The influence of microscopic and macroscopic non-stoichiometry on interfacial planarity during the solid-phase epitaxial growth of amorphized GaAs

Energy Technology Data Exchange (ETDEWEB)

Belay, K.B.; Ridgway, M.C.; Llewellyn, D.J. [Australian National Univ., Canberra, ACT (Australia). Dept. of Physics

1996-12-31

The influence of microscopic and macroscopic non-stoichiometry on the Solid-Phase Epitaxial Growth of GaAs has been studied. Ion implantation has been employed to produce microscopic non-stoichiometry via Ga and As implants and macroscopic non-stoichiometry via Ga or As implants. In-situ Time Resolved Reflectivity and Transmission Electron Microscopy and ex-situ Rutherford Backscattering Spectroscopy and Channeling have been used to investigate the regrowth of amorphized GaAs layers. As non-stoichiometry shifts from microscopic to macroscopic the interface loses its planar nature and subsequently gets rougher. 7 refs., 3 figs.

The influence of microscopic and macroscopic non-stoichiometry on interfacial planarity during the solid-phase epitaxial growth of amorphized GaAs

Energy Technology Data Exchange (ETDEWEB)

Belay, K B; Ridgway, M C; Llewellyn, D J [Australian National Univ., Canberra, ACT (Australia). Dept. of Physics

1997-12-31

The influence of microscopic and macroscopic non-stoichiometry on the Solid-Phase Epitaxial Growth of GaAs has been studied. Ion implantation has been employed to produce microscopic non-stoichiometry via Ga and As implants and macroscopic non-stoichiometry via Ga or As implants. In-situ Time Resolved Reflectivity and Transmission Electron Microscopy and ex-situ Rutherford Backscattering Spectroscopy and Channeling have been used to investigate the regrowth of amorphized GaAs layers. As non-stoichiometry shifts from microscopic to macroscopic the interface loses its planar nature and subsequently gets rougher. 7 refs., 3 figs.

The kinetics of solid phase epitaxy in As-doped buried amorphous silicon layers

International Nuclear Information System (INIS)

McCallum, J.C.

1999-01-01

Ion implantation is the principal method used to introduce dopants into silicon for fabrication of semiconductor devices. During ion implantation, damage accumulates in the crystalline silicon lattice and amorphisation may occur over the depth range of the ions if the implant dose is sufficiently high. As device dimensions shrink, the need to produce shallower and shallower highly-doped layers increases and the probability of amorphisation also increases. To achieve dopant-activation, the amorphous or damaged material must be returned to the crystalline state by thermal annealing. Amorphous silicon layers can be crystallised by the solid-state process of solid phase epitaxy (SPE) in which the amorphous layer transforms to crystalline silicon (c-Si) layer by layer using the underlying c-Si as a seed. The atomic mechanism that is responsible for the crystallisation is thought to involve highly-localised bond-breaking and rearrangement processes at the amorphous/crystalline (a/c) interface but the defect responsible for these bond rearrangements has not yet been identified. Since the bond breaking process necessarily generates dangling bonds, it has been suggested that the crystallisation process may solely involve the formation and migration of dangling bonds at the interface. One of the key factors which may shed further light on the nature of the SPE defect is the observed dopant-dependence of the rate of crystallisation. It has been found that moderate concentrations of dopants enhance the SPE crystallisation rate while the presence of equal concentrations of an n-type and a p-type dopant (impurity compensation) returns the SPE rate to the intrinsic value. This provides crucial evidence that the SPE mechanism is sensitive to the position of the Fermi level in the bandgap of the crystalline and/or the amorphous silicon phases and may lead to identification of an energy level within the bandgap that can be associated with the defect. This paper gives details of SPE

A Simple Approach to Characterize Gas-Aqueous Liquid Two-phase Flow Configuration Based on Discrete Solid-Liquid Contact Electrification.

Science.gov (United States)

Choi, Dongwhi; Lee, Donghyeon; Kim, Dong Sung

2015-10-14

In this study, we first suggest a simple approach to characterize configuration of gas-aqueous liquid two-phase flow based on discrete solid-liquid contact electrification, which is a newly defined concept as a sequential process of solid-liquid contact and successive detachment of the contact liquid from the solid surface. This approach exhibits several advantages such as simple operation, precise measurement, and cost-effectiveness. By using electric potential that is spontaneously generated by discrete solid-liquid contact electrification, the configurations of the gas-aqueous liquid two-phase flow such as size of a gas slug and flow rate are precisely characterized. According to the experimental and numerical analyses on parameters that affect electric potential, gas slugs have been verified to behave similarly to point electric charges when the measuring point of the electric potential is far enough from the gas slug. In addition, the configuration of the gas-aqueous liquid two-phase microfluidic system with multiple gas slugs is also characterized by using the presented approach. For a proof-of-concept demonstration of using the proposed approach in a self-triggered sensor, a gas slug detector with a counter system is developed to show its practicality and applicability.

Taylor flow hydrodynamics in gas-liquid-solid micro reactors

NARCIS (Netherlands)

Warnier, M.J.F.

2009-01-01

Chemical reactions in which a gas phase component reacts with a liquid phase omponent at the surface of a solid catalyst are often encountered in chemical industry. The rate of such a gas-liquid-solid reaction is often limited by the mass transfer rate of the gas phase component, which depends on

Multiple Multidentate Halogen Bonding in Solution, in the Solid State, and in the (Calculated) Gas Phase.

Science.gov (United States)

Jungbauer, Stefan H; Schindler, Severin; Herdtweck, Eberhardt; Keller, Sandro; Huber, Stefan M

2015-09-21

The binding properties of neutral halogen-bond donors (XB donors) bearing two multidentate Lewis acidic motifs toward halides were investigated. Employing polyfluorinated and polyiodinated terphenyl and quaterphenyl derivatives as anion receptors, we obtained X-ray crystallographic data of the adducts of three structurally related XB donors with tetraalkylammonium chloride, bromide, and iodide. The stability of these XB complexes in solution was determined by isothermal titration calorimetry (ITC), and the results were compared to X-ray analyses as well as to calculated binding patterns in the gas phase. Density functional theory (DFT) calculations on the gas-phase complexes indicated that the experimentally observed distortion of the XB donors during multiple multidentate binding can be reproduced in 1:1 complexes with halides, whereas adducts with two halides show a symmetric binding pattern in the gas phase that is markedly different from the solid state structures. Overall, this study demonstrates the limitations in the transferability of binding data between solid state, solution, and gas phase in the study of complex multidentate XB donors. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Iodine removal from a gas phase

International Nuclear Information System (INIS)

Vikis, A. Ch.

1982-01-01

Iodine, e.g. radioactive iodine, present as one or more organic iodides, optionally with elemental iodine, in a gas phase (e.g. air) are removed by photochemically decomposing the organic iodides to elemental iodine, reacting the iodine produced, and any initially present with excess ozone, preferably photochemically produced in situ in the gas phase to produce solid iodine oxides, and removing the solid oxides from the gas phase. (author)

Iodine removal from a gas phase

International Nuclear Information System (INIS)

Vikis, A.C.

1984-01-01

Iodine, e.g. radioactive iodine, present as one or more organic iodides, optionally with elemental iodine, in a gas phase (e.g. air) are removed by photochemically decomposing the organic iodides to elemental iodine, reacting the iodine produced, and any initially present with excess ozone, preferably photochemically produced in situ in the gas phase to produce solid iodine oxides, and removing the solid oxides from the gas phase

Organometallic vapor-phase epitaxy theory and practice

CERN Document Server

Stringfellow, Gerald B

1989-01-01

Here is one of the first single-author treatments of organometallic vapor-phase epitaxy (OMVPE)--a leading technique for the fabrication of semiconductor materials and devices. Also included are metal-organic molecular-beam epitaxy (MOMBE) and chemical-beam epitaxy (CBE) ultra-high-vacuum deposition techniques using organometallic source molecules. Of interest to researchers, students, and people in the semiconductor industry, this book provides a basic foundation for understanding the technique and the application of OMVPE for the growth of both III-V and II-VI semiconductor materials and the

Solid phase epitaxial growth of high mobility La:BaSnO_3 thin films co-doped with interstitial hydrogen

International Nuclear Information System (INIS)

Niedermeier, Christian A.; Rhode, Sneha; Fearn, Sarah; Moram, Michelle A.; Ide, Keisuke; Hiramatsu, Hidenori; Hosono, Hideo; Kamiya, Toshio

2016-01-01

This work presents the solid phase epitaxial growth of high mobility La:BaSnO_3 thin films on SrTiO_3 single crystal substrates by crystallization through thermal annealing of nanocrystalline thin films prepared by pulsed laser deposition at room temperature. The La:BaSnO_3 thin films show high epitaxial quality and Hall mobilities up to 26 ± 1 cm"2/Vs. Secondary ion mass spectroscopy is used to determine the La concentration profile in the La:BaSnO_3 thin films, and a 9%–16% La doping activation efficiency is obtained. An investigation of H doping to BaSnO_3 thin films is presented employing H plasma treatment at room temperature. Carrier concentrations in previously insulating BaSnO_3 thin films were increased to 3 × 10"1"9" cm"−"3 and in La:BaSnO_3 thin films from 6 × 10"1"9" cm"−"3 to 1.5 × 10"2"0" cm"−"3, supporting a theoretical prediction that interstitial H serves as an excellent n-type dopant. An analysis of the free electron absorption by infrared spectroscopy yields a small (H,La):BaSnO_3 electron effective mass of 0.27 ± 0.05 m_0 and an optical mobility of 26 ± 7 cm"2/Vs. As compared to La:BaSnO_3 single crystals, the smaller electron mobility in epitaxial thin films grown on SrTiO_3 substrates is ascribed to threading dislocations as observed in high resolution transmission electron micrographs.

The liquid phase epitaxy approach for the successful construction of ultra-thin and defect-free ZIF-8 membranes: Pure and mixed gas transport study

KAUST Repository

Shekhah, Osama; Swaidan, Raja; Belmabkhout, Youssef; Du Plessis, Marike; Jacobs, Tia; Barbour, Leonard J.; Pinnau, Ingo; Eddaoudi, Mohamed

2014-01-01

The liquid-phase epitaxy (LPE) method was effectively implemented to deliberately grow/construct ultrathin (0.5-1 μm) continuous and defect-free ZIF-8 membranes. Permeation properties of different gas pair systems (O 2-N2, H2-CO2, CO2-CH 4, C3H6-C3H8, CH 4-n-C4H10) were studied using the time lag technique. This journal is © The Royal Society of Chemistry.

Comprehensive modeling of solid phase epitaxial growth using Lattice Kinetic Monte Carlo

International Nuclear Information System (INIS)

Martin-Bragado, Ignacio

2013-01-01

Damage evolution of irradiated silicon is, and has been, a topic of interest for the last decades for its applications to the semiconductor industry. In particular, sometimes, the damage is heavy enough to collapse the lattice and to locally amorphize the silicon, while in other cases amorphization is introduced explicitly to improve other implanted profiles. Subsequent annealing of the implanted samples heals the amorphized regions through Solid Phase Epitaxial Regrowth (SPER). SPER is a complicated process. It is anisotropic, it generates defects in the recrystallized silicon, it has a different amorphous/crystalline (A/C) roughness for each orientation, leaving pits in Si(1 1 0), and in Si(1 1 1) it produces two modes of recrystallization with different rates. The recently developed code MMonCa has been used to introduce a physically-based comprehensive model using Lattice Kinetic Monte Carlo that explains all the above singularities of silicon SPER. The model operates by having, as building blocks, the silicon lattice microconfigurations and their four twins. It detects the local configurations, assigns microscopical growth rates, and reconstructs the positions of the lattice locally with one of those building blocks. The overall results reproduce the (a) anisotropy as a result of the different growth rates, (b) localization of SPER induced defects, (c) roughness trends of the A/C interface, (d) pits on Si(1 1 0) regrown surfaces, and (e) bimodal Si(1 1 1) growth. It also provides physical insights of the nature and shape of deposited defects and how they assist in the occurrence of all the above effects

Epitaxial growth and new phase of single crystal Dy by molecular beam epitaxy

International Nuclear Information System (INIS)

Yang, Kai-Yueh; Homma, Hitoshi; Schuller, I.K.

1987-09-01

We have grown two novel epitaxial phases of dysprosium (Dy) on vanadium (V) by molecular beam epitaxy technique. Surface and bulk structures are studied by in-situ reflection high energy electron diffraction (RHEED) and x-ray diffraction techniques. The new hcp phases are ∼4% expanded uniformly in-plane (0001), and ∼9% and ∼4% expanded out of plane along the c-axes for non-interrupted and interrupted deposition case, respectively. We also observed (2 x 2), (3 x 3), and (4 x 4) Dy surface reconstruction patterns and a series of transitions as the Dy film thickness increases. 12 refs., 3 figs

Strain relaxation during solid-phase epitaxial crystallisation of Ge{sub x}Si{sub 1-x} alloy layers with depth dependent G{sub e} compositions

Energy Technology Data Exchange (ETDEWEB)

Wong, Wahchung; Elliman, R.G.; Kringhoj, P. [Australian National Univ., Canberra, ACT (Australia). Research School of Physical Sciences

1993-12-31

The solid-phase epitaxial crystallisation of depth dependent Ge{sub x}Si{sub lx} alloy layers produced by implanting Ge into Si substrates was studied. In-situ monitoring was done using time-resolved reflectivity (TRR) whilst post-anneal defect structures were characterised by Rutherford backscattering and channeling spectrometry (RBS-C) and transmission electron microscopy (TEM). Particular attention was directed at Ge concentrations above the critical concentration for the growth of fully strained layers. Strain relief is shown to be correlated with a sudden reduction in crystallisation velocity caused by roughening of the crystalline/amorphous interface. 11 refs., 1 tab., 2 figs.

Strain relaxation during solid-phase epitaxial crystallisation of Ge{sub x}Si{sub 1-x} alloy layers with depth dependent G{sub e} compositions

Energy Technology Data Exchange (ETDEWEB)

Wong, Wahchung; Elliman, R G; Kringhoj, P [Australian National Univ., Canberra, ACT (Australia). Research School of Physical Sciences

1994-12-31

The solid-phase epitaxial crystallisation of depth dependent Ge{sub x}Si{sub lx} alloy layers produced by implanting Ge into Si substrates was studied. In-situ monitoring was done using time-resolved reflectivity (TRR) whilst post-anneal defect structures were characterised by Rutherford backscattering and channeling spectrometry (RBS-C) and transmission electron microscopy (TEM). Particular attention was directed at Ge concentrations above the critical concentration for the growth of fully strained layers. Strain relief is shown to be correlated with a sudden reduction in crystallisation velocity caused by roughening of the crystalline/amorphous interface. 11 refs., 1 tab., 2 figs.

Critical comparison of hydrodynamic models for gas-solid fluidized beds - Part II: freely bubbling gas-solid fluidized beds

NARCIS (Netherlands)

Patil, D.J.; van Sint Annaland, M.; Kuipers, J.A.M.

2005-01-01

Correct prediction of spontaneous bubble formation in freely bubbling gas¿solid fluidized beds using Eulerian models, strongly depends on the description of the internal momentum transfer in the particulate phase. In this part, the comparison of the simple classical model, describing the solid phase

Effect of gas flow on the selective area growth of gallium nitride via metal organic vapor phase epitaxy

Science.gov (United States)

Rodak, L. E.; Kasarla, K. R.; Korakakis, D.

2007-08-01

The effect of gas flow on the selective area growth (SAG) of gallium nitride (GaN) grown via metal organic vapor phase epitaxy (MOVPE) has been investigated. In this study, the SAG of GaN was carried out on a silicon dioxide striped pattern along the GaN direction. SAG was initiated with the striped pattern oriented parallel and normal to the incoming gas flow in a horizontal reactor. The orientation of the pattern did not impact cross section of the structure after re-growth as both orientations resulted in similar trapezoidal structures bounded by the (0 0 0 1) and {1 1 2¯ n} facets ( n≈1.7-2.2). However, the growth rates were shown to depend on the orientation of the pattern as the normally oriented samples exhibited enhanced vertical and cross-sectional growth rates compared to the parallel oriented samples. All growths occurred under identical conditions and therefore the difference in growth rates must be attributed to a difference in mass transport of species.

Epitaxial III-V nanowires on silicon for vertical devices

NARCIS (Netherlands)

Bakkers, E.P.A.M.; Borgström, M.T.; Einden, Van Den W.; Weert, van M.H.M.; Helman, A.; Verheijen, M.A.

2006-01-01

We show the epitaxial integration of III-V semiconductor nanowires with silicon technology. The wires are grown by the Vapor-Liquid-Solid (VLS) mechanism with laser ablation as well as metal organic vapor phase epitaxy. The VLS growth enables the fabrication of complex axial and radial

The complete information for phenomenal distributed parameter control of multicomponent chemical processes in gas, fluid and solid phase

International Nuclear Information System (INIS)

Niemiec, W.

1985-01-01

A constitutive mathematical model of distributed parameters of multicomponent chemical processes in gas, fluid and solid phase is utilized to the realization of phenomenal distributed parameter control of these processes. Original systems of partial differential constitutive state equations, in the following derivative forms /I/, /II/ and /III/ are solved in this paper from the point of view of information for phenomenal distributed parameter control of considered processes. Obtained in this way for multicomponent chemical processes in gas, fluid and solid phase: -dynamical working space-time characteristics/analytical solutions in working space-time of chemical reactors/, -dynamical phenomenal Green functions as working space-time transfer functions, -statical working space characteristics /analytical solutions in working space of chemical reactors/, -statical phenomenal Green functions as working space transfer functions, are applied, as information for realization of constitutive distributed parameter control of mass, energy and momentum aspects of above processes. Two cases are considered by existence of: A/sup o/ - initial conditions, B/sup o/ - initial and boundary conditions, for multicomponent chemical processes in gas, fluid and solid phase

Operando Spectroscopy of the Gas-Phase Aldol Condensation of Propanal over Solid Base Catalysts

NARCIS (Netherlands)

Hernández-giménez, Ana M.; Ruiz-martínez, Javier; Puértolas, Begoña; Pérez-ramírez, Javier; Bruijnincx, Pieter C. A.; Weckhuysen, Bert M.

2017-01-01

The gas-phase aldol condensation of propanal, taken as model for the aldehyde components in bio-oils, has been studied with a combined operando set-up allowing to perform FT-IR & UV–Vis diffuse reflectance spectroscopy (DRS) with on-line mass spectrometry (MS). The selected solid base catalysts, a

Laser-induced carbon plasma emission spectroscopic measurements on solid targets and in gas-phase optical breakdown

International Nuclear Information System (INIS)

Nemes, Laszlo; Keszler, Anna M.; Hornkohl, James O.; Parigger, Christian

2005-01-01

We report measurements of time- and spatially averaged spontaneous-emission spectra following laser-induced breakdown on a solid graphite/ambient gas interface and on solid graphite in vacuum, and also emission spectra from gas-phase optical breakdown in allene C3H4 and helium, and in CO2 and helium mixtures. These emission spectra were dominated by CII (singly ionized carbon), CIII (doubly ionized carbon), hydrogen Balmer beta (H b eta), and Swan C2 band features. Using the local thermodynamic equilibrium and thin plasma assumptions, we derived electron number density and electron temperature estimates. The former was in the 1016 cm -3 range, while the latter was found to be near 20000 K. In addition, the vibration-rotation temperature of the Swan bands of the C2 radical was determined to be between 4500 and 7000 K, using an exact theoretical model for simulating diatomic emission spectra. This temperature range is probably caused by the spatial inhomogeneity of the laser-induced plasma plume. Differences are pointed out in the role of ambient CO2 in a solid graphite target and in gas-phase breakdown plasma

Epitaxial growth and characterization of CuGa2O4 films by laser molecular beam epitaxy

OpenAIRE

Hongling Wei; Zhengwei Chen; Zhenping Wu; Wei Cui; Yuanqi Huang; Weihua Tang

2017-01-01

Ga2O3 with a wide bandgap of ∼ 4.9 eV can crystalize in five crystalline phases. Among those phases, the most stable monoclinic β-Ga2O3 has been studied most, however, it is hard to find materials lattice matching with β-Ga2O3 to grown epitaxial thin films for optoelectronic applications. In this work, CuGa2O4 bulk were prepared by solid state reaction as target, and the films were deposited on sapphire substrates by laser molecular beam epitaxy (L-MBE) at different substrate temperatures. Th...

Mass transfer between gas and particles in a gas-solid trickle flow reactor

NARCIS (Netherlands)

Kiel, J.H.A.; Kiel, J.H.A.; Prins, W.; van Swaaij, Willibrordus Petrus Maria

1992-01-01

Gas-solids mass transfer was studied for counter-current flow of gas and millimetre-sized solid particles over an inert packing at dilute phase or trickle flow conditions. Experimental data were obtained from the adsorption of water vapour on 640 and 2200 ¿m diameter molecular sieve spheres at

Valorization of Calcium Carbonate-Based Solid Wastes for the Treatment of Hydrogen Sulfide from the Gas Phase

OpenAIRE

Pham Xuan , Huynh; Pham Minh , Doan; Galera Martinez , Marta; Nzihou , Ange; Sharrock , Patrick

2015-01-01

International audience; This paper focuses on the valorization of calcium carbonate-based solid wastes for theremoval of hydrogen sulfide from gas phase. Two solid wastes taken from industrial sites for theproduction of sodium carbonate and sodium bicarbonate by the Solvay process® were analyzedby different physico-chemical methods. Calcium carbonate was found as the main component ofboth the solid wastes. Trace amounts of other elements such as Mg, Al, Fe, Si, Cl, Na etc. werealso present in...

Dislocations limited electronic transport in hydride vapour phase epitaxy grown GaN templates: A word of caution for the epitaxial growers

Energy Technology Data Exchange (ETDEWEB)

Chatterjee, Abhishek, E-mail: cabhishek@rrcat.gov.in; Khamari, Shailesh K.; Kumar, R.; Dixit, V. K.; Oak, S. M.; Sharma, T. K., E-mail: tarun@rrcat.gov.in [Semiconductor Physics and Devices Laboratory, Raja Ramanna Centre for Advanced Technology, Indore 452013 (India)

2015-01-12

GaN templates grown by hydride vapour phase epitaxy (HVPE) and metal organic vapour phase epitaxy (MOVPE) techniques are compared through electronic transport measurements. Carrier concentration measured by Hall technique is about two orders larger than the values estimated by capacitance voltage method for HVPE templates. It is learnt that there exists a critical thickness of HVPE templates below which the transport properties of epitaxial layers grown on top of them are going to be severely limited by the density of charged dislocations lying at layer-substrate interface. On the contrary MOVPE grown templates are found to be free from such limitations.

Epitaxial lift-off for solid-state cavity quantum electrodynamics

International Nuclear Information System (INIS)

Greuter, Lukas; Najer, Daniel; Kuhlmann, Andreas V.; Starosielec, Sebastian; Warburton, Richard J.; Valentin, Sascha R.; Ludwig, Arne; Wieck, Andreas D.

