient terms of ρ in the hydrodynamic basic equations. The contact angle θ is controlled through the density at the solid substrate ρ S , a free parameter varying between 0 and 1 [R. Borcia, I.D. Borcia, M. Bestehorn, Phys. Rev. E 78, 066307 (2008)]. We emphasize the swaying and the spreading modes, earlier theoretically identified by Benilov and Billingham via a shallow-water model for drops climbing uphill along an inclined plane oscillating vertically [E.S. Benilov, J. Billingham, J. Fluid Mech. 674, 93 (2011)]. The numerical phase field simulations will be completed by experiments. Some ways to prevent the release of the dancing drops along a hydrophobic surface into the gas atmosphere are also discussed in this paper.

FIBER OPTICS. ACOUSTOOPTICS: Amplitude and phase nonreciprocities of acoustooptic modulators for counterpropagating light waves under the Bragg diffraction conditions

NASA Astrophysics Data System (ADS)

Veselovskaya, T. V.; Klochan, E. L.; Lariontsev, E. G.; Parfenov, S. V.; Shelaev, A. N.

1990-07-01

Theoretical and experimental investigations demonstrated that in real acoustooptic modulators the diffraction of light by a standing ultrasonic wave may give rise to both phase and amplitude nonreciprocities of counterpropagating light waves. Analytic expressions are derived for the dependences of these nonreciprocities on the parameters of the traveling component of an ultrasonic wave in a modulator. It is shown that when the angle of incidence of light on a modulator deviates from the Bragg angle, the phase nonreciprocity may be suppressed, but the amplitude nonreciprocity becomes maximal and its sign is governed by the law of deviation of the angle of incidence from the Bragg angle. A diffraction acoustooptic feedback makes it possible not only to achieve mode locking with an acoustooptic modulator utilizing a traveling ultrasonic wave, but also to control the magnitude and sign of amplitude-frequency nonreciprocities. It is reported that an acoustooptic feedback can be used to generate self-pumping waves in a solid-state mode-locked ring laser and thus stabilize bidirectional lasing in a wide range of the frequency offset between the counterpropagating waves.

Graphene saturable absorber mirror for ultra-fast-pulse solid-state laser.

PubMed

Xu, Jin-Long; Li, Xian-Lei; Wu, Yong-Zhong; Hao, Xiao-Peng; He, Jing-Liang; Yang, Ke-Jian

2011-05-15

High-quality graphene sheets with lateral size over 20 μm have been obtained by bath sonicating after subjecting the wormlike graphite marginally to mixed oxidizer. To date, to our knowledge, they are the largest graphene sheets prepared by exfoliation in the liquid phase. A saturable absorber mirror was fabricated based on these sheets. We exploited it to realize mode-locking operation in a diode-pumped Nd:GdVO(4) laser. A pulse duration of 16 ps was produced with an average power of 360 mW and a highest pulse energy of 8.4 nJ for a graphene mode-locked laser. © 2011 Optical Society of America

Direct detection of boldenone sulfate and glucuronide conjugates in horse urine by ion trap liquid chromatography-mass spectrometry.

PubMed

Pu, Fan; McKinney, Andrew R; Stenhouse, Allen M; Suann, Craig J; McLeod, Malcolm D

2004-12-25

A study of the equine phase II metabolism of the anabolic agent boldenone is reported. Boldenone sulfate, boldenone glucuronide and their C17-epimers were synthesised as reference standards in our lab and a method was developed for their detection in a horse urine matrix. Solid phase extraction was used to purify the analytes, which were then detected by ion trap LC/MS. Negative and positive ionisation mode MS(2) were used for the detection of sulfate and glucuronide conjugates, respectively. Boldenone sulfate and 17-epiboldenone glucuronide were detected as the major and minor phase II metabolites, respectively, in horse urine samples collected following the administration of boldenone undecylenate by intramuscular injection.

Efficient carrier-envelope offset frequency stabilization through gain modulation via stimulated emission.

PubMed

Karlen, Lauriane; Buchs, Gilles; Portuondo-Campa, Erwin; Lecomte, Steve

2016-01-15

A novel scheme for intracavity control of the carrier-envelope offset (CEO) frequency of a 100 MHz mode-locked Er:Yb:glass diode-pumped solid-state laser (DPSSL) based on the modulation of the laser gain via stimulated emission of the excited Er(3+) ions is demonstrated. This method allows us to bypass the ytterbium system few-kHz low-pass filter in the f(CEO) stabilization loop and thus to push the phase lock bandwidth up to a limit close to the relaxation oscillations frequency of the erbium system. A phase lock bandwidth above 70 kHz has been achieved with the fully stabilized laser, leading to an integrated phase noise [1 Hz-1 MHz] of 120 mrad.

Continuum limit of the vibrational properties of amorphous solids.

PubMed

Mizuno, Hideyuki; Shiba, Hayato; Ikeda, Atsushi

2017-11-14

The low-frequency vibrational and low-temperature thermal properties of amorphous solids are markedly different from those of crystalline solids. This situation is counterintuitive because all solid materials are expected to behave as a homogeneous elastic body in the continuum limit, in which vibrational modes are phonons that follow the Debye law. A number of phenomenological explanations for this situation have been proposed, which assume elastic heterogeneities, soft localized vibrations, and so on. Microscopic mean-field theories have recently been developed to predict the universal non-Debye scaling law. Considering these theoretical arguments, it is absolutely necessary to directly observe the nature of the low-frequency vibrations of amorphous solids and determine the laws that such vibrations obey. Herein, we perform an extremely large-scale vibrational mode analysis of a model amorphous solid. We find that the scaling law predicted by the mean-field theory is violated at low frequency, and in the continuum limit, the vibrational modes converge to a mixture of phonon modes that follow the Debye law and soft localized modes that follow another universal non-Debye scaling law.

Continuum limit of the vibrational properties of amorphous solids

PubMed Central

Mizuno, Hideyuki; Ikeda, Atsushi

2017-01-01

The low-frequency vibrational and low-temperature thermal properties of amorphous solids are markedly different from those of crystalline solids. This situation is counterintuitive because all solid materials are expected to behave as a homogeneous elastic body in the continuum limit, in which vibrational modes are phonons that follow the Debye law. A number of phenomenological explanations for this situation have been proposed, which assume elastic heterogeneities, soft localized vibrations, and so on. Microscopic mean-field theories have recently been developed to predict the universal non-Debye scaling law. Considering these theoretical arguments, it is absolutely necessary to directly observe the nature of the low-frequency vibrations of amorphous solids and determine the laws that such vibrations obey. Herein, we perform an extremely large-scale vibrational mode analysis of a model amorphous solid. We find that the scaling law predicted by the mean-field theory is violated at low frequency, and in the continuum limit, the vibrational modes converge to a mixture of phonon modes that follow the Debye law and soft localized modes that follow another universal non-Debye scaling law. PMID:29087941

A complete assignment of the vibrational spectra of 2-furoic acid based on the structures of the more stable monomer and dimer.

PubMed

Ghalla, Houcine; Issaoui, Noureddine; Castillo, María Victoria; Brandán, Silvia Antonia; Flakus, Henryk T

2014-01-01

The structural and vibrational properties of cyclic dimer of 2-furoic acid (2FA) were predicted by combining the available experimental infrared and Raman spectra in the solid phase and ab initio calculations based on density functional theory (DFT) with Pople's basis sets. The calculations show that there are two cyclic dimers for the title molecule that have been theoretically determined in the gas phase, and that only one of them, cis conformer, is present in the solid phase. The complete assignment of the 66 normal vibrational modes for the cis cyclic dimer was performed using the Pulay's Scaled Quantum Mechanics Force Field (SQMFF) methodology. Four strong bands in the infrared spectrum at 1583, 1427, 1126 and 887 cm(-1) and the group of bands in the Raman spectrum at 1464, 1452, 1147, 1030, 885, 873, 848, 715 and 590 cm(-1) are characteristic of the dimeric form of 2FA in the solid phase. In this work, the calculated structural and vibrational properties of both dimeric species were analyzed and compared between them. In addition, three types of atomic charges, bond orders, possible charge transfer, topological properties of the furan rings, Natural Bond Orbital (NBO) and Atoms in Molecules (AIM) theory calculations were employed to study the stabilities and intermolecular interactions of the both dimers of 2FA. Copyright © 2013 Elsevier B.V. All rights reserved.

Preparation of a reversed-phase/anion-exchange mixed-mode spherical sorbent by Pickering emulsion polymerization for highly selective solid-phase extraction of acidic pharmaceuticals from wastewater.

PubMed

Huang, Chaonan; Li, Yun; Yang, Jiajia; Peng, Junyu; Jin, Jing; Dhanjai; Wang, Jincheng; Chen, Jiping

2017-10-27

The present work represents a simple and effective preparation of a novel mixed-mode anion-exchange (MAX) sorbent based on porous poly[2-(diethylamino)ethyl methacrylate-divinylbenzene] (poly(DEAEMA-DVB)) spherical particles synthesized by one-step Pickering emulsion polymerization. The poly(DEAEMA-DVB) particles were quaternized with 1,4-butanediol diglycidyl ether (BDDE) followed by triethylamine (TEA) via epoxy-amine reaction to offer strong anion exchange properties. The synthesized MAX sorbent was characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy, nitrogen adsorption-desorption measurements and elemental analysis. The MAX sorbent possessed regular spherical shape and narrow diameter distribution (15-35μm), a high IEC of 0.54meq/g, with carbon and nitrogen contents of 80.3% and 1.62%, respectively. Compared to poly(DEAEMA-DVB), the MAX sorbent exhibited decreased S BET (390.5 vs. 515.3m 2 g -1 ), pore volume (0.74 vs. 0.85cm 3 g -1 ) and pore size (16.8 vs. 17.3nm). Moreover, changes of N content for producing the MAX sorbent reveal a successful two-step quaternization, which can be highly related to such a high IEC. Finally, the MAX sorbent was successfully evaluated for selective isolation and purification of some selected acidic pharmaceuticals (ketoprofen, KEP; naproxen, NAP; and ibuprofen, IBP) from neutral (hydrocortisone, HYC), basic (carbamazepine, CAZ; amitriptyline, AMT) pharmaceuticals and other interferences in water samples using solid phase extraction (SPE). An efficient analytical method based on the MAX-based mixed-mode SPE coupled with HPLC-UV was developed for highly selective extraction and cleanup of acidic KEP, NAP and IBP in spiked wastewater samples. The developed method exhibited good sensitivity (0.009-0.085μgL -1 limit of detection), satisfactory recoveries (82.1%-105.5%) and repeatabilities (relative standard deviation < 7.9%, n=3). Copyright © 2017 Elsevier B.V. All rights reserved.

Ultra-low noise combs in the palm of your hand

NASA Astrophysics Data System (ADS)

Schibli, Thomas R.

Mode-locked lasers are attractive tools for precision measurements and for photonic microwave generation. The technology around these lasers has rapidly evolved, and with the invention of optical frequency combs, fs-technology has become a ubiquitous tool science and engineering. At first, most of these combs were generated by bulky and delicate Kerr-Lens mode-locked Ti:sapphire systems, but have now been mostly replaced by the much more robust and compact fiber lasers. However, the move from table-top solid-state lasers to the fully self-contained fiber systems came with a price: the optical phase noise performance degraded due to design constraints. While this is of no concern for most spectroscopic applications, it poses a challenge for applications that require excellent short-term phase noise performance, such as, for example, required for photonic microwave generation. While much of this has been improved by ingenious laser designs, it remains a challenge to obtain ultra-low phase-noise combs from high-repetition-rate fiber lasers. Here we present a new approach consisting of a monolithic cavity design, in which the laser light is fully confined inside an optical material. Thanks to this monolithic design, these solid-state lasers are inherently robust against environmental perturbations, such as acoustics, vibrations, air pressure and humidity. Opposed to the omnipresent mode-locked fiber lasers, these monolithic lasers exhibit very low round-trip loss, dispersion and nonlinearities. As a result, they produce highly stable pulse trains, with free-running relative line-widths of the order of a few Hz in the optical domain, despite their moderately high fundamental repetition rates of 1 GHz. The compact design further simplifies integration into complex systems, and eliminates the need for an optics bench or a vibration isolated platform. These lasers produce less than 0.2 W of heat, and are fully turn-key. This work was supported by the DARPA PULSE program with a Grant from AMRDEC and by the NSF Early Career Award.

Separation and determination of polyurethane amine catalysts in polyether polyols by using UHPLC-Q-TOF-MS on a reversed-phase/cation-exchange mixed-mode column.

PubMed

Li, Jiaxiao; Zhu, Marcel

2018-02-01

A simple, selective, and accurate ultra-high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry method was established and validated for the efficient separation and quantification of polyurethane amine catalysts in polyether polyols. Amine catalysts were primarily separated in polyether polyol-based sample by solid-phase extraction, and further baseline separated on a reversed-phase/cation-exchange mixed-mode column (SiELC Primesep™ 200) using 0.1% trifluoroacetic acid/acetonitrile as a mobile phase in gradient elution mode at a flow rate of 0.2 mL/min. High-resolution quadrupole time-of-flight mass spectrometry analysis in electrospray ionization positive mode allowed the identification as N,N'-bis[3-(dimethylamino)propyl]urea, N-[2-(2-dimethylaminoethoxy)ethyl]-N-methyl-1,3-propanediamine, and N,N,N',N'-tetramethyldipropylenetriamine. The method was validated and presented good linearity for all the analytes in blank matrices within the concentration range of 0.20-5.0 or 0.1-2.0 μg/mL with the correlation coefficients (R 2 ) ranging from 0.986 to 0.997. Method recovery ranged within 81-105% at all three levels (80, 100, and 120% of the original amount) with relative standard deviations of 1.0-6.2%. The limits of detection were in the range of 0.007-0.051 μg/mL. Good precision was obtained with relative standard deviation below 3.2 and 0.72% for peak area and retention time of three amines, respectively. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Study of long-range orders of hard-core bosons coupled to cooperative normal modes in two-dimensional lattices

NASA Astrophysics Data System (ADS)

Ghosh, A.; Yarlagadda, S.

2017-09-01

Understanding the microscopic mechanism of coexisting long-range orders (such as lattice supersolidity) in strongly correlated systems is a subject of immense interest. We study the possible manifestations of long-range orders, including lattice-supersolid phases with differently broken symmetry, in a two-dimensional square lattice system of hard-core bosons (HCBs) coupled to archetypal cooperative/coherent normal-mode distortions such as those in perovskites. At strong HCB-phonon coupling, using a duality transformation to map the strong-coupling problem to a weak-coupling one, we obtain an effective Hamiltonian involving nearest-neighbor, next-nearest-neighbor, and next-to-next-nearest-neighbor hoppings and repulsions. Using stochastic series expansion quantum Monte Carlo, we construct the phase diagram of the system. As coupling strength is increased, we find that the system undergoes a first-order quantum phase transition from a superfluid to a checkerboard solid at half-filling and from a superfluid to a diagonal striped solid [with crystalline ordering wave vector Q ⃗=(2 π /3 ,2 π /3 ) or (2 π /3 ,4 π /3 )] at one-third filling without showing any evidence of supersolidity. On tuning the system away from these commensurate fillings, checkerboard supersolid is generated near half-filling whereas a rare diagonal striped supersolid is realized near one-third filling. Interestingly, there is an asymmetry in the extent of supersolidity about one-third filling. Within our framework, we also provide an explanation for the observed checkerboard and stripe formations in La2 -xSrxNiO4 at x =1 /2 and x =1 /3 .

Majorana modes in solid state systems and its dynamics

NASA Astrophysics Data System (ADS)

Zhang, Qi; Wu, Biao

2018-04-01

We review the properties of Majorana fermions in particle physics and point out that Majorana modes in solid state systems are significantly different. The key reason is the concept of anti-particle in solid state systems is different from its counterpart in particle physics. We define Majorana modes as the eigenstates of Majorana operators and find that they can exist both at edges and in the bulk. According to our definition, only one single Majorana mode can exist in a system no matter at edges or in the bulk. Kitaev's spinless p-wave superconductor is used to illustrate our results and the dynamical behavior of the Majorana modes.

Miniaturized Amperometric Solid Electrolyte Carbon Dioxide Sensors

NASA Technical Reports Server (NTRS)

Hunter, G. W.; Xu, J. C.; Liu, C. C.; Hammond, J. W.; Ward, B.; Lukco, D.; Lampard, P.; Artale, M.; Androjna, D.

2006-01-01

A miniaturized electrochemical carbon dioxide (CO2) sensor using Na3Z r2Si2PO12 (NASICON) as a solid electrolyte has been fabricated and de monstrated. Microfabrication techniques were used for sensor fabricat ion to yield a sensing area around 1.0 mm x 1.1 mm. The NASICON solid electrolyte and the Na2CO3/BaCO3 (1:1.7 molar ratio) auxiliary elect rolyte were deposited by sputtering in between and on top of the inte rdigitated finger-shaped platinum electrodes. This structure maximize s the length of the three-phase boundary (electrode, solid electrolyt e, and auxiliary electrolyte), which is critical for gas sensing. The robust CO2 sensor operated up to 600 C in an amperometric mode and a ttempts were made to optimize sensor operating parameters. Concentrat ions of CO2 between 0.02% and 4% were detected and the overall sensor performance was evaluated. Linear response of sensor current output to ln[CO2 concentration] ranging from 0.02% to 1% was achieved.

A DFT study on structural, vibrational properties, and quasiparticle band structure of solid nitromethane.

PubMed

Appalakondaiah, S; Vaitheeswaran, G; Lebègue, S

2013-05-14

We report a detailed theoretical study of the structural and vibrational properties of solid nitromethane using first principles density functional calculations. The ground state properties were calculated using a plane wave pseudopotential code with either the local density approximation, the generalized gradient approximation, or with a correction to include van der Waals interactions. Our calculated equilibrium lattice parameters and volume using a dispersion correction are found to be in reasonable agreement with the experimental results. Also, our calculations reproduce the experimental trends in the structural properties at high pressure. We found a discontinuity in the bond length, bond angles, and also a weakening of hydrogen bond strength in the pressure range from 10 to 12 GPa, picturing the structural transition from phase I to phase II. Moreover, we predict the elastic constants of solid nitromethane and find that the corresponding bulk modulus is in good agreement with experiments. The calculated elastic constants show an order of C11> C22 > C33, indicating that the material is more compressible along the c-axis. We also calculated the zone center vibrational frequencies and discuss the internal and external modes of this material under pressure. From this, we found the softening of lattice modes around 8-11 GPa. We have also attempted the quasiparticle band structure of solid nitromethane with the G0W0 approximation and found that nitromethane is an indirect band gap insulator with a value of the band gap of about 7.8 eV with G0W0 approximation. Finally, the optical properties of this material, namely the absorptive and dispersive part of the dielectric function, and the refractive index and absorption spectra are calculated and the contribution of different transition peaks of the absorption spectra are analyzed. The static dielectric constant and refractive indices along the three inequivalent crystallographic directions indicate that this material has a considerable optical anisotropy.

Determination of cocaine, benzoylecgonine, cocaethylene and norcocaine in human hair using solid-phase extraction and liquid chromatography with tandem mass spectrometric detection.

PubMed

Moore, Christine; Coulter, Cynthia; Crompton, Katherine

2007-11-15

A quantitative analytical procedure for the determination of cocaine, benzoylecgonine and cocaethylene and norcocaine in hair has been developed and validated. The hair samples were washed, incubated, and any drugs present were quantified using mixed mode solid-phase extraction and liquid chromatography with tandem mass spectrometric detection in positive atmospheric pressure chemical ionization mode. For confirmation, two transitions were monitored and one ion ratio was determined, which was within 20% of that of the known calibration standards. The monitoring of the qualifying transition and requirement for its presence within a specific ratio to the primary ion limited the sensitivity of the assay, particularly for benzoylecgonine, however, the additional confidence in the final result as well as forensic defensibility were considered to be of greater importance. Even with simultaneous monitoring, the concentrations proposed by the United States Federal guidelines for hair analysis were achieved. The limits of quantitation were 50 pg/mg; the limit of detection was 25 pg/mg. The intra-day precision of the assays at 100 pg/mg (n=5) was 1.3%, 8.1%, 0.8% and 0.4%; inter-day precision 4.8%, 9.2%, 15.7% and 12.6% (n=10) for cocaine, benzoylecgonine, cocaethylene and norcocaine, respectively. The methods were applied to both proficiency specimens and to samples obtained during research studies in the USA.

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

PubMed

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

2017-06-29

In this study, a high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for simultaneous determination of eight paralytic shellfish poisoning (PSP) toxins, including saxitoxin (STX), neosaxitoxin (NEO), gonyautoxins (GTX1-4) and the N -sulfo carbamoyl toxins C1 and C2, in sea shellfish. The samples were extracted by acetonitrile/water (80:20, v / v ) with 0.1% formic and purified by dispersive solid-phase extraction (dSPE) with C18 silica and acidic alumina. Qualitative and quantitative detection for the target toxins were conducted under the multiple reaction monitoring (MRM) mode by using the positive electrospray ionization (ESI) mode after chromatographic separation on a TSK-gel Amide-80 HILIC column with water and acetonitrile. Matrix-matched calibration was used to compensate for matrix effects. The established method was further validated by determining the linearity ( R ² ≥ 0.9900), average recovery (81.52-116.50%), sensitivity (limits of detection (LODs): 0.33-5.52 μg·kg -1 ; limits of quantitation (LOQs): 1.32-11.29 μg·kg -1 ) and precision (relative standard deviation (RSD) ≤ 19.10%). The application of this proposed approach to thirty shellfish samples proved its desirable performance and sufficient capability for simultaneous determination of multiclass PSP toxins in sea foods.

The Role of Carboxydothermus hydrogenoformans in the Conversion of Calcium Phosphate from Amorphous to Crystalline State

PubMed Central

Haddad, Mathieu; Vali, Hojatollah; Paquette, Jeanne; Guiot, Serge R.

2014-01-01

Two previously unknown modes of biomineralization observed in the presence of Carboxydothermus hydrogenoformans are presented. Following the addition of NaHCO3 and the formation of an amorphous calcium phosphate precipitate in a DSMZ medium inoculated with C. hydrogenoformans, two distinct crystalline solids were recovered after 15 and 30 days of incubation. The first of these solids occurred as micrometric clusters of blocky, angular crystals, which were associated with bacterial biofilm. The second solid occurred as 30–50 nm nanorods that were found scattered among the organic products of bacterial lysis. The biphasic mixture of solids was clearly dominated by the first phase. The X-ray diffractometry (XRD) peaks and Fourier transform infrared spectroscopy (FTIR) spectrum of this biphasic material consistently showed features characteristic of Mg-whitlockite. No organic content or protein could be identified by dissolving the solids. In both cases, the mode of biomineralization appears to be biologically induced rather than biologically controlled. Since Mg is known to be a strong inhibitor of the nucleation and growth of CaP, C. hydrogenoformans may act by providing sites that chelate Mg or form complexes with it, thus decreasing its activity as nucleation and crystal growth inhibitor. The synthesis of whitlockite and nano-HAP-like material by C. hydrogenoformans demonstrates the versatility of this organism also known for its ability to perform the water-gas shift reaction, and may have applications in bacterially mediated synthesis of CaP materials, as an environmentally friendly alternative process. PMID:24586811

Fine-particle pH for Beijing winter haze as inferred from different thermodynamic equilibrium models

NASA Astrophysics Data System (ADS)

Song, Shaojie; Gao, Meng; Xu, Weiqi; Shao, Jingyuan; Shi, Guoliang; Wang, Shuxiao; Wang, Yuxuan; Sun, Yele; McElroy, Michael B.

2018-05-01

pH is an important property of aerosol particles but is difficult to measure directly. Several studies have estimated the pH values for fine particles in northern China winter haze using thermodynamic models (i.e., E-AIM and ISORROPIA) and ambient measurements. The reported pH values differ widely, ranging from close to 0 (highly acidic) to as high as 7 (neutral). In order to understand the reason for this discrepancy, we calculated pH values using these models with different assumptions with regard to model inputs and particle phase states. We find that the large discrepancy is due primarily to differences in the model assumptions adopted in previous studies. Calculations using only aerosol-phase composition as inputs (i.e., reverse mode) are sensitive to the measurement errors of ionic species, and inferred pH values exhibit a bimodal distribution, with peaks between -2 and 2 and between 7 and 10, depending on whether anions or cations are in excess. Calculations using total (gas plus aerosol phase) measurements as inputs (i.e., forward mode) are affected much less by these measurement errors. In future studies, the reverse mode should be avoided whereas the forward mode should be used. Forward-mode calculations in this and previous studies collectively indicate a moderately acidic condition (pH from about 4 to about 5) for fine particles in northern China winter haze, indicating further that ammonia plays an important role in determining this property. The assumed particle phase state, either stable (solid plus liquid) or metastable (only liquid), does not significantly impact pH predictions. The unrealistic pH values of about 7 in a few previous studies (using the standard ISORROPIA model and stable state assumption) resulted from coding errors in the model, which have been identified and fixed in this study.

Determination of Three Organochlorine Pesticides in Aqueous Samples by Solid-Phase Extraction Based on Natural Nano Diatomite in Packed Syringe Coupled to Gas Chromatography-Mass Spectrometry.

PubMed

Taghani, Abdollah; Goudarzi, Nasser; Bagherian, Ghadamali; Chamjangali, Mansour Arab

2017-01-01

A rapid, simple, and sensitive technique is proposed based on a miniaturized solid-phase extraction method named mictroextraction in a packed syringe coupled with gas chromatography-mass spectrometry for the preconcentration and determination of three organochlorine pesticides. These include hexachlorobenzene, heptachlor and aldrine in aqueous samples. For the first time, the natural nano diatomite is used a sorbent. Based on this technique, 6.0 mg of the nano sorbent is inserted in a syringe between two polypropylene frits. The analytes would be adsorbed on the solid phase, and would subsequently be eluted using organic solvents. The influence of some important parameters, such as the solution pH, type and volume of the organic desorption solvent, and amount of sorbent on the extraction efficiency of the selected pesticides, is investigated. The proposed method shows good linearity in the range of 0.1 - 40.0 μg L -1 , and at low limits of detection in the range of 0.02 - 0.13 μg L -1 using the selected ion-monitoring mode. The reproducibility of this method was found to be in the range of 3.5 - 11.1% for the understudied pesticides. In order to evaluate the matrix effect, the developed method is also applied to the preconcentration and determination of the selected pesticides in different water samples.

Two-dimensional numerical simulation of acoustic wave phase conjugation in magnetostrictive elastic media.

PubMed

Voinovich, Peter; Merlen, Alain

2005-12-01

The effect of parametric wave phase conjugation (WPC) in application to ultrasound or acoustic waves in magnetostrictive solids has been addressed numerically by Ben Khelil et al. [J. Acoust. Soc. Am. 109, 75-83 (2001)] using 1-D unsteady formulation. Here the numerical method presented by Voinovich et al. [Shock waves 13(3), 221-230 (2003)] extends the analysis to the 2-D effects. The employed model describes universally elastic solids and liquids. A source term similar to Ben Khelil et al.'s accounts for the coupling between deformation and magnetostriction due to external periodic magnetic field. The compatibility between the isotropic constitutive law of the medium and the model of magnetostriction has been considered. Supplementary to the 1-D simulations, the present model involves longitudinal/transversal mode conversion at the sample boundaries and separate magnetic field coupling with dilatation and shear stress. The influence of those factors in a 2-D geometry on the potential output of a magneto-elastic wave phase conjugator is analyzed in this paper. The process under study includes propagation of a wave burst of a given frequency from a point source in a liquid into the active solid, amplification of the waves due to parametric resonance, and formation of time-reversed waves, their radiation into liquid, and focusing. The considered subject is particularly important for ultrasonic applications in acoustic imaging, nondestructive testing, or medical diagnostics and therapy.

A multiphysics and multiscale model for low frequency electromagnetic direct-chill casting

NASA Astrophysics Data System (ADS)

Košnik, N.; Guštin, A. Z.; Mavrič, B.; Šarler, B.

2016-03-01

Simulation and control of macrosegregation, deformation and grain size in low frequency electromagnetic (EM) direct-chill casting (LFEMC) is important for downstream processing. Respectively, a multiphysics and multiscale model is developed for solution of Lorentz force, temperature, velocity, concentration, deformation and grain structure of LFEMC processed aluminum alloys, with focus on axisymmetric billets. The mixture equations with lever rule, linearized phase diagram, and stationary thermoelastic solid phase are assumed, together with EM induction equation for the field imposed by the coil. Explicit diffuse approximate meshless solution procedure [1] is used for solving the EM field, and the explicit local radial basis function collocation method [2] is used for solving the coupled transport phenomena and thermomechanics fields. Pressure-velocity coupling is performed by the fractional step method [3]. The point automata method with modified KGT model is used to estimate the grain structure [4] in a post-processing mode. Thermal, mechanical, EM and grain structure outcomes of the model are demonstrated. A systematic study of the complicated influences of the process parameters can be investigated by the model, including intensity and frequency of the electromagnetic field. The meshless solution framework, with the implemented simplest physical models, will be further extended by including more sophisticated microsegregation and grain structure models, as well as a more realistic solid and solid-liquid phase rheology.

Two-dimensional numerical simulation of acoustic wave phase conjugation in magnetostrictive elastic media

NASA Astrophysics Data System (ADS)

Voinovich, Peter; Merlen, Alain

2005-12-01

The effect of parametric wave phase conjugation (WPC) in application to ultrasound or acoustic waves in magnetostrictive solids has been addressed numerically by Ben Khelil et al. [J. Acoust. Soc. Am. 109, 75-83 (2001)] using 1-D unsteady formulation. Here the numerical method presented by Voinovich et al. [Shock waves 13(3), 221-230 (2003)] extends the analysis to the 2-D effects. The employed model describes universally elastic solids and liquids. A source term similar to Ben Khelil et al.'s accounts for the coupling between deformation and magnetostriction due to external periodic magnetic field. The compatibility between the isotropic constitutive law of the medium and the model of magnetostriction has been considered. Supplementary to the 1-D simulations, the present model involves longitudinal/transversal mode conversion at the sample boundaries and separate magnetic field coupling with dilatation and shear stress. The influence of those factors in a 2-D geometry on the potential output of a magneto-elastic wave phase conjugator is analyzed in this paper. The process under study includes propagation of a wave burst of a given frequency from a point source in a liquid into the active solid, amplification of the waves due to parametric resonance, and formation of time-reversed waves, their radiation into liquid, and focusing. The considered subject is particularly important for ultrasonic applications in acoustic imaging, nondestructive testing, or medical diagnostics and therapy.

Oscillatory fluid flow in deformable tubes: Implications for pore-scale hydromechanics from comparing experimental observations with theoretical predictions.

PubMed

Kurzeja, Patrick; Steeb, Holger; Strutz, Marc A; Renner, Jörg

2016-12-01

Oscillatory flow of four fluids (air, water, two aqueous sodium-tungstate solutions) was excited at frequencies up to 250 Hz in tubes of two materials (steel, silicone) covering a wide range in length, diameter, and thickness. The hydrodynamical response was characterized by phase shift and amplitude ratio between pressures in an upstream (pressure excitation) and a downstream reservoir connected by the tubes. The resulting standing flow waves reflect viscosity-controlled diffusive behavior and inertia-controlled wave behavior for oscillation frequencies relatively low and high compared to Biot's critical frequency, respectively. Rigid-tube theories correspond well with the experimental results for steel tubes filled with air or water. The wave modes observed for silicone tubes filled with the rather incompressible liquids or air, however, require accounting for the solid's shear and bulk modulus to correctly predict speed of pressure propagation and deformation mode. The shear mode may be responsible for significant macroscopic attenuation in porous materials with effective frame-shear moduli lower than the bulk modulus of the pore fluid. Despite notable effects of the ratio of densities and of acoustic and shear velocity of fluid and solid, Biot's frequency remains an approximate indicator of the transition from the viscosity to the inertia controlled regime.

Interface wave propagation and edge conversion at a low stiffness interphase layer between two solids: A numerical study.

PubMed

Cho, Hideo; Rokhlin, Stanislav I

2015-09-01

The Rayleigh-to-interface wave conversion and the propagation of the resulting symmetric and antisymmetric modes on a bonded interface between solids is analyzed by the two dimensional finite difference time domain method. The propagated patterns were visualized to improve understanding of the phenomena. It is found that the partition of the energy of the interface waves above and below the interface changes repeatedly with propagation distance due to interference between the two modes which have slightly different phase velocities. The destructive interference of those two modes results in dips in the amplitude spectrum of the interface waves, which shift in frequency with propagation distance. The Rayleigh wave received that is created by the interface wave at the exit corner of the joint also shows interference dips in its spectrum. Those dips depend on the interface properties and can potentially be used for interface characterization. Conversion factors related to the interface wave at the upward and downward corners are determined and discussed. As a result, the total transition factor through the upward and downward corners for the interface wave was estimated as 0.37 and would be sufficiently large to probe the interface by coupling from the Rayleigh to the interface wave. Copyright © 2015 Elsevier B.V. All rights reserved.

Solid motor diagnostic instrumentation. [design of self-contained instrumentation

NASA Technical Reports Server (NTRS)

Nakamura, Y.; Arens, W. E.; Wuest, W. S.

1973-01-01

A review of typical surveillance and monitoring practices followed during the flight phases of representative solid-propellant upper stages and apogee motors was conducted to evaluate the need for improved flight diagnostic instrumentation on future spacecraft. The capabilities of the flight instrumentation package were limited to the detection of whether or not the solid motor was the cause of failure and to the identification of probable primary failure modes. Conceptual designs of self-contained flight instrumentation packages capable of meeting these reqirements were generated and their performance, typical cost, and unit characteristics determined. Comparisons of a continuous real time and a thresholded hybrid design were made on the basis of performance, mass, power, cost, and expected life. The results of this analysis substantiated the feasibility of a self-contained independent flight instrumentation module as well as the existence of performance margins by which to exploit growth option applications.

Determination of nucleoside analog mono-, di-, and tri-phosphates in cellular matrix by solid phase extraction and ultra-sensitive LC-MS/MS detection.

PubMed

Bushman, Lane R; Kiser, Jennifer J; Rower, Joseph E; Klein, Brandon; Zheng, Jia-Hua; Ray, Michelle L; Anderson, Peter L

2011-09-10

An ultra-sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) assay was developed and validated to facilitate the assessment of clinical pharmacokinetics of nucleotide analogs from lysed intracellular matrix. The method utilized a strong anion exchange isolation of mono-(MP), di-(DP), and tri-phosphates (TP) from intracellular matrix. Each fraction was then dephosphorylated to the parent moiety yielding a molar equivalent to the original nucleotide analog intracellular concentration. The analytical portion of the methodology was optimized in specific nucleoside analog centric modes (i.e. tenofovir (TFV) centric, zidovudine (ZDV) centric), which included desalting/concentration by solid phase extraction and detection by LC-MS/MS. Nucleotide analog MP-, DP-, and TP-determined on the TFV centric mode of analysis include TFV, lamivudine (3TC), and emtricitibine (FTC). The quantifiable linear range for TFV was 2.5-2000 fmol/sample, and that for 3TC/FTC was 0.1 200 pmol/sample. Nucleoside analog MP-, DP-, and TP-determined on the ZDV centric mode of analysis included 3TC and ZDV. The quantifiable linear range for 3TC was 0.1 100 pmol/sample, and 5-2000 fmol/sample for ZDV. Stable labeled isotopic internal standards facilitated accuracy and precision in alternative cell matrices, which supported the intended use of the method for MP, DP, and TP determinations in various cell types. The method was successfully applied to clinical research samples generating novel intracellular information for TFV, FTC, ZDV, and 3TC nucleotides. This document outlines method development, validation, and application to clinical research. Copyright © 2011 Elsevier B.V. All rights reserved.

Applicability of solid-phase microextraction combined with gas chromatography atomic emission detection (GC-MIP AED) for the determination of butyltin compounds in sediment samples.

PubMed

Carpinteiro, J; Rodríguez, I; Cela, R

2004-11-01

The performance of solid-phase microextraction (SPME) applied to the determination of butyltin compounds in sediment samples is systematically evaluated. Matrix effects and influence of blank signals on the detection limits of the method are studied in detail. The interval of linear response is also evaluated in order to assess the applicability of the method to sediments polluted with butyltin compounds over a large range of concentrations. Advantages and drawbacks of including an SPME step, instead of the classic liquid-liquid extraction of the derivatized analytes, in the determination of butyltin compounds in sediment samples are considered in terms of achieved detection limits and experimental effort. Analytes were extracted from the samples by sonication using glacial acetic acid. An aliquot of the centrifuged extract was placed on a vial where compounds were ethylated and concentrated on a PDMS fiber using the headspace mode. Determinations were carried out using GC-MIP AED.

[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.

Determination of 17 kinds of banned organochlorine pesticides in water by activated carbon fiber-solid phase microextraction coupled with GC-MS.

PubMed

Sun, Tonghua; Jia, Jinping; Zhong, Dengjie; Wang, Yalin

2006-02-01

Activated carbon fiber (ACF) as extraction fiber for solid-phase microextraction (SPME) and its application for the analysis of banned organochlorine pesticides (OCPs) were investigated. Firstly, ACF was activated by different concentration of zinc chloride, which indicated that ACF activated by 60% zinc chloride had a reasonable specific surface area, pore volume and pore distribution. Secondly, the parameters for the ACF-SPME procedure, the adsorption and desorption conditions, were also optimized when coupled with gas chromatography-mass spectrometry (GC-MS). Thirdly, the ACF-SPME was used to analyze 17 kinds of OCPs in water. The linearity of most pesticides was found to be between 0.2 and 50 microg/l with GC-MS under the selected ion monitoring (SIM) acquisition mode. The limits of detection (LOD) at the sub microg/l were obtained. The work demonstrated here shows that ACF is a promising alternative for the SPME procedure.

[Determination of azoxystrobin residues in fruits and vegetables by gas chromatography/mass spectrometry with solid-phase extraction].

PubMed

Bo, Haibo

2007-11-01

A method was developed for the determination of azoxystrobin residues in fruits and vegetables by gas chromatography/mass spectrometry (GC/MS). Azoxystrobin residues were extracted with ethyl acetate-cyclohexane (1 : 1, v/v) by ultrasonication and then they were cleaned up on a silica solid-phase extraction (SPE) column to obtain an extract suitable for analysis by GC/MS in the selective ion monitoring (SIM) mode (the selected ion: m/z 344, 372, 388 and 403). The calibration curves were linear between area and concentration of azoxystrobin from 0.01 to 1.0 mg/kg with the correlation coefficient greater than 0.99. The average recoveries from spiked fruit and vegetable matrixes at three concentrations of 0.01, 0.1, 1.0 mg/kg ranged from 85.2% to 98.2% with relative standard deviation less than 21.5%. The limit of detection was 0.01 mg/kg and the limit of quantity was 0.05 mg/kg in fruit and vegetable matrixes, respectively.

An improved dispersive solid-phase extraction clean-up method for the gas chromatography-negative chemical ionisation tandem mass spectrometric determination of multiclass pesticide residues in edible oils.

PubMed

Deme, Pragney; Azmeera, Tirupathi; Prabhavathi Devi, B L A; Jonnalagadda, Padmaja R; Prasad, R B N; Vijaya Sarathi, U V R

2014-01-01

An improved sample preparation using dispersive solid-phase extraction clean-up was proposed for the trace level determination of 35 multiclass pesticide residues (organochlorine, organophosphorus and synthetic pyrethroids) in edible oils. Quantification of the analytes was carried out by gas chromatography-mass spectrometry in negative chemical ionisation mode (GC-NCI-MS/MS). The limit of detection and limit of quantification of residues were in the range of 0.01-1ng/g and 0.05-2ng/g, respectively. The analytes showed recoveries between 62% and 110%, and the matrix effect was observed to be less than 25% for most of the pesticides. Crude edible oil samples showed endosulfan isomers, p,p'-DDD, α-cypermethrin, chlorpyrifos, and diazinon residues in the range of 0.56-2.14ng/g. However, no pesticide residues in the detection range of the method were observed in refined oils. Copyright © 2013 Elsevier Ltd. All rights reserved.

Trapped-mode-induced Fano resonance and acoustical transparency in a one-dimensional solid-fluid phononic crystal

NASA Astrophysics Data System (ADS)

Quotane, Ilyasse; El Boudouti, El Houssaine; Djafari-Rouhani, Bahram

2018-01-01

We investigate theoretically and numerically the possibility of existence of Fano and acoustic-induced transparency (AIT) resonances in a simple though realistic one-dimensional acoustic structure made of solid-fluid layers inserted between two fluids. These resonances are obtained by combining appropriately the zeros of transmission (antiresonance) induced by the solid layers and the local resonances induced by the solid or combined solid-fluid layers with surface free boundary conditions. In particular, we show the possibility of trapped modes, also called bound states in continuum, which have recently found a high renewal interest. These modes appear as resonances with zero width in the transmission spectra as well as in the density of states (DOS). We consider three different structures: (i) a single solid layer inserted between two fluids. This simple structure shows the possibility of existence of trapped modes, which are discrete modes of the solid layer that lie in the continuum modes of the surrounding fluids. We give explicit analytical expressions of the dispersion relation of these eigenmodes of the solid layer which are found independent of the nature of the surrounding fluids. By slightly detuning the angle of incidence from that associated to the trapped mode, we get a well-defined Fano resonance characterized by an asymmetric Fano profile in the transmission spectra. (ii) The second structure consists of a solid-fluid-solid triple layer embedded between two fluids. This structure is found more appropriate to show both Fano and acoustic-induced transparency resonances. We provide detailed analytical expressions for the transmission and reflection coefficients that enable us to deduce a closed-form expression of the dispersion relation giving the trapped modes. Two situations can be distinguished in the triple-layer system: in the case of a symmetric structure (i.e., the same solid layers) we show, by detuning the incidence angle θ , the possibility of existence of Fano resonances that can be fitted following a Fano-type expression. The variation of the Fano parameter that describes the asymmetry of such resonances as well as their width versus θ is studied in detail. In the case of an asymmetric structure (i.e., different solid layers), we show the existence of an incidence angle that enables to squeeze a resonance between two transmission zeros induced by the two solid layers. This resonance behaves like an AIT resonance, its position and width depend on the nature of the fluid and solid layers as well as on the difference between the thicknesses of the solid layers. (iii) In the case of a periodic structure (phononic crystal), we show that trapped modes and Fano resonances give rise, respectively, to dispersionless flat bands with zero group velocity and nearly flat bands with negative or positive group velocities. The analytical results presented here are obtained by means of the Green's function method which enables to deduce in closed form: dispersion curves, transmission and reflection coefficients, DOS, as well as the displacement fields. The proposed solid-fluid layered structures should have important applications for designing acoustic mirrors and acoustic filters as well as supersonic and subsonic materials.

Enhanced bioethanol production by fed-batch simultaneous saccharification and co-fermentation at high solid loading of Fenton reaction and sodium hydroxide sequentially pretreated sugarcane bagasse.

PubMed

Zhang, Teng; Zhu, Ming-Jun

2017-04-01

A study on the fed-batch simultaneous saccharification and co-fermentation (SSCF) of Fenton reaction combined with NaOH pretreated sugarcane bagasse (SCB) at a high solid loading of 10-30% (w/v) was investigated. Enzyme feeding mode, substrate feeding mode and combination of both were compared with the batch mode under respective solid loadings. Ethanol concentrations of above 80g/L were obtained in batch and enzyme feeding modes at a solid loading of 30% (w/v). Enzyme feeding mode was found to increase ethanol productivity and reduce enzyme loading to a value of 1.23g/L/h and 9FPU/g substrate, respectively. The present study provides an economically feasible process for high concentration bioethanol production. Copyright © 2017 Elsevier Ltd. All rights reserved.

Phase-field crystal modeling of heteroepitaxy and exotic modes of crystal nucleation

NASA Astrophysics Data System (ADS)

Podmaniczky, Frigyes; Tóth, Gyula I.; Tegze, György; Pusztai, Tamás; Gránásy, László

2017-01-01

We review recent advances made in modeling heteroepitaxy, two-step nucleation, and nucleation at the growth front within the framework of a simple dynamical density functional theory, the Phase-Field Crystal (PFC) model. The crystalline substrate is represented by spatially confined periodic potentials. We investigate the misfit dependence of the critical thickness in the StranskiKrastanov growth mode in isothermal studies. Apparently, the simulation results for stress release via the misfit dislocations fit better to the PeopleBean model than to the one by Matthews and Blakeslee. Next, we investigate structural aspects of two-step crystal nucleation at high undercoolings, where an amorphous precursor forms in the first stage. Finally, we present results for the formation of new grains at the solid-liquid interface at high supersaturations/supercoolings, a phenomenon termed Growth Front Nucleation (GFN). Results obtained with diffusive dynamics (applicable to colloids) and with a hydrodynamic extension of the PFC theory (HPFC, developed for simple liquids) will be compared. The HPFC simulations indicate two possible mechanisms for GFN.

Enhancing radiation tolerance by controlling defect mobility and migration pathways in multicomponent single-phase alloys

DOE PAGES

Lu, Chenyang; Niu, Liangliang; Chen, Nanjun; ...

2016-12-15

A grand challenge in material science is to understand the correlation between intrinsic properties and defect dynamics. Radiation tolerant materials are in great demand for safe operation and advancement of nuclear and aerospace systems. Unlike traditional approaches that rely on microstructural and nanoscale features to mitigate radiation damage, this study demonstrates enhancement of radiation tolerance with the suppression of void formation by two orders magnitude at elevated temperatures in equiatomic single-phase concentrated solid solution alloys, and more importantly, reveals its controlling mechanism through a detailed analysis of the depth distribution of defect clusters and an atomistic computer simulation. The enhancedmore » swelling resistance is attributed to the tailored interstitial defect cluster motion in the alloys from a long-range one-dimensional mode to a short-range three-dimensional mode, which leads to enhanced point defect recombination. Finally, the results suggest design criteria for next generation radiation tolerant structural alloys.« less

β-Na2TeO4: Phase Transition from an Orthorhombic to a Monoclinic Form. Reversible CO2 Capture.

PubMed

Galven, Cyrille; Pagnier, Thierry; Rosman, Noël; Le Berre, Françoise; Crosnier-Lopez, Marie-Pierre

2018-06-18

The present work concerns the tellurate Na 2 TeO 4 which has a 1D structure and could then present a CO 2 capture ability. It has been synthesized in a powder form via a solid-state reaction and structurally characterized by thermal X-ray diffraction experiments, Raman spectroscopy, and differential scanning calorimetry. The room temperature structure corresponds to the β-Na 2 TeO 4 orthorhombic form, and we show that it undergoes a reversible structural transition near 420 °C toward a monoclinic system. Ab initio computations were also performed on the room temperature structure, the Raman vibration modes calculated, and a normal mode attribution proposed. In agreement with our expectations, this sodium oxide is able to trap CO 2 by a two-step mechanism: Na + /H + exchange and carbonation of the released sodium as NaHCO 3 . This capture is reversible since CO 2 can be released upon heating by recombination of the mother phase.

Optical Absorption and Raman Spectroscopy of Multiple Shocked Liquid Benzene to 10 GPa

NASA Astrophysics Data System (ADS)

Root, S.

2005-07-01

Liquid benzene samples were multiply shocked to peak pressures ranging from 3 GPa to 10 GPa to examine physical and chemical changes in benzene. A xenon flashlamp was used to probe the visible spectrum of benzene for loses in transmitted light intensity caused by changes in the electronic structure (absorption) or a possible liquid to solid phase transition (scattering). Raman spectroscopy was used to corroborate transmission measurements by examining changes in the benzene vibrational modes. The C-C symmetric ring breathing mode (992 cm-1), C-H symmetric stretch (3061 cm-1), along with several weaker modes at 607 cm-1, 1178 cm-1, 1586 cm-1, and 1606 cm-1 were monitored during shock loading. An EOS was developed to calculate the temperature of the shock compressed benzene. The present work has demonstrated that liquid benzene remains unchanged during multiple shock loading up to 10 GPa. Work supported by ONR and DOE.

Topologically protected edge states for out-of-plane and in-plane bulk elastic waves.

PubMed

Huo, Shao-Yong; Chen, Jiu-Jiu; Huang, Hong-Bo

2018-04-11

Topological phononic insulators (TPnIs) show promise for application in the manipulation of acoustic waves for the design of low-loss transmission and perfectly integrated communication devices. Since solid phononic crystals exist as a transverse polarization mode and a mixed longitudinal-transverse polarization mode, the realization of topological edge states for both out-of-plane and in-plane bulk elastic waves is desirable to enhance the controllability of the edge waves in solid systems. In this paper, a two-dimensional (2D) solid/solid hexagonal-latticed phononic system that simultaneously supports the topologically protected edge states for out-of-plane and in-plane bulk elastic waves is investigated. Firstly, two pairs of two-fold Dirac cones, respectively corresponding to the out-of-plane and in-plane waves, are obtained at the same frequency by tuning the crystal parameters. Then, a strategy of zone folding is invoked to form double Dirac cones. By shrinking and expanding the steel scatterer, the lattice symmetry is broken, and band inversions induced, giving rise to an intriguing topological phase transition. Finally, the topologically protected edge states for both out-of-plane and in-plane bulk elastic waves, which can be simultaneously located at the frequency range from 1.223 to 1.251 MHz, are numerically observed. Robust pseudospin-dependent elastic edge wave propagation along arbitrary paths is further demonstrated. Our results will significantly broaden its practical application in the engineering field.

Topologically protected edge states for out-of-plane and in-plane bulk elastic waves

NASA Astrophysics Data System (ADS)

Huo, Shao-Yong; Chen, Jiu-Jiu; Huang, Hong-Bo

2018-04-01

Topological phononic insulators (TPnIs) show promise for application in the manipulation of acoustic waves for the design of low-loss transmission and perfectly integrated communication devices. Since solid phononic crystals exist as a transverse polarization mode and a mixed longitudinal-transverse polarization mode, the realization of topological edge states for both out-of-plane and in-plane bulk elastic waves is desirable to enhance the controllability of the edge waves in solid systems. In this paper, a two-dimensional (2D) solid/solid hexagonal-latticed phononic system that simultaneously supports the topologically protected edge states for out-of-plane and in-plane bulk elastic waves is investigated. Firstly, two pairs of two-fold Dirac cones, respectively corresponding to the out-of-plane and in-plane waves, are obtained at the same frequency by tuning the crystal parameters. Then, a strategy of zone folding is invoked to form double Dirac cones. By shrinking and expanding the steel scatterer, the lattice symmetry is broken, and band inversions induced, giving rise to an intriguing topological phase transition. Finally, the topologically protected edge states for both out-of-plane and in-plane bulk elastic waves, which can be simultaneously located at the frequency range from 1.223 to 1.251 MHz, are numerically observed. Robust pseudospin-dependent elastic edge wave propagation along arbitrary paths is further demonstrated. Our results will significantly broaden its practical application in the engineering field.

High average power diode pumped solid state laser

NASA Astrophysics Data System (ADS)

Gao, Yue; Wang, Yanjie; Chan, Amy; Dawson, Murray; Greene, Ben

2017-03-01

A new generation of high average power pulsed multi-joule solid state laser system has been developed at EOS Space Systems for various space related tracking applications. It is a completely diode pumped, fully automated multi-stage system consisting of a pulsed single longitudinal mode oscillator, three stages of pre-amplifiers, two stages of power amplifiers, completely sealed phase conjugate mirror or stimulated Brillouin scattering (SBS) cell and imaging relay optics with spatial filters in vacuum cells. It is capable of generating pulse energy up to 4.7 J, a beam quality M 2 ~ 3, pulse width between 10-20 ns, and a pulse repetition rate between 100-200 Hz. The system has been in service for more than two years with excellent performance and reliability.

Why solid oxide cells can be reversibly operated in solid oxide electrolysis cell and fuel cell modes?

PubMed

Chen, Kongfa; Liu, Shu-Sheng; Ai, Na; Koyama, Michihisa; Jiang, San Ping

2015-12-14

High temperature solid oxide cells (SOCs) are attractive for storage and regeneration of renewable energy by operating reversibly in solid oxide electrolysis cell (SOEC) and solid oxide fuel cell (SOFC) modes. However, the stability of SOCs, particularly the deterioration of the performance of oxygen electrodes in the SOEC operation mode, is the most critical issue in the development of high performance and durable SOCs. In this study, we investigate in detail the electrochemical activity and stability of La0.8Sr0.2MnO3 (LSM) oxygen electrodes in cyclic SOEC and SOFC modes. The results show that the deterioration of LSM oxygen electrodes caused by anodic polarization can be partially or completely recovered by subsequent cathodic polarization. Using in situ assembled LSM electrodes without pre-sintering, we demonstrate that the deteriorated LSM/YSZ interface can be repaired and regenerated by operating the cells under cathodic polarization conditions. This study for the first time establishes the foundation for the development of truly reversible and stable SOCs for hydrogen fuel production and electricity generation in cyclic SOEC and SOFC operation modes.

Rapid determination of six carcinogenic primary aromatic amines in mainstream cigarette smoke by two-dimensional online solid phase extraction combined with liquid chromatography tandem mass spectrometry.

PubMed

Bie, Zhenying; Lu, Wei; Zhu, You; Chen, Yusong; Ren, Hubo; Ji, Lishun

2017-01-27

A fully automated, rapid, and reliable method for simultaneous determination of six carcinogenic primary aromatic amines (AAs), including o-toluidine (o-TOL), 2, 6-dimethylaniline (2, 6-DMA), o-anisidine (o-ASD), 1-naphthylamine (1-ANP), 2-naphthylamine (2-ANP), and 4-aminobiphenyl (4-ABP), in mainstream cigarette smoke was established. The proposed method was based on two-dimensional online solid phase extraction combined with liquid chromatography tandem mass spectrometry (SPE/LC-MS/MS). The particulate phase of the mainstream cigarette smoke was collected on a Cambridge filter pad and pretreated via ultrasonic extraction with 2% formic acid (FA), while the gas phase was trapped by 2% FA without pretreatment for determination. The two-dimensional online SPE comprised of two cartridges with different absorption characteristics was applied for sample pretreatment. Analysis was performed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) under multiple reaction monitoring mode. Each sample required about 0.5h for solid phase extraction and analysis. The limit of detections (LODs) for six AAs ranged from 0.04 to 0.58ng/cig and recoveries were within 84.5%-122.9%. The relative standard deviations of intra- and inter-day tests for 3R4F reference cigarette were less than 6% and 7%, respectively, while no more than 7% and 8% separately for a type of Virginia cigarette. The proposed method enabled minimum sample pretreatment, full automation, and high throughput with high selectivity, sensitivity, and accuracy. As a part of the validation procedure, fifteen brands of cigarettes were tested by the designed method. Copyright © 2016 Elsevier B.V. All rights reserved.

Superfluid--Solid Quantum Phase Transitions and Landau-Ginzburg-Wilson Paradigm

NASA Astrophysics Data System (ADS)

Kuklov, A. B.; Prokof'ev, N. V.

2005-03-01

We study superfluid (SF)--solid zero-temperature transitions in 2d lattice boson/spin models by Worm-Algorithm Monte Carlo simulations. The SF -- Valence Bond Solid (VBS) transition was recently argued to be generically of II order in violation of the Ginzburg-Landau- Wilson (GLW) paradigm [1]. We simulate the J-current model on lattices up to 64x64x64, and observe that SF- columnar VBS and SF-checkerboard solid transitions are typically weak I-order ones and in small systems they may be confused with the continuous or high-symmetry points [2]. Thus, in the simulated model, the SF-VBS transition proceeds in agreement with the GLW paradigm. We explain this by dominance of standard particle and hole excitations, as opposed to fractionalized (spinon) excitations [1]. We developed a technique based on tunneling events (instantons) in the insulating phase which reveals charges of the revelant long-wave modes. While in 1d systems spinons are clearly seen in tunneling events, in two spatial dimensions tunneling is solely controlled by particles and holes in our system. This work is supported by NSF grant ITR-405460001 and PSC-CUNY- 665560035. [1] T. Senthil, A. Vishwanath, L. Balents, S. Sachdev, and M.P.A. Fisher, Science 303, 1490 (2004); [2] A.B. Kuklov, N.V. Prokof'ev, B.V. Svistunov, condmat/0406061; PRL, to be published.

Cold-induced aqueous acetonitrile phase separation: A salt-free way to begin quick, easy, cheap, effective, rugged, safe.

PubMed

Shao, Gang; Agar, Jeffrey; Giese, Roger W

2017-07-14

Cooling a 1:1 (v/v) solution of acetonitrile and water at -16° C is known to result in two clear phases. We will refer to this event as "cold-induced aqueous acetonitrile phase separation (CIPS)". On a molar basis, acetonitrile is 71.7% and 13.6% in the upper and lower phases, respectively, in our study. The phase separation proceeds as a descending cloud of microdroplets. At the convenient temperature (typical freezer) employed here the lower phase is rather resistant to solidification, although it emerges from the freezer as a solid if various insoluble matter is present at the outset. In a preliminary way, we replaced the initial (salting-out) step of a representative QuEChERS procedure with CIPS, applying this modified procedure ("CIPS-QuEChERS") to a homogenate of salmon (and partly to beef). Three phases resulted, where only the upper, acetonitrile-rich phase is a liquid (that is completely clear). The middle phase comprises ice and precipitated lipids, while the lower phase is the residual matrix of undissolved salmon or meat. Treating the upper phase from salmon, after isolation, with anhydrous MgSO 4 and C18-Si (typical QuEChERS dispersive solid phase extraction sorbents), and injecting into a GC-MS in a nontargeted mode, gives two-fold more preliminary hits for chemicals, and also number of spiked pesticides recovered, relative to that from a comparable QuEChERS method. In part, this is because of much higher background signals in the latter case. Further study of CIPS-QuEChERS is encouraged, including taking advantage of other QuERChERS conditions. Copyright © 2017 Elsevier B.V. All rights reserved.

Dispersive solid-phase extraction followed by high-performance liquid chromatography/tandem mass spectrometry for the determination of ricinine in cooking oil.

PubMed

Cai, Meiqiang; Chen, Xiaohong; Wei, Xiaoqing; Pan, Shengdong; Zhao, Yonggang; Jin, Micong

2014-09-01

A rapid and accurate method by liquid chromatography/tandem mass spectrometry (LC-MS/MS) using positive electrospray was established for the determination of ricinine in cooking oils. The homogenized samples, spiked with (13)C6-labelled ricinine as an internal standard, were extracted using ethanol/water (20:80, v/v) and purified by dispersive solid-phase extraction (dSPE) using primary-secondary amine (PSA) and C18 as adsorbents. The extract was separated in a short C18 reversed-phase column using methanol/water (25:75, v/v) as the mobile phase and detected in multiple reaction monitoring (MRM) mode with the absolute matrix effect of 93.2-102.2%. The alkali-metal adduct ions were discussed and the mass/mass fragmentation pathway was explained. Ricinine showed good linearity in the range of 0.5-50.0 μg/kg with the limit of quantitation 0.5 μg/kg. The recoveries were between 86.0% and 98.3% with the intra- and inter-day RSDs of 2.6-7.0%, 5.5-10.8%, respectively. This method could be applied to the rapid quantification of ricinine in cooking oils. Crown Copyright © 2014. Published by Elsevier Ltd. All rights reserved.

Solid-gas phase equilibria and thermodynamic properties of cadmium selenide.

NASA Technical Reports Server (NTRS)

Sigai, A. G.; Wiedemeier, H.

1972-01-01

Accurate vapor pressures are determined through direct weight loss measurements using the Knudsen effusion technique. The experimental data are evaluated by establishing the mode of vaporization and determining the heat capacity of cadmium selenide at elevated temperatures. Additional information is obtained through a second- and third-law evaluation of data, namely, the heat of formation and the absolute entropy of cadmium selenide. A preferential loss of selenium during the initial heating of CdSe is observed, which leads to a deviation in stoichiometry.

Linear friction weld process monitoring of fixture cassette deformations using empirical mode decomposition

NASA Astrophysics Data System (ADS)

Bakker, O. J.; Gibson, C.; Wilson, P.; Lohse, N.; Popov, A. A.

2015-10-01

Due to its inherent advantages, linear friction welding is a solid-state joining process of increasing importance to the aerospace, automotive, medical and power generation equipment industries. Tangential oscillations and forge stroke during the burn-off phase of the joining process introduce essential dynamic forces, which can also be detrimental to the welding process. Since burn-off is a critical phase in the manufacturing stage, process monitoring is fundamental for quality and stability control purposes. This study aims to improve workholding stability through the analysis of fixture cassette deformations. Methods and procedures for process monitoring are developed and implemented in a fail-or-pass assessment system for fixture cassette deformations during the burn-off phase. Additionally, the de-noised signals are compared to results from previous production runs. The observed deformations as a consequence of the forces acting on the fixture cassette are measured directly during the welding process. Data on the linear friction-welding machine are acquired and de-noised using empirical mode decomposition, before the burn-off phase is extracted. This approach enables a direct, objective comparison of the signal features with trends from previous successful welds. The capacity of the whole process monitoring system is validated and demonstrated through the analysis of a large number of signals obtained from welding experiments.

[Simultaneous determination of 9 ultraviolet stabilizers in food plastic packaging materials by solid phase extraction-high performance liquid chromatography].

PubMed

Zhang, Juzhou; Li, Jing; Shao, Dongliang; Yao, Bangben; Jiang, Junshu

2012-02-01

An effective high performance liquid chromatographic (HPLC) method has been developed for the simultaneous determination of 9 ultraviolet stabilizers in food plastic packaging materials. The food packaging samples were firstly extracted by methanol-ethyl acetate, and then purified by a C18 solid-phase extraction (SPE) column. The target compounds were separated on a ZORBAX SB-C18 column (250 mm x 4.6 mm, 5 microm) in gradient elution mode using methanol and water as mobile phases. The detection wavelength was at 310 nm. The linear plots of the nine ultraviolet stabilizers were obtained between 0.2 and 10 mg/L, with the correlation coefficients of above 0. 999 for the nine ultraviolet stabilizers. The limits of detection for this method were in the range from 0.05 to 0.1 mg/L. The recoveries spiked in commercial food plastic packaging materials were in the range of 70.2% - 89.0% with the relative standard deviations of 0.4% - 4.5%. The results indicated that the method is simple, accurate, and suitable for the simultaneous determination of the nine ultraviolet stabilizers in food plastic packaging materials.

Simultaneous analysis of carotenoids and tocopherols in botanical species using one step solid-liquid extraction followed by high performance liquid chromatography.

PubMed

Valdivielso, Izaskun; Bustamante, María Ángeles; Ruiz de Gordoa, Juan Carlos; Nájera, Ana Isabel; de Renobales, Mertxe; Barron, Luis Javier R

2015-04-15

Carotenoids and tocopherols from botanical species abundant in Atlantic mountain grasslands were simultaneously extracted using one-step solid-liquid phase. A single n-hexane/2-propanol extract containing both types of compounds was injected twice under two different sets of HPLC conditions to separate the tocopherols by normal-phase chromatography and carotenoids by reverse-phase mode. The method allowed reproducible quantification in plant samples of very low amounts of α-, β-, γ- and δ-tocopherols (LOD from 0.0379 to 0.0720 μg g(-1) DM) and over 15 different xanthophylls and carotene isomers. The simplified one-step extraction without saponification significantly increased the recovery of tocopherols and carotenoids, thereby enabling the determination of α-tocopherol acetate in plant samples. The two different sets of chromatographic analysis provided near baseline separation of individual compounds without interference from other lipid compounds extracted from plants, and a very sensitive and accurate detection of tocopherols and carotenoids. The detection of minor individual components in botanical species from grasslands is nowadays of high interest in searching for biomarkers for foods derived from grazing animals. Copyright © 2014 Elsevier Ltd. All rights reserved.

Achromatic vector vortex beams from a glass cone

PubMed Central

Radwell, N.; Hawley, R. D.; Götte, J. B.; Franke-Arnold, S.

2016-01-01

The reflection of light is governed by the laws first described by Augustin-Jean Fresnel: on internal reflection, light acquires a phase shift, which depends on its polarization direction with respect to the plane of incidence. For a conical reflector, the cylindrical symmetry is echoed in an angular variation of this phase shift, allowing us to create light modes with phase and polarization singularities. Here we observe the phase and polarization profiles of light that is back reflected from a solid glass cone and, in the case of circular input light, discover that not only does the beam contain orbital angular momentum but can trivially be converted to a radially polarized beam. Importantly, the Fresnel coefficients are reasonably stable across the visible spectrum, which we demonstrate by measuring white light polarization profiles. This discovery provides a highly cost-effective technique for the generation of broadband orbital angular momentum and radially polarized beams. PMID:26861191

Prediction of binary nanoparticle superlattices from soft potentials

DOE PAGES

Horst, Nathan; Travesset, Alex

2016-01-07

Driven by the hypothesis that a sufficiently continuous short-ranged potential is able to account for shell flexibility and phonon modes and therefore provides a more realistic description of nanoparticle interactions than a hard sphere model, we compute the solid phase diagram of particles of different radii interacting with an inverse power law potential. From a pool of 24 candidate lattices, the free energy is optimized with respect to additional internal parameters and the p-exponent, determining the short-range properties of the potential, is varied between p = 12 and p = 6. The phase diagrams contain the phases found in ongoingmore » self-assembly experiments, including DNA programmable self-assembly and nanoparticles with capping ligands assembled by evaporation from an organic solvent. Thus, the resulting phase diagrams can be mapped quantitatively to existing experiments as a function of only two parameters: Nanoparticle radius ratio (γ) and softness asymmetry.« less

Prediction of Binary Nanoparticle Superlattices from Soft Potentials

NASA Astrophysics Data System (ADS)

Horst, Nathan; Travesset, Alex

Driven by the hypothesis that a sufficiently continuous short-ranged potential is able to account for shell flexibility and phonon modes and therefore provides a more realistic description of nanoparticle interactions than a hard sphere model, we compute the solid phase diagram of particles of different radii interacting with an inverse power law potential. We explore 24 candidate lattices where the p-exponent, determining the short-range properties of the potential, is varied between p=12 and p=6, and optimize the free energy with respect to additional internal parameters. The phase diagrams contain the phases found in ongoing self-assembly experiments, including DNA programmable self-assembly and nanoparticles with capping ligands assembled by evaporation from an organic solvent. The resulting phase diagrams can be mapped quantitatively to existing experiments as a function of only two parameters: nanoparticle radius ratio (γ) and softness asymmetry (SA). Supported by DOE under Contract Number DE-AC02-07CH11358.

Prediction of binary nanoparticle superlattices from soft potentials

NASA Astrophysics Data System (ADS)

Horst, Nathan; Travesset, Alex

2016-01-01

Driven by the hypothesis that a sufficiently continuous short-ranged potential is able to account for shell flexibility and phonon modes and therefore provides a more realistic description of nanoparticle interactions than a hard sphere model, we compute the solid phase diagram of particles of different radii interacting with an inverse power law potential. From a pool of 24 candidate lattices, the free energy is optimized with respect to additional internal parameters and the p-exponent, determining the short-range properties of the potential, is varied between p = 12 and p = 6. The phase diagrams contain the phases found in ongoing self-assembly experiments, including DNA programmable self-assembly and nanoparticles with capping ligands assembled by evaporation from an organic solvent. The resulting phase diagrams can be mapped quantitatively to existing experiments as a function of only two parameters: Nanoparticle radius ratio (γ) and softness asymmetry.

Achromatic vector vortex beams from a glass cone

NASA Astrophysics Data System (ADS)

Radwell, N.; Hawley, R. D.; Götte, J. B.; Franke-Arnold, S.

2016-02-01

The reflection of light is governed by the laws first described by Augustin-Jean Fresnel: on internal reflection, light acquires a phase shift, which depends on its polarization direction with respect to the plane of incidence. For a conical reflector, the cylindrical symmetry is echoed in an angular variation of this phase shift, allowing us to create light modes with phase and polarization singularities. Here we observe the phase and polarization profiles of light that is back reflected from a solid glass cone and, in the case of circular input light, discover that not only does the beam contain orbital angular momentum but can trivially be converted to a radially polarized beam. Importantly, the Fresnel coefficients are reasonably stable across the visible spectrum, which we demonstrate by measuring white light polarization profiles. This discovery provides a highly cost-effective technique for the generation of broadband orbital angular momentum and radially polarized beams.

Analytical modeling of localized surface plasmon resonance in heterostructure copper sulfide nanocrystals

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

Caldwell, Andrew H.; Ha, Don-Hyung; Ding, Xiaoyue

2014-10-28

Localized surface plasmon resonance (LSPR) in semiconductor nanocrystals is a relatively new field of investigation that promises greater tunability of plasmonic properties compared to metal nanoparticles. A novel process by which the LSPR in semiconductor nanocrystals can be altered is through heterostructure formation arising from solution-based cation exchange. Herein, we describe the development of an analytical model of LSPR in heterostructure copper sulfide-zinc sulfide nanocrystals synthesized via a cation exchange reaction between copper sulfide (Cu 1.81S) nanocrystals and Zn ions. The cation exchange reaction produces dual-interface, heterostructure nanocrystals in which the geometry of the copper sulfide phase can be tunedmore » from a sphere to a thin disk separating symmetrically-grown sulfide (ZnS) grains. Drude model electronic conduction and Mie-Gans theory are applied to describe how the LSPR wavelength changes during cation exchange, taking into account the morphology evolution and changes to the local permittivity. The results of the modeling indicate that the presence of the ZnS grains has a significant effect on the out-of-plane LSPR mode. By comparing the results of the model to previous studies on solid-solid phase transformations of copper sulfide in these nanocrystals during cation exchange, we show that the carrier concentration is independent of the copper vacancy concentration dictated by its atomic phase. The evolution of the effective carrier concentration calculated from the model suggests that the out-of-plane resonance mode is dominant. The classical model was compared to a simplified quantum mechanical model which suggested that quantum mechanical effects become significant when the characteristic size is less than ~8 nm. Overall, we find that the analytical models are not accurate for these heterostructured semiconductor nanocrystals, indicating the need for new model development for this emerging field.« less

Analytical modeling of localized surface plasmon resonance in heterostructure copper sulfide nanocrystals

NASA Astrophysics Data System (ADS)

Caldwell, Andrew H.; Ha, Don-Hyung; Ding, Xiaoyue; Robinson, Richard D.

2014-10-01

Localized surface plasmon resonance (LSPR) in semiconductor nanocrystals is a relatively new field of investigation that promises greater tunability of plasmonic properties compared to metal nanoparticles. A novel process by which the LSPR in semiconductor nanocrystals can be altered is through heterostructure formation arising from solution-based cation exchange. Herein, we describe the development of an analytical model of LSPR in heterostructure copper sulfide-zinc sulfide nanocrystals synthesized via a cation exchange reaction between copper sulfide (Cu1.81S) nanocrystals and Zn ions. The cation exchange reaction produces dual-interface, heterostructure nanocrystals in which the geometry of the copper sulfide phase can be tuned from a sphere to a thin disk separating symmetrically-grown sulfide (ZnS) grains. Drude model electronic conduction and Mie-Gans theory are applied to describe how the LSPR wavelength changes during cation exchange, taking into account the morphology evolution and changes to the local permittivity. The results of the modeling indicate that the presence of the ZnS grains has a significant effect on the out-of-plane LSPR mode. By comparing the results of the model to previous studies on solid-solid phase transformations of copper sulfide in these nanocrystals during cation exchange, we show that the carrier concentration is independent of the copper vacancy concentration dictated by its atomic phase. The evolution of the effective carrier concentration calculated from the model suggests that the out-of-plane resonance mode is dominant. The classical model was compared to a simplified quantum mechanical model which suggested that quantum mechanical effects become significant when the characteristic size is less than ˜8 nm. Overall, we find that the analytical models are not accurate for these heterostructured semiconductor nanocrystals, indicating the need for new model development for this emerging field.

High-Resolution Infrared Spectrscopy of the Hydroxymethyl Radical in Solid Parahydrogen

NASA Astrophysics Data System (ADS)

Balabanoff, Morgan E.; Anderson, David T.

2016-06-01

Interest in the hydroxymethyl radical, CH2OH, stems primarily from its importance as a reaction intermediate. However, this radical is also of interest from a spectroscopic point of view with large amplitude COH torsional tunneling and out of plane CH2 wagging motions. The first IR detection of CH2OH was accomplished via matrix isolation spectroscopy over 40 years ago by Jacox. Reisler and co-workers detected CH2OH in the gas-phase using the sensitivity of double resonance ionization detected IR spectroscopy to probe the OH stretch, asymmetric CH stretch, and symmetric CH stretch vibrational modes with partial rotational resolution (0.4 wn). Most recently, the Nesbitt group published the first fully rotationally resolved IR spectrum of CH2OH via the Ka=0←0 band of the symmetric CH stretch. These researchers were able to unambiguously assign the identified transitions to a Watson A-reduced symmetric top Hamiltonian thereby producing improved values for the symmetric CH stretch rotational constants and vibrational band origin. However, in this same work the authors point out a number of remaining unresolved issues. Motivated by these gas-phase observations, we decided to return to the matrix isolation studies of CH2OH, however utilizing solid parahydrogen as a matrix host to improve upon the sensitivity and resolution of the previous matrix isolation studies. Based on our measurements, while the end-over-end rotation of the CH2OH radical is quenched, rotational motion around the a-axis is nearly free permitting both A-type and B-type transitions to be resolved. In the case of the OH stretch mode, both A-type and B-type transitions are observed with an energy difference that makes sense based on the gas-phase CH2OH rotational constants. However, for the symmetric CH stretch mode, the same mode recently assigned by Nesbitt and co-workers, two absorption features are also observed but the energy difference and intensities of the two features do not match predictions based on the rotational constants. M.E. Jacox, D.E. Milligan, J. Mol. Spec. 47, 148-162 (1973) L. Feng, J. Wei, H. Reisler, J. Phys. Chem. A 108, 7903-7908 (2004). M.A. Roberts, E.N. Sharp-Williams, D.J. Nesbitt, J. Phys. Chem. A 117, 7042-7049 (2013).

Mixed-mode isolation of triazine metabolites from soil and aquifer sediments using automated solid-phase extraction

USGS Publications Warehouse

Mills, M.S.; Thurman, E.M.

1992-01-01

Reversed-phase isolation and ion-exchange purification were combined in the automated solid-phase extraction of two polar s-triazine metabolites, 2-amino-4-chloro-6-(isopropylamino)-s-triazine (deethylatrazine) and 2-amino-4-chloro-6-(ethylamino)-s-triazine (deisopropylatrazine) from clay-loam and slit-loam soils and sandy aquifer sediments. First, methanol/ water (4/1, v/v) soil extracts were transferred to an automated workstation following evaporation of the methanol phase for the rapid reversed-phase isolation of the metabolites on an octadecylresin (C18). The retention of the triazine metabolites on C18 decreased substantially when trace methanol concentrations (1%) remained. Furthermore, the retention on C18 increased with decreasing aqueous solubility and increasing alkyl-chain length of the metabolites and parent herbicides, indicating a reversed-phase interaction. The analytes were eluted with ethyl acetate, which left much of the soil organic-matter impurities on the resin. Second, the small-volume organic eluate was purified on an anion-exchange resin (0.5 mL/min) to extract the remaining soil pigments that could foul the ion source of the GC/MS system. Recoveries of the analytes were 75%, using deuterated atrazine as a surrogate, and were comparable to recoveries by soxhlet extraction. The detection limit was 0.1 ??g/kg with a coefficient of variation of 15%. The ease and efficiency of this automated method makes it viable, practical technique for studying triazine metabolites in the environment.

An optoelectronic framework enabled by low-dimensional phase-change films.

PubMed

Hosseini, Peiman; Wright, C David; Bhaskaran, Harish

2014-07-10

The development of materials whose refractive index can be optically transformed as desired, such as chalcogenide-based phase-change materials, has revolutionized the media and data storage industries by providing inexpensive, high-speed, portable and reliable platforms able to store vast quantities of data. Phase-change materials switch between two solid states--amorphous and crystalline--in response to a stimulus, such as heat, with an associated change in the physical properties of the material, including optical absorption, electrical conductance and Young's modulus. The initial applications of these materials (particularly the germanium antimony tellurium alloy Ge2Sb2Te5) exploited the reversible change in their optical properties in rewritable optical data storage technologies. More recently, the change in their electrical conductivity has also been extensively studied in the development of non-volatile phase-change memories. Here we show that by combining the optical and electronic property modulation of such materials, display and data visualization applications that go beyond data storage can be created. Using extremely thin phase-change materials and transparent conductors, we demonstrate electrically induced stable colour changes in both reflective and semi-transparent modes. Further, we show how a pixelated approach can be used in displays on both rigid and flexible films. This optoelectronic framework using low-dimensional phase-change materials has many likely applications, such as ultrafast, entirely solid-state displays with nanometre-scale pixels, semi-transparent 'smart' glasses, 'smart' contact lenses and artificial retina devices.

Aging Wire Insulation Assessment by Phase Spectrum Examination of Ultrasonic Guided Waves

NASA Technical Reports Server (NTRS)

Anastasi, Robert F.; Madaras, Eric I.

2003-01-01

Wire integrity has become an area of concern to the aerospace community including DoD, NASA, FAA, and Industry. Over time and changing environmental conditions, wire insulation can become brittle and crack. The cracks expose the wire conductor and can be a source of equipment failure, short circuits, smoke, and fire. The technique of using the ultrasonic phase spectrum to extract material properties of the insulation is being examined. Ultrasonic guided waves will propagate in both the wire conductor and insulation. Assuming the condition of the conductor remains constant then the stiffness of the insulator can be determined by measuring the ultrasonic guided wave velocity. In the phase spectrum method the guided wave velocity is obtained by transforming the time base waveform to the frequency domain and taking the phase difference between two waveforms. The result can then be correlated with a database, derived by numerical model calculations, to extract material properties of the wire insulator. Initial laboratory tests were performed on a simple model consisting of a solid cylinder and then a solid cylinder with a polymer coating. For each sample the flexural mode waveform was identified. That waveform was then transformed to the frequency domain and a phase spectrum was calculated from a pair of waveforms. Experimental results on the simple model compared well to numerical calculations. Further tests were conducted on aircraft or mil-spec wire samples, to see if changes in wire insulation stiffness can be extracted using the phase spectrum technique.

A Resonator for Low-Threshold Frequency Conversion

NASA Technical Reports Server (NTRS)

Iltchenko, Vladimir; Matsko, Andrey; Savchenkov, Anatoliy; Maleki, Lute

2004-01-01

A proposed toroidal or disklike dielectric optical resonator (dielectric optical cavity) would be made of an optically nonlinear material and would be optimized for use in parametric frequency conversion by imposition of a spatially periodic permanent electric polarization. The poling (see figure) would suppress dispersions caused by both the material and the geometry of the optical cavity, thereby effecting quasi-matching of the phases of high-resonance-quality (high-Q) whispering-gallery electromagnetic modes. The quasi-phase-matching of the modes would serve to maximize the interactions among them. Such a resonator might be a prototype of a family of compact, efficient nonlinear devices for operation over a broad range of optical wavelengths. A little background information is prerequisite to a meaningful description of this proposal: (1) Described in several prior NASA Tech Briefs articles, the whispering-gallery modes in a component of spheroidal, disklike, or toroidal shape are waveguide modes that propagate circumferentially and are concentrated in a narrow toroidal region centered on the equatorial plane and located near the outermost edge. (2) For the sake of completeness, it must be stated that even though optical resonators of the type considered here are solid dielectric objects and light is confined within them by total internal reflection at dielectric interfaces without need for mirrors, such components are sometimes traditionally called cavities because their effects upon the light propagating within them are similar to those of true cavities bounded by mirrors. (3) For a given set of electromagnetic modes interacting with each other in an optically nonlinear material (e.g., modes associated with the frequencies involved in a frequency-conversion scheme), the threshold power for oscillation depends on the mode volumes and the mode-overlap integral. (4) Whispering-gallery modes are attractive in nonlinear optics because they maximize the effects of nonlinearities by occupying small volumes and affording high Q values

Low-field nuclear magnetic resonance characterization of organic content in shales

USGS Publications Warehouse

Washburn, Kathryn E.; Birdwell, Justin E.; Seymour, Joseph D.; Kirkland, Catherine; Vogt, Sarah J.

2013-01-01

Low-field nuclear magnetic resonance (LF-NMR) relaxometry is a non-invasive technique commonly used to assess hydrogen-bearing fluids in petroleum reservoir rocks. Longitudinal T1 and transverse T2 relaxation time measurements made using LF-NMR on conventional reservoir systems provides information on rock porosity, pore size distributions, and fluid types and saturations in some cases. Recent improvements in LF-SNMR instrument electronics have made it possible to apply these methods to assess highly viscous and even solid organic phases within reservoir rocks. T1 and T2 relaxation responses behave very differently in solids and liquids, therefore the relationship between these two modes of relaxation can be used to differentiate organic phases in rock samples or to characterize extracted organic materials. Using T1-T2 correlation data, organic components present in shales, such as kerogen and bitumen, can be examined in laboratory relaxometry measurements. In addition, implementation of a solid-echo pulse sequence to refocus some types of T2 relaxation during correlation measurements allows for improved resolution of solid phase photons. LF-NMR measurements of T1 and T2 relaxation time correlations were carried out on raw oil shale samples from resources around the world. These shales vary widely in mineralogy, total organic carbon (TOC) content and kerogen type. NMR results were correlcated with Leco TOC and geochemical data obtained from Rock-Eval. There is excellent correlation between NMR data and programmed pyrolysis parameters, particularly TOC and S2, and predictive capability is also good. To better understand the NMR response, the 2D NMR spectra were compared to similar NMR measurements made using high-field (HF) NMR equipment.

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

PubMed Central

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

2017-01-01

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

Quantitative determination of chromium picolinate in animal feeds by solid phase extraction and liquid chromatography-tandem mass spectrometry.

PubMed

Han, Miaomiao; Tian, Ying; Li, Zhen; Chen, Yiqiang; Yang, Wenjun; Zhang, Liying

2017-12-01

Chromium picolinate is one of the important Cr 3+ resources and is widely used in animal production. A convenient, reliable and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantitative determination of chromium picolinate in animal feeds. Feed samples were extracted with acetonitrile and subsequently cleaned up by solid phase extraction cartridges Supelclean™ LC-18. Chromium picolinate was efficiently separated with a Waters ACQUITY UPLC ® BEH C18 column, ionized with electrospray ion source in positive mode (ESI + ), and quantitatively determined by tandem mass spectrometry in multiple reaction monitoring mode. Standard calibration curve of chromium picolinate in the concentration range from 0.5 to 1000ng/mL was obtained with good linearity correlation coefficient (R 2 =0.9982). Average recoveries ranged from 95.37%∼105.54%, as detected by spiking 0.02∼640mg/kg of chromium picolinate in complete feed, concentrated feed and premix. Intra-day and inter-day coefficient of variation were 0.59%∼6.67% and 2.36%∼6.97%, respectively. The limits of quantitation were 0.02mg/kg, 0.025mg/kg, and 2mg/kg for complete feed, concentrated feed, and premix, respectively. Actual sample analysis indicated that the developed method can be an effective tool to monitoring CrPic content in animal feed. Copyright © 2017. Published by Elsevier B.V.

Baseline toxicity of a chlorobenzene mixture and total body residues measured and estimated with solid-phase microextraction.

PubMed

Leslie, Heather A; Hermens, Joop L M; Kraak, Michiel H S

2004-08-01

Body residues of compounds with a narcotic mode of action that exceed critical levels result in baseline toxicity in organisms. Previous studies have shown that internal concentrations in organisms also can be estimated by way of passive sampling. In this experiment, solid-phase microextraction (SPME) fibers were used as a tool to estimate the body residues, which were then compared to measured levels. Past application of SPME fibers in the assessment of toxicity risk of samples has focused on separate exposure of fibers and organisms, often necessitated by the amount of agitation needed in order to achieve steady state in the fibers within a convenient time period. Uptake kinetic studies have shown that in SPME fibers with thin coatings, equilibrium concentrations can be reached without agitation within the time frame of a toxicity test. In contrast to toxicity experiments to date, the SPME fibers in the current study were exposed concomitantly to the test water with the organisms, ensuring an exposure under the exact same conditions. Fibers and two aquatic invertebrate species were exposed to a mixture of four chlorobenzenes with a narcotic mode of action. The total body residue of these compounds in the organisms was determined, as was the acute toxicity resulting from the accumulation. The total body residues of both species were correlated to the total concentrations in SPME fibers. It was concluded that toxicity could be predicted based on total body residue (TBR) estimates from fiber concentrations.

Determination of the clean-up efficiency of the solid-phase extraction of rosemary extracts: Application of full-factorial design in hyphenation with Gaussian peak fit function.

PubMed

Meischl, Florian; Kirchler, Christian Günter; Jäger, Michael Andreas; Huck, Christian Wolfgang; Rainer, Matthias

2018-02-01

We present a novel method for the quantitative determination of the clean-up efficiency to provide a calculated parameter for peak purity through iterative fitting in conjunction with design of experiments. Rosemary extracts were used and analyzed before and after solid-phase extraction using a self-fabricated mixed-mode sorbent based on poly(N-vinylimidazole/ethylene glycol dimethacrylate). Optimization was performed by variation of washing steps using a full three-level factorial design and response surface methodology. Separation efficiency of rosmarinic acid from interfering compounds was calculated using an iterative fit of Gaussian-like signals and quantifications were performed by the separate integration of the two interfering peak areas. Results and recoveries were analyzed using Design-Expert® software and revealed significant differences between the washing steps. Optimized parameters were considered and used for all further experiments. Furthermore, the solid-phase extraction procedure was tested and compared with commercial available sorbents. In contrast to generic protocols of the manufacturers, the optimized procedure showed excellent recoveries and clean-up rates for the polymer with ion exchange properties. Finally, rosemary extracts from different manufacturing areas and application types were studied to verify the developed method for its applicability. The cleaned-up extracts were analyzed by liquid chromatography with tandem mass spectrometry for detailed compound evaluation to exclude any interference from coeluting molecules. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis and application of mesoporous molecular sieve for miniaturized matrix solid-phase dispersion extraction of bioactive flavonoids from toothpaste, plant, and saliva.

PubMed

Cao, Wan; Cao, Jun; Ye, Li-Hong; Xu, Jing-Jing; Hu, Shuai-Shuai; Peng, Li-Qing

2015-12-01

This article describes the use of the mesoporous molecular sieve KIT-6 as a sorbent in miniaturized matrix solid-phase dispersion (MSPD) in combination with ultra-performance LC for the determination of bioactive flavonoids in toothpaste, Scutellariae Radix, and saliva. In this study, for the first time, KIT-6 was used as a sorbent material for this mode of extraction. Compared with common silica-based sorbents (C18 and activated silica gel), the proposed KIT-6 dispersant with a three-dimensional cubic Ia3d structure and highly ordered arrays of mesoporous channels exhibits excellent adsorption capability of the tested compounds. In addition, several experimental variables, such as the mass ratio of sample to dispersant, grinding time, and elution solvent, were optimized to maximize the extraction efficiency. The proposed analytical method is simple, fast, and entails low consumption of samples, dispersants and elution solvents, thereby meeting "green chemistry" requirements. Under the optimized conditions, the recoveries of three bioactive flavonoids obtained by analyzing the spiked samples were from 89.22 to 101.17%. Also, the LODs and LOQs for determining the analytes were in the range of 0.02-0.04 μg/mL and 0.07-0.13 μg/mL, respectively. Finally, the miniaturized matrix solid-phase dispersion method was successfully applied to the analysis of target solutes in real samples, and satisfactory results were obtained. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of aflatoxins in food samples by automated on-line in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry.

PubMed

Nonaka, Y; Saito, K; Hanioka, N; Narimatsu, S; Kataoka, H

2009-05-15

A simple and sensitive automated method for determination of aflatoxins (B1, B2, G1, and G2) in nuts, cereals, dried fruits, and spices was developed consisting of in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-mass spectrometry (LC-MS). Aflatoxins were separated within 8 min by high-performance liquid chromatography using a Zorbax Eclipse XDB-C8 column with methanol/acetonitrile (60/40, v/v): 5mM ammonium formate (45:55) as the mobile phase. Electrospray ionization conditions in the positive ion mode were optimized for MS detection of aflatoxins. The pseudo-molecular ions [M+H](+) were used to detect aflatoxins in selected ion monitoring (SIM) mode. The optimum in-tube SPME conditions were 25draw/eject cycles of 40 microL of sample using a Supel-Q PLOT capillary column as an extraction device. The extracted aflatoxins were readily desorbed from the capillary by passage of the mobile phase, and no carryover was observed. Using the in-tube SPME LC-MS with SIM method, good linearity of the calibration curve (r>0.9994) was obtained in the concentration range of 0.05-2.0 ng/mL using aflatoxin M1 as an internal standard, and the detection limits (S/N=3) of aflatoxins were 2.1-2.8 pg/mL. The in-tube SPME method showed >23-fold higher sensitivity than the direct injection method (10 microL injection volume). The within-day and between-day precision (relative standard deviations) at the concentration of 1 ng/mL aflatoxin mixture were below 3.3% and 7.7% (n=5), respectively. This method was applied successfully to analysis of food samples without interference peaks. The recoveries of aflatoxins spiked into nuts and cereals were >80%, and the relative standard deviations were <11.2%. Aflatoxins were detected at <10 ng/g in several commercial food samples.

Research on acting mechanism and behavior of a gas bubble in the air dense medium fluidized bed

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

Tao, X.; Chen, Q.; Yang, Y.

1996-12-31

Coal dry beneficiation with air-dense medium fluidized bed has now been established as a high efficiency dry separation technology, it is the application of fluidization technology to the coal preparation field. The tiny particle media forms an uniform and stable fluidized bed with a density acted by airflow, which is used to separate 80{micro}m to {approximately}6mm size coal. This technology has achieved satisfied industrialization results, and attracted the expert`s attention in the field. In fluidized bed, the interaction between gas and solid was mainly decided by the existence state of heavy media particles mass (position and distance) relative velocity ofmore » gas-solid two phase, as well turbulent action. A change of vertical gas-solid fluidizing state essentially is the one of a energy transforming process. For a coal separating process with air-dense medium fluidized bed, the gas bubble, producing a turbulent and stirring action in the bed, leads to two effects. It can promote a uniform distribution of heavy media particles, and a uniform and stability of a bed density. Otherwise it will decrease effective contacts between gas-solids two phases, producing a bigger gas bubble. Therefore controlling a gas bubble size in bed should be optimized. This paper analyzes mutual movement between gas-solid, and studies the gas bubble behavior in the bed. A mechanic mode and a separating process of coal in the bed is discussed. It aims to research the coal separating mechanism with air-dense fluidized bed.« less

An in-plane solid-liquid-solid growth mode for self-avoiding lateral silicon nanowires.

PubMed

Yu, Linwei; Alet, Pierre-Jean; Picardi, Gennaro; Roca i Cabarrocas, Pere

2009-03-27

We report an in-plane solid-liquid-solid (IPSLS) mode for obtaining self-avoiding lateral silicon nanowires (SiNW) in a reacting-gas-free annealing process, where the growth of SiNWs is guided by liquid indium drops that transform the surrounding a-SiratioH matrix into crystalline SiNWs. The SiNWs can be approximately mm long, with the smallest diameter down to approximately 22 nm. A high growth rate of >10(2) nm/s and rich evolution dynamics are revealed in a real-time in situ scanning electron microscopy observation. A qualitative growth model is proposed to account for the major features of this IPSLS SiNW growth mode.

Superhard BC(3) in cubic diamond structure.

PubMed

Zhang, Miao; Liu, Hanyu; Li, Quan; Gao, Bo; Wang, Yanchao; Li, Hongdong; Chen, Changfeng; Ma, Yanming

2015-01-09

We solve the crystal structure of recently synthesized cubic BC(3) using an unbiased swarm structure search, which identifies a highly symmetric BC(3) phase in the cubic diamond structure (d-BC(3)) that contains a distinct B-B bonding network along the body diagonals of a large 64-atom unit cell. Simulated x-ray diffraction and Raman peaks of d-BC(3) are in excellent agreement with experimental data. Calculated stress-strain relations of d-BC(3) demonstrate its intrinsic superhard nature and reveal intriguing sequential bond-breaking modes that produce superior ductility and extended elasticity, which are unique among superhard solids. The present results establish the first boron carbide in the cubic diamond structure with remarkable properties, and these new findings also provide insights for exploring other covalent solids with complex bonding configurations.

Comparative evaluation of liquid-liquid extraction, solid-phase extraction and solid-phase microextraction for the gas chromatography-mass spectrometry determination of multiclass priority organic contaminants in wastewater.

PubMed

Robles-Molina, José; Gilbert-López, Bienvenida; García-Reyes, Juan F; Molina-Díaz, Antonio

2013-12-15

The European Water Framework Directive (WFD) 2000/60/EC establishes guidelines to control the pollution of surface water by sorting out a list of priority substances that involves a significant risk to or via the aquatic systems. In this article, the analytical performance of three different sample preparation methodologies for the GC-MS/MS determination of multiclass organic contaminants-including priority comprounds from the WFD-in wastewater samples using gas chromatography-mass spectrometry was evaluated. The methodologies tested were: (a) liquid-liquid extraction (LLE) with n-hexane; (b) solid-phase extraction (SPE) with C18 cartridges and elution with ethyl acetate:dichloromethane (1:1 (v/v)), and (c) headspace solid-phase microextraction (HS-SPME) using two different fibers: polyacrylate and polydimethylsiloxane/carboxen/divinilbenzene. Identification and confirmation of the selected 57 compounds included in the study (comprising polycyclic aromatic hydrocarbons (PAHs), pesticides and other contaminants) were accomplished using gas chromatography tandem mass spectrometry (GC-MS/MS) with a triple quadrupole instrument operated in the multiple reaction monitoring (MRM) mode. Three MS/MS transitions were selected for unambiguous confirmation of the target chemicals. The different advantages and pitfalls of each method were discussed. In the case of both LLE and SPE procedures, the method was validated at two different concentration levels (15 and 150 ng L(-1)) obtaining recovery rates in the range 70-120% for most of the target compounds. In terms of analyte coverage, results with HS-SPME were not satisfactory, since 14 of the compounds tested were not properly recovered and the overall performance was worse than the other two methods tested. LLE, SPE and HS-SPME (using polyacrylate fiber) procedures also showed good linearity and precision. Using any of the three methodologies tested, limits of quantitation obtained for most of the detected compounds were in the low nanogram per liter range. © 2013 Elsevier B.V. All rights reserved.

Microscale reconstruction of biogeochemical substrates using multimode X-ray tomography and scanning electron microscopy

NASA Astrophysics Data System (ADS)

Miller, M.; Miller, E.; Liu, J.; Lund, R. M.; McKinley, J. P.

2012-12-01

X-ray computed tomography (CT), scanning electron microscopy (SEM), electron microprobe analysis (EMP), and computational image analysis are mature technologies used in many disciplines. Cross-discipline combination of these imaging and image-analysis technologies is the focus of this research, which uses laboratory and light-source resources in an iterative approach. The objective is to produce images across length scales, taking advantage of instrumentation that is optimized for each scale, and to unify them into a single compositional reconstruction. Initially, CT images will be collected using both x-ray absorption and differential phase contrast modes. The imaged sample will then be physically sectioned and the exposed surfaces imaged and characterized via SEM/EMP. The voxel slice corresponding to the physical sample surface will be isolated computationally, and the volumetric data will be combined with two-dimensional SEM images along CT image planes. This registration step will take advantage of the similarity between the X-ray absorption (CT) and backscattered electron (SEM) coefficients (both proportional to average atomic number in the interrogated volume) as well as the images' mutual information. Elemental and solid-phase distributions on the exposed surfaces, co-registered with SEM images, will be mapped using EMP. The solid-phase distribution will be propagated into three-dimensional space using computational methods relying on the estimation of compositional distributions derived from the CT data. If necessary, solid-phase and pore-space boundaries will be resolved using X-ray differential phase contrast tomography, x-ray fluorescence tomography, and absorption-edge microtomography at a light-source facility. Computational methods will be developed to register and model images collected over varying scales and data types. Image resolution, physically and dynamically, is qualitatively different for the electron microscopy and CT methodologies. Routine CT images are resolved at 10-20 μm, while SEM images are resolved at 10-20 nm; grayscale values vary according to collection time and instrument sensitivity; and compositional sensitivities via EMP vary in interrogation volume and scale. We have so far successfully registered SEM imagery within a multimode tomographic volume and have used standard methods to isolate pore space within the volume. We are developing a three-dimensional solid-phase identification and registration method that is constrained by bulk-sample X-ray diffraction Rietveld refinements. The results of this project will prove useful in fields that require the fine-scale definition of solid-phase distributions and relationships, and could replace more inefficient methods for making these estimations.

Development of a novel mixed hemimicelles dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene for the separation and preconcentration of fluoxetine in different matrices before its determination by fiber optic linear array spectrophotometry and mode-mismatched thermal lens spectroscopy.

PubMed

Kazemi, Elahe; Haji Shabani, Ali Mohammad; Dadfarnia, Shayessteh; Abbasi, Amir; Rashidian Vaziri, Mohammad Reza; Behjat, Abbas

2016-01-28

This study aims at developing a novel, sensitive, fast, simple and convenient method for separation and preconcentration of trace amounts of fluoxetine before its spectrophotometric determination. The method is based on combination of magnetic mixed hemimicelles solid phase extraction and dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene as a sorbent. The magnetic graphene was synthesized by a simple coprecipitation method and characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). The retained analyte was eluted using a 100 μL mixture of methanol/acetic acid (9:1) and converted into fluoxetine-β-cyclodextrin inclusion complex. The analyte was then quantified by fiber optic linear array spectrophotometry as well as mode-mismatched thermal lens spectroscopy (TLS). The factors affecting the separation, preconcentration and determination of fluoxetine were investigated and optimized. With a 50 mL sample and under optimized conditions using the spectrophotometry technique, the method exhibited a linear dynamic range of 0.4-60.0 μg L(-1), a detection limit of 0.21 μg L(-1), an enrichment factor of 167, and a relative standard deviation of 2.1% and 3.8% (n = 6) at 60 μg L(-1) level of fluoxetine for intra- and inter-day analyses, respectively. However, with thermal lens spectrometry and a sample volume of 10 mL, the method exhibited a linear dynamic range of 0.05-300 μg L(-1), a detection limit of 0.016 μg L(-1) and a relative standard deviation of 3.8% and 5.6% (n = 6) at 60 μg L(-1) level of fluoxetine for intra- and inter-day analyses, respectively. The method was successfully applied to determine fluoxetine in pharmaceutical formulation, human urine and environmental water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Polymeric Sorbent with Controlled Surface Polarity: An Alternate for Solid-Phase Extraction of Nerve Agents and Their Markers from Organic Matrix.

PubMed

Roy, Kanchan Sinha; Purohit, Ajay Kumar; Chandra, Buddhadeb; Goud, D Raghavender; Pardasani, Deepak; Dubey, Devendra Kumar

2018-06-05

Extraction and identification of lethal nerve agents and their markers in complex organic background have a prime importance from the forensic and verification viewpoint of the Chemical Weapons Convention (CWC). Liquid-liquid extraction with acetonitrile and commercially available solid phase silica cartridges are extensively used for this purpose. Silica cartridges exhibit limited applicability for relatively polar analytes, and acetonitrile extraction shows limited efficacy toward relatively nonpolar analytes. The present study describes the synthesis of polymeric sorbents with tunable surface polarity, their application as a solid-phase extraction (SPE) material against nerve agents and their polar as well as nonpolar markers from nonpolar organic matrices. In comparison with the acetonitrile extraction and commercial silica cartridges, the new sorbent showed better extraction efficiency toward analytes of varying polarity. The extraction parameters were optimized for the proposed method, which included ethyl acetate as an extraction solvent and n-hexane as a washing solvent. Under optimized conditions, method linearity ranged from 0.10 to 10 μg mL -1 ( r 2 = 0.9327-0.9988) for organophosphorus esters and 0.05-20 μg mL -1 ( r 2 = 0.9976-0.9991) for nerve agents. Limits of detection (S:N = 3:1) in the SIM mode were found in the range of 0.03-0.075 μg mL -1 for organophosphorus esters and 0.015-0.025 μg mL -1 for nerve agents. Limits of quantification (S:N = 10:1) were found in the range of 0.100-0.25 μg mL -1 for organophosphorus esters and 0.05-0.100 μg mL -1 for nerve agents in the SIM mode. The recoveries of the nerve agents and their markers ranged from 90.0 to 98.0% and 75.0 to 95.0% respectively. The repeatability and reproducibility (with relative standard deviations (RSDs) %) for organophosphorus esters were found in the range of 1.35-8.61% and 2.30-9.25% respectively. For nerve agents, the repeatability range from 1.00 to 7.75% and reproducibility were found in the range of 2.17-6.90%.

Signatures of exciton condensation in a transition metal dichalcogenide

NASA Astrophysics Data System (ADS)

Kogar, Anshul; Rak, Melinda S.; Vig, Sean; Husain, Ali A.; Flicker, Felix; Joe, Young Il; Venema, Luc; MacDougall, Greg J.; Chiang, Tai C.; Fradkin, Eduardo; van Wezel, Jasper; Abbamonte, Peter

2017-12-01

Bose condensation has shaped our understanding of macroscopic quantum phenomena, having been realized in superconductors, atomic gases, and liquid helium. Excitons are bosons that have been predicted to condense into either a superfluid or an insulating electronic crystal. Using the recently developed technique of momentum-resolved electron energy-loss spectroscopy (M-EELS), we studied electronic collective modes in the transition metal dichalcogenide semimetal 1T-TiSe2. Near the phase-transition temperature (190 kelvin), the energy of the electronic mode fell to zero at nonzero momentum, indicating dynamical slowing of plasma fluctuations and crystallization of the valence electrons into an exciton condensate. Our study provides compelling evidence for exciton condensation in a three-dimensional solid and establishes M-EELS as a versatile technique sensitive to valence band excitations in quantum materials.

Use of unnatural amino acids to probe structure-activity relationships and mode-of-action of antimicrobial peptides.

PubMed

Tossi, Alessandro; Scocchi, Marco; Zahariev, Sotir; Gennaro, Renato

2012-01-01

Endogenous antimicrobial peptides (AMPs) can have multimodal mechanisms of bacterial inactivation, such as membrane lysis, interference with cell wall biosynthesis or membrane-based protein machineries, or translocation through the membrane to intracellular targets. The controlled variation of side-chain characteristics in their amino acid residues can provide much useful information on structure-activity relationships and mode-of-action, and also lead to improved activities. The small size and relatively low complexity of AMPs make them amenable to solid-phase peptide synthesis, facilitating the use of nonproteinogenic amino acids and vastly increasing the accessible molecular diversity of side chains. Here, we describe how such residues can be used to modulate such key parameters as cationicity, hydrophobicity, steric factors conformational stability, and H-bonding.

Structural properties and electrochemistry of α-LiFeO2

NASA Astrophysics Data System (ADS)

Abdel-Ghany, A. E.; Mauger, A.; Groult, H.; Zaghib, K.; Julien, C. M.

2012-01-01

In this work, we study the physico-chemistry and electrochemistry of lithium ferrite synthesized by solid-state reaction. Characterization included X-ray diffraction (XRD), scanning electronic microscopy (SEM), Raman scattering (RS), Fourier transform infrared spectroscopy (FTIR), and SQUID magnetometry. XRD peaks gradually sharpen with increasing firing temperature; all the diffraction peaks can be indexed to the cubic α-LiFeO2 phase (Fm3m space group) with the refined cell parameter a = 4.155 Å. RS and FTIR spectra show the vibrational modes due to covalent Fe-O bonds and the Li-cage mode at low-frequency. The electrochemical properties of Li/LiFeO2 are revisited along with the post-mortem analysis of the positive electrode material using XRD and Raman experiments.

A new approach for downscaling of electromembrane extraction as a lab on-a-chip device followed by sensitive Red-Green-Blue detection.

PubMed

Baharfar, Mahroo; Yamini, Yadollah; Seidi, Shahram; Arain, Muhammad Balal

2018-05-30

A new design of electromembrane extraction (EME) as a lab on-a-chip device was proposed for the extraction and determination of phenazopyridine as the model analyte. The extraction procedure was accomplished by coupling of EME and the packing of a sorbent. The analyte was extracted under the applied electrical field across a membrane sheet impregnated by nitrophenyl octylether (NPOE) into an acceptor phase. It was followed by the absorption of the analyte on strong cation exchanger as a sorbent. The designed chip contained separate spiral channels for donor and acceptor phases featuring embedded platinum electrodes to enhance extraction efficiency. The selected donor and acceptor phases were 0 mM HCl and 100 mM HCl, respectively. The on-chip electromembrane extraction was carried out under the voltage level of 70 V for 50 min. The analysis was carried out by two modes of a simple Red-Green-Blue (RGB) image analysis tool and a conventional HPLC-UV system. After the absorption of the analyte on the solid phase, its color changed and a digital picture of the sorbent was taken for the RGB analysis. The effective parameters on the performance of the chip device, comprising the EME and solid phase microextraction steps, were distinguished and optimized. The accumulation of the analyte on the solid phase showed excellent sensitivity and a limit of detection (LOD) lower than 1.0 μg L-1 achieved by an image analysis using a smartphone. This device also offered acceptable intra- and inter-assay RSD% (<10%). The calibration curves were linear within the range of 10-1000 μg L-1 and 30-1000 μg L-1 (r2 > 0.9969) for HPLC-UV and RGB analysis, respectively. To investigate the applicability of the method in complicated matrices, urine samples of patients being treated with phenazopyridine were analyzed.