2015-01-01

We demonstrate an approach to incorporate self-assembled quantum dots into a Fabry-Pérot-like microcavity. Thereby, a 3λ/4 GaAs layer containing quantum dots is epitaxially removed and attached by van der Waals bonding to one of the microcavity mirrors. We reach a finesse as high as 4100 with this configuration limited by the reflectivity of the dielectric mirrors and not by scattering at the semiconductor-mirror interface, demonstrating that the epitaxial lift-off procedure is a promising procedure for cavity quantum electrodynamics in the solid state. As a first step in this direction, we demonstrate a clear cavity-quantum dot interaction in the weak coupling regime with a Purcell factor in the order of 3. Estimations of the coupling strength via the Purcell factor suggest that we are close to the strong coupling regime

Lead-germanium ohmic contact on to gallium arsenide formed by the solid phase epitaxy of germanium: A microstructure study

Science.gov (United States)

Radulescu, Fabian

2000-12-01

Driven by the remarkable growth in the telecommunication market, the demand for more complex GaAs circuitry continued to increase in the last decade. As a result, the GaAs industry is faced with new challenges in its efforts to fabricate devices with smaller dimensions that would permit higher integration levels. One of the limiting factors is the ohmic contact metallurgy of the metal semiconductor field effect transistor (MESFET), which, during annealing, induces a high degree of lateral diffusion into the substrate. Because of its limited reaction with the substrate, the Pd-Ge contact seems to be the most promising candidate to be used in the next generation of MESFET's. The Pd-Ge system belongs to a new class of ohmic contacts to compound semiconductors, part of an alloying strategy developed only recently, which relies on solid phase epitaxy (SPE) and solid phase regrowth to "un-pin" the Fermi level at the surface of the compound semiconductor. However, implementing this alloy into an integrated process flow proved to be difficult due to our incomplete understanding of the microstructure evolution during annealing and its implications on the electrical properties of the contact. The microstructure evolution and the corresponding solid state reactions that take place during annealing of the Pd-Ge thin films on to GaAs were studied in connection with their effects on the electrical properties of the ohmic contact. The phase transformations sequence, transition temperatures and activation energies were determined by combining differential scanning calorimetry (DSC) for thermal analysis with transmission electron microscopy (TEM) for microstructure identification. In-situ TEM annealing experiments on the Pd/Ge/Pd/GaAs ohmic contact system have permitted real time determination of the evolution of contact microstructure. The kinetics of the solid state reactions, which occur during ohmic contact formation, were determined by measuring the grain growth rates

Surface functionalization of epitaxial graphene on SiC by ion irradiation for gas sensing application

Energy Technology Data Exchange (ETDEWEB)

Kaushik, Priya Darshni, E-mail: kaushik.priyadarshni@gmail.com [Department of Physics, Chemistry and Biology, Linköping University, SE-58183 Linköping (Sweden); Department of Physics, Jamia Millia Islamia, New Delhi, 110025 (India); Ivanov, Ivan G.; Lin, Pin-Cheng [Department of Physics, Chemistry and Biology, Linköping University, SE-58183 Linköping (Sweden); Kaur, Gurpreet [Department of Physics and Astrophysics, University of Delhi, Delhi, 110007 (India); Eriksson, Jens [Department of Physics, Chemistry and Biology, Linköping University, SE-58183 Linköping (Sweden); Lakshmi, G.B.V.S. [Inter-University Accelerator Centre, Aruna Asaf Ali Marg, New Delhi, 110067 (India); Avasthi, D.K. [Inter-University Accelerator Centre, Aruna Asaf Ali Marg, New Delhi, 110067 (India); Amity Institute of Nanotechnology, Noida 201313 (India); Gupta, Vinay [Department of Physics and Astrophysics, University of Delhi, Delhi, 110007 (India); Aziz, Anver; Siddiqui, Azher M. [Department of Physics, Jamia Millia Islamia, New Delhi, 110025 (India); Syväjärvi, Mikael [Department of Physics, Chemistry and Biology, Linköping University, SE-58183 Linköping (Sweden); Yazdi, G. Reza, E-mail: yazdi@ifm.liu.se [Department of Physics, Chemistry and Biology, Linköping University, SE-58183 Linköping (Sweden)

2017-05-01

Highlights: • For the first time the gas sensing application of SHI irradiated epitaxial graphene on SiC is explored. • Surface morphology of irradiated graphene layers showed graphene folding, hillocks, and formation of wrinkles. • Existence of an optimal fluence which maximize the gas sensing response towards NO{sub 2} and NH{sub 3} gases. - Abstract: In this work, surface functionalization of epitaxial graphene grown on silicon carbide was performed by ion irradiation to investigate their gas sensing capabilities. Swift heavy ion irradiation using 100 MeV silver ions at four varying fluences was implemented on epitaxial graphene to investigate morphological and structural changes and their effects on the gas sensing capabilities of graphene. Sensing devices are expected as one of the first electronic applications using graphene and most of them use functionalized surfaces to tailor a certain function. In our case, we have studied irradiation as a tool to achieve functionalization. Morphological and structural changes on epitaxial graphene layers were investigated by atomic force microscopy, Raman spectroscopy, Raman mapping and reflectance mapping. The surface morphology of irradiated graphene layers showed graphene folding, hillocks, and formation of wrinkles at highest fluence (2 × 10{sup 13} ions/cm{sup 2}). Raman spectra analysis shows that the graphene defect density is increased with increasing fluence, while Raman mapping and reflectance mapping show that there is also a reduction of monolayer graphene coverage. The samples were investigated for ammonia and nitrogen dioxide gas sensing applications. Sensors fabricated on pristine and irradiated samples showed highest gas sensing response at an optimal fluence. Our work provides new pathways for introducing defects in controlled manner in epitaxial graphene, which can be used not only for gas sensing application but also for other applications, such as electrochemical, biosensing, magnetosensing and

Surface functionalization of epitaxial graphene on SiC by ion irradiation for gas sensing application

International Nuclear Information System (INIS)

Kaushik, Priya Darshni; Ivanov, Ivan G.; Lin, Pin-Cheng; Kaur, Gurpreet; Eriksson, Jens; Lakshmi, G.B.V.S.; Avasthi, D.K.; Gupta, Vinay; Aziz, Anver; Siddiqui, Azher M.; Syväjärvi, Mikael; Yazdi, G. Reza

2017-01-01

Highlights: • For the first time the gas sensing application of SHI irradiated epitaxial graphene on SiC is explored. • Surface morphology of irradiated graphene layers showed graphene folding, hillocks, and formation of wrinkles. • Existence of an optimal fluence which maximize the gas sensing response towards NO_2 and NH_3 gases. - Abstract: In this work, surface functionalization of epitaxial graphene grown on silicon carbide was performed by ion irradiation to investigate their gas sensing capabilities. Swift heavy ion irradiation using 100 MeV silver ions at four varying fluences was implemented on epitaxial graphene to investigate morphological and structural changes and their effects on the gas sensing capabilities of graphene. Sensing devices are expected as one of the first electronic applications using graphene and most of them use functionalized surfaces to tailor a certain function. In our case, we have studied irradiation as a tool to achieve functionalization. Morphological and structural changes on epitaxial graphene layers were investigated by atomic force microscopy, Raman spectroscopy, Raman mapping and reflectance mapping. The surface morphology of irradiated graphene layers showed graphene folding, hillocks, and formation of wrinkles at highest fluence (2 × 10"1"3 ions/cm"2). Raman spectra analysis shows that the graphene defect density is increased with increasing fluence, while Raman mapping and reflectance mapping show that there is also a reduction of monolayer graphene coverage. The samples were investigated for ammonia and nitrogen dioxide gas sensing applications. Sensors fabricated on pristine and irradiated samples showed highest gas sensing response at an optimal fluence. Our work provides new pathways for introducing defects in controlled manner in epitaxial graphene, which can be used not only for gas sensing application but also for other applications, such as electrochemical, biosensing, magnetosensing and spintronic

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

Directory of Open Access Journals (Sweden)

Naseva Olivera S.

2002-01-01

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

Derivatisation/solid-phase microextraction followed by gas chromatography-mass spectrometry for the analysis of phenoxy acid herbicides in aqueous samples

DEFF Research Database (Denmark)

Nilsson, Torben; Baglio, Daniela; Galdo-Miguez, Isabel

1998-01-01

Different combinations of derivatisation and solid-phase microextraction followed by gas chromatography-mass spectrometry were optimised and evaluated for the analysis of phenoxy acid herbicides in water. The most successful derivatisation approach was aqueous-phase derivatisation with benzyl...

Set-Up and Validation of a Dynamic Solid/Gas Bioreactor

KAUST Repository

Lloyd-Randol, Jennifer D.

2012-05-01

The limited availability of fossil resourses mandates the development of new energy vectors, which is one of the Grand Challenges of the 21st Century [1]. Biocatalytic energy conversion is a promising solution to meet the increased energy demand of industrialized societies. Applications of biocatalysis in the gas-phase are so far limited to production of fine chemicals and pharmaceuticals. However, this technology has the potential for large scale biocatalytic applications [2], e.g. for the formation of novel energy carriers. The so-called solid/gas biocatalysis is defined as the application of a biocatalyst immobilized on solid-phase support acting on gaseous substrates [3]. This process combines the advantages of bio-catalysis (green chemistry, mild reaction conditions, high specicity & selectivity) and heterogeneous dynamic gas-phase processes (low diffusion limitation, high conversion, simple scale-up). This work presents the modifications of a PID Microactivity Reference reactor in order to make it suitable for solid/gas biocatalysis. The reactor design requirements are based on previously published laboratory scale solid/gas systems with a feed of saturated vapors [4]. These vapors are produced in saturation flasks, which were designed and optimized during this project. Other modifications included relocation of the gas mixing chamber, redesigning the location and heating mechanism for the reactor tube, and heating of the outlet gas line. The modified reactor system was verified based on the Candida antarctica lipase B catalyzed transesterication of ethyl acetate with 1-hexanol to hexyl acetate and ethanol and results were compared to liquid-phase model reactions. Products were analyzed on line by a gas chromatograph with a flame ionization detector. C. antarc- tica physisorbed on silica particles produced a 50% conversion of hexanol at 40 C in the gas-phase. A commercial immobilized lipase from Iris Biotech produced 99% and 97% conversions of hexanol in

Silica, alumina and aluminosilicates as solid stationary phases in gas chromatography

Directory of Open Access Journals (Sweden)

S. Faramawy

2016-09-01

Full Text Available Silica, alumina and Aluminosilicates of different Si/Al ratios were prepared by conventional precipitation or co-precipitation methods and then subjected to thermal treatment at 800 °C. The parent and thermally treated materials were characterized by means of FTIR, SEM and thermal analysis (DTA and TGA in order to elucidate the main structural properties. Surface textural characteristics were investigated by means of nitrogen adsorption–desorption isotherms at −196 °C. Pore size distribution curves indicated the presence of mesopores (10–150 Å exhibiting maxima at 35 Å. The maxima were shifted toward higher values by increasing the alumina content. Thermodynamic parameters, ΔH, ΔG and ΔS, were determined by means of inverse gas chromatography using n-hexane as a probe. The untreated and thermally treated materials were tested as solid stationary phases in gas chromatography. The separation efficiency of various non polar and polar compounds was explained in terms of surface texture and thermodynamic parameters.

Pseudomorphic growth of organic semiconductor thin films driven by incommensurate epitaxy

International Nuclear Information System (INIS)

Sassella, A.; Campione, M.; Raimondo, L.; Borghesi, A.; Bussetti, G.; Cirilli, S.; Violante, A.; Goletti, C.; Chiaradia, P.

2009-01-01

A stable pseudomorphic phase of α-quaterthiophene, a well known organic semiconductor, is obtained by growing films with organic molecular beam epitaxy (OMBE) on a single crystal of another organic semiconductor, namely, tetracene. The structural characteristics of the new phase are investigated by monitoring in situ the OMBE process by reflectance anisotropy spectroscopy; thus assessing that incommensurate epitaxy is in this case, the driving force for tuning the molecular packing in organic molecular films and in turn, their solid state properties

Digital image processing based mass flow rate measurement of gas/solid two-phase flow

Energy Technology Data Exchange (ETDEWEB)

Song Ding; Peng Lihui; Lu Geng; Yang Shiyuan [Tsinghua National Laboratory for Information Science and Technology, Department of Automation, Tsinghua University, Beijing, 100084 (China); Yan Yong, E-mail: lihuipeng@tsinghua.edu.c [University of Kent, Canterbury, Kent CT2 7NT (United Kingdom)

2009-02-01

With the rapid growth of the process industry, pneumatic conveying as a tool for the transportation of a wide variety of pulverized and granular materials has become widespread. In order to improve plant control and operational efficiency, it is essential to know the parameters of the particle flow. This paper presents a digital imaging based method which is capable of measuring multiple flow parameters, including volumetric concentration, velocity and mass flow rate of particles in the gas/solid two phase flow. The measurement system consists of a solid state laser for illumination, a low-cost CCD camera for particle image acquisition and a microcomputer with bespoke software for particle image processing. The measurements of particle velocity and volumetric concentration share the same sensing hardware but use different exposure time and different image processing methods. By controlling the exposure time of the camera a clear image and a motion blurred image are obtained respectively. The clear image is thresholded by OTSU method to identify the particles from the dark background so that the volumetric concentration is determined by calculating the ratio between the particle area and the total area. Particle velocity is derived from the motion blur length, which is estimated from the motion blurred images by using the travelling wave equation method. The mass flow rate of particles is calculated by combining the particle velocity and volumetric concentration. Simulation and experiment results indicate that the proposed method is promising for the measurement of multiple parameters of gas/solid two-phase flow.

Digital image processing based mass flow rate measurement of gas/solid two-phase flow

International Nuclear Information System (INIS)

Song Ding; Peng Lihui; Lu Geng; Yang Shiyuan; Yan Yong

2009-01-01

With the rapid growth of the process industry, pneumatic conveying as a tool for the transportation of a wide variety of pulverized and granular materials has become widespread. In order to improve plant control and operational efficiency, it is essential to know the parameters of the particle flow. This paper presents a digital imaging based method which is capable of measuring multiple flow parameters, including volumetric concentration, velocity and mass flow rate of particles in the gas/solid two phase flow. The measurement system consists of a solid state laser for illumination, a low-cost CCD camera for particle image acquisition and a microcomputer with bespoke software for particle image processing. The measurements of particle velocity and volumetric concentration share the same sensing hardware but use different exposure time and different image processing methods. By controlling the exposure time of the camera a clear image and a motion blurred image are obtained respectively. The clear image is thresholded by OTSU method to identify the particles from the dark background so that the volumetric concentration is determined by calculating the ratio between the particle area and the total area. Particle velocity is derived from the motion blur length, which is estimated from the motion blurred images by using the travelling wave equation method. The mass flow rate of particles is calculated by combining the particle velocity and volumetric concentration. Simulation and experiment results indicate that the proposed method is promising for the measurement of multiple parameters of gas/solid two-phase flow.

Numerical simulation of gas-solid two-phase flow in U-beam separator

International Nuclear Information System (INIS)

Zhou, X Y; Chen, X P; Dou, H S; Zhang, H Z; Ruan, J M

2015-01-01

Numerical simulation is carried out for gas-solid two-phase flow in a U-beam separator. In this study, the U-beam is altered with the inlet fins in order to improve the performance of the separator. The inlet fin angle of the separator are 30°, 35°, 40°, 45°, 50°, 55 ° and 60°. The governing equations are the Reynolds-Averaged Navier-Stokes equation with the standard k-ε model and the discrete phase model (DPM) describing the discrete two - phase flow as well as stochastic tracking model. Results show that the pressure drop deviation with fins is within 3% from those without fins. It is found that there is a maximum separation efficiency at the fin angle of 35°. Fin induces generation of a stagnation region which could collect particles and lead to change of vortical structures. The fin induced flow also causes the turbulent intensity inside the baffle to decrease to facilitate separation

Structural evolution of epitaxial SrCoOx films near topotactic phase transition

OpenAIRE

Hyoungjeen Jeen; Ho Nyung Lee

2015-01-01

Control of oxygen stoichiometry in complex oxides via topotactic phase transition is an interesting avenue to not only modifying the physical properties, but utilizing in many energy technologies, such as energy storage and catalysts. However, detailed structural evolution in the close proximity of the topotactic phase transition in multivalent oxides has not been much studied. In this work, we used strontium cobaltites (SrCoOx) epitaxially grown by pulsed laser epitaxy (PLE) as a model syste...

Vapor phase epitaxial growth of FeS sub 2 pyrite and evaluation of the carrier collection in liquid-junction solar cell

Energy Technology Data Exchange (ETDEWEB)

Ennaoui, A.; Schlichthoerl, G.; Fiechter, S.; Tributsch, H. (Hahn-Meitner-Inst., Abt. Solare Energetik und Materialforschung, Berlin (Germany))

1992-01-01

Photoactive epitaxial layers of FeS{sub 2} were grown using bromine as a transport agent and a simple closed ampoule technique. The substrates used were (100)-oriented slices of natural pyrite 1 mm thick. A vapor-liquid-solid (VLS) growth mechanism was elucidated by means of optical microscopy. Macrosteps, terrace surfaces and protuberances are often accompanied with the presence of liquid FeBr{sub 3} droplets. In the absence of a liquid phase growth hillocks are found. Localized photovoltaic response for the evaluation of carrier collection using a scanning laser spot system has been used to effectively locate and characterize non-uniformities present in the epitaxial thin films. (orig.).

Growth of pseudomorphic structures through organic epitaxy

International Nuclear Information System (INIS)

Kaviyil, Sreejith Embekkat; Sassella, Adele; Borghesi, Alessandro; Campione, Marcello; Su Genbo; He Youping; Chen Chenjia

2012-01-01

The control of molecular orientation in thin solid film phases of organic semiconductors is a basic factor for the exploitation of their physical properties for optoelectronic devices. We compare structural and optical properties of thin films of the organic semiconductor α-quarterthiophene grown by molecular beam epitaxy on different organic substrates. We show how epitactic interactions, characteristic of the surface of organic crystals, can drive the orientation of the crystalline overlayer and the selection of specific polymorphs and new pseudomorphic phases. We identify a key role in this phenomenon played by the marked groove-like corrugations present in some organic crystal surfaces. Since different polymorphs possess rather different performance in terms of, e.g., charge carrier mobility, this strategy is demonstrated to allow for the growth of oriented phases with enhanced physical properties, while keeping the substrate at room temperature. These results provide useful guidelines for the design of technological substrates for organic epitaxy and they substantiate the adoption of an organic epitaxy approach for the fabrication of optoelectronic devices based on thin films of organic semiconductors.

Determination of volatile compounds in grape distillates by solid-phase extraction and gas chromatography.

Science.gov (United States)

Lukić, Igor; Banović, Mara; Persurić, Dordano; Radeka, Sanja; Sladonja, Barbara

2006-01-06

Solid-phase extraction (SPE) procedure on octadecylsilica (C18) was developed for accumulation of volatile compounds from grape distillates. The procedure was optimised for final analysis by capillary gas chromatography. At mass concentrations in model solutions ranging from 0.1 to 50 mg/l solid-phase extraction recoveries of all analytes ranged from 69% for 2-phenylethanol to 102% for capric acid, with RSD values from 2 to 9%. SPE recoveries of internal standards to be added in the sample solution prior to extraction, higher alcohols 2-ethyl-1-hexanol and 1-undecanol, were 97 and 93%, respectively, with RSD values of 3%. Detection limits of analyzed compounds in model solutions ranged from 0.011 mg/l for isoamyl acetate to 0.037 mg/l for caproic acid. Method efficiency was tested in relation to acetic acid content, volume fraction of ethanol and possible matrix effects. A significant influence of matrix on SPE efficiency for geraniol, cis-2-hexen-1-ol and cis-3-hexen-1-ol was detected. For the same reason, 2-phenylethanol could not be determined by developed SPE method in samples of grape distillates. The developed solid-phase extraction method was successfully applied to determine the differences in volatile compound content in different grape distillates produced by the distillation of crushed, pressed and fermented grapes.

Direct solid-phase microextraction combined with gas and liquid chromatography for the determination of lidocaine in human urine

NARCIS (Netherlands)

Koster, E.H M; Hofman, N.S K; de Jong, G.J.

Solid-phase microextraction (SPME) has been combined with gas chromatography (GC) and liquid chromatography (LC) for the determination of lidocaine in human urine. A polydimethylsiloxane (PDMS) coated fibre was directly immersed into buffered urine. Extraction conditions such as time, pH, ionic

The mechanism of reequilibration of solids in the presence of a fluid phase

International Nuclear Information System (INIS)

Putnis, Andrew; Putnis, Christine V.

2007-01-01

The preservation of morphology (pseudomorphism) and crystal structure during the transformation of one solid phase to another is regularly used as a criterion for a solid-state mechanism, even when there is a fluid phase present. However, a coupled dissolution-reprecipitation mechanism also preserves the morphology and transfers crystallographic information from parent to product by epitaxial nucleation. The generation of porosity in the product phase is a necessary condition for such a mechanism as it allows fluid to maintain contact with a reaction interface which moves through the parent phase from the original surface. We propose that interface-coupled dissolution-reprecipitation is a general mechanism for reequilibration of solids in the presence of a fluid phase. - Graphical abstract: A single crystal of KBr is transformed to a porous single crystal of KCl by immersion in saturated KCl solution. The image shows partial transformation of a crystal of KBr (core) to KCl (porous, milky rim) by an interface coupled dissolution-reprecipitation mechanism. The external dimensions and crystallographic orientation of the original crystal are preserved, while a reaction interface moves through the crystal

New phenomena in epitaxial growth: solid films on quasicrystalline substrates

International Nuclear Information System (INIS)

Fournee, V; Thiel, P A

2005-01-01

An overview is given of the research conducted in the field of solid film growth on quasiperiodic surfaces. An atomistic description of quasicrystalline surfaces is presented and discussed in relation to bulk structural models. The various systems for which thin film growth has been attempted so far are reviewed. Emphasis is placed on the nucleation mechanisms of the solid films, on their growth modes in relation to the nature of the deposited metals, on the possibility of intermixing or alloying at the interface and on the epitaxial relationships at the crystal-quasicrystal interfaces. We also describe situations where the deposited elements adopt a quasiperiodic structure, which opens up the possibility of extending our understanding of the relation between quasiperiodicity and the physical properties of such structurally and chemically complex solids. (topical review)

Zirconia-based solid state chemical gas sensors

CERN Document Server

Zhuiykov, S

2000-01-01

This paper presents an overview of chemical gas sensors, based on solid state technology, that are sensitive to environmental gases, such as O sub 2 , SO sub x , NO sub x , CO sub 2 and hydrocarbons. The paper is focussed on performance of electrochemical gas sensors that are based on zirconia as a solid electrolyte. The paper considers sensor structures and selection of electrode materials. Impact of interfaces on sensor performance is discussed. This paper also provides a brief overview of electrochemical properties of zirconia and their effect on sensor performance. Impact of auxiliary materials on sensors performance characteristics, such as sensitivity, selectivity, response time and recovery time, is also discussed. Dual gas sensors that can be applied for simultaneous monitoring of the concentration of both oxygen and other gas phase components, are briefly considered

Abstracts of 4. International Workshop on Molecular Beam Epitaxy and Vapour Phase Epitaxy Growth Physics and Technology

International Nuclear Information System (INIS)

2001-01-01

4. International Workshop on Molecular Beam Epitaxy and Vapour Phase Epitaxy Growth Physics and Technology is the periodically held forum for discussion the problems connected with manufacturing of different nanostructures (thin films, quantum wells, quantum dots) needed in microelectronics. Preparation of such materials with desirable optical, electrical and magnetic properties being determined by their chemical composition and crystal structure has been discussed in detail during the workshop sessions. Optimization of crystal growth methods such as VPE and MBE from the view point of obtained material properties has also been extensively discussed

solid phase extraction method for selective determination

African Journals Online (AJOL)

FATOKI

determination of phthalate ester plasticizers in rivers and marine water samples. Of the ... samples that receive effluent from industries that use phthalate esters. ... Keywords Phthalates, Plasticizers, Solid Phase Gas Chromatography.

Surface phase transitions in cu-based solid solutions

Science.gov (United States)

Zhevnenko, S. N.; Chernyshikhin, S. V.

2017-11-01

We have measured surface energy in two-component Cu-based systems in H2 + Ar gas atmosphere. The experiments on solid Cu [Ag] and Cu [Co] solutions show presence of phase transitions on the surfaces. Isotherms of the surface energy have singularities (the minimum in the case of copper solid solutions with silver and the maximum in the case of solid solutions with cobalt). In both cases, the surface phase transitions cause deficiency of surface miscibility: formation of a monolayer (multilayer) (Cu-Ag) or of nanoscale particles (Cu-Co). At the same time, according to the volume phase diagrams, the concentration and temperature of the surface phase transitions correspond to the solid solution within the volume. The method permits determining the rate of diffusional creep in addition to the surface energy. The temperature and concentration dependence of the solid solutions' viscosity coefficient supports the fact of the surface phase transitions and provides insights into the diffusion properties of the transforming surfaces.

Data correlation in on-line solid-phase extraction-gas chromatography-atomic emission/mass spectrometric detection of unknown microcontaminants

NARCIS (Netherlands)

Hankemeier, Th.; Rozenbrand, J.; Abhadur, M.; Vreuls, J.J.; Brinkman, U.A.Th.

1998-01-01

A procedure is described for the (non-target) screening of hetero-atom-containing compounds in tap and waste water by correlating data obtained by gas chromatography (GC) using atomic emission (AED) and mass selective (MS) detection. Solid-phase extraction (SPE) was coupled on-line to both GC

Heterogeneous Two-Phase Pillars in Epitaxial NiFe ₂ O ₄ -LaFeO ₃ Nanocomposites

Energy Technology Data Exchange (ETDEWEB)

Comes, Ryan B. [Physical and Computational Sciences Directorate, Pacific Northwest National Laboratory, Richland WA 99352 USA; Department of Physics, Auburn University, Auburn AL 36849 USA; Perea, Daniel E. [Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, Richland WA 99352 USA; Spurgeon, Steven R. [Physical and Computational Sciences Directorate, Pacific Northwest National Laboratory, Richland WA 99352 USA

2017-07-10

Self-assembled epitaxial oxide nanocomposites have been explored for a wide range of applications, including multiferroic and magnetoelectric properties, plasmonics, and catalysis. These so-called “vertically aligned nanocomposites” form spontaneously during the deposition process when segregation into two phases is energetically favorable as compared to a solid solution. However, there has been surprisingly little work understanding the driving forces that govern the synthesis of these materials, which can include point defect energetics, surface diffusion, and interfacial energies. To explore these factors, La-Ni-Fe-O films have been synthesized by molecular beam epitaxy and it is shown that these phase segregate into spinel-perovskite nanocomposites. Using complementary scanning transmission electron microscopy and atom-probe tomography, the elemental composition of each phase is examined and found that Ni ions are exclusively found in the spinel phase. From correlative analysis, a model for the relative favorability of the Ni2+ and Ni3+ valences under the growth conditions is developed. It is shown that multidimensional characterization techniques provide previously unobserved insight into the growth process and complex driving forces for phase segregation.

Abnormal gas-liquid-solid phase transition behaviour of water observed with in situ environmental SEM.

Science.gov (United States)

Chen, Xin; Shu, Jiapei; Chen, Qing

2017-04-24

Gas-liquid-solid phase transition behaviour of water is studied with environmental scanning electron microscopy for the first time. Abnormal phenomena are observed. At a fixed pressure of 450 Pa, with the temperature set to -7 °C, direct desublimation happens, and ice grows continuously along the substrate surface. At 550 Pa, although ice is the stable phase according to the phase diagram, metastable liquid droplets first nucleate and grow to ~100-200 μm sizes. Ice crystals nucleate within the large sized droplets, grow up and fill up the droplets. Later, the ice crystals grow continuously through desublimation. At 600 Pa, the metastable liquid grows quickly, with some ice nuclei floating in it, and the liquid-solid coexistence state exists for a long time. By lowering the vapour pressure and/or increasing the substrate temperature, ice sublimates into vapour phase, and especially, the remaining ice forms a porous structure due to preferential sublimation in the concave regions, which can be explained with surface tension effect. Interestingly, although it should be forbidden for ice to transform into liquid phase when the temperature is well below 0 °C, liquid like droplets form during the ice sublimation process, which is attributed to the surface tension effect and the quasiliquid layers.

An integration scheme for stiff solid-gas reactor models

Directory of Open Access Journals (Sweden)

Bjarne A. Foss

2001-04-01

Full Text Available Many dynamic models encounter numerical integration problems because of a large span in the dynamic modes. In this paper we develop a numerical integration scheme for systems that include a gas phase, and solid and liquid phases, such as a gas-solid reactor. The method is based on neglecting fast dynamic modes and exploiting the structure of the algebraic equations. The integration method is suitable for a large class of industrially relevant systems. The methodology has proven remarkably efficient. It has in practice performed excellent and been a key factor for the success of the industrial simulator for electrochemical furnaces for ferro-alloy production.