Study on solid liquid interface heat transfer of PCM under simultaneous charging and discharging (SCD) in horizontal cylinder annulus

NASA Astrophysics Data System (ADS)

Omojaro, Adebola Peter; Breitkopf, Cornelia

2017-07-01

Heat transfer performance during the simultaneous charging and discharging (SCD) operation process for phase change materials (PCM) contained inside the annulus of concentric horizontal cylinder was investigated. In the experimental set-up, the PCM inside the annulus serves as the heat sink along with an externally imposed forced cooling air. The obtained time wise temperature profile was used to determine the effects of different heat fluxes and the imposed forced convection cooling on the melt fraction values and the transition shift time from the observed conduction to natural convection heat transfer patterns. Furthermore, non-dimensional analysis was presented for the heat transfer at the interface to enable generalizing the result. Comparison of the results show that the SCD operation mode establish the condition that enables much PCM phase transition time and thus longer time of large latent heat transfer effect than the Partial and non simultaneous operations. Analysis results show that the variation of the heat flux for the SCD mode did not change the dominance of the natural convection over conduction heat transfers in the PCM. However, it significantly influences the commencement/transition shift time and melting rate while higher heat fluxes yields melt fraction that was 38-63% more for investigated process time. Variation with different cooling air flow rate shows more influences on the melt fraction than on the mode of heat transfer occurring in the PCM during melting. Available non-SCD modes correlation was shown to be insufficient to accurately predict interface heat transfer for the SCD modes.

Design of C18 Organic Phases with Multiple Embedded Polar Groups for Ultraversatile Applications with Ultrahigh Selectivity.

PubMed

Mallik, Abul K; Qiu, Hongdeng; Oishi, Tomohiro; Kuwahara, Yutaka; Takafuji, Makoto; Ihara, Hirotaka

2015-07-07

For the first time, we synthesized multiple embedded polar groups (EPGs) containing linear C18 organic phases. The new materials were characterized by elemental analysis, IR spectroscopy, (1)H NMR, diffuse reflectance infrared Fourier transform (DRIFT), solid-state (13)C cross-polarization magic angle spinning (CP/MAS) NMR, suspended-state (1)H NMR, and differential scanning calorimetry (DSC). (29)Si CP/MAS NMR was carried out to investigate the degree of cross-linking of the silane and silane functionality of the modified silica. Solid-state (13)C CP/MAS NMR and suspended-state (1)H NMR spectroscopy indicated a higher alkyl chain order for the phase containing four EPGs than for the phase with three EPGs. To correlate the NMR results with temperature-dependent chromatographic studies, standard reference materials (SRM 869b and SRM 1647e), a column selectivity test mixture for liquid chromatography was employed. A single EPG containing the C18 phase was also prepared in a similar manner to be used as a reference column especially for the separation of basic and polar compounds in reversed-phase liquid chromatography (RPLC) and hydrophilic interaction liquid chromatography (HILIC), respectively. Detailed chromatographic characterization of the new phases was performed in terms of their surface coverage, hydrophobic selectivity, shape selectivity, hydrogen bonding capacity, and ion-exchange capacity at pH 2.7 and 7.6 for RPLC as well as their hydrophilicity, the selectivity for hydrophilic-hydrophobic substituents, the selectivity for the region and configurational differences in hydrophilic substituents, the evaluation of electrostatic interactions, and the evaluation of the acidic-basic nature for HILIC-mode separation. Furthermore, peak shapes for the basic analytes propranolol and amitriptyline were studied as a function of the number of EPGs on the C18 phases in the RPLC. The chromatographic performance of multiple EPGs containing C18 HILIC phases is illustrated by the separation of sulfa drugs, β-blockers, xanthines, nucleic acid bases, nucleosides, and water-soluble vitamins. Both of the phases showed the best performance for the separation of shape-constrained isomers, nonpolar, polar, and basic compounds in RPLC- and HILIC-mode separation of sulfa drugs, and other polar and basic analytes compared to the conventional alkyl phases with and without embedded polar groups and HILIC phases. Surprisingly, one phase would be able to serve the performance of three different types of phases with very high selectivity, and we named this phase the "smart phase". Versatile applications with a single column will reduce the column purchasing cost for the analyst as well as achieve high separation, which is challenging with the commercially available columns.

Single-frequency Ince-Gaussian mode operations of laser-diode-pumped microchip solid-state lasers.

PubMed

Ohtomo, Takayuki; Kamikariya, Koji; Otsuka, Kenju; Chu, Shu-Chun

2007-08-20

Various single-frequency Ince-Gaussian mode oscillations have been achieved in laser-diode-pumped microchip solid-state lasers, including LiNdP(4)O(12) (LNP) and Nd:GdVO(4), by adjusting the azimuthal symmetry of the short laser resonator. Ince-Gaussian modes formed by astigmatic pumping have been reproduced by numerical simulation.

Optical and Raman microspectroscopy of nitrogen and hydrogen mixtures at high pressures

NASA Astrophysics Data System (ADS)

Ciezak, Jennifer; Jenkins, T.; Hemley, R.

2009-06-01

Extended phases of molecular solids formed from simple molecules have led to polymeric materials under extreme conditions with advanced optical, mechanical and energetic properties. Although the existence of extended phases has been demonstrated in N2, CO and CO2, recovery of the materials to ambient conditions has posed considerable difficulty. Recent molecular dynamics simulations have predicted that the addition of hydrogen to nitrogen may increase the stability of the cubic-gauche nitrogen polymer and thereby offer the possibility of synthesis at lower pressures and temperatures. Here we present optical and Raman microspectroscopy measurements performed on nitrogen and hydrogen mixtures to 85 GPa. To pressures of 30 GPa, large deviations in the internal molecular stretching modes of the mixtures relative to those of the pure material reveal unusual phase behavior. After an unusual phase separation near 35 GPa, a phase assemblage of consisting of a phase rich in both nitrogen and hydrogen, a phase of relatively amorphous nitrogen and a mixture of the two is observed. Near this pressure, Raman bands attributed to the N-N single bonded stretch were observed.

Spectroscopic studies of U(VI) sorption at the kaolinite-water interface. Final report

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

Thompson, H.A.; Parks, G.A.; Brown, G.E. Jr.

Efficient use of U as a resource and safe handling, recycling and disposal of U-containing wastes require an understanding of the factors controlling the fate of U, where fate refers to the destination of U, typically expressed as an environmental medium or a process phase. The sorption process constitutes a change in elemental fate. Partitioning of an element from solution to a solid phase, or sorption, can be divided into three broad categories: adsorption, surface precipitation, and absorption. Extended X-ray absorption fine structure (EXAFS), a type of X-ray absorption spectroscopy (XAS), offers the possibility for distinguishing among different modes ofmore » sorption by characterizing the atomic environment of the sorbing element. In this study, the authors use EXAFS to determine the structure of U(VI) sorption complexes at the kaolinite-water interface. In Chapter One, they present an overview of selected aspects of U structural chemistry as a basis for considering the structural environment of U at the solid-water interface. To evaluate the utility of XAS for characterization of the structural environment of U(VI) at the solid-water interface, they have carried out an in-depth analysis of XAS data from U(VI)-containing solid and solution model compounds, which they describe in Chapter Two. In Chapter three, they consider sorption of U by kaolinite as a means of effecting the removal of U from surface collection pond waters on the Rocky Flats Plant site in northern Colorado.« less

[Simultaneous determination of nine estrogens in eel by ultrafast liquid chromatography-tandem mass spectrometry with isotope dilution technique and solid-phase extraction].

PubMed

Chen, Xiaohong; Yao, Shanshan; Li, Xiaoping; Zhao, Yonggang; Jin, Micong

2012-11-01

Developing a rapid and sensitive analytical method based on ultrafast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) with solid-phase extraction (SPE) for the simultaneous determination of nine estrogens (dienestrol, diethylstilbestrol, estrone, hexestrol, 17-alpha-estradiol, 17-beta-estradiol, estriol, 17alpha-ethinylestradiol and estradiol valerate) in eel. After the sample was extracted by acetonitrile and cleaned by Waters Oasis HLB solid-phase extraction cartridge, the UFLC separation was performed on a Shim-pack XR-ODS II column (100 mm x 2.0 mm, 2.2 microm) with a linear gradient elution program of methanol solution containing 0.04% ammonia (v/v) and 0.04% ammonia aqueous solution (v/v) as the mobile phase. Electrospray ionization was applied and operated in the negative multiple reaction monitoring (MRM) mode. The quantitation was used by isotope internal standard dilution technique. The results showed that the limits of quantitation (LOQs, S/N(10) were in the range of 0.07-0.4 microg/kg, the calibration curves were in good linearities for the nine analytes in the range of 0.5-50.0 microg/L with the correlative coefficients (r2) more than 0.998, the recoveries were between 81.0% and 110.0% with the relative standard deviations (RSDs) of 1.92%-8.24%. Additional, the mass spectra characterization of the nine estrogens was discussed and the fragmentation pathways were speculated. The developed method is rapid, sensitive, specific and reproducible, and adapts not only to the simultaneous determination of the nine trace estrogens including the epimer of 17-alpha-estradiol and 17-beta-estradiol but also to the identified detection in other fish tissues.

Determination of diphenylether herbicides in water samples by solid-phase microextraction coupled to liquid chromatography.

PubMed

Sheu, Hong-Li; Sung, Yu-Hsiang; Melwanki, Mahaveer B; Huang, Shang-Da

2006-11-01

Solid-phase microextraction (SPME) coupled to LC for the analysis of five diphenylether herbicides (aclonifen, bifenox, fluoroglycofen-ethyl, oxyfluorfen, and lactofen) is described. Various parameters of extraction of analytes onto the fiber (such as type of fiber, extraction time and temperature, pH, impact of salt and organic solute) and desorption from the fiber in the desorption chamber prior to separation (such as type and composition of desorption solvent, desorption mode, soaking time, and flush-out time) were studied and optimized. Four commercially available SPME fibers were studied. PDMS/divinylbenzene (PDMS/DVB, 60 microm) and carbowax/ templated resin (CW/TPR, 50 microm) fibers were selected due to better extraction efficiencies. Repeatability (RSD, < 7%), correlation coefficient (> 0.994), and detection limit (0.33-1.74 and 0.22-1.94 ng/mL, respectively, for PDMS/DVB and CW/TPR) were investigated. Relative recovery (81-104% for PDMS/DVB and 83-100% for CW/TPR fiber) values have also been calculated. The developed method was successfully applied to the analysis of river water and water collected from a vegetable garden.

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

PubMed

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

2015-09-30

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

A novel method for the elaboration of hydroxyapatite with high purity by sol-gel using the albumin and comparison with the classical methods

NASA Astrophysics Data System (ADS)

Mohammed, Eddya; Bouazza, Tbib; Khalil, El-Hami

2018-02-01

In this paper, we report the first synthesis of hydroxyapatite (Hap) by sol-gel using the albumin (egg white) compared with the four classical elaboration methods such as co-precipitation, solid state, and solid-liquid samples of hydroxyapatite. We use a reference sample of hydroxyapatite bought from Fluka Chemika company (Lot and Filling code 385330/1 14599). All samples are characterized by X-ray diffraction (XRD), Uv-visible spectroscopy (Uv-Vis), and Fourier transforms infrared spectroscopy (FT-IR). The XRD study showed the existence of a Hexagonal phase for all our samples prepared in our laboratory and an orthorhombic phase for the Fulka Chemika sample of Hap (Lot and Filling code 385330/1 14599). The study by Uv-visible spectroscopy was performed to determine and compare the optical gap and the disorder of each sample of Hap. The FT-IR spectroscopy demonstrated that all our Hap samples had a similar mode of vibration of the chemical bonds (OH-) and (PO4)3-.

Development and validation of a matrix solid-phase dispersion method to determine acrylamide in coffee and coffee substitutes.

PubMed

Soares, Cristina M Dias; Alves, Rita C; Casal, Susana; Oliveira, M Beatriz P P; Fernandes, José Oliveira

2010-04-01

The present study describes the development and validation of a new method based on a matrix solid-phase dispersion (MSPD) sample preparation procedure followed by GC-MS for determination of acrylamide levels in coffee (ground coffee and brewed coffee) and coffee substitute samples. Samples were dispersed in C(18) sorbent and the mixture was further packed into a preconditioned custom-made ISOLUTE bilayered SPE column (C(18)/Multimode; 1 g + 1 g). Acrylamide was subsequently eluted with water, and then derivatized with bromine and quantified by GC-MS in SIM mode. The MSPD/GC-MS method presented a LOD of 5 microg/kg and a LOQ of 10 microg/kg. Intra and interday precisions ranged from 2% to 4% and 4% to 10%, respectively. To evaluate the performance of the method, 11 samples of ground and brewed coffee and coffee substitutes were simultaneously analyzed by the developed method and also by a previously validated method based in a liquid-extraction (LE) procedure, and the results were compared showing a high correlation between them.

Improved conditions for the application of solid phase microextraction prior to HPLC-FLD analysis of anatoxin-a.

PubMed

Rellán, Sandra; Gago-Martínez, Ana

2007-10-01

Solid phase microextraction coupled with high performance liquid chromatography with fluorescence detection has been optimized and evaluated for a simple, rapid, and selective analysis of anatoxin-a. Four kinds of fiber (100 microm polydimethylsiloxane, 60 microm polydimethylsiloxane/divinylbenzene, 50 microm Carbowax/templated resin-100, and 85 microm polyacrylate) were evaluated for an efficient extraction of the toxin. Parameters relating to the desorption step, such as desorption mode, solvent composition, time for both static and dynamic desorption, as well as carryover, have been studied and optimized. The derivatization process was investigated using NBD-F as derivatizing reagent. Anatoxin-a derivative was formed when the anatoxin-a-loaded fiber was inserted in a vial containing 5 microL of NBD-F. Variables affecting extraction such us ionic strength, temperature, and time have been also optimized. The results obtained showed linearity in the range of 10-2000 ng and a limit of detection of 0.29 ng/mL in river water. The presented method has been applied to different environmental samples.

Analysis of pesticides in soy milk combining solid-phase extraction and capillary electrophoresis-mass spectrometry.

PubMed

Hernández-Borges, Javier; Rodriguez-Delgado, Miguel Angel; García-Montelongo, Francisco J; Cifuentes, Alejandro

2005-06-01

In this work, the determination of a group of triazolopyrimidine sulfoanilide herbicides (cloransulam-methyl, metosulam, flumetsulam, florasulam, and diclosulam) in soy milk by capillary electrophoresis-mass spectrometry (CE-MS) is presented. The main electrospray interface (ESI) parameters (nebulizer pressure, dry gas flow rate, dry gas temperature, and composition of the sheath liquid) are optimized using a central composite design. To increase the sensitivity of the CE-MS method, an off-line sample preconcentration procedure based on solid-phase extraction (SPE) is combined with an on-line stacking procedure (i.e. normal stacking mode, NSM). Samples could be injected for up to 100 s, providing limits of detection (LODs) down to 74 microg/L, i.e., at the low ppb level, with relative standard deviation values (RSD,%) between 3.8% and 6.4% for peak areas on the same day, and between 6.5% and 8.1% on three different days. The usefulness of the optimized SPE-NSM-CE-MS procedure is demonstrated through the sensitive quantification of the selected pesticides in soy milk samples.

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.

Simultaneous determination of fumonisins B1 and B2 in different types of maize by matrix solid phase dispersion and HPLC-MS/MS.

PubMed

de Oliveira, Gabriel Barros; de Castro Gomes Vieira, Carolyne Menezes; Orlando, Ricardo Mathias; Faria, Adriana Ferreira

2017-10-15

This work involved the optimization and validation of a method, according to Directive 2002/657/EC and the Analytical Quality Assurance Manual of Ministério da Agricultura, Pecuária e Abastecimento, Brazil, for simultaneous extraction and determination of fumonisins B1 and B2 in maize. The extraction procedure was based on a matrix solid phase dispersion approach, the optimization of which employed a sequence of different factorial designs. A liquid chromatography-tandem mass spectrometry method was developed for determining these analytes using the selected reaction monitoring mode. The optimized method employed only 1g of silica gel for dispersion and elution with 70% ammonium formate aqueous buffer (50mmolL -1 , pH 9), representing a simple, cheap and chemically friendly sample preparation method. Trueness (recoveries: 86-106%), precision (RSD ≤19%), decision limits, detection capabilities and measurement uncertainties were calculated for the validated method. The method scope was expanded to popcorn kernels, white maize kernels and yellow maize grits. Copyright © 2017 Elsevier Ltd. All rights reserved.

Potential and kinetic energetic analysis of phonon modes in varied molecular solids

NASA Astrophysics Data System (ADS)

Kraczek, Brent

2015-03-01

We calculate partitioned kinetic and potential energies of the phonon modes in molecular solids to illuminate the dynamical behavior of the constituent molecules. This enables analysis of the relationship between the characteristics of sets of phonon modes, molecular structure and chemical reactivity by partitioning the kinetic energy into the translational, rotational and vibrational motions of groups of atoms (including molecules), and the potential energy into the energy contained within interatomic interactions. We consider three solids of differing size and rigidity: naphthalene (C1 0 H6), nitromethane (CH3NO2)andα-HMX(C4H8N8O8). Naphthalene and nitromethane mostly act in the semi-rigid manner often expected in molecular solids. HMX exhibits behavior that is significantly less-rigid. While there are definite correlations between the kinetic and potential energetic analyses, there are also differences, particularly in the excitation of chemical bonds by low-frequency lattice modes. This suggests that in many cases computational and experimental methods dependent on atomic displacements may not identify phonon modes active in chemical reactivity.

One-pot preparation of a mixed-mode organic-silica hybrid monolithic capillary column and its application in determination of endogenous gibberellins in plant tissues.

PubMed

Zhang, Zheng; Hao, Yan-Hong; Ding, Jun; Xu, Sheng-Nan; Yuan, Bi-Feng; Feng, Yu-Qi

2015-10-16

A newly improved one-pot method, based on "thiol-ene" click chemistry and sol-gel approach in microemulsion system, was developed for the preparation of C8/PO(OH)2-silica hybrid monolithic capillary column. The prepared monolith possesses large specific surface area, narrow mesopore size distribution and high column efficiency. The monolithic column was demonstrated to have cation exchange/reversed-phase (CX/RP) mixed-mode retention for analytes on nano-liquid chromatography (nano-LC). On the basis of the developed nano-LC system with MS detector coupled to pipette tip solid phase extraction (PT-SPE) and derivatization process, we then realized simultaneous determination of 10 gibberellins (GAs) with low limits of detection (LODs, 0.003-0.025 ng/mL). Furthermore, 6 endogenous GAs in only 5mg rice leaves (fresh weight) were successfully detected and quantified. The developed PT-SPE-nano-LC-MS strategy may offer promising applications in the determination of low abundant bioactive molecules from complex matrix. Copyright © 2015 Elsevier B.V. All rights reserved.

MCX based solid phase extraction combined with liquid chromatography tandem mass spectrometry for the simultaneous determination of 31 endocrine-disrupting compounds in surface water of Shanghai.

PubMed

Zhang, Hong-Chang; Yu, Xue-jun; Yang, Wen-chao; Peng, Jin-feng; Xu, Ting; Yin, Da-Qiang; Hu, Xia-lin

2011-10-15

A novel analytical method employing MCX (mixed-mode cationic exchange) based solid phase extraction (SPE) coupled with liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed to detect 31 endocrine-disrupting compounds (EDCs) in surface water samples simultaneously. The target EDCs belong to five classes, including seven estrogens, eight androgens, six progesterones, five adrenocortical hormones and five industrial compounds. In order to simultaneously concentrate the target EDCs and eliminate matrix interferences in the water samples, MCX SPE cartridges were employed for SPE, and then followed by a simple and highly efficient three-step sequential elution procedure. Two electrospray ionization (ESI) detection modes, positive (ESI+) and (ESI-), were optimized for HPLC-MS/MS analysis to obtain the highest sensitivity for all the EDCs. The limits of detection (LODs) were 0.02-1.9 ng L(-1), which are lower than or comparable to these reported in references. Wide linear ranges (LOD-100 ng L(-1) for ESI+ mode, and LOD-200 ng L(-1) for ESI- mode) were obtained with determination coefficients (R(2)) higher than 0.99 for all the compounds. With five internal standards, good recoveries (84.4-103.0%) of all the target compounds were obtained in selected surface water samples. The developed method was successfully applied to investigate the EDCs occurrence in the surface water of Shanghai by analyzing surface water samples from 11 sites. The results showed that nearly all the target compounds (30 in 31) were present in the surface water samples of Shanghai, of which three industrial compounds (4-t-OP, BPA, and BPF) showed the highest concentrations (median concentrations were 11.88-23.50 ng L(-1)), suggesting that industrial compounds were the dominating EDCs in the surface water of Shanghai, and much more attention should be paid on these compounds. Our present research demonstrated that SPE with MCX cartridges combined with HPLC-MS/MS was convenient, efficient and reliable for multiclass analysis of EDCs in surface water. Copyright © 2011 Elsevier B.V. All rights reserved.

Efficient excitation of nonlinear phonons via chirped pulses: Induced structural phase transitions

NASA Astrophysics Data System (ADS)

Itin, A. P.; Katsnelson, M. I.

2018-05-01

Nonlinear phononics play important role in strong laser-solid interactions. We discuss a dynamical protocol for efficient phonon excitation, considering recent inspiring proposals: inducing ferroelectricity in paraelectric perovskites, and inducing structural deformations in cuprates [Subedi et al., Phys. Rev. B 89, 220301(R) (2014), 10.1103/PhysRevB.89.220301; Phys. Rev. B 95, 134113 (2017), 10.1103/PhysRevB.95.134113]. High-frequency phonon modes are driven by midinfrared pulses, and coupled to lower-frequency modes those indirect excitations cause structural deformations. We study in more detail the case of KTaO3 without strain, where it was not possible to excite the needed low-frequency phonon mode by resonant driving of the higher frequency one. Behavior of the system is explained using a reduced model of coupled driven nonlinear oscillators. We find a dynamical mechanism which prevents effective excitation at resonance driving. To induce ferroelectricity, we employ driving with sweeping frequency, realizing so-called capture into resonance. The method can be applied to many other related systems.

The properties of optimal two-dimensional phononic crystals with different material contrasts

NASA Astrophysics Data System (ADS)

Liu, Zong-Fa; Wu, Bin; He, Cun-Fu

2016-09-01

By modifying the spatial distribution of constituent material phases, phononic crystals (PnCs) can be designed to exhibit band gaps within which sound and vibration cannot propagate. In this paper, the developed topology optimization method (TOM), based on genetic algorithms (GAs) and the finite element method (FEM), is proposed to design two-dimensional (2D) solid PnC structures composed of two contrasting elastic materials. The PnCs have the lowest order band gap that is the third band gap for the coupled mode, the first band gap for the shear mode or the XY 34 Z band gap for the mixed mode. Moreover, the effects of the ratios of contrasting material properties on the optimal layout of unit cells and the corresponding phononic band gaps (PBGs) are investigated. The results indicate that the topology of the optimal PnCs and corresponding band gaps varies with the change of material contrasts. The law can be used for the rapid design of desired PnC structures.

Search for soliton modes in helical poly-γ-benzyl-l-glutamate

NASA Astrophysics Data System (ADS)

Renthal, Robert; Taboada, J.

1989-07-01

Solid α-helical poly(γ-benzyl-L-glutamate) was examined at low temperature for evidence of the unusual temperature-dependent vibrational mode found by Careri and co-workers in solid acetanilide and attributed to a soliton wave trapped in protein-like hydrogen bonds. We have confirmed the anomaly in acetanilide, however, a similar temperature-dependent mode was not observed in poly(γ-benzyl-L-glutamate). These results indicate that anharmonic amide modes may only be present in certain α-helical structures. Two new low frequency modes (180 and 90 cm -1) are observed for poly(γ-benzyl-L-glutamate).

Systematic evaluation of matrix effects in hydrophilic interaction chromatography versus reversed phase liquid chromatography coupled to mass spectrometry.

PubMed

Periat, Aurélie; Kohler, Isabelle; Thomas, Aurélien; Nicoli, Raul; Boccard, Julien; Veuthey, Jean-Luc; Schappler, Julie; Guillarme, Davy

2016-03-25

Reversed phase liquid chromatography (RPLC) coupled to mass spectrometry (MS) is the gold standard technique in bioanalysis. However, hydrophilic interaction chromatography (HILIC) could represent a viable alternative to RPLC for the analysis of polar and/or ionizable compounds, as it often provides higher MS sensitivity and alternative selectivity. Nevertheless, this technique can be also prone to matrix effects (ME). ME are one of the major issues in quantitative LC-MS bioanalysis. To ensure acceptable method performance (i.e., trueness and precision), a careful evaluation and minimization of ME is required. In the present study, the incidence of ME in HILIC-MS/MS and RPLC-MS/MS was compared for plasma and urine samples using two representative sets of 38 pharmaceutical compounds and 40 doping agents, respectively. The optimal generic chromatographic conditions in terms of selectivity with respect to interfering compounds were established in both chromatographic modes by testing three different stationary phases in each mode with different mobile phase pH. A second step involved the assessment of ME in RPLC and HILIC under the best generic conditions, using the post-extraction addition method. Biological samples were prepared using two different sample pre-treatments, i.e., a non-selective sample clean-up procedure (protein precipitation and simple dilution for plasma and urine samples, respectively) and a selective sample preparation, i.e., solid phase extraction for both matrices. The non-selective pretreatments led to significantly less ME in RPLC vs. HILIC conditions regardless of the matrix. On the contrary, HILIC appeared as a valuable alternative to RPLC for plasma and urine samples treated by a selective sample preparation. Indeed, in the case of selective sample preparation, the compounds influenced by ME were different in HILIC and RPLC, and lower and similar ME occurrence was generally observed in RPLC vs. HILIC for urine and plasma samples, respectively. The complementary of both chromatographic modes was also demonstrated, as ME was observed only scarcely for urine and plasma samples when selecting the most appropriate chromatographic mode. Copyright © 2015 Elsevier B.V. All rights reserved.

Production of proteases from organic wastes by solid-state fermentation: downstream and zero waste strategies.

PubMed

Marín, Maria; Artola, Adriana; Sánchez, Antoni

2018-04-01

Production of enzymes through solid-state fermentation (SSF) of agro-industrial wastes reports high productivity with low investment. The extraction of the final product from the solid waste and solid disposal represent the main cost of the process. In this work, the complete downstream processes of SSF of two industrial residues for the production of proteases, soy fibre (SF) and a mixture of hair and sludge (HS), were studied in terms of activity recovery, using different extraction parameters (extracting solvent, ratio solid: solvent and extraction mode). Activity after lyophilisation was tested. Solid waste valorisation after extraction was studied using respiration techniques and biogas production tests, as part of a zero waste strategy. Results showed a maximum extraction yield of 91% for SF and 121% for HS, both in agitated mode and distilled water as extraction agent. An average activity recovery of 95 ± 6 and 94 ± 6% for SF and HS, respectively, was obtained after lyophilisation and redissolution. To reduce the cost of extraction, a ratio 1:3 w : v solid-solvent in static mode is advised for SF, and 1:2 w : v extraction ratio in agitated mode for HS, both with distilled water as extracting agent. Both composting and anaerobic digestion are suitable techniques for valorisation of the waste material.

Effect of Binding Components in Complex Sample Matrices on Recovery in Direct Immersion Solid-Phase Microextraction: Friends or Foe?

PubMed

Alam, Md Nazmul; Pawliszyn, Janusz

2018-02-20

The development of matrix compatible coatings for solid-phase microextraction (SPME) has enabled direct extraction of analytes from complex sample matrices. The direct immersion (DI) mode of SPME when utilized in conjunction with such extraction phases facilitates extraction of a wide range of analytes from complex matrices without the incurrence of fouling or coating saturation. In this work, mathematical models and computational simulations were employed to investigate the effect of binding components present in complex samples on the recovery of small molecules varying in logP for extractions carried out using the direct immersion approach. The presented findings corroborate that the studied approach indeed enables the extraction of both polar and nonpolar analytes from complex matrices, provided a suitable sorbent is employed. Further results indicated that, in certain cases, the kinetics of extraction of a given analyte in its free form might be dependent on the desorption kinetics of their bound form from matrix components, which might lower total recoveries of analytes with high affinity for the matrix. However, the binding of analytes to matrix components also enables SPME to extract a balanced quantity of different logP analytes, facilitated by multiphase equilibria, with a single extraction device.

Chiral liquid chromatography-mass spectrometry (LC-MS/MS) method development for the detection of salbutamol in urine samples.

PubMed

Chan, Sue Hay; Lee, Warren; Asmawi, Mohd Zaini; Tan, Soo Choon

2016-07-01

A sequential solid-phase extraction (SPE) method was developed and validated using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) for the detection and quantification of salbutamol enantiomers in porcine urine. Porcine urine samples were hydrolysed with β-glucuronidase/arylsulfatase from Helix pomatia and then subjected to a double solid-phase extraction (SPE) first using the Abs-Elut Nexus SPE and then followed by the Bond Elut Phenylboronic Acid (PBA) SPE. The salbutamol enantiomers were separated using the Astec CHIROBIOTIC™ T HPLC column (3.0mm×100mm; 5μm) maintained at 15°C with a 15min isocratic run at a flow rate of 0.4mL/min. The mobile phase constituted of 5mM ammonium formate in methanol. Salbutamol and salbutamol-tert-butyl-d9 (internal standard, IS) was monitored and quantified with the multiple reaction monitoring (MRM) mode. The method showed good linearity for the range of 0.1-10ng/mL with limit of quantification at 0.3ng/mL. Analysis of the QC samples showed intra- and inter-assay precisions to be less than 5.04%, and recovery ranging from 83.82 to 102.33%. Copyright © 2016 Elsevier B.V. All rights reserved.

Modulation of magnetic interaction in Bismuth ferrite through strain and spin cycloid engineering

NASA Astrophysics Data System (ADS)

Yadav, Rama Shanker; Reshi, Hilal Ahmad; Pillai, Shreeja; Rana, D. S.; Shelke, Vilas

2016-12-01

Bismuth ferrite, a widely studied room temperature multiferroic, provides new horizons of multifunctional behavior in phase transited bulk and thin film forms. Bismuth ferrite thin films were deposited on lattice mismatched LaAlO3 substrate using pulsed laser deposition technique. X-ray diffraction confirmed nearly tetragonal (T-type) phase of thin film involving role of substrate induced strain. The film thickness of 56 nm was determined by X-ray reflectivity measurement. The perfect coherence and epitaxial nature of T- type film was observed through reciprocal space mapping. The room temperature Raman measurement of T-type bismuth ferrite thin film also verified phase transition with appearance of only few modes. In parallel, concomitant La and Al substituted Bi1-xLaxFe0.95Al0.05O3 (x = 0.1, 0.2, 0.3) bulk samples were synthesized using solid state reaction method. A structural phase transition into orthorhombic (Pnma) phase at x = 0.3 was observed. The structural distortion at x = 0.1, 0.2 and phase transition at x = 0.3 substituted samples were also confirmed by changes in Raman active modes. The remnant magnetization moment of 0.199 emu/gm and 0.28 emu/gm were observed for x = 0.2 and 0.3 bulk sample respectively. The T-type bismuth ferrite thin film also showed high remnant magnetization of around 20emu/cc. The parallelism in magnetic behavior between T-type thin film and concomitant La and Al substituted bulk samples is indication of modulation, frustration and break in continuity of spiral spin cycloid.

Solid state phase change materials for thermal energy storage in passive solar heated buildings

NASA Astrophysics Data System (ADS)

Benson, D. K.; Christensen, C.

1983-11-01

A set of solid state phase change materials was evaluated for possible use in passive solar thermal energy storage systems. The most promising materials are organic solid solutions of pentaerythritol, pentaglycerine and neopentyl glycol. Solid solution mixtures of these compounds can be tailored so that they exhibit solid-to-solid phase transformations at any desired temperature within the range from less than 25 deg to 188 deg. Thermophysical properties such as thermal conductivity, density and volumetric expansion were measured. Computer simulations were used to predict the performance of various Trombe wall designs incorporating solid state phase change materials. Optimum performance was found to be sensitive to the choice of phase change temperatures and to the thermal conductivity of the phase change material. A molecular mechanism of the solid state phase transition is proposed and supported by infrared spectroscopic evidence.

[Separation and purification of the components in Trachelospermum jasminoides by two dimensional hydrophilic interaction liquid chromatography- reversed-phase liquid chromatography].

PubMed

Jia, Youmei; Cai, Jianfeng; Xin, Huaxia; Feng, Jiatao; Fu, Yanhui; Fu, Qing; Jin, Yu

2017-06-08

A preparative two dimensional hydrophilic interaction liquid chromatography/reversed-phase liquid chromatography (Pre-2D-HILIC/RPLC) method was established to separate and purify the components in Trachelospermum jasminoides . The pigments and strongly polar components were removed from the crude extract after the active carbon decolorization and solid phase extraction processes. A Click XIon column (250 mm×20 mm, 10 μm) was selected as stationary phase and water-acetonitrile as mobile phases in the first dimensional HILIC. Finally, 15 fractions were collected under UV-triggered mode. In the second dimensional RPLC, a C18 column (250 mm×20 mm, 5 μm) was selected and water-acetonitrile was used as mobile phases. As a result, 14 compounds with high purity were obtained, which were further identified by mass spectrometry (MS) and nuclear magnetic resonance (NMR). Finally, 11 lignan compounds and three flavonoid compounds were obtained. The method has a good orthogonality, and can improve the resolution and the peak capacity. It is significant for the separation of complex components from Trachelospermum jasminoides .

The solid-state terahertz spectrum of MDMA (Ecstasy) - A unique test for molecular modeling assignments

NASA Astrophysics Data System (ADS)

Allis, Damian G.; Hakey, Patrick M.; Korter, Timothy M.

2008-10-01

The terahertz (THz, far-infrared) spectrum of 3,4-methylene-dioxymethamphetamine hydrochloride (Ecstasy) is simulated using solid-state density functional theory. While a previously reported isolated-molecule calculation is noteworthy for the precision of its solid-state THz reproduction, the solid-state calculation predicts that the isolated-molecule modes account for only half of the spectral features in the THz region, with the remaining structure arising from lattice vibrations that cannot be predicted without solid-state molecular modeling. The molecular origins of the internal mode contributions to the solid-state THz spectrum, as well as the proper consideration of the protonation state of the molecule, are also considered.

Mixed-mode sorption of hydroxylated atrazine degradation products to sell: A mechanism for bound residue

USGS Publications Warehouse

Lerch, R.N.; Thurman, E.M.; Kruger, E.L.

1997-01-01

This study tested the hypothesis that sorption of hydroxylated atrazine degradation products (HADPs: hydroxyatrazine, HA; deethylhydroxyatrazine, DEHA; and deisopropylhydroxyatrazine, DIHA) to soils occurs by mixed-mode binding resulting from two simultaneous mechanisms: (1) cation exchange and (2) hydrophobic interaction. The objective was to use liquid chromatography and soil extraction experiments to show that mixed-mode binding is the mechanism controlling HADP sorption to soils and is also a mechanism for bound residue. Overall, HADP binding to solid-phase extraction (SPE) sorbents occurred in the order: cation exchange >> octadecyl (C18) >> cyanopropyl. Binding to cation exchange SPE and to a high-performance liquid chromatograph octyl (C8) column showed evidence for mixed-mode binding. Comparison of soil extracted by 0.5 M KH2P04, pH 7.5, or 25% aqueous CH3CN showed that, for HA and DIHA, cation exchange was a more important binding mechanism to soils than hydrophobic interaction. Based on differences between several extractants, the extent of HADP mixed-mode binding to soil occurred in the following order: HA > DIHA > DEHA. Mixed-mode extraction recovered 42.8% of bound atrazine residues from aged soil, and 88% of this fraction was identified as HADPs. Thus, a significant portion of bound atrazine residues in soils is sorbed by the mixed-mode binding mechanisms.

First principles study on structural, lattice dynamical and thermal properties of BaCeO3

NASA Astrophysics Data System (ADS)

Zhang, Qingping; Ding, Jinwen; He, Min

2017-09-01

BaCeO3 exhibits impressive application potentials on solid oxide fuel cell electrolyte, hydrogen separation membrane and photocatalyst, owing to its unique ionic and electronic properties. In this article, the electronic structures, phonon spectra and thermal properties of BaCeO3 in orthorhombic, rhombohedral and cubic phases are investigated based on density functional theory. Comparisons with reported experimental results are also presented. The calculation shows that orthorhombic structure is both energetically and dynamically stable under ground state, which is supported by the experiment. Moreover, charge transfer between cations and anions accompanied with phase transition is observed, which is responsible for the softened phonon modes in rhombohedral and cubic phases. Besides, thermal properties are discussed. Oxygen atoms contribute most to the specific heat. The calculated entropy and specific heat at constant pressure fit well with the experimental ones within the measured temperature range.

Superhard BC 3 in cubic diamond structure

DOE PAGES

Zhang, Miao; Liu, Hanyu; Li, Quan; ...

2015-01-06

We solve the crystal structure of recently synthesized cubic BC 3 using an unbiased swarm structure search, which identifies a highly symmetric BC 3 phase in the cubic diamond structure (d–BC3) that contains a distinct B-B bonding network along the body diagonals of a large 64-atom unit cell. Simulated x-ray diffraction and Raman peaks of d–BC 3 are in excellent agreement with experimental data. Calculated stress-strain relations of d–BC 3 demonstrate its intrinsic superhard nature and reveal intriguing sequential bond-breaking modes that produce superior ductility and extended elasticity, which are unique among superhard solids. Here, the present results establish themore » first boron carbide in the cubic diamond structure with remarkable properties, and these new findings also provide insights for exploring other covalent solids with complex bonding configurations.« less

Research Progress on F-P Interference—Based Fiber-Optic Sensors

PubMed Central

Huang, Yi Wen; Tao, Jin; Huang, Xu Guang

2016-01-01

We review our works on Fabry-Perot (F-P) interferometric fiber-optic sensors with various applications. We give a general model of F-P interferometric optical fiber sensors including diffraction loss caused by the beam divergence and the Gouy phase shift. Based on different structures of an F-P cavity formed on the end of a single-mode fiber, the F-P interferometric optical sensor has been extended to measurements of the refractive index (RI) of liquids and solids, temperature as well as small displacement. The RI of liquids and solids can be obtained by monitoring the fringe contrast related to Fresnel reflections, while the ambient temperature and small displacement can be obtained by monitoring the wavelength shift of the interference fringes. The F-P interferometric fiber-optic sensors can be used for many scientific and technological applications. PMID:27598173

Ternary mixed-mode silica sorbent of solid-phase extraction for determination of basic, neutral and acidic drugs in human serum.

PubMed

Jin, Shupei; Qiao, Yinghua; Xing, Jun

2018-06-01

In this study, a ternary mixed-mode silica sorbent (TMSS) with octamethylene, carboxyl, and amino groups was prepared via Cu(I)-catalyzed azide-alkyne cycloaddition (CuAAC) click reaction and a subsequent reduction of azide to primary amine. While used in solid-phase extraction (SPE), the retention behavior of TMSS towards a total of nine kinds of basic, neutral, and acidic drugs was investigated in detail. The results revealed that hydrophobic, ion-exchange interaction, and electrostatic repulsion between TMSS and the analytes were closely related to the retention behavior of TMSS. Besides, the log K ow value of the analyte was also a factor influencing the retention behavior of analytes on TMSS. The nine analytes could be retained by TMSS simultaneously and then, were eluted into two fractions according to the acid-base property of the analytes for further determinations. The acidic and neutral analytes were in one fraction, and the basic ones in the other fraction. When used to treat the human serum spiked with the nine drugs, TMSS offered higher recoveries than BakerBond CBA and comparable recoveries to Oasis WCX. It should be noted TMSS had better purifying capability for human serum than Oasis WCX. Under the optimized SPE conditions, a method of SPE hyphenated to high-performance liquid chromatography-ultraviolet detection (HPLC-UV) for determination of the basic, neutral, and acidic drugs spiked in human serum was established. For the nine drugs, the linear ranges were all between 5.0 and 1000 μg L -1 with correlation coefficients (R 2 ) above 0.9990, and the limits of detection (LODs) were in the range of 0.8-2.3 μg L -1 . The intra-day and inter-day relative standard deviations (RSDs) were less than 5.3 and 8.8%, respectively. Graphical abstract Treating drugs in human serum by SPE with ternary mixed-mode silica sorbent.

Fast determination of octinoxate and oxybenzone uv filters in swimming pool waters by gas chromatography/mass spectrometry after solid-phase microextraction.

PubMed

Yılmazcan, Ö; Kanakaki, C; Izgi, B; Rosenberg, E

2015-07-01

A fast gas chromatography/mass spectrometry method was developed and validated for the analysis of the potential endocrine disrupters octinoxate and oxybenzone in swimming pool water samples based on the solvent-free solid-phase microextraction technique. The low-pressure gas chromatography/mass spectrometry method used for the fast identification of UV filter substances was compared to a conventional method in terms of sensitivity and speed. The fast method proposed resulted in 2 min runs, leading to an eightfold decrease in the total analysis time and a sevenfold improvement in detection limits. The main parameters affecting the solid-phase microextraction process were also studied in detail and the optimized conditions were as follows: fiber coating, polyacrylate; extraction mode, direct immersion; extraction temperature, 25°C; sample volume, 5 mL; extraction time 45 min; pH 6.5. Under the optimized conditions, a linear response was obtained in the concentration range of 0.5-25 μg/L with correlation coefficients in the range 0.990-0.999. The limits of detection were 0.17-0.29 μg/L, and the recoveries were 80-83%. Combined method uncertainty was assessed and found to be less than 7% for both analytes for concentrations equal to or higher than 5 μg/L. Pool water samples were analyzed to demonstrate the applicability of the proposed method. Neither octinoxate nor oxybenzone were detected in the swimming pool water samples at concentrations above the respective limits of detection. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Headspace-Solid Phase Microextraction Approach for Dimethylsulfoniopropionate Quantification in Solanum lycopersicum Plants Subjected to Water Stress

PubMed Central

Catola, Stefano; Kaidala Ganesha, Srikanta Dani; Calamai, Luca; Loreto, Francesco; Ranieri, Annamaria; Centritto, Mauro

2016-01-01

Dimethylsulfoniopropionate (DMSP) and dimethyl sulphide (DMS) are compounds found mainly in marine phytoplankton and in some halophytic plants. DMS is a globally important biogenic volatile in regulating of global sulfur cycle and planetary albedo, whereas DMSP is involved in the maintenance of plant-environment homeostasis. Plants emit minute amounts of DMS compared to marine phytoplankton and there is a need for hypersensitive analytic techniques to enable its quantification in plants. Solid Phase Micro Extraction from Head Space (HS-SPME) is a simple, rapid, solvent-free and cost-effective extraction mode, which can be easily hyphenated with GC-MS for the analysis of volatile organic compounds. Using tomato (Solanum lycopersicum) plants subjected to water stress as a model system, we standardized a sensitive and accurate protocol for detecting and quantifying DMSP pool sizes, and potential DMS emissions, in cryoextracted leaves. The method relies on the determination of DMS free and from DMSP pools before and after the alkaline hydrolysis via Headspace-Solid Phase Micro Extraction-Gas Chromatography-Mass Spectrometry (HS-SPME-GC-MS). We found a significant (2.5 time) increase of DMSP content in water-stressed leaves reflecting clear stress to the photosynthetic apparatus. We hypothesize that increased DMSP, and in turn DMS, in water-stressed leaves are produced by carbon sources other than direct photosynthesis, and function to protect plants either osmotically or as antioxidants. Finally, our results suggest that SPME is a powerful and suitable technique for the detection and quantification of biogenic gasses in trace amounts. PMID:27602039

KSC-08pd1383

NASA Image and Video Library

2008-05-14

CAPE CANAVERAL, Fla. -- Off Florida's central east coast, a support boat from a rescue training exercise, known as Mode VIII, returns to the Freedom Star, one of NASA's solid rocket booster retrieval ships from NASA's Kennedy Space Center. In support of, and with logistical support from, NASA, USSTRATCOM is hosting a major exercise involving Department of Defense, Department of Homeland Security, search and rescue (SAR) forces, including the 45th Space Wing at Patrick Air Force Base, which support space shuttle astronaut bailout contingency operations, known as Mode VIII. This exercise tests SAR capabilities to locate, recover and provide medical treatment for astronauts following a space shuttle launch phase open-ocean bailout. Participants include members of the U.S. Navy, U.S. Coast Guard, U.S. Air Force, and NASA's Kennedy Space Center and Johnson Space Center. Photo credit: NASA/Dimitri Gerondidakis

Evaluation of the JPL X-band 32 element active array. [for deep space communication

NASA Technical Reports Server (NTRS)

Boreham, J. F.; Postal, R. B.; Conroy, B. L.

1979-01-01

Tests performed on an X-band 32-element active array are described. Antenna pattern characteristics of the array were tested in its standard operating mode as well as several degraded performance modes, including failures of 1, 2, 3, 4, 8, 16, and 31 elements. Additionally, the array was characterized with the addition of a metallic shroud, and also characterized versus rf drive level and at a single off-axis electronic beamsteered position. Characterization was performed on several of the 3/4-watt, three-stage, X-band solid-state power amplifier modules. The characterization included swept amplitude response, amplitude and phase versus temperature from -20 to +60 C, and intermodulation distortion of selected modules. The array is described and conclusions and recommendations based upon the experience and results achieved are included.

Dynamics of the OH stretching mode in crystalline Ba(ClO4)2.3H2O

NASA Astrophysics Data System (ADS)

Hutzler, Daniel; Brunner, Christian; Petkov, Petko St.; Heine, Thomas; Fischer, Sighart F.; Riedle, Eberhard; Kienberger, Reinhard; Iglev, Hristo

2018-02-01

The vibrational dynamics of the OH stretching mode in Ba(ClO4)2 trihydrate are investigated by means of femtosecond infrared spectroscopy. The sample offers plane cyclic water trimers in the solid phase that feature virtually no hydrogen bond interaction between the water molecules. Selective excitation of the symmetric and asymmetric stretching leads to fast population redistribution, while simultaneous excitation yields quantum beats, which are monitored via a combination tone that dominates the overtone spectrum. The combination of steady-state and time-resolved spectroscopy with quantum chemical simulations and general theoretical considerations gives indication of various aspects of symmetry breakage. The system shows a joint population lifetime of 8 ps and a long-lived coherence between symmetric and asymmetric stretching, which decays with a time constant of 0.6 ps.

Acceleration effects in solid propellant rocket motors

NASA Technical Reports Server (NTRS)

Langhenry, M. T.

1986-01-01

The performance variations due to acceleration loads imposed on spinning solid propellant rocket motors are investigated. The four potentially most significant modes of acceleration-induced phenomena are identified from a study of the literature and modeled. The four modes are a mechanical mode which deals with deformations of the propellant and case: a thermodynamic mode which covers acceleration-induced combustion phenomena; a stress mode which covers the stressed propellant's effect on burn rate; and a gas dynamic mode which deals with changes in gas flow in the chamber and through the nozzle. Simplified models of each mode are developed or taken from the literature and are added to an internal ballistics evaluation computer program. The resulting analysis is the first to include all of the modes. In order to do this an original analysis of the mechanical and stress modes was necessary. However, the analysis shows that the stress mode is not important for the circular perforated grains studied. The other effects are shown to have a significant influence on solid rocket motor performance. The magnitude of the different mode effects are such that one may not be ignored over the others as has been done in the past. The results of the analysis are compared to published rocket motor data. The comparisons indicate an erosive burning effect that is a function of spin rate. A qualitative explanation of the erosive effect is presented.

Quantitative determination of acidic hydrolysis products of Chemical Weapons Convention related chemicals from aqueous and soil samples using ion-pair solid-phase extraction and in situ butylation.

PubMed

Pal Anagoni, Suresh; Kauser, Asma; Maity, Gopal; Upadhyayula, Vijayasarathi V R

2018-02-01

Chemical warfare agents such as organophosphorus nerve agents, mustard agents, and psychotomimetic agent like 3-quinuclidinylbenzilate degrade in the environment and form acidic degradation products, the analysis of which is difficult under normal analytical conditions. In the present work, a simultaneous extraction and derivatization method in which the analytes are butylated followed by gas chromatography and mass spectrometric identification of the analytes from aqueous and soil samples was carried out. The extraction was carried out using ion-pair solid-phase extraction with tetrabutylammonium hydroxide followed by gas chromatography with mass spectrometry in the electron ionization mode. Various parameters such as optimum concentration of the ion-pair reagent, pH of the sample, extraction solvent, and type of ion-pair reagent were optimized. The method was validated for various parameters such as linearity, accuracy, precision, and limit of detection and quantification. The method was observed to be linear from 1 to 1000 ng/mL range in selected ion monitoring mode. The extraction recoveries were in the range of 85-110% from the matrixes with the limit of quantification for alkyl phosphonic acids at 1 ng/mL, thiodiglycolic acid at 20 ng/mL, and benzilic acid at 50 ng/mL with intra- and interday precisions below 15%. The developed method was applied for the samples prepared in the scenario of challenging inspection. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A rapid and sensitive assay of perfluorocarboxylic acids in aqueous matrices by headspace solid phase microextraction-gas chromatography-triple quadrupole mass spectrometry.

PubMed

Monteleone, Marcello; Naccarato, Attilio; Sindona, Giovanni; Tagarelli, Antonio

2012-08-17

The work aims at developing a rapid and sensitive method for the quantification of perfluorocarboxylic acids in aqueous matrices. The proposed analytical approach is based on the use of solid phase microextraction in headspace mode after a fast derivatization of the carboxylate function by propylchloroformate/propanol mixture. Several fibers were evaluated and the optimization of the parameters affecting the SPME process was carried out using a central composite design. The optimum working conditions in terms of response values were achieved by performing analysis with CAR/PDMS fiber at room temperature, without addition of NaCl, with a sample volume of 6 ml and an extraction time of 10 min. Assay of PFCAs was performed by using a gas chromatography-triple quadrupole mass spectrometry (GC-QqQ MS) system in negative chemical ionization mode with ammonia as reagent gas. An overall evaluation of all analytical parameters shows that the proposed method provides satisfactory results. In particular, the observed accuracies, ranging from 84.4% to 116.8%, and the RSD values in the range 0.4% and 14.5% confirm the effectiveness of the developed protocol in the assay of PFCAs content in aqueous matrices. Moreover, LOD and LOQ values ranging from 0.08 to 6.6 ng l(-1) and from 0.17 to 14.3 ng l(-1), respectively, can be considered very satisfactory. None of the compounds were detected in six samples of river collected in Calabria. Copyright © 2012 Elsevier B.V. All rights reserved.

Raman studies of nanocomposites catalysts: temperature and pressure effects of CeAl, CeMn and NiAl oxides

NASA Astrophysics Data System (ADS)

da Silva, Antonio N.; Neto, Antonio B. S.; Oliveira, Alcemira C.; Junior, Manoel C.; Junior, Jose A. L.; Freire, Paulo T. C.; Filho, Josué M.; Oliveira, Alcineia C.; Lang, Rossano

2018-06-01

High temperature and pressure effects on the physicochemical properties of binary oxides catalysts were investigated. The nanocomposites catalysts comprising of CeAl, CeMn and NiAl were characterized through various physicochemical techniques. A study of the temperature and pressure induced phenomena monitored by Raman spectroscopy was proposed and discussed. Spectral modifications of the Raman modes belonging to the CeMn suggest structural changes in the solid due to the MnO2 phase oxidation with increasing temperature. The thermal expansion and lattice anharmonicity effects were observed on CeMn due to lack of stability of the lattice vacancies. The CeAl and NiAl composites presented crystallographic stability at low temperatures however, undertake a phase transformation of NiO/Al2O3 into NiAl2O4, mostly without any deformation in its structure with increasing the temperature. It was also inferred that the binary oxides are more stables in comparison with monoxides. Detailed pressure-dependent Raman measurements of the T2g phonon mode of CeMn and NiAl revealed that the pressure contributes to modify bonds length and reduces the particles sizes of the solids. On the contrary, high pressure on CeAl sample improved the stability with addition of Al2O3 in the CeO2 lattice. The results then suggest a good stability of CeAl and NiAl composite catalysts at high pressure and low temperature and show how to prospect of tuning the catalysis for surface reactions entirely through in situ spectroscopic investigations means.

New Phases of YBaCuGeO Superconductors Identified from X-ray Diffraction and Infra-red Absorption Measurements

NASA Astrophysics Data System (ADS)

Abo-Arais, Ahmed; Dawoud, Mohamad Ahmad Taher

2005-01-01

X-ray powder diffraction patterns and infra-red absorption spectra have been evaluated and analysed for the Y1 Ba2 Cu3 O7-d - Gex compound samples prepared by the solid state reaction with x values ranging from 0.0 to 1.13. All samples show bulk superconductivity above liquid nitrogen temperature using the levitation test (Meissner effect). Samples with Ge content up to x = 0.2 have offset Tc between 83K and 92K while the sample with x = 1.13 shows semiconducting behavior above 100K. As a result of the solid state interaction between YBCO and Ge, new phases are observed and determined, mainly three phases are concluded from X-ray powder diffraction analysis: (i) Ba2GeO4 (ii) Y2BaCuO5 (iii) BaCO3. The unit cell parameters a, b and c of the orthorhombic superconducting phase are calculated for all the prepared samples. The anisotropy factor is evaluated and related to the new structural phases in YBCO-Ge composite system. The I-R absorption spectra for the samples with orthorhombic symmetry have been determined. The phonon modes between ~ 400 cm-1 and 630 cm-1 are attributed to the Cu - O octahedron and pyramid vibrations for the CuO2 -planes and CuO-chains, while the peaks in the range from ~ 700 cm-1 to ~ 860 cm-1 may be due to defects such as the new phase Ba2GeO4 and the green phase Y2BaCuO5. The obtained results are discussed according to the superconductor - semi-conductor composite model and with the phonon-mediated charge transfer between CuO2 -planes and CuO- chains through apex oxygen (BaO).

Phase transformation strengthening of high-temperature superalloys

PubMed Central

Smith, T. M.; Esser, B. D.; Antolin, N.; Carlsson, A.; Williams, R. E. A.; Wessman, A.; Hanlon, T.; Fraser, H. L.; Windl, W.; McComb, D. W.; Mills, M. J.

2016-01-01

Decades of research has been focused on improving the high-temperature properties of nickel-based superalloys, an essential class of materials used in the hot section of jet turbine engines, allowing increased engine efficiency and reduced CO2 emissions. Here we introduce a new ‘phase-transformation strengthening' mechanism that resists high-temperature creep deformation in nickel-based superalloys, where specific alloying elements inhibit the deleterious deformation mode of nanotwinning at temperatures above 700 °C. Ultra-high-resolution structure and composition analysis via scanning transmission electron microscopy, combined with density functional theory calculations, reveals that a superalloy with higher concentrations of the elements titanium, tantalum and niobium encourage a shear-induced solid-state transformation from the γ′ to η phase along stacking faults in γ′ precipitates, which would normally be the precursors of deformation twins. This nanoscale η phase creates a low-energy structure that inhibits thickening of stacking faults into twins, leading to significant improvement in creep properties. PMID:27874007

Fracton-Elasticity Duality

NASA Astrophysics Data System (ADS)

Pretko, Michael; Radzihovsky, Leo

2018-05-01

Motivated by recent studies of fractons, we demonstrate that elasticity theory of a two-dimensional quantum crystal is dual to a fracton tensor gauge theory, providing a concrete manifestation of the fracton phenomenon in an ordinary solid. The topological defects of elasticity theory map onto charges of the tensor gauge theory, with disclinations and dislocations corresponding to fractons and dipoles, respectively. The transverse and longitudinal phonons of crystals map onto the two gapless gauge modes of the gauge theory. The restricted dynamics of fractons matches with constraints on the mobility of lattice defects. The duality leads to numerous predictions for phases and phase transitions of the fracton system, such as the existence of gauge theory counterparts to the (commensurate) crystal, supersolid, hexatic, and isotropic fluid phases of elasticity theory. Extensions of this duality to generalized elasticity theories provide a route to the discovery of new fracton models. As a further consequence, the duality implies that fracton phases are relevant to the study of interacting topological crystalline insulators.

Pipette-tip solid-phase extraction using polypyrrole as efficient adsorbent for extraction of avermectins and milbemycins in milk.

PubMed

Florez, Diego Hernando Ângulo; Teixeira, Roseane Andrade; da Silva, Ricky Cássio Santos; Pires, Bruna Carneiro; Dutra, Flávia Viana Avelar; Borges, Keyller Bastos

2018-05-01

In this work, we developed a HPLC method for the multidetermination of avermectins (AVM) (abamectin-ABA 1b and ABA 1a, eprinomectin-EPR, and ivermectin-IVM) and milbemycins (moxidectin-MOX) in milk samples using polypyrrole (PPy) as adsorbent material in pipette-tip solid-phase extraction (PT-PPy-SPE). PPy was characterized by scanning electron microscopy, thermogravimetric analysis, Fourier transform infrared spectroscopy, and X-ray diffraction and the data agreed with the literature. The sample preparation included the clean-up of the milk by protein precipitation (PP) with acetonitrile and extraction of the analytes by PT-PPy-SPE. The chromatographic method was developed in reverse phase and isocratic mode with flow rate at 1.2 mL min -1 and ultraviolet detection at 250 nm. The mobile phase composition was acetonitrile:methanol:water (55:25:20, v/v/v). The studied parameters and the optimized conditions for the sample preparation were washing solvent (300 μL water), volume and type of eluent (500 μL methanol), volume and pH of sample (1 mL and pH 10), amount of adsorbent material (50 mg PPy), and without addition of salt (NaCl). The method was linear over the concentration range from 20 to 3000 ng mL -1 with coefficients of correlation (r) ≥ 0.99 for all analytes and recoveries around 100%. The method developed and validated was used for the analyses of real milk samples from cow treated with Ivomec ® (IVM 3.5%), in which were found 21.51 ± 2.94 ng mL -1 of IVM. Finally, the results proved that PT-PPy-SPE coupled to HPLC-UV was economical, simple, and easy-to-perform technique. Graphical abstract Pipette-tip solid phase extraction using polypirrole as adsorbent material for determination of avermectins and milbemycins in milk.

Large-mode-area single-mode-output Neodymium-doped silicate glass all-solid photonic crystal fiber

PubMed Central

Li, Wentao; Chen, Danping; Qinling, Zhou; Hu, Lili

2015-01-01

We have demonstrated a 45 μm core diameter Neodymium-doped all-solid silicate glass photonic crystal fiber laser with a single mode laser output. The structure parameters and modes information of the fiber are both demonstrated by theoretical calculations using Finite Difference Time Domain (FDTD) method and experimental measurements. Maximum 0.8 W output power limited by launched pump power has been generated in 1064 nm with laser beam quality factor M2 1.18. PMID:26205850

Effect of organometallic fuel additives on nanoparticle emissions from a gasoline passenger car.

PubMed

Gidney, Jeremy T; Twigg, Martyn V; Kittelson, David B

2010-04-01

Particle size measurements were performed on the exhaust of a car operating on a chassis dynamometer fueled with standard gasoline and gasoline containing low levels of Pb, Fe, and Mn organometallic additives. When additives were present there was a distinct nucleation mode consisting primarily of sub-10 nm nanoparticles. At equal molar dosing Mn and Fe gave similar nanoparticle concentrations at the tailpipe, whereas Pb gave a considerably lower concentration. A catalytic stripper was used to remove the organic component of these particles and revealed that they were mainly solid and, because of their association with inorganic additives, presumably inorganic. Solid nucleation mode nanoparticles of similar size and concentration to those observed here from a gasoline engine with Mn and Fe additives have also been observed from modern heavy-duty diesel engines without aftertreatment at idle, but these solid particles are a small fraction of the primarily volatile nucleation mode particles emitted. The solid nucleation mode particles emitted by the diesel engines are likely derived from metal compounds in the lubrication oil, although carbonaceous particles cannot be ruled out. Significantly, most of these solid nanoparticles emitted by both engine types fall below the 23 nm cutoff of the PMP number regulation.

Development of all-solid-state coherent 589 nm light source: toward the realization of sodium lidar and laser guide star adaptive optics

NASA Astrophysics Data System (ADS)

Saito, Norihito; Akagawa, Kazuyuki; Kato, Mayumi; Takazawa, Akira; Hayano, Yutaka; Saito, Yoshihiko; Ito, Meguru; Takami, Hideki; Iye, Masanori; Wada, Satoshi

2006-12-01

We report an all-solid-state coherent 589 nm light source in single-pass sum-frequency generation (SFG) with actively mode-locked Nd:YAG lasers for the realization of sodium lidar and laser guide star adaptive optics. The Nd:YAG lasers are constructed as a LD-side-pumped configuration and are operated at 1064 and 1319 nm for 589 nm light generation in SFG. Output powers of 16.5 and 5.3 W at 1064 and 1319 nm are obtained with two pumping chambers. Each chamber consisted of three 80-W-LD arrays. Single transverse mode TEM 00; M2 ~1.1 is achieved with adjustment of cavity length considering thermal lens effect with increase of input LD power. The cavity length is set to approximately 1 m. Accordingly the mode-locked lasers are operated at a repetition rate of approximately 150 MHz. Synchronization of two pulse trains at 1064 and 1319 nm is accomplished by control of phase difference between two radio frequencies input in acousto-optic mode-lockers. Then temporal delay is controlled with a resolution of 37 ps/degree. Pump beams are mixed in periodically poled stoichiometric lithium tantalate (PPSLT) without an antireflection coating. The effective aperture and length of the crystal are 0.5 × 2 mm2 and 15 mm. When input intensity is set at 5.6 MW/cm , an average output power of 4.6 W is obtained at 589.159 nm. Precise tuning to the sodium D II line is accomplished by thermal control of etalons set in the Nd:YAG lasers. The output power at 589.159 nm is stably maintained within +/-1.2% for 8 hours.

77 FR 8946 - Notice of Application for Special Permits

Federal Register 2010, 2011, 2012, 2013, 2014

2012-02-15

... service motor vehicles for use in transporting a corrosive solid material in alternative packaging. (modes... the ``Nature of Application'' portion of the table below as follows: 1--Motor vehicle, 2--Rail freight... limitations and certain loading and stowage requirements. (mode 4) 15536-N ......... WavesinSolids LLC, 49 CFR...

40 CFR 227.32 - Liquid, suspended particulate, and solid phases of a material.

Code of Federal Regulations, 2010 CFR

2010-07-01

... solid phases of a material. 227.32 Section 227.32 Protection of Environment ENVIRONMENTAL PROTECTION... MATERIALS Definitions § 227.32 Liquid, suspended particulate, and solid phases of a material. (a) For the... obtained above prior to centrifugation and filtration. The solid phase includes all material settling to...

40 CFR 227.32 - Liquid, suspended particulate, and solid phases of a material.

Code of Federal Regulations, 2011 CFR

2011-07-01

... solid phases of a material. 227.32 Section 227.32 Protection of Environment ENVIRONMENTAL PROTECTION... MATERIALS Definitions § 227.32 Liquid, suspended particulate, and solid phases of a material. (a) For the... obtained above prior to centrifugation and filtration. The solid phase includes all material settling to...

Evaporation kinetics of sessile water droplets on micropillared superhydrophobic surfaces.

PubMed

Xu, Wei; Leeladhar, Rajesh; Kang, Yong Tae; Choi, Chang-Hwan

2013-05-21

Evaporation modes and kinetics of sessile droplets of water on micropillared superhydrophobic surfaces are experimentally investigated. The results show that a constant contact radius (CCR) mode and a constant contact angle (CCA) mode are two dominating evaporation modes during droplet evaporation on the superhydrophobic surfaces. With the decrease in the solid fraction of the superhydrophobic surfaces, the duration of a CCR mode is reduced and that of a CCA mode is increased. Compared to Rowan's kinetic model, which is based on the vapor diffusion across the droplet boundary, the change in a contact angle in a CCR (pinned) mode shows a remarkable deviation, decreasing at a slower rate on the superhydrophobic surfaces with less-solid fractions. In a CCA (receding) mode, the change in a contact radius agrees well with the theoretical expectation, and the receding speed is slower on the superhydrophobic surfaces with lower solid fractions. The discrepancy between experimental results and Rowan's model is attributed to the initial large contact angle of a droplet on superhydrophobic surfaces. The droplet geometry with a large contact angle results in a narrow wedge region of air along the contact boundary, where the liquid-vapor diffusion is significantly restricted. Such an effect becomes minor as the evaporation proceeds with the decrease in a contact angle. In both the CCR and CCA modes, the evaporative mass transfer shows the linear relationship between mass(2/3) and evaporation time. However, the evaporation rate is slower on the superhydrophobic surfaces, which is more significant on the surfaces with lower solid fractions. As a result, the superhydrophobic surfaces slow down the drying process of a sessile droplet on them.

Ultrasonic Imaging in Solids Using Wave Mode Beamforming.

PubMed

di Scalea, Francesco Lanza; Sternini, Simone; Nguyen, Thompson Vu

2017-03-01

This paper discusses some improvements to ultrasonic synthetic imaging in solids with primary applications to nondestructive testing of materials and structures. Specifically, the study proposes new adaptive weights applied to the beamforming array that are based on the physics of the propagating waves, specifically the displacement structure of the propagating longitudinal (L) mode and shear (S) mode that are naturally coexisting in a solid. The wave mode structures can be combined with the wave geometrical spreading to better filter the array (in a matched filter approach) and improve its focusing ability compared to static array weights. This paper also proposes compounding, or summing, images obtained from the different wave modes to further improve the array gain without increasing its physical aperture. The wave mode compounding can be performed either incoherently or coherently, in analogy with compounding multiple frequencies or multiple excitations. Numerical simulations and experimental testing demonstrate the potential improvements obtainable by the wave structure adaptive weights compared to either static weights in conventional delay-and-sum focusing, or adaptive weights based on geometrical spreading alone in minimum-variance distortionless response focusing.

Biological treatment of soils contaminated with hydrophobic organics using slurry- and solid-phase techniques

NASA Astrophysics Data System (ADS)

Cassidy, Daniel H.; Irvine, Robert L.

1995-10-01

Both slurry-phase and solid-phase bioremediation are effective ex situ soil decontamination methods. Slurrying is energy intensive relative to solid-phase treatment, but provides homogenization and uniform nutrient distribution. Limited contaminant bioavailability at concentrations above the required cleanup level reduces biodegradation rates and renders solid phase bioremediation more cost effective than complete treatment in a bio-slurry reactor. Slurrying followed by solid-phase bioremediation combines the advantages and minimizes the weaknesses of each treatment method when used alone. A biological treatment system consisting of slurrying followed by aeration in solid phase bioreactors was developed and tested in the laboratory using a silty clay loam contaminated with diesel fuel. The first set of experiments was designed to determine the impact of the water content and mixing time during slurrying on the rate an extent of contaminant removal in continuously aerated solid phase bioreactors. The second set of experiments compared the volatile and total diesel fuel removal in solid phase bioreactors using periodic and continuous aeration strategies. Results showed that slurrying for 1.5 hours at a water content less than saturation markedly increased the rate and extent of contaminant biodegradation in the solid phase bioreactors compared with soil having no slurry pretreatment. Slurrying the soil at or above its saturation moisture content resulted in lengthy dewatering times which prohibited aeration, thereby delaying the onset of biological treatment in the solid phase bioreactors. Results also showed that properly operated periodic aeration can provide less volatile contaminant removal and a grater fraction of biological contaminant removal than continuous aeration.

Overcoming nanoscale friction barriers in transition metal dichalcogenides

NASA Astrophysics Data System (ADS)

Cammarata, Antonio; Polcar, Tomas

2017-08-01

We study the atomic contributions to the nanoscale friction in layered M X2 (M =Mo , W; X =S , Se, Te) transition metal dichalcogenides by combining ab initio techniques with group-theoretical analysis. Starting from stable atomic configurations, we propose a computational method, named normal-modes transition approximation (NMTA), to individuate possible sliding paths from only the analysis of the phonon modes of the stable geometry. The method provides a way to decompose the atomic displacements realizing the layer sliding in terms of phonon modes of the stable structure, so as to guide the selection and tuning of specific atomic motions promoting M X2 sheets gliding, and to adjust the corresponding energy barrier. The present results show that main contributions to the nanoscale friction are due to few low frequency phonon modes, corresponding to rigid shifts of M X2 layers. We also provide further evidences that a previously reported Ti-doped MoS2 phase is a promising candidate as new material with enhanced tribologic properties. The NMTA approach can be exploited to tune the energetic and the structural features of specific phonon modes, and, thanks to its general formulation, can also be applied to any solid state system, irrespective of the chemical composition and structural topology.

Distinct ice patterns on solid surfaces with various wettabilities

PubMed Central

Liu, Jie; Zhu, Chongqin; Liu, Kai; Jiang, Ying; Song, Yanlin; Francisco, Joseph S.; Zeng, Xiao Cheng; Wang, Jianjun

2017-01-01

No relationship has been established between surface wettability and ice growth patterns, although ice often forms on top of solid surfaces. Here, we report experimental observations obtained using a process specially designed to avoid the influence of nucleation and describe the wettability-dependent ice morphology on solid surfaces under atmospheric conditions and the discovery of two growth modes of ice crystals: along-surface and off-surface growth modes. Using atomistic molecular dynamics simulation analysis, we show that these distinct ice growth phenomena are attributable to the presence (or absence) of bilayer ice on solid surfaces with different wettability; that is, the formation of bilayer ice on hydrophilic surface can dictate the along-surface growth mode due to the structural match between the bilayer hexagonal ice and the basal face of hexagonal ice (ice Ih), thereby promoting rapid growth of nonbasal faces along the hydrophilic surface. The dramatically different growth patterns of ice on solid surfaces are of crucial relevance to ice repellency surfaces. PMID:29073045

Distinct ice patterns on solid surfaces with various wettabilities.

PubMed

Liu, Jie; Zhu, Chongqin; Liu, Kai; Jiang, Ying; Song, Yanlin; Francisco, Joseph S; Zeng, Xiao Cheng; Wang, Jianjun

2017-10-24

No relationship has been established between surface wettability and ice growth patterns, although ice often forms on top of solid surfaces. Here, we report experimental observations obtained using a process specially designed to avoid the influence of nucleation and describe the wettability-dependent ice morphology on solid surfaces under atmospheric conditions and the discovery of two growth modes of ice crystals: along-surface and off-surface growth modes. Using atomistic molecular dynamics simulation analysis, we show that these distinct ice growth phenomena are attributable to the presence (or absence) of bilayer ice on solid surfaces with different wettability; that is, the formation of bilayer ice on hydrophilic surface can dictate the along-surface growth mode due to the structural match between the bilayer hexagonal ice and the basal face of hexagonal ice (ice I h ), thereby promoting rapid growth of nonbasal faces along the hydrophilic surface. The dramatically different growth patterns of ice on solid surfaces are of crucial relevance to ice repellency surfaces. Published under the PNAS license.

Grating enhanced solid-state laser amplifiers

DOEpatents

Erlandson, Alvin C.; Britten, Jerald A.

2010-11-09

A novel method and apparatus for suppressing ASE and parasitic oscillation modes in a high average power laser is introduced. Such an invention, as disclosed herein, uses diffraction gratings to increase gain, stored energy density, and pumping efficiency of solid-state laser gain media, such as, but not limited to rods, disks and slabs. By coupling predetermined gratings to solid-state gain media, such as crystal or ceramic laser gain media, ASE and parasitic oscillation modes can be effectively suppressed.

Compression selective solid-state chemistry

NASA Astrophysics Data System (ADS)

Hu, Anguang

Compression selective solid-state chemistry refers to mechanically induced selective reactions of solids under thermomechanical extreme conditions. Advanced quantum solid-state chemistry simulations, based on density functional theory with localized basis functions, were performed to provide a remarkable insight into bonding pathways of high-pressure chemical reactions in all agreement with experiments. These pathways clearly demonstrate reaction mechanisms in unprecedented structural details, showing not only the chemical identity of reactive intermediates but also how atoms move along the reaction coordinate associated with a specific vibrational mode, directed by induced chemical stress occurred during bond breaking and forming. It indicates that chemical bonds in solids can break and form precisely under compression as we wish. This can be realized through strongly coupling of mechanical work to an initiation vibrational mode when all other modes can be suppressed under compression, resulting in ultrafast reactions to take place isothermally in a few femtoseconds. Thermodynamically, such reactions correspond to an entropy minimum process on an isotherm where the compression can force thermal expansion coefficient equal to zero. Combining a significantly brief reaction process with specific mode selectivity, both statistical laws and quantum uncertainty principle can be bypassed to precisely break chemical bonds, establishing fundamental principles of compression selective solid-state chemistry. Naturally this leads to understand the ''alchemy'' to purify, grow, and perfect certain materials such as emerging novel disruptive energetics.

Phase-sensitive terahertz spectroscopy with backward-wave oscillators in reflection mode.

PubMed

Pronin, A V; Goncharov, Yu G; Fischer, T; Wosnitza, J

2009-12-01

In this article we describe a method which allows accurate measurements of the complex reflection coefficient r = absolute value(r) x exp(i phi(R)) of a solid at frequencies of 1-50 cm(-1) (30 GHz-1.5 THz). Backward-wave oscillators are used as sources for monochromatic coherent radiation tunable in frequency. The amplitude of the complex reflection (the reflectivity) is measured in a standard way, while the phase shift, introduced by the reflection from the sample surface, is measured using a Michelson interferometer. This method is particular useful for nontransparent samples, where phase-sensitive transmission measurements are not possible. The method requires no Kramers-Kronig transformation in order to extract the sample's electrodynamic properties (such as the complex dielectric function or complex conductivity). Another area of application of this method is the study of magnetic materials with complex dynamic permeabilities different from unity at the measurement frequencies (for example, colossal-magnetoresistance materials and metamaterials). Measuring both the phase-sensitive transmission and the phase-sensitive reflection allows for a straightforward model-independent determination of the dielectric permittivity and magnetic permeability of such materials.

Phase-sensitive terahertz spectroscopy with backward-wave oscillators in reflection mode

NASA Astrophysics Data System (ADS)

Pronin, A. V.; Goncharov, Yu. G.; Fischer, T.; Wosnitza, J.

2009-12-01

In this article we describe a method which allows accurate measurements of the complex reflection coefficient r̂=|r̂|ṡexp(iφR) of a solid at frequencies of 1-50 cm-1 (30 GHz-1.5 THz). Backward-wave oscillators are used as sources for monochromatic coherent radiation tunable in frequency. The amplitude of the complex reflection (the reflectivity) is measured in a standard way, while the phase shift, introduced by the reflection from the sample surface, is measured using a Michelson interferometer. This method is particular useful for nontransparent samples, where phase-sensitive transmission measurements are not possible. The method requires no Kramers-Kronig transformation in order to extract the sample's electrodynamic properties (such as the complex dielectric function or complex conductivity). Another area of application of this method is the study of magnetic materials with complex dynamic permeabilities different from unity at the measurement frequencies (for example, colossal-magnetoresistance materials and metamaterials). Measuring both the phase-sensitive transmission and the phase-sensitive reflection allows for a straightforward model-independent determination of the dielectric permittivity and magnetic permeability of such materials.

Raman scattering in HfxZr1-xO2 nanoparticles

NASA Astrophysics Data System (ADS)

Robinson, Richard D.; Tang, Jing; Steigerwald, Michael L.; Brus, Louis E.; Herman, Irving P.

2005-03-01

Raman spectroscopy demonstrates that ˜5nm dimension HfxZr1-xO2 nanocrystals prepared by a nonhydrolytic sol-gel synthesis method are solid solutions of hafnia and zirconia, with no discernable segregation within the individual nanoparticles. Zirconia-rich particles are tetragonal and ensembles of hafnia-rich particles show mixed tetragonal/monoclinic phases. Sintering at 1200 °C produces larger particles (20-30 nm) that are monoclinic. A simple lattice dynamics model with composition-averaged cation mass and scaled force constants is used to understand how the Raman mode frequencies vary with composition in the tetragonal HfxZr1-xO2 nanoparticles. Background luminescence from these particles is minimized after oxygen treatment, suggesting possible oxygen defects in the as-prepared particles. Raman scattering is also used to estimate composition and the relative fractions of tetragonal and monoclinic phases. In some regimes there are mixed phases, and Raman analysis suggests that in these regimes the tetragonal phase particles are relatively rich in zirconium and the monoclinic phase particles are relatively rich in hafnium.

Extraction of acidic degradation products of organophosphorus chemical warfare agents. Comparison between silica and mixed-mode strong anion-exchange cartridges.

PubMed

Kanaujia, Pankaj K; Pardasani, Deepak; Gupta, A K; Kumar, Rajesh; Srivastava, R K; Dubey, D K

2007-08-17

The analysis of alkyl alkylphosphonic acids (AAPAs) and alkylphosphonic acids (APAs), the hydrolyzed products of nerve agents, constitutes an important aspect for verifying the compliance to the Chemical weapons convention (CWC). This work devotes on the development of solid-phase extraction method using polymeric mixed-mode strong anion-exchange (Oasis MAX) cartridges for extraction of AAPAs and APAs from water. The extracted analytes were analyzed by GC-MS under full scan and selected ion monitoring mode. The extraction efficiencies of MAX and silica-based anion-exchange cartridges were compared, and results revealed that MAX sorbents yielded better recoveries. Extraction parameters, such as loading capacity, extraction solvent, its volume, and washing solvent were optimized. Best recoveries were obtained using 1 mL of acidic methanol (0.1 M), and limits of detection could be achieved up to 5 x 10(-4) microg mL(-1) (in SIM) and 0.05 microg mL(-1) in full scan mode. The method was successfully employed for the detection and identification of alkylphosphonic acids present in soil sample sent by the Organization for Prohibition of Chemical Weapons (OPCW) in the official proficiency tests.

Frequency-bin entanglement of ultra-narrow band non-degenerate photon pairs

NASA Astrophysics Data System (ADS)

Rieländer, Daniel; Lenhard, Andreas; Jime`nez Farìas, Osvaldo; Máttar, Alejandro; Cavalcanti, Daniel; Mazzera, Margherita; Acín, Antonio; de Riedmatten, Hugues

2018-01-01

We demonstrate frequency-bin entanglement between ultra-narrowband photons generated by cavity enhanced spontaneous parametric down conversion. Our source generates photon pairs in widely non-degenerate discrete frequency modes, with one photon resonant with a quantum memory material based on praseodymium doped crystals and the other photon at telecom wavelengths. Correlations between the frequency modes are analyzed using phase modulators and narrowband filters before detection. We show high-visibility two photon interference between the frequency modes, allowing us to infer a coherent superposition of the modes. We develop a model describing the state that we create and use it to estimate optimal measurements to achieve a violation of the Clauser-Horne (CH) Bell inequality under realistic assumptions. With these settings we perform a Bell test and show a significant violation of the CH inequality, thus proving the entanglement of the photons. Finally we demonstrate the compatibility with a quantum memory material by using a spectral hole in the praseodymium (Pr) doped crystal as spectral filter for measuring high-visibility two-photon interference. This demonstrates the feasibility of combining frequency-bin entangled photon pairs with Pr-based solid state quantum memories.

Phased laser diode array permits selective excitation of ultrasonic guided waves in coated bone-mimicking tubes

NASA Astrophysics Data System (ADS)

Moilanen, Petro; Salmi, Ari; Kilappa, Vantte; Zhao, Zuomin; Timonen, Jussi; Hæggström, Edward

2017-10-01

This paper validates simulation predictions, which state that specific modes could be enhanced in quantitative ultrasonic bone testing. Tunable selection of ultrasonic guided wave excitation is useful in non-destructive testing since it permits the mediation of energy into diagnostically useful modes while reducing the energy mediated into disturbing contributions. For instance, it is often challenging to distinguish and extract the useful modes from ultrasound signals measured in bone covered by a soft tissue. We show that a laser diode array can selectively excite ultrasound in bone mimicking phantoms. A fiber-coupled diode array (4 elements) illuminated two solid tubes (2-3 mm wall thickness) embraced by an opaque soft-tissue mimicking elastomer coating (5 mm thick). A predetermined time delay matching the selected mode and frequency was employed between the outputs of the elements. The generated ultrasound was detected by a 215 kHz piezo receiver. Our results suggest that this array reduces the disturbances caused by the elastomer cover and so pave way to permit non-contacting in vivo guided wave ultrasound assessment of human bones. The implementation is small, inexpensive, and robust in comparison with the conventional pulsed lasers.

First-Principles Calculations of Lattice Dynamics in La_2CuO_4

NASA Astrophysics Data System (ADS)

Wang, C.-Z.; Yu, Rici; Krakauer, Henry

1998-03-01

To investigate wavevector-dependent lattice vibrational properties of the high-temperature cuprate superconductor La_2-xSr_xCuO_4, we have performed first principles calculations for tetragonal I4/mmm La_2CuO_4, using the linear response LAPW method(R. Yu and H. Krakauer, Phys. Rev. B 49), 4467 (1994). Phonon frequencies and polarization vectors are obtained throughout the Brillouin zone. Generally good agreement is obtained with experiment, but we underestimate the frequencies of the low lying modes, which involve either motions of the apical oxygen atoms parallel to the CuO2 planes or motions of the plane O atoms along the c-axis. The discrepancy may be due to anharmonic coupling of these modes(R. Cohen, W. Pickett, and H. Krakauer, Phys. Rev. Lett. 62), 831 (1989)^,(D. J. Singh, Solid State Commun. 98), 575 (1996). The X point tilt phonon mode is found to be the most unstable mode, consistent with previous frozen phonon calculations^3 and the observed phase transition to the orthorhombic structure at low temperature. The results will be discussed in comparison with previous calculations^3,4 and experiment.

History of Solid Rockets

NASA Technical Reports Server (NTRS)

Green, Becky; Hales, Christy

2017-01-01

Solid rockets were created by accident and their design and uses have evolved over time. Solid rockets are more simple and reliable than liquid rockets, but they have reduced performance capability. All solid rockets have a similar set of failure modes.

Determining solid-fluid interface temperature distribution during phase change of cryogenic propellants using transient thermal modeling

NASA Astrophysics Data System (ADS)

Bellur, K.; Médici, E. F.; Hermanson, J. C.; Choi, C. K.; Allen, J. S.

2018-04-01

Control of boil-off of cryogenic propellants is a continuing technical challenge for long duration space missions. Predicting phase change rates of cryogenic liquids requires an accurate estimation of solid-fluid interface temperature distributions in regions where a contact line or a thin liquid film exists. This paper described a methodology to predict inner wall temperature gradients with and without evaporation using discrete temperature measurements on the outer wall of a container. Phase change experiments with liquid hydrogen and methane in cylindrical test cells of various materials and sizes were conducted at the Neutron Imaging Facility at the National Institute of Standards and Technology. Two types of tests were conducted. The first type of testing involved thermal cycling of an evacuated cell (dry) and the second involved controlled phase change with cryogenic liquids (wet). During both types of tests, temperatures were measured using Si-diode sensors mounted on the exterior surface of the test cells. Heat is transferred to the test cell by conduction through a helium exchange gas and through the cryostat sample holder. Thermal conduction through the sample holder is shown to be the dominant mode with the rate of heat transfer limited by six independent contact resistances. An iterative methodology is employed to determine contact resistances between the various components of the cryostat stick insert, test cell and lid using the dry test data. After the contact resistances are established, inner wall temperature distributions during wet tests are calculated.

Observation of a new surface mode on a fluid-saturated permeable solid

NASA Astrophysics Data System (ADS)

Nagy, Peter B.

1992-06-01

Almost ten years ago, S. Feng and D. L. Johnson predicted the presence of a new surface mode on a fluid/fluid-saturated porous solid interface with closed surface pores [J. Acoust. Soc. Am. 74, 906 (1983)]. We found that, due to surface tension, practically closed-pore boundary conditions can prevail at an interface between a nonwetting fluid (e.g., air) and a porous solid saturated with a wetting fluid (e.g., water or alcohol). Surface wave velocity and attenuation measurements were made on alcohol-saturated porous sintered glass at 100 kHz. The experimental results show clear evidence of the new ``slow'' surface mode predicted by Feng and Johnson.

Atmospheric resonances of the Rayleigh and tsunami normal modes and its sensitivity to local time and geographical location.

NASA Astrophysics Data System (ADS)

Rakoto, V.; Astafyeva, E.; Lognonne, P. H.

2017-12-01

It is known that natural hazard events, such as earthquakes, tsunamis, volcano eruptions, etc. can generate atmospheric/ionospheric perturbations. During earthquakes, vertical displacements of the ground or of the ocean floor generate acoustic-gravity waves that further propagate upward in the upper atmosphere and ionosphere. In turn, tsunamis propagating in the open sea, generate gravity waves which propagate obliquely and reach the ionosphere in 45-60 min. The properties of the atmospheric "channel" in the vertical and oblique propagation depend on a variety of factors such as solar and geomagnetic conditions, latitude, local time, season, and their influence on propagation and properties of co-seismic and co-tsunamic perturbations is not well understood yet. In this work, we use present a detailed study of the coupling efficiency between solid earth, ocean and atmosphere. For this purpose, we use the normal mode technique extended to the whole solid Earth-ocean-atmosphere system. In our study, we focus on the Rayleigh modes (solid modes) and tsunami modes (oceanic modes). As the normal modes amplitude are also depending on the spatial and temporal variation of the structure of the atmosphere, we also performed a sensitivity study location of the normal modes amplitude with local time and geographical position.

THz Time-Domain Spectroscopy of Interstellar Ice Analogs

NASA Astrophysics Data System (ADS)

Ioppolo, Sergio; McGuire, Brett A.; de Vries, Xander; Carroll, Brandon; Allodi, Marco; Blake, Geoffrey

2015-08-01

The unambiguous identification of nearly 200 molecular species in different astronomical environments proves that our cosmos is a ‘Molecular Universe’. The cumulative outcome of recent observations, laboratory studies, and astrochemical models indicates that there is a strong interplay between the gas and the solid phase throughout the process of forming molecules in space. Observations of interstellar ices are generally limited to lines-of-sight along which infrared absorption spectroscopy is possible. Therefore, the identification of more complex prebiotic molecules in the mid-IR is difficult because of their low expected interstellar abundances and the overlap of their absorption features with those from the more abundant species. In the THz region, telescopes can detect Interstellar ices in emission or absorption against dust continuum. Thus, THz searches do not require a background point source. Moreover, since THz spectra are the fingerprint of inter- and intramolecular forces, complex species can present unique modes that do not overlap with those from simpler, more abundant molecules. THz modes are also sensitive to temperature and phase changes in the ice. Therefore, spectroscopy at THz frequencies has the potential to better characterize the physics and chemistry of the ISM. Currently, the Herschel Space Telescope, SOFIA, and ALMA databases contain a vast amount of new THz spectral data that require THz laboratory spectra for interpretation. The latter, however, are largely lacking. We have recently constructed a new THz time-domain spectroscopy system operating in the range between 0.3 - 7.5 THz. This work focuses on the laboratory investigation of the composition and structure of the most abundant interstellar ice analogs compared to some more complex species. Different temperatures, mixing ratios, and matrix isolation experiments will be shown. The ultimate goal of this research is to provide the scientific community with an extensive THz ice-database, which will allow quantitative studies of the ISM, and guide future astronomical observations of species in the solid phase.

Fast liquid chromatographic-tandem mass spectrometric method using mixed-mode phase chromatography and solid phase extraction for the determination of 12 mono-hydroxylated brominated diphenyl ethers in human serum.

PubMed

Petropoulou, Syrago-Styliani E; Duong, Wendy; Petreas, Myrto; Park, June-Soo

2014-08-22

Hydroxylated polybrominated diphenyl ethers (OH-PBDEs) are formed from the oxidative metabolism of polybrominated diphenyl ethers (PBDEs) in humans, rats and mice, but their quantitation in human blood and other matrices with liquid chromatography-mass spectrometric techniques has been a challenge. In this study, a novel analytical method was developed and validated using only 250 μL of human serum for the quantitation of twelve OH-PBDEs, fully chromatographically separated in a 15 min analytical run. This method includes two novel approaches: an enzymatic hydrolysis procedure and a chromatographic separation using a mixed mode chromatography column. The enzymatic hydrolysis (EH) was found critical for 4'-OH-BDE17, which was not detectable without it. For the sample clean up, a solid phase extraction protocol was developed and validated for the extraction of the 12 congeners from human serum. In addition, for the first time baseline resolution of two components was achieved that correspond to a single peak previously identified as 6'-OH-BDE99. The method was validated for linearity, accuracy, precision, matrix effects, limit of quantification, limit of detection, sample stability and overall efficiency. Recoveries (absolute and relative) ranged from 66 to 130% with relative standard deviations <21% for all analytes. Limit of detection and quantitation ranged from 4 to 90 pg mL(-1) and 6-120 pg mL(-1), respectively, with no carry over effects. This method was applied in ten commercially available human serum samples from the general US population. The mean values of the congeners detected in all samples are 4'-OH-BDE17 (34.2 pg mL(-1)), 4-OH-BDE42 (33.9 pg mL(-1)), 5-OH-BDE47 (17.5 pg mL(-1)) and 4'-OH-BDE49 (12.4 pg mL(-1)). Copyright © 2014 Elsevier B.V. All rights reserved.

Analytical modeling of localized surface plasmon resonance in heterostructure copper sulfide nanocrystals

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

Caldwell, Andrew H.; Ha, Don-Hyung; Robinson, Richard D., E-mail: rdr82@cornell.edu

2014-10-28

Localized surface plasmon resonance (LSPR) in semiconductor nanocrystals is a relatively new field of investigation that promises greater tunability of plasmonic properties compared to metal nanoparticles. A novel process by which the LSPR in semiconductor nanocrystals can be altered is through heterostructure formation arising from solution-based cation exchange. Herein, we describe the development of an analytical model of LSPR in heterostructure copper sulfide-zinc sulfide nanocrystals synthesized via a cation exchange reaction between copper sulfide (Cu{sub 1.81}S) nanocrystals and Zn ions. The cation exchange reaction produces dual-interface, heterostructure nanocrystals in which the geometry of the copper sulfide phase can be tunedmore » from a sphere to a thin disk separating symmetrically-grown sulfide (ZnS) grains. Drude model electronic conduction and Mie-Gans theory are applied to describe how the LSPR wavelength changes during cation exchange, taking into account the morphology evolution and changes to the local permittivity. The results of the modeling indicate that the presence of the ZnS grains has a significant effect on the out-of-plane LSPR mode. By comparing the results of the model to previous studies on solid-solid phase transformations of copper sulfide in these nanocrystals during cation exchange, we show that the carrier concentration is independent of the copper vacancy concentration dictated by its atomic phase. The evolution of the effective carrier concentration calculated from the model suggests that the out-of-plane resonance mode is dominant. The classical model was compared to a simplified quantum mechanical model which suggested that quantum mechanical effects become significant when the characteristic size is less than ∼8 nm. Overall, we find that the analytical models are not accurate for these heterostructured semiconductor nanocrystals, indicating the need for new model development for this emerging field.« less

Duffing revisited: phase-shift control and internal resonance in self-sustained oscillators

NASA Astrophysics Data System (ADS)

Arroyo, Sebastián I.; Zanette, Damián H.

2016-01-01

We address two aspects of the dynamics of the forced Duffing oscillator which are relevant to the technology of micromechanical devices and, at the same time, have intrinsic significance to the field of nonlinear oscillating systems. First, we study the stability of periodic motion when the phase shift between the external force and the oscillation is controlled - contrary to the standard case, where the control parameter is the frequency of the force. Phase-shift control is the operational configuration under which self-sustained oscillators - and, in particular, micromechanical oscillators - provide a frequency reference useful for time keeping. We show that, contrary to the standard forced Duffing oscillator, under phase-shift control oscillations are stable over the whole resonance curve, and provide analytical approximate expressions for the time dependence of the oscillation amplitude and frequency during transients. Second, we analyze a model for the internal resonance between the main Duffing oscillation mode and a higher-harmonic mode of a vibrating solid bar clamped at its two ends. We focus on the stabilization of the oscillation frequency when the resonance takes place, and present preliminary experimental results that illustrate the phenomenon. This synchronization process has been proposed to counteract the undesirable frequency-amplitude interdependence in nonlinear time-keeping micromechanical devices. Supplementary material in the form of one pdf file and one gif file available from the Journal web page at http://dx.doi.org/10.1140/epjb/e2015-60517-3

Single-phase and two-phase anaerobic digestion of fruit and vegetable waste: Comparison of start-up, reactor stability and process performance

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

Ganesh, Rangaraj; Torrijos, Michel, E-mail: michel.torrijos@supagro.inra.fr; Sousbie, Philippe

Highlights: • Single-phase and two-phase systems were compared for fruit and vegetable waste digestion. • Single-phase digestion produced a methane yield of 0.45 m{sup 3} CH{sub 4}/kg VS and 83% VS removal. • Substrate solubilization was high in acidification conditions at 7.0 kg VS/m{sup 3} d and pH 5.5–6.2. • Energy yield was lower by 33% for two-phase system compared to the single-phase system. • Simple and straight-forward operation favored single phase process over two-phase process. - Abstract: Single-phase and two-phase digestion of fruit and vegetable waste were studied to compare reactor start-up, reactor stability and performance (methane yield, volatilemore » solids reduction and energy yield). The single-phase reactor (SPR) was a conventional reactor operated at a low loading rate (maximum of 3.5 kg VS/m{sup 3} d), while the two-phase system consisted of an acidification reactor (TPAR) and a methanogenic reactor (TPMR). The TPAR was inoculated with methanogenic sludge similar to the SPR, but was operated with step-wise increase in the loading rate and with total recirculation of reactor solids to convert it into acidification sludge. Before each feeding, part of the sludge from TPAR was centrifuged, the centrifuge liquid (solubilized products) was fed to the TPMR and centrifuged solids were recycled back to the reactor. Single-phase digestion produced a methane yield of 0.45 m{sup 3} CH{sub 4}/kg VS fed and VS removal of 83%. The TPAR shifted to acidification mode at an OLR of 10.0 kg VS/m{sup 3} d and then achieved stable performance at 7.0 kg VS/m{sup 3} d and pH 5.5–6.2, with very high substrate solubilization rate and a methane yield of 0.30 m{sup 3} CH{sub 4}/kg COD fed. The two-phase process was capable of high VS reduction, but material and energy balance showed that the single-phase process was superior in terms of volumetric methane production and energy yield by 33%. The lower energy yield of the two-phase system was due to the loss of energy during hydrolysis in the TPAR and the deficit in methane production in the TPMR attributed to COD loss due to biomass synthesis and adsorption of hard COD onto the flocs. These results including the complicated operational procedure of the two-phase process and the economic factors suggested that the single-phase process could be the preferred system for FVW.« less

Controlling the Localization of Liquid Droplets in Polymer Matrices by Evaporative Lithography.

PubMed

Zhao, Huaixia; Xu, Jiajia; Jing, Guangyin; Prieto-López, Lizbeth Ofelia; Deng, Xu; Cui, Jiaxi

2016-08-26

Localized inclusions of liquids provide solid materials with many functions, such as self-healing, secretion, and tunable mechanical properties, in a spatially controlled mode. However, a strategy to control the distribution of liquid droplets in solid matrices directly obtained from a homogeneous solution has not been reported thus far. Herein, we describe an approach to selectively localize liquid droplets in a supramolecular gel directly obtained from its solution by using evaporative lithography. In this process, the formation of droplet-embedded domains occurs in regions of free evaporation where the non-volatile liquid is concentrated and undergoes a phase separation to create liquid droplets prior to gelation, while a homogeneous gel matrix is formed in the regions of hindered evaporation. The different regions of a coating with droplet embedment patterns display different secretion abilities, enabling the control of the directional movement of water droplets. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Scaling for hard-sphere colloidal glasses near jamming

NASA Astrophysics Data System (ADS)

Zargar, Rojman; DeGiuli, Eric; Bonn, Daniel

2016-12-01

Hard-sphere colloids are model systems in which to study the glass transition and universal properties of amorphous solids. Using covariance matrix analysis to determine the vibrational modes, we experimentally measure here the scaling behavior of the density of states, shear modulus, and mean-squared displacement (MSD) in a hard-sphere colloidal glass. Scaling the frequency with the boson-peak frequency, we find that the density of states at different volume fractions all collapse on a single master curve, which obeys a power law in terms of the scaled frequency. Below the boson peak, the exponent is consistent with theoretical results obtained by real-space and phase-space approaches to understanding amorphous solids. We find that the shear modulus and the MSD are nearly inversely proportional, and show a singular power-law dependence on the distance from random close packing. Our results are in very good agreement with the theoretical predictions.

Seasonal multiphase equilibria in the atmospheres of Titan and Pluto

NASA Astrophysics Data System (ADS)

Tan, S. P.; Kargel, J. S.

2017-12-01

At the extremely low temperatures in Titan's upper troposphere and on Pluto's surface, the atmospheres as a whole are subject to freeze into solid solutions, not pure ices. The presence of the solid phases introduces conditions with rich phase equilibria upon seasonal changes, even if the temperature undergoes only small changes. For the first time, the profile of atmospheric methane in Titan's troposphere will be reproduced complete with the solid solutions. This means that the freezing point, i.e. the altitude where the first solid phase appears, is determined. The seasonal change will also be evaluated both at the equator and the northern polar region. For Pluto, also for the first time, the seasonal solid-vapor equilibria will be evaluated. The fate of the two solid phases, the methane-rich and carbon-monoxide-rich solid solutions, will be analyzed upon temperature and pressure changes. Such investigations are enabled by the development of a molecular-based thermodynamic model for cryogenic chemical systems, referred to as CRYOCHEM, which includes solid solutions in its phase-equilibria calculations. The atmospheres of Titan and Pluto are modeled as ternary gas mixtures: nitrogen-methane-ethane and nitrogen-methane-carbon monoxide, respectively. Calculations using CRYOCHEM can provide us with compositions not only in two-phase equilibria, but also that in three-phase equilibria. Densities of all phases involved will also be calculated. For Titan, density inversion between liquid and solid phases will be identified and presented. In the inversion, the density of solid phase is less than that in the liquid phase. The method and results of this work will be useful for further investigations and modeling on the atmospheres of Titan, Pluto, and other bodies with similar conditions in the Solar System and beyond.

Helicon modes in uniform plasmas. I. Low m modes

NASA Astrophysics Data System (ADS)

Urrutia, J. M.; Stenzel, R. L.

2015-09-01

Helicons are whistler modes with azimuthal wave numbers. They arise in bounded gaseous and solid state plasmas, but the present work shows that very similar modes also exist in unbounded uniform plasmas. The antenna properties determine the mode structure. A simple antenna is a magnetic loop with dipole moment aligned either along or across the ambient background magnetic field B0. For such configurations, the wave magnetic field has been measured in space and time in a large and uniform laboratory plasma. The observed wave topology for a dipole along B0 is similar to that of an m = 0 helicon mode. It consists of a sequence of alternating whistler vortices. For a dipole across B0, an m = 1 mode is excited which can be considered as a transverse vortex which rotates around B0. In m = 0 modes, the field lines are confined to each half-wavelength vortex while for m = 1 modes they pass through the entire wave train. A subset of m = 1 field lines forms two nested helices which rotate in space and time like corkscrews. Depending on the type of the antenna, both m = + 1 and m = -1 modes can be excited. Helicons in unbounded plasmas also propagate transverse to B0. The transverse and parallel wave numbers are about equal and form oblique phase fronts as in whistler Gendrin modes. By superimposing small amplitude fields of several loop antennas, various antenna combinations have been created. These include rotating field antennas, helical antennas, and directional antennas. The radiation efficiency is quantified by the radiation resistance. Since helicons exist in unbounded laboratory plasmas, they can also arise in space plasmas.

Bidentate urea-based chiral selectors for enantioselective high performance liquid chromatography: synthesis and evaluation of "Crab-like" stationary phases.

PubMed

Kotoni, Dorina; Villani, Claudio; Bell, David S; Capitani, Donatella; Campiglia, Pietro; Gasparrini, Francesco

2013-07-05

A rational approach for the design and preparation of two new "Crab-like" totally synthetic, brush-type chiral stationary phases is presented. Enantiopure diamines, namely 1,2-diaminocyclohexane and 1,2-diphenyl-1,2-ethylene-diamine were treated with 3-(triethoxysilyl)propyl isocyanate, to yield reactive ureido selectors that were eventually attached to unmodified silica particles through a stable, bidentate tether, through a facile two-step one-pot procedure. A full chemical characterization of the new materials has been obtained through solid-state NMR (both (29)Si and (13)C CPMAS) spectroscopy. Columns packed with the two Crab-like chiral stationary phases allow for different mechanisms of separation: normal phase liquid chromatography, reversed phase liquid chromatography and polar organic mode and show a high stability at basic pH values. In particular, the Crab-like column containing the 1,2-diphenyl-1,2-ethylene-diamine selector proved a promising candidate for the resolution of a wide range of racemates (including benzodiazepines, N-derivatized amino acids, and free carboxylic acids) both in normal phase and polar organic mode. An Hmin of 9.57 at a μsf of 0.80mm/s (corresponding to 0.8mL/min) was obtained through van Deemter analysis, based on toluene, for the Crab-like column with the 1,2-diphenyl-1,2-ethylene-diamine selector (250mm×4.6mm I.D.), with a calculated reduced height equivalent to a theoretical plate (h) of only 1.91. Finally, comparative studies were performed with a polymeric commercially available P-CAP-DP column in order to evaluate enantioselectivity and resolution of the Crab-like columns. Copyright © 2013 Elsevier B.V. All rights reserved.

Magnetic solid phase extraction and gas chromatography-mass spectrometrical analysis of sixteen polycyclic aromatic hydrocarbons.

PubMed

Cai, Ying; Yan, Zhihong; NguyenVan, Manh; Wang, Lijia; Cai, Qingyun

2015-08-07

Fluorenyl functionalized superparamagnetic core/shell magnetic nanoparticles (MNPs, Fe3O4@SiO2@Flu) were prepared and characterized by transmission electron microscope, X-ray diffraction and infrared spectroscopy. The MNPs having an average diameter of 200nm were then used as solid-phase extraction sorbent for the determination of 16 priority pollutants polycyclic aromatic hydrocarbons (PAHs) in water samples designated by United States Environmental Protection Agency (U.S. EPA). The main influencing parameters, including sorbent amount, desorption solvent, sample volume and extraction time were optimized. Analyses were performed on gas chromatography-mass spectrometry (GC-MS) using selected ion monitoring (SIM) mode. Method validation proved the feasibility of the developed sorbents for the quantitation of the investigated analytes at trace levels. Limit of detection ranging from 0.5 to 4.0ng/L were obtained. The repeatability was investigated by evaluating the intra- and inter-day precisions with relative standard deviations (RSDs) lower than 13.1%. Finally, the proposed method was successfully applied for the determination of PAHs in water samples with the recoveries in the range of 96.0-106.7%. Copyright © 2015 Elsevier B.V. All rights reserved.

Solid-phase microextraction based on polyaniline doped with perfluorooctanesulfonic acid coupled to HPLC for the quantitative determination of chlorophenols in water samples.

PubMed

He, Huan; Zhuang, Yuan; Peng, Ying; Gao, Zhanqi; Yang, Shaogui; Sun, Cheng

2014-02-01

A porous and highly efficient polyaniline-based solid-phase microextraction (SPME) coating was successfully prepared by the electrochemical deposition method. A method based on headspace SPME followed by HPLC was established to rapidly determine trace chlorophenols in water samples. Influential parameters for the SPME, including extraction mode, extraction temperature and time, pH and ionic strength procedures, were investigated intensively. Under the optimized conditions, the proposed method was linear in the range of 0.5-200 μg/L for 4-chlorophenol and 2,4,6-trichlorophenol, 0.2-200 μg/L for 2,4-dichlorophenol and 2-200 μg/L for 2,3,4,6-tetrachlorophenol and pentachlorophenol, with satisfactory correlation coefficients (>0.99). RSDs were <15% (n = 5) and LODs were relatively low (0.10-0.50 μg/L). Compared to commercial 85 μm polyacrylate and 60 μm polydimethylsiloxane/divinylbenzene fibers, the homemade polyaniline fiber showed a higher extraction efficiency. The proposed method has been successfully applied to the determination of chlorophenols in water samples with satisfactory recoveries. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Lipidomic fingerprint of almonds (Prunus dulcis L. cv Nonpareil) using TiO₂ nanoparticle based matrix solid-phase dispersion and MALDI-TOF/MS and its potential in geographical origin verification.

PubMed

Shen, Qing; Dong, Wei; Yang, Mei; Li, Linqiu; Cheung, Hon-Yeung; Zhang, Zhifeng

2013-08-14

A matrix solid-phase dispersion (MSPD) procedure with titanium dioxide (TiO2) nanoparticles (NP) as sorbent was developed for the selective extraction of phospholipids from almond samples, and matrix-assisted laser desorption ionization-time-of-flight mass spectrometry (MALDI-TOF/MS) was employed for analysis. A remarkable increase in the signals of phospholipid accompanied by a decrease in those of triacylglycerols and diacylglycerols was observed in the relevant mass spectra. The proposed method was applied to five batches of almonds originating from four geographical areas, whereas principal component analysis (PCA) was utilized to normalize the relative amounts of the identified phospholipid species. The results indicated that the lipidomic fingerprint of almonds was successfully established by the negative ion mode spectrum, and the ratio of m/z 833.6 to 835.6 as well as m/z 821.6 could be introduced as potential markers for the differentiation of the tested almonds with different geographical origins. The whole method is of great promise for selective separation of phospholipids from nonphospholipids, especially the glycerides, and superior in fast screening and characterization of phospholipids in almond samples.

Preliminary investigation on the use of low current pulsed power Z-pinch plasma devices for the study of early stage plasma instabilities

NASA Astrophysics Data System (ADS)

Kaselouris, E.; Dimitriou, V.; Fitilis, I.; Skoulakis, A.; Koundourakis, G.; Clark, E. L.; Chatzakis, J.; Bakarezos, Μ; Nikolos, I. K.; Papadogiannis, N. A.; Tatarakis, M.