Growth kinetics and mass transport mechanisms of GaN columns by selective area metal organic vapor phase epitaxy

Science.gov (United States)

Wang, Xue; Hartmann, Jana; Mandl, Martin; Sadat Mohajerani, Matin; Wehmann, Hergo-H.; Strassburg, Martin; Waag, Andreas

2014-04-01

Three-dimensional GaN columns recently have attracted a lot of attention as the potential basis for core-shell light emitting diodes for future solid state lighting. In this study, the fundamental insights into growth kinetics and mass transport mechanisms of N-polar GaN columns during selective area metal organic vapor phase epitaxy on patterned SiOx/sapphire templates are systematically investigated using various pitch of apertures, growth time, and silane flow. Species impingement fluxes on the top surface of columns Jtop and on their sidewall Jsw, as well as, the diffusion flux from the substrate Jsub contribute to the growth of the GaN columns. The vertical and lateral growth rates devoted by Jtop, Jsw and Jsub are estimated quantitatively. The diffusion length of species on the SiOx mask surface λsub as well as on the sidewall surfaces of the 3D columns λsw are determined. The influences of silane on the growth kinetics are discussed. A growth model is developed for this selective area metal organic vapor phase epitaxy processing.

Metal organic vapor phase epitaxy growth of (Al)GaN heterostructures on SiC/Si(111) templates synthesized by topochemical method of atoms substitution

DEFF Research Database (Denmark)

Rozhavskaya, Mariia M.; Kukushkin, Sergey A.; Osipov, Andrey V.

2017-01-01

We report a novel approach for metal organic vapor phase epitaxy of (Al)GaN heterostructures on Si substrates. An approximately 90–100 nm thick SiC buffer layer is synthesized using the reaction between Si substrate and CO gas. Highresolution transmission electron microscopy reveals sharp...

Stability analysis of unsaturated soil slope during rainfall infiltration using coupled liquid-gas-solid three-phase model

Directory of Open Access Journals (Sweden)

Dong-mei Sun

2016-07-01

Full Text Available Generally, most soil slope failures are induced by rainfall infiltration, a process that involves interactions between the liquid phase, gas phase, and solid skeleton in an unsaturated soil slope. In this study, a loosely coupled liquid-gas-solid three-phase model, linking two numerical codes, TOUGH2/EOS3, which is used for water-air two-phase flow analysis, and FLAC3D, which is used for mechanical analysis, was established. The model was validated through a documented water drainage experiment over a sandy column and a comparison of the results with measured data and simulated results from other researchers. The proposed model was used to investigate the features of water-air two-phase flow and stress fields in an unsaturated soil slope during rainfall infiltration. The slope stability analysis was then performed based on the simulated water-air two-phase seepage and stress fields on a given slip surface. The results show that the safety factor for the given slip surface decreases first, then increases, and later decreases until the rainfall stops. Subsequently, a sudden rise occurs. After that, the safety factor decreases continually and reaches its lowest value, and then increases slowly to a steady value. The lowest value does not occur when the rainfall stops, indicating a delayed effect of the safety factor. The variations of the safety factor for the given slip surface are therefore caused by a combination of pore-air pressure, matric suction, normal stress, and net normal stress.

Ultra-Shallow P+/N Junction Formation in Si Using Low Temperature Solid Phase Epitaxy Assisted with Laser Activation

International Nuclear Information System (INIS)

Hara, Shuhei; Tanaka, Yuki; Fukaya, Takumi; Matsumoto, Satoru; Suzuki, Toshiharu; Fuse, Genshu; Kudo, Toshio; Sakuragi, Susumu

2008-01-01

A combination of Ge pre-amorphization implantation (Ge-PAI), low-energy B implantation and laser annealing is a promising method to form highly-activated, abrupt and ultra-shallow junctions (USJ). In our previous report of IIT 2006, we succeeded in forming pn junctions less than 10 nm using non-melt double-pulsed green laser. However, a large leakage current under reverse bias was observed consequently due to residual defects in the implanted layer. In this study, a method to form USJ is proposed: a combination of low-temperature solid phase epitaxy and non-melt laser irradiation for B activation. Ge pre-amorphization implantation was performed at energy of 6 keV with a dose of 3x10 14 /cm 2 . Then B implantation was performed at energy of 0.2 keV with a dose of 1.2x10 15 /cm 2 . Samples were annealed at 400 deg. C for 10 h in nitrogen atmosphere. Subsequently, non-melt laser irradiation was performed at energy of 690 mJ/cm 2 and pulse duration of 100 ns with intervals of 300 ns. As a result, USJ around 10 nm with better crystallinity was successfully formed. And the leakage current of pn diodes was reduced significantly. Moreover, it is proven from secondary ion mass spectroscopy (SIMS) analysis that transient enhanced diffusion (TED) of B is specifically suppressed.

Modelling of non-catalytic reactors in a gas-solid trickle flow reactor: Dry, regenerative flue gas desulphurization using a silica-supported copper oxide sorbent

NARCIS (Netherlands)

Kiel, J.H.A.; Kiel, J.H.A.; Prins, W.; van Swaaij, Willibrordus Petrus Maria

1992-01-01

A one-dimensional, two-phase dispersed plug flow model has been developed to describe the steady-state performance of a relatively new type of reactor, the gas-solid trickle flow reactor (GSTFR). In this reactor, an upward-flowing gas phase is contacted with as downward-flowing dilute solids phase

Vapor-solid-solid grown Ge nanowires at integrated circuit compatible temperature by molecular beam epitaxy

Science.gov (United States)

Zhu, Zhongyunshen; Song, Yuxin; Zhang, Zhenpu; Sun, Hao; Han, Yi; Li, Yaoyao; Zhang, Liyao; Xue, Zhongying; Di, Zengfeng; Wang, Shumin

2017-09-01

We demonstrate Au-assisted vapor-solid-solid (VSS) growth of Ge nanowires (NWs) by molecular beam epitaxy at the substrate temperature of ˜180 °C, which is compatible with the temperature window for Si-based integrated circuit. Low temperature grown Ge NWs hold a smaller size, similar uniformity, and better fit with Au tips in diameter, in contrast to Ge NWs grown at around or above the eutectic temperature of Au-Ge alloy in the vapor-liquid-solid (VLS) growth. Six ⟨110⟩ growth orientations were observed on Ge (110) by the VSS growth at ˜180 °C, differing from only one vertical growth direction of Ge NWs by the VLS growth at a high temperature. The evolution of NWs dimension and morphology from the VLS growth to the VSS growth is qualitatively explained by analyzing the mechanism of the two growth modes.

Simulation of granular and gas-solid flows using discrete element method

Science.gov (United States)

Boyalakuntla, Dhanunjay S.

2003-10-01

In recent years there has been increased research activity in the experimental and numerical study of gas-solid flows. Flows of this type have numerous applications in the energy, pharmaceuticals, and chemicals process industries. Typical applications include pulverized coal combustion, flow and heat transfer in bubbling and circulating fluidized beds, hopper and chute flows, pneumatic transport of pharmaceutical powders and pellets, and many more. The present work addresses the study of gas-solid flows using computational fluid dynamics (CFD) techniques and discrete element simulation methods (DES) combined. Many previous studies of coupled gas-solid flows have been performed assuming the solid phase as a continuum with averaged properties and treating the gas-solid flow as constituting of interpenetrating continua. Instead, in the present work, the gas phase flow is simulated using continuum theory and the solid phase flow is simulated using DES. DES treats each solid particle individually, thus accounting for its dynamics due to particle-particle interactions, particle-wall interactions as well as fluid drag and buoyancy. The present work involves developing efficient DES methods for dense granular flow and coupling this simulation to continuum simulations of the gas phase flow. Simulations have been performed to observe pure granular behavior in vibrating beds. Benchmark cases have been simulated and the results obtained match the published literature. The dimensionless acceleration amplitude and the bed height are the parameters governing bed behavior. Various interesting behaviors such as heaping, round and cusp surface standing waves, as well as kinks, have been observed for different values of the acceleration amplitude for a given bed height. Furthermore, binary granular mixtures (granular mixtures with two particle sizes) in a vibrated bed have also been studied. Gas-solid flow simulations have been performed to study fluidized beds. Benchmark 2D

Solid phase radioimmunoassays

International Nuclear Information System (INIS)

Wide, L.

1977-01-01

Solid phase coupled antibodies were introduced to facilitate the separation of bound and free labelled ligand in the competitive inhibition radioimmunoassay. Originally, the solid matrix used was in the form of small particles and since then a number of different matrices have been used such as very fine powder particles, gels, paper and plastic discs, magnetic particles and the inside surface of plastic tubes. The coupling of antibodies may be that of a covalent chemical binding, a strong physical adsorbtion, or an immunological binding to a solid phase coupled antigen. New principles of radioimmunoassay such as the solid phase sandwich techniques and the immunoradiometric assay were developped from the use of solid phase coupled antigens and antibodies. The solid phase sandwich techniques are reagent excess methods with a very wide applicability. Several of the different variants of solid phase techniques are suitable for automation. Advantages and disadvantages of solid phase radioimmunoassays when compared with those using soluble reagents are discussed. (orig.) [de

Effect of extrapolation length on the phase transformation of epitaxial ferroelectric thin films

International Nuclear Information System (INIS)

Hu, Z.S.; Tang, M.H.; Wang, J.B.; Zheng, X.J.; Zhou, Y.C.

2008-01-01

Effects of extrapolation length on the phase transformation of epitaxial ferroelectric thin films on dissimilar cubic substrates have been studied on the basis of the mean-field Landau-Ginzburg-Devonshire (LGD) thermodynamic theory by taking an uneven distribution of the interior stress with thickness into account. It was found that the polarization of epitaxial ferroelectric thin films is strongly dependent on the extrapolation length of films. The physical origin of the extrapolation length during the phase transformation from paraelectric to ferroelectric was revealed in the case of ferroelectric thin films

Numerical Simulation of Gas-Solid Two-Phase Flow for Four-Channels Pulverized Swirling Burner

Directory of Open Access Journals (Sweden)

Defu LI

2013-05-01

Full Text Available This article presents a mathematical model of cold gas-solid two-phase flow which is based on the cement rotary kiln in service. By altering the parameters of air supply system of four- channels pulverized burner, investigations are taken of that motion trajectory and particle distributions in the very turbulent field. The results show that motion trail of most particles in rotary kiln is a combination process of gradual diffusion and slow sedimentation; increasing internal flow velocity would aggravate coal particles to diffuse; external flow velocity should be controlled in a reasonable range.

Thermodynamics of gas adsorption on solid adsorbents

International Nuclear Information System (INIS)

Budrugeac, P.

1979-01-01

Starting with several hypotheses about the adsorbtion system and the adsorption phenomenon, a thermodynamic treatment of gas adsorption on solid adsorbants is presented. The relationships for determination from isotherms and calorimetric data of thermodynamic functions are derived. The problem of the phase changes in adsorbed layer is discussed. (author)

Biogasification of solid wastes by two-phase anaerobic fermentation

International Nuclear Information System (INIS)

Ghosh, S.; Vieitez, E.R.; Liu, T.; Kato, Y.

1997-01-01

Municipal, industrial and agricultural solid wastes, and biomass deposits, cause large-scale pollution of land and water. Gaseous products of waste decomposition pollute the air and contribute to global warming. This paper describes the development of a two-phase fermentation system that alleviates methanogenic inhibition encountered with high-solids feed, accelerates methane fermentation of the solid bed, and captures methane (renewable energy) for captive use to reduce global warming. The innovative system consisted of a solid bed reactor packed with simulated solid waste at a density of 160 kg/m 3 and operated with recirculation of the percolated culture (bioleachate) through the bed. A rapid onset of solids hydrolysis, acidification, denitrification and hydrogen gas formation was observed under these operating conditions. However, these fermentative reactions stopped at a total fatty acids concentration of 13,000 mg/l (as acetic) at pH 5, with a reactor head-gas composition of 75 percent carbon dioxide, 20 percent nitrogen, 2 percent hydrogen and 3 percent methane. Fermentation inhibition was alleviated by moving the bioleachate to a separate methane-phase fermenter, and recycling methanogenic effluents at pH 7 to the solid bed. Coupled operation of the two reactors promoted methanogenic conversion of the high-solids feed. (author)

Modelling of interactions between variable mass and density solid particles and swirling gas stream

International Nuclear Information System (INIS)

Wardach-Święcicka, I; Kardaś, D; Pozorski, J

2011-01-01

The aim of this work is to investigate the solid particles - gas interactions. For this purpose, numerical modelling was carried out by means of a commercial code for simulations of two-phase dispersed flows with the in-house models accounting for mass and density change of solid phase. In the studied case the particles are treated as spherical moving grains carried by a swirling stream of hot gases. Due to the heat and mass transfer between gas and solid phase, the particles are losing their mass and they are changing their volume. Numerical simulations were performed for turbulent regime, using two methods for turbulence modelling: RANS and LES.

Molecular beam epitaxy of GeTe-Sb2Te3 phase change materials studied by X-ray diffraction

International Nuclear Information System (INIS)

Shayduk, Roman

2010-01-01

The integration of phase change materials into semiconductor heterostructures may lead to the development of a new generation of high density non-volatile phase change memories. Epitaxial phase change materials allow to study the detailed structural changes during the phase transition and to determine the scaling limits of the memory. This work is dedicated to the epitaxial growth of Ge-Sb-Te phase change alloys on GaSb(001). We deposit Ge-Sb-Te (GST) films on GaSb(001) substrates by means of molecular beam epitaxy (MBE). The film orientation and lattice constant evolution is determined in real time during growth using grazing incidence X-ray diffraction (GID). The nucleation stage of the growth is studied in situ using reflection high energy electron diffraction (RHEED). Four growth regimes of GST on GaSb(001) were observed: amorphous, polycrystalline, incubated epitaxial and direct epitaxial. Amorphous film grows for substrate temperatures below 100 C. For substrate temperatures in the range 100-160 C, the film grows in polycrystalline form. Incubated epitaxial growth is observed at temperatures from 180 to 210 C. This growth regime is characterized by an initial 0.6nm thick amorphous layer formation, which crystallizes epitaxially as the film thickness increases. The determined lattice constant of the films is 6.01 A, very close to that of the metastable GST phase. The films predominantly possess an epitaxial cube-on-cube relationship. At higher temperatures the films grow epitaxially, however the growth rate is rapidly decreasing with temperature. At temperatures above 270 C the growth rate is zero. The composition of the grown films is close to 2:2:5 for Ge, Sb and Te, respectively. The determined crystal structure of the films is face centered cubic (FCC) with a rhombohedral distortion. The analysis of X-ray peak widths gives a value for the rhombohedral angle of 89.56 . We observe two types of reflections in reciprocal space indicating two FCC sublattices in

Structural evolution of epitaxial SrCoOx films near topotactic phase transition

Science.gov (United States)

Jeen, Hyoungjeen; Lee, Ho Nyung

2015-12-01

Control of oxygen stoichiometry in complex oxides via topotactic phase transition is an interesting avenue to not only modifying the physical properties, but utilizing in many energy technologies, such as energy storage and catalysts. However, detailed structural evolution in the close proximity of the topotactic phase transition in multivalent oxides has not been much studied. In this work, we used strontium cobaltites (SrCoOx) epitaxially grown by pulsed laser epitaxy (PLE) as a model system to study the oxidation-driven evolution of the structure, electronic, and magnetic properties. We grew coherently strained SrCoO2.5 thin films and performed post-annealing at various temperatures for topotactic conversion into the perovskite phase (SrCoO3-δ). We clearly observed significant changes in electronic transport, magnetism, and microstructure near the critical temperature for the topotactic transformation from the brownmillerite to the perovskite phase. Nevertheless, the overall crystallinity was well maintained without much structural degradation, indicating that topotactic phase control can be a useful tool to control the physical properties repeatedly via redox reactions.

Structural evolution of epitaxial SrCoOx films near topotactic phase transition

Directory of Open Access Journals (Sweden)

Hyoungjeen Jeen

2015-12-01

Full Text Available Control of oxygen stoichiometry in complex oxides via topotactic phase transition is an interesting avenue to not only modifying the physical properties, but utilizing in many energy technologies, such as energy storage and catalysts. However, detailed structural evolution in the close proximity of the topotactic phase transition in multivalent oxides has not been much studied. In this work, we used strontium cobaltites (SrCoOx epitaxially grown by pulsed laser epitaxy (PLE as a model system to study the oxidation-driven evolution of the structure, electronic, and magnetic properties. We grew coherently strained SrCoO2.5 thin films and performed post-annealing at various temperatures for topotactic conversion into the perovskite phase (SrCoO3-δ. We clearly observed significant changes in electronic transport, magnetism, and microstructure near the critical temperature for the topotactic transformation from the brownmillerite to the perovskite phase. Nevertheless, the overall crystallinity was well maintained without much structural degradation, indicating that topotactic phase control can be a useful tool to control the physical properties repeatedly via redox reactions.

Epitaxial growth of Ge-Sb-Te based phase change materials

International Nuclear Information System (INIS)

Perumal, Karthick

2013-01-01

Ge-Sb-Te based phase change materials are considered as a prime candidate for optical and electrical data storage applications. With the application of an optical or electrical pulse, they can be reversibly switched between amorphous and crystalline state, thereby exhibiting large optical and electrical contrast between the two phases, which are then stored as information in the form of binary digits. Single crystalline growth is interesting from both the academic and industrial perspective, as ordered Ge-Sb-Te based metamaterials are known to exhibit switching at reduced energies. The present study deals with the epitaxial growth and analysis of Ge-Sb-Te based thin films. The first part of the thesis deals with the epitaxial growth of GeTe. Thin films of GeTe were grown on highly mismatched Si(111) and (001) substrates. On both the substrate orientations the film grows along [111] direction with an amorphous-to-crystalline transition observed during the initial stages of growth. The amorphous-to-crystalline transition was studied in-vivo using azimuthal reflection high-energy electron diffraction scans and grazing incidence X-ray diffraction. In the second part of the thesis epitaxy and characterization of Sb 2 Te 3 thin films are presented. The third part of the thesis deals with the epitaxy of ternary Ge-Sb-Te alloys. The composition of the films are shown to be highly dependent on growth temperatures and vary along the pseudobinary line from Sb 2 Te 3 to GeTe with increase in growth temperatures. A line-of-sight quadrupole mass spectrometer was used to reliably control the GeSbTe growth temperature. Growth was performed at different Ge, Sb, Te fluxes to study the compositional variation of the films. Incommensurate peaks are observed along the [111] direction by X-ray diffraction. The possibility of superstructural vacancy ordering along the [111] direction is discussed.

Headspace Solid Phase Micro Extraction Gas Chromatographic Determination of Fenthion in Human Serum

Directory of Open Access Journals (Sweden)

Kyriaki Machera

2008-05-01

Full Text Available A simple and effective analytical procedure was developed for the determination of fenthion residues in human serum samples. The sample treatment was performed using the headspace solid-phase micro extraction with polyacrylate fiber, which has the advantage to require low amount of serum (1 mL without tedious pre-treatment. The quantification of fenthion was carried out by gas chromatography-mass spectrometry and the recoveries ranged from 79 to 104% at two spiking levels for 6 replicates. Detection and quantification limits were calculated as 1.51 and 4.54 ng/mL of serum respectively. Two fenthion metabolites − fenoxon and fenthion–sulfoxide − were also identified.

Electrical activation of solid-phase epitaxially regrown ultra-low energy boron implants in Ge preamorphised silicon and SOI

International Nuclear Information System (INIS)

Hamilton, J.J.; Collart, E.J.H.; Colombeau, B.; Jeynes, C.; Bersani, M.; Giubertoni, D.; Sharp, J.A.; Cowern, N.E.B.; Kirkby, K.J.

2005-01-01

The formation of highly activated ultra-shallow junctions (USJ) is one of the key requirements for the next generation of CMOS devices. One promising method for achieving this is the use of Ge preamorphising implants (PAI) prior to ultra-low energy B implantation. In future technology nodes, bulk silicon wafers may be supplanted by Silicon-on-Insulator (SOI), and an understanding of the Solid Phase Epitaxial (SPE) regrowth process and its correlation to dopant electrical activation in both bulk silicon and SOI is essential in order to understand the impact of this potential technology change. This kind of understanding will also enable tests of fundamental models for defect evolution and point-defect reactions at silicon/oxide interfaces. In the present work, B is implanted into Ge PAI silicon and SOI wafers with different PAI conditions and B doses, and resulting samples are annealed at various temperatures and times. Glancing-exit Rutherford Backscattering Spectrometry (RBS) is used to monitor the regrowth of the amorphous silicon, and the resulting redistribution and electrical activity of B are monitored by SIMS and Hall measurements. The results confirm the expected enhancement of regrowth velocity by B doping, and show that this velocity is otherwise independent of the substrate type and the Ge implant distribution within the amorphised layer. Hall measurements on isochronally annealed samples show that B deactivates less in SOI material than in bulk silicon, in cases where the Ge PAI end-of-range defects are close to the SOI back interface

Method and system for purification of gas streams for solid oxide cells

DEFF Research Database (Denmark)

2011-01-01

of: - providing at least one scrubber in the gas stream at the inlet side of the first electrode of the solid oxide cell; and/or providing at least one scrubber in the gas stream at the inlet side of the second electrode of the solid oxide cell; and - purifying the gas streams towards the first...... and second electrode; wherein the at least one scrubber in the gas stream at the inlet side of the first electrode and/or the at least one scrubber in the gas stream at the inlet side of the second electrode comprises a material suitable as an electrolyte material and a material suitable as an electrode...... material, and wherein the material suitable as an electrolyte material and a material suitable as an electrode material form triple phase boundaries similar to or identical to the triple phase boundaries of the electrode for which the gas stream is purified with the at least one scrubber....

Heat transfer across the interface between nanoscale solids and gas.

Science.gov (United States)

Cheng, Chun; Fan, Wen; Cao, Jinbo; Ryu, Sang-Gil; Ji, Jie; Grigoropoulos, Costas P; Wu, Junqiao

2011-12-27

When solid materials and devices scale down in size, heat transfer from the active region to the gas environment becomes increasingly significant. We show that the heat transfer coefficient across the solid-gas interface behaves very differently when the size of the solid is reduced to the nanoscale, such as that of a single nanowire. Unlike for macroscopic solids, the coefficient is strongly pressure dependent above ∼10 Torr, and at lower pressures it is much higher than predictions of the kinetic gas theory. The heat transfer coefficient was measured between a single, free-standing VO(2) nanowire and surrounding air using laser thermography, where the temperature distribution along the VO(2) nanowire was determined by imaging its domain structure of metal-insulator phase transition. The one-dimensional domain structure along the nanowire results from the balance between heat generation by the focused laser and heat dissipation to the substrate as well as to the surrounding gas, and thus serves as a nanoscale power-meter and thermometer. We quantified the heat loss rate across the nanowire-air interface, and found that it dominates over all other heat dissipation channels for small-diameter nanowires near ambient pressure. As the heat transfer across the solid-gas interface is nearly independent of the chemical identity of the solid, the results reveal a general scaling relationship for gaseous heat dissipation from nanostructures of all solid materials, which is applicable to nanoscale electronic and thermal devices exposed to gaseous environments.

Amperometric detector for gas chromatography based on a silica sol-gel solid electrolyte.

Science.gov (United States)

Steinecker, William H; Miecznikowski, Krzysztof; Kulesza, Pawel J; Sandlin, Zechariah D; Cox, James A

2017-11-01

An electrochemical cell comprising a silica sol-gel solid electrolyte, a working electrode that protrudes into a gas phase, and reference and counter electrodes that contact the solid electrolyte comprises an amperometric detector for gas chromatography. Under potentiostatic conditions, a current related to the concentration of an analyte in the gas phase is produced by its oxidation at the three-phase boundary among the sol-gel, working electrode, and the gas phase. The sol-gel is processed to contain an electrolyte that also serves as a humidistat to maintain a constant water activity even in the presence the gas chromatographic mobile phase. Response was demonstrated toward a diverse set of analytes, namely hydrogen, 1,2-ethandithiol, phenol, p-cresol, and thioanisole. Using flow injection amperometry of hydrogen with He as the carrier gas, 90% of the steady-state current was achieved in < 1s at a flow rate of 20mLmin -1 . A separation of 1,2-ethandithiol, phenol, p-cresol, and thioanisole at a 2.2mLmin -1 flow rate was achieved with respective detection limits (k = 3 criterion) of 4, 1, 3, and 70 ppmv when the working electrode potential was 800mV. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of headspace solid-phase microextraction method for ...

African Journals Online (AJOL)

A headspace solid-phase microextraction (HS-SPME) method was developed as a preliminary investigation using univariate approach for the analysis of 14 multiclass pesticide residues in fruits and vegetable samples. The gas chromatography mass spectrometry parameters (desorption temperature and time, column flow ...

Liquid phase electro epitaxy growth kinetics of GaAs-A three-dimensional numerical simulation study

International Nuclear Information System (INIS)

Mouleeswaran, D.; Dhanasekaran, R.

2006-01-01

A three-dimensional numerical simulation study for the liquid phase electro epitaxial growth kinetic of GaAs is presented. The kinetic model is constructed considering (i) the diffusive and convective mass transport, (ii) the heat transfer due to thermoelectric effects such as Peltier effect, Joule effect and Thomson effect, (iii) the electric current distribution with electromigration and (iv) the fluid flow coupled with concentration and temperature fields. The simulations are performed for two configurations namely (i) epitaxial growth from the arsenic saturated gallium rich growth solution, i.e., limited solution model and (ii) epitaxial growth from the arsenic saturated gallium rich growth solution with polycrystalline GaAs feed. The governing equations of liquid phase electro epitaxy are solved numerically with appropriate initial and boundary conditions using the central difference method. Simulations are performed to determine the following, a concentration profiles of solute atoms (As) in the Ga-rich growth solution, shape of the substrate evolution, the growth rate of the GaAs epitaxial film, the contributions of Peltier effect and electromigration of solute atoms to the growth with various experimental growth conditions. The growth rate is found to increase with increasing growth temperature and applied current density. The results are discussed in detail

Composition tailoring in the Ce-doped multicomponent garnet epitaxial film scintillators

Czech Academy of Sciences Publication Activity Database

Průša, Petr; Kučera, M.; Mareš, Jiří A.; Onderišinová, Z.; Hanuš, M.; Babin, Vladimir; Beitlerová, Alena; Nikl, Martin

2015-01-01

Roč. 15, č. 8 (2015), s. 3715-3723 ISSN 1528-7483 R&D Projects: GA ČR GAP204/12/0805 Institutional support: RVO:68378271 Keywords : scintillation * liquid phase epitaxy * photoelectron yield * Ce 3+ * multicomponent garnet Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 4.425, year: 2015

Acoustic probe for solid-gas-liquid suspensions. 1998 annual progress report

International Nuclear Information System (INIS)

Greenwood, M.S.; Sangani, A.S.; Tavlarides, L.L.