2018-01-01

This article addresses key features for the implementation of low current pulsed power plasma devices for the study of matter dynamics from the solid to the plasma phase. The renewed interest in such low current plasma devices lies in the need to investigate methods for the mitigation of prompt seeding mechanisms for the generation of plasma instabilities. The low current when driven into thick wires (skin effect mode) allows for the simultaneous existence of all phases of matter from solid to plasma. Such studies are important for the concept of inertial confinement fusion where the mitigation of the instability seeding mechanisms arising from the very early moments within the target’s heating is of crucial importance. Similarly, in the magnetized liner inertial fusion concept it is an open question as to how much surface non-uniformity correlates with the magneto-Rayleigh-Taylor instability, which develops during the implosion. This study presents experimental and simulation results, which demonstrate that the use of low current pulsed power devices in conjunction with appropriate diagnostics can be important for studying seeding mechanisms for the imminent generation of plasma instabilities in future research.

[Ultrasonic sludge treatment and its application on aerobic digestion].

PubMed

Li, Huan; Jin, Yi-ying; Nie, Yong-feng; Li, Lei; Yang, Hai-ying

2007-07-01

In order to enhance the degradation efficiency of waste activated sludge (WAS) in conventional aerobic digestion, various ultrasonic assisted treatment methods were investigated including ultrasonic disintegration of influent sludge, ultrasonic improvement of influent sludge activity and ultrasonic disintegration of return sludge. Firstly the effects of ultrasonic sludge treatment were studied to choose appropriate ultrasonic parameters, and then the experiments of aerobic digestion with different ultrasonic treatments were carried out. The results show that 1.0 W/mL, 10 minutes ultrasonic treatment can increase soluble chemical oxygen demand (SCOD) in the supernatant phase of sludge sample by 5.4 times and decrease total suspended solid (TSS) by 16%; 0.05 W/mL, 10 min ultrasonic treatment can increase the specific oxygen uptake rate (SOUR) of sludge sample by 29%. The two kinds of ultrasonic influent sludge pretreatment can't improve aerobic digestion effectively. Ultrasonic return sludge disintegration can enhance the volatile suspended solid (VSS) degradation ratio by 15%. Furthermore, the settlement performance of digested sludge is still good and the pollutant concentrations of supernatant phase increase slightly. So ultrasonic return sludge disintegration is considered as the most appropriate assisted treatment mode for aerobic digestion.

Multivariate optimization of the factors influencing the solid-phase microextraction of pyrethroid pesticides in water.

PubMed

Casas, Vanessa; Llompart, Maria; García-Jares, Carmen; Cela, Rafael; Dagnac, Thierry

2006-08-18

A method based on solid-phase microextraction (SPME) and gas chromatography with micro-electron capture detection (GC-microECD) has been optimized for the analysis of pyrethroids in water samples. The influence of parameters such as temperature, fibre coating, salting-out effect and sampling mode on the extraction efficiency has been studied by means of a mix-level factorial design, which allowed the study of main effects as well as two factor interactions. Finally, a method based on direct SPME at 50 degrees C, using polydimethylsiloxane fibre is proposed. The method showed good linearity (R2>0.995) and repeatability (RSD

Solid-phase micro-extraction procedure for the determination of 1,3-dichloro-2-propanol in water by on-fibre derivatisation with bis(trimethylsilyl)trifluoroacetamide.

PubMed

Carro, Antonia María; González, Paula; Fajar, Noelia; Lorenzo, Rosa Antonia; Cela, Rafael

2009-06-01

The headspace solid-phase micro-extraction technique with on-fibre derivatisation followed by gas chromatography-tandem mass spectrometry has been evaluated for the analysis of 1,3-dichloro-2-propanol in water. An asymmetric factorial design has been performed to study the influence of five experimental factors: extraction time and temperature, derivatisation time and temperature and pH. The best extraction performance is achieved in the headspace mode, with 5 mL stirred water samples (pH 4) containing 1.3 g of NaCl, equilibrated for 30 min at 25 degrees C, using divinylbenzene-carboxen-polydimethylsiloxane as the fibre coating. On-fibre derivatisation has been used for the first time with 50 microL of bis(trimethylsilyl)trifluoroacetamide at 25 degrees C during 15 min, leading to effective yields. The proposed method provides high sensitivity, good linearity and repeatability (relative standard deviation of 5.1% for 10 ng mL(-1) and n = 5). The limits of detection and quantification were 0.4 and 1.4 ng mL(-1), respectively. Analytical recoveries obtained for different water samples were approx. 100%.

Ultra-high performance liquid chromatography tandem mass spectrometry for the determination of five glycopeptide antibiotics in food and biological samples using solid-phase extraction.

PubMed

Deng, Fenfang; Yu, Hong; Pan, Xinhong; Hu, Guoyuan; Wang, Qiqin; Peng, Rongfei; Tan, Lei; Yang, Zhicong

2018-02-23

This paper demonstrated the development and validation of an ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method for simultaneous determination of five glycopeptide antibiotics in food and biological samples. The target glycopeptide antibiotics were isolated from the samples by solvent extraction, and the extracts were cleaned with a tandem solid-phase extraction step using mixed strong cation exchange and hydrophilic/lipophilic balance cartridges. Subsequently, the analytes were eluted with different solvents, and then quantified by UHPLC-MS/MS in the positive ionization mode with multiple reaction monitoring. Under optimal conditions, good linear correlations were obtained for the five glycopeptide antibiotics in the concentration range of 1.0 μg/L to 20.0 μg/L, and with linear correlation coefficients >0.998. Employing this method, the target glycopeptide antibiotics in food and biological samples were identified with a recovery of 83.0-102%, and a low quantitation limit of 1.0 μg/kg in food and 2.0 μg/L in biological samples with low matrix effects. Copyright © 2018 Elsevier B.V. All rights reserved.

Authentication of pineapple (Ananas comosus [L.] Merr.) fruit maturity stages by quantitative analysis of γ- and δ-lactones using headspace solid-phase microextraction and chirospecific gas chromatography-selected ion monitoring mass spectrometry (HS-SPME-GC-SIM-MS).

PubMed

Steingass, Christof B; Langen, Johannes; Carle, Reinhold; Schmarr, Hans-Georg

2015-02-01

Headspace solid phase microextraction and chirospecific gas chromatography-mass spectrometry in selected ion monitoring mode (HS-SPME-GC-SIM-MS) allowed quantitative determination of δ-lactones (δ-C8, δ-C10) and γ-lactones (γ-C6, γ-C8, γ-C10). A stable isotope dilution assay (SIDA) with d7-γ-decalactone as internal standard was used for quantitative analysis of pineapple lactones that was performed at three progressing post-harvest stages of fully ripe air-freighted and green-ripe sea-freighted fruits, covering the relevant shelf-life of the fruits. Fresh pineapples harvested at full maturity were characterised by γ-C6 of high enantiomeric purity remaining stable during the whole post-harvest period. In contrast, the enantiomeric purity of γ-C6 significantly decreased during post-harvest storage of sea-freighted pineapples. The biogenetical background and the potential of chirospecific analysis of lactones for authentication and quality evaluation of fresh pineapple fruits are discussed. Copyright © 2014 Elsevier Ltd. All rights reserved.

Determination of Sucrose in Honey with Derivatization/Solid-Phase Microextraction and Gas-Chromatography/Mass Spectrometry.

PubMed

Wang, Haijing; Geppert, Helmut; Fischer, Thomas; Wieprecht, Wolfgang; Möller, Detlev

2015-10-01

A new method for the determination of sucrose in honey with derivatization solid-phase microextraction and gas chromatography/mass spectrometry (D-SPME-GC/MS) was developed. The method incorporates a sample derivatization with acetic anhydride using N-methylimidazole as the catalyst and the subsequent enrichment of the analyte in a Polyacrylate-SPME fiber. Results show that 100 µL N-methylimidazole and 800 µL acetic anhydride were sufficient to complete the acetylation for sucrose in 100 µL aqueous sample at room temperature. For SPME, an enrichment time of 30 min was sufficient. SPME was performed by immersing the fiber into the solution with additional vibration. Then, the analyte was desorbed for 5 min at 280°C in the GC/MS injection port with splitless mode. The present method exhibits good linearity at a concentration range of 0.3-8% of sucrose in honey with excellent regression (R = 0.9993). The method has been successfully applied to the control of sucrose adulteration in honey. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Innovative separation and preconcentration technique of coagulating homogenous dispersive micro solid phase extraction exploiting graphene oxide nanosheets.

PubMed

Ghazaghi, Mehri; Mousavi, Hassan Zavvar; Rashidi, Ali Morad; Shirkhanloo, Hamid; Rahighi, Reza

2016-01-01

A uniquely novel, fast, and facile technique is introduced for the first time in which a scant amount of graphene oxide (GO), without modification, has been utilized in dispersive mode of solid phase extraction (SPE) for an efficient yet simple separation. The proposed method of coagulating homogenous dispersive micro solid phase extraction (CHD-µSPE) is based on coagulation of homogeneous GO solution with the aid of polyetheneimine (PEI). CHD-µSPE use full adsorption capacity of GO because in this method was used GO solution obtained from synthesis process without drying step and stacking nanosheets. In optimized condition, 30 µL GO solution (7 mg mL(-1)), obtained in synthesis process, was injected into 1.5 mL the sample solution followed by immediate injection of 53 µL PEI solution (1 mg mL(-1)). After inserting PEI, GO sheets aggregate and can be readily separated by centrifugation. PEI not only cause aggregation of GO, but also form three-dimensional network of GO with easy handling in following separation steps. Lead, cadmium, and chromium were selected as model analytes and the effecting parameters including the amount of GO, concentration of PEI, sample pH, extraction time, and type of desorption solvent were investigated and optimized. The results indicate that the proposed CHD-µSPE method can be successfully applied GO in dispersive mode of SPE without effecting on good capability adsorption of GO. The novel method was applied in determination of lead, cadmium, and chromium in water, human saliva, and urine samples by electrothermal atomic absorption spectrometry. The detection limits are as low as 0.035, 0.005, and 0.012 µg L(-1) for Pb, Cd, and Cr respectively. The intra-day precisions (RSDs) were lower than 3.8%. CHD-µSPE method showed a good linear ranges of 0.24-15.6, 0.015-0.95 and 0.039-2.33 µg L(-1) for Pb, Cd and Cr respectively. Method performance was investigated by determination of mentioned metal ions in river water, human urine and saliva sample with good recoveries in range of 94.2-103.0%. The accuracy of the method was underpinned by correct analysis of a standard reference material (SRM: 2668 level I, Urine). Copyright © 2015 Elsevier B.V. All rights reserved.

Materials research for passive solar systems: Solid-state phase-change materials

NASA Astrophysics Data System (ADS)

Benson, D. K.; Webb, J. D.; Burrows, R. W.; McFadden, J. D. O.; Christensen, C.

1985-03-01

A set of solid-state phase-change materials is being evaluated for possible use in passive solar thermal energy storage systems. The most promising materials are organic solid solutions of pentaerythritol (C5H12O4), pentaglycerinve (C5H12O3), and neopentyl glycol (C5H12O2). Solid solution mixtures of these compounds can be tailored so that they exhibit solid-to-solid phase transformations at any desired temperature between 25 C and 188 C, and have latent heats of transformation etween 20 and 70 cal/g. Transformation temperatures, specific heats, and latent heats of transformation have been measured for a number of these materials. Limited cyclic experiments suggest that the solid solutions are stable. These phase-change materials exhibit large amounts of undercooling; however, the addition of certain nucleating agents as particulate dispersions in the solid phase-change material greatly reduces this effect. Computer simulations suggest that the use of an optimized solid-state phase-change material in a Trombe wall could provide better performance than a concrete Trombe wall four times thicker and nine times heavier.

High pressure far infrared spectroscopy of ionic solids

NASA Technical Reports Server (NTRS)

Lowndes, R. P.

1974-01-01

A high-pressure far-infrared cell operating at up to truly hydrostatic pressures of 8 kbar is described and used to determine the anharmonic self-energies associated with the transverse optic modes of ionic solids in which q approximately equals zero. The cell allows far-infrared studies in the spectral range below 120 reciprocal cm. The transverse optic modes were investigated to determine their mode Gruneisen constants and the pressure dependence of their inverse lifetimes in RbI, CsI, and TlCl.

FT-IR standoff detection of thermally excited emissions of trinitrotoluene (TNT) deposited on aluminum substrates.

PubMed

Castro-Suarez, John R; Pacheco-Londoño, Leonardo C; Vélez-Reyes, Miguel; Diem, Max; Tague, Thomas J; Hernandez-Rivera, Samuel P

2013-02-01

A standoff detection system was assembled by coupling a reflecting telescope to a Fourier transform infrared spectrometer equipped with a cryo-cooled mercury cadmium telluride detector and used for detection of solid-phase samples deposited on substrates. Samples of highly energetic materials were deposited on aluminum substrates and detected at several collector-target distances by performing passive-mode, remote, infrared detection measurements on the heated analytes. Aluminum plates were used as support material, and 2,4,6-Trinitrotoluene (TNT) was used as the target. For standoff detection experiments, the samples were placed at different distances (4 to 55 m). Several target surface temperatures were investigated. Partial least squares regression analysis was applied to the analysis of the intensities of the spectra obtained. Overall, standoff detection in passive mode was useful for quantifying TNT deposited on the aluminum plates with high confidence up to target-collector distances of 55 m.

The 4-pyridylmethyl ester as a protecting group for glutamic and aspartic acids: 'flipping' peptide charge states for characterization by positive ion mode ESI-MS.

PubMed

Garapati, Sriramya; Burns, Colin S

2014-03-01

Use of the 4-pyridylmethyl ester group for side-chain protection of glutamic acid residues in solid-phase peptide synthesis enables switching of the charge state of a peptide from negative to positive, thus making detection by positive ion mode ESI-MS possible. The pyridylmethyl ester moiety is readily removed from peptides in high yield by hydrogenation. Combining the 4-pyridylmethyl ester protecting group with benzyl ester protection reduces the number of the former needed to produce a net positive charge and allows for purification by RP HPLC. This protecting group is useful in the synthesis of highly acidic peptide sequences, which are often beset by problems with purification by standard RP HPLC and characterization by ESI-MS. Copyright © 2014 European Peptide Society and John Wiley & Sons, Ltd.

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

Costa, R. C. da; Universidade Federal de Campina Grande, Pombal-PB, 58840-000; Toledo, T. A. de

The effects of the atomic substitution of Pb by Ni in the PbTiO{sub 3} ferroelectric perovskite on the vibrational and structural properties was studied using x-ray diffraction and Raman scattering. It was observed that for Ni concentrations between 0.0 and 0.4, there is the formation of a solid solution with reduction of the Raman wavenumber of the E(TO1) soft mode and the tetragonallity factor, which influence directly the temperature of the tetragonal ferroelectric to cubic paraelectric phase transition, the Curie temperature. For concentrations greater than 0.4, it is observed the formation of a PbTiO{sub 3} and NiTiO{sub 3} composite, denouncedmore » by the recovering of the both, tetragonallity factor and the E(TO1) soft mode wavenumber. The values of the Curie temperatures were estimated by the Raman scattering measurements for temperatures ranging from 300 to 950 K.« less

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

Lu, Chenyang; Niu, Liangliang; Chen, Nanjun

A grand challenge in material science is to understand the correlation between intrinsic properties and defect dynamics. Radiation tolerant materials are in great demand for safe operation and advancement of nuclear and aerospace systems. Unlike traditional approaches that rely on microstructural and nanoscale features to mitigate radiation damage, this study demonstrates enhancement of radiation tolerance with the suppression of void formation by two orders magnitude at elevated temperatures in equiatomic single-phase concentrated solid solution alloys, and more importantly, reveals its controlling mechanism through a detailed analysis of the depth distribution of defect clusters and an atomistic computer simulation. The enhancedmore » swelling resistance is attributed to the tailored interstitial defect cluster motion in the alloys from a long-range one-dimensional mode to a short-range three-dimensional mode, which leads to enhanced point defect recombination. Finally, the results suggest design criteria for next generation radiation tolerant structural alloys.« less

Preparation and characterization of host-guest system between inosine and β-cyclodextrin through inclusion mode

NASA Astrophysics Data System (ADS)

Prabu, Samikannu; Sivakumar, Krishnamurty; Swaminathan, Meenakshisundaram; Rajamohan, Rajaram

2015-08-01

Inosine is a nucleoside that is formed when hypoxanthine is attached to a ribose ring (also known as a ribofuranose) via a β-N9-glycosidic bond. Inosine is commonly found in tRNAs. Inosine (INS) has been used widely as an antiviral drug. The inclusion complex of INS with β-CDx in solution phase is studied by ground and excited state with UV-visible and fluorescence spectroscopy, respectively. A binding constant and stoichiometric ratio between INS and β-CDx are calculated by BH equation. The lifetime and relative amplitude of INS is increases with increasing the concentrations of β-CDx, confirms the formation of inclusion complex in liquid state. The solid complexes are prepared by kneading method (KM) and co-precipitation method (CP). The solid complex is characterized by Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), powder X-ray diffraction (XRD) and differential scanning colorimetry (DSC). CP method gives the solid product with good yield than that of physical mixture and KM method. The structure of complex is proposed based on the study of Patch - Dock server.

Comprehensive solid-phase extraction of multitudinous bioactive peptides from equine plasma and urine for doping detection.

PubMed

Guan, Fuyu; Robinson, Mary A

2017-09-08

The ability to analyze biological samples for multitudinous exogenous peptides with a single analytical method is desired for doping control in horse racing. The key to achieving this goal is the capability of extracting all target peptides from the sample matrix. In the present study, theory of mixed-mode solid-phase extraction (SPE) of peptides from plasma is described, and a generic mixed-mode SPE procedure has been developed for recovering multitudinous exogenous peptides with remarkable sequence diversity, from equine plasma and urine in a single procedure. Both the theory and the developed SPE procedure have led to the development of a novel analytical method for comprehensive detection of multitudinous bioactive peptides in equine plasma and urine using liquid chromatography coupled to high resolution mass spectrometry (LC-HRMS). Thirty nine bioactive peptides were extracted with strong anion-exchange mixed-mode SPE sorbent, separated on a reversed-phase C 18 column and detected by HRMS and data-dependent tandem mass spectrometry. The limit of detection (LOD) was 10-50 pg mL -1 in plasma for most of the peptides and 100 pg mL -1 for the remaining. For urine, LOD was 20-400 pg mL -1 for most of the peptides and 1-4 ng mL -1 for the others. In vitro degradation of the peptides in equine plasma and urine was examined at ambient temperature; the peptides except those with a D-amino acid at position 2 were unstable not only in plasma but also in urine. The developed method was successful in analysis of plasma and urine samples from horses administered dermorphin. Additionally, dermorphin metabolites were identified in the absence of reference standards. The developed SPE procedure and LC-HRMS method can theoretically detect virtually all peptides present at a sufficient concentration in a sample. New peptides can be readily included in the method to be detected without method re-development. The developed method also generates such data that can be retrospectively analyzed for peptides unknown at the time of sample analysis. It is the first generic analytical method for comprehensive detection of multitudinous exogenous peptides in biological samples, to the authors' knowledge. Copyright © 2017 Elsevier B.V. All rights reserved.

Influence of La doping on structural and dielectric properties of SrBi2Nb2O9 ceramics

NASA Astrophysics Data System (ADS)

Verma, Maya; Sreenivas, K.; Gupta, Vinay

2009-01-01

Lanthanum doped SrBi2Nb2O9 ceramics with the chemical formula SrBi2-xLaxNb2O9 (SBLN) (x =0-0.5) have been prepared through conventional solid state route. X-ray diffraction reveals the shrinkage of unit cell of strontium bismuth niobate with incorporation of La3+ dopant, having no lone pair electrons. Shifting of Raman phonon modes indicates the reduced rattling space of NbO6 octahedra with increase in La doping concentration. Further, the softening of lowest frequency phonon mode with increasing x in SBLN shows the transition from ferroelectric to paraelectric at room temperature. The dielectric properties for all the compositions are studied as a function of temperature (25 to 500 °C) over the frequency range of 10 kHz-1 MHz. With increase in lanthanum doping concentration the phase transition becomes diffused and transition temperature gets shifted toward lower temperature. A phase transition from normal ferroelectric to paraelectric has been observed via relaxor-type ferroelectrics with increase in x. The frequency dependence of transition temperature was studied in terms of Vogel-Fulcher relation for SBLN (x =0.4).

Application of internal quality control to the analysis of quaternary ammonium compounds in surface and groundwater from Andalusia (Spain) by liquid chromatography with mass spectrometry.

PubMed

Vidal, J L Martínez; Vega, A Belmonte; López, F J Sánchez; Frenich, A Garrido

2004-10-01

A method has been developed for the simultaneous determination of paraquat (PQ), deiquat (DQ), chlormequat (CQ) and mepiquat (MQ) in water samples by liquid chromatography (LC) coupled with electrospray ionization mass spectrometry (MS). The LC separations of the target compounds, as well as their MS parameters, were optimized in order to improve selectivity and sensitivity. Separation was carried out in a Xterra C8 column, using as mobile phase methanol-heptafluorobutyric acid (HFBA) in isocratic mode. The molecular ion was selected for the quantitation in selected ion monitoring (SIM) mode. Off-line solid-phase extraction (SPE) was applied with silica cartridges in order to preconcentrate the compounds from waters. Detection limits were in the range 0.02-0.40 microg l(-1). Recovery range varied between 89 and 99.5% with precision values lower than 6%. The method has been applied successfully to the analysis of both surface and groundwater samples from agricultural areas of Andalusia (Spain), using well defined internal quality control (IQC) criteria. The results revealed the presence of deiquat and paraquat in some samples.

Benzocaine polymorphism: pressure-temperature phase diagram involving forms II and III.

PubMed

Gana, Inès; Barrio, Maria; Do, Bernard; Tamarit, Josep-Lluís; Céolin, René; Rietveld, Ivo B

2013-11-18

Understanding the phase behavior of an active pharmaceutical ingredient in a drug formulation is required to avoid the occurrence of sudden phase changes resulting in decrease of bioavailability in a marketed product. Benzocaine is known to possess three crystalline polymorphs, but their stability hierarchy has so far not been determined. A topological method and direct calorimetric measurements under pressure have been used to construct the topological pressure-temperature diagram of the phase relationships between the solid phases II and III, the liquid, and the vapor phase. In the process, the transition temperature between solid phases III and II and its enthalpy change have been determined. Solid phase II, which has the highest melting point, is the more stable phase under ambient conditions in this phase diagram. Surprisingly, solid phase I has not been observed during the study, even though the scarce literature data on its thermal behavior appear to indicate that it might be the most stable one of the three solid phases. Copyright © 2013 Elsevier B.V. All rights reserved.

Gigahertz frequency comb from a diode-pumped solid-state laser.

PubMed

Klenner, Alexander; Schilt, Stéphane; Südmeyer, Thomas; Keller, Ursula

2014-12-15

We present the first stabilization of the frequency comb offset from a diode-pumped gigahertz solid-state laser oscillator. No additional external amplification and/or compression of the output pulses is required. The laser is reliably modelocked using a SESAM and is based on a diode-pumped Yb:CALGO gain crystal. It generates 1.7-W average output power and pulse durations as short as 64 fs at a pulse repetition rate of 1 GHz. We generate an octave-spanning supercontinuum in a highly nonlinear fiber and use the standard f-to-2f carrier-envelope offset (CEO) frequency f_CEO detection method. As a pump source, we use a reliable and cost-efficient commercial diode laser. Its multi-spatial-mode beam profile leads to a relatively broad frequency comb offset beat signal, which nevertheless can be phase-locked by feedback to its current. Using improved electronics, we reached a feedback-loop-bandwidth of up to 300 kHz. A combination of digital and analog electronics is used to achieve a tight phase-lock of f_CEO to an external microwave reference with a low in-loop residual integrated phase-noise of 744 mrad in an integration bandwidth of [1 Hz, 5 MHz]. An analysis of the laser noise and response functions is presented which gives detailed insights into the CEO stabilization of this frequency comb.

"Two-dimensional" molecularly imprinted solid-phase extraction coupled with crystallization and high performance liquid chromatography for fast semi-preparative purification of tannins from pomegranate husk extract.

PubMed

Sun, Guangying; Liu, Yanfang; Ahat, Hasanjan; Shen, Aijin; Liang, Xinmiao; Xue, Xingya; Luo, Yuqin; Yang, Jian; Liu, Zhao-Sheng; Aisa, Haji Akber

2017-07-07

In this study, "two dimensional" molecularly imprinted solid-phase extraction (2D-MIP-SPE) of semi-preparative grade was constructed to fast purify ellagitannins in pomegranate husk extract with the help of crystallization and reverse-phase liquid chromatgoraphy (RPLC). Ellagic acid and punicalagin imprinted polymers were synthesized in batch mode and two semi-preparative MIP-SPE columns were individually packed. After investigaing "functional complementation", 2D-MIP-SPE was constructed using ellagic acid MIP and punicalagin MIP-SPE as the first and second dimension, respectively. Then, pomegranate husk extract was fast divided into four fractions individually enriching in ellagic acid, granatin A, punicalagin and ellagic acid glucoside by 2D-MIP-SPE. With the aid of crystallization and RPLC, ellagic acid (13.5mg) and punicalagin (53.4mg) were fast obtained in 30min. Ellagic acid glucoside was purified to the purity near 100% with a recovery of 86.1%. Granatin A (92%) was directly obtained by 2D-MIP-SPE with the recovery of 81.8%. All above indicated that 2D-MIP-SPE was highly efficient in natural product purification. The concept of "functional complementation" was expected to be a useful tool in the construction of 2D-MIP-SPE. Copyright © 2017 Elsevier B.V. All rights reserved.

The Potential of Graphene as an Adsorbent for Five Pesticides from Different Classes in Rape Oil Samples Using Dispersive Solid-Phase Extraction.

PubMed

Madej, Katarzyna; Janiga, Katarzyna; Piekoszewski, Wojciech

2018-01-01

Isolation conditions for five pesticides (metazachlor, tebuconazole, λ -cyhalothrin, chlorpyrifos, and deltamethrin) from rape oil samples were examined using the dispersive solid-phase graphene extraction technique. To determine the optimal extraction conditions, a number of experimental factors (amount of graphene, amount of salt, type and volume of the desorbing solvent, desorption time with and without sonication energy, and temperature during desorption) were studied. The compounds of interest were separated and detected by an HPLC-UV employing a Kinetex XB-C18 column and a mobile phase consisting of acetonitrile and water flowing in a gradient mode. The optimized extraction conditions were: the amount of graphene 15 mg, desorbing solvent (acetonitrile) 5 mL, time desorption 10 min at 40°C, and amount of NaCl 1 g. The detection limit for metazachlor, tebuconazole, λ -cyhalothrin, and chlorpyrifos was 62.5 ng·g -1 , and for deltamethrin, it was 500 ng·g -1 . The obtained results lead to the conclusion that graphene may be successfully used for the isolation of the five pesticides from rape oil. However, their determination at low concentration levels, as they occur in real oil samples, requires the employment of appropriately highly sensitive analytical methods, as well as a more suitable graphene form (e.g., magnetically modified graphene).

Spectrophotometric and Reversed-Phase High-Performance Liquid Chromatographic Method for the Determination of Doxophylline in Pharmaceutical Formulations

PubMed Central

Joshi, HR; Patel, AH; Captain, AD

2010-01-01

Two methods are described for determination of Doxophylline in a solid dosage form. The first method was based on ultraviolet (UV)-spectrophotometric determination of the drug. It involves absorbance measurement at 274 nm (λmax of Doxophylline) in 0.1 N hydrochloric acid. The calibration curve was linear, with the correlation coefficient between 0.99 and 1.0 over a concentration range of 0.20–30 mg/ml for the drug. The second method was based on high-performance liquid chromatography (HPLC) separation of the drug in reverse-phase mode using the Hypersil ODS C18 column (250 × 4.6 mm, 5 mm). The mobile phase constituted of buffer acetonitrile (80:20) and pH adjusted to 3.0, with dilute orthophosphoric acid delivered at a flow rate 1.0 ml/min. Detection was performed at 210 nm. Separation was completed within 7 min. The calibration curve was linear, with the correlation coefficient between 0.99 and 1.0 over a concentration range of 0.165–30 mg/ml for the drug. The relative standard deviation was found to be <2.0% for the UV-spectrophotometry and HPLC methods. Both these methods have been successively applied to the solid dosage pharmaceutical formulation, and were fully validated according to ICH guidelines. PMID:21042488

Separation and quantitation of three acidic herbicide residues in tobacco and soil by dispersive solid-phase extraction and UPLC-MS/MS.

PubMed

Xiong, Wei; Tao, Xiaoqiu; Pang, Su; Yang, Xue; Tang, GangLing; Bian, Zhaoyang

2014-01-01

A method for the determination of three acidic herbicides, dicamba, 2,4-dichlorophenoxyacetic acid (2,4-D) and 2,4,5-trichlorophenoxyacetic acid (2,4,5-T) in tobacco and soil has been developed based on the use of liquid-liquid extraction and dispersive solid-phase extraction (dispersive-SPE) followed by UPLC-MS/MS. Two percentage of (v/v) formic acid in acetonitrile as the extraction helped partitioning of analytes into the acetonitrile phase. The extract was then cleaned up by dispersive-SPE using primary secondary amine as selective sorbents. Quantitative analysis was done in the multiple-reaction monitoring mode using stable isotope-labeled internal standards for each compound. A separate internal standard for each analyte is required to minimize sample matrix effects on each analyte, which can lead to poor analyte recoveries and decreases in method accuracy and precision. The total analysis time was <4 min. The linear range of the method was from 1 to 100 ng mL(-1) with a limit of detection of each herbicide varied from 0.012 to 0.126 ng g(-1). The proposed method is faster, more sensitive and selective than the traditional methods and more accurate and robust than the published LC-MS/MS methods. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Simultaneous determination of ezetimibe and its glucuronide metabolite in human plasma by solid phase extraction and liquid chromatography-tandem mass spectrometry.

PubMed

Guo, Lin; Wang, Meng-meng; He, Min; Qiu, Fu-rong; Jiang, Jian

2015-04-01

A liquid chromatography-tandem mass spectrometry method (LC-MS/MS) was developed to quantify ezetimibe (EZM) and its major glucuronide (ezetimibe glucuronide, EZM-G) in human plasma simultaneously. The analytes were purified by solid phase extraction (SPE) without hydrolysis. Separation of the analytes was achieved using acetonitrile-water (0.08% formic acid) (70:30, v/v) as the mobile phase at a flow rate of 0.8 mL/min on an Agilent Extend C18 column. The analytes were detected by LC-MS/MS using negative ionization in multiple reaction monitoring (MRM) mode. The mass transition pairs of m/z 408.4→271.0 and m/z 584.5→271.0 were used to detect EZM and EZM-G, respectively. The analytical method was linear over the concentration range of 0.1-20 ng/mL for EZM and 0.5-200 ng/mL for EZM-G. Within- and between-run precision for EZM was no more than 8.6% and 12.8%; and for EZM-G was no more than 9.0% and 8.7%, respectively. This method was reproducible and reliable, and was successfully used to analyze human plasma samples for application in a bioequivalence study. Copyright © 2015 Elsevier B.V. All rights reserved.

The global phase diagram of the Gay-Berne model

NASA Astrophysics Data System (ADS)

de Miguel, Enrique; Vega, Carlos

2002-10-01

The phase diagram of the Gay-Berne model with anisotropy parameters κ=3, κ'=5 has been evaluated by means of computer simulations. For a number of temperatures, NPT simulations were performed for the solid phase leading to the determination of the free energy of the solid at a reference density. Using the equation of state and free energies of the isotropic and nematic phases available in the existing literature the fluid-solid equilibrium was calculated for the temperatures selected. Taking these fluid-solid equilibrium results as the starting points, the fluid-solid equilibrium curve was determined for a wide range of temperatures using Gibbs-Duhem integration. At high temperatures the sequence of phases encountered on compression is isotropic to nematic, and then nematic to solid. For reduced temperatures below T=0.85 the sequence is from the isotropic phase directly to the solid state. In view of this we locate the isotropic-nematic-solid triple point at TINS=0.85. The present results suggest that the high-density phase designated smectic B in previous simulations of the model is in fact a molecular solid and not a smectic liquid crystal. It seems that no thermodynamically stable smectic phase appears for the Gay-Berne model with the choice of parameters used in this work. We locate the vapor-isotropic liquid-solid triple point at a temperature TVIS=0.445. Considering that the critical temperatures is Tc=0.473, the Gay-Berne model used in this work presents vapor-liquid separation over a rather narrow range of temperatures. It is suggested that the strong lateral attractive interactions present in the Gay-Berne model stabilizes the layers found in the solid phase. The large stability of the solid phase, particularly at low temperatures, would explain the unexpectedly small liquid range observed in the vapor-liquid region.

Development of a multi-preservative method based on solid-phase microextraction-gas chromatography-tandem mass spectrometry for cosmetic analysis.

PubMed

Alvarez-Rivera, Gerardo; Vila, Marlene; Lores, Marta; Garcia-Jares, Carmen; Llompart, Maria

2014-04-25

A simple methodology based on solid-phase microextraction (SPME) followed by gas chromatography-tandem mass spectrometry (GC-MS/MS) has been developed for the simultaneous analysis of different classes of preservatives including benzoates, bronidox, 2-phenoxyethanol, parabens, BHA, BHT and triclosan in cosmetic products. In situ acetylation and subsequent organic modifier addition have been successfully implemented in the SPME process as an effective extractive strategy for matrix effect compensation and chromatographic performance improvement. Main factors affecting SPME procedure such as fiber coating, sampling mode, extraction temperature and salt addition (NaCl) were evaluated by means of a 3×2(3-1) factorial experimental design. The optimal experimental conditions were established as follows: direct solid-phase microextraction (SPME) at 40°C and addition of NaCl (20%, w/v), using a DVB/CAR/PDMS fiber coating. Due to the complexity of the studied matrices, method performance was evaluated in a representative variety of both rinse-off and leave-on samples, demonstrating to have a broad linear range (R(2)>0.9964). In general, quantitative recoveries (>85% in most cases) and satisfactory precision (RSD<13% for most of compounds) were obtained, with limits of detection (LODs) well below the maximum authorized concentrations established by the European legislation. One of the most important achievements of this work was the use of external calibration with cosmetic-matched standards to accurately quantify the target analytes. The validated methodology was successfully applied to the analysis of different types of cosmetic formulations including body milks, moisturizing creams, deodorants, sunscreen, bath gel, dental cream and make-up products amongst others, demonstrating to be a reliable multi-preservative methododology for routine control. Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of perfluorinated carboxylic acids in fish fillet by micro-solid phase extraction, followed by liquid chromatography-triple quadrupole mass spectrometry.

PubMed

Lashgari, Maryam; Lee, Hian Kee

2014-11-21

In the current study, a simple, fast and efficient combination of protein precipitation and micro-solid phase extraction (μ-SPE) followed by liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS) was developed for the determination of perfluorinated carboxylic acids (PFCAs) in fish fillet. Ten PFCAs with different hydrocarbon chain lengths (C5-C14) were analysed simultaneously using this method. Protein precipitation by acetonitrile and μ-SPE by surfactant-incorporated ordered mesoporous silica were applied to the extraction and concentration of the PFCAs as well as for removal of interferences. Determination of the PFCAs was carried out by LC-MS/MS in negative electrospray ionization mode. MS/MS parameters were optimized for multiple reaction monitoring of the analytes. (13)C mass labelled PFOA as a stable-isotopic internal standard, was used for calibration. The detection limits of the method ranged from 0.97 ng/g to 2.7 ng/g, with a relative standard deviation of between 5.4 and 13.5. The recoveries were evaluated for each analyte and were ranged from 77% to 120%. The t-test at 95% confidence level showed that for all the analytes, the relative recoveries did not depend on their concentrations in the explored concentration range. The effect of the matrix on MS signals (suppression or enhancement) was also evaluated. Contamination at low levels was detected for some analytes in the fish samples. The protective role of the polypropylene membrane used in μ-SPE in the elimination of matrix effects was evaluated by parallel experiments in classical dispersive solid phase extraction. The results evidently showed that the polypropylene membrane was significantly effective in reducing matrix effects. Copyright © 2014 Elsevier B.V. All rights reserved.

Ultrasensitive Speciation Analysis of Mercury in Rice by Headspace Solid Phase Microextraction Using Porous Carbons and Gas Chromatography-Dielectric Barrier Discharge Optical Emission Spectrometry.

PubMed

Lin, Yao; Yang, Yuan; Li, Yuxuan; Yang, Lu; Hou, Xiandeng; Feng, Xinbin; Zheng, Chengbin

2016-03-01

Rice consumption is a primary pathway for human methylmercury (MeHg) exposure in inland mercury mining areas of Asia. In addition, the use of iodomethane, a common fumigant that significantly accelerates the methylation of mercury in soil under sunlight, could increase the MeHg exposure from rice. Conventional hyphenated techniques used for mercury speciation analysis are usually too costly for most developing countries. Consequently, there is an increased interest in the development of sensitive and inexpensive methods for the speciation of mercury in rice. In this work, gas chromatography (GC) coupled to dielectric barrier discharge optical emission spectrometry (DBD-OES) was developed for the speciation analysis of mercury in rice. Prior to GC-DBD-OES analysis, mercury species were derivatized to their volatile species with NaBPh4 and preconcentrated by headspace solid phase microextraction using porous carbons. Limits of detection of 0.5 μg kg(-1) (0.16 ng), 0.75 μg kg(-1) (0.24 ng), and 1.0 μg kg(-1) (0.34 ng) were obtained for Hg(2+), CH3Hg(+), and CH3CH2Hg(+), respectively, with relative standard deviations (RSDs) better than 5.2% and 6.8% for one fiber or fiber-to-fiber mode, respectively. Recoveries of 90-105% were obtained for the rice samples, demonstrating the applicability of the proposed technique. Owing to the small size, low power, and low gas consumption of DBD-OES as well as efficient extraction of mercury species by porous carbons headspace solid phase micro-extraction, the proposed technique provides several advantages including compactness, cost-effectiveness, and potential to couple with miniature GC to accomplish the field speciation of mercury in rice compared to conventional hyphenated techniques.

Methods of analysis by the U.S. Geological Survey Organic Geochemistry Research Group : determination of selected herbicides and their degradation products in water using solid-phase extraction and gas chromatography/mass spectrometry

USGS Publications Warehouse

Kish, J.L.; Thurman, E.M.; Scribner, E.A.; Zimmerman, L.R.

2000-01-01

A method for the extraction and analysis of eight herbicides and five degradation products using solid-phase extraction from natural water samples followed by gas chromatography/mass spectrometry is presented in this report. This method was developed for dimethenamid; flufenacet; fluometuron and its degradation products, demethylfluometuron (DMFM), 3-(trifluromethyl)phenylurea (TFMPU), 3-(trifluromethyl)-aniline (TFMA); molinate; norflurazon and its degradation product, demethylnorflurazon; pendamethalin; the degradation product of prometryn, deisopropylprometryn; propanil; and trifluralin. The eight herbicides are used primarily in the southern United States where cotton, rice, and soybeans are produced. The exceptions are dimethenamid and flufenacet, which are used on corn in the Midwest. Water samples received by the U.S. Geological Survey's Organic Geochemistry Research Group in Lawrence, Kansas, are filtered to remove suspended particulate matter and then passed through disposable solid-phase extraction columns containing octadecyl-bonded porous silica (C-18) to extract the compounds. The herbicides and their degradation products are removed from the column by ethyl acetate elution. The eluate is evaporated under nitrogen, and components then are separated, identified, and quantified by injecting an aliquot of the concentrated extract into a high-resolution, fused-silica capillary column of a gas chromatograph/mass spectrometer under selected-ion mode. Method detection limits ranged from 0.02 to 0.05 ?g/L for all compounds with the exception of TFMPU, which has a method detection limit of 0.32 ?g/L. The mean absolute recovery is 107 percent. This method for the determination of herbicides and their degradation products is valuable for acquiring information about water quality and compound fate and transport in water.

Mode Selection for a Single-Frequency Fiber Laser

NASA Technical Reports Server (NTRS)

Liu, Jian

2010-01-01

A superstructured fiber-grating-based mode selection filter for a single-frequency fiber laser eliminates all free-space components, and makes the laser truly all-fiber. A ring cavity provides for stable operations in both frequency and power. There is no alignment or realignment required. After the fibers and components are spliced together and packaged, there is no need for specially trained technicians for operation or maintenance. It can be integrated with other modules, such as telescope systems, without extra optical alignment due to the flexibility of the optical fiber. The filter features a narrow line width of 1 kHz and side mode suppression ratio of 65 dB. It provides a high-quality laser for lidar in terms of coherence length and signal-to-noise ratio, which is 20 dB higher than solid-state or microchip lasers. This concept is useful in material processing, medical equipment, biomedical instrumentation, and optical communications. The pulse-shaping fiber laser can be directly used in space, airborne, and satellite applications including lidar, remote sensing, illuminators, and phase-array antenna systems.

Topology optimization of embedded piezoelectric actuators considering control spillover effects

NASA Astrophysics Data System (ADS)

Gonçalves, Juliano F.; De Leon, Daniel M.; Perondi, Eduardo A.

2017-02-01

This article addresses the problem of active structural vibration control by means of embedded piezoelectric actuators. The topology optimization method using the solid isotropic material with penalization (SIMP) approach is employed in this work to find the optimum design of actuators taken into account the control spillover effects. A coupled finite element model of the structure is derived assuming a two-phase material and this structural model is written into the state-space representation. The proposed optimization formulation aims to determine the distribution of piezoelectric material which maximizes the controllability for a given vibration mode. The undesirable effects of the feedback control on the residual modes are limited by including a spillover constraint term containing the residual controllability Gramian eigenvalues. The optimization of the shape and placement of the conventionally embedded piezoelectric actuators are performed using a Sequential Linear Programming (SLP) algorithm. Numerical examples are presented considering the control of the bending vibration modes for a cantilever and a fixed beam. A Linear-Quadratic Regulator (LQR) is synthesized for each case of controlled structure in order to compare the influence of the additional constraint.

A selective and sensitive method for quantitation of lysergic acid diethylamide (LSD) in whole blood by gas chromatography-ion trap tandem mass spectrometry.

PubMed

Libong, Danielle; Bouchonnet, Stéphane; Ricordel, Ivan

2003-01-01

A gas chromatography-ion trap tandem mass spectrometry (GC-ion trap MS-MS) method for detection and quantitation of LSD in whole blood is presented. The sample preparation process, including a solid-phase extraction step with Bond Elut cartridges, was performed with 2 mL of whole blood. Eight microliters of the purified extract was injected with a cold on-column injection method. Positive chemical ionization was performed using acetonitrile as reagent gas; LSD was detected in the MS-MS mode. The chromatograms obtained from blood extracts showed the great selectivity of the method. GC-MS quantitation was performed using lysergic acid methylpropylamide as the internal standard. The response of the MS was linear for concentrations ranging from 0.02 ng/mL (detection threshold) to 10.0 ng/mL. Several parameters such as the choice of the capillary column, the choice of the internal standard and that of the ionization mode (positive CI vs. EI) were rationalized. Decomposition pathways under both ionization modes were studied. Within-day and between-day stability were evaluated.

Comparative Effects of Two Modes of Computer-Assisted Instructional Package on Solid Geometry Achievement

ERIC Educational Resources Information Center

Gambari, Isiaka Amosa; Ezenwa, Victoria Ifeoma; Anyanwu, Romanus Chogozie

2014-01-01

The study examined the effects of two modes of computer-assisted instructional package on solid geometry achievement amongst senior secondary school students in Minna, Niger State, Nigeria. Also, the influence of gender on the performance of students exposed to CAI(AT) and CAI(AN) packages were examined. This study adopted a pretest-posttest…

Viscoelastic propellant effects on Space Shuttle Dynamics

NASA Technical Reports Server (NTRS)

Bugg, F.

1981-01-01

The program of solid propellant research performed in support of the space shuttle dynamics modeling effort is described. Stiffness, damping, and compressibility of the propellant and the effects of many variables on these properties are discussed. The relationship between the propellant and solid rocket booster dynamics during liftoff and boost flight conditions and the effects of booster vibration and propellant stiffness on free free solid rocket booster modes are described. Coupled modes of the shuttle system and the effect of propellant stiffness on the interfaces of the booster and the external tank are described. A finite shell model of the solid rocket booster was developed.

Development of high-throughput multi-residue method for non-steroidal anti-inflammatory drugs monitoring in swine muscle by LC-MS/MS.

PubMed

Castilhos, Tamara S; Barreto, Fabiano; Meneghini, Leonardo; Bergold, Ana Maria

2016-07-01

A reliable and simple method for the detection and quantification of residues of 14 non-steroidal anti-inflammatory drugs and a metamizole metabolite in swine muscle was developed using liquid chromatography-electrospray ionisation-tandem mass spectrometry (LC-ESI-MS/MS). The samples were extracted with acetonitrile (ACN) in solid-liquid extraction followed by a low-temperature partitioning (LLE-LTP) process at -20 ± 2°C. After evaporation to dryness, the residue was reconstituted with hexane and a mixture of water:acetonitrile (1:1). LC separation was achieved on a reversed-phase (RP18) column with gradient elution using water (phase A) and ACN (phase B) both containing 1 mmol l(-)(1) ammonium acetate (NH4COO) with 0.025% acetic acid. Analysis was carried out on a triple-quadrupole tandem mass spectrometer (LC-MS/MS) in multiple reaction monitoring mode using an electrospray interface in negative and positive mode in a single run. Method validation was performed according to the criteria of Commission Decision No. 2002/657/EC. The matrix effect and linearity were evaluated. Decision limit (CCα), detection capability (CCβ), accuracy and repeatability of the method are also reported. The proposed method proved to be simple, easy and adequate for high-throughput analysis and was applied to routine analysis by the Brazilian Ministry of Agriculture, Livestock and Food Supply.

Study of Surface Wave Propagation in Fluid-Saturated Porous Solids.

NASA Astrophysics Data System (ADS)

Azcuaga, Valery Francisco Godinez

1995-01-01

This study addresses the surface wave propagation phenomena on fluid-saturated porous solids. The analytical method for calculation of surface wave velocities (Feng and Johnson, JASA, 74, 906, 1983) is extended to the case of a porous solid saturated with a wetting fluid in contact with a non-wetting fluid, in order to study a material combination suitable for experimental investigation. The analytical method is further extended to the case of a non-wetting fluid/wetting fluid-saturated porous solid interface with an arbitrary finite surface stiffness. These extensions of the analytical method allows to theoretically study surface wave propagation phenomena during the saturation process. A modification to the 2-D space-time reflection Green's function (Feng and Johnson, JASA, 74, 915, 1983) is introduced in order to simulate the behavior of surface wave signals detected during the experimental investigation of surface wave propagation on fluid-saturated porous solids (Nagy, Appl. Phys. Lett., 60, 2735, 1992). This modification, together with the introduction of an excess attenuation for the Rayleigh surface mode, makes it possible to explain the apparent velocity changes observed on the surface wave signals during saturation. Experimental results concerning the propagation of surface waves on an alcohol-saturated porous glass are presented. These experiments were performed at frequencies of 500 and 800 kHz and show the simultaneous propagation of the two surface modes predicted by the extended analytical method. Finally an analysis of the displacements associated with the different surface modes is presented. This analysis reveals that it is possible to favor the generation of the Rayleigh surface mode or of the slow surface mode, simply by changing the type of transducer used in the generation of surface waves. Calculations show that a shear transducer couples more energy into the Rayleigh mode, whereas a longitudinal transducer couples more energy into the slow surface mode. Experimental results obtained with the modified experimental system show a qualitative agreement with the theoretical predictions.

Determination of N,N-dimethyltryptamine in beverages consumed in religious practices by headspace solid-phase microextraction followed by gas chromatography ion trap mass spectrometry.

PubMed

Gaujac, Alain; Dempster, Nicola; Navickiene, Sandro; Brandt, Simon D; de Andrade, Jailson Bittencourt

2013-03-15

A novel analytical approach combining solid-phase microextraction (SPME)/gas chromatography ion trap mass spectrometry (GC-IT-MS) was developed for the detection and quantification N,N-dimethyltryptamine (DMT), a powerful psychoactive indole alkaloid present in a variety of South American indigenous beverages, such as ayahuasca and vinho da jurema. These particular plant products, often used within a religious context, are increasingly consumed throughout the world following an expansion of religious groups and the availability of plant material over the Internet and high street shops. The method described in the present study included the use of SPME in headspace mode combined GC-IT-MS and included the optimization of the SPME procedure using multivariate techniques. The method was performed with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber in headspace mode (70 min at 60 °C) which resulted in good precision (RSD<8.6%) and accuracy values (71-109%). Detection and quantification limits obtained for DMT were 0.78 and 9.5 mg L(-1), respectively and good linearity (1.56-300 mg L(-1), r(2)=0.9975) was also observed. In addition, the proposed method showed good robustness and allowed for the minimization of sample manipulation. Five jurema beverage samples were prepared in the laboratory in order to study the impact of temperature, pH and ethanol on the ability to extract DMT into solution. The developed method was then applied to the analysis of twelve real ayahuasca and vinho da jurema samples, obtained from Brazilian religious groups, which revealed DMT concentration levels between 0.10 and 1.81 g L(-1). Copyright © 2013 Elsevier B.V. All rights reserved.

Iron oxide functionalized graphene oxide as an efficient sorbent for dispersive micro-solid phase extraction of sulfadiazine followed by spectrophotometric and mode-mismatched thermal lens spectrometric determination.

PubMed

Kazemi, Elahe; Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad; Abbasi, Amir; Rashidian Vaziri, Mohammad Reza; Behjat, Abbas

2016-01-15

A simple and rapid dispersive micro-solid phase extraction (DMSPE) combined with mode-mismatched thermal lens spectrometry as well as fiber optic linear array spectrophotometry was developed for the separation, extraction and determination of sulfadiazine. Graphene oxide was synthesized using the modified Hummers method and functionalized with iron oxide nanoparticles by means of a simple one step chemical coprecipitation method. The synthesized iron oxide functionalized graphene oxide was utilized as an efficient sorbent in DMSPE of sulfadiazine. The retained analyte was eluted by using 180µL of a 6:4 mixture of methanol/acetic acid solution and was spectrophotometrically determined based on the formation of an azo dye through coupling with thenoyltrifluoroacetone. Under the optimized conditions, with the application of spectrophotometry technique and with a sample volume of 100mL, the method exhibited a linear dynamic range of 3-80µg L(-1) with a detection limit of 0.82µg L(-1), an enrichment factor of 200 as well as the relative standard deviations of 2.6% and 4.3% (n=6) at 150µg L(-1) level of sulfadiazine for intra- and inter-day analyses, respectively. Whereas, through the application of the thermal lens spectrometry and a sample volume of 10mL, the method exhibited a linear dynamic range of 1-800µg L(-1) with a detection limit of 0.34µg L(-1) and the relative standard deviations of 3.1% and 5.4% (n=6) at 150µg L(-1) level of sulfadiazine for intra- and inter-day analyses, respectively. The method was successfully applied to the determination of sulfadiazine in milk, honey and water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Simultaneous screening and quantification of 29 drugs of abuse in oral fluid by solid-phase extraction and ultraperformance LC-MS/MS.

PubMed

Badawi, Nora; Simonsen, Kirsten Wiese; Steentoft, Anni; Bernhoft, Inger Marie; Linnet, Kristian

2009-11-01

The European DRUID (Driving under the Influence of Drugs, Alcohol And Medicines) project calls for analysis of oral fluid (OF) samples, collected randomly and anonymously at the roadside from drivers in Denmark throughout 2008-2009. To analyze these samples we developed an ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for detection of 29 drugs and illicit compounds in OF. The drugs detected were opioids, amphetamines, cocaine, benzodiazepines, and Delta-9-tetrahydrocannabinol. Solid-phase extraction was performed with a Gilson ASPEC XL4 system equipped with Bond Elut Certify sample cartridges. OF samples (200 mg) diluted with 5 mL of ammonium acetate/methanol (vol/vol 90:10) buffer were applied to the columns and eluted with 3 mL of acetonitrile with aqueous ammonium hydroxide. Target drugs were quantified by use of a Waters ACQUITY UPLC system coupled to a Waters Quattro Premier XE triple quadrupole (positive electrospray ionization mode, multiple reaction monitoring mode). Extraction recoveries were 36%-114% for all analytes, including Delta-9-tetrahydrocannabinol and benzoylecgonine. The lower limit of quantification was 0.5 mug/kg for all analytes. Total imprecision (CV) was 5.9%-19.4%. With the use of deuterated internal standards for most compounds, the performance of the method was not influenced by matrix effects. A preliminary account of OF samples collected at the roadside showed the presence of amphetamine, cocaine, codeine, Delta-9-tetrahydrocannabinol, tramadol, and zopiclone. The UPLC-MS/MS method makes it possible to detect all 29 analytes in 1 chromatographic run (15 min), including Delta-9-tetrahydrocannabinol and benzoylecgonine, which previously have been difficult to incorporate into multicomponent methods.

Computational and Experimental Characterization of Five Crystal Forms of Thymine: Packing Polymorphism, Polytypism/Disorder and Stoichiometric 0.8-Hydrate.

PubMed

Braun, Doris E; Gelbrich, Thomas; Wurst, Klaus; Griesser, Ulrich J

2016-06-01

New polymorphs of thymine emerged in an experimental search for solid forms, which was guided by the computationally generated crystal energy landscape. Three of the four anhydrates (AH) are homeoenergetic ( A° - C ) and their packing modes differ only in the location of oxygen and hydrogen atoms. AHs A° and B are ordered phases, whereas AH C shows disorder (X-ray diffuse scattering). Anhydrates AHs A° and B are ordered phases, whereas AH C shows disorder (X-ray diffuse scattering). Analysis of the crystal energy landscape for alternative AH C hydrogen bonded ribbon motifs identified a number of different packing modes, whose 3D structures were calculated to deviate by less than 0.24 kJ mol -1 in lattice energy. These structures provide models for stacking faults. The three anhydrates A ° - C show strong similarity in their powder X-ray diffraction, thermoanalytical and spectroscopic (IR and Raman) characteristics. The already known anhydrate AH A ° was identified as the thermodynamically most stable form at ambient conditions; AH B and AH C are metastable but show high kinetic stability. The hydrate of thymine is stable only at water activities ( a w ) > 0.95 at temperatures ≤ 25 °C. It was found to be a stoichiometric hydrate despite being a channel hydrate with an unusual water:thymine ratio of 0.8:1. Depending on the dehydration conditions, either AH C or AH D is obtained. The hydrate is the only known precursor to AH D . This study highlights the value and complementarity of simultaneous explorations of computationally and experimentally generated solid form landscapes of a small molecule anhydrate ↔ hydrate system.

Computational and Experimental Characterization of Five Crystal Forms of Thymine: Packing Polymorphism, Polytypism/Disorder and Stoichiometric 0.8-Hydrate

PubMed Central

Braun, Doris E.; Gelbrich, Thomas; Wurst, Klaus; Griesser, Ulrich J.

2017-01-01

New polymorphs of thymine emerged in an experimental search for solid forms, which was guided by the computationally generated crystal energy landscape. Three of the four anhydrates (AH) are homeoenergetic (A° – C) and their packing modes differ only in the location of oxygen and hydrogen atoms. AHs A° and B are ordered phases, whereas AH C shows disorder (X-ray diffuse scattering). Anhydrates AHs A° and B are ordered phases, whereas AH C shows disorder (X-ray diffuse scattering). Analysis of the crystal energy landscape for alternative AH C hydrogen bonded ribbon motifs identified a number of different packing modes, whose 3D structures were calculated to deviate by less than 0.24 kJ mol–1 in lattice energy. These structures provide models for stacking faults. The three anhydrates A° – C show strong similarity in their powder X-ray diffraction, thermoanalytical and spectroscopic (IR and Raman) characteristics. The already known anhydrate AH A° was identified as the thermodynamically most stable form at ambient conditions; AH B and AH C are metastable but show high kinetic stability. The hydrate of thymine is stable only at water activities (aw) > 0.95 at temperatures ≤ 25 °C. It was found to be a stoichiometric hydrate despite being a channel hydrate with an unusual water:thymine ratio of 0.8:1. Depending on the dehydration conditions, either AH C or AH D is obtained. The hydrate is the only known precursor to AH D. This study highlights the value and complementarity of simultaneous explorations of computationally and experimentally generated solid form landscapes of a small molecule anhydrate ↔ hydrate system. PMID:28663717

Investigating the Use of Ultrasonic Guided Waves for Aging Wire Insulation Assessment

NASA Technical Reports Server (NTRS)

Anastasi, Robert F.; Madaras, Eric I.

2002-01-01

Aging wiring has become a critical issue to DoD, NASA, FAA, and Industry. The problem is that insulation on environmentally aged wire becomes brittle and cracks. This exposes the underlying conductive wire to the potential for short circuits and fire. The difficulty is that techniques to monitor aging wire problems focus on applying electrical sensing techniques that are not very sensitive to the wire insulation. Thus, the development of methods to quantify and monitor aging wire insulation is highly warranted. Measurement of wire insulation stiffness by ultrasonic guided waves is being examined. Initial laboratory tests were performed on a simple model consisting of a solid cylinder and then a solid cylinder with a polymer coating. Experimental measurements showed that the lowest order axisymmetric mode may be sensitive to stiffness changes in the wire insulation. To test this theory, mil-spec wire samples MIL-W-81381, MIL-W-22759/34, and MIL-W-22759/87 (typically found in aircraft) were heat-damaged in an oven, in a range of heating conditions. The samples were 12, 16, and 20 gauge and the heat-damage introduced material changes in the wire-insulation that made the originally flexible insulation brittle and darker in color. Axisymmetric mode phase velocity increased for the samples that were exposed to heat for longer duration. For example, the phase velocity in the 20-gauge MIL-W-22759/34 wire changed from a baseline value of 2790m/s to 3280m/s and 3530m/s for one-hour exposures to 3490C and 3990C, respectively. Although the heat-damage conditions are not the same as environmental aging, we believe that with further development and refinements, the ultrasonic guided waves can be used to inspect wire-insulation for detrimental environmental aging conditions.

Noise properties of an optical frequency comb from a SESAM-mode-locked 1.5-μm solid-state laser stabilized to the 10-13 level

NASA Astrophysics Data System (ADS)

Schilt, S.; Dolgovskiy, V.; Bucalovic, N.; Schori, C.; Stumpf, M. C.; Di Domenico, G.; Pekarek, S.; Oehler, A. E. H.; Südmeyer, T.; Keller, U.; Thomann, P.

2012-11-01

We present a detailed investigation of the noise properties of an optical frequency comb generated from a femtosecond diode-pumped solid-state laser operating in the 1.5-μm spectral region. The stabilization of the passively mode-locked Er:Yb:glass laser oscillator, referred to as ERGO, is achieved using pump power modulation for the control of the carrier envelope offset (CEO) frequency and by adjusting the laser cavity length for the control of the repetition rate. The stability and the noise of the ERGO comb are characterized in free-running and in phase-locked operation by measuring the noise properties of the CEO, of the repetition rate, and of a comb line at 1558 nm. The comb line is analyzed from the heterodyne beat signal with a cavity-stabilized ultra-narrow-linewidth laser using a frequency discriminator. Two different schemes to stabilize the comb to a radio-frequency (RF) reference are compared. The comb properties (phase noise, frequency stability) are limited in both cases by the RF oscillator used to stabilize the repetition rate, while the contribution of the CEO is negligible at all Fourier frequencies, as a consequence of the low-noise characteristics of the CEO-beat. A linewidth of ≈150 kHz and a fractional frequency instability of 4.2×10-13 at 1 s are obtained for an optical comb line at 1558 nm. Improved performance is obtained by stabilizing the comb to an optical reference, which is a cavity-stabilized ultra-narrow linewidth laser at 1558 nm. The fractional frequency stability of 8×10-14 at 1 s, measured in preliminary experiments, is limited by the reference oscillator used in the frequency comparison.

Effects of 3 Feeding Modes on the Volatile and Nonvolatile Compounds in the Edible Tissues of Female Chinese Mitten Crab (Eriocheir sinensis).

PubMed

Zhuang, Kejin; Wu, Na; Wang, Xichang; Wu, Xugan; Wang, Shuai; Long, Xiaowen; Wei, Xuan

2016-04-01

To reveal the impact of different feeding modes on the flavor quality of female Chinese mitten crab (Eriocheir sinensis) this study was conducted to compare the sensory evaluation scores, flavor compounds in meat and hepatopancreas of female E. sinensis fed with 3 feeding modes, that is, natural diets (NDs), traditional diets (TDs), and formulated diets (FDs). The result showed that crabs fed with ND had significantly lower sensory scores than the other 2 feeding modes in both edible tissues. The odor and taste profiles were evaluated by Electronic nose (E-nose) and tongue (E-tongue) techniques, respectively; results of perchloric acid showed each edible tissue had significant differences among the 3 modes. Contents of volatile compounds were measured by Headspace-solid phase micro extraction combined with gas chromatography-mass spectrometer. A total of 35 and 44 volatile compounds were identified in meat and hepatopancreas, respectively. ND mode of meat had the highest relative odor activity value (ROAV) summation among the 3 diet modes. TD mode of hepatopancreas had significantly higher ROAV summations. Based on the analysis of free amino acids and 5'-nucleotides, nonvolatile compounds were evaluated by equivalent umami concentration (EUC) and taste active values (TAVs) methods. For both meat and hepatopancreas, TD had the highest contents of umami amino acid, as for the 5'-nucleotide, FD had the highest 5'-inosin monophosphate concentrations. Overall, the EUC and TAVs of TD were higher than that of FD, whereas ND mode had the lowest values in the 2 edible tissues. In conclusion, TD mode had the best performance in terms of sensory evaluation, ROAVs of aroma-active compounds, and nonvolatile active compounds. © 2016 Institute of Food Technologists®

Fabrication of a saturable absorber WS2 and its mode locking in solid-state laser

NASA Astrophysics Data System (ADS)

Zhang, Chun-Yu; Zhang, Ling; Tang, Xiao-Ying; Yang, Ying-Ying

2018-04-01

We report on a passively mode-locked Nd : LuVO4 laser using a type saturable absorber of tungsten disulfide (WS2) fabricated by chemical vapor deposition method. At the pump power of 3.3 W, 1.18-W average output power of continuous-wave mode-locked laser with optical conversion efficiency of 36% was achieved. To the best of our knowledge, this is the highest output power of passively mode-locked solid-state laser based on WS2. The repetition rate of passively mode-locked pulse was 80 MHz with the pulse energy of 14.8 nJ. Our experimental results show that WS2 is an excellent type of saturable absorber.

Contrast Dose and Radiation Dose Reduction in Abdominal Enhanced Computerized Tomography Scans with Single-phase Dual-energy Spectral Computerized Tomography Mode for Children with Solid Tumors

PubMed Central

Yu, Tong; Gao, Jun; Liu, Zhi-Min; Zhang, Qi-Feng; Liu, Yong; Jiang, Ling; Peng, Yun

2017-01-01

Background: Contrast dose and radiation dose reduction in computerized tomography (CT) scan for adult has been explored successfully, but there have been few studies on the application of low-concentration contrast in pediatric abdominal CT examinations. This was a feasibility study on the use of dual-energy spectral imaging and adaptive statistical iterative reconstruction (ASiR) for the reduction of radiation dose and iodine contrast dose in pediatric abdominal CT patients with solid tumors. Methods: Forty-five patients with solid tumors who had initial CT (Group B) and follow-up CT (Group A) after chemotherapy were enrolled. The initial diagnostic CT scan (Group B) was performed using the standard two-phase enhanced CT with 320 mgI/ml concentration contrast, and the follow-up scan (Group A) was performed using a single-phase enhanced CT at 45 s after the beginning of the 270 mgI/ml contrast injection using spectral mode. Forty percent ASiR was used for the images in Group B and monochromatic images with energy levels ≥60 keV in Group A. In addition, filtered back-projection (FBP) reconstruction was used for monochromatic images <60 keV in Group A. The total radiation dose, total iodine load, contrast injection speed, and maximum injection pressure were compared between the two groups. The 40 keV and 60 keV spectral CT images of Group A were compared with the images of Group B to evaluate overall image quality. Results: The total radiation dose, total iodine load, injection speed, and maximum injection pressure for Group A were decreased by 19%, 15%, 34.4%, and 18.3%, respectively. The optimal energy level in spectral CT for displaying the abdominal vessels was 40 keV. At this level, the CT values in the abdominal aorta and its three branches, the portal vein and its two branches, and the inferior vena cava were all greater than 340 hounsfield unit (HU). The abdominal organs of Groups A and B had similar degrees of absolute and relative enhancement (t = 0.36 and −1.716 for liver, −0.153 and −1.546 for pancreas, and 2.427 and 0.866 for renal cortex, all P > 0.05). Signal-to-noise ratio of the abdominal organs was significantly lower in Group A than in Group B (t = −8.11 for liver, −7.83 for pancreas, and −5.38 for renal cortex, all P < 0.05). However, the subjective scores for the 40 keV (FBP) and 60 keV (40% ASiR) spectral CT images determined by two radiologists were all >3, indicating clinically acceptable image quality. Conclusions: Single-phase, dual-energy spectral CT used for children with solid abdominal tumors can reduce contrast dose and radiation dose and can also maintain clinically acceptable image quality. PMID:28345547

Contrast Dose and Radiation Dose Reduction in Abdominal Enhanced Computerized Tomography Scans with Single-phase Dual-energy Spectral Computerized Tomography Mode for Children with Solid Tumors.

PubMed

Yu, Tong; Gao, Jun; Liu, Zhi-Min; Zhang, Qi-Feng; Liu, Yong; Jiang, Ling; Peng, Yun

2017-04-05

Contrast dose and radiation dose reduction in computerized tomography (CT) scan for adult has been explored successfully, but there have been few studies on the application of low-concentration contrast in pediatric abdominal CT examinations. This was a feasibility study on the use of dual-energy spectral imaging and adaptive statistical iterative reconstruction (ASiR) for the reduction of radiation dose and iodine contrast dose in pediatric abdominal CT patients with solid tumors. Forty-five patients with solid tumors who had initial CT (Group B) and follow-up CT (Group A) after chemotherapy were enrolled. The initial diagnostic CT scan (Group B) was performed using the standard two-phase enhanced CT with 320 mgI/ml concentration contrast, and the follow-up scan (Group A) was performed using a single-phase enhanced CT at 45 s after the beginning of the 270 mgI/ml contrast injection using spectral mode. Forty percent ASiR was used for the images in Group B and monochromatic images with energy levels ≥60 keV in Group A. In addition, filtered back-projection (FBP) reconstruction was used for monochromatic images <60 keV in Group A. The total radiation dose, total iodine load, contrast injection speed, and maximum injection pressure were compared between the two groups. The 40 keV and 60 keV spectral CT images of Group A were compared with the images of Group B to evaluate overall image quality. The total radiation dose, total iodine load, injection speed, and maximum injection pressure for Group A were decreased by 19%, 15%, 34.4%, and 18.3%, respectively. The optimal energy level in spectral CT for displaying the abdominal vessels was 40 keV. At this level, the CT values in the abdominal aorta and its three branches, the portal vein and its two branches, and the inferior vena cava were all greater than 340 hounsfield unit (HU). The abdominal organs of Groups A and B had similar degrees of absolute and relative enhancement (t = 0.36 and -1.716 for liver, -0.153 and -1.546 for pancreas, and 2.427 and 0.866 for renal cortex, all P> 0.05). Signal-to-noise ratio of the abdominal organs was significantly lower in Group A than in Group B (t = -8.11 for liver, -7.83 for pancreas, and -5.38 for renal cortex, all P< 0.05). However, the subjective scores for the 40 keV (FBP) and 60 keV (40% ASiR) spectral CT images determined by two radiologists were all> 3, indicating clinically acceptable image quality. Single-phase, dual-energy spectral CT used for children with solid abdominal tumors can reduce contrast dose and radiation dose and can also maintain clinically acceptable image quality.

The resistance of Bacillus atrophaeus spores to the bactericidal activity of peracetic acid is influenced by both the nature of the solid substrates and the mode of contamination.

PubMed

Grand, I; Bellon-Fontaine, M-N; Herry, J-M; Hilaire, D; Moriconi, F-X; Naïtali, M

2010-11-01

To evaluate the impact of the mode of contamination in relation with the nature of solid substrates on the resistance of spores of Bacillus atrophaeus -selected as surrogates of Bacillus anthracis- to a disinfectant, peracetic acid. Six materials confronted in urban and military environments were selected for their different structural and physicochemical properties. In parallel, two modes of contamination were examined, i.e. deposition and immersion. Deposition was used to simulate contamination by an aerosol and immersion by an extended contact with liquids. A pronounced difference in the biocontamination levels and spatial organization of spores was observed depending on the mode of contamination and the nature of the solid substrate considered, with consequences on decontamination. Contamination by immersion led to lower efficiency of peracetic acid decontamination than contamination by deposition. Infiltration of spores into porous materials after immersion is one reason. In contrast, the deposition mode aggregates cells at the surface of materials, explaining the similar disinfecting behaviour of porous and nonporous substrates when considering this inoculation route. The inoculation route was shown to be as influential a parameter as material characteristics (porosity and wettability) for decontamination efficacy. These results provide comparative information for the decontamination of B. atrophaeus spores in function of the mode of contamination and the nature of solid substrates. Journal of Applied Microbiology © 2010 The Society for Applied Microbiology. No claim to French government works.

Mini-cavity plasma core reactors for dual-mode space nuclear power/propulsion systems. M.S. Thesis

NASA Technical Reports Server (NTRS)

Chow, S.

1976-01-01

A mini-cavity plasma core reactor is investigated for potential use in a dual-mode space power and propulsion system. In the propulsive mode, hydrogen propellant is injected radially inward through the reactor solid regions and into the cavity. The propellant is heated by both solid driver fuel elements surrounding the cavity and uranium plasma before it is exhausted out the nozzle. The propellant only removes a fraction of the driver power, the remainder is transferred by a coolant fluid to a power conversion system, which incorporates a radiator for heat rejection. Neutronic feasibility of dual mode operation and smaller reactor sizes than those previously investigated are shown to be possible. A heat transfer analysis of one such reactor shows that the dual-mode concept is applicable when power generation mode thermal power levels are within the same order of magnitude as direct thrust mode thermal power levels.

Selective excitation of LG 00, LG 01, and LG 02 modes by a solid core PCF based mode selector in MDM-Ro-FSO transmission systems

NASA Astrophysics Data System (ADS)

Chaudhary, Sushank; Amphawan, Angela

2018-07-01

Radio over free space (Ro-FSO) provides an ambitious platform for seamless integration of radio networks to optical networks. Three independent channels, each carrying 2.5 Gbps–5 GHz data, are successfully transmitted over a free space link of 2.5 km by using mode division multiplexing (MDM) of three modes LG 00, LG 01, and LG 02 modes in conjunction with solid core photonic crystal fibers (SC-PCFs). Moreover, SC-PCFs are used as a mode selector in the proposed MDM-Ro-FSO system. The results are reported in terms of bit error rate, mode spectrum, and spatial profiles. The performance of the proposed Ro-FSO system is also evaluated under the influence of atmospheric turbulence in the form of different levels of fog, namely, light fog, thin fog, and heavy fog.

Simultaneous determination of esculin and its metabolite esculetin in rat plasma by LC-ESI-MS/MS and its application in pharmacokinetic study.

PubMed

Li, Ying-yi; Song, Ye-ying; Liu, Chang-hui; Huang, Xiao-tao; Zheng, Xia; Li, Neng; Xu, Mei-li; Mi, Sui-qing; Wang, Ning-sheng

2012-10-15

A new liquid chromatography-tandem mass spectrometry (LC-MS/MS) method operated in the negative electrospray ionization (ESI) switching mode has been developed and validated for the simultaneous determination of esculin and its metabolite esculetin in rat plasma. After addition of internal standards scopoletin, the plasma sample was pretreated by solid-phase extraction (SPE), and separated on a reversed phase C(18) column with a mobile phase of 0.01% formic acid in water (solvent A) and methanol (solvent B) using isocratic elution (A:B=20:80, v/v). The detection of target compounds was done in multiple reaction monitoring (MRM) mode. The MRM detection was operated in the negative ESI mode using the transitions of m/z 339.1 ([M-H](-))→176.7 for esculetin, m/z 176.9 ([M-H](-))→133.0 and m/z 191.0 ([M-H](-))→175.9 for scopoletin. The standard curves, which ranged from 25 to 3200 ng/mL for esculin with the lowest limit of quantification (LLOQ) of 0.25 ng/mL and from 1.25 to 160 ng/mL for esculetin with the LLOQ of 1.25 ng/mL, were fitted to a 1/x weighted quadratic regression model. The method also afforded satisfactory results in terms of the sensitivity, specificity, precision (intra- and inter-day, RSD<8.73%), accuracy, recovery as well as the stability of the analyte under various conditions. The method was successfully applied to study the pharmacokinetics of esculin and its metabolite esculetin in rat plasma after oral administration of esculin at a dose of 100mg/kg. Copyright © 2012 Elsevier B.V. All rights reserved.

Development and Validation of an LC-MS-MS Method for Determination of Simvastatin and Simvastatin Acid in Human Plasma: Application to a Pharmacokinetic Study.

PubMed

Partani, Pankaj; Verma, Saurabh Manaswita; Monif, Tausif

2016-09-01

A liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous determination of simvastatin (SV) and simvastatin acid (SVA) in human plasma. To improve assay sensitivity and achieve simultaneous analysis, SVA monitored in (-)ESI (electrospray ionization) mode within the first 4.5 min and SV thereafter in (+)ESI mode. The separation of all compounds was achieved in about 6.2 min using a C18 reverse-phase fused-core(®) column (Ascentis(®) Express C18) and a mobile phase, which was composed of 2.00 ± 0.05 mM ammonium acetate buffer titrated to pH 3.8 with glacial acetic acid-acetonitrile (25:75, v/v), in isocratic mode at a flow rate of 0.500 mL/min. Additionally, a solid-phase extraction step was performed to reduce any ion-suppression and/or enhancement effects. The developed method was linear in the concentration range of 0.100-74.626 ng/mL for SV, and 0.100-48.971 ng/mL for SVA, with correlation coefficient greater than 0.99 for both analytes. The method has shown tremendous reproducibility, with intra- and inter-day precision <7.6%, and intra- and interday accuracy within ±10.9% of nominal values, for the both analytes. The method was successfully applied to characterize the pharmacokinetic profiles of SV and SVA following an oral administration of 40 mg SV tablet to healthy human volunteers. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Evaluation of bi-functionalized mesoporous silicas as reversed phase/cation-exchange mixed-mode sorbents for multi-residue solid phase extraction of veterinary drug residues in meat samples.

PubMed

Casado, Natalia; Pérez-Quintanilla, Damián; Morante-Zarcero, Sonia; Sierra, Isabel

2017-04-01

A SBA-15 type mesoporous silica was synthesized and bi-functionalized with octadecylsilane (C18) or octylsilane (C8), and sulfonic acid (SO 3 - ) groups in order to obtain materials with reversed-phase/strong cation-exchange mixed-mode retention mechanism. The resulting hybrid materials (SBA-15-C18-SO 3 - and SBA-15-C8-SO 3 - ) were comprehensively characterized. They showed high surface area, high pore volume and controlled porous size. Elemental analysis of the materials revealed differences in the amount of C18 and C8. SBA-15-C18-SO 3 - contained 0.19mmol/g of C18, while SBA-15-C8-SO 3 - presented 0.54mmol/g of C8. The SO 3 - groups anchored to the silica surface of the pore walls were 0.20 and 0.09mmol/g, respectively. The bi-functionalized materials were evaluated as SPE sorbents for the multi-residue extraction of 26 veterinary drug residues in meat samples using ultra-high-performance liquid chromatography coupled to mass spectrometry detector (UHPLC-MS/MS). Different sorbent amounts (100 and 200mg) and organic solvents were tested to optimize the extraction procedure. Both silicas showed big extraction potential and were successful in the extraction of the target analytes. The mixed-mode retention mechanism was confirmed by comparing both silicas with SBA-15 mesoporous silica mono-functionalized with C18 and C8. Best results were achieved with 200mg of SBA-15-C18-SO 3 - obtaining recoveries higher than 70% for the majority of analytes. Copyright © 2016 Elsevier B.V. All rights reserved.

Mode conversion efficiency to Laguerre-Gaussian OAM modes using spiral phase optics.

PubMed

Longman, Andrew; Fedosejevs, Robert

2017-07-24

An analytical model for the conversion efficiency from a TEM 00 mode to an arbitrary Laguerre-Gaussian (LG) mode with null radial index spiral phase optics is presented. We extend this model to include the effects of stepped spiral phase optics, spiral phase optics of non-integer topological charge, and the reduction in conversion efficiency due to broad laser bandwidth. We find that through optimization, an optimal beam waist ratio of the input and output modes exists and is dependent upon the output azimuthal mode number.

Femtosecond Fiber Lasers

NASA Astrophysics Data System (ADS)

Bock, Katherine J.

This thesis focuses on research I have done on ytterbium-doped femtosecond fiber lasers. These lasers operate in the near infrared region, lasing at 1030 nm. This wavelength is particularly important in biomedical applications, which includes but is not limited to confocal microscopy and ablation for surgical incisions. Furthermore, fiber lasers are advantageous compared to solid state lasers in terms of their cost, form factor, and ease of use. Solid state lasers still dominate the market due to their comparatively high energy pulses. High energy pulse generation in fiber lasers is hindered by either optical wave breaking or by multipulsing. One of the main challenges for fiber lasers is to overcome these limitations to achieve high energy pulses. The motivation for the work done in this thesis is increasing the output pulse peak power and energy. The main idea of the work is that decreasing the nonlinearity that acts on the pulse inside the cavity will prevent optical wave breaking, and thus will generate higher energy pulses. By increasing the output energy, ytterbium-doped femtosecond fiber lasers can be competitive with solid state lasers which are used commonly in research. Although fiber lasers tend to lack the wavelength tuning ability of solid state lasers, many biomedical applications take advantage of the 1030 microm central wavelength of ytterbium-doped fiber lasers, so the major limiting factor of fiber lasers in this field is simply the output power. By increasing the output energy without resorting to external amplification, the cavity is optimized and cost can remain low and economical. During verification of the main idea, the cavity was examined for possible back-reflections and for components with narrow spectral bandwidths which may have contributed to the presence of multipulsing. Distinct cases of multipulsing, bound pulse and harmonic mode-locking, were observed and recorded as they may be of more interest in the future. The third-order dispersion contribution from the diffraction gratings inside the laser cavity was studied, as it was also considered to be an energy-limiting factor. No significant effect was found as a result of third-order dispersion; however, a region of operation was observed where two different pulse regimes were found at the same values of net cavity group velocity dispersion. Results verify the main idea and indicate that a long length of low-doped gain fiber is preferable to a shorter, more highly doped one. The low-doped fiber in an otherwise equivalent cavity allows the nonlinear phase shift to grow at a slower rate, which results in the pulse achieving a higher peak power before reaching the nonlinear phase shift threshold at which optical wave breaking occurs. For a range of net cavity group velocity dispersion values, the final result is that the low doped fiber generates pulses of approximately twice the value of energy of the highly-doped gain fiber. Two techniques of mode-locking cavities were investigated to achieve this result. The first cavity used NPE mode-locking which masked the results, and the second used a SESAM for mode-locking which gave clear results supporting the hypothesis.

In situ Observation of Phase Transformation in MnAl(C) Magnetic Materials

PubMed Central

Si, Ping-Zhan; Qian, Hui-Dong; Choi, Chul-Jin; Park, Jihoon; Han, Sangho; Ge, Hong-Liang; Shinde, Kiran P.

2017-01-01

The phase transformation in two modes, including both displacive and massive growth of τ-phase from ε-MnAl(C), was observed by in situ transmission electron microscopy. The exact temperature range for different phase transformation modes was determined by magnetic measurements. The displacive growth of ε→τ in Mn54Al46 (or Mn54Al46C2.44) occurs at temperatures below 650 K (or 766 K), above which both modes coexist. One-third or less of the ε-phase can be transformed into τ-phase via displacive mode while the remaining two-thirds or more via massive mode. In bulk τ-phase, most τ-nanocrystals formed via displacive mode are distributed in the matrix of large τ-grains that formed via massive mode. The typical massive growth rate of the τ-phase is 8–60 nm/s, while the displacive growth rate is low. A more complete understanding of the ε→τ phase transformations in the MnAl-based magnets was provided in this work, based on which the annealing process for ε→τ was optimized and thus high purity τ-phase with high saturation magnetization was obtained. PMID:28858231

Infrared observations and laboratory simulations of interstellar CH_4_ and SO_2_.

NASA Astrophysics Data System (ADS)

Boogert, A. C. A.; Schutte, W. A.; Helmich, F. P.; Tielens, A. G. G. M.; Wooden, D. H.

1997-02-01

Interstellar CH_4_ may consume a fair amount of the carbon budget in dense molecular clouds, but probably less than CO, CH_3_OH, and CO_2_. However, it can only be observed at wavelength regions in the infrared that are heavily affected by the earth atmosphere. With new space and airborne missions (e.g. ISO, SOFIA) in mind we have studied the near infrared absorption spectra of solid and gaseous CH_4_. We obtained laboratory spectra of the ν_4_ deformation mode (1302cm^-1^, 7.68μm) of solid CH_4_ in astrophysically relevant mixtures. We found that the peak position and width of this absorption band vary strongly as a function of molecular environment, compared to temperature and particle shape effects. Hence, observations of this feature will provide a powerful probe of the molecular composition of interstellar ices. Also the gas phase CH_4_ ro-vibrational spectrum of the same band has been calculated. Using observed physical conditions around the protostar W 33A, we show that unresolved gaseous CH_4_ lines are detectable (at the 2-5% level) at a resolution R>1000, when the column density N>=10^16^ cm^-2^. An astrophysically relevant molecule with a very strong transition in the same wavelength regime, is SO_2_. We studied the ν _3_ asymmetric stretching mode (1319 cm^-1^, 7.58 μm) of solid SO_2_ in several mixtures, revealing that the peak position, width and detailed profile of this band are very sensitive to the molecular environment. Besides probing the composition of ice mantles, observations of solid SO_2_ will provide important information on the sulfur budget locked up in grain mantles, which is currently poorly known. We compare the laboratory and calculated spectra of CH_4_ and SO_2_ with previously published ground based spectra and new airborne observations of young stellar objects in the 7-8μm region. W 33A, NGC 7538 : IRS1 and IRS9 show a feature near 7.68μm that is consistent with absorption by solid CH_4_ or the Q-branch of gaseous CH_4_. The column density of solid CH_4_ would be 0.3-4% of solid H_2_O, indicating that solid CH_4_ consumes 0.5+/-0.3% of the cosmic carbon abundance. A gaseous origin would imply a column density of at least this amount, being highly dependent on the assumed temperature of the absorbing gas. A second absorption feature is detected toward W 33A and NGC 7538 : IRS1 at 7.58 μm. The peak position and width of this feature are consistent with the ν_3_ mode of solid SO_2_ in a matrix of solid CH_3_OH or pure SO_2_. The derived column density is 0.1-1% of solid H_2_O, indicating that solid SO_2_ locks up 0.6-6% of the cosmic sulfur abundance. This study shows that 7-8μm spectroscopy of dense molecular clouds, using new airborne and space-based platforms, will provide valuable information on the composition of icy grain mantles and molecular cloud chemistry.

Wave propagation through elastic porous media containing two immiscible fluids

NASA Astrophysics Data System (ADS)

Lo, Wei-Cheng; Sposito, Garrison; Majer, Ernest

2005-02-01

Acoustic wave phenomena in porous media containing multiphase fluids have received considerable attention in recent years because of an increasing scientific awareness of poroelastic behavior in groundwater aquifers. To improve quantitative understanding of these phenomena, a general set of coupled partial differential equations was derived to describe dilatational wave propagation through an elastic porous medium permeated by two immiscible fluids. These equations, from which previous models of dilatational wave propagation can be recovered as special cases, incorporate both inertial coupling and viscous drag in an Eulerian frame of reference. Two important poroelasticity concepts, the linearized increment of fluid content and the closure relation for porosity change, originally defined for an elastic porous medium containing a single fluid, also are generalized for a two-fluid system. To examine the impact of relative fluid saturation and wave excitation frequency (50, 100, 150, and 200 Hz) on free dilatational wave behavior in unconsolidated porous media, numerical simulations of the three possible modes of wave motion were conducted for Columbia fine sandy loam containing either an air-water or oil-water mixture. The results showed that the propagating (P1) mode, which results from in-phase motions of the solid framework and the two pore fluids, moves with a speed equal to the square root of the ratio of an effective bulk modulus to an effective density of the fluid-containing porous medium, regardless of fluid saturation and for both fluid mixtures. The nature of the pore fluids exerts a significant influence on the attenuation of the P1 wave. In the air-water system, attenuation was controlled by material density differences and the relative mobilities of the pore fluids, whereas in the oil-water system an effective kinematic shear viscosity of the pore fluids was the controlling parameter. On the other hand, the speed and attenuation of the two diffusive modes (P2, resulting from out-of-phase motions of the solid framework and the fluids, and P3, the result of capillary pressure fluctuations) were closely associated with an effective dynamic shear viscosity of the pore fluids. The P2 and P3 waves also had the same constant value of the quality factor, and by comparison of our results with previous research on these two dilatational wave modes in sandstones, both were found to be sensitive to the state of consolidation of the porous medium.

Precipitation in Al–Mg solid solution prepared by solidification under high pressure

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

Jie, J.C., E-mail: jiejc@dlut.edu.cn; School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001; Wang, H.W.

2014-01-15

The precipitation in Al–Mg solid solution containing 21.6 at.% Mg prepared by solidification under 2 GPa was investigated. The results show that the γ-Al{sub 12}Mg{sub 17} phase is formed and the β′ phase cannot be observed in the solid solution during ageing process. The precipitation of γ and β phases takes place in a non-uniform manner during heating process, i.e. the γ and β phases are first formed in the interdendritic region, which is caused by the inhomogeneous distribution of Mg atoms in the solid solution solidified under high pressure. Peak splitting of X-ray diffraction patterns of Al(Mg) solid solutionmore » appears, and then disappears when the samples are aged at 423 K for different times, due to the non-uniform precipitation in Al–Mg solid solution. The direct transformation from the γ to β phase is observed after ageing at 423 K for 24 h. It is considered that the β phase is formed through a peritectoid reaction of α + γ → β which needs the diffusion of Mg atoms across the interface of α/γ phases. - Highlights: • The γ phase is formed and the β′ phase is be observed in Al(Mg) solid solution. • Peak splitting of XRD pattern of Al(Mg) solid solution appears during aged at 150 °C. • The β phase is formed through a peritectoid reaction of α + γ → β.« less

Optimization of high solids fed-batch saccharification of sugarcane bagasse based on system viscosity changes.

PubMed

Liu, Yunyun; Xu, Jingliang; Zhang, Yu; Yuan, Zhenhong; Xie, Jun

2015-10-10

Viscosity trends in alkali-pretreated sugarcane bagasse (SCB) slurries undergoing high solids fed-batch enzymatic hydrolysis were measured for a range of solids loading from 15% to 36%. Solids liquefaction times were related to system viscosity changes. The viscosity decreased quickly for low solids loading, and increased with increasing solids content. Fed-batch hydrolysis was initiated with 15% solids loading, and an additional 8%, 7% and 6% were successively added after the system viscosity decreased to stable values to achieve a final solids content of 36%. Two enzyme-adding modes with 8.5FPU/g solid were investigated. The batch mode with all enzyme being added at the beginning of the reaction produced the highest yields, with approximately 231.7g/L total sugars and 134.9g/L glucose being obtained after 96h with nearly 60% of the final glucan conversion rate. This finding indicates that under the right conditions, the fed-batch strategy might be a plausible way to produce high sugars under high solids. Copyright © 2015 Elsevier B.V. All rights reserved.

Phase control of entanglement and quantum steering in a three-mode optomechanical system

NASA Astrophysics Data System (ADS)

Sun, F. X.; Mao, D.; Dai, Y. T.; Ficek, Z.; He, Q. Y.; Gong, Q. H.

2017-12-01

The theory of phase control of coherence, entanglement and quantum steering is developed for an optomechanical system composed of a single mode cavity containing a partially transmitting dielectric membrane and driven by short laser pulses. The membrane divides the cavity into two mutually coupled optomechanical cavities resulting in an effective three-mode closed loop system, two field modes of the two cavities and a mechanical mode representing the oscillating membrane. The closed loop in the coupling creates interfering channels which depend on the relative phase of the coupling strengths of the field modes to the mechanical mode. Populations and correlations of the output modes are calculated analytically and show several interesting phase dependent effects such as reversible population transfer from one field mode to the other, creation of collective modes, and induced coherence without induced emission. We find that these effects result from perfect mutual coherence between the field modes which is preserved even if one of the modes is not populated. The inseparability criterion for the output modes is also investigated and we find that entanglement may occur only between the field modes and the mechanical mode. We show that depending on the phase, the field modes can act on the mechanical mode collectively or individually resulting, respectively, in tripartite or bipartite entanglement. In addition, we examine the phase sensitivity of quantum steering of the mechanical mode by the field modes. Deterministic phase transfer of the steering from bipartite to collective is predicted and optimum steering corresponding to perfect EPR state can be achieved. These different types of quantum steering can be distinguished experimentally by measuring the coincidence rate between two detectors adjusted to collect photons of the output cavity modes. In particular, we find that the minima of the interference pattern of the coincidence rate signal the bipartite steering, while the maxima signal the collective steering.

FIBER AND INTEGRATED OPTICS, LASER APPLICATIONS, AND OTHER PROBLEMS IN QUANTUM ELECTRONICS: Optical components for the analysis and formation of the transverse mode composition

NASA Astrophysics Data System (ADS)

Golub, M. A.; Sisakyan, I. N.; Soĭfer, V. A.; Uvarov, G. V.

1989-04-01

Theoretical and experimental investigations are reported of new mode optical components (elements) which are analogs of sinusoidal phase diffraction gratings with a variable modulation depth. Expressions are derived for nonlinear predistortion and depth of modulation, which are essential for effective operation of amplitude and phase mode optical components in devices used for analysis and formation of the transverse mode composition of coherent radiation. An estimate is obtained of the energy efficiency of phase and amplitude mode optical components, and a comparison is made with the results of an experimental investigation of a set of phase optical components matched to Gauss-Laguerre modes. It is shown that the improvement in the energy efficiency of phase mode components, compared with amplitude components, is the same as the improvement achieved using a phase diifraction grating, compared with amplitude grating with the same depth of modulation.

A two-pronged approach to detecting ICB Stoneley modes

NASA Astrophysics Data System (ADS)

Jasperson, H. A.; Ye, J.; Shi, J.; De Hoop, M. V.

2017-12-01

Stoneley modes are special kinds of normal modes that are confined to the boundary between a fluid layer and a solid layer inside the Earth. Thus, these modes theoretically occur at the core-mantle boundary (CMB) and inner core boundary (ICB). CMB Stoneley modes were identified in observational data by Koelemeijer, et al. in 2013, but ICB Stoneley modes have remained relatively unexplored. Here we use a joint numerical and data-driven approach to identify ICB Stoneley modes from the deep 2013 Mw 8.3 Sea of Okhotsk earthquake. For the data-driven portion, we use 50 stacked traces from the USArray to identify potential occurrences of ICB Stoneley modes. Next, we verify each occurrence by comparing the spectrum to its equivalent from the shallow 2011 Mw 9.1 Tohoku earthquake. We also develop a novel computational approach to compute normal modes in a spherically symmetric non-rotating Earth building on the work of Wiggins (1976) and Buland and Gilbert (1984). We successfully resolve the clustering eigenvalue problem with non-orthogonal eigenfunctions from which Mineos suffers. By choosing the displacement/pressure formulation in the fluid outer core and handling boundary conditions properly, we remarkably project out the essential spectrum and provide the correct point spectrum. The utilization of weak variational form to perform the Rayleigh-Ritz procedure contributes to preserving the high accuracy across the solid-fluid boundary, which makes it possible to capture Stoneley modes' exponentially decaying behavior across the solid-fluid boundary, leading to more accurate and reliable eigenvalues and eigenfunctions. This allows us to compare the observation data and numerical computations. With this approach, we eliminate false signals from consideration, leaving only true ICB Stoneley mode peaks. In the future, information from these modes can be used to study the properties of the ICB and inner core.

Scalability, Scintillation Readout and Charge Drift in a Kilogram Scale Solid Xenon Particle Detector

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

Yoo, J.; Cease, H.; Jaskierny, W. F.

2014-10-23

We report a demonstration of the scalability of optically transparent xenon in the solid phase for use as a particle detector above a kilogram scale. We employ a liquid nitrogen cooled cryostat combined with a xenon purification and chiller system to measure the scintillation light output and electron drift speed from both the solid and liquid phases of xenon. Scintillation light output from sealed radioactive sources is measured by a set of high quantum efficiency photomultiplier tubes suitable for cryogenic applications. We observed a reduced amount of photons in solid phase compared to that in liquid phase. We used amore » conventional time projection chamber system to measure the electron drift time in a kilogram of solid xenon and observed faster electron drift speed in the solid phase xenon compared to that in the liquid phase.« less

Fuel spill identification using solid-phase extraction and solid-phase microextraction. 1. Aviation turbine fuels.

PubMed

Lavine, B K; Brzozowski, D M; Ritter, J; Moores, A J; Mayfield, H T

2001-12-01

The water-soluble fraction of aviation jet fuels is examined using solid-phase extraction and solid-phase microextraction. Gas chromatographic profiles of solid-phase extracts and solid-phase microextracts of the water-soluble fraction of kerosene- and nonkerosene-based jet fuels reveal that each jet fuel possesses a unique profile. Pattern recognition analysis reveals fingerprint patterns within the data characteristic of fuel type. By using a novel genetic algorithm (GA) that emulates human pattern recognition through machine learning, it is possible to identify features characteristic of the chromatographic profile of each fuel class. The pattern recognition GA identifies a set of features that optimize the separation of the fuel classes in a plot of the two largest principal components of the data. Because principal components maximize variance, the bulk of the information encoded by the selected features is primarily about the differences between the fuel classes.

Structural and optical properties of rare earth-doped (Ba{sub 0.77}Ca{sub 0.23}){sub 1-x}(Sm, Nd, Pr, Yb){sub x}TiO{sub 3}

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

Moraes, A. P. A.; Universidade Federal do Mato Grosso, 78060-900, Araguaia-MT; Filho, A. G. Souza

2011-06-15

The structural, dielectric, and vibrational properties of pure and rare earth (RE)-doped Ba{sub 0.77}Ca{sub 0.23}TiO{sub 3} (BCT23; RE = Nd, Sm, Pr, Yb) ceramics obtained via solid-state reaction were investigated. The pure and RE-doped BCT23 ceramics sintered at 1450 deg. C in air for 4 h showed a dense microstructure in all ceramics. The use of RE ions as dopants introduced lattice-parameter changes that manifested in the reduction of the volume of the unit cell. RE-doped BCT23 samples exhibit a more homogenous microstructure due to the absence of a Ti-rich phase in the grain boundaries as demonstrated by scanning electronmore » microscopy imaging. The incorporation of REs led to perturbations of the local symmetry of TiO{sub 6} octahedra and the creation of a new Raman mode. The results of Raman scattering measurements indicated that the Curie temperature of the ferroelectric phase transition depends on the RE ion and ion content, with the Curie temperature shifting toward lower values as the RE content increases, with the exception of Yb{sup 3+} doping, which did not affect the ferroelectric phase transition temperature. The phase transition behavior is explained using the standard soft mode model. Electronic paramagnetic resonance measurements showed the existence of Ti vacancies in the structure of RE-doped BCT23. Defects are created via charge compensation mechanisms due to the incorporation of elements with a different valence state relative to the ions of the pure BCT23 host. It is concluded that the Ti vacancies are responsible for the activation of the Raman mode at 840 cm{sup -1}, which is in agreement with lattice dynamics calculations.« less

Determination of imidacloprid, metalaxyl, myclobutanil, propham, and thiabendazole in fruits and vegetables by liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry.

PubMed

Pous, X; Ruíz, M J; Picó, Y; Font, G

2001-09-01

Imidacloprid, metalaxyl, myclobutanil, propham, and thiabendazole have been simultaneously determined in strawberries, oranges, potatoes, pears, and melons by matrix solid-phase dispersion (MSPD) followed by liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (LC-APCI-MS) in positive-ion mode. The samples were homogenized with C8 bonded silica as MSPD sorbent, placed in a glass column, and eluted with dichloromethane. Chromatographic separation of the compounds was achieved on a reversed-phase LC column using a methanol-ammonium formate (50 mmol L(-1)) gradient as a mobile phase. Samples were screened by monitoring the protonated molecular ion at m/z 256 for imidacloprid, 280 for metalaxyl, 289 for myclobutanil, and 202 for thiabendazole, and the main fragment at m/z 138 for propham. Positive samples were confirmed by multiple-ion monitoring. The repeatability (<20%) and recovery (>57%) of the method were good, and limits of detection (<0.05 mg kg(-1)) were adequate.

Solid-solid phase change thermal storage application to space-suit battery pack

NASA Astrophysics Data System (ADS)

Son, Chang H.; Morehouse, Jeffrey H.

1989-01-01

High cell temperatures are seen as the primary safety problem in the Li-BCX space battery. The exothermic heat from the chemical reactions could raise the temperature of the lithium electrode above the melting temperature. Also, high temperature causes the cell efficiency to decrease. Solid-solid phase-change materials were used as a thermal storage medium to lower this battery cell temperature by utilizing their phase-change (latent heat storage) characteristics. Solid-solid phase-change materials focused on in this study are neopentyl glycol and pentaglycerine. Because of their favorable phase-change characteristics, these materials appear appropriate for space-suit battery pack use. The results of testing various materials are reported as thermophysical property values, and the space-suit battery operating temperature is discussed in terms of these property results.

Inelastic neutron scattering spectrum of cyclotrimethylenetrinitramine: a comparison with solid-state electronic structure calculations.

PubMed

Ciezak, Jennifer A; Trevino, S F

2006-04-20

Solid-state geometry optimizations and corresponding normal-mode analysis of the widely used energetic material cyclotrimethylenetrinitramine (RDX) were performed using density functional theory with both the generalized gradient approximation (BLYP and BP functionals) and the local density approximation (PWC and VWN functionals). The structural results were found to be in good agreement with experimental neutron diffraction data and previously reported calculations based on the isolated-molecule approximation. The vibrational inelastic neutron scattering (INS) spectrum of polycrystalline RDX was measured and compared with simulated INS constructed from the solid-state calculations. The vibrational frequencies calculated from the solid-state methods had average deviations of 10 cm(-1) or less, whereas previously published frequencies based on an isolated-molecule approximation had deviations of 65 cm(-1) or less, illustrating the importance of including crystalline forces. On the basis of the calculations and analysis, it was possible to assign the normal modes and symmetries, which agree well with previous assignments. Four possible "doorway modes" were found in the energy range defined by the lattice modes, which were all found to contain fundamental contributions from rotation of the nitro groups.

Parameter study of dual-mode space nuclear fission solid core power and propulsion systems, NUROC3A. AMS report No. 1239c

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

Smith, W.W.; Layton, J.P.

1976-09-13

The three-volume report describes a dual-mode nuclear space power and propulsion system concept that employs an advanced solid-core nuclear fission reactor coupled via heat pipes to one of several electric power conversion systems. The NUROC3A systems analysis code was designed to provide the user with performance characteristics of the dual-mode system. Volume 3 describes utilization of the NUROC3A code to produce a detailed parameter study of the system.

Measuring the Nonuniform Evaporation Dynamics of Sprayed Sessile Microdroplets with Quantitative Phase Imaging.

PubMed

Edwards, Chris; Arbabi, Amir; Bhaduri, Basanta; Wang, Xiaozhen; Ganti, Raman; Yunker, Peter J; Yodh, Arjun G; Popescu, Gabriel; Goddard, Lynford L

2015-10-13

We demonstrate real-time quantitative phase imaging as a new optical approach for measuring the evaporation dynamics of sessile microdroplets. Quantitative phase images of various droplets were captured during evaporation. The images enabled us to generate time-resolved three-dimensional topographic profiles of droplet shape with nanometer accuracy and, without any assumptions about droplet geometry, to directly measure important physical parameters that characterize surface wetting processes. Specifically, the time-dependent variation of the droplet height, volume, contact radius, contact angle distribution along the droplet's perimeter, and mass flux density for two different surface preparations are reported. The studies clearly demonstrate three phases of evaporation reported previously: pinned, depinned, and drying modes; the studies also reveal instances of partial pinning. Finally, the apparatus is employed to investigate the cooperative evaporation of the sprayed droplets. We observe and explain the neighbor-induced reduction in evaporation rate, that is, as compared to predictions for isolated droplets. In the future, the new experimental methods should stimulate the exploration of colloidal particle dynamics on the gas-liquid-solid interface.

The stability and Raman spectra of ikaite, CaCO3·6H2O, at high pressure and temperature

USGS Publications Warehouse

Shahar, Anat; Bassett, William A.; Mao, Ho-kwang; Chou, I-Ming; Mao, Wendy

2005-01-01

Raman analyses of single crystals of ikaite, CaCO3·6H2O, synthesized in a diamond-anvil cell at ambient temperature yield spectra from 0.14 to 4.08 GPa; the most intense peaks are at 228 and 1081 cm−1 corresponding to Eg(external) and A1g (internal) modes of vibrations in CO2− 3 ions, respectively. These are in good agreement with Raman spectra previously published for ikaite in powder form at ambient temperature and pressure. Visual observations of a sample consisting initially of a mixture of calcite + water in a hydrothermal diamond-anvil cell yielded a P-T phase diagram up to 2 GPa and 120 °C; the boundary for the reaction ikaite ↔ aragonite + water has a positive slope and is curved convexly toward the aragonite + water field similar to typical melt curves. This curvature can be explained in terms of the Clapeyron equation for a boundary between a solid phase and a more compressible liquid phase or largely liquid phase assemblage.

Energy and Resource Saving of Steelmaking Process: Utilization of Innovative Multi-phase Flux During Dephosphorization Process

NASA Astrophysics Data System (ADS)

Matsuura, Hiroyuki; Hamano, Tasuku; Zhong, Ming; Gao, Xu; Yang, Xiao; Tsukihashi, Fumitaka

2014-09-01

An increase in the utilization efficiency of CaO, one of the major fluxing agents used in various steelmaking processes, is required to reduce the amount of discharged slag and energy consumption of the process. The authors have intensively focused on the development of innovative dephosphorization process by using so called "multi-phase flux" composed of solid and liquid phases. This article summarizes the research on the above topic done by the authors, in which the formation mechanisms of P2O5-containing phase during CaO or 2CaO·SiO2 dissolution into molten slag, the phase relationship between solid and liquid phases at equilibrium, and thermodynamic properties of P2O5-containing phase have been clarified. The reactions between solid CaO or 2CaO·SiO2 and molten CaO-FeO x -SiO2-P2O5 slag were observed by dipping solid specimen in the synthesized slag at 1573 K or 1673 K. The formation of the CaO-FeO layer and dual-phase layer of solid 2CaO·SiO2 and FeO x -rich liquid phase was observed around the interface from the solid CaO side toward the bulk slag phase side. Condensation of P2O5 into 2CaO·SiO2 phase as 2CaO·SiO2-3CaO·P2O5 solid solution was observed in both cases of CaO and 2CaO·SiO2 as solid specimens. Measurement of the phase relationship for the CaO-FeO x -SiO2-P2O5 system confirmed the condensation of P2O5 in solid phase at low oxygen partial pressure. The thermodynamics of 2CaO·SiO2-3CaO·P2O5 solid solution are to be clarified to quantitatively simulate the dephosphorization process, and the current results are also introduced. Based on the above results, the reduction of CaO consumption, the discharged slag curtailment, and energy-saving effects have been discussed.

Surface instability of a thin electrolyte film undergoing coupled electroosmotic and electrophoretic flows in a microfluidic channel.

PubMed

Ray, Bahni; Reddy, Puchalapalli Dinesh Sankar; Bandyopadhyay, Dipankar; Joo, Sang W; Sharma, Ashutosh; Qian, Shizhi; Biswas, Gautam

2011-11-01

We consider the stability of a thin liquid film with a free charged surface resting on a solid charged substrate by performing a general Orr-Sommerfeld (O-S) analysis complemented by a long-wave (LW) analysis. An externally applied field generates an electroosmotic flow (EOF) near the solid substrate and an electrophoretic flow (EPF) at the free surface. The EPF retards the EOF when both the surfaces have the same sign of the potential and can even lead to the flow reversal in a part of the film. In conjunction with the hydrodynamic stress, the Maxwell stress is also considered in the problem formulation. The electrokinetic potential at the liquid-air and solid-liquid interfaces is modelled by the Poisson-Boltzmann equation with the Debye-Hückel approximation. The O-S analysis shows a finite-wavenumber shear mode of instability when the inertial forces are strong and an LW interfacial mode of instability in the regime where the viscous force dominates. Interestingly, both the modes are found to form beyond a critical flow rate. The shear (interfacial) mode is found to be dominant when the film is thick (thin), the electric field applied is strong (weak), and the zeta-potentials on the liquid-air and solid-liquid interfaces are high (small). The LW analysis predicts the presence of the interfacial mode, but fails to capture the shear mode. The change in the propagation direction of the interfacial mode with the zeta-potential is predicted by both O-S and LW analyses. The parametric range in which the LW analysis is valid is thus demonstrated. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Helicon waves in uniform plasmas. II. High m numbers

NASA Astrophysics Data System (ADS)

Stenzel, R. L.; Urrutia, J. M.