1998-01-01

'The proposed research will develop an acoustic probe for monitoring particle size and volume fraction in slurries in the absence and presence of gas. The goals are to commission and verify the probe components and system operation, develop theory for the forward and inverse problems for acoustic wave propagation through a three phase medium, and experimentally verify the theoretical analysis. The acoustic probe will permit measurement of solid content in gas-liquid-solid waste slurries in tanks across the DOE complex.'

Quantitative Analysis of Bisphenol A Leached from Household Plastics by Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry (SPME-GC-MS)

Science.gov (United States)

Johnson, Bettie Obi; Burke, Fernanda M.; Harrison, Rebecca; Burdette, Samantha

2012-01-01

The measurement of trace levels of bisphenol A (BPA) leached out of household plastics using solid-phase microextraction (SPME) with gas chromatography-mass spectrometry (GC-MS) is reported here. BPA is an endocrine-disrupting compound used in the industrial manufacture of polycarbonate plastic bottles and epoxy resin can liners. This experiment…

All solid-state SBS phase conjugate mirror

Science.gov (United States)

Dane, C.B.; Hackel, L.A.

1999-03-09

A stimulated Brillouin scattering (SBS) phase conjugate laser mirror uses a solid-state nonlinear gain medium instead of the conventional liquid or high pressure gas medium. The concept has been effectively demonstrated using common optical-grade fused silica. An energy threshold of 2.5 mJ and a slope efficiency of over 90% were achieved, resulting in an overall energy reflectivity of >80% for 15 ns, 1 um laser pulses. The use of solid-state materials is enabled by a multi-pass resonant architecture which suppresses transient fluctuations that would otherwise result in damage to the SBS medium. This all solid state phase conjugator is safer, more reliable, and more easily manufactured than prior art designs. It allows nonlinear wavefront correction to be implemented in industrial and defense laser systems whose operating environments would preclude the introduction of potentially hazardous liquids or high pressure gases. 8 figs.

High purity liquid phase epitaxial gallium arsenide nuclear radiation detector

International Nuclear Information System (INIS)

Alexiev, D.; Butcher, K.S.A.

1991-11-01

Surface barrier radiation detector made from high purity liquid phase epitaxial gallium arsenide wafers have been operated as X- and γ-ray detectors at various operating temperatures. Low energy isotopes are resolved including 241 Am at 40 deg C. and the higher gamma energies of 235 U at -80 deg C. 15 refs., 1 tab., 6 figs

Molecular beam epitaxy of GeTe-Sb{sub 2}Te{sub 3} phase change materials studied by X-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Shayduk, Roman

2010-05-20

The integration of phase change materials into semiconductor heterostructures may lead to the development of a new generation of high density non-volatile phase change memories. Epitaxial phase change materials allow to study the detailed structural changes during the phase transition and to determine the scaling limits of the memory. This work is dedicated to the epitaxial growth of Ge-Sb-Te phase change alloys on GaSb(001). We deposit Ge-Sb-Te (GST) films on GaSb(001) substrates by means of molecular beam epitaxy (MBE). The film orientation and lattice constant evolution is determined in real time during growth using grazing incidence X-ray diffraction (GID). The nucleation stage of the growth is studied in situ using reflection high energy electron diffraction (RHEED). Four growth regimes of GST on GaSb(001) were observed: amorphous, polycrystalline, incubated epitaxial and direct epitaxial. Amorphous film grows for substrate temperatures below 100 C. For substrate temperatures in the range 100-160 C, the film grows in polycrystalline form. Incubated epitaxial growth is observed at temperatures from 180 to 210 C. This growth regime is characterized by an initial 0.6nm thick amorphous layer formation, which crystallizes epitaxially as the film thickness increases. The determined lattice constant of the films is 6.01 A, very close to that of the metastable GST phase. The films predominantly possess an epitaxial cube-on-cube relationship. At higher temperatures the films grow epitaxially, however the growth rate is rapidly decreasing with temperature. At temperatures above 270 C the growth rate is zero. The composition of the grown films is close to 2:2:5 for Ge, Sb and Te, respectively. The determined crystal structure of the films is face centered cubic (FCC) with a rhombohedral distortion. The analysis of X-ray peak widths gives a value for the rhombohedral angle of 89.56 . We observe two types of reflections in reciprocal space indicating two FCC sublattices in

Thermodynamic analysis of trimethylgallium decomposition during GaN metal organic vapor phase epitaxy

Science.gov (United States)

Sekiguchi, Kazuki; Shirakawa, Hiroki; Chokawa, Kenta; Araidai, Masaaki; Kangawa, Yoshihiro; Kakimoto, Koichi; Shiraishi, Kenji

2018-04-01

We analyzed the decomposition of Ga(CH3)3 (TMG) during the metal organic vapor phase epitaxy (MOVPE) of GaN on the basis of first-principles calculations and thermodynamic analysis. We performed activation energy calculations of TMG decomposition and determined the main reaction processes of TMG during GaN MOVPE. We found that TMG reacts with the H2 carrier gas and that (CH3)2GaH is generated after the desorption of the methyl group. Next, (CH3)2GaH decomposes into (CH3)GaH2 and this decomposes into GaH3. Finally, GaH3 becomes GaH. In the MOVPE growth of GaN, TMG decomposes into GaH by the successive desorption of its methyl groups. The results presented here concur with recent high-resolution mass spectroscopy results.

Epitaxial growth of Ge-Sb-Te based phase change materials

Energy Technology Data Exchange (ETDEWEB)

Perumal, Karthick

2013-07-30

Ge-Sb-Te based phase change materials are considered as a prime candidate for optical and electrical data storage applications. With the application of an optical or electrical pulse, they can be reversibly switched between amorphous and crystalline state, thereby exhibiting large optical and electrical contrast between the two phases, which are then stored as information in the form of binary digits. Single crystalline growth is interesting from both the academic and industrial perspective, as ordered Ge-Sb-Te based metamaterials are known to exhibit switching at reduced energies. The present study deals with the epitaxial growth and analysis of Ge-Sb-Te based thin films. The first part of the thesis deals with the epitaxial growth of GeTe. Thin films of GeTe were grown on highly mismatched Si(111) and (001) substrates. On both the substrate orientations the film grows along [111] direction with an amorphous-to-crystalline transition observed during the initial stages of growth. The amorphous-to-crystalline transition was studied in-vivo using azimuthal reflection high-energy electron diffraction scans and grazing incidence X-ray diffraction. In the second part of the thesis epitaxy and characterization of Sb{sub 2}Te{sub 3} thin films are presented. The third part of the thesis deals with the epitaxy of ternary Ge-Sb-Te alloys. The composition of the films are shown to be highly dependent on growth temperatures and vary along the pseudobinary line from Sb{sub 2}Te{sub 3} to GeTe with increase in growth temperatures. A line-of-sight quadrupole mass spectrometer was used to reliably control the GeSbTe growth temperature. Growth was performed at different Ge, Sb, Te fluxes to study the compositional variation of the films. Incommensurate peaks are observed along the [111] direction by X-ray diffraction. The possibility of superstructural vacancy ordering along the [111] direction is discussed.

Gas Generation from Solids in Aqueous Suspensions

International Nuclear Information System (INIS)

Meisel, D.; Schatz, T.

1999-01-01

The presence of solid particles suspended in solution may change the radiation-induced chemistry of a system in many ways. Catalytic surface effects may manifest themselves through the acceleration or inhibition of various reactions. As importantly, the yield of primary radiolysis products may be affected as the solids absorb a significant fraction of the radiation energy. The latter is the subject of this study. We explore the possibility that absorption of radiation by the solid particles may initiate chemistry in the water. This is a question of fundamental as well as practical significance. On the fundamental side we ask whether electron-hole pairs generated in the solid phase can escape and cross into the aqueous phase and initiate chemical reactions such as gas generation and how this possibility depends on the energy levels of the material and on particle size. From a practical angle, such questions are directly relevant to any heterogeneous system exposed to radiation. High-level waste temporarily stored in underground tanks, low-level waste permanently stored in humid grout, or soil particles migrating in geological formations are but a few examples

Liquid phase epitaxy of gallium arsenide - a review

International Nuclear Information System (INIS)

Alexiev, D.; Edmondson, M.; Butcher, K.S.A.; Tansley, T.

1992-07-01

Liquid phase epitaxy of gallium arsenide has been investigated intensively from the late 1960's to the present and has now a special place in the manufacture of wide band, compound semiconductor radiation detectors. Although this particular process appears to have gained prominence in the last three decades, the authors point out that its origins reach back to 1836 when Frankenheim made his first observations. A brief review is presented from a semiconductor applications point of view on how this subject developed. 70 refs., 5 figs

N-MOSFETs Formed on Solid Phase Epitaxially Grown GeSn Film with Passivation by Oxygen Plasma Featuring High Mobility.

Science.gov (United States)

Fang, Yung-Chin; Chen, Kuen-Yi; Hsieh, Ching-Heng; Su, Chang-Chia; Wu, Yung-Hsien

2015-12-09

Solid phase epitaxially grown GeSn was employed as the platform to assess the eligibility of direct O2 plasma treatment on GeSn surface for passivation of GeSn N-MOSFETs. It has been confirmed that O2 plasma treatment forms a GeSnO(x) film on the surface and the GeSnO(x) topped by in situ Al2O3 constitutes the gate stack of GeSn MOS devices. The capability of the surface passivation was evidenced by the low interface trap density (D(it)) of 1.62 × 10(11) cm(-2) eV(-1), which is primarily due to the formation of Ge-O and Sn-O bonds at the surface by high density/reactivity oxygen radicals that effectively suppress dangling bonds and decrease gap states. The good D(it) not only makes tiny frequency dispersion in the characterization of GeSn MOS capacitors, but results in GeSn N-MOSFETs with outstanding peak electron mobility as high as 518 cm(2)/(V s) which outperforms other devices reported in the literature due to reduced undesirable carrier scattering. In addition, the GeSn N-MOSFETs also exhibit promising characteristics in terms of acceptable subthreshold swing of 156 mV/dec and relatively large I(ON)/I(OFF) ratio more than 4 orders. Moreover, the robust reliability in terms small V(t) variation against high field stress attests the feasibility of using the O2 plasma-treated passivation to advanced GeSn technology.

Determination of amphetamine-type stimulants in oral fluid by solid-phase microextraction and gas chromatography-mass spectrometry

International Nuclear Information System (INIS)

Souza, Daniele Z.; Boehl, Paula O.; Comiran, Eloisa; Mariotti, Kristiane C.; Pechansky, Flavio; Duarte, Paulina C.A.V.; De Boni, Raquel; Froehlich, Pedro E.; Limberger, Renata P.

2011-01-01

Graphical abstract: Highlights: → Propylchloroformate derivatization of amphetamine-type stimulants in oral fluid. → Direct immersion solid-phase microextraction/gas chromatography-mass spectrometry. → Linear range 2(4)-256 ng mL -1 , detection limits 0.5-2 ng mL -1 . → Accuracy 98-112%, precision TM device has been developed and validated. Thereunto, in-matrix propylchloroformate derivatization followed by direct immersion solid-phase microextraction and gas chromatography-mass spectrometry were employed. Deuterium labeled AMP was used as internal standard for all the stimulants and analysis was performed using the selected ion monitoring mode. The detector response was linear for the studied drugs in the concentration range of 2-256 ng mL -1 (neat oral fluid), except for FEN, whereas the linear range was 4-256 ng mL -1 . The detection limits were 0.5 ng mL -1 (MET), 1 ng mL -1 (MPH) and 2 ng mL -1 (DIE, AMP, FEN), respectively. Accuracy of quality control samples remained within 98.2-111.9% of the target concentrations, while precision has not exceeded 15% of the relative standard deviation. Recoveries with Quantisal TM device ranged from 77.2% to 112.1%. Also, the goodness-of-fit concerning the ordinary least squares model in the statistical inference of data has been tested through residual plotting and ANOVA. The validated method can be easily automated and then used for screening and confirmation of amphetamine-type stimulants in drivers' oral fluid.

GaN Bulk Growth and Epitaxy from Ca-Ga-N Solutions, Phase I

Data.gov (United States)

National Aeronautics and Space Administration — This SBIR proposal addresses the liquid phase epitaxy (LPE) of gallium nitride (GaN) films using nitrogen-enriched metal solutions. Growth of GaN from solutions...

Development of solid-gas equilibrium propulsion system for small spacecraft

Science.gov (United States)

Chujo, Toshihiro; Mori, Osamu; Kubo, Yuki

2017-11-01

A phase equilibrium propulsion system is a kind of cold-gas jet in which the phase equilibrium state of the fuel is maintained in a tank and its vapor is ejected when a valve is opened. One such example is a gas-liquid equilibrium propulsion system that uses liquefied gas as fuel. This system was mounted on the IKAROS solar sail and has been demonstrated in orbit. The system has a higher storage efficiency and a lighter configuration than a high-pressure cold-gas jet because the vapor pressure is lower, and is suitable for small spacecraft. However, the system requires a gas-liquid separation device in order to avoid leakage of the liquid, which makes the system complex. As another example of a phase equilibrium propulsion system, we introduce a solid-gas equilibrium propulsion system, which uses a sublimable substance as fuel and ejects its vapor. This system has an even lower vapor pressure and does not require such a separation device, instead requiring only a filter to keep the solid inside the tank. Moreover, the system is much simpler and lighter, making it more suitable for small spacecraft, especially CubeSat-class spacecraft, and the low thrust of the system allows spacecraft motion to be controlled precisely. In addition, the thrust level can be controlled by controlling the temperature of the fuel, which changes the vapor pressure. The present paper introduces the concept of the proposed system, and describes ejection experiments and its evaluation. The basic function of the proposed system is demonstrated in order to verify its usefulness.

Scalable solution-phase epitaxial growth of symmetry-mismatched heterostructures on two-dimensional crystal soft template.

Science.gov (United States)

Lin, Zhaoyang; Yin, Anxiang; Mao, Jun; Xia, Yi; Kempf, Nicholas; He, Qiyuan; Wang, Yiliu; Chen, Chih-Yen; Zhang, Yanliang; Ozolins, Vidvuds; Ren, Zhifeng; Huang, Yu; Duan, Xiangfeng

2016-10-01

Epitaxial heterostructures with precisely controlled composition and electronic modulation are of central importance for electronics, optoelectronics, thermoelectrics, and catalysis. In general, epitaxial material growth requires identical or nearly identical crystal structures with small misfit in lattice symmetry and parameters and is typically achieved by vapor-phase depositions in vacuum. We report a scalable solution-phase growth of symmetry-mismatched PbSe/Bi 2 Se 3 epitaxial heterostructures by using two-dimensional (2D) Bi 2 Se 3 nanoplates as soft templates. The dangling bond-free surface of 2D Bi 2 Se 3 nanoplates guides the growth of PbSe crystal without requiring a one-to-one match in the atomic structure, which exerts minimal restriction on the epitaxial layer. With a layered structure and weak van der Waals interlayer interaction, the interface layer in the 2D Bi 2 Se 3 nanoplates can deform to accommodate incoming layer, thus functioning as a soft template for symmetry-mismatched epitaxial growth of cubic PbSe crystal on rhombohedral Bi 2 Se 3 nanoplates. We show that a solution chemistry approach can be readily used for the synthesis of gram-scale PbSe/Bi 2 Se 3 epitaxial heterostructures, in which the square PbSe (001) layer forms on the trigonal/hexagonal (0001) plane of Bi 2 Se 3 nanoplates. We further show that the resulted PbSe/Bi 2 Se 3 heterostructures can be readily processed into bulk pellet with considerably suppressed thermal conductivity (0.30 W/m·K at room temperature) while retaining respectable electrical conductivity, together delivering a thermoelectric figure of merit ZT three times higher than that of the pristine Bi 2 Se 3 nanoplates at 575 K. Our study demonstrates a unique epitaxy mode enabled by the 2D nanocrystal soft template via an affordable and scalable solution chemistry approach. It opens up new opportunities for the creation of diverse epitaxial heterostructures with highly disparate structures and functions.

Photovoltaic x-ray detectors based on the GaAs epitaxial structures

CERN Document Server

Akhmadullin, R A; Dvoryankina, G G; Dikaev, Y M; Ermakov, M G; Ermakova, O N; Krikunov, A I; Kudryashov, A A; Petrov, A G; Telegin, A A

2002-01-01

The new photovoltaic detector of the X-ray radiation is proposed on the basis of the GaAs epitaxial structures, which operates with high efficiency of the charge carriers collection without shift voltage and at the room temperature. The structures are grown by the method of the gas-phase epitaxy on the n sup + -type highly-alloyed substrates. The range of sensitivity to the X-ray radiation is within the range of effective energies from 8 up to 120 keV. The detector maximum response in the current short circuit mode is determined

Solid phase micro-extraction in environmental atmosphere

International Nuclear Information System (INIS)

Tao Ping; Wei Lifan; Tan Yun

2002-01-01

Solid phase micro-extraction (SPME) is an advanced technique of sample pretreatment in environmental atmosphere analysis, i.e., a sampling method of extracting volatile organic compounds from environmental gas. According to the primary survey on the theory and application of SPME, a suitable extraction tip, i.e., a coated fused silica fiber, is selected to construct a SPME apparatus. This SPME apparatus is used to extract volatile organic compounds from environmental atmosphere and a qualitative detection is conducted in gas chromatography-mass spectrometer system. Good experimental results are obtained

Liquid epitaxy of Gasub(1-x)Alsub(x)Sb varizone structures

International Nuclear Information System (INIS)

Dedegkaev, T.T.; Kryukov, I.I.; Lidejkis, T.P.; Tsarenkov, B.V.; Yakovlev, Yu.P.

1980-01-01

To produce Gasub (1-x)Alsub(x)Sb varizon structures with preset limits for the change of the width of Eg forbidden zone and preset Eg gradient value and sign, epitaxy growth from the liquid phase of solid solutions of GaSb-AlSb system was investigated. The epitaxy was realized in two ways: by cooling the saturated solution of Ga-Al-Sb melt and using the isometric contineous mixing of two solution-melts with different Al content. As a result it was ascertained that: 1 the epitaxy by cooling a solution-melt permitted to produce Gasub(1-x)Alsub(x)Sb varizon structures only with small Eg gradients (<=30eV/cm); 2 the epitaxy by contineously mixing the solution-melts permitted to produce Gasub(1-x)Alsub(x)Sb varizon structures with increasing and decreasing Eg in the direction of layer growth in the whole interval of compositions. Eg gradient can be as great as thousands of eV/cm

Solid-solid and gas-solid interactions induced during high-energy milling to produce PbTe nanopowders

Energy Technology Data Exchange (ETDEWEB)

Rojas-Chavez, H., E-mail: rojas_hugo@ittlahuac2.edu.mx [Instituto Tecnologico de Tlahuac - II (Mexico); Reyes-Carmona, F. [Facultad de Quimica - UNAM (Mexico); Garibay-Febles, V. [Instituto Mexicano del Petroleo, Laboratorio de Microscopia Electronica de Ultra Alta Resolucion (Mexico); Jaramillo-Vigueras, D. [Centro de Investigacion e Innovacion Tecnologica - IPN (Mexico)

2013-05-15

Transformations from precursors to nanoparticles by high-energy milling are promoted by two major driving forces, namely physical and/or chemical. While the former has been difficult to trace since stress, strain and recovery may occur almost simultaneously during milling, the latter has been sequentially followed as an evolution from precursors to intermediate phases and thereof to high purity nanocrystals. The specific objective of this work is to discern how solid-solid and partially solid-gas reactions manifest themselves correspondingly as a short-range diffusion through an interface or how vapor species, as a subliming phenomenon, grows as a different phase on an active local surface. These series of changes were traced by sub-cooling the as-milled powders extracted during a milling cycle. Through this experimental technique, samples were electron microscopically analyzed and where it was required, selected area electron diffraction images were obtained. High-resolution transmission electron microscopy results, unambiguously, confirm that nanocrystals in the last stage show a cubic morphology which average size distributions are around 17 nm.

Gas transport in solid oxide fuel cells

CERN Document Server

He, Weidong; Dickerson, James

2014-01-01

This book provides a comprehensive overview of contemporary research and emerging measurement technologies associated with gas transport in solid oxide fuel cells. Within these pages, an introduction to the concept of gas diffusion in solid oxide fuel cells is presented. This book also discusses the history and underlying fundamental mechanisms of gas diffusion in solid oxide fuel cells, general theoretical mathematical models for gas diffusion, and traditional and advanced techniques for gas diffusivity measurement.

Preparation and Characterization of Epitaxial VO2 Films on Sapphire Using Postepitaxial Topotaxy Route via Epitaxial V2O3 Films

Science.gov (United States)

Yamaguchi, Iwao; Manabe, Takaaki; Tsuchiya, Tetsuo; Nakajima, Tomohiko; Sohma, Mitsugu; Kumagai, Toshiya

2008-02-01

Epitaxial VO2 films were prepared on the C-planes of α-Al2O3 substrates by a metal organic deposition (MOD) process. It was difficult to obtain the single phase of (010)M-oriented VO2 films, in which the subscript M refers to the monoclinic indices, by the heat treatment of amorphous precursor films in the VO2-stable region after the pyrolysis of the coating solution. The product films consisted of discontinuous circular grains of 1-2 µm size on the substrate surface. Therefore, we prepared the (010)M-oriented epitaxial VO2 films using postepitaxial topotaxy (PET), that is, topotactic oxidation of (0001)-oriented epitaxial V2O3 films. First, epitaxial V2O3(0001) films were obtained by MOD starting with a vanadium naphthenate solution. Second, the epitaxial V2O3(0001) films were topotactically oxidized at 500 °C in an Ar-O2 gas mixture with pO2 = 10-4 atm to obtain (010)M-oriented epitaxial VO2 films. The epitaxial relationships were VO2(010)M ∥ α-Al2O3(0001) and VO2[100]M ∥ α-Al2O3[0110], [1010], [1100]. The VO2(010)M films exhibited metal-semiconductor transitions with hysteresis loops at 60-80 °C. The resistivity change before and after the transition of the VO2(010)M film oxidized for 6 h was three orders of magnitude.

Epitaxial growth and characterization of CuGa2O4 films by laser molecular beam epitaxy

Directory of Open Access Journals (Sweden)

Hongling Wei

2017-11-01

Full Text Available Ga2O3 with a wide bandgap of ∼ 4.9 eV can crystalize in five crystalline phases. Among those phases, the most stable monoclinic β-Ga2O3 has been studied most, however, it is hard to find materials lattice matching with β-Ga2O3 to grown epitaxial thin films for optoelectronic applications. In this work, CuGa2O4 bulk were prepared by solid state reaction as target, and the films were deposited on sapphire substrates by laser molecular beam epitaxy (L-MBE at different substrate temperatures. The influences of substrate temperature on structural and optical properties have been systematically investigated by means of X-ray diffraction, Transmission electron microscope and UV-vis absorption spectra. High quality cubic structure and [111] oriented CuGa2O4 film can be obtained at substrate temperature of 750 °C. It’s also demonstrated that the CuGa2O4 film has a bandgap of ∼ 4.4 eV and a best crystal quality at 750 °C, suggesting that CuGa2O4 film is a promising candidate for applications in ultraviolet optoelectronic devices.

Investigation into process of solid-phase synthesis of calcium vanadates

International Nuclear Information System (INIS)

Fotiev, A.A.; Krasnenko, T.I.; Slobodin, B.V.

1983-01-01

Processes of solid-phase synthesis of calcium vanadates by Toubandt method, measuring electric conductivity and Ca 45 and V 48 radioactive indicators are investigated. It is shown that reaction diffusion during calcium vanadates production from oxides is ensured by calcium and oxygen ions or calcium ions and electrons through the product layer, as to oxygen - through the gas phase

Structural evolution of epitaxial SrCoO{sub x} films near topotactic phase transition

Energy Technology Data Exchange (ETDEWEB)

Jeen, Hyoungjeen [Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831 (United States); Department of Physics, Pusan National University, Busan, 609735 (Korea, Republic of); Lee, Ho Nyung, E-mail: hnlee@ornl.gov [Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831 (United States)

2015-12-15

Control of oxygen stoichiometry in complex oxides via topotactic phase transition is an interesting avenue to not only modifying the physical properties, but utilizing in many energy technologies, such as energy storage and catalysts. However, detailed structural evolution in the close proximity of the topotactic phase transition in multivalent oxides has not been much studied. In this work, we used strontium cobaltites (SrCoO{sub x}) epitaxially grown by pulsed laser epitaxy (PLE) as a model system to study the oxidation-driven evolution of the structure, electronic, and magnetic properties. We grew coherently strained SrCoO{sub 2.5} thin films and performed post-annealing at various temperatures for topotactic conversion into the perovskite phase (SrCoO{sub 3-δ}). We clearly observed significant changes in electronic transport, magnetism, and microstructure near the critical temperature for the topotactic transformation from the brownmillerite to the perovskite phase. Nevertheless, the overall crystallinity was well maintained without much structural degradation, indicating that topotactic phase control can be a useful tool to control the physical properties repeatedly via redox reactions.

Revisiting low-fidelity two-fluid models for gas-solids transport

Science.gov (United States)

Adeleke, Najeem; Adewumi, Michael; Ityokumbul, Thaddeus

2016-08-01

Two-phase gas-solids transport models are widely utilized for process design and automation in a broad range of industrial applications. Some of these applications include proppant transport in gaseous fracking fluids, air/gas drilling hydraulics, coal-gasification reactors and food processing units. Systems automation and real time process optimization stand to benefit a great deal from availability of efficient and accurate theoretical models for operations data processing. However, modeling two-phase pneumatic transport systems accurately requires a comprehensive understanding of gas-solids flow behavior. In this study we discuss the prevailing flow conditions and present a low-fidelity two-fluid model equation for particulate transport. The model equations are formulated in a manner that ensures the physical flux term remains conservative despite the inclusion of solids normal stress through the empirical formula for modulus of elasticity. A new set of Roe-Pike averages are presented for the resulting strictly hyperbolic flux term in the system of equations, which was used to develop a Roe-type approximate Riemann solver. The resulting scheme is stable regardless of the choice of flux-limiter. The model is evaluated by the prediction of experimental results from both pneumatic riser and air-drilling hydraulics systems. We demonstrate the effect and impact of numerical formulation and choice of numerical scheme on model predictions. We illustrate the capability of a low-fidelity one-dimensional two-fluid model in predicting relevant flow parameters in two-phase particulate systems accurately even under flow regimes involving counter-current flow.