2015-09-01

Helicons are whistler modes with azimuthal wave numbers. They have been studied in solids and plasmas where boundaries play a role. The present work shows that very similar modes exist in unbounded gaseous plasmas. Instead of boundaries, the antenna properties determine the topology of the wave packets. The simplest antenna is a magnetic loop which excites m = 0 or m = 1 helicons depending on whether the dipole moment is aligned parallel or perpendicular to the ambient background magnetic field B0. While these low order helicons have been described by J. M. Urrutia and R. L. Stenzel ["Helicon modes in uniform plasmas. I. Low m modes," Phys. Plasmas 22, 092111 (2015)], the present work focuses on high order modes up to m = 8. These are excited by antenna arrays forming magnetic multipoles. Their wave magnetic field has been measured in space and time in a large and uniform laboratory plasma free of boundary effects. The observed wave topology exhibits m pairs of unique field line spirals which may have inspired the name "helicon" to this mode. All field lines converge into these nested spirals which propagate like corkscrews along B0. The field lines near the axis of helicons are perpendicular to B0 and circularly polarized as in parallel whistlers. Helical antennas couple to these transverse fields but not to the spiral fields of helicons. Using a circular antenna array of phased m = 0 loops, right or left rotating or non-rotating multipole antenna fields are generated. They excite m < 0 and m > 0 modes, showing that the plasma supports both modes equally well. The poor excitation of m < 0 modes is a characteristic of loops with dipole moment across B0. The radiation efficiency of multipole antennas has been found to decrease with m.

Crystallization process

DOEpatents

Adler, Robert J.; Brown, William R.; Auyang, Lun; Liu, Yin-Chang; Cook, W. Jeffrey

1986-01-01

An improved crystallization process is disclosed for separating a crystallizable material and an excluded material which is at least partially excluded from the solid phase of the crystallizable material obtained upon freezing a liquid phase of the materials. The solid phase is more dense than the liquid phase, and it is separated therefrom by relative movement with the formation of a packed bed of solid phase. The packed bed is continuously formed adjacent its lower end and passed from the liquid phase into a countercurrent flow of backwash liquid. The packed bed extends through the level of the backwash liquid to provide a drained bed of solid phase adjacent its upper end which is melted by a condensing vapor.

PLZT block data composers operated in differential phase mode. [lanthanum-modified lead zirconate titanate ceramic device for digital holographic memory

NASA Technical Reports Server (NTRS)

Drake, M. D.; Klingler, D. E.

1973-01-01

The use of PLZT ceramics with the 7/65/35 composition in block data composer (BDC) input devices for holographic memory systems has previously been described for operation in the strain biased, scattering, and edge effect modes. A new and promising mode of BDC operation is the differential phase mode in which each element of a matrix array BDC acts as a phase modulator. The phase modulation results from a phase difference in the optical path length between the electrically poled and depoled states of the PLZT. It is shown that a PLZT BDC can be used as a matrix-type phase modulator to record and process digital data by the differential phase mode in a holographic recording/processing system with readout contrast ratios of between 10:1 and 15:1. The differential phase mode has the advantages that strain bias is not required and that the thickness and strain variations in the PLZT are cancelled out.

The nature and pollutant role of solids at the water-sediment interface in combined sewer networks.

PubMed

Chebbo, G; Ashley, R; Gromaire, M C

2003-01-01

Solids at the water-sediment interface in combined sewers are known to be important for pollution potential during storm washout via CSOs. They have been investigated in several studies, but nonetheless, little is known about the origins, build-up, transport and nature of these solids. From a review of current knowledge it is apparent that whilst there is general agreement that these solids are largely organic and have high polluting potential, their modes of transport and definition are not generally agreed upon. It is possible that there may be several "types" of these solids, defined as either: "near bed solids" or "fluid sediments/dense undercurrents", possibly representing transport modes in flows with different ranges of ambient (dry weather) velocities and with differing sewerage layouts. Current knowledge is presented and new ideas for resolving the uncertainties regarding the nature, movement and effects of this material are outlined.

Determination of human pharmaceuticals in pre- and post-sewage treatment

NASA Astrophysics Data System (ADS)

Tahrim, Nurfaizah Abu; Abdullah, Md. Pauzi; Aziz, Yang Farina Abdul

2013-11-01

In this present work, an analytical method based on solid phase extraction (SPE) followed by liquid chromatography-time-of-flight mass spectrometry (LC-TOF-MS) in positive electrospray ionisation mode was successfully applied to real samples for the determination of human pharmaceuticals in pre- and post-sewage treatment samples. The ten target compounds selected in this study include acetaminophen, theophylline, caffeine, metoprolol, sulfamethoxazole, carbamazepine, prednisolone, ketoprofen, norgestrel and simvastatin. Acetaminophen, theophylline and caffeine were present at all five raw sewage samples. In addition, this work provides the first report on the investigation and detection of theophylline in sewage treatment plant (STP) samples in Malaysia.

Fiber laser cleaning of metal mirror surfaces for optical diagnostic systems of the ITER

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

Kuznetsov, A. P., E-mail: APKuznetsov@mephi.ru; Alexandrova, A. S.; Buzhinsky, O. I.

2015-12-15

The results of experimental studies into efficiency of removal of films with a complex composition from metal mirrors by pulsed fiber laser irradiation are presented. It is shown that the initial reflectivity of optical elements can be restored by the selection of modes of irradiation impacting the surface with the sputtered film. Effective cleaning is performed by radiation with a power density lower than 10{sup 7} W/cm{sup 2}. The removal of contaminations at such a relatively low power density occurs in a solid phase, owing to which the thermal effect on the mirror is insignificant.

Experimental investigation of particle surface interactions for turbomachinery application

NASA Astrophysics Data System (ADS)

Hamed, A.; Tabakoff, W.

This paper describes an experimental investigation to determine the particle restitution characteristics after impacting solid targets in a particulate flow wind tunnel. The tests simulate the two phase flow conditions encountered in turbomachinery operating in particle laden flow environments. Both incoming and rebounding velocities are measured using a three color Argon Ion laser in backward scattered mode through a window in the tunnel section containing the impact target. The experimental results are presented for ash particles impinging on RENE 41 targets at different impact conditions. The presented results are applicable to particle dynamics simulations in gas turbine engines and to the prediction of the associated blade surface erosion.

Dramatically different kinetics and mechanism at solid/liquid and solid/gas interfaces for catalytic isopropanol oxidation over size-controlled platinum nanoparticles.

PubMed

Wang, Hailiang; Sapi, Andras; Thompson, Christopher M; Liu, Fudong; Zherebetskyy, Danylo; Krier, James M; Carl, Lindsay M; Cai, Xiaojun; Wang, Lin-Wang; Somorjai, Gabor A

2014-07-23

We synthesize platinum nanoparticles with controlled average sizes of 2, 4, 6, and 8 nm and use them as model catalysts to study isopropanol oxidation to acetone in both the liquid and gas phases at 60 °C. The reaction at the solid/liquid interface is 2 orders of magnitude slower than that at the solid/gas interface, while catalytic activity increases with the size of platinum nanoparticles for both the liquid-phase and gas-phase reactions. The activation energy of the gas-phase reaction decreases with the platinum nanoparticle size and is in general much higher than that of the liquid-phase reaction which is largely insensitive to the size of catalyst nanoparticles. Water substantially promotes isopropanol oxidation in the liquid phase. However, it inhibits the reaction in the gas phase. The kinetic results suggest different mechanisms between the liquid-phase and gas-phase reactions, correlating well with different orientations of IPA species at the solid/liquid interface vs the solid/gas interface as probed by sum frequency generation vibrational spectroscopy under reaction conditions and simulated by computational calculations.

Solidification and solid-state transformation sciences in metals additive manufacturing

DOE PAGES

Kirka, Michael M.; Nandwana, Peeyush; Lee, Yousub; ...

2017-02-11

Additive manufacturing (AM) of metals is rapidly emerging as an established manufacturing process for metal components. Unlike traditional metals fabrication processes, metals fabricated via AM undergo localized thermal cycles during fabrication. As a result, AM presents the opportunity to control the liquid-solid phase transformation, i.e. material texture. But, thermal cycling presents challenges from the standpoint of solid-solid phase transformations. We will discuss the opportunities and challenges in metals AM in the context of texture control and associated solid-solid phase transformations in Ti-6Al-4V and Inconel 718.

Microwave spectroscopic observation of distinct electron solid phases in wide quantum wells

NASA Astrophysics Data System (ADS)

Hatke, A. T.; Liu, Yang; Magill, B. A.; Moon, B. H.; Engel, L. W.; Shayegan, M.; Pfeiffer, L. N.; West, K. W.; Baldwin, K. W.

2014-06-01

In high magnetic fields, two-dimensional electron systems can form a number of phases in which interelectron repulsion plays the central role, since the kinetic energy is frozen out by Landau quantization. These phases include the well-known liquids of the fractional quantum Hall effect, as well as solid phases with broken spatial symmetry and crystalline order. Solids can occur at the low Landau-filling termination of the fractional quantum Hall effect series but also within integer quantum Hall effects. Here we present microwave spectroscopy studies of wide quantum wells that clearly reveal two distinct solid phases, hidden within what in d.c. transport would be the zero diagonal conductivity of an integer quantum-Hall-effect state. Explanation of these solids is not possible with the simple picture of a Wigner solid of ordinary (quasi) electrons or holes.

Extinguishment of a Diffusion Flame Over a PMMA Cylinder by Depressurization in Reduced-Gravity

NASA Technical Reports Server (NTRS)

Goldmeer, Jeffrey Scott

1996-01-01

Extinction of a diffusion flame burning over horizontal PMMA (Polymethyl methacrylate) cylinders in low-gravity was examined experimentally and via numerical simulations. Low-gravity conditions were obtained using the NASA Lewis Research Center's reduced-gravity aircraft. The effects of velocity and pressure on the visible flame were examined. The flammability of the burning solid was examined as a function of pressure and the solid-phase centerline temperature. As the solid temperature increased, the extinction pressure decreased, and with a centerline temperature of 525 K, the flame was sustained to 0.1 atmospheres before extinguishing. The numerical simulation iteratively coupled a two-dimensional quasi-steady, gas-phase model with a transient solid-phase model which included conductive heat transfer and surface regression. This model employed an energy balance at the gas/solid interface that included the energy conducted by the gas-phase to the gas/solid interface, Arrhenius pyrolysis kinetics, surface radiation, and the energy conducted into the solid. The ratio of the solid and gas-phase conductive fluxes Phi was a boundary condition for the gas-phase model at the solid-surface. Initial simulations modeled conditions similar to the low-gravity experiments and predicted low-pressure extinction limits consistent with the experimental limits. Other simulations examined the effects of velocity, depressurization rate and Phi on extinction.

Characterization of the leachate in an urban landfill by physicochemical analysis and solid phase microextraction-GC/MS.

PubMed

Banar, Müfide; Ozkan, Aysun; Kürkçüoğlu, Mine

2006-10-01

The aim of this study is to evaluate extensively the characterization and identification of major pollutant parameters by paying attention to the organic chemical pollution for unregulated dumping site leachate in Eskişehir/Turkey. The study that is first and only one research has been very important data related with before new sanitary landfill site in Eskişehir city. For this purpose, in this study leachate samples were collected in-situ at monthly interval for a period of 8 months. Firstly, thirty three physicochemical parameters were monitored. Secondly, SPME technique was used for identification of organic pollutants. Meteorological data were also recorded for the same sampling period to correlate meteorological data and physicochemical parameters. Mean values are used in the correlation analysis. Correlation is shown only for the relationship between air temperature and NO(3) (-). No correlation has been found between rain and leachate quality parameters since the amount of rain was very low during the sampling period. However, analysis results were generally decreased in winter season when each parameter and each sampling point are examined separately. According to correlation between every parameter, especially solid content and dissolved oxygen concentration of leachate is affecting to other parameters. Also, sodium and potassium are changing proportionally with same parameters (suspended solids, fixed solids, dissolved oxygen) and high correlation between chloride and heavy metal concentration is showing. The results were statistically evaluated by use of SPSS 10.0 program. Second part of the study, the leachate was extracted by Solid Phase Microextraction (SPME) technique and then analyzed. Of the methodologies tested in this study, the best one selected was based on 100 micro m polydimethylsiloxane coated fiber (PDMS), headspace with heating (Delta HS) sampling mode and an extraction time of 15 min. at a temperature of 50 degrees C. Thirty three organic compounds in leachate were identified by GC/MS.

SOLID-LIQUID PHASE TRANSFER CATALYZED SYNTHESIS OF CINNAMYL ACETATE-KINETICS AND ANALYSIS OF FACTORS AFFECTING THE REACTION IN A BATCH REACTOR

EPA Science Inventory

The use of solid-liquid phase transfer catalysis has an advantage of carrying out reaction between two immiscible substrates, one in solid phase and the other in liquid phase, with high selectivity and at relatively low temperatures. In this study we investigated the synthesis ci...

Far infrared spectra of solid state aliphatic amino acids in different protonation states

NASA Astrophysics Data System (ADS)

Trivella, Aurélien; Gaillard, Thomas; Stote, Roland H.; Hellwig, Petra

2010-03-01

Far infrared spectra of zwitterionic, cationic, and anionic forms of aliphatic amino acids in solid state have been studied experimentally. Measurements were done on glycine, L-alanine, L-valine, L-leucine, and L-isoleucine powder samples and film samples obtained from dried solutions prepared at pH ranging from 1 to 13. Solid state density functional theory calculations were also performed, and detailed potential energy distributions were obtained from normal mode results. A good correspondence between experimental and simulated spectra was achieved and this allowed us to propose an almost complete band assignment for the far infrared spectra of zwitterionic forms. In the 700-50 cm-1 range, three regions were identified, each corresponding to a characteristic set of normal modes. A first region between 700 and 450 cm-1 mainly contained the carboxylate bending, rocking, and wagging modes as well as the ammonium torsional mode. The 450-250 cm-1 region was representative of backbone and sidechain skeletal bending modes. At last, the low wavenumber zone, below 250 cm-1, was characteristic of carboxylate and skeletal torsional modes and of lattice modes. Assignments are also proposed for glycine cationic and anionic forms, but could not be obtained for all aliphatic amino acids due to the lack of structural data. This work is intended to provide fundamental information for the understanding of peptides vibrational properties.

Correlation among far-infrared reflection modes, crystal structures and dielectric properties of Ba(Zn{sub 1/3}Nb{sub 2/3})O{sub 3}–CaTiO{sub 3} ceramics

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

Shi, Feng, E-mail: sf751106@sina.com.cn; Sun, Haiqing; Liu, Hongquan

Highlights: • Crystal symmetry decreases with CT concentration from cubic to hexagonal structure. • Lattice constants as well as the ordered degree change with CT concentration. • Ordered structures turn from 1:1 to 1:2 ordering with change of crystal structures. • There is a correlation between FIR phonon modes and dielectric properties. • There is a correlation between FIR phonon modes and crystal structures. - Abstract: Ba(Zn{sub 1/3}Nb{sub 2/3})O{sub 3} (BZN)–CaTiO{sub 3} (CT) microwave dielectric ceramics were synthesized at 1395 °C for 4 h using conventional solid-state sintering technique with different CT contents. The ceramics were characterized by X-ray diffractionmore » (XRD) and far-infrared reflection (FIR) spectroscopy to evaluate correlations among crystal structures, dielectric properties, and infrared modes. XRD results showed that crystal symmetry decreased with increased CT concentration from cubic to hexagonal structure, and lattice constants and ordered degree changed accordingly. Ordered phases transformed from 1:1 to 1:2 ordered structure with crystal-structure change. FIR results demonstrated that two new IR active modes appeared at 300 cm{sup −1}, and another new mode appeared at 600 cm{sup −1} for the x ≥ 0.60 sample, which agreed with the change in crystal structures as confirmed by XRD results. Correlations between FIR modes and dielectric properties were established.« less

Numerical modelling of biomass combustion: Solid conversion processes in a fixed bed furnace

NASA Astrophysics Data System (ADS)

Karim, Md. Rezwanul; Naser, Jamal

2017-06-01

Increasing demand for energy and rising concerns over global warming has urged the use of renewable energy sources to carry a sustainable development of the world. Bio mass is a renewable energy which has become an important fuel to produce thermal energy or electricity. It is an eco-friendly source of energy as it reduces carbon dioxide emissions. Combustion of solid biomass is a complex phenomenon due to its large varieties and physical structures. Among various systems, fixed bed combustion is the most commonly used technique for thermal conversion of solid biomass. But inadequate knowledge on complex solid conversion processes has limited the development of such combustion system. Numerical modelling of this combustion system has some advantages over experimental analysis. Many important system parameters (e.g. temperature, density, solid fraction) can be estimated inside the entire domain under different working conditions. In this work, a complete numerical model is used for solid conversion processes of biomass combustion in a fixed bed furnace. The combustion system is divided in to solid and gas phase. This model includes several sub models to characterize the solid phase of the combustion with several variables. User defined subroutines are used to introduce solid phase variables in commercial CFD code. Gas phase of combustion is resolved using built-in module of CFD code. Heat transfer model is modified to predict the temperature of solid and gas phases with special radiation heat transfer solution for considering the high absorptivity of the medium. Considering all solid conversion processes the solid phase variables are evaluated. Results obtained are discussed with reference from an experimental burner.

Theory of amorphous ices.

PubMed

Limmer, David T; Chandler, David

2014-07-01

We derive a phase diagram for amorphous solids and liquid supercooled water and explain why the amorphous solids of water exist in several different forms. Application of large-deviation theory allows us to prepare such phases in computer simulations. Along with nonequilibrium transitions between the ergodic liquid and two distinct amorphous solids, we establish coexistence between these two amorphous solids. The phase diagram we predict includes a nonequilibrium triple point where two amorphous phases and the liquid coexist. Whereas the amorphous solids are long-lived and slowly aging glasses, their melting can lead quickly to the formation of crystalline ice. Further, melting of the higher density amorphous solid at low pressures takes place in steps, transitioning to the lower-density glass before accessing a nonequilibrium liquid from which ice coarsens.

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

Kirka, Michael M.; Nandwana, Peeyush; Lee, Yousub

Additive manufacturing (AM) of metals is rapidly emerging as an established manufacturing process for metal components. Unlike traditional metals fabrication processes, metals fabricated via AM undergo localized thermal cycles during fabrication. As a result, AM presents the opportunity to control the liquid-solid phase transformation, i.e. material texture. But, thermal cycling presents challenges from the standpoint of solid-solid phase transformations. We will discuss the opportunities and challenges in metals AM in the context of texture control and associated solid-solid phase transformations in Ti-6Al-4V and Inconel 718.

Coupled-mode analysis of gain and wavelength oscillation characteristics of diode laser phased arrays

NASA Technical Reports Server (NTRS)

Butler, J. K.; Ettenberg, M.; Ackley, D. E.

1985-01-01

The lasing wavelengths and gain characteristics of the modes of phase-locked arrays of channel-substrate-planar (CSP) lasers are presented. The gain values for the array modes are determined from complex coupling coefficients calculated using the fields of neighboring elements of the array. The computations show that, for index guided lasers which have nearly planar phase fronts, the highest order array mode will be preferred. The 'in-phase' or fundamental mode, which produces only one major lobe in the far-field radiation pattern, has the lowest modal gain of all array modes. The modal gain differential between the highest order and fundamental modes is less than 10/cm for weak coupling between the elements.

Phase relations in the system NaCl-KCl-H2O: V. Thermodynamic-PTX analysis of solid-liquid equilibria at high temperatures and pressures

USGS Publications Warehouse

Sterner, S.M.; Chou, I.-Ming; Downs, R.T.; Pitzer, Kenneth S.

1992-01-01

The Gibbs energies of mixing for NaCl-KCl binary solids and liquids and solid-saturated NaCl-KCl-H2O ternary liquids were modeled using asymmetric Margules treatments. The coefficients of the expressions were calibrated using an extensive array of binary solvus and solidus data, and both binary and ternary liquidus data. Over the PTX range considered, the system exhibits complete liquid miscibility among all three components and extensive solid solution along the anhydrous binary. Solid-liquid and solid-solid phase equilibria were calculated by using the resulting equations and invoking the equality of chemical potentials of NaCl and KCl between appropriate phases at equilibrium. The equations reproduce the ternary liquidus and predict activity coefficients for NaCl and KCl components in the aqueous liquid under solid-saturation conditions between 673 and 1200 K from vapor saturation up to 5 kbar. In the NaCl-KCl anhydrous binary system, the equations describe phase equilibria and predict activity coefficients of the salt components for all stable compositions of solid and liquid phases between room temperature and 1200 K and from 1 bar to 5 kbar. ?? 1992.

Phase diagram of two-dimensional hard ellipses.

PubMed

Bautista-Carbajal, Gustavo; Odriozola, Gerardo

2014-05-28

We report the phase diagram of two-dimensional hard ellipses as obtained from replica exchange Monte Carlo simulations. The replica exchange is implemented by expanding the isobaric ensemble in pressure. The phase diagram shows four regions: isotropic, nematic, plastic, and solid (letting aside the hexatic phase at the isotropic-plastic two-step transition [E. P. Bernard and W. Krauth, Phys. Rev. Lett. 107, 155704 (2011)]). At low anisotropies, the isotropic fluid turns into a plastic phase which in turn yields a solid for increasing pressure (area fraction). Intermediate anisotropies lead to a single first order transition (isotropic-solid). Finally, large anisotropies yield an isotropic-nematic transition at low pressures and a high-pressure nematic-solid transition. We obtain continuous isotropic-nematic transitions. For the transitions involving quasi-long-range positional ordering, i.e., isotropic-plastic, isotropic-solid, and nematic-solid, we observe bimodal probability density functions. This supports first order transition scenarios.

Binary Solid-Liquid Phase Diagram of Phenol and t-Butanol: An Undergraduate Physical Chemistry Experiment

ERIC Educational Resources Information Center

Xu, Xinhua; Wang, Xiaogang; Wu, Meifen

2014-01-01

The determination of the solid-liquid phase diagram of a binary system is always used as an experiment in the undergraduate physical chemistry laboratory courses. However, most phase diagrams investigated in the lab are simple eutectic ones, despite the fact that complex binary solid-liquid phase diagrams are more common. In this article, the…

Phase transitions of amorphous solid acetone in confined geometry investigated by reflection absorption infrared spectroscopy.

PubMed

Shin, Sunghwan; Kang, Hani; Kim, Jun Soo; Kang, Heon

2014-11-26

We investigated the phase transformations of amorphous solid acetone under confined geometry by preparing acetone films trapped in amorphous solid water (ASW) or CCl4. Reflection absorption infrared spectroscopy (RAIRS) and temperature-programmed desorption (TPD) were used to monitor the phase changes of the acetone sample with increasing temperature. An acetone film trapped in ASW shows an abrupt change in the RAIRS features of the acetone vibrational bands during heating from 80 to 100 K, which indicates the transformation of amorphous solid acetone to a molecularly aligned crystalline phase. Further heating of the sample to 140 K produces an isotropic solid phase, and eventually a fluid phase near 157 K, at which the acetone sample is probably trapped in a pressurized, superheated condition inside the ASW matrix. Inside a CCl4 matrix, amorphous solid acetone crystallizes into a different, isotropic structure at ca. 90 K. We propose that the molecularly aligned crystalline phase formed in ASW is created by heterogeneous nucleation at the acetone-water interface, with resultant crystal growth, whereas the isotropic crystalline phase in CCl4 is formed by homogeneous crystal growth starting from the bulk region of the acetone sample.

"Crypto-Display" in Dual-Mode Metasurfaces by Simultaneous Control of Phase and Spectral Responses.

PubMed

Yoon, Gwanho; Lee, Dasol; Nam, Ki Tae; Rho, Junsuk

2018-06-26

Although conventional metasurfaces have demonstrated many promising functionalities in light control by tailoring either phase or spectral responses of subwavelength structures, simultaneous control of both responses has not been explored yet. Here, we propose a concept of dual-mode metasurfaces that enables simultaneous control of phase and spectral responses for two kinds of operation modes of transmission and reflection, respectively. In the transmission mode, the dual-mode metasurface acts as conventional metasurfaces by tailoring phase distribution of incident light. In the reflection mode, a reflected colored image is produced under white light illumination. We also experimentally demonstrate a crypto-display as one application of the dual-mode metasurface. The crypto-display looks a normal reflective display under white light illumination but generates a hologram that reveals the encrypted phase information under single-wavelength coherent light illumination. Because two operation modes do not affect each other, the crypto-display can have applications in security techniques.

Generation of high-order Hermite-Gaussian modes in end-pumped solid-state lasers for square vortex array laser beam generation.

PubMed

Chu, Shu-Chun; Chen, Yun-Ting; Tsai, Ko-Fan; Otsuka, Kenju

2012-03-26

This study reports the first systematic approach to the excitation of all high-order Hermite-Gaussian modes (HGMs) in end-pumped solid-state lasers. This study uses a metal-wire-inserted laser resonator accompanied with the "off axis pumping" approach. This study presents numerical analysis of the excitation of HGMs in end-pumped solid-state lasers and experimentally generated HGM patterns. This study also experimentally demonstrates the generation of an square vortex array laser beams by passing specific high-order HGMs (HGn,n + 1 or HGn + 1,n modes) through a Dove prism-embedded unbalanced Mach-Zehnder interferometer [Optics Express 16, 19934-19949]. The resulting square vortex array laser beams with embedded vortexes aligned in a square array can be applied to multi-spot dark optical traps in the future.

Negative refraction of elastic waves at the deep-subwavelength scale in a single-phase metamaterial.

PubMed

Zhu, R; Liu, X N; Hu, G K; Sun, C T; Huang, G L

2014-11-24

Negative refraction of elastic waves has been studied and experimentally demonstrated in three- and two-dimensional phononic crystals, but Bragg scattering is impractical for low-frequency wave control because of the need to scale the structures to manageable sizes. Here we present an elastic metamaterial with chiral microstructure made of a single-phase solid material that aims to achieve subwavelength negative refraction of elastic waves. Both negative effective mass density and modulus are observed owing to simultaneous translational and rotational resonances. We experimentally demonstrate negative refraction of the longitudinal elastic wave at the deep-subwavelength scale in the metamaterial fabricated in a stainless steel plate. The experimental measurements are in good agreement with numerical simulations. Moreover, wave mode conversion related with negative refraction is revealed and discussed. The proposed elastic metamaterial may thus be used as a flat lens for elastic wave focusing.

Determination of chlorinated acid herbicides in vegetation and soil by liquid chromatography/electrospray-tandem mass spectrometry.

PubMed

Schaner, Angela; Konecny, Jaclyn; Luckey, Laura; Hickes, Heidi

2007-01-01

The method presented uses reversed-phase liquid chromatography with negative electrospray ionization and tandem mass spectrometry to analyze 9 chlorinated acid herbicides in soil and vegetation matrixes: clopyralid, dicamba, MCPP, MCPA, 2,4-DP, 2,4-D, triclopyr, 2,4-DB, and picloram. A 20 g portion is extracted with a basic solution and an aliquot acidified and micropartitioned with 3 mL chloroform. Vegetation samples are subjected to an additional cleanup with a mixed-mode anion exchange solid-phase extraction cartridge. Two precursor product ion transitions per analyte are measured and evaluated to provide the maximum degree of confidence in results. Average recoveries for 3 different soil types tested ranged from 72 to 107% for all compounds with the exception of 2,4-DB at 56-99%. Average recoveries for the 3 different vegetation types studied were lower and ranged from 53 to 80% for all compounds.

Numerical simulation of electron beam welding with beam oscillations

NASA Astrophysics Data System (ADS)

Trushnikov, D. N.; Permyakov, G. L.

2017-02-01

This research examines the process of electron-beam welding in a keyhole mode with the use of beam oscillations. We study the impact of various beam oscillations and their parameters on the shape of the keyhole, the flow of heat and mass transfer processes and weld parameters to develop methodological recommendations. A numerical three-dimensional mathematical model of electron beam welding is presented. The model was developed on the basis of a heat conduction equation and a Navier-Stokes equation taking into account phase transitions at the interface of a solid and liquid phase and thermocapillary convection (Marangoni effect). The shape of the keyhole is determined based on experimental data on the parameters of the secondary signal by using the method of a synchronous accumulation. Calculations of thermal and hydrodynamic processes were carried out based on a computer cluster, using a simulation package COMSOL Multiphysics.

A Study of Oxides for Solid Oxide Cells

NASA Astrophysics Data System (ADS)

Comets, Olivier

As the world energy consumption increases, it is a question of global health to increase energy production efficiency and to reduce CO2 emissions. In that respect, solid oxide cells are solid state devices that convert directly fuel into electricity, or vice versa. In fact, when run in fuel cell mode, such devices produce electricity with efficiency up to twice that of current natural gas power plants. However, systems equipped with them have only seen limited commercialization owing to issues of cost, durability, and performance. In this thesis, three different aspects of solid oxide cells are studied. First, the effects of stress on the properties of mixed ionic electronic conducting oxides are considered. Such oxides can be used as electrode materials, where they are often subject to large stresses, which can, in turn, affect their performance. Hence, understanding the relationship between stress and properties in such materials is crucial. Non-stoichiometry in strontium substituted lanthanum cobaltite is found to increase under tension and to decrease under compression. Then, degradation taking place when the cell is run in electrolysis mode is discussed. A high current allows for a high production rate of hydrogen gas. However, this can also lead to oxygen bubble nucleating in the electrolyte and subsequent degradation of the cell. The analysis conducted here shows that such nucleation phenomenon can be avoided by keeping the overpotential at the oxygen electrode below a critical value. Finally, the growth and coarsening of catalyst nanoparticles at the surface of an oxide is studied. Scientists have developed new oxides for anodes in which a catalyst material is dissolved and exsolves under operating conditions. As the performance of the cell is controlled by the surface area of the catalyst phase, understanding the kinetics of the growth is critical to predict the performance of the cell. An approach is developed to study the growth of one particle, in the limiting case where only bulk transport is allowed.

Experimental research on the stability and the multilongitudinal mode interference of bidirectional outputs of LD-pumped solid state ring laser

NASA Astrophysics Data System (ADS)

Wan, Shunping; Tian, Qian; Sun, Liqun; Yao, Minyan; Mao, Xianhui; Qiu, Hongyun

2004-05-01

This paper reports an experimental research on the stability of bidirectional outputs and multi-longitudinal mode interference of laser diode end-pumped Nd:YVO4 solid-state ring laser (DPSSL). The bidirectional, multi-longitudinal and TEM00 mode continuous wave outputs are obtained and the output powers are measured and their stabilities are analyzed respectively. The spectral characteristic of the outputs is measured. The interfering pattern of the bidirectional longitudinal mode outputs is obtained and analyzed in the condition of the ring cavity with rotation velocity. The movement of the interfering fringe of the multi-longitudinal modes is very sensitive to the deformation of the setup base and the fluctuation of the intracavity air, but is stationary or randomly dithers when the stage is rotating.

Femtosecond solid-state laser based on a few-layered black phosphorus saturable absorber.

PubMed

Su, Xiancui; Wang, Yiran; Zhang, Baitao; Zhao, Ruwei; Yang, Kejian; He, Jingliang; Hu, Qiangqiang; Jia, Zhitai; Tao, Xutang

2016-05-01

In this Letter, a high-quality, few-layered black phosphorus (BP) saturable absorber (SA) was fabricated successfully, and a femtosecond solid-state laser modulated by BP-SA was experimentally demonstrated for the first time, to the best of our knowledge. Pulses as short as 272 fs were achieved with an average output power of 0.82 W, corresponding to the pulse energy of 6.48 nJ and peak power of 23.8 MW. So far, these represent the shortest pulse duration and highest output power ever obtained with a BP-based mode-locked solid-state laser. The results indicate the promising potential of few-layered BP-SA for applications in solid-state femtosecond mode-locked lasers.

Direct-write liquid phase transformations with a scanning transmission electron microscope

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

Unocic, Raymond R.; Lupini, Andrew R.; Borisevich, Albina Y.

The highly energetic electron beam from a scanning transmission electron microscope (STEM) can induce local changes in the state of matter, ranging from local knock-out and atomic movement, to amorphization/crystallization, and chemical/electrochemical reactions occuring at localized liquid-solid and gas-solid interfaces. To date, fundamental studies of e-beam induced phenomena and practical applications have been limited by conventional e-beam rastering modes that allow only for uniform e-beam exposures. Here we develop an automated liquid phase nanolithography method that is capable of directly writing nanometer scaled features within silicon nitride encapsulated liquid cells. An external beam control system, connected to the scan coilsmore » of an aberration-corrected STEM, is used to precisely control the position, dwell time, and scan velocity of a sub-nanometer STEM probe. Site-specific locations in a sealed liquid cell containing an aqueous solution of H 2PdCl 4 are irradiated to controllably deposit palladium onto silicon nitride membranes. We determine the threshold electron dose required for the radiolytic deposition of metallic palladium, explore the influence of electron dose on the feature size and morphology of nanolithographically patterned nanostructures, and propose a feedback-controlled monitoring method for active control of the nanofabricated structures through STEM detector signal monitoring. As a result, this approach enables both fundamental studies of electron beam induced interactions with matter, as well as opens a pathway to fabricate nanostructures with tailored architectures and chemistries via shape-controlled nanolithographic patterning from liquid phase precursors.« less

A simple assay for the simultaneous determination of human plasma albendazole and albendazole sulfoxide levels by high performance liquid chromatography in tandem mass spectrometry with solid-phase extraction.

PubMed

Wojnicz, Aneta; Cabaleiro-Ocampo, Teresa; Román-Martínez, Manuel; Ochoa-Mazarro, Dolores; Abad-Santos, Francisco; Ruiz-Nuño, Ana

2013-11-15

A simple, reproducible and fast (4 min chromatogram) method of liquid chromatography in tandem with mass spectrometry (LC/MS-MS) was developed to determine simultaneously the plasma levels of albendazole (ABZ) and its metabolite albendazole sulfoxide (ABZOX) for pharmacokinetic and clinical analysis. Each plasma sample was extracted by solid phase extraction (SPE) using phenacetin as internal standard (IS). The extracted sample was eluted with a Zorbax XDB-CN column using an isocratic method. The mobile phase consisting of water with 1% acetic acid (40%, A) and MeOH (60%, B), was used at a flow rate of 1 mL/min. ABZ and ABZOX were detected and identified by mass spectrometry with electrospray ionization (ESI) in the positive ion and multiple-reaction monitoring (MRM) mode. The method was linear in the range of 5-1000 ng/mL for ABZ and 10-1500 ng/mL (full validation) or 10-5000 ng/mL (partial validation) for ABZOX, with 5 and 10 ng/mL lower limit of quantification (LLOQ) for ABZ and ABZOX, respectively. The tests of accuracy and precision, matrix effect, extraction recovery and stability of the samples for both ABZ and ABZOX did not deviate more than 20% for the LLOQ and no more than 15% for other quality controls (QCs), according to regulatory agencies. © 2013.

[Simultaneous determination of 6 pesticides in drinking water by high performance liquid chromatography-tandem mass spectrometry with solid phase extraction].

PubMed

Liu, Hua-liang; Wang, Lian-hong

2013-05-01

To develop an analytical method for simultaneous determination of 6 pesticides, namely bentazone, 2,4-dichlorophenoxyacetic acid,carbofuran, carbaryl, atrazine and pentachlorophenol, in drinking water by high performance liquid chromatography-tandem mass spectrometry, and thereby to provide a reference to revise the Health Standards for Drinking Water (GB/T 5750-2006). Meanwhile, to evaluate the content of the above 6 pesticides in the drinking water samples supplied by 12 centralized water plants in Jiangsu province. The 10 ml water sample was acidized by hydrochloric acid to pH ≤ 2, and then concentrated by solid phase extraction cartridge and eluted with acetone. The solvent was changed into methanol after drying by nitrogen blow. The target compounds were separated by C18 column using methanol/water as mobile phase, and detected by mass spectrometry with multi-reaction-monitoring(MRM) mode. The repeatability and sensitivity of the assay were evaluated. The drinking water samples from the 12 water plants were then detected. In this experimental method, the minimum detectable concentration were around 0.02-0.41 µg/L, with the recovery rate at 75%-115%, and the RSD between 2% and 10%. Under the experimental condition, there were no pesticides detected in the drinking water samples from the 12 centralized water plants. The method is efficient and environment-friendly, with little discharge of effluent, which could meet the requirement of the drinking water monitor.

Direct-write liquid phase transformations with a scanning transmission electron microscope

DOE PAGES

Unocic, Raymond R.; Lupini, Andrew R.; Borisevich, Albina Y.; ...

2016-08-03

The highly energetic electron beam from a scanning transmission electron microscope (STEM) can induce local changes in the state of matter, ranging from local knock-out and atomic movement, to amorphization/crystallization, and chemical/electrochemical reactions occuring at localized liquid-solid and gas-solid interfaces. To date, fundamental studies of e-beam induced phenomena and practical applications have been limited by conventional e-beam rastering modes that allow only for uniform e-beam exposures. Here we develop an automated liquid phase nanolithography method that is capable of directly writing nanometer scaled features within silicon nitride encapsulated liquid cells. An external beam control system, connected to the scan coilsmore » of an aberration-corrected STEM, is used to precisely control the position, dwell time, and scan velocity of a sub-nanometer STEM probe. Site-specific locations in a sealed liquid cell containing an aqueous solution of H 2PdCl 4 are irradiated to controllably deposit palladium onto silicon nitride membranes. We determine the threshold electron dose required for the radiolytic deposition of metallic palladium, explore the influence of electron dose on the feature size and morphology of nanolithographically patterned nanostructures, and propose a feedback-controlled monitoring method for active control of the nanofabricated structures through STEM detector signal monitoring. As a result, this approach enables both fundamental studies of electron beam induced interactions with matter, as well as opens a pathway to fabricate nanostructures with tailored architectures and chemistries via shape-controlled nanolithographic patterning from liquid phase precursors.« less

Subsonic leaky Rayleigh waves at liquid-solid interfaces.

PubMed

Mozhaev, V G; Weihnacht, M

2002-05-01

The paper is devoted to the study of leaky Rayleigh waves at liquid-solid interfaces close to the border of the existence domain of these modes. The real and complex roots of the secular equation are computed for interface waves at the boundary between water and a binary isotropic alloy of gold and silver with continuously variable composition. The change of composition of the alloy allows one to cross a critical velocity for the existence of leaky waves. It is shown that, contrary to popular opinion, the critical velocity does not coincide with the phase velocity of bulk waves in liquid. The true threshold velocity is found to be smaller, the correction being of about 1.45%. Attention is also drawn to the fact that using the real part of the complex phase velocity as a velocity of leaky waves gives only approximate value. The most interesting feature of the waves under consideration is the presence of energy leakage in the subsonic range of the phase velocities where, at first glance, any radiation by harmonic waves is not permitted. A simple physical explanation of this radiation with due regard for inhomogeneity of radiated and radiating waves is given. The controversial question of the existence of leaky Rayleigh waves at a water/ice interface is reexamined. It is shown that the solution considered previously as a leaky wave is in fact the solution of the bulk-wave-reflection problem for inhomogeneous waves.

Solid electrolyte-electrode system for an electrochemical cell

DOEpatents

Tuller, Harry L.; Kramer, Steve A.; Spears, Marlene A.

1995-01-01

An electrochemical device including a solid electrolyte and solid electrode composed of materials having different chemical compositions and characterized by different electrical properties but having the same crystalline phase is provided. A method for fabricating an electrochemical device having a solid electrode and solid electrolyte characterized by the same crystalline phase is also provided.

Two-dimensional solid-phase extraction strategy for the selective enrichment of aminoglycosides in milk.

PubMed

Shen, Aijin; Wei, Jie; Yan, Jingyu; Jin, Gaowa; Ding, Junjie; Yang, Bingcheng; Guo, Zhimou; Zhang, Feifang; Liang, Xinmiao

2017-03-01

An orthogonal two-dimensional solid-phase extraction strategy was established for the selective enrichment of three aminoglycosides including spectinomycin, streptomycin, and dihydrostreptomycin in milk. A reversed-phase liquid chromatography material (C 18 ) and a weak cation-exchange material (TGA) were integrated in a single solid-phase extraction cartridge. The feasibility of two-dimensional clean-up procedure that experienced two-step adsorption, two-step rinsing, and two-step elution was systematically investigated. Based on the orthogonality of reversed-phase and weak cation-exchange procedures, the two-dimensional solid-phase extraction strategy could minimize the interference from the hydrophobic matrix existing in traditional reversed-phase solid-phase extraction. In addition, high ionic strength in the extracts could be effectively removed before the second dimension of weak cation-exchange solid-phase extraction. Combined with liquid chromatography and tandem mass spectrometry, the optimized procedure was validated according to the European Union Commission directive 2002/657/EC. A good performance was achieved in terms of linearity, recovery, precision, decision limit, and detection capability in milk. Finally, the optimized two-dimensional clean-up procedure incorporated with liquid chromatography and tandem mass spectrometry was successfully applied to the rapid monitoring of aminoglycoside residues in milk. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Determination of carbendazim and thiabendazole in tomatoes by solid-phase microextraction coupled with high performance liquid chromatography and fluorescence detection].

PubMed

Hu, Yanxue; Yang, Xiumin; Wang, Zhi; Wang, Chun; Zhao, Jin

2005-11-01

A novel method for the determination of carbendazim (MBC) and thiabendazole (TBZ) in tomatoes by solid-phase microextraction (SPME) coupled with high performance liquid chromatography (HPLC) and fluorescence detection was developed. The experimental conditions of SPME, including extraction fiber, extraction time, extraction temperature, desorption time, desorption solvent, desorption mode, pH value, organic solvent and ionic strength, and HPLC conditions were optimized. The SPME for MBC and TBZ was performed on a 65 microm polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre for 50 min at room temperature with the solution being stirred at 1 100 r/min. The florescence detection was made at 315 nm with excitation wavelength at 280 nm. The method is linear for MBC and TBZ over the range assayed from 0.01 to 1.0 mg/kg tomatoes with the detection limits of 0.003 mg/kg and 0. 001 mg/kg and the correlation coefficients of 0.995 8 and 0.996 7, respectively. The average recoveries for MBC and TBZ were 83.5% and 85.6% with the relative standard deviations (RSDs) of 6.5% and 3.8%, respectively. The method is fast, simple, sensitive, solvent-free and suitable for the determination of MBC and TBZ in tomatoes.

Development of a polymeric ionic liquid coating for direct-immersion solid-phase microextraction using polyhedral oligomeric silsesquioxane as cross-linker.

PubMed

Chen, Chunyan; Liang, Xiaotong; Wang, Jianping; Zou, Ying; Hu, Huiping; Cai, Qingyun; Yao, Shouzhuo

2014-06-27

A novel solid-phase microextraction (SPME) fiber was developed by chemical binding of a crosslinked polymeric ionic liquid (PIL) on the surface of an anodized Ti wire, and was applied in direct-immersion mode for the extraction of perfluorinated compounds (PFCs) from water samples coupled with high performance liquid chromatography-tandem mass spectrometry analysis. The PIL coatings were synthesized by using 1-vinyl-3-hexylimidazolium hexafluorophosphate as monomer and methylacryloyl-substituted polyhedral oligomeric silsesquioxane (POSS) as cross-linker via free radical reaction. The proposed fiber coating exhibited high mechanical stability due to the chemical bonding between the coating and the Ti wire surface. The integration of POSS reagent enhanced the organic solvent resistance of the coating. The parameters affecting the extraction performance of the fiber coating including extraction time, pH of solution, ionic strength and desorption conditions were optimized. The developed PIL-POSS fiber showed good linearity (R<0.998) between 0.1 and 50ngmL(-1) with method detection limits ranging from 0.005 to 0.08ngmL(-1) depending on the analyte, and with relative standard deviation for single-fiber repeatability and fiber-to-fiber reproducibility less than 8.6% and 9.5%, respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

Nucleation and strain-stabilization during organic semiconductor thin film deposition.

PubMed

Li, Yang; Wan, Jing; Smilgies, Detlef-M; Bouffard, Nicole; Sun, Richard; Headrick, Randall L

2016-09-07

The nucleation mechanisms during solution deposition of organic semiconductor thin films determine the grain morphology and may influence the crystalline packing in some cases. Here, in-situ optical spectromicroscopy in reflection mode is used to study the growth mechanisms and thermal stability of 6,13-bis(trisopropylsilylethynyl)-pentacene thin films. The results show that the films form in a supersaturated state before transforming to a solid film. Molecular aggregates corresponding to subcritical nuclei in the crystallization process are inferred from optical spectroscopy measurements of the supersaturated region. Strain-free solid films exhibit a temperature-dependent blue shift of optical absorption peaks due to a continuous thermally driven change of the crystalline packing. As crystalline films are cooled to ambient temperature they become strained although cracking of thicker films is observed, which allows the strain to partially relax. Below a critical thickness, cracking is not observed and grazing incidence X-ray diffraction measurements confirm that the thinnest films are constrained to the lattice constants corresponding to the temperature at which they were deposited. Optical spectroscopy results show that the transition temperature between Form I (room temperature phase) and Form II (high temperature phase) depends on the film thickness, and that Form I can also be strain-stabilized up to 135 °C.

A novel optimised and validated method for analysis of multi-residues of pesticides in fruits and vegetables by microwave-assisted extraction (MAE)-dispersive solid-phase extraction (d-SPE)-retention time locked (RTL)-gas chromatography-mass spectrometry with Deconvolution reporting software (DRS).

PubMed

Satpathy, Gouri; Tyagi, Yogesh Kumar; Gupta, Rajinder Kumar

2011-08-01

A rapid, effective and ecofriendly method for sensitive screening and quantification of 72 pesticides residue in fruits and vegetables, by microwave-assisted extraction (MAE) followed by dispersive solid-phase extraction (d-SPE), retention time locked (RTL) capillary gas-chromatographic separation in trace ion mode mass spectrometric determination has been validated as per ISO/IEC: 17025:2005. Identification and reporting with total and extracted ion chromatograms were facilitated to a great extent by Deconvolution reporting software (DRS). For all compounds LOD were 0.002-0.02mg/kg and LOQ were 0.025-0.100mg/kg. Correlation coefficients of the calibration curves in the range of 0.025-0.50mg/kg were >0.993. To validate matrix effects repeatability, reproducibility, recovery and overall uncertainty were calculated for the 35 matrices at 0.025, 0.050 and 0.100mg/kg. Recovery ranged between 72% and 114% with RSD of <20% for repeatability and intermediate precision. The reproducibility of the method was evaluated by an inter laboratory participation and Z score obtained within ±2. Copyright © 2011 Elsevier Ltd. All rights reserved.

Tensile Strength and Hardness Correlations with Microscopy in Friction welded Aluminium to Copper

NASA Astrophysics Data System (ADS)

Satish, Rengarajan; Seshagiri Rao, Vaddi; Ananthapadmanaban, Dattaguru; Ravi, Balappa

2016-01-01

Aluminium and copper are good conductors of heat and electricity, copper being the better conductor, is a costly metal indeed. On the other hand, aluminium is cheap, easily available and also has a lower density than copper. Hence, worldwide efforts are being made to partially replace copper wire. Solid state welding should be used to join aluminium to copper. This is because the use of fusion welding results in brittle phases formed in the weld interface. One of the solid state welding techniques used for joining aluminium to copper is friction welding. In this paper, an attempt has been made to join aluminium to copper by friction welding by varying the friction welding parameters, namely friction pressure, upset pressure, burn-off length and speed of rotation of the workpiece. Nine different friction welding parameter combinations were used during welding in accordance with ASTM standards and results have been reported. Tensile strength and hardness tests were carried out for each parameter combination. Optimum friction welding parameter combination was identified with respect to tensile strength. Scanning Electron Microscopy and Electron dispersive spectroanalysis were obtained to identify modes of fracture and presence of intermetallic phases for each friction welding combination with the aim to narrow down friction welding parameters that give good properties on the whole.

Rapid determination of amino acids in neonatal blood samples based on derivatization with isobutyl chloroformate followed by solid-phase microextraction and gas chromatography/mass spectrometry.

PubMed

Deng, Chunhui; Li, Ning; Zhang, Xiangmin

2004-01-01

The purpose of this study was to develop a simple, rapid and sensitive analytical method for determination of amino acids in neonatal blood samples. The developed method involves the employment of derivatization and a solid-phase microextraction (SPME) technique together with gas chromatography/mass spectrometry (GC/MS). Amino acids in blood samples were derivatized by a mixture of isobutyl chloroformate, methanol and pyridine, and the N(O,S)-alkoxycarbonyl alkyl esters thus formed were headspace extracted by a SPME fiber. Finally, the extracted analytes on the fiber were desorbed and detected by GC/MS in electron impact (EI) mode. L-Valine, L-leucine, L-isoleucine, L-phenylanaline and L-tyrosine in blood samples were quantitatively analyzed by measurement of the corresponding N(O,S)-alkoxycarbonyl alkyl esters using an external standard method. SPME conditions were optimized, and the method was validated. The method was applied to diagnosis of neonatal phenylkenuria (PKU) and maple syrup urine disease (MSUD) by the analyses of five amino acids in blood samples. The results showed that the proposed method is a potentially powerful tool for simultaneous screening for neonatal PKU and MSUD. Copyright (c) 2004 John Wiley & Sons, Ltd.

An electrochemically enhanced solid-phase microextraction approach based on a multi-walled carbon nanotubes/Nafion composite coating.

PubMed

Zeng, Jingbin; Chen, Jinmei; Song, Xinhong; Wang, Yiru; Ha, Jaeho; Chen, Xi; Wang, Xiaoru

2010-03-12

In this paper, we proposed an approach using a multi-walled carbon nanotubes (MWCNTs)/Nafion composite coating as a working electrode for the electrochemically enhanced solid-phase microextraction (EE-SPME) of charged compounds. Suitable negative and positive potentials were applied to enhance the extraction of cationic (protonated amines) and anionic compounds (deprotonated carboxylic acids) in aqueous solutions, respectively. Compared to the direct SPME mode (DI-SPME) (without applying potential), the EE-SPME presented more effective and selective extraction of charged analytes primarily via electrophoresis and complementary charge interaction. The experimental parameters relating to extraction efficiency of the EE-SPME such as applied potentials, extraction time, ionic strength, sample pH were studied and optimized. The linear dynamic range of developed EE-SPME-GC for the selected amines spanned three orders of magnitude (0.005-1mugmL(-1)) with R(2) larger than 0.9933, and the limits of detection were in the range of 0.048-0.070ngmL(-1). All of these characteristics demonstrate that the proposed MWCNTs/Nafion EE-SPME is an efficient, flexible and versatile sampling and extraction tool which is ideally suited for use with chromatographic methods. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Thermo-responsive polymer tethered metal-organic framework core-shell magnetic microspheres for magnetic solid-phase extraction of alkylphenols from environmental water samples.

PubMed

Jia, Yuqian; Su, Hao; Wong, Y-L Elaine; Chen, Xiangfeng; Dominic Chan, T-W

2016-07-22

In this work, the thermo-responsive polymer PNIPAM tethered to Fe3O4@SiO2@MOF core-shell magnetic microspheres was first synthesized by a surface-selective post-synthetic strategy and underwent highly efficient magnetic solid-phase extraction (MSPE) of alkylphenols from aqueous samples. Alkylphenols, including 4-tert-octylphenol (OP) and 4-n-nonylphenol (NP), were selected as target compounds. The sample quantification was carried out using LC-MS/MS in multiple reaction monitor (MRM) mode. Under optimal working conditions, the developed method showed good linearity in the range of 5-1000ngL(-1), a low limit of detection (1.5ngL(-1)), and good repeatability (relative standard deviation, <8%, n=5) for NP and OP. Owning to the hydrophilic/hydrophobic switchable properties of the nanocomposite, high recoveries (78.7-104.3%) of alkylphenols were obtained under different extraction conditions. The levels of OP and NP in environmental samples collected from local river, lake and pond waters were analyzed using the developed method. It was believed that the synthesized material with the thermo-responsive coating, large surface areas and magnetic properties should have great potential in the extraction and removal of alkylphenols from environmental samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Focused microwave-assisted extraction combined with solid-phase microextraction and gas chromatography-mass spectrometry for the selective analysis of cocaine from coca leaves.