Spin Filtering in Epitaxial Spinel Films with Nanoscale Phase Separation

KAUST Repository

Li, Peng

2017-05-08

The coexistence of ferromagnetic metallic phase and antiferromagnetic insulating phase in nanoscaled inhomogeneous perovskite oxides accounts for the colossal magnetoresistance. Although the model of spin-polarized electron transport across antiphase boundaries has been commonly employed to account for large magnetoresistance (MR) in ferrites, the magnetic anomalies, the two magnetic phases and enhanced molecular moment, are still unresolved. We observed a sizable MR in epitaxial spinel films (NiCo2O4-δ) that is much larger than that commonly observed in spinel ferrites. Detailed analysis reveals that this MR can be attributed to phase separation, in which the perfect ferrimagnetic metallic phase and ferrimagnetic insulating phase coexist. The magnetic insulating phase plays an important role in spin filtering in these phase separated spinel oxides, leading to a sizable MR effect. A spin filtering model based on Zeeman effect and direct tunneling is developed to account for MR of the phase separated films.

Investigation into the determination of trimethylarsine in natural gas and its partitioning into gas and condensate phases using (cryotrapping)/gas chromatography coupled to inductively coupled plasma mass spectrometry and liquid/solid sorption techniques

International Nuclear Information System (INIS)

Krupp, E.M.; Johnson, C.; Rechsteiner, C.; Moir, M.; Leong, D.; Feldmann, J.

2007-01-01

Speciation of trialkylated arsenic compunds in natural gas, pressurized and stable condensate samples from the same gas well was performed using (Cryotrapping) Gas Chromatography-Inductively Coupled Plasma Mass Spectrometry. The major species in all phases investigated was found to be trimethylarsine with a highest concentration of 17.8 ng/L (As) in the gas phase and 33.2 μg/L (As) in the stable condensate phase. The highest amount of trimethylarsine (121 μg/L (As)) was found in the pressurized condensate, along with trace amounts of non-identified higher alkylated arsines. Volatile arsenic species in natural gas and its related products cause concern with regards to environment, safety, occupational health and gas processing. Therefore, interest lies in a fast and simple field method for the determination of volatile arsenicals. Here, we use simple liquid and solid sorption techniques, namely absorption in silver nitrate solution and adsorption on silver nitrate impregnated silica gel tubes followed by total arsenic determination as a promising tool for field monitoring of volatile arsenicals in natural gas and gas condensates. Preliminary results obtained for the sorption-based methods show that around 70% of the arsenic is determined with these methods in comparison to volatile arsenic determination using GC-ICP-MS. Furthermore, an inter-laboratory- and inter-method comparison was performed using silver nitrate impregnated silica tubes on 14 different gas samples with concentrations varying from below 1 to 1000 μg As/m 3 natural gas. The results obtained from the two laboratories differ in a range of 10 to 60%, but agree within the order of magnitude, which is satisfactory for our purposes

A comparative study of transport properties in polycrystalline and epitaxial chromium nitride films

KAUST Repository

Duan, X. F.; Mi, Wenbo; Guo, Zaibing; Bai, Haili

2013-01-01

Polycrystalline CrNx films on Si(100) and glass substrates and epitaxial CrNx films on MgO(100) substrates were fabricated by reactive sputtering with different nitrogen gas flow rates (fN2). With the increase of fN2, a lattice phase transformation

Process for forming epitaxial perovskite thin film layers using halide precursors

Science.gov (United States)

Clem, Paul G.; Rodriguez, Mark A.; Voigt, James A.; Ashley, Carol S.

2001-01-01

A process for forming an epitaxial perovskite-phase thin film on a substrate. This thin film can act as a buffer layer between a Ni substrate and a YBa.sub.2 Cu.sub.3 O.sub.7-x superconductor layer. The process utilizes alkali or alkaline metal acetates dissolved in halogenated organic acid along with titanium isopropoxide to dip or spin-coat the substrate which is then heated to about 700.degree. C. in an inert gas atmosphere to form the epitaxial film on the substrate. The YBCO superconductor can then be deposited on the layer formed by this invention.

Surface passivation of liquid phase epitaxial GaAs

International Nuclear Information System (INIS)

Alexiev, D.; Butcher, K.S.A.; Mo, L.; Edmondson, M.

1995-10-01

Passivation of the liquid phase epitaxial GaAs surface was attempted using aqueous P 2 S 5 -NH 4 OH, (NH 4 ) 2 S x and plasma nitrogenation and hydrogenation. Results indicate that plasma nitrogenation with pretreatment of plasma hydrogenation produced consistent reduction in reverse leakage current at room temperature for all p and n type Schottky diodes. Some diodes showed an order of magnitude improvement in current density. (NH 4 ) 2 S x passivation also results in improved I-V characteristics, though the long term stability of this passivation is questionable. 26 refs., 6 figs

Determination of some selected pesticide residues in apple juice by solid-phase microextraction coupled to gas chromatography – mass spectrometry

Directory of Open Access Journals (Sweden)

Andrea Hercegová

2011-01-01

Full Text Available The performance of solid phase microextraction (SPME for enrichment of pesticides from apple juice was investigated. Samples were diluted with water, extracted by solid-phase microextraction and analysed by gas chromatography using mass-spectrometry detector (MSD in selected ion monitoring mode (SIM. The method was tested for the following pesticides used mostly in fruit culturing at Slovakia: tebuthylazine, fenitrothion, chlorpyrifos, myclobutanil, cyprodinil, phosalone, pyrimethanil, tebuconazole, kresoxim-methyl, methidathion, penconazole. All pesticides were extracted with polydimethylsiloxane fibre 100 μm thickness. The linear concentration range of application was 0.05 μg dm−3–10 μg dm−3. The method described provides detectabilities complying with the maximum residue levels (MRLs set by regulatory organizations for pesticides in apple juice matrices. The solvent – free SPME procedure was found to be quicker and more cost effective then the solvent extraction methods commonly used.

Non-intrusive measurement and hydrodynamics characterization of gas-solid fluidized beds: a review

Science.gov (United States)

Sun, Jingyuan; Yan, Yong

2016-11-01

Gas-solid fluidization is a well-established technique to suspend or transport particles and has been applied in a variety of industrial processes. Nevertheless, our knowledge of fluidization hydrodynamics is still limited for the design, scale-up and operation optimization of fluidized bed reactors. It is, therefore, essential to characterize the two-phase flow behaviours in gas-solid fluidized beds and monitor the fluidization processes for control and optimization. A range of non-intrusive techniques have been developed or proposed for measuring the fluidization dynamic parameters and monitoring the flow status without disturbing or distorting the flow fields. This paper presents a comprehensive review of the non-intrusive measurement techniques and the current state of knowledge and experience in the characterization and monitoring of gas-solid fluidized beds. These techniques are classified into six main categories as per sensing principles, electrostatic, acoustic emission and vibration, visualization, particle tracking, laser Doppler anemometry and phase Doppler anemometry as well as pressure-fluctuation methods. Trends and future developments in this field are also discussed.

Headspace solid-phase microextraction procedures for gas chromatographic analysis of biological fluids and materials.

Science.gov (United States)

Mills, G A; Walker, V

2000-12-01

Solid-phase microextraction (SPME) is a new solventless sample preparation technique that is finding wide usage. This review provides updated information on headspace SPME with gas chromatographic separation for the extraction and measurement of volatile and semivolatile analytes in biological fluids and materials. Firstly the background to the technique is given in terms of apparatus, fibres used, extraction conditions and derivatisation procedures. Then the different matrices, urine, blood, faeces, breast milk, hair, breath and saliva are considered separately. For each, methods appropriate for the analysis of drugs and metabolites, solvents and chemicals, anaesthetics, pesticides, organometallics and endogenous compounds are reviewed and the main experimental conditions outlined with specific examples. Then finally, the future potential of SPME for the analysis of biological samples in terms of the development of new devices and fibre chemistries and its coupling with high-performance liquid chromatography is discussed.

Crystal phase-based epitaxial growth of hybrid noble metal nanostructures on 4H/fcc Au nanowires

Science.gov (United States)

Lu, Qipeng; Wang, An-Liang; Gong, Yue; Hao, Wei; Cheng, Hongfei; Chen, Junze; Li, Bing; Yang, Nailiang; Niu, Wenxin; Wang, Jie; Yu, Yifu; Zhang, Xiao; Chen, Ye; Fan, Zhanxi; Wu, Xue-Jun; Chen, Jinping; Luo, Jun; Li, Shuzhou; Gu, Lin; Zhang, Hua

2018-03-01

Crystal-phase engineering offers opportunities for the rational design and synthesis of noble metal nanomaterials with unusual crystal phases that normally do not exist in bulk materials. However, it remains a challenge to use these materials as seeds to construct heterometallic nanostructures with desired crystal phases and morphologies for promising applications such as catalysis. Here, we report a strategy for the synthesis of binary and ternary hybrid noble metal nanostructures. Our synthesized crystal-phase heterostructured 4H/fcc Au nanowires enable the epitaxial growth of Ru nanorods on the 4H phase and fcc-twin boundary in Au nanowires, resulting in hybrid Au-Ru nanowires. Moreover, the method can be extended to the epitaxial growth of Rh, Ru-Rh and Ru-Pt nanorods on the 4H/fcc Au nanowires to form unique hybrid nanowires. Importantly, the Au-Ru hybrid nanowires with tunable compositions exhibit excellent electrocatalytic performance towards the hydrogen evolution reaction in alkaline media.

Automated mini-column solid-phase extraction cleanup for high-throughput analysis of chemical contaminants in foods by low-pressure gas chromatography – tandem mass spectrometry

Science.gov (United States)

This study demonstrated the application of an automated high-throughput mini-cartridge solid-phase extraction (mini-SPE) cleanup for the rapid low-pressure gas chromatography – tandem mass spectrometry (LPGC-MS/MS) analysis of pesticides and environmental contaminants in QuEChERS extracts of foods. ...

Experimental and theoretical studies on the gas/solid/gas transformation cycle in extraterrestrial environments

Science.gov (United States)

Cottin, Hervé; Gazeau, Marie-Claire; Chaquin, Patrick; Raulin, François; Bénilan, Yves

2001-12-01

The ubiquity of molecular material in the universe, from hydrogen to complex organic matter, is the result of intermixed physicochemical processes that have occurred throughout history. In particular, the gas/solid/gas phase transformation cycle plays a key role in chemical evolution of organic matter from the interstellar medium to planetary systems. This paper focuses on two examples that are representative of the diversity of environments where such transformations occur in the Solar System: (1) the photolytic evolution from gaseous to solid material in methane containing planetary atmospheres and (2) the degradation of high molecular weight compounds into gas phase molecules in comets. We are currently developing two programs which couple experimental and theoretical studies. The aim of this research is to provide data necessary to build models in order to better understand (1) the photochemical evolution of Titan's atmosphere, through a laboratory program to determine quantitative spectroscopic data on long carbon chain molecules (polyynes) obtained in the SCOOP program (French acronym for Spectroscopy of Organic Compounds Oriented for Planetology), and (2) the extended sources in comets, through a laboratory program of quantitative studies of photochemical and thermal degradation processes on relevant polymers (e.g., Polyoxymethylene) by the SEMAPhOrE Cometaire program (French acronym for Experimental Simulation and Modeling Applied to Organic Chemistry in Cometary Environment).

In-situ transmission electron microscopy of the solid-phase epitaxial growth of GaAs: sample preparation and artifact characterization

International Nuclear Information System (INIS)

Llewellyn, D.J.; Llewellyn, D.J.; Belay, K.B.; Ridgway, M.C.

1998-01-01

In-situ transmission electron microscopy (TEM) has been used to characterize the solid phase epitaxial growth of amorphized GaAs at a temperature of 260 deg C. To maximize heat transfer from the heated holder to the sample and minimize electron-irradiation induced artifacts, non-conventional methodologies were utilized for the preparation of cross-sectional samples. GaAs 3x1 mm rectangular wafers were cleaved then glued face-to-face to form a wafer stack size of 3x3 mm while maintaining the TEM region at the center. This stack was subsequently polished on the cross-section to a thickness of ∼ 200 μm. A 3 mm disc was then cut perpendicular to the cross-section using a Gatan ultrasonic cutter. The disc was polished then dimpled on both sides to a thickness of ∼ 15 μm. This was ion-beam milled at liquid nitrogen temperature to an electron-transparent layer. From a comparison of in-situ and ex-situ measurements of the recrystallization rate, the actual sample temperature during in-situ characterization was estimated to deviate by ≤ 20 deg C from that of the heated holder. The influence of electron-irradiation was found to be negligible by comparing the recrystallization rate and microstructure of irradiated and unirradiated regions of comparable thickness. Similarly, the influence of the 'thin-foil effect' was found to be negligible by comparing the recrystallization rate and microstructure of thick and thin regions, the former determined after the removal of the sample from the microscope and further ion-beam milling of tens of microns of material. In conclusion, the potential influence of artifacts during in-situ TEM can be minimized by the appropriate choice of sample preparation procedures. (authors)

Thermal and Hydrothermal Treatment of Silica Gels as Solid Stationary Phases in Gas Chromatography

Directory of Open Access Journals (Sweden)

Ashraf Yehia El-Naggar

2013-01-01

Full Text Available Silica gel was prepared and treated thermally and hydrothermally and was characterized as solid stationary phase in gas chromatography. The characteristics have been evaluated in terms of polarity, selectivity, and separation efficiencies. These parameters were used to assess the outer silica surface contributions and the degree of surface deactivation brought about by different treatment techniques. The parent silica elutes the paraffinic hydrocarbons with high efficiency of separation and elutes aromatic hydrocarbons with nearly good separation and has bad separation of alcohols. The calcined silica at 500°C and 1000°C has a pronounced effect on the separation of aromatic hydrocarbons compared with the parent silica and hydrothermal treatment of silica. With respect to alcohols separation, the obtained bad separations using treated and untreated silica reflect the little effect of the thermal and hydrothermal treatment on the silica surface deactivation.

The electron spectrum of UF6 recorded in the gas phase

Science.gov (United States)

Mârtensson, N.; Malmquist, P.-Å.; Svensson, S.; Johansson, B.

1984-06-01

Gas phase core and valence electron spectra from UF6, excited by AlKα monochromatized x rays, in the binding energy range 0-1000 eV are presented. It is shown that the AlKα excited valence electron spectrum can be used to reassign the highest occupied molecular orbital (HOMO) in UF6. Many-body effects on the core levels are discussed and core level lifetimes are determined. The shift between solid phase and gas phase electron binding energies for core lines is used to discuss the U5 f population in UF6.

A comparative study of transport properties in polycrystalline and epitaxial chromium nitride films

KAUST Repository

Duan, X. F.

2013-01-08

Polycrystalline CrNx films on Si(100) and glass substrates and epitaxial CrNx films on MgO(100) substrates were fabricated by reactive sputtering with different nitrogen gas flow rates (fN2). With the increase of fN2, a lattice phase transformation from metallic Cr2N to semiconducting CrN appears in both polycrystalline and epitaxial CrNx films. At fN2= 100 sccm, the low-temperature conductance mechanism is dominated by both Mott and Efros-Shklovskii variable-range hopping in either polycrystalline or epitaxial CrN films. In all of the polycrystalline and epitaxial films, only the polycrystalline CrNx films fabricated at fN2 = 30 and 50 sccm exhibit a discontinuity in ρ(T) curves at 260-280 K, indicating that both the N-vacancy concentration and grain boundaries play important roles in the metal-insulator transition. © 2013 American Institute of Physics.

Fast thermal annealing of implantation defects in silicon. Solid phase epitaxy and residual imperfection recovery

International Nuclear Information System (INIS)

Adekoya, O.A.

1987-06-01

Basic processes ruling the crystal reconstitution in solid phase during fast thermal annealing are studied; the role of electronic and thermodynamic effects at the interface is precised, following the implantations of a donor element (p + ), an acceptor element (B + ) and an intrinsic element (Ge + ). Then, after recrystallization, the electric role of residual point defects is shown together with the possibility of total recovery and an important electric activation of the doping [fr

Flow regimes in vertical gas-solid contact systems

Energy Technology Data Exchange (ETDEWEB)

Yerushalmi, J.; Cankurt, N. T.; Geldart, D.; Liss, B.

1976-01-01

The flow characteristics in fluidized beds, i.e., gas-solid systems, was studied to determine the flow regimes, the interaction of gas and solid in the various flow regimes and the dependence of this interaction and of transition between flow regimes on the properties of the gas and solid, on the gas and solid flow rates, and on the containing vessel. Fluidized beds with both coarse and fine particles are considered. Test results using high speed photography to view the operation of a 2-dimensional bed are discussed. (LCL)

Nanoselective area growth of GaN by metalorganic vapor phase epitaxy on 4H-SiC using epitaxial graphene as a mask

International Nuclear Information System (INIS)

Puybaret, Renaud; Jordan, Matthew B.; Voss, Paul L.; Ougazzaden, Abdallah; Patriarche, Gilles; Sundaram, Suresh; El Gmili, Youssef; Salvestrini, Jean-Paul; Heer, Walt A. de; Berger, Claire

2016-01-01

We report the growth of high-quality triangular GaN nanomesas, 30-nm thick, on the C-face of 4H-SiC using nanoselective area growth (NSAG) with patterned epitaxial graphene grown on SiC as an embedded mask. NSAG alleviates the problems of defects in heteroepitaxy, and the high mobility graphene film could readily provide the back low-dissipative electrode in GaN-based optoelectronic devices. A 5–8 graphene-layer film is first grown on the C-face of 4H-SiC by confinement-controlled sublimation of silicon carbide. Graphene is then patterned and arrays of 75-nm-wide openings are etched in graphene revealing the SiC substrate. A 30-nm-thick GaN is subsequently grown by metal organic vapor phase epitaxy. GaN nanomesas grow epitaxially with perfect selectivity on SiC, in the openings patterned through graphene. The up-or-down orientation of the mesas on SiC, their triangular faceting, and cross-sectional scanning transmission electron microscopy show that they are biphasic. The core is a zinc blende monocrystal surrounded with single-crystal wurtzite. The GaN crystalline nanomesas have no threading dislocations or V-pits. This NSAG process potentially leads to integration of high-quality III-nitrides on the wafer scalable epitaxial graphene/silicon carbide platform.

Nanoselective area growth of GaN by metalorganic vapor phase epitaxy on 4H-SiC using epitaxial graphene as a mask

Energy Technology Data Exchange (ETDEWEB)

Puybaret, Renaud; Jordan, Matthew B.; Voss, Paul L.; Ougazzaden, Abdallah, E-mail: aougazza@georgiatech-metz.fr [School of Electrical and Computer Engineering, Georgia Institute of Technology, Atlanta, Georgia 30332 (United States); CNRS UMI 2958, Georgia Institute of Technology, 2 Rue Marconi, 57070 Metz (France); Patriarche, Gilles [CNRS, Laboratoire de Photonique et de Nanostructures, Route de Nozay, 91460 Marcoussis (France); Sundaram, Suresh; El Gmili, Youssef [CNRS UMI 2958, Georgia Institute of Technology, 2 Rue Marconi, 57070 Metz (France); Salvestrini, Jean-Paul [Université de Lorraine, CentraleSupélec, LMOPS, EA4423, 57070 Metz (France); Heer, Walt A. de [School of Physics, Georgia Institute of Technology, Atlanta, Georgia 30332 (United States); Berger, Claire [School of Physics, Georgia Institute of Technology, Atlanta, Georgia 30332 (United States); CNRS, Institut Néel, BP166, 38042 Grenoble Cedex 9 (France)

2016-03-07

We report the growth of high-quality triangular GaN nanomesas, 30-nm thick, on the C-face of 4H-SiC using nanoselective area growth (NSAG) with patterned epitaxial graphene grown on SiC as an embedded mask. NSAG alleviates the problems of defects in heteroepitaxy, and the high mobility graphene film could readily provide the back low-dissipative electrode in GaN-based optoelectronic devices. A 5–8 graphene-layer film is first grown on the C-face of 4H-SiC by confinement-controlled sublimation of silicon carbide. Graphene is then patterned and arrays of 75-nm-wide openings are etched in graphene revealing the SiC substrate. A 30-nm-thick GaN is subsequently grown by metal organic vapor phase epitaxy. GaN nanomesas grow epitaxially with perfect selectivity on SiC, in the openings patterned through graphene. The up-or-down orientation of the mesas on SiC, their triangular faceting, and cross-sectional scanning transmission electron microscopy show that they are biphasic. The core is a zinc blende monocrystal surrounded with single-crystal wurtzite. The GaN crystalline nanomesas have no threading dislocations or V-pits. This NSAG process potentially leads to integration of high-quality III-nitrides on the wafer scalable epitaxial graphene/silicon carbide platform.

Deliberate and Accidental Gas-Phase Alkali Doping of Chalcogenide Semiconductors: Cu(In,Ga)Se2.

Science.gov (United States)

Colombara, Diego; Berner, Ulrich; Ciccioli, Andrea; Malaquias, João C; Bertram, Tobias; Crossay, Alexandre; Schöneich, Michael; Meadows, Helene J; Regesch, David; Delsante, Simona; Gigli, Guido; Valle, Nathalie; Guillot, Jérome; El Adib, Brahime; Grysan, Patrick; Dale, Phillip J

2017-02-24

Alkali metal doping is essential to achieve highly efficient energy conversion in Cu(In,Ga)Se 2 (CIGSe) solar cells. Doping is normally achieved through solid state reactions, but recent observations of gas-phase alkali transport in the kesterite sulfide (Cu 2 ZnSnS 4 ) system (re)open the way to a novel gas-phase doping strategy. However, the current understanding of gas-phase alkali transport is very limited. This work (i) shows that CIGSe device efficiency can be improved from 2% to 8% by gas-phase sodium incorporation alone, (ii) identifies the most likely routes for gas-phase alkali transport based on mass spectrometric studies, (iii) provides thermochemical computations to rationalize the observations and (iv) critically discusses the subject literature with the aim to better understand the chemical basis of the phenomenon. These results suggest that accidental alkali metal doping occurs all the time, that a controlled vapor pressure of alkali metal could be applied during growth to dope the semiconductor, and that it may have to be accounted for during the currently used solid state doping routes. It is concluded that alkali gas-phase transport occurs through a plurality of routes and cannot be attributed to one single source.

The leaf volatile constituents of Isatis tinctoria by Solid-Phase Microextraction and Gas chromatography/Mass Spectrometry.

Science.gov (United States)

Condurso, Cettina; Verzera, Antonella; Romeo, Vincenza; Ziino, Marisa; Trozzi, Alessandra; Ragusa, Salvatore

2006-08-01

The leaf volatile constituents of Isatis tinctoria L. (Brassicaceae) have been studied by Solid-Phase Microextraction and Gas chromatography/Mass Spectrometry (SPME/GC-MS). Seventy components were fully characterized by mass spectra, linear retention indices, and injection of standards; the average composition (ppm) as single components and classes of substances is reported. Aliphatic hydrocarbons, acids, alcohols, aldehydes and esters, aromatic aldehydes, esters and ethers, furans, isothiocyanates and thiocyanates, sulfurated compounds, nitriles, terpenes and sesquiterpenes were identified. Leaf volatiles in Isatis tinctoria L. were characterized by a high amount of isothiocyanates which accounted for about 40 % of the total volatile fraction. Isothiocyanates are important and characteristic flavour compounds in Brassica vegetables and the cancer chemo-protective attributes are recently responsible for their growing interest.

Vapor-phase etching of InP using anhydrous HCl and PH/sub 3/ gas

International Nuclear Information System (INIS)

Pak, K.; Koide, Y.; Imai, K.; Yoshida, A.; Nakamura, T.; Yasuda, Y.; Nishinaga, T.

1986-01-01

In situ etching of the substrate surface for vapor-phase epitaxy is a useful technique for obtaining a smooth and damage-free surface prior to the growth. Previous work showed that the incorporation of in situ etching of InP substrate with anhydrous HCl gas resulted in a significant improvement in the surface morphologies for MOVPE-grown InGaAs/InP and InP epitaxial layers. However, the experiment on the HCl etching of the InP substrate for a wide temperature range has not been performed as yet. In this note, the authors describe the effect of the substrate temperature on the etching morphology of InP substrate by using the anhydrous HCl and PH/sub 3/ gases. In the experiment, they used a standard MOVPE horizontal system. A quartz reactor tube in a 60 mm ID, 60 cm long, was employed

Epitaxial graphene

Science.gov (United States)

de Heer, Walt A.; Berger, Claire; Wu, Xiaosong; First, Phillip N.; Conrad, Edward H.; Li, Xuebin; Li, Tianbo; Sprinkle, Michael; Hass, Joanna; Sadowski, Marcin L.; Potemski, Marek; Martinez, Gérard

2007-07-01

Graphene multilayers are grown epitaxially on single crystal silicon carbide. This system is composed of several graphene layers of which the first layer is electron doped due to the built-in electric field and the other layers are essentially undoped. Unlike graphite the charge carriers show Dirac particle properties (i.e. an anomalous Berry's phase, weak anti-localization and square root field dependence of the Landau level energies). Epitaxial graphene shows quasi-ballistic transport and long coherence lengths; properties that may persist above cryogenic temperatures. Paradoxically, in contrast to exfoliated graphene, the quantum Hall effect is not observed in high-mobility epitaxial graphene. It appears that the effect is suppressed due to the absence of localized states in the bulk of the material. Epitaxial graphene can be patterned using standard lithography methods and characterized using a wide array of techniques. These favorable features indicate that interconnected room temperature ballistic devices may be feasible for low-dissipation high-speed nanoelectronics.

Magnetic micro-solid-phase extraction based on magnetite-MCM-41 with gas chromatography-mass spectrometry for the determination of antidepressant drugs in biological fluids.

Science.gov (United States)

Kamaruzaman, Sazlinda; Sanagi, Mohd Marsin; Yahaya, Noorfatimah; Wan Ibrahim, Wan Aini; Endud, Salasiah; Wan Ibrahim, Wan Nazihah

2017-11-01

A new facile magnetic micro-solid-phase extraction coupled to gas chromatography and mass spectrometry detection was developed for the extraction and determination of selected antidepressant drugs in biological fluids using magnetite-MCM-41 as adsorbent. The synthesized sorbent was characterized by several spectroscopic techniques. The maximum extraction efficiency for extraction of 500 μg/L antidepressant drugs from aqueous solution was obtained with 15 mg of magnetite-MCM-41 at pH 12. The analyte was desorbed using 100 μL of acetonitrile prior to gas chromatography determination. This method was rapid in which the adsorption procedure was completed in 60 s. Under the optimized conditions using 15 mL of antidepressant drugs sample, the calibration curve showed good linearity in the range of 0.05-500 μg/L (r 2  = 0.996-0.999). Good limits of detection (0.008-0.010 μg/L) were obtained for the analytes with good relative standard deviations of solid-phase extraction with gas chromatography and mass spectrometry is a convenient, fast, and economical method for the extraction and determination of amitriptyline and chlorpromazine in biological samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Dielectric relaxation in epitaxial films of paraelectric-magnetic SrTiO.sub.3./sub.-SrMnO.sub.3./sub. solid solution

Czech Academy of Sciences Publication Activity Database

Savinov, Maxim; Bovtun, Viktor; Tereshina-Chitrova, Evgenia; Stupakov, Alexandr; Dejneka, Alexandr; Tyunina, Marina

2018-01-01

Roč. 112, č. 5 (2018), s. 1-4, č. článku 052901. ISSN 0003-6951 R&D Projects: GA ČR GA15-15123S Institutional support: RVO:68378271 Keywords : dielectric relaxation * epitaxial films * paraelectric-magnetic * SrTiO 3 -SrMnO 3 solid solution Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics , supercond.) Impact factor: 3.411, year: 2016

Determination of amphetamine-type stimulants in oral fluid by solid-phase microextraction and gas chromatography-mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Souza, Daniele Z., E-mail: daniele.dzs@dpf.gov.br [Setor Tecnico-Cientifico, Superintendencia Regional do Departamento de Policia Federal no Rio Grande do Sul, 1365 Ipiranga Avenue, Azenha, Zip Code 90160-093 Porto Alegre, Rio Grande do Sul (Brazil); Programa de Pos-Graduacao em Ciencias Farmaceuticas, Faculdade de Farmacia, Universidade Federal do Rio Grande do Sul, 2752 Ipiranga Avenue, Santana, Zip Code 90610-000 Porto Alegre, Rio Grande do Sul (Brazil); Boehl, Paula O.; Comiran, Eloisa; Mariotti, Kristiane C. [Programa de Pos-Graduacao em Ciencias Farmaceuticas, Faculdade de Farmacia, Universidade Federal do Rio Grande do Sul, 2752 Ipiranga Avenue, Santana, Zip Code 90610-000 Porto Alegre, Rio Grande do Sul (Brazil); Pechansky, Flavio [Centro de Pesquisa em Alcool e Drogas (CPAD), Hospital de Clinicas de Porto Alegre, Universidade Federal do Rio Grande do Sul, 2350, Ramiro Barcelos Street, Zip Code 90035-903 Porto Alegre, Rio Grande do Sul (Brazil); Duarte, Paulina C.A.V. [Secretaria Nacional de Politicas sobre Drogas (SENAD), Esplanada dos Ministerios, Block ' A' , 5th floor, Zip Code 70050-907 Brasilia, Distrito Federal (Brazil); De Boni, Raquel [Centro de Pesquisa em Alcool e Drogas (CPAD), Hospital de Clinicas de Porto Alegre, Universidade Federal do Rio Grande do Sul, 2350, Ramiro Barcelos Street, Zip Code 90035-903 Porto Alegre, Rio Grande do Sul (Brazil); Froehlich, Pedro E.; Limberger, Renata P. [Programa de Pos-Graduacao em Ciencias Farmaceuticas, Faculdade de Farmacia, Universidade Federal do Rio Grande do Sul, 2752 Ipiranga Avenue, Santana, Zip Code 90610-000 Porto Alegre, Rio Grande do Sul (Brazil)

2011-06-24

Graphical abstract: Highlights: > Propylchloroformate derivatization of amphetamine-type stimulants in oral fluid. > Direct immersion solid-phase microextraction/gas chromatography-mass spectrometry. > Linear range 2(4)-256 ng mL{sup -1}, detection limits 0.5-2 ng mL{sup -1}. > Accuracy 98-112%, precision <15% of RSD, recovery 77-112%. > Importance of residual evaluation in checking model goodness-of-fit. - Abstract: A method for the simultaneous identification and quantification of amphetamine (AMP), methamphetamine (MET), fenproporex (FEN), diethylpropion (DIE) and methylphenidate (MPH) in oral fluid collected with Quantisal{sup TM} device has been developed and validated. Thereunto, in-matrix propylchloroformate derivatization followed by direct immersion solid-phase microextraction and gas chromatography-mass spectrometry were employed. Deuterium labeled AMP was used as internal standard for all the stimulants and analysis was performed using the selected ion monitoring mode. The detector response was linear for the studied drugs in the concentration range of 2-256 ng mL{sup -1} (neat oral fluid), except for FEN, whereas the linear range was 4-256 ng mL{sup -1}. The detection limits were 0.5 ng mL{sup -1} (MET), 1 ng mL{sup -1} (MPH) and 2 ng mL{sup -1} (DIE, AMP, FEN), respectively. Accuracy of quality control samples remained within 98.2-111.9% of the target concentrations, while precision has not exceeded 15% of the relative standard deviation. Recoveries with Quantisal{sup TM} device ranged from 77.2% to 112.1%. Also, the goodness-of-fit concerning the ordinary least squares model in the statistical inference of data has been tested through residual plotting and ANOVA. The validated method can be easily automated and then used for screening and confirmation of amphetamine-type stimulants in drivers' oral fluid.

Thin film phase diagram of iron nitrides grown by molecular beam epitaxy

Science.gov (United States)

Gölden, D.; Hildebrandt, E.; Alff, L.

2017-01-01

A low-temperature thin film phase diagram of the iron nitride system is established for the case of thin films grown by molecular beam epitaxy and nitrided by a nitrogen radical source. A fine-tuning of the nitridation conditions allows for growth of α ‧ -Fe8Nx with increasing c / a -ratio and magnetic anisotropy with increasing x until almost phase pure α ‧ -Fe8N1 thin films are obtained. A further increase of nitrogen content below the phase decomposition temperature of α ‧ -Fe8N (180 °C) leads to a mixture of several phases that is also affected by the choice of substrate material and symmetry. At higher temperatures (350 °C), phase pure γ ‧ -Fe4N is the most stable phase.

Control growth of silicon nanocolumns' epitaxy on silicon nanowires

Energy Technology Data Exchange (ETDEWEB)

Chong, Su Kong, E-mail: sukong1985@yahoo.com.my [University of Malaya, Low Dimensional Materials Research Centre, Department of Physics (Malaysia); Dee, Chang Fu [Universiti Kebangsaan Malaysia (UKM), Institute of Microengineering and Nanoelectronics (IMEN) (Malaysia); Yahya, Noorhana [Universiti Teknologi PETRONAS, Faculty of Science and Information Technology (Malaysia); Rahman, Saadah Abdul [University of Malaya, Low Dimensional Materials Research Centre, Department of Physics (Malaysia)

2013-04-15

The epitaxial growth of Si nanocolumns on Si nanowires was studied using hot-wire chemical vapor deposition. A single-crystalline and surface oxide-free Si nanowire core (core radius {approx}21 {+-} 5 nm) induced by indium crystal seed was used as a substance for the vapor phase epitaxial growth. The growth process is initiated by sidewall facets, which then nucleate upon certain thickness to form Si islands and further grow to form nanocolumns. The Si nanocolumns with diameter of 10-20 nm and aspect ratio up to 10 can be epitaxially grown on the surface of nanowires. The results showed that the radial growth rate of the Si nanocolumns remains constant with the increase of deposition time. Meanwhile, the radial growth rates are controllable by manipulating the hydrogen to silane gas flow rate ratio. The optical antireflection properties of the Si nanocolumns' decorated SiNW arrays are discussed in the text.

Analysis of volatile organic compounds in pleural effusions by headspace solid-phase microextraction coupled with cryotrap gas chromatography and mass spectrometry.

Science.gov (United States)

Huang, Zhongping; Zhang, Jie; Zhang, Peipei; Wang, Hong; Pan, Zaifa; Wang, Lili

2016-07-01

Headspace solid-phase microextraction coupled with cryotrap gas chromatography and mass spectrometry was applied to the analysis of volatile organic compounds in pleural effusions. The highly volatile organic compounds were separated successfully with high sensitivity by the employment of a cryotrap device, with the construction of a cold column head by freezing a segment of metal capillary with liquid nitrogen. A total of 76 volatile organic compounds were identified in 50 pleural effusion samples (20 malignant effusions and 30 benign effusions). Among them, 34 more volatile organic compounds were detected with the retention time less than 8 min, by comparing with the normal headspace solid-phase microextraction coupled with gas chromatography and mass spectrometry method. Furthermore, 24 volatile organic compounds with high occurrence frequency in pleural effusion samples, 18 of which with the retention time less than 8 min, were selected for the comparative analysis. The results of average peak area comparison and box-plot analysis showed that except for cyclohexanone, 2-ethyl-1-hexanol, and tetramethylbenzene, which have been reported as potential cancer biomarkers, cyclohexanol, dichloromethane, ethyl acetate, n-heptane, ethylbenzene, and xylene also had differential expression between malignant and benign effusions. Therefore, the proposed approach was valuable for the comprehensive characterization of volatile organic compounds in pleural effusions. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Excitons in the rare gas solids

International Nuclear Information System (INIS)

1988-01-01

Excitons play a prominent role in the chemistry and physics of condensed matter. Excitons in the rare gas solids, the prototypical van der Waals insulators, will be the focus of the remainder of this report. The goal here is to investigate the controversies surrounding the description of excitons in insulators and, therefore the simplest class of these solids, namely the rare gas solids, is chosen as the exemplary system. Specific problems associated with molecular crystals are, therefore, avoided and only the salient features of excitons are thus considered. 47 refs., 9 figs., 4 tabs

Formation of (111) orientation-controlled ferroelectric orthorhombic HfO{sub 2} thin films from solid phase via annealing

Energy Technology Data Exchange (ETDEWEB)

Mimura, Takanori; Katayama, Kiliha [Department of Innovative and Engineered Materials, Tokyo Institute of Technology, Yokohama 226-8502 (Japan); Shimizu, Takao [Materials Research Center for Element Strategy, Tokyo Institute of Technology, Yokohama 226-8503 (Japan); Uchida, Hiroshi [Department of Materials and Life Sciences, Sophia University, Tokyo 102-8554 (Japan); Kiguchi, Takanori; Akama, Akihiro; Konno, Toyohiko J. [Institute for Materials Research, Tohoku University, Sendai 980-8577 (Japan); Sakata, Osami [Synchrotron X-ray Station at SPring-8 and Synchrotron X-ray Group, National Institute for Materials Science, Sayo, Hyogo 679-5148 (Japan); Funakubo, Hiroshi, E-mail: funakubo.h.aa@m.titech.ac.jp [Department of Innovative and Engineered Materials, Tokyo Institute of Technology, Yokohama 226-8502 (Japan); Materials Research Center for Element Strategy, Tokyo Institute of Technology, Yokohama 226-8503 (Japan); School of Materials and Chemical Technology, Tokyo Institute of Technology, Yokohama 226-8502 (Japan)

2016-08-01

0.07YO{sub 1.5}-0.93HfO{sub 2} (YHO7) films were prepared on various substrates by pulse laser deposition at room temperature and subsequent heat treatment to enable a solid phase reaction. (111)-oriented 10 wt. % Sn-doped In{sub 2}O{sub 3}(ITO)//(111) yttria-stabilized zirconia, (111)Pt/TiO{sub x}/SiO{sub 2}/(001)Si substrates, and (111)ITO/(111)Pt/TiO{sub x}/SiO{sub 2}/(001)Si substrates were employed for film growth. In this study, X-ray diffraction measurements including θ–2θ measurements, reciprocal space mappings, and pole figure measurements were used to study the films. The film on (111)ITO//(111)yttria-stabilized zirconia was an (111)-orientated epitaxial film with ferroelectric orthorhombic phase; the film on (111)ITO/(111)Pt/TiO{sub x}/SiO{sub 2}/(001)Si was an (111)-oriented uniaxial textured film with ferroelectric orthorhombic phase; and no preferred orientation was observed for the film on the (111)Pt/TiO{sub x}/SiO{sub 2}/(001)Si substrate, which does not contain ITO. Polarization–hysteresis measurements confirmed that the films on ITO covered substrates had saturated ferroelectric hysteresis loops. A remanent polarization (P{sub r}) of 9.6 and 10.8 μC/cm{sup 2} and coercive fields (E{sub c}) of 1.9 and 2.0 MV/cm were obtained for the (111)-oriented epitaxial and uniaxial textured YHO7 films, respectively. These results demonstrate that the (111)-oriented ITO bottom electrodes play a key role in controlling the orientation and ferroelectricity of the phase formation of the solid films deposited at room temperature.

Evolution of weak perturbations in gas-solid suspension with chemical reaction

Energy Technology Data Exchange (ETDEWEB)

Sharypov, O.V. [Russian Academy of Sciences, Novosibirsk (Russian Federation). Inst. of Thermophysics; Novosibirsk State Univ. (Russian Federation); Anufriev, I.S. [Novosibirsk State Univ. (Russian Federation)

2013-07-01

Dynamics of weak finite-amplitude perturbations in two-phase homogeneous medium (gas + solid particles) with non-equilibrium chemical reaction in gas is studied theoretically. Non-linear model of plane perturbation evolution is substantiated. The model takes into account wave-kinetic interaction and dissipation effects, including inter-phase heat and momentum transfer. Conditions for uniform state of the system are analyzed. Non-linear equation describing evolution of plane perturbation is derived under weak dispersion and dissipation effects. The obtained results demonstrate self-organization in the homogeneous system: steady-state periodic structure arises, its period, amplitude and velocity depends on the features of the medium. The dependencies of these parameters on dissipation and chemical kinetics are analyzed.

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

Directory of Open Access Journals (Sweden)

Mergheni Ali Mohamed

2008-01-01

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

Growth of CrTe thin films by molecular-beam epitaxy

International Nuclear Information System (INIS)

Sreenivasan, M.G.; Hou, X.J.; Teo, K.L.; Jalil, M.B.A.; Liew, T.; Chong, T.C.

2006-01-01

We report the growth of Cr 1-δ Te films on (100) GaAs substrates using ZnTe buffer layers by solid-source molecular-beam epitaxial technique. RHEED patterns indicate a clear structural change during the initial stages of deposition. Temperature-dependent magnetization results reveal that different NiAs-related phases of Cr 1-δ Te can be obtained at different substrate temperatures. By varying the film thickness, a metastable zinc blende structure of CrTe could be obtained at lower substrate temperature

Determination of Low Concentrations of Acetochlor in Water by Automated Solid-Phase Extraction and Gas Chromatography with Mass-Selective Detection

Science.gov (United States)

Lindley, C.E.; Stewart, J.T.; Sandstrom, M.W.

1996-01-01

A sensitive and reliable gas chromatographic/mass spectrometric (GC/MS) method for determining acetochlor in environmental water samples was developed. The method involves automated extraction of the herbicide from a filtered 1 L water sample through a C18 solid-phase extraction column, elution from the column with hexane-isopropyl alcohol (3 + 1), and concentration of the extract with nitrogen gas. The herbicide is quantitated by capillary/column GC/MS with selected-ion monitoring of 3 characteristic ions. The single-operator method detection limit for reagent water samples is 0.0015 ??g/L. Mean recoveries ranged from about 92 to 115% for 3 water matrixes fortified at 0.05 and 0.5 ??g/L. Average single-operator precision, over the course of 1 week, was better than 5%.

Determination of amphetamine-type stimulants (ATSs) and synthetic cathinones in urine using solid phase micro-extraction fibre tips and gas chromatography-mass spectrometry

OpenAIRE

Alsenedi, Khalid A.; Morrison, Calum

2018-01-01

In recent years, an increasing number of stimulant drugs and new psychoactive substances (NPSs) have caused concern in scientific communities and therefore innovative methods to extract compounds from complex biological samples are required. This work is aimed at developing and validating a clean, convenient and straightforward extraction procedure with microliter amounts of organic solvent using Solid Phase Micro-Extraction tips (SPME tips) and analysis using Gas Chromatography-Mass Spectrom...

Epitaxial GaN around ZnO nanopillars

Energy Technology Data Exchange (ETDEWEB)

Fikry, Mohamed; Scholz, Ferdinand [Institut fuer Optoelektronik, Universitaet Ulm, Albert-Einstein-Allee 45, 89081 Ulm (Germany); Madel, Manfred; Tischer, Ingo; Thonke, Klaus [Institut fuer Quantenmaterie, Universitaet Ulm, Albert-Einstein-Allee 45, 89081 Ulm (Germany)

2011-07-01

We report on an investigation of the epitaxial quality of GaN layers overgrown coaxially around ZnO nanopillars. In a first step, regularly arranged ZnO nanopillars were grown using pre-patterning by e-beam lithography or self-organized hexagonal polystyrene sphere masks. Alternatively, ZnO pillars were also successfully grown on top of GaN pyramids. In a second step, GaN layers were grown around the ZnO pillars by Metal Organic Vapor Phase Epitaxy. At growth temperatures above 800 C, the ZnO pillars are dissolved by the hydrogen carrier gas leaving hollow GaN nanotubes. Characterization involved photoluminescence (PL), scanning electron microscopy and cathodoluminescence. The fair quality of the deposited GaN layers is confirmed by a sharp low temperature PL peak at 3.48 eV attributed to the donor bound exciton emission. Further peaks at 3.42 eV and 3.29 eV show the possible existence of basal plane and prismatic stacking faults.

Ultrasonic detection of solid phase mass flow ratio of pneumatic conveying fly ash

Science.gov (United States)

Duan, Guang Bin; Pan, Hong Li; Wang, Yong; Liu, Zong Ming

2014-04-01

In this paper, ultrasonic attenuation detection and weight balance are adopted to evaluate the solid mass ratio in this paper. Fly ash is transported on the up extraction fluidization pneumatic conveying workbench. In the ultrasonic test. McClements model and Bouguer-Lambert-Beer law model were applied to formulate the ultrasonic attenuation properties of gas-solid flow, which can give the solid mass ratio. While in the method of weigh balance, the averaged mass addition per second can reveal the solids mass flow ratio. By contrast these two solid phase mass ratio detection methods, we can know, the relative error is less.

Gas phase ion chemistry

CERN Document Server

Bowers, Michael T

1979-01-01

Gas Phase Ion Chemistry, Volume 2 covers the advances in gas phase ion chemistry. The book discusses the stabilities of positive ions from equilibrium gas-phase basicity measurements; the experimental methods used to determine molecular electron affinities, specifically photoelectron spectroscopy, photodetachment spectroscopy, charge transfer, and collisional ionization; and the gas-phase acidity scale. The text also describes the basis of the technique of chemical ionization mass spectrometry; the energetics and mechanisms of unimolecular reactions of positive ions; and the photodissociation

Epitaxial lateral overgrowth - a tool for dislocation blockade in multilayer system

International Nuclear Information System (INIS)

Zytkiewicz, Z.R.

1998-01-01

Results on epitaxial lateral overgrowth of GaAs layers are reported. The methods of controlling the growth anisotropy, the effect of substrate defects filtration in epitaxial lateral overgrowth procedure and influence of the mask on properties of epitaxial lateral overgrowth layers will be discussed. The case od GaAs epitaxial lateral overgrowth layers grown by liquid phase epitaxy on heavily dislocated GaAs substrates was chosen as an example to illustrate the processes discussed. The similarities between our results and those reported recently for GaN layers grown laterally by metalorganic vapour phase epitaxy will be underlined. (author)

Epitaxial growth and electronic structure of a layered zinc pnictide semiconductor, β-BaZn2As2

International Nuclear Information System (INIS)

Xiao, Zewen; Ran, Fan-Yong; Hiramatsu, Hidenori; Matsuishi, Satoru; Hosono, Hideo; Kamiya, Toshio

2014-01-01

BaZn 2 As 2 is expected for a good p-type semiconductor and has two crystalline phases of an orthorhombic α phase and a higher-symmetry tetragonal β phase. Here, we report that high-quality epitaxial films of the tetragonal β-BaZn 2 As 2 were grown on single-crystal MgO (001) substrates by a reactive solid-phase epitaxy technique. Out-of-plane and in-plane epitaxial relationships between the film and the substrate were BaZn 2 As 2 (00 l)//MgO (001) and BaZn 2 As 2 [200]//MgO [200], respectively. The full-widths at half maximum were 0.082° for a 008 out-of-plane rocking curve and 0.342° for a 200 in-plane rocking curve. A step-and-terrace structure was observed by atomic force microscopy. The band gap of β-BaZn 2 As 2 was evaluated to be around 0.2 eV, which is much smaller than that of a family compound LaZnOAs (1.5 eV). Density functional theory calculation using the Heyd–Scuseria–Ernzerhof hybrid functionals supports the small band gap. - Highlights: • High-quality epitaxial β-BaZn 2 As 2 films were obtained. • The band gap of β-BaZn 2 As 2 was evaluated to around 0.2 eV. • Hybrid Heyd–Scuseria–Ernzerhof calculation supports the small band gap

Epitaxial growth of hybrid nanostructures

Science.gov (United States)

Tan, Chaoliang; Chen, Junze; Wu, Xue-Jun; Zhang, Hua

2018-02-01

Hybrid nanostructures are a class of materials that are typically composed of two or more different components, in which each component has at least one dimension on the nanoscale. The rational design and controlled synthesis of hybrid nanostructures are of great importance in enabling the fine tuning of their properties and functions. Epitaxial growth is a promising approach to the controlled synthesis of hybrid nanostructures with desired structures, crystal phases, exposed facets and/or interfaces. This Review provides a critical summary of the state of the art in the field of epitaxial growth of hybrid nanostructures. We discuss the historical development, architectures and compositions, epitaxy methods, characterization techniques and advantages of epitaxial hybrid nanostructures. Finally, we provide insight into future research directions in this area, which include the epitaxial growth of hybrid nanostructures from a wider range of materials, the study of the underlying mechanism and determining the role of epitaxial growth in influencing the properties and application performance of hybrid nanostructures.

Solid phase stability of molybdenum under compression: Sound velocity measurements and first-principles calculations

Energy Technology Data Exchange (ETDEWEB)

Zhang, Xiulu [Laboratory for Shock Wave and Detonation Physics Research, Institute of Fluid Physics, P.O. Box 919-102, 621900 Mianyang, Sichuan (China); Laboratory for Extreme Conditions Matter Properties, Southwest University of Science and Technology, 621010 Mianyang, Sichuan (China); Liu, Zhongli [Laboratory for Shock Wave and Detonation Physics Research, Institute of Fluid Physics, P.O. Box 919-102, 621900 Mianyang, Sichuan (China); College of Physics and Electric Information, Luoyang Normal University, 471022 Luoyang, Henan (China); Jin, Ke; Xi, Feng; Yu, Yuying; Tan, Ye; Dai, Chengda; Cai, Lingcang [Laboratory for Shock Wave and Detonation Physics Research, Institute of Fluid Physics, P.O. Box 919-102, 621900 Mianyang, Sichuan (China)

2015-02-07

The high-pressure solid phase stability of molybdenum (Mo) has been the center of a long-standing controversy on its high-pressure melting. In this work, experimental and theoretical researches have been conducted to check its solid phase stability under compression. First, we performed sound velocity measurements from 38 to 160 GPa using the two-stage light gas gun and explosive loading in backward- and forward-impact geometries, along with the high-precision velocity interferometry. From the sound velocities, we found no solid-solid phase transition in Mo before shock melting, which does not support the previous solid-solid phase transition conclusion inferred from the sharp drops of the longitudinal sound velocity [Hixson et al., Phys. Rev. Lett. 62, 637 (1989)]. Then, we searched its structures globally using the multi-algorithm collaborative crystal structure prediction technique combined with the density functional theory. By comparing the enthalpies of body centered cubic structure with those of the metastable structures, we found that bcc is the most stable structure in the range of 0–300 GPa. The present theoretical results together with previous ones greatly support our experimental conclusions.

Trace-level determination of polar flavour compounds in butter by solid-phase extraction and gas chromatography-mass spectrometry.

Science.gov (United States)

Adahchour, M; Vreuls, R J; van der Heijden, A; Brinkman, U A

1999-06-04

Volatile compounds are responsible for the aromas of butter. A simple technique for the determination of these components is described which is based on solid-phase extraction (SPE) after melting of the butter and separation of the aqueous phase from the fat. Volatile flavours present in the water fraction are collected by off-line SPE on cartidges packed with a copolymer sorbent. After desorption with 500 microliters of methyl acetate, 1-microliter aliquots are quantified and/or identified by gas chromatography-mass spectrometry. The procedure was tested with respect to recovery, linearity and limit of detection in real-life samples using five polar model analytes. It allows the characterisation of polar flavour compounds in butter prior to and after heat treatment at 170 degrees C. From the five model compounds, vanillin, traces of diacetyl and maltol were found to be present in the butter samples. After heat treatment 500-1000-fold increased concentration of maltol, and substantial amounts of furaneol were detected.

Characterization of the Key Aroma Compounds in Proso Millet Wine Using Headspace Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry

Directory of Open Access Journals (Sweden)

Jingke Liu

2018-02-01

Full Text Available The volatile compounds in proso millet wine were extracted by headspace solid-phase microextraction (85 μm polyacrylate (PA, 100 μm polydimethylsiloxane (PDMS, 75 μm Carboxen (CAR/PDMS, and 50/30 μm divinylbenzene (DVB/CAR/PDMS fibers, and analyzed using gas chromatography-mass spectrometry; the odor characteristics and intensities were analyzed by the odor activity value (OAV. Different sample preparation factors were used to optimize this method: sample amount, extraction time, extraction temperature, and content of NaCl. A total of 64 volatile compounds were identified from the wine sample, including 14 esters, seven alcohols, five aldehydes, five ketones, 12 benzene derivatives, 12 hydrocarbons, two terpenes, three phenols, two acids, and two heterocycles. Ethyl benzeneacetate, phenylethyl alcohol, and benzaldehyde were the main volatile compounds found in the samples. According to their OAVs, 14 volatile compounds were determined to be odor-active compounds (OAV > 1, and benzaldehyde, benzeneacetaldehyde, 1-methyl-naphthalene, 2-methyl-naphthalene, and biphenyl were the prominent odor-active compounds (OAV > 50, having a high OAV. Principal component analysis (PCA showed the difference of distribution of the 64 volatile compounds and 14 odor-active compounds with four solid-phase microextraction (SPME fibers.

Solid-solid phase transitions in Fe nanowires induced by axial strain

International Nuclear Information System (INIS)

Sandoval, Luis; Urbassek, Herbert M

2009-01-01

By means of classical molecular-dynamics simulations we investigate the solid-solid phase transition from a bcc to a close-packed crystal structure in cylindrical iron nanowires, induced by axial strain. The interatomic potential employed has been shown to be capable of describing the martensite-austenite phase transition in iron. We study the stress versus strain curves for different temperatures and show that for a range of temperatures it is possible to induce a solid-solid phase transition by axial strain before the elasticity is lost; these transition temperatures are below the bulk transition temperature. The two phases have different (non-linear) elastic behavior: the bcc phase softens, while the close-packed phase stiffens with temperature. We also consider the reversibility of the transformation in the elastic regimes, and the role of the strain rate on the critical strain necessary for phase transition.

Position-controlled epitaxial III-V nanowires on silicon

NARCIS (Netherlands)

Roest, A.L.; Verheijen, M.A.; Wunnicke, O.; Serafin, S.N.; Wondergem, H.J.; Bakkers, E.P.A.M.

2006-01-01

We show the epitaxial integration of III-V semiconductor nanowires with silicon technology. The wires are grown by the VLS mechanism with laser ablation as well as metal-organic vapour phase epitaxy. The hetero-epitaxial growth of the III-V nanowires on silicon was confirmed with x-ray diffraction

Formation of organic solid phases in hydrocarbon reservoir fluids. Final report

Energy Technology Data Exchange (ETDEWEB)

Andersen, S.I.; Lindeloff, N.; Stenby, E.H.

1998-12-31

The occurrence of solid phases during oil recovery is a potential problem. The present work has mainly been concerned with wax formation due to cooling of oils with a large paraffin content. 8 oils have been included in this project, although only a few of these have till now been subject to all the experimental techniques applied. The oils and wax fractions from these have been characterized using techniques such as GC-MS and Ftir. The goal has in part been to get a detailed description of the oil composition for use in model evaluation and development and in part to get a fundamental understanding of waxy oil properties and behaviour. A high pressure (200 bar) equipment has been developed for automatic detection of wax appearance using a filtration technique and laser light turbidimetry. The latter was found to be far superior to the filtration. The filtration was used to sample the incipient solid phase for characterization. However entrapment of liquid in the filters currently used have hampered this part. A number of model systems and one gas condensate have been investigated. The GC-MS procedure was found only to been able to detect molecules up to n-C45 and the group type analysis was not accurate enough for modelling purposes. Using Ftir it was obvious that incipient phases may contain very complex molecules (asphaltenes) which are not captured by GC-MS especially when fractionation is done using the acetone precipitation at elevated temperature. The latter fractionation procedure has been investigated thoroughly as a tool for understanding wax distribution etc. Within thermodynamic modelling a delta lattice parameter model has been developed which incorporates the non-ideality of the solid phases into the calculation of SLE. The non-ideality is estimated from pure component properties. A new algorithm for phase equilibria involving gas-liquid-solid has been developed. Currently both the model work and the experimental works are continued. (au)

[Determination of short chain chlorinated paraffins in leather products by solid phase extraction coupled with gas chromatography-mass spectrometry].

Science.gov (United States)

Zhang, Weiya; Wan, Xin; Li, Lixia; Wang, Chengyun; Jin, Shupei; Xing, Jun

2014-10-01

The short chain chlorinated paraffins (SCCPs) are the additives frequently used in the leather production in China, but they have been put into the list of forbidden chemicals issued by European Union recently. In fact, there is not a commonly recognized method for the determination of the SCCPs in the leather products due to the serious matrix interferences from the leather products and the complex chemical structures of the SCCPs. A method of solid phase extraction coupled with gas chromatography-mass spectrometry (SPE-GC-MS) was established for the determination of the SCCPs in the leather products after the optimization of the SPE conditions. It was found that the interferences from the leather products were thor- oughly separated from the analyte of the SCCPs on a home-made solid phase extraction (SPE) column filled with silica packing while eluted with a mixed solvent of n-hexane-methylene chloride (2:1, v/v). With this method, the recoveries for the SCCPs spiked in the real leather samples varied from 90.47% to 99.00% with the relative standard deviations (RSDs) less than 6.7%, and the limits of detection (LODs) were between 0.069 and 0.110 mg/kg. This method is suitable for qualitative and quantitative analysis of SCCPs in the leather products.

The potential for the fabrication of wires embedded in the crystalline silicon substrate using the solid phase segregation of gold in crystallising amorphous volumes

International Nuclear Information System (INIS)

Liu, A.C.Y.; McCallum, J.C.

2004-01-01

The refinement of gold in crystallising amorphous silicon volumes was tested as a means of creating a conducting element embedded in the crystalline matrix. Amorphous silicon volumes were created by self-ion-implantation through a mask. Five hundred kiloelectronvolt Au + was then implanted into the volumes. The amorphous volumes were crystallised on a hot stage in air, and the crystallisation was characterised using cross sectional transmission electron microscopy. It was found that the amorphous silicon volumes crystallised via solid phase epitaxy at all the lateral and vertical interfaces. The interplay of the effects of the gold and also the hydrogen that infilitrated from the surface oxide resulted in a plug of amorphous material at the surface. Further annealing at this temperature demonstrated that the gold, once it had reached a certain critical concentration nucleated poly-crystalline growth instead of solid phase epitaxy. Time resolved reflectivity and Rutherford backscattering and channeling measurements were performed on large area samples that had been subject to the same implantation regime to investigate this system further. It was discovered that the crystallisation dynamics and zone refinement of the gold were complicated functions of both gold concentration and temperature. These findings do not encourage the use of this method to obtain conducting elements embedded in the crystalline silicon substrate

Determination of some volatile compounds in alcoholic beverage by headspace solid-phase microextraction gas chromatography - mass spectrometry

Science.gov (United States)

Schmutzer, G.; Avram, V.; Feher, I.; David, L.; Moldovan, Z.

2012-02-01

The volatile composition of alcoholic beverage was studied by headspace solid-phase microextraction (HSSPME) method and gas chromatography - mass spectrometry (GC-MS). Some volatile compounds, such as alcohols, esters, terpenes and other are mainly responsible for the flavor of fortified wines and their amounts specify the quality of the alcoholic beverages. From this perspective it is interesting to develop a rapid, selective and sensitive analytical method suitable for simultaneous quantification of the main molecules being responsible for the organoleptic characteristic of alcoholic beverages. Vermouth fortified drink was analyzed in order to characterize the volatile profile. Using the HS-SPME/GC-MS a number of twenty-six volatile compounds from a commercial market alcoholic beverage were identified. The most abundant compounds were m-thymol, o-thymol and eugenol, alongside of the ethyl ester compounds.

High sensitive quasi freestanding epitaxial graphene gas sensor on 6H-SiC

NARCIS (Netherlands)

Iezhokin, I.; Offermans, P.; Brongersma, S.H.; Giesbers, A.J.M.; Flipse, C.F.J.

2013-01-01

We have measured the electrical response to NO2, N2, NH3, and CO for epitaxial graphene and quasi freestanding epitaxial graphene on 6H-SiC substrates. Quasi freestanding epitaxial graphene shows a 6 fold increase in NO2 sensitivity compared to epitaxial graphene. Both samples show a sensitivity

Stabilisation of late transition metal and noble metal films in hexagonal and body centred tetragonal phases by epitaxial growth

Energy Technology Data Exchange (ETDEWEB)

Hueger, E.

2005-08-26

In this work ultrathin metallic films with a crystal phase different to their natural bulk structure were produced by hetero-epitaxial growth on metallic substrates. A further aim of this work was to understand the initiation, growth and stability of crystal phase modifications of these films. there exist cases where the films turn beyond the pseudomorphic-growth to a crystal phase different from their natural bulk structure. The present work presents and discusses such a case in addition to the general phenomenon of pseudomorphic-growth. In particular it is shown that metals whose natural phase is face centred cubic (fcc) can be grown in body centred tetragonal (bct) or hexagonal close packed (hcp) phases in the form of thin films on (001) surfaces of appropriate substrates. The growth behavior, electron diffraction analysis, appearance conditions, geometric fit considerations, examples and a discussion of the phase stability of non-covered films and superlattices is given reviewing all epitaxial-systems whose diffraction pattern can be explained by the hexagonal or pseudomorphic bct phase. (orig.)

Industrial aspects of gas-liquid two-phase flow

International Nuclear Information System (INIS)

Hewitt, G.F.

1977-01-01

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

Epitaxial rare-earth superlattices and films

International Nuclear Information System (INIS)

Salamon, M.B.; Beach, R.S.; Flynn, C.P.; Matheny, A.; Tsui, F.; Rhyne, J.J.

1992-01-01

This paper reports on epitaxial growth of rare-earth superlattices which is demonstrated to have opened important new areas of research on magnetic materials. The propagation magnetic order through non-magnetic elements, including its range and anisotropy, has been studied. The importance of magnetostriction in determining the phase diagram is demonstrated by the changes induced by epitaxial clamping. The cyrstallinity of epitaxial superlattices provides the opportunity to study interfacial magnetism by conventional x-ray and neutron scattering methods

Influence of Bubble-Bubble interactions on the macroscale circulation patterns in a bubbling gas-solid fluidized bed

NARCIS (Netherlands)

Laverman, J.A.; van Sint Annaland, M.; Kuipers, J.A.M.

2007-01-01

The macro-scale circulation patterns in the emulsion phase of a gas-solid fluidized bed in the bubbling regime have been studied with a 3D Discrete Bubble Model. It has been shown that bubble-bubble interactions strongly influence the extent of the solids circulation and the bubble size

Contact line motion in confined liquid–gas systems: Slip versus phase transition

KAUST Repository

Xu, Xinpeng

2010-11-30

In two-phase flows, the interface intervening between the two fluid phases intersects the solid wall at the contact line. A classical problem in continuum fluid mechanics is the incompatibility between the moving contact line and the no-slip boundary condition, as the latter leads to a nonintegrable stress singularity. Recently, various diffuse-interface models have been proposed to explain the contact line motion using mechanisms missing from the sharp-interface treatments in fluid mechanics. In one-component two-phase (liquid–gas) systems, the contact line can move through the mass transport across the interface while in two-component (binary) fluids, the contact line can move through diffusive transport across the interface. While these mechanisms alone suffice to remove the stress singularity, the role of fluid slip at solid surface needs to be taken into account as well. In this paper, we apply the diffuse-interface modeling to the study of contact line motion in one-component liquid–gas systems, with the fluid slip fully taken into account. The dynamic van der Waals theory has been presented for one-component fluids, capable of describing the two-phase hydrodynamics involving the liquid–gas transition [A. Onuki, Phys. Rev. E 75, 036304 (2007)]. This theory assumes the local equilibrium condition at the solid surface for density and also the no-slip boundary condition for velocity. We use its hydrodynamicequations to describe the continuum hydrodynamics in the bulk region and derive the more general boundary conditions by introducing additional dissipative processes at the fluid–solid interface. The positive definiteness of entropy production rate is the guiding principle of our derivation. Numerical simulations based on a finite-difference algorithm have been carried out to investigate the dynamic effects of the newly derived boundary conditions, showing that the contact line can move through both phase transition and slip, with their relative

Liquid phase epitaxy of abrupt junctions in InAs and studies of injection radiative tunneling processes

International Nuclear Information System (INIS)

Bull, D.J.

1977-01-01

The p-n junction in a InAs crystal, by liquid phase epitaxy is obtained. The processes of injection and tunneling radiative recombination by emitted radiation from active region of p-n junction for low injection current are studied. (M.C.K.) [pt

Synthesis of Si epitaxial layers from technical silicon by liquid-phase epitaxy method

International Nuclear Information System (INIS)

Ibragimov, Sh.I.; Saidov, A.S.; Sapaev, B.; Horvat, M.A.

2004-01-01

Full text: For today silicon is one of the most suitable materials because it is investigated, cheap and several its parameters are even just as good as those of connections A III B V . Disintegration of the USSR has led to the must difficult position of the industry of silicon instrument manufacture because of all industry of semiconductor silicon manufacture had generally concentrated in Ukraine. The importance of semiconductor silicon is rather great, because of, in opinion of expects, the nearest decade this material will dominate over not only on microelectronics but also in the majority of basic researches. Research of obtain of semiconductor silicon, power electronics and solar conversion, is topical interest of the science. In the work research of technological conditions of obtain and measurement of parameters of epitaxial layers obtained from technical silicon + stannum is resulted. Growth of silicon epitaxial layer with suitable parameters on thickness, cleanliness uniformity and structural perfection depends on the correct choice of condition of the growth and temperature. It is shown that in this case the growth occurring without preliminary clearing of materials (mix materials and substrates) at crystallization of epitaxial layer from technical silicon is accompanied by clearing of silicon film from majority of impurities order-of-magnitude. As starting raw material technical silicon of mark Kr.3 has been taken. By means of X-ray microanalyzer 'Jeol' JSM 5910 LV - Japan the quantitative analysis from the different points has been and from the different sides and from different points has been carried out. After corresponding chemical and mechanical processing the quantitative analysis of layer on chip has been carried out. Results of the quantitative analysis are shown. More effective clearing occurs that of the impurity atoms such as Al, P, Ca, Ti and Fe. The obtained material (epitaxial layer) has the parameters: specific resistance ρ∼0.1-4.0 �

Solid state gas sensors. Industrial application

Energy Technology Data Exchange (ETDEWEB)

Fleischer, Maximilian [Siemens AG, Muenchen (Germany). Corporate Technology; Lehmann, Mirko (eds.) [Innovative Sensor Technology (IST) AG, Wattwil (Switzerland)

2012-11-01

Written by experts. Richly illustrated. Encourages future research and investments in the fascinating field of gas sensors. Gas sensor products are very often the key to innovations in the fields of comfort, security, health, environment, and energy savings. This compendium focuses on what the research community labels as solid state gas sensors, where a gas directly changes the electrical properties of a solid, serving as the primary signal for the transducer. It starts with a visionary approach to how life in future buildings can benefit from the power of gas sensors. The requirements for various applications, such as for example the automotive industry, are then discussed in several chapters. Further contributions highlight current trends in new sensing principles, such as the use of nanomaterials and how to use new sensing principles for innovative applications in e.g. meteorology. So as to bring together the views of all the different groups needed to produce new gas sensing applications, renowned industrial and academic representatives report on their experiences and expectations in research, applications and industrialisation.

Gas-phase synthesis of semiconductor nanocrystals and its applications

Science.gov (United States)

Mandal, Rajib

photoluminescence (PL), surface analysis, and defect identification indicate the shell is protective against oxidation compared to Si NCs without any shell growth. Gallium Nitride (GaN) is one of the most well-known semiconductor material and the industry standard for fabricating LEDs. The problem is that epitaxial growth of high-quality GaN requires costly substrates (e.g. sapphire), high temperatures, and long processing times. Synthesizing freestanding NCs of GaN, on the other hand, could enable these novel device morphologies, as the NCs could be incorporated into devices without the requirements imposed by epitaxial GaN growth. Synthesis of GaN NCs was performed using a fully gas-phase process. Different sizes of crystalline GaN nanoparticles were produced indicating versatility of this gas-phase process. Elemental analysis using X-ray photoelectron spectroscopy (XPS) indicated a possible nitrogen deficiency in the NCs; addition of secondary plasma for surface treatment indicates improving stoichiometric ratio and points towards a unique method for creating high-quality GaN NCs with ultimate alloying and doping for full-spectrum luminescence.

The gas-solid trickle-flow reactor for the catalytic oxidation of hydrogen sulphide: a trickle-phase model

NARCIS (Netherlands)

Verver, A.B.; van Swaaij, Willibrordus Petrus Maria

1987-01-01

The oxidation of H2S by O2 producing elemental sulphur has been studied at temperatures of 100–300°C and at atmospheric pressure in a laboratory-scale gas-solid trickle-flow reactor. In this reactor one of the reaction products, i.e. sulphur, is removed continuously by flowing solids. A porous,

Phase diagrams of ZnTe-HgTe-Te and ZnTe-CdTe-HgTe-Te systems

International Nuclear Information System (INIS)

Andrukhiv, A.M.; Litvak, A.M.; Mironov, K.E.

1992-01-01

ZnTe-HgTe-Te system liquidus surface is investigated and solid solution layers are produced in this system by the method of liquid-phase epitaxy (LPE). The theoretical analysis of experimental and theoretical data allows to calculate the diagram of ZnTe-CdTe-HgTe-Te system fusibility. A significant effect of elastic stresses of the epitaxial layer, grown on CdTe substrate, on the process of LPE of solid solutions is established

Hydride vapor phase epitaxy growth of GaN, InGaN, ScN, and ScAIN

NARCIS (Netherlands)

Bohnen, T.

2010-01-01

Chemical vapor deposition (CVD); hydride vapor phase epitaxy (HVPE); gallium nitride (GaN); indium gallium nitride (InGaN); scandium nitride (ScN); scandium aluminum nitride (ScAlN); semiconductors; thin films; nanowires; III nitrides; crystal growth - We studied the HVPE growth of different III

Epitaxy-enabled vapor-liquid-solid growth of tin-doped indium oxide nanowires with controlled orientations

KAUST Repository

Shen, Youde

2014-08-13

Controlling the morphology of nanowires in bottom-up synthesis and assembling them on planar substrates is of tremendous importance for device applications in electronics, photonics, sensing and energy conversion. To date, however, there remain challenges in reliably achieving these goals of orientation-controlled nanowire synthesis and assembly. Here we report that growth of planar, vertical and randomly oriented tin-doped indium oxide (ITO) nanowires can be realized on yttria-stabilized zirconia (YSZ) substrates via the epitaxy-assisted vapor-liquid-solid (VLS) mechanism, by simply regulating the growth conditions, in particular the growth temperature. This robust control on nanowire orientation is facilitated by the small lattice mismatch of 1.6% between ITO and YSZ. Further control of the orientation, symmetry and shape of the nanowires can be achieved by using YSZ substrates with (110) and (111), in addition to (100) surfaces. Based on these insights, we succeed in growing regular arrays of planar ITO nanowires from patterned catalyst nanoparticles. Overall, our discovery of unprecedented orientation control in ITO nanowires advances the general VLS synthesis, providing a robust epitaxy-based approach toward rational synthesis of nanowires. © 2014 American Chemical Society.

High-quality single crystalline NiO with twin phases grown on sapphire substrate by metalorganic vapor phase epitaxy

Directory of Open Access Journals (Sweden)

Kazuo Uchida

2012-12-01

Full Text Available High-quality single crystalline twin phase NiO grown on sapphire substrates by metalorganic vapor phase epitaxy is reported. X-ray rocking curve analysis of NiO films grown at different temperatures indicates a minimum full width at half maximum of the cubic (111 diffraction peak of 0.107° for NiO film grown at as low as 550 °C. Detailed microstructural analysis by Φ scan X-ray diffraction and transmission electron microscopy reveal that the NiO film consists of large single crystalline domains with two different crystallographic orientations which are rotated relative to each other along the [111] axis by 60°. These single crystal domains are divided by the twin phase boundaries.

Rare-earth-ion doped KY(WO4)2 optical waveguides grown by liquid-phase epitaxy

NARCIS (Netherlands)

Romanyuk, Y.E.; Apostolopoulos, V.; Utke, U.; Pollnau, Markus

High-quality KY(WO4)2 thin layers doped with rare-earth-ions were grown using liquid-phase epitaxy. A low-temperature mixture of chlorides was used as the flux and undoped KY(WO4)2 crystals as substrates. The crystalline layers possessed thicknesses up to 10 µm. Passive and active planar waveguiding

Growth and characterization of Hg 1– Cd Te epitaxial films by ...

Indian Academy of Sciences (India)

Growth of Hg1–CdTe epitaxial films by a new technique called asymmetric vapour phase epitaxy (ASVPE) has been carried out on CdTe and CZT substrates. The critical problems faced in normal vapour phase epitaxy technique like poor surface morphology, composition gradient and dislocation multiplication have ...

Gas chromatographic-mass spectrometric determination of hydrophilic compounds in environmental water by solid-phase extraction with activated carbon fiber felt.

Science.gov (United States)

Kawata, K; Ibaraki, T; Tanabe, A; Yagoh, H; Shinoda, A; Suzuki, H; Yasuhara, A

2001-03-09

Simple gas chromatographic-mass spectrometric determination of hydrophilic organic compounds in environmental water was developed. A cartridge containing activated carbon fiber felt was made by way of trial and was evaluated for solid-phase extraction of the compounds in water. The hydrophilic compounds investigated were acrylamide, N,N-dimethylacetamide, N,N-dimethylformamide, 1,4-dioxane, furfural, furfuryl alcohol, N-nitrosodiethylamine and N-nitrosodimethylamine. Overall recoveries were good (80-100%) from groundwater and river water. The relative standard deviations ranged from 4.5 to 16% for the target compounds. The minimum detectable concentrations were 0.02 to 0.03 microg/l. This method was successfully applied to several river water samples.

A variational approach to multi-phase motion of gas, liquid and solid based on the level set method

Science.gov (United States)

Yokoi, Kensuke

2009-07-01

We propose a simple and robust numerical algorithm to deal with multi-phase motion of gas, liquid and solid based on the level set method [S. Osher, J.A. Sethian, Front propagating with curvature-dependent speed: Algorithms based on Hamilton-Jacobi formulation, J. Comput. Phys. 79 (1988) 12; M. Sussman, P. Smereka, S. Osher, A level set approach for capturing solution to incompressible two-phase flow, J. Comput. Phys. 114 (1994) 146; J.A. Sethian, Level Set Methods and Fast Marching Methods, Cambridge University Press, 1999; S. Osher, R. Fedkiw, Level Set Methods and Dynamics Implicit Surface, Applied Mathematical Sciences, vol. 153, Springer, 2003]. In Eulerian framework, to simulate interaction between a moving solid object and an interfacial flow, we need to define at least two functions (level set functions) to distinguish three materials. In such simulations, in general two functions overlap and/or disagree due to numerical errors such as numerical diffusion. In this paper, we resolved the problem using the idea of the active contour model [M. Kass, A. Witkin, D. Terzopoulos, Snakes: active contour models, International Journal of Computer Vision 1 (1988) 321; V. Caselles, R. Kimmel, G. Sapiro, Geodesic active contours, International Journal of Computer Vision 22 (1997) 61; G. Sapiro, Geometric Partial Differential Equations and Image Analysis, Cambridge University Press, 2001; R. Kimmel, Numerical Geometry of Images: Theory, Algorithms, and Applications, Springer-Verlag, 2003] introduced in the field of image processing.

Advanced Si solid phase crystallization for vertical channel in vertical NANDs

Directory of Open Access Journals (Sweden)

Sangsoo Lee

2014-07-01

Full Text Available The advanced solid phase crystallization (SPC method using the SiGe/Si bi-layer structure is proposed to obtain high-mobility poly-Si thin-film transistors in next generation vertical NAND (VNAND devices. During the SPC process, the top SiGe thin film acts as a selective nucleation layer to induce surface nucleation and equiaxial microstructure. Subsequently, this SiGe thin film microstructure is propagated to the underlying Si thin film by epitaxy-like growth. The initial nucleation at the SiGe surface was clearly observed by in situ transmission electron microscopy (TEM when heating up to 600 °C. The equiaxial microstructures of both SiGe nucleation and Si channel layers were shown in the crystallized bi-layer plan-view TEM measurements. Based on these experimental results, the large-grained and less-defective Si microstructure is expected to form near the channel region of each VNAND cell transistor, which may improve the electrical characteristics.

Determination of organoarsenicals in the environment by solid-phase microextraction-gas chromatography-mass spectrometry.

Energy Technology Data Exchange (ETDEWEB)

Szostek, B.; Aldstadt, J. H.; Environmental Research

1998-05-22

The development of a method for the analysis of organoarsenic compounds that combines dithiol derivatization with solid-phase microextraction (SPME) sample preparation and gas chromatography-mass spectrometry (GC-MS) is described. Optimization focused on a SPME-GC-MS procedure for determination of 2-chlorovinylarsonous acid (CVAA), the primary decomposition product of the chemical warfare agent known as Lewisite. Two other organoarsenic compounds of environmental interest, dimethylarsinic acid and phenylarsonic acid, were also studied. A series of dithiol compounds was examined for derivatization of the arsenicals, and the best results were obtained either with 1,3-propanedithiol or 1,2-ethanedithiol. The derivatization procedure, fiber type, and extraction time were optimized. For CVAA, calibration curves were linear over three orders of magnitude and limits-of-detection were <6x10{sup -9} M in solution, the latter a more than 400x improvement compared to conventional solvent extraction GC-MS methods. A precision of <10% R.S.D. was typical for the SPME-GC-MS procedure. The method was applied to a series of water samples and soil/sediment extracts, as well as to aged soil samples that had been contaminated with Lewisite.

Solid-phase peptide synthesis

DEFF Research Database (Denmark)

Jensen, Knud Jørgen

2013-01-01

This chapter provides an introduction to and overview of peptide chemistry with a focus on solid-phase peptide synthesis. The background, the most common reagents, and some mechanisms are presented. This chapter also points to the different chapters and puts them into perspective.......This chapter provides an introduction to and overview of peptide chemistry with a focus on solid-phase peptide synthesis. The background, the most common reagents, and some mechanisms are presented. This chapter also points to the different chapters and puts them into perspective....

Validation of mechanistic models for gas precipitation in solids during postirradiation annealing experiments

Science.gov (United States)

Rest, J.

1989-12-01

A number of different phenomenological models for gas precipitation in solids during postirradiation annealing experiments have been proposed. Validation of such mechanistic models for gas release and swelling is complicated by the use of data containing large systematic errors, and phenomena characterized by synergistic effects as well as uncertainties in materials properties. Statistical regression analysis is recommended for the selection of a reasonably well characterized data base for gas release from irradiated fuel under transient heating conditions. It is demonstrated that an appropriate data selection method is required in order to realistically examine the impact of differing descriptions of the phenomena, and uncertainties in selected materials properties, on the validation results. The results of the analysis show that the kinetics of gas precipitation in solids depend on bubble overpressurization effects and need to be accounted for during the heatup phase of isothermal heating experiments. It is shown that if only the total gas release values (as opposed to time-dependent data) were available, differentiation between different gas precipitation models would be ambiguous. The observed sustained increase in the fractional release curve at relatively high temperatures after the total precipitation of intragranular gas in fission gas bubbles is ascribed to the effects of a grain-growth/grain-boundary sweeping mechanism.

Validation of mechanistic models for gas precipitation in solids during postirradiation annealing experiments

International Nuclear Information System (INIS)

Rest, J.

1989-01-01

A number of different phenomenological models for gas precipitation in solids during postirradiation annealing experiments have been proposed. Validation of such mechanistic models for gas release and swelling is complicated by the use of data containing large systematic errors, and phenomena characterized by synergistic effects as well as uncertainties in materials properties. Statistical regression analysis is recommended for the selection of a reasonably well characterized data base for gas release from irradiated fuel under transient heating conditions. It is demonstrated that an appropriate data selection method is required in order to realistically examine the impact of differing descriptions of the phenomena, and uncertainties in selected materials properties, on the validation results. The results of the analysis show that the kinetics of gas precipitation in solid depend on bubble overpressurization effects and need to be accounted for during the heatup phase of isothermal heating experiments. It is shown that if only the total gas release values (as opposed to time-dependent data) were available, differentiation between different gas precipitation models would be ambiguous. The observed sustained increase in the fractional release curve at relatively high temperatures after the total precipitation of intragranular gas in fission gas bubbles is ascribed to the effects of a grain-growth/grain-boundary sweeping mechanism. (orig.)

Numerical simulation of the gas-solid flow in a square circulating fluidized bed with secondary air injection

Energy Technology Data Exchange (ETDEWEB)

Wang, Zhengyang [Harbin Institute of Technology, Harbin (China). Post-doctor Station of Civil Engineering; Harbin Institute of Technology, Harbin (China). Combustion Engineering Research Inst.; Sun, Shaozeng; Zhao, Ningbo; Wu, Shaohua [Harbin Institute of Technology, Harbin (China). Combustion Engineering Research Inst.; Tan, Yufei [Harbin Institute of Technology, Harbin (China). School of Municipal and Environmental Engineering

2013-07-01

The dynamic behavior of gas-solid flow in an experimental square circulating fluidized bed setup (0.25 m x 0.25 m x 6.07 m) is predicted with numerical simulation based on the theory of Euler-Euler gas-solid two-phase flow and the kinetic theory of granular flows. The simulation includes the operation cases with secondary injection and without air-staging. The pressure drop profile, local solids concentration and particle velocity was compared with experimental results. Both simulation and experimental results show that solids concentration increases significantly below the secondary air injection ports when air-staging is adopted. Furthermore, the flow asymmetry in the solid entrance region of the bed was investigated based on the particle concentration/velocity profile. The simulation results are in agreement with the experimental results qualitatively.

Microstructures of GaN1-xPx layers grown on (0001) GaN substrates by gas source molecular beam epitaxy

Science.gov (United States)

Seong, Tae-Yeon; Bae, In-Tae; Choi, Chel-Jong; Noh, D. Y.; Zhao, Y.; Tu, C. W.

1999-03-01

Transmission electron microscope (TEM), transmission electron diffraction (TED), and synchrotron x-ray diffraction (XRD) studies have been performed to investigate microstructural behavior of gas source molecular beam epitaxial GaN1-xPx layers grown on (0001) GaN/sapphire at temperatures (Tg) in the range 500-760 °C. TEM, TED, and XRD results indicate that the samples grown at Tg⩽600 °C undergo phase separation resulting in a mixture of GaN-rich and GaP-rich GaNP with zinc-blende structure. However, the samples grown at Tg⩾730 °C are found to be binary zinc-blende GaN(P) single crystalline materials. As for the 500 °C layer, the two phases are randomly oriented and distributed, whereas the 600 °C layer consists of phases that are elongated and inclined by 60°-70° clockwise from the [0001]α-GaN direction. The samples grown at Tg⩾730 °C are found to consist of two types of microdomains, namely, GaN(P)I and GaN(P)II; the former having twin relation to the latter.

Lateral epitaxial overgrowth of GaN on a patterned GaN-on-silicon substrate by molecular beam epitaxy

International Nuclear Information System (INIS)

Wang, Yongjin; Hu, Fangren; Hane, Kazuhiro

2011-01-01

We report here the lateral epitaxial overgrowth (LEO) of GaN on a patterned GaN-on-silicon substrate by molecular beam epitaxy (MBE) growth with radio frequency nitrogen plasma as a gas source. Two kinds of GaN nanostructures are defined by electron beam lithography and realized on a GaN substrate by fast atom beam etching. The epitaxial growth of GaN by MBE is performed on the prepared GaN template, and the selective growth of GaN takes place with the assistance of GaN nanostructures. The LEO of GaN produces novel GaN epitaxial structures which are dependent on the shape and the size of the processed GaN nanostructures. Periodic GaN hexagonal pyramids are generated inside the air holes, and GaN epitaxial strips with triangular section are formed in the grating region. This work provides a promising way for producing novel GaN-based devices by the LEO of GaN using the MBE technique

Glass bottle sampling solid phase microextraction gas chromatography mass spectrometry for breath analysis of drug metabolites.

Science.gov (United States)

Lu, Yan; Niu, Wenqi; Zou, Xue; Shen, Chengyin; Xia, Lei; Huang, Chaoqun; Wang, Hongzhi; Jiang, Haihe; Chu, Yannan

2017-05-05

Breath analysis is a non-invasive approach which may be applied to disease diagnosis and pharmacokinetic study. In the case of offline analysis, the exhaled gas needs to be collected and the sampling bag is often used as the storage vessel. However, the sampling bag usually releases some extra compounds, which may interfere with the result of the breath test. In this study, a novel breath sampling glass bottle was developed with a syringe needle sampling port for solid phase microextraction (SPME). Such a glass bottle scarcely liberates compounds and can be used to collect exhaled gas for ensuing analysis by gas chromatography-mass spectrometry (GC-MS). The glass bottle sampling SPME-GC-MS analysis was carried out to investigate the breath metabolites of myrtol, a multicompound drug normally used in the treatment of bronchitis and sinusitis. Four compounds, α-pinene, 2,3-dehydro-1,8-cineole, d-limonene and 1,8-cineole were found in the exhaled breath of all eight volunteers who had taken the myrtol. While for other ten subjects who had not used the myrtol, these compounds were undetectable. In the SPME-GC-MS analysis of the headspace of myrtol, three compounds were detected including α-pinene, d-limonene and 1,8-cineole. Comparing the results of breath and headspace analysis, it indicates that 2,3-dehydro-1,8-cineole in the breath is the metabolite of 1,8-cineole. It is the first time that this metabolite was identified in human breath. The study demonstrates that the glass bottle sampling SPME-GC-MS method is applicable to exhaled gas analysis including breath metabolites investigation of drugs like myrtol. Copyright © 2017 Elsevier B.V. All rights reserved.

An investigation of particle behavior in gas-solid horizontal pipe flow by an extended LDA technique

Energy Technology Data Exchange (ETDEWEB)

Yong Lu; Donald H. Glass; William J. Easson [University of Edinburgh, Edinburgh (United Kingdom). Institute for Materials and Processes

2009-12-15

An extended Laser Doppler Anemometry (LDA) technique has been developed to measure the distributions of particle velocities and particle number rates over a whole pipe cross-section in a dilute pneumatic conveying system. The first extension concentrates on the transform matrix for predicting the laser beams' cross point in a pipe according to the shift coordinate of the 3D computer-controlled traverse system on which the probes of the LDA system were mounted. The second focuses on the proper LDA sample rate for the measurement of gas-solid pipe flow with polydisperse particles. A suitable LDA sample rate should ensure that enough data is recorded in the measurement interval to precisely calculate the particle mean velocity or other statistical values at every sample point. The present study explores the methodology as well as the fundamentals of measurements, using a laser facility, of the cross-sectional distributions of solid phase. In the horizontal gas-solid pipe flow (glass beads less than 110 {mu}m), the experimental data show that the cross-sectional flow patterns of the solid phase can be classified by annulus-like flow describing the axial particle velocity contours and stratified flow characterising particle number rate distribution over a cross-section. Thus, the cross-sectional flow pattern of the solid phase in a horizontal pipe may be annular or stratified dependent on whether the axial particle velocity or particle number rate is the phenomenon studied. 13 refs., 16 figs., 1 tab.

Solid-phase characterization in flammable-gas-tank sludges by electron microscopy

International Nuclear Information System (INIS)

Liu, J.; Pederson, L.R.; Qang, L.Q.

1995-09-01

The crystallinity, morphology, chemical composition, and crystalline phases of several Tank 241-SY-101 (hereinafter referred to as SY-101) and Tank 241-SY-103 (hereinafter referred to as SY-103) solid samples were studied by transmission electron microscopy (TEM), electron energy dispersive spectroscopy (EDS), and electron diffraction. The main focus is on the identification of aluminum hydroxide thought to be present in these tank samples. Aluminum hydroxide was found in SY-103, but not in SY-101. This difference can be explained by the different OH/Al ratios found in the two tank samples: a high OH/Al ratio in SY-101 favors the formation of sodium aluminate, but a low OH/Al ratio in SY-103 favors aluminum hydroxide. These results were confirmed by a magnetic resonance study on SY-101 and SY-103 simulant. The transition from aluminum hydroxide to sodium aluminate occurs at an OH/Al molar ratio of 3.6. It is believed that the study of Al(OH) 3 was not affected by sample preparation because all Al(OH) 3 is in the solid form according to the NMR experiments. There is no Al(OH) 3 in the liquid. It is, therefore, most likely that the observation of Al(OH) 3 is representative of the real sludge sample, and is not affected by drying. Similar conclusions also apply to other insoluble phases such as iron and chromium

Preparation and characterization of a novel polymeric based solid-solid phase change heat storage material

International Nuclear Information System (INIS)

Xi Peng; Gu Xiaohua; Cheng Bowen; Wang Yufei

2009-01-01

Here we reported a two-step procedure for preparing a novel polymeric based solid-solid phase change heat storage material. Firstly, a copolymer monomer containing a polyethylene glycol monomethyl ether (MPEG) phase change unit and a vinyl unit was synthesized via the modification of hydrogen group of MPEG. Secondly, by copolymerization of the copolymer monomer and phenyl ethylene, a novel polymeric based solid-solid phase change heat storage material was prepared. The composition, structure and properties of the novel polymeric based solid-solid phase change material were characterized by IR, 1 H NMR, DSC, WAXD, and POM, respectively. The results show that the novel polymeric based solid-solid phase change material possesses of excellent crystal properties and high phase change enthalpy.

Development of an interface for directly coupled solid-phase extraction and GC-MS analysis

NARCIS (Netherlands)

Öllers, M.J.H.; van Lieshout, H.P.M.; Janssen, J.G.M.; Cramers, C.A.M.G.

Solid-phase extraction (SPE) is widely used as a sample preparation technique in numerous application areas of chromatography. Large-volume injection is an attractive technique for coupling SPE to gas chromatography (GC) because it provides improved detection limits and circumvents the need for

Gas Phase Nanoparticle Synthesis

Science.gov (United States)

Granqvist, Claes; Kish, Laszlo; Marlow, William

This book deals with gas-phase nanoparticle synthesis and is intended for researchers and research students in nanomaterials science and engineering, condensed matter physics and chemistry, and aerosol science. Gas-phase nanoparticle synthesis is instrumental to nanotechnology - a field in current focus that raises hopes for environmentally benign, resource-lean manufacturing. Nanoparticles can be produced by many physical, chemical, and even biological routes. Gas-phase synthesis is particularly interesting since one can achieve accurate manufacturing control and hence industrial viability.

Rapid screening of selective serotonin re-uptake inhibitors in urine samples using solid-phase microextraction gas chromatography-mass spectrometry.

Science.gov (United States)

Salgado-Petinal, Carmen; Lamas, J Pablo; Garcia-Jares, Carmen; Llompart, Maria; Cela, Rafael

2005-07-01

In this paper a solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS) method is proposed for a rapid analysis of some frequently prescribed selective serotonin re-uptake inhibitors (SSRI)-venlafaxine, fluvoxamine, mirtazapine, fluoxetine, citalopram, and sertraline-in urine samples. The SPME-based method enables simultaneous determination of the target SSRI after simple in-situ derivatization of some of the target compounds. Calibration curves in water and in urine were validated and statistically compared. This revealed the absence of matrix effect and, in consequence, the possibility of quantifying SSRI in urine samples by external water calibration. Intra-day and inter-day precision was satisfactory for all the target compounds (relative standard deviation, RSD, detection limits achieved were detected and tentatively identified.

Effect of crystal orientation on the phase diagrams, dielectric and piezoelectric properties of epitaxial BaTiO3 thin films

Directory of Open Access Journals (Sweden)

Huaping Wu

2016-01-01

Full Text Available The influence of crystal orientations on the phase diagrams, dielectric and piezoelectric properties of epitaxial BaTiO3 thin films has been investigated using an expanded nonlinear thermodynamic theory. The calculations reveal that crystal orientation has significant influence on the phase stability and phase transitions in the misfit strain-temperature phase diagrams. In particular, the (110 orientation leads to a lower symmetry and more complicated phase transition than the (111 orientation in BaTiO3 films. The increase of compressive strain will dramatically enhance the Curie temperature TC of (110-oriented BaTiO3 films, which matches well with previous experimental data. The polarization components experience a great change across the boundaries of different phases at room temperature in both (110- and (111-oriented films, which leads to the huge dielectric and piezoelectric responses. A good agreement is found between the present thermodynamics calculation and previous first-principles calculations. Our work provides an insight into how to use crystal orientation, epitaxial strain and temperature to tune the structure and properties of ferroelectrics.

Different Mechanism Effect between Gas-Solid and Liquid-Solid Interface on the Three-Phase Coexistence Hydrate System Dissociation in Seawater: A Molecular Dynamics Simulation Study

Directory of Open Access Journals (Sweden)

Zhixue Sun

2017-12-01

Full Text Available Almost 98% of methane hydrate is stored in the seawater environment, the study of microscopic mechanism for methane hydrate dissociation on the sea floor is of great significance to the development of hydrate production, involving a three-phase coexistence system of seawater (3.5% NaCl + hydrate + methane gas. The molecular dynamics method is used to simulate the hydrate dissociation process. The dissociation of hydrate system depends on diffusion of methane molecules from partially open cages and a layer by layer breakdown of the closed cages. The presence of liquid or gas phases adjacent to the hydrate has an effect on the rate of hydrate dissociation. At the beginning of dissociation process, hydrate layers that are in contact with liquid phase dissociated faster than layers adjacent to the gas phase. As the dissociation continues, the thickness of water film near the hydrate-liquid interface became larger than the hydrate-gas interface giving more resistance to the hydrate dissociation. Dissociation rate of hydrate layers adjacent to gas phase gradually exceeds the dissociation rate of layers adjacent to the liquid phase. The difficulty of methane diffusion in the hydrate-liquid side also brings about change in dissociation rate.

Growth and characterization of Hg1–xCdxTe epitaxial films by ...

Indian Academy of Sciences (India)

Unknown

Abstract. Growth of Hg1–xCdxTe epitaxial films by a new technique called asymmetric vapour phase epitaxy. (ASVPE) has been carried out on CdTe and CZT substrates. The critical problems faced in normal vapour phase epitaxy technique like poor surface morphology, composition gradient and dislocation multiplication.

Vapor-solid-solid growth mechanism driven by an epitaxial match between solid Au Zn alloy catalyst particle and Zn O nano wire at low temperature

International Nuclear Information System (INIS)

Campos, Leonardo C.; Tonezzer, Matteo; Ferlauto, Andre S.; Magalhaes-Paniago, Rogerio; Oliveira, Sergio; Ladeira, Luiz O.; Lacerda, Rodrigo G.

2008-01-01

Nowadays, the growth of nano materials, like nano wires and nano tubes, is one of the key research areas of nano technology. However, a full picture of the growth mechanism of these quasi-one dimensional systems still needs to be achieved if these materials are to be applied electronics, biology and medicinal fields. Nevertheless, in spite of considerable advances on the growth of numerous nano wires, a clear understanding of the growth mechanism is still controversial and highly discussed. The present work provides a comprehensive picture of the precise mechanism of Zn O vapor-solid-solid (VSS) nano wire growth at low temperatures and gives the fundamental reasons responsible. We demonstrate by using a combination of synchrotron XRD and high resolution TEM that the growth dynamics at low temperatures is not governed by the well-known vapor-liquid solid (VLS) mechanisms. A critical new insight on the driving factor of VSS growth is proposed in which the VSS process occurs by a solid diffusion mechanism that is driven by a preferential oxidation process of the Zn inside the alloy catalyst induced by an epitaxial match between the Zn O(10-10) plane and the γ-Au Zn(222) plane. We believe that these results are not only important for the understanding of Zn O nano wire growth but could also have significant impact on the understanding of growth mechanisms of other nano wire systems. (author)

Investigations on the emission of fragrance allergens from scented toys by means of headspace solid-phase microextraction gas chromatography-mass spectrometry.

Science.gov (United States)

Masuck, Ines; Hutzler, Christoph; Luch, Andreas

2010-04-30

In the revised European toy safety directive 2009/48/EC the application of fragrance allergens in children's toys is restricted. The focus of the present work lies on the instrumental analytics of 13 banned fragrance allergens, as well as on 11 fragrance allergens that require declaration when concentrations surpass 100 microg per gram material. Applying a mixture of ethyl acetate and toluene solid/liquid extraction was performed prior to quantitative analysis of mass contents of fragrances in scented toys. In addition, an easy-to-perform method for the determination of emitted fragrances at 23 degrees C (handling conditions) or at 40 degrees C (worst case scenario) has been worked out to allow for the evaluation of potential risks originating from inhalation of these compounds during handling of or playing with toys. For this purpose a headspace solid-phase microextraction (HS-SPME) technique was developed and coupled to subsequent gas chromatography-mass spectrometry (GC-MS) analysis. Fragrance allergens were adsorbed (extracted) from the gas phase onto an 85 microm polyacrylate fiber while incubating pieces of the scented toys in sealed headspace vials at 23 degrees C and 40 degrees C. Quantification of compounds was performed via external calibration. The newly developed headspace method was subsequently applied to five perfumed toys. As expected, the emission of fragrance allergens from scented toys depends on the temperature and on the content of fragrance allergens present in those samples. In particular at conditions mimicking worst case (40 degrees C), fragrance allergens in toys may pose a risk to children since considerable amounts of compound might be absorbed by lung tissue via breathing of contaminated air. 2010 Elsevier B.V. All rights reserved.

Solid-state harmonics beyond the atomic limit.

Science.gov (United States)

Ndabashimiye, Georges; Ghimire, Shambhu; Wu, Mengxi; Browne, Dana A; Schafer, Kenneth J; Gaarde, Mette B; Reis, David A

2016-06-23

Strong-field laser excitation of solids can produce extremely nonlinear electronic and optical behaviour. As recently demonstrated, this includes the generation of high harmonics extending into the vacuum-ultraviolet and extreme-ultraviolet regions of the electromagnetic spectrum. High harmonic generation is shown to occur fundamentally differently in solids and in dilute atomic gases. How the microscopic mechanisms in the solid and the gas differ remains a topic of intense debate. Here we report a direct comparison of high harmonic generation in the solid and gas phases of argon and krypton. Owing to the weak van der Waals interaction, rare (noble)-gas solids are a near-ideal medium in which to study the role of high density and periodicity in the generation process. We find that the high harmonic generation spectra from the rare-gas solids exhibit multiple plateaus extending well beyond the atomic limit of the corresponding gas-phase harmonics measured under similar conditions. The appearance of multiple plateaus indicates strong interband couplings involving multiple single-particle bands. We also compare the dependence of the solid and gas harmonic yield on laser ellipticity and find that they are similar, suggesting the importance of electron-hole recollision in these solids. This implies that gas-phase methods such as polarization gating for attosecond pulse generation and orbital tomography could be realized in solids.

Laboratory Studies on the Formation of Carbon-Bearing Molecules in Extraterrestrial Environments: From the Gas Phase to the Solid State

Science.gov (United States)

Jamieson, C. S.; Guo, Y.; Gu, X.; Zhang, F.; Bennett, C. J.; Kaiser, R. I.

2006-01-01

A detailed knowledge of the formation of carbon-bearing molecules in interstellar ices and in the gas phase of the interstellar medium is of paramount interest to understand the astrochemical evolution of extraterrestrial environments (1). This research also holds strong implications to comprehend the chemical processing of Solar System environments such as icy planets and their moons together with the atmospheres of planets and their satellites (2). Since the present composition of each interstellar and Solar System environment reflects the matter from which it was formed and the processes which have changed the chemical nature since the origin (solar wind, planetary magnetospheres, cosmic ray exposure, photolysis, chemical reactions), a detailed investigation of the physicochemical mechanisms altering the pristine environment is of paramount importance to grasp the contemporary composition. Once these underlying processes have been unraveled, we can identify those molecules, which belonged to the nascent setting, distinguish molecular species synthesized in a later stage, and predict the imminent chemical evolution of, for instance, molecular clouds. Laboratory experiments under controlled physicochemical conditions (temperature, pressure, chemical composition, high energy components) present ideal tools for simulating the chemical evolution of interstellar and Solar System environments. Here, laboratory experiments can predict where and how (reaction mechanisms; chemicals necessary) in extraterrestrial environments and in the interstellar medium complex, carbon bearing molecules can be formed on interstellar grains and in the gas phase. This paper overviews the experimental setups utilized in our laboratory to mimic the chemical processing of gas phase and solid state (ices) environments. These are a crossed molecular beams machine (3) and a surface scattering setup (4). We also present typical results of each setup (formation of amino acids, aldehydes, epoxides

YBa2Cu3O7-δ/NdBa2(Cu1-xNix)3O7-δ double layers by liquid-phase epitaxial growth

International Nuclear Information System (INIS)

Yao, X.; Izumi, Toru; Hobara, Natsuro; Nakamura, Yuichi; Izumi, Teruo; Shiohara, Yuh

2001-01-01

Our present investigation has answered questions pertaining to the REBa 2 Cu 3 O 7-δ (RE123, RE=rare-earth elements)-coated conductor application when NdBa 2 (Cu 1-x Ni x ) 3 O 7-δ (Ni-NdBCO) solid solution is used as a buffer layer by the liquid-phase epitaxy(LPE) process. The NiO/Ni substrate has no substantial reaction in the Ni-saturated Nd-Ba-Cu-O liquid. There is no essential Ni interdiffusion between YBa 2 Cu 3 O 7-δ (YBCO) and Ni-NdBCO LPE thick films as evident from T c values of 90 K obtained from multilayer YBCO/Ni-NdBCO samples. (author)

Advanced fabrication method for the preparation of MOF thin films: Liquid-phase epitaxy approach meets spin coating method.

KAUST Repository

Chernikova, Valeriya; Shekhah, Osama; Eddaoudi, Mohamed

2016-01-01

Here we report a new and advanced method for the fabrication of highly oriented/polycrystalline metal-organic framework (MOF) thin films. Building on the attractive features of the liquid-phase epitaxy (LPE) approach, a facile spin coating method

Multiplexed Colorimetric Solid-Phase Extraction

Science.gov (United States)

Gazda, Daniel B.; Fritz, James S.; Porter, Marc D.

2009-01-01

Multiplexed colorimetric solid-phase extraction (MC-SPE) is an extension of colorimetric solid-phase extraction (C-SPE) an analytical platform that combines colorimetric reagents, solid phase extraction, and diffuse reflectance spectroscopy to quantify trace analytes in water. In CSPE, analytes are extracted and complexed on the surface of an extraction membrane impregnated with a colorimetric reagent. The analytes are then quantified directly on the membrane surface using a handheld diffuse reflectance spectrophotometer. Importantly, the use of solid-phase extraction membranes as the matrix for impregnation of the colorimetric reagents creates a concentration factor that enables the detection of low concentrations of analytes in small sample volumes. In extending C-SPE to a multiplexed format, a filter holder that incorporates discrete analysis channels and a jig that facilitates the concurrent operation of multiple sample syringes have been designed, enabling the simultaneous determination of multiple analytes. Separate, single analyte membranes, placed in a readout cartridge create unique, analyte-specific addresses at the exit of each channel. Following sample exposure, the diffuse reflectance spectrum of each address is collected serially and the Kubelka-Munk function is used to quantify each water quality parameter via calibration curves. In a demonstration, MC-SPE was used to measure the pH of a sample and quantitate Ag(I) and Ni(II).

p-type ZnO films with solid-source phosphorus doping by molecular-beam epitaxy

International Nuclear Information System (INIS)

Xiu, F.X.; Yang, Z.; Mandalapu, L.J.; Liu, J.L.; Beyermann, W. P.

2006-01-01

Phosphorus-doped p-type ZnO films were grown on r-plane sapphire substrates using molecular-beam epitaxy with a solid-source GaP effusion cell. X-ray diffraction spectra and reflection high-energy electron diffraction patterns indicate that high-quality single crystalline (1120) ZnO films were obtained. Hall and resistivity measurements show that the phosphorus-doped ZnO films have high hole concentrations and low resistivities at room temperature. Photoluminescence (PL) measurements at 8 K reveal a dominant acceptor-bound exciton emission with an energy of 3.317 eV. The acceptor energy level of the phosphorus dopant is estimated to be 0.18 eV above the valence band from PL spectra, which is also consistent with the temperature dependence of PL measurements

Density-functional theory for fluid-solid and solid-solid phase transitions.

Science.gov (United States)

Bharadwaj, Atul S; Singh, Yashwant

2017-03-01

We develop a theory to describe solid-solid phase transitions. The density functional formalism of classical statistical mechanics is used to find an exact expression for the difference in the grand thermodynamic potentials of the two coexisting phases