PubMed

Bieri, Stefan; Ilias, Yara; Bicchi, Carlo; Veuthey, Jean-Luc; Christen, Philippe

2006-04-21

An effective combination of focused microwave-assisted extraction (FMAE) with solid-phase microextraction (SPME) prior to gas chromatography (GC) is described for the selective extraction and quantitative analysis of cocaine from coca leaves (Erythroxylum coca). This approach required switching from an organic extraction solvent to an aqueous medium more compatible with SPME liquid sampling. SPME was performed in the direct immersion mode with a universal 100 microm polydimethylsiloxane (PDMS) coated fibre. Parameters influencing this extraction step, such as solution pH, sampling time and temperature are discussed. Furthermore, the overall extraction process takes into account the stability of cocaine in alkaline aqueous solutions at different temperatures. Cocaine degradation rate was determined by capillary electrophoresis using the short end injection procedure. In the selected extraction conditions, less than 5% of cocaine was degraded after 60 min. From a qualitative point of view, a significant gain in selectivity was obtained with the incorporation of SPME in the extraction procedure. As a consequence of SPME clean-up, shorter columns could be used and analysis time was reduced to 6 min compared to 35 min with conventional GC. Quantitative results led to a cocaine content of 0.70 +/- 0.04% in dry leaves (RSD <5%) which agreed with previous investigations.

Novel double-confined polymeric ionic liquids as sorbents for solid-phase microextraction with enhanced stability and durability in high-ionic-strength solution.

PubMed

Feng, Juanjuan; Sun, Min; Xu, Lili; Wang, Shuai; Liu, Xia; Jiang, Shengxiang

2012-12-14

Because of the occurrence of ion exchange between high-ionic-strength solution and anions of polymeric ionic liquids (PILs), PILs based solid-phase microextraction (SPME) fibers were rarely used in direct immersion mode to high-salt-added samples. In this work, a novel double-confined PIL sorbent was prepared by co-polymerization of cation and anion of 1-vinyl-3-octylimidzaolium p-styrenesulfonate (VOIm(+)SS(-)). The poly(VOIm(+)-SS(-)) was chemically bonded onto functionalized stainless steel wire via surface radical chain-transfer reaction. Stability of poly(VOIm(+)-SS(-)) in high-ionic-strength solution was investigated and compared with that of poly(1-vinyl-3-octylimidzaolium benzenesulfonate) (poly(VOIm(+)BS(-))) by elemental analysis of sulfur element, and results turned out that the poly(VOIm(+)-SS(-)) was more stable. Coupled to gas chromatography (GC), the poly(VOIm(+)-SS(-)) fiber was used to extract three sorts of compounds including anilines, phenols and phthalate esters in aqueous solution. The as-established method showed good linearity, low detection limits, and acceptable repeatability. The direct immersion SPME-GC method was applied to determine the model phthalate esters in bottled mineral water. The determination results were satisfactory. Copyright © 2012 Elsevier B.V. All rights reserved.

Trends in long-period seismicity related to magmatic fluid compositions

USGS Publications Warehouse

Morrissey, M.M.; Chouet, B.A.

2001-01-01

Sound speeds and densities are calculated for three different types of fluids: gas-gas mixture; ash-gas mixture; and bubbly liquid. These fluid properties are used to calculate the impedance contrast (Z) and crack stiffness (C) in the fluid-driven crack model (Chouet: J. Geophys. Res., 91 (1986) 13,967; 101 (1988) 4375; A seismic model for the source of long-period events and harmonic tremor. In: Gasparini, P., Scarpa, R., Aki, K. (Eds.), Volcanic Seismology, IAVCEI Proceedings in Volcanology, Springer, Berlin, 3133). The fluid-driven crack model describes the far-field spectra of long-period (LP) events as modes of resonance of the crack. Results from our calculations demonstrate that ash-laden gas mixtures have fluid to solid density ratios comparable to, and fluid to solid velocity ratios lower than bubbly liquids (gas-volume fractions 20% gas-volume fraction yields values of Q-1r similar to those for a rectangular crack. As with gas-gas and ash-gas mixtures, an increase in mass fraction narrows the bandwidth of the dominant mode and shifts the spectra to lower frequencies. Including energy losses due to dissipative processes in a bubbly liquid increases attenuation. Attenuation may also be higher in ash-gas mixtures and foams if the effects of momentum and mass transfer between the phases were considered in the calculations. ?? 2001 Elsevier Science B. V. All rights reserved.

Adsorption of the Three-phase Emulsion on Various Solid Surfaces.

PubMed

Enomoto, Yasutaka; Imai, Yoko; Tajima, Kazuo

2017-07-01

The present study investigates the adsorption of the three-phase emulsion on various solid/water interfaces. Vesicles can be used as emulsifiers in the three-phase emulsions and act as an independent phase unlike the surfactant used in conventional emulsions; therefore, it is expected that the three-phase emulsion formed by the adhesion of vesicles to the oil/water interface will adsorb on various solid/water interfaces. The cationic three-phase emulsion was prepared to encourage emulsion adsorption on negatively charged solid substrates in water. The emulsifier polyoxyethylene-(10) hydrogenated castor oil was rendered cationic by mixing with the surfactant cetyltrimethylammonium bromide and then used to prepare the cationic three-phase emulsion of hexadecane-in-water. Three solid substrates (silicon, glass, and copper) were dipped in the cationic emulsion and the emulsion was found to adsorb on the solid substrates while maintaining its structure. The amount of hexadecane adsorbed on the various surfaces was investigated by gas chromatography and found to increase with increasing hexadecane concentration in the emulsion and eventually plateaued just like molecular adsorption. The maximum surface coverage of the emulsion on the substrates was approximately 80%. However, even the equivalent nonionic three-phase emulsion was found to adsorb on the three solid surfaces. This was attributed to a novel mechanism of irreversible adhesion via the van der Waals attractive force.

Manual Solid-Phase Peptide Synthesis of Metallocene-Peptide Bioconjugates

ERIC Educational Resources Information Center

Kirin, Srecko I.; Noor, Fozia; Metzler-Nolte, Nils; Mier, Walter

2007-01-01

A simple and relatively inexpensive procedure for preparing a biologically active peptide using solid phase peptide synthesis (SPPS) is described. Fourth-year undergraduate students have gained firsthand experience from the solid-phase synthesis techniques and they have become familiar with modern analytical techniques based on the particular…

Effect of solid-meal caloric content on gastric emptying kinetics of solids and liquids.

PubMed

Urbain, J L; Siegel, J A; Mortelmans, L; van Cutsem, E; van den Maegdenbergh, V; de Roo, M

1989-08-01

In this study, we have evaluated the effect of the caloric content of a physiological test meal on the gastric emptying kinetics of solids and liquids. 22 healthy male volunteers were studied in two groups matched for age. After an overnight fast, each volunteer underwent the same test procedure; in the first group (G I), 10 volunteers received a meal consisting of bread, 111In-DTPA water and 1 scrambled egg labeled with 99mTc-labelled sulphur colloid; in the second group (G II) 12 volunteers were given the same meal but with 2 labeled eggs in order to increase the caloric content of the solid phase meal. Simultaneous anterior and posterior images were recorded using a dual-headed gamma camera. Solid and liquid geometric mean data were analyzed to determine the lag phase, the emptying rate and the half-emptying time for both solids and liquids. Solid and liquid gastric half-emptying times were significantly prolonged in G II compared to G I volunteers. For the solid phased, the delay was accounted for by a longer lag phase and a decrease in the equilibrium emptying rate. The emptying rate of the liquid phase was significantly decreased in G II compared to G I. Within each group, no statistically significant difference was observed between solid and liquid emptying rates. We conclude that the caloric content of the solid portion of a meal not only alters the emptying of the solid phase but also affects the emptying of the liquid component of the meal.

Vibrational investigations of CO2-H2O, CO2-(H2O)2, and (CO2)2-H2O complexes isolated in solid neon.

PubMed

Soulard, P; Tremblay, B

2015-12-14

The van der Waals complex of H2O with CO2 has attracted considerable theoretical interest as a typical example of a weak binding complex with a dissociation energy less than 3 kcal/mol. Up to now, experimental vibrational data are sparse. We have studied by FTIR the complexes involving CO2 and water molecules in solid neon. Many new absorption bands close to the well known monomers fundamentals give evidence for at least three (CO2)n-(H2O)m complexes, noted n:m. Concentration effects combined with a detailed vibrational analysis allow for the identification of sixteen, twelve, and five transitions for the 1:1, 1:2, and 2:1 complexes, respectively. Careful examination of the far infrared spectral region allows the assignment of several 1:1 and 1:2 intermolecular modes, confirmed by the observation of combinations of intra + intermolecular transitions, and anharmonic coupling constants have been derived. Our results demonstrate the high sensibility of the solid neon isolation to investigate the hydrogen-bonded complexes in contrast with the gas phase experiments for which two quanta transitions cannot be easily observed.

Use of oleic-acid functionalized nanoparticles for the magnetic solid-phase microextraction of alkylphenols in fruit juices using liquid chromatography-tandem mass spectrometry.

PubMed

Viñas, Pilar; Pastor-Belda, Marta; Torres, Aitor; Campillo, Natalia; Hernández-Córdoba, Manuel

2016-05-01

Magnetic nanoparticles of cobalt ferrite with oleic acid as the surfactant (CoFe2O4/oleic acid) were used as sorbent material for the determination of alkylphenols in fruit juices. High sensitivity and specificity were achieved by liquid chromatography and detection using both diode-array (DAD) and electrospray-ion trap-tandem mass spectrometry (ESI-IT-MS/MS) in the selected reaction monitoring (SRM) mode of the negative fragment ions for alkylphenols (APs) and in positive mode for ethoxylate APs (APEOs). The optimized conditions for the different variables influencing the magnetic separation procedure were: mass of magnetic nanoparticles, 50mg, juice volume, 10mL diluted to 25mL with water, pH 6, stirring for 10min at room temperature, separation with an external neodymium magnet, desorption with 3mL of methanol and orbital shaking for 5min. The enriched organic phase was evaporated and reconstituted with 100µL acetonitrile before injecting 30µL into a liquid chromatograph with a mobile phase composed of acetonitrile/0.1% (v/v) formic acid under gradient elution. Quantification limits were in the range 3.6 to 125ngmL(-1). The recoveries obtained were in the 91-119% range, with RSDs lower than 14%. The ESI-MS/MS spectra permitted the correct identification of both APs and APEOs in the fruit juice samples. Copyright © 2016 Elsevier B.V. All rights reserved.

[LC-MS/MS analysis of determination of strychnine and brucine in formaldehyde fixed tissue].

PubMed

Zhan, Lan-fen; Liu, Ming-dong; Yan, You-yi; Ye, Yi; Wang, Wei; Wang, Zhi-hui; Zhao, Jun-hong; Liao, Lin-chuan

2012-10-01

To establish a method for determination of strychnine and brucine in formaldehyde fixed tissue by LC-MS/MS analysis. The samples were pretreated with solid phase extraction using SCX cartridges and separated on SB-C18 column with mobile phase 0.1% formic acid : 0.1% formic acid-acetonitrile (75:25). Electrospray ionization (ESI) source was utilized and operated in positive ion mode. Multiple reactions monitoring (MRM) mode was applied. External standard method was applied for quantitation. The chromatographic separation of strychnine and brucine in formaldehyde fixed nephritic and hepatic tissues resulted successfully. The standard curve was linear in the range of 0.002-2.0 microg/g for strychnine and brucine in formaldehyde fixed tissues, and the correlation coefficient was more than 0.996. The limits of detection (LOD) of strychnine and brucine in nephritic tissues were 0.06ng/g and 0.03 ng/g, respectively. The LOD of both chemicals were 0.3 ng/g in hepatic tissues. The extraction recovery rate was more than 74.5%. The precision of intra-day and inter-day were both less than 8.2%. Strychnine and brucine can be sensitive to be determined in formaldehyde fixed tissue by LC-MS/MS analysis. It can be applied in the forensic toxicological analysis.

Effect of Zn doping on structural and dielectric properties of tetragonal Ni{sub 1-x}Zn{sub x}Fe{sub 2}O{sub 4} (0.0 ≤ x ≤ 0.5)

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

Lone, S. A.; Dar, M. A.; Kumar, A.

2015-06-24

A series of Ni-Zn ferrite with compositional formula Ni{sub 1-x}Zn{sub x}Fe{sub 2}O{sub 4} (0.0 ≤ x ≤ 0.5) were prepared by solid-state reaction route. The influence of the Zn content on the structural and dielectric properties of NiFe{sub 2}O{sub 4} was investigated using X-ray powder diffraction (XRD), Raman spectroscopy and dielectric measurements. XRD analysis reveals that the samples are polycrystalline single-phase cubic spinel in structure excluding the presence of any secondary phase corresponding to any structure. Slight variation in the lattice parameter of Zn doped NiFe{sub 2}O{sub 4} has been observed due to difference in ionic radii of cations. Ramanmore » analysis reveals the doublet like nature of A{sub 1g} mode for all synthesized samples. Small shift in Raman modes and increment in the line width has been observed with the doping ions. Furthermore, room temperature dielectric properties of all the prepared samples have been reported. It is observed that for each sample the dielectric constant decreases with an increase of frequency and becomes constant at higher frequencies.« less

Determination of perfluoroalkyl carboxylic, sulfonic, and phosphonic acids in food.

PubMed

Ullah, Shahid; Alsberg, Tomas; Vestergren, Robin; Berger, Urs

2012-11-01

A sensitive and accurate method was developed and validated for simultaneous analysis of perfluoroalkyl carboxylic acids, sulfonic acids, and phosphonic acids (PFPAs) at low picograms per gram concentrations in a variety of food matrices. The method employed extraction with acetonitrile/water and cleanup on a mixed-mode co-polymeric sorbent (C8 + quaternary amine) using solid-phase extraction. High-performance liquid chromatographic separation was achieved on a C18 column using a mobile phase gradient containing 5 mM 1-methyl piperidine for optimal chromatographic resolution of PFPAs. A quadrupole time-of-flight high-resolution mass spectrometer operating in negative ion mode was used as detector. Method detection limits were in the range of 0.002 to 0.02 ng g(-1) for all analytes. Sample preparation (extraction and cleanup) recoveries at a spiking level of 0.1 ng g(-1) to a baby food composite were in the range of 59 to 98 %. A strong matrix effect was observed in the analysis of PFPAs in food extracts, which was tentatively assigned to sorption of PFPAs to the injection vial in the solvent-based calibration standard. The method was successfully applied to a range of different food matrices including duplicate diet samples, vegetables, meat, and fish samples.

Theory of amorphous ices

PubMed Central

Limmer, David T.; Chandler, David

2014-01-01

We derive a phase diagram for amorphous solids and liquid supercooled water and explain why the amorphous solids of water exist in several different forms. Application of large-deviation theory allows us to prepare such phases in computer simulations. Along with nonequilibrium transitions between the ergodic liquid and two distinct amorphous solids, we establish coexistence between these two amorphous solids. The phase diagram we predict includes a nonequilibrium triple point where two amorphous phases and the liquid coexist. Whereas the amorphous solids are long-lived and slowly aging glasses, their melting can lead quickly to the formation of crystalline ice. Further, melting of the higher density amorphous solid at low pressures takes place in steps, transitioning to the lower-density glass before accessing a nonequilibrium liquid from which ice coarsens. PMID:24858957

Electron drift in a large scale solid xenon

DOE PAGES

Yoo, J.; Jaskierny, W. F.

2015-08-21

A study of charge drift in a large scale optically transparent solid xenon is reported. A pulsed high power xenon light source is used to liberate electrons from a photocathode. The drift speeds of the electrons are measured using a 8.7 cm long electrode in both the liquid and solid phase of xenon. In the liquid phase (163 K), the drift speed is 0.193 ± 0.003 cm/μs while the drift speed in the solid phase (157 K) is 0.397 ± 0.006 cm/μs at 900 V/cm over 8.0 cm of uniform electric fields. Furthermore, it is demonstrated that a factor twomore » faster electron drift speed in solid phase xenon compared to that in liquid in a large scale solid xenon.« less

Properties of two-mode squeezed number states

NASA Technical Reports Server (NTRS)

Chizhov, Alexei V.; Murzakhmetov, B. K.

1994-01-01

Photon statistics and phase properties of two-mode squeezed number states are studied. It is shown that photon number distribution and Pegg-Barnett phase distribution for such states have similar (N + 1)-peak structure for nonzero value of the difference in the number of photons between modes. Exact analytical formulas for phase distributions based on different phase approaches are derived. The Pegg-Barnett phase distribution and the phase quasiprobability distribution associated with the Wigner function are close to each other, while the phase quasiprobability distribution associated with the Q function carries less phase information.

[Characteristics of electroosmotic flow in open-tubular capillary electrochromatography with magnetic nanoparticle coating as mixed-mode stationary phase].

PubMed

Qin, Sasa; Zhou, Chaoran; Zhu, Yaxian; Ren, Zhiyu; Zhang, Lingyi; Fu, Honggang; Zhang, Weibing

2011-09-01

A novel open-tubular capillary electrochromatography (OT-CEC) column with magnetic nanoparticle coating as mixed-mode stationary phase was prepared. The mixed-mode stationary phases were obtained by mixing C18 and amino modified magnetic nanoparticles with different ratios. The mixed modified magnetic nanoparticles as stationary phase were introduced into the capillary by using external magnetic force. The magnetic nanoparticle coating can be easily regenerated by removing the external magnetic field, and applied to other separation modes. The characteristics of electroosmotic flow (EOF) were theoretically investigated through the effect of physicochemical properties of different stationary phases on EOF. The experiment was conducted under different ratios of mixed-mode stationary phases and coating lengths, and it was verified that the theoretical conclusions accorded with the experimental results. It was shown that the EOF can be easily adjusted by changing the ratio of stationary phases or the number of permanent magnets.

Grain Floatation During Equiaxed Solidification of an Al-Cu Alloy in a Side-Cooled Cavity: Part II—Numerical Studies

NASA Astrophysics Data System (ADS)

Kumar, Arvind; Walker, Mike J.; Sundarraj, Suresh; Dutta, Pradip

2011-08-01

In this article, a single-phase, one-domain macroscopic model is developed for studying binary alloy solidification with moving equiaxed solid phase, along with the associated transport phenomena. In this model, issues such as thermosolutal convection, motion of solid phase relative to liquid and viscosity variations of the solid-liquid mixture with solid fraction in the mobile zone are taken into account. Using the model, the associated transport phenomena during solidification of Al-Cu alloys in a rectangular cavity are predicted. The results for temperature variation, segregation patterns, and eutectic fraction distribution are compared with data from in-house experiments. The model predictions compare well with the experimental results. To highlight the influence of solid phase movement on convection and final macrosegregation, the results of the current model are also compared with those obtained from the conventional solidification model with stationary solid phase. By including the independent movement of the solid phase into the fluid transport model, better predictions of macrosegregation, microstructure, and even shrinkage locations were obtained. Mechanical property prediction models based on microstructure will benefit from the improved accuracy of this model.

Solid phase pegylation of hemoglobin.

PubMed

Suo, Xiaoyan; Zheng, Chunyang; Yu, Pengzhan; Lu, Xiuling; Ma, Guanghui; Su, Zhiguo

2009-01-01

A solid phase conjugation process was developed for attachment of polyethylene glycol to hemoglobin molecule. Bovine hemoglobin was loaded onto an ion exchange chromatography column and adsorbed by the solid medium. Succinimidyl carbonate mPEG was introduced in the mobile phase after the adsorption. Pegylation took place between the hemoglobin on the solid phase, and the pegylation reagent in the liquid phase. A further elution was carried out to separate the pegylated and the unpegylated protein. Analysis by HPSEC, SDS-PAGE, and MALLS demonstrated that the fractions eluted from the solid phase contained well-defined components. Pegylated hemoglobin with one PEG chain was obtained with the yield of 75%, in comparison to the yield of 30% in the liquid phase pegylation. The P(50) values of the mono-pegylated hemoglobin, prepared with SC-mPEG 5 kDa, 10 kDa and 20 kDa, were 19.97, 20.23 and 20.54 mmHg, which were much closer to the value of red blood cells than that of pegylated hemoglobin prepared with the conventional method.

Mechanism of Formation of Li 7 P 3 S 11 Solid Electrolytes through Liquid Phase Synthesis

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

Wang, Yuxing; Lu, Dongping; Bowden, Mark

Crystalline Li7P3S11 is a promising solid electrolyte for all solid state lithium/lithium ion batteries. A controllable liquid phase synthesis of Li7P3S11 is more desirable compared to conventional mechanochemical synthesis, but recent attempts suffer from reduced ionic conductivities. Here we elucidate the formation mechanism of crystalline Li7P3S11 synthesized in the liquid phase (acetonitrile, or ACN). We conclude that the crystalline Li7P3S11 forms through a two-step reaction: 1) formation of solid Li3PS4∙ACN and amorphous Li2S∙P2S5 phases in the liquid phase; 2) solid-state conversion of the two phases. The implication of this two-step reaction mechanism to the morphology control and the transport propertiesmore » of liquid phase synthesized Li7P3S11 is identified and discussed.« less

Inflationary tensor fossils in large-scale structure

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

Dimastrogiovanni, Emanuela; Fasiello, Matteo; Jeong, Donghui

Inflation models make specific predictions for a tensor-scalar-scalar three-point correlation, or bispectrum, between one gravitational-wave (tensor) mode and two density-perturbation (scalar) modes. This tensor-scalar-scalar correlation leads to a local power quadrupole, an apparent departure from statistical isotropy in our Universe, as well as characteristic four-point correlations in the current mass distribution in the Universe. So far, the predictions for these observables have been worked out only for single-clock models in which certain consistency conditions between the tensor-scalar-scalar correlation and tensor and scalar power spectra are satisfied. Here we review the requirements on inflation models for these consistency conditions to bemore » satisfied. We then consider several examples of inflation models, such as non-attractor and solid-inflation models, in which these conditions are put to the test. In solid inflation the simplest consistency conditions are already violated whilst in the non-attractor model we find that, contrary to the standard scenario, the tensor-scalar-scalar correlator probes directly relevant model-dependent information. We work out the predictions for observables in these models. For non-attractor inflation we find an apparent local quadrupolar departure from statistical isotropy in large-scale structure but that this power quadrupole decreases very rapidly at smaller scales. The consistency of the CMB quadrupole with statistical isotropy then constrains the distance scale that corresponds to the transition from the non-attractor to attractor phase of inflation to be larger than the currently observable horizon. Solid inflation predicts clustering fossils signatures in the current galaxy distribution that may be large enough to be detectable with forthcoming, and possibly even current, galaxy surveys.« less

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

Weese, Randall K.

In order to calculate the kinetic parameters from DSC data, we have used the generally accepted methods of Bershtein [13]. We have calculated the rate constants for 4 temperatures and the activation energy based on the shift in the transition temperature, β→δ for HMX. The values of E a from this work is 402 kJ/mol compared to previous results by Brill [9] of 204 kJ/mol. Brill and associates measured the phase transition of HMX using FTIR, sodium chloride plates and silicon oil. Given the differences in technique between FTIR and DSC the results found in this work are reasonable. Inmore » this investigation a large sample set (16) proved to be statistically valid for the determinations of k. Linear regressions were performed, observed and good fits were obtained, for each temperature. The enthalpy determination of ΔH o, for the β→δ phase transition was reproducible with in 3 parts in 100 over the range of this experiment. Thus, the data derived from this experiment k, E a, and ΔH o are valid parameters for the solid-solid phase transition. Obtaining pure β phase HMX was very important for this investigation. Related to the phase change is the particle size distribution and is presented in Figure 3. Compared to previous work on HMX, this study utilized very pure β phase material. In addition, the particle size was controlled more rigorously at about 160 μm, giving a more consistent result for α. Thus, these kinetic results should have less scatter than results with less control of HMX purity and particle size. The kinetic basis of the polymorphic conversion is due to the cohesive forces in the HMX crystal lattice [21]. The energy required to bring about change from chair to chair-chair conformation has been reported by Brill [21] as ring torsion and is essentially a normal mode of the molecule that requires about 4 kJ mol -1. For the purpose of this investigation the energy of activation found in this work relates to the disruption of the intermolecular interactions with in the crystal lattice of β phase HMX and is much larger (100X) than that of simple conformational changes. The evidence of a straightforward one step mechanism is not supported by this research. Solid-solid phase transition kinetics is very complexed. There are many factors that contribute to an overall reaction mechanism. The initial assumptions that were chosen to allow simple manipulation of the HMX phase transition data prove to be too limiting. The rate constant by definition should in fact be constant, however, our data reflects it is not (refer to k vs time plot in Appendix 2). The assumption of a first order, simple single step reaction is a good starting point for the study of HMX phase transition kinetics, but further analysis should be done with other reaction orders and multiple step mechanisms. Understanding the kinetics of β phase HMX will clearly help the custodian understand the limitations of storage and use of this compound.« less

n-Type Doping of Vapor-Liquid-Solid Grown GaAs Nanowires.

PubMed

Gutsche, Christoph; Lysov, Andrey; Regolin, Ingo; Blekker, Kai; Prost, Werner; Tegude, Franz-Josef

2011-12-01

In this letter, n-type doping of GaAs nanowires grown by metal-organic vapor phase epitaxy in the vapor-liquid-solid growth mode on (111)B GaAs substrates is reported. A low growth temperature of 400°C is adjusted in order to exclude shell growth. The impact of doping precursors on the morphology of GaAs nanowires was investigated. Tetraethyl tin as doping precursor enables heavily n-type doped GaAs nanowires in a relatively small process window while no doping effect could be found for ditertiarybutylsilane. Electrical measurements carried out on single nanowires reveal an axially non-uniform doping profile. Within a number of wires from the same run, the donor concentrations ND of GaAs nanowires are found to vary from 7 × 10(17) cm(-3) to 2 × 10(18) cm(-3). The n-type conductivity is proven by the transfer characteristics of fabricated nanowire metal-insulator-semiconductor field-effect transistor devices.

Size distributions of hydrophilic and hydrophobic fractions of water-soluble organic carbon in an urban atmosphere in Hong Kong

NASA Astrophysics Data System (ADS)

Wang, Nijing; Yu, Jian Zhen

2017-10-01

Water-soluble organic carbon (WSOC) is a significant part of ambient aerosol and plays an active role in contributing to aerosol's effect on visibility degradation and radiation budget through its interactions with atmospheric water. Size-segregated aerosol samples in the range of 0.056-18 μm were collected using a ten-stage impactor sampler at an urban site in Hong Kong over one-year period. The WSOC samples were separated into hydrophilic (termed WSOC_h) and hydrophobic fractions (i.e., the humic-like substances (HULIS) fraction) through solid-phase extraction procedure. Carbon in HULIS accounted for 40 ± 14% of WSOC. The size distribution of HULIS was consistently characterized in all seasons with a dominant droplet mode (46-71%) and minor condensation (9.0-18%) and coarse modes (20-35%). The droplet mode had a mass median aerodynamic diameter in the range of 0.7-0.8 μm. This size mode showed the largest seasonal variation in abundance, lowest in the summer (0.41 μg/m3) and highest in the winter (3.3 μg/m3). WSOC_h also had a dominant droplet mode, but was more evenly distributed among different size modes. Inter-species correlations within the same size mode suggest that the condensation-mode HULIS was partly associated with combustion sources and the droplet-mode was strongly associated with secondary sulfate formation and biomass burning particle aging processes. There is evidence to suggest that the coarse-mode HULIS largely originated from coagulation of condensation-mode HULIS with coarse soil/sea salt particles. The formation process and possible sources of WSOC_h was more complicated and multiple than HULIS and need further investigation. Our measurements indicate that WSOC components contributed a dominant fraction of water-soluble aerosol mass in particles smaller than 0.32 μm while roughly 20-30% in the larger particles.

Engineered glass seals for solid-oxide fuel cells

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

Surdoval, Wayne; Lara-Curzio, Edgar; Stevenson, Jeffry

2017-02-07

A seal for a solid oxide fuel cell includes a glass matrix having glass percolation therethrough and having a glass transition temperature below 650.degree. C. A deformable second phase material is dispersed in the glass matrix. The second phase material can be a compliant material. The second phase material can be a crushable material. A solid oxide fuel cell, a precursor for forming a seal for a solid oxide fuel cell, and a method of making a seal for a solid oxide fuel cell are also disclosed.

Solid electrolyte-electrode system for an electrochemical cell

DOEpatents

Tuller, H.L.; Kramer, S.A.; Spears, M.A.

1995-04-04

An electrochemical device including a solid electrolyte and solid electrode composed of materials having different chemical compositions and characterized by different electrical properties but having the same crystalline phase is provided. A method for fabricating an electrochemical device having a solid electrode and solid electrolyte characterized by the same crystalline phase is also provided. 17 figures.

Rapid determination of the volatile components in tobacco by ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction with gas chromatography-mass spectrometry.

PubMed

Yang, Yanqin; Chu, Guohai; Zhou, Guojun; Jiang, Jian; Yuan, Kailong; Pan, Yuanjiang; Song, Zhiyu; Li, Zuguang; Xia, Qian; Lu, Xinbo; Xiao, Weiqiang

2016-03-01

An ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction was first employed to determine the volatile components in tobacco samples. The method combined the advantages of ultrasound, microwave, and headspace solid-phase microextraction. The extraction, separation, and enrichment were performed in a single step, which could greatly simplify the operation and reduce the whole pretreatment time. In the developed method, several experimental parameters, such as fiber type, ultrasound power, and irradiation time, were optimized to improve sampling efficiency. Under the optimal conditions, there were 37, 36, 34, and 36 components identified in tobacco from Guizhou, Hunan, Yunnan, and Zimbabwe, respectively, including esters, heterocycles, alkanes, ketones, terpenoids, acids, phenols, and alcohols. The compound types were roughly the same while the contents were varied from different origins due to the disparity of their growing conditions, such as soil, water, and climate. In addition, the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method was compared with the microwave-assisted extraction coupled to headspace solid-phase microextraction and headspace solid-phase microextraction methods. More types of volatile components were obtained by using the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method, moreover, the contents were high. The results indicated that the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction technique was a simple, time-saving and highly efficient approach, which was especially suitable for analysis of the volatile components in tobacco. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Numerical investigation of influence on heat transfer characteristics to pneumatically conveyed dense phase flow by selecting models and boundary conditions

NASA Astrophysics Data System (ADS)

Zheng, Y.; Liu, Q.; Li, Y.

2012-03-01

Solids moving with a gas stream in a pipeline can be found in many industrial processes, such as power generation, chemical, pharmaceutical, food and commodity transfer processes. A mass flow rate of the solids is important characteristic that is often required to be measured (and controlled) to achieve efficient utilization of energy and raw materials in pneumatic conveying systems. The methods of measuring the mass flow rate of solids in a pneumatic pipeline can be divided into direct and indirect (inferential) measurements. A thermal solids' mass flow-meter, in principle, should ideally provide a direct measurement of solids flow rate, regardless of inhomogeneities in solids' distribution and environmental impacts. One key issue in developing a thermal solids' mass flow-meter is to characterize the heat transfer between the hot pipe wall and the gas-solids dense phase flow. The Eulerian continuum modeling with gas-solid two phases is the most common method for pneumatic transport. To model a gas-solid dense phase flow passing through a heated region, the gas phase is described as a continuous phase and the particles as the second phase. This study aims to describe the heat transfer characteristics between the hot wall and the gas-solids dense phase flow in pneumatic pipelines by modeling a turbulence gas-solid plug passing through the heated region which involves several actual and crucial issues: selections of interphase exchange coefficient, near-wall region functions and different wall surface temperatures. A sensitivity analysis was discussed to identify the influence on the heat transfer characteristics by selecting different interphase exchange coefficient models and different boundary conditions. Simulation results suggest that sensitivity analysis in the choice of models is very significant. The simulation results appear to show that a combination of choosing the Syamlal-O'Brien interphase exchange coefficient model and the standard k-ɛ model along with the standard wall function model might be the best approach, by which, the simulation data seems to be closest to the experimental results.

An UHPLC-MS/MS method for simultaneous quantification of human amyloid beta peptides Aβ1-38, Aβ1-40 and Aβ1-42 in cerebrospinal fluid using micro-elution solid phase extraction.

PubMed

Lin, Ping-Ping; Chen, Wei-Li; Yuan, Fei; Sheng, Lei; Wu, Yu-Jia; Zhang, Wei-Wei; Li, Guo-Qing; Xu, Hong-Rong; Li, Xue-Ning

2017-12-01

Amyloid beta (Aβ) peptides in cerebrospinal fluid are extensively estimated for identification of Alzheimer's disease (AD) as diagnostic biomarkers. Unfortunately, their pervasive application is hampered by interference from Aβ propensity of self-aggregation, nonspecifically bind to surfaces and matrix proteins, and by lack of quantitive standardization. Here we report on an alternative Ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for simultaneous measurement of human amyloid beta peptides Aβ1-38, Aβ1-40 and Aβ1-42 in cerebrospinal fluid (CSF) using micro-elution solid phase extraction (SPE). Samples were pre-processing by the mixed-mode micro-elution solid phase extraction and quantification was performed in the positive ion multiple reaction monitoring (MRM) mode using electrospray ionization. The stable-isotope labeled Aβ peptides 15 N 51 - Aβ1-38, 15 N 53 - Aβ1-40 and 15 N 55 - Aβ1-42 peptides were used as internal standards. And the artificial cerebrospinal fluid (ACSF) containing 5% rat plasma was used as a surrogate matrix for calibration curves. The quality control (QC) samples at 0.25, 2 and 15ng/mL were prepared. A "linear" regression (1/x 2 weighting): y=ax+b was used to fit the calibration curves over the concentration range of 0.1-20ng/mL for all three peptides. Coefficient of variation (CV) of intra-batch and inter-batch assays were all less than 6.44% for Aβ1-38, 6.75% for Aβ1-40 and 10.74% for Aβ1-42. The precision values for all QC samples of three analytes met the acceptance criteria. Extract recoveries of Aβ1-38, Aβ1-40 and Aβ1-42 were all greater than 70.78%, both in low and high QC samples. The stability assessments showed that QC samples at both low and high levels could be stable for at least 24h at 4°C, 4h at room temperature and through three freeze-thaw cycles without sacrificing accuracy or precision. And no significant carryover effect was observed. This validated UHPLC/MS/MS method was successfully applied to the quantitation of Aβ peptides in real human CSF samples. Our work may provide a reference method for simultaneous quantitation of human Aβ1-38, Aβ1-40 and Aβ1-42 from CSF. Copyright © 2017 Elsevier B.V. All rights reserved.

Liquid-phase and solid-phase microwave irradiations for reduction of graphite oxide

NASA Astrophysics Data System (ADS)

Zhao, Na; Wen, Chen-Yu; Zhang, David Wei; Wu, Dong-Ping; Zhang, Zhi-Bin; Zhang, Shi-Li

2014-12-01

In this paper, two microwave irradiation methods: (i) liquid-phase microwave irradiation (MWI) reduction of graphite oxide suspension dissolved in de-ionized water and N, N-dimethylformamide, respectively, and (ii) solid-phase MWI reduction of graphite oxide powder have been successfully carried out to reduce graphite oxide. The reduced graphene oxide products are thoroughly characterized by scanning electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, Fourier transform infrared spectral analysis, Raman spectroscopy, UV-Vis absorption spectral analysis, and four-point probe conductivity measurements. The results show that both methods can efficiently remove the oxygen-containing functional groups attached to the graphite layers, though the solid-phase MWI reduction method can obtain far more efficiently a higher quality-reduced graphene oxide with fewer defects. The I(D)/I(G) ratio of the solid-phase MWI sample is as low as 0.46, which is only half of that of the liquid-phase MWI samples. The electrical conductivity of the reduced graphene oxide by the solid method reaches 747.9 S/m, which is about 25 times higher than that made by the liquid-phase method.

Colloidal mode of transport in the Potomac River watershed

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

Maher, I.L.; Foster, G.D.

1995-12-31

Similarly to the particulate phase the colloidal phase may play an important role in the organic contaminant transport downstream the river. The colloidal phase consisting of microparticles and micromolecules which are small enough to be mobile and large enough to attract pollutants can absorb nonpolar organic compounds similarly as do soil and sediment particles. To test the hypothesis three river water samples have been analyzed for PAH content in the dissolved, the colloidal, and the particulate phase. The first sample was collected at the Blue Ridge province of Potomac River watershed, at Point of Rocks, the second one in themore » Pidmont province, at Riverbend Park, and the third sample at Coastal Plane, at Dyke Marsh (Belle Heven marina). In the laboratory environment each water sample was prefiltered to separate the particulate phase form the dissolved and colloidal phase. One part of the prefiltered water sample was ultrafiltered to separate colloids while the second part of the water was Goulden extracted. The separated colloidal phase was liquid-liquid extracted (LLE) while filters containing the suspended solids were Soxhlet extracted. The extracts of the particulate phase, the colloidal phase, and the dissolved plus colloidal phase were analyzed for selected PAHs via GC/MS. It is planned that concentrations of selected PAHs in three phases will be used for calculations of the partition coefficients, the colloid/dissolved partition coefficient and the particle/dissolved partition coefficient. Both partition coefficients will be compared to define the significance of organic contaminant transport by aquatic colloids.« less

Efficient Storing Energy Harvested by Triboelectric Nanogenerators Using a Safe and Durable All-Solid-State Sodium-Ion Battery.

PubMed

Hou, Huidan; Xu, Qingkai; Pang, Yaokun; Li, Lei; Wang, Jiulin; Zhang, Chi; Sun, Chunwen

2017-08-01

Storing energy harvested by triboelectric nanogenerators (TENGs) from ambient mechanical motion is still a great challenge for achieving low-cost and environmental benign power sources. Here, an all-solid-state Na-ion battery with safe and durable performance used for efficient storing pulsed energy harvested by the TENG is demonstrated. The solid-state sodium-ion batteries are charged by galvanostatic mode and pulse mode with the TENG, respectively. The all-solid-state sodium-ion battery displays excellent cyclic performance up to 1000 cycles with a capacity retention of about 85% even at a high charge and discharge current density of 48 mA g -1 . When charged by the TENG, an energy conversion efficiency of 62.3% is demonstrated. The integration of TENGs with the safe and durable all-solid-state sodium-ion batteries is potential for providing more stable power output for self-powered systems.

Multi scale modeling of ignition and combustion of micro and nano aluminum particles

NASA Astrophysics Data System (ADS)

Puri, Puneesh

With renewed interest in nano scale energetic materials like aluminum, many fundamental issues concerning the ignition and combustion characteristics at nano scales, remain to be clarified. The overall aim of the current study is the establishment of a unified theory accommodating the various processes and mechanisms involved in the combustion and ignition of aluminum particles at micro and nano scales. A comprehensive review on the ignition and combustion of aluminum particles at multi scales was first performed identifying various processes and mechanisms involved. Research focus was also placed on the establishment of a Molecular Dynamics (MD) simulation tool to investigate the characteristics of nano-particulate aluminum through three major studies. The general computational framework involved parallelized preprocessing, post-processing and main code with capability to simulate different ensembles using appropriate algorithms. Size dependence of melting temperature of pure aluminum particles was investigated in the first study. Phenomena like dynamic coexistence of solid and liquid phase and effect of surface charges on melting were explored. The second study involved the study of effect of defects in the form of voids on melting of bulk and particulate phase aluminum. The third MD study was used to analyze the thermo-mechanical behavior of nano-sized aluminum particles with total diameter of 5-10 nm and oxide thickness of 1-2.5 nm. The ensuing solid-solid and solid-liquid phase changes in the core and shell, stresses developed within the shell, and the diffusion of aluminum cations in the oxide layer, were explored in depth for amorphous and crystalline oxide layers. In the limiting case, the condition for pyrophoricity/explosivity of nano-particulate aluminum was analyzed and modified. The size dependence of thermodynamic properties at nano scales were considered and incorporated into the existing theories developed for micro and larger scales. Finally, a phenomenological theory for ignition and combustion of aluminum particles was proposed. The whole time history from ignition till particle burnout was divided into five stages. An attempt was made to explore different modes of ignition based on the effect of pressure, temperature, oxidizer, oxide thickness and particle diameter and was investigated using length and time scales involved during ignition and combustion.

Estimating production and consumption of solid reactive Fe phases in marine sediments from concentration profiles

EPA Science Inventory

1D diffusion models may be used to estimate rates of production and consumption of dissolved metabolites in marine sediments, but are applied less often to the solid phase. Here we used a numerical inverse method to estimate solid phase Fe(III) and Fe(II) consumption and product...

An experimental and theoretical study of molecular structure and vibrational spectra of 2-methylphenyl boronic acid by density functional theory calculations

NASA Astrophysics Data System (ADS)

Hiremath, Sudhir M.; Hiremath, C. S.; Khemalapure, S. S.; Patil, N. R.

2018-05-01

This paper reports the experimental and theoretical study on the structure and vibrations of 2-Methylphenyl boronic acid (2MPBA). The different spectroscopic techniques such as FT-IR (4000-400 cm-1) and FT-Raman (4000-50 cm-1) of the title molecule in the solid phase were recorded. The geometry of the molecule was fully optimized using density functional theory (DFT) (B3LYP) with 6-311++G(d, p) basis set calculations. The vibrational wavenumbers were also corrected with scale factor to take better results for the calculated data. Vibrational spectra were calculated and fundamental vibrations were assigned on the basis of the potential energy distribution (PED) of the vibrational modes obtained from VEDA 4 program. The calculated wavenumbers showed the best agreement with the experimental results. Whereas, it is observed that, the theoretical frequencies are more than the experimental one for O-H stretching vibration modes of the title molecule.

Using corona discharge-ion mobility spectrometry for detection of 2,4,6-Trichloroanisole.

PubMed

Lichvanová, Zuzana; Ilbeigi, Vahideh; Sabo, Martin; Tabrizchi, Mahmoud; Matejčík, Stefan

2014-09-01

In this work possible application of the corona discharge-ion mobility spectrometer (CD-IMS) for detection of 2,4,6-Trichloroanisole (TCA) has been investigated. We applied CD-IMS interfaced with orthogonal acceleration time of flight mass spectrometer (CD-IMS-oaTOF) to study the ion processes within the CD-IMS technique. The CD-IMS instrument was operated in two modes, (i) standard and (ii) reverse flow modes resulting in different chemical ionisation schemes by NO3(-)(HNO3)n (n=0,1,2) and O2(-)(H2O)n (n=0,1,2), respectively. The O2(-)(H2O)n ionisation was associated with formation of Cl(-) and (TCA-CH3)(-) ions from TCA. The NO3(-)(HNO3)n ionisation, resulted in formation of NO3(-)(HNO3)(TCA-Cl) adduct ions. Limit of detection (LOD) for TCA was determined in gas (100 ppb) and solid phases (150 ng). Copyright © 2014 Elsevier B.V. All rights reserved.

Structural analysis and ferroelectric properties of Fe doped BaTiO{sub 3}

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

Mishra, Ashutosh, E-mail: a.mansuri14@gmail.com, E-mail: amishra1960@yahoo.co.in; Mansuri, Amantulla, E-mail: a.mansuri14@gmail.com, E-mail: amishra1960@yahoo.co.in; Dwivedi, J. P.

2016-05-23

The polycrystalline samples of Fe doped BaTiO{sub 3} (BTO) with compositional formula BaTi{sub 1-x}Fe{sub x}O{sub 3} (x = 0, 0.03, 0.04 and 0.05) were prepared by solid-state reaction route. The influence of the Fe content on the structural, vibrational and electric properties of BaTiO{sub 3} was investigated using X-ray powder diffraction (XRD), Raman spectroscopy and Polarization techniques. XRD analysis indicates the formation of single-phase tetragonal structure for all the prepared samples. Tetragonal cubic structure with space group P4mm of all samples is further approved by Rietveld refinement. Room temperature Raman spectra of pure BaTiO{sub 3} show four active modes ofmore » vibration whose intensity decreases with increasing Fe doping. Small shift in Raman modes and increment in the line width has been observed with the doping ions. The hysteresis loop is very well performed with regular sharp characteristic of ferroelectric materials.« less

Self-consistent modeling of CFETR baseline scenarios for steady-state operation

NASA Astrophysics Data System (ADS)

Chen, Jiale; Jian, Xiang; Chan, Vincent S.; Li, Zeyu; Deng, Zhao; Li, Guoqiang; Guo, Wenfeng; Shi, Nan; Chen, Xi; CFETR Physics Team

2017-07-01

Integrated modeling for core plasma is performed to increase confidence in the proposed baseline scenario in the 0D analysis for the China Fusion Engineering Test Reactor (CFETR). The steady-state scenarios are obtained through the consistent iterative calculation of equilibrium, transport, auxiliary heating and current drives (H&CD). Three combinations of H&CD schemes (NB + EC, NB + EC + LH, and EC + LH) are used to sustain the scenarios with q min > 2 and fusion power of ˜70-150 MW. The predicted power is within the target range for CFETR Phase I, although the confinement based on physics models is lower than that assumed in 0D analysis. Ideal MHD stability analysis shows that the scenarios are stable against n = 1-10 ideal modes, where n is the toroidal mode number. Optimization of RF current drive for the RF-only scenario is also presented. The simulation workflow for core plasma in this work provides a solid basis for a more extensive research and development effort for the physics design of CFETR.

Combining cationic and anionic mixed-mode sorbents in a single cartridge to extract basic and acidic pharmaceuticals simultaneously from environmental waters.

PubMed

Salas, Daniela; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa Maria

2018-01-01

The aim of the present study is to broaden the applications of mixed-mode ion-exchange solid-phase extraction sorbents to extract both basic and acidic compounds simultaneously by combining the sorbents in a single cartridge and developing a simplified extraction procedure. Four different cartridges containing negative and positive charges in the same configuration were evaluated and compared to extract a group of basic, neutral, and acidic pharmaceuticals selected as model compounds. After a thorough optimization of the extraction conditions, the four different cartridges showed to be capable of retaining basic and acidic pharmaceuticals simultaneously through ionic interactions, allowing the introduction of a washing step with 15 mL methanol to eliminate interferences retained by hydrophobic interactions. Using the best combined cartridge, a method was developed, validated, and further applied to environmental waters to demonstrate that the method is promising for the extraction of basic and acidic compounds from very complex samples.

Surface-enhanced Raman spectroscopy of hexabenzobenzene, C24H12, an analogue of a graphene nanostructure

NASA Astrophysics Data System (ADS)

Owens, Frank J.

2018-05-01

While large scale fabrication of graphene nanoribbons remains a challenge, there exist materials which can be fabricated in quantities such as hexabenzobenzene,HBZB, (C24H12) and which have a two-dimensional (2D) carbon structure similar to graphene nanostructures. Using a 632 nm laser, no Raman spectra could be obtained from the solid material because of a strong luminescence produced by the laser. However, surface-enhanced Raman spectroscopy enabled the measurement of some of the Raman active modes. The G and D modes, which are characteristic fingerprints of a 2D graphene structure, were observed at 1331 and 1600 cm-1, respectively. Density functional theory at the B3LYP/6-31G* level was used to calculate the minimum energy structure and the Raman active vibrational frequencies of HBZB. The calculated minimum energy structure was 2D having D6h symmetry in agreement with the experimental structure in the liquid phase. The calculated frequencies were in good agreement with the measured values.

Polarizing Ytterbium-Doped all-Solid Photonic Bandgap Fiber with 1150 micrometers2 Effective Mode Area

DTIC Science & Technology

2015-02-11

RESPONSIBLE PERSON 19b. TELEPHONE NUMBER Liang Dong Fanting Kong,, Guancheng Gu,, Thomas W. Hawkins ,, Joshua Parsons, Maxwell Jones,, Christopher...Dunn,, Monica T. Kalichevsky-Dong,, Benjamin Pulford,, Iyad Dajani,, Kunimasa Saitoh,, Stephen P. Palese,, Eric Cheung,, Liang Dong c. THIS PAGE The...ytterbium-doped all-solid photonic bandgap fiber with ~1150µm2 effective mode area Fanting Kong,1,* Guancheng Gu,1 Thomas W. Hawkins ,1 Joshua Parsons

Cladding for transverse-pumped solid-state laser

NASA Technical Reports Server (NTRS)

Byer, Robert L. (Inventor); Fan, Tso Y. (Inventor)

1989-01-01

In a transverse pumped, solid state laser, a nonabsorptive cladding surrounds a gain medium. A single tranverse mode, namely the Transverse Electromagnetic (TEM) sub 00 mode, is provided. The TEM sub 00 model has a cross sectional diameter greater than a transverse dimension of the gain medium but less than a transverse dimension of the cladding. The required size of the gain medium is minimized while a threshold for laser output is lowered.

Investigation of Super Tube Structure and Performance (Postprint)

DTIC Science & Technology

2010-04-01

thermosyphon is claimed as thermally superconductive and offers solid state mode of heat transport. A host of speculations about this claim was emerging...sealed structure and design of a conventional heat pipe or thermosyphon is claimed as thermally superconductive and offers solid state mode of heat...matrix. The tilt angle was varied to check for gravity dependence. Tests were run as step functions allowing the tube to reach steady state at a new

Interferometric space-mode multiplexing based on binary phase plates and refractive phase shifters.

PubMed

Liñares, Jesús; Prieto-Blanco, Xesús; Moreno, Vicente; Montero-Orille, Carlos; Mouriz, Dolores; Nistal, María C; Barral, David

2017-05-15

A Mach-Zehnder interferometer (MZI) that includes in an arm either a reflective image inverter or a Gouy phase shifter (RGPS) can (de)multiplex many types of modes of a few mode fiber without fundamental loss. The use of RGPSs in combination with binary phase plates for multiplexing purposes is studied for the first time, showing that the particular RGPS that shifts π the odd modes only multiplexes accurately low order modes. To overcome such a restriction, we present a new exact refractive image inverter, more compact and flexible than its reflective counterpart. Moreover, we show that these interferometers remove or reduce the crosstalk that the binary phase plates could introduce between the multiplexed modes. Finally, an experimental analysis of a MZI with both an approximated and an exact refractive image inverter is presented for the case of a bimodal multiplexing. Likewise, it is proven experimentally that a RGPS that shifts π/2 demultiplexes two odd modes which can not be achieved by any image inverter.

Recent Application of Solid Phase Based Techniques for Extraction and Preconcentration of Cyanotoxins in Environmental Matrices.

PubMed

Mashile, Geaneth Pertunia; Nomngongo, Philiswa N

2017-03-04

Cyanotoxins are toxic and are found in eutrophic, municipal, and residential water supplies. For this reason, their occurrence in drinking water systems has become a global concern. Therefore, monitoring, control, risk assessment, and prevention of these contaminants in the environmental bodies are important subjects associated with public health. Thus, rapid, sensitive, selective, simple, and accurate analytical methods for the identification and determination of cyanotoxins are required. In this paper, the sampling methodologies and applications of solid phase-based sample preparation methods for the determination of cyanotoxins in environmental matrices are reviewed. The sample preparation techniques mainly include solid phase micro-extraction (SPME), solid phase extraction (SPE), and solid phase adsorption toxin tracking technology (SPATT). In addition, advantages and disadvantages and future prospects of these methods have been discussed.

Effect of Internal Pressure and Temperature on Phase Transitions in Perovskite Oxides: The Case of the Solid Oxide Fuel Cell Cathode Materials of the La2-xSrxCoTiO6 Series.

PubMed

Gómez-Pérez, Alejandro; Hoelzel, Markus; Muñoz-Noval, Álvaro; García-Alvarado, Flaviano; Amador, Ulises

2016-12-19

The symmetry of the room-temperature (RT) structure of title compounds La 2-x Sr x CoTiO 6-δ changes with x, from P2 1 /n (0 ≤ x ≤ 0.2) to Pnma (0.3 ≤ x ≤ 0.5) and to R3̅c (0.6 ≤ x ≤ 1). For x = 1 the three pseudocubic cell parameters become very close suggesting a transition to a cubic structure for higher Sr contents. Similar phase transitions were expected to occur on heating, paralleling the effect of internal pressure induced by substitution of La 3+ by Sr 2+ . However, only some of these aforementioned transitions have been thermally induced. The symmetry-adapted modes formalism is used in the structural refinements and fitting of neutron diffraction data recorded from RT to 1273 K. Thus, for x = 1, the out-of-phase tilting of the BO 6 octahedra vanishes progressively on heating, and a cubic structure with Pm3̅m symmetry is found at 1073 K. For lower Sr contents this transition is predicted to occur far above the temperature limit of common experimental setups. The analysis of the evolution of the perovskite tolerance factor, t-factor, with both Sr content and temperature indicates that temperature has a limited ability to release structural stress and thus to enable transitions to more symmetric phases. This is particularly true when compared to the effect of internal pressure induced by substitution of La by Sr. The existence of phase transitions in materials for solid oxide fuel cells that are usually exposed to heating-cooling cycles may have a detrimental effect. This work suggests strategies to stabilize the high-symmetry high-temperature phase of perovskite oxides through internal-pressure chemically induced.

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.

Solid-solution CrCoCuFeNi high-entropy alloy thin films synthesized by sputter deposition

DOE PAGES

An, Zhinan; Jia, Haoling; Wu, Yueying; ...

2015-05-04

The concept of high configurational entropy requires that the high-entropy alloys (HEAs) yield single-phase solid solutions. However, phase separations are quite common in bulk HEAs. A five-element alloy, CrCoCuFeNi, was deposited via radio frequency magnetron sputtering and confirmed to be a single-phase solid solution through the high-energy synchrotron X-ray diffraction, energy-dispersive spectroscopy, wavelength-dispersive spectroscopy, and transmission electron microscopy. The formation of the solid-solution phase is presumed to be due to the high cooling rate of the sputter-deposition process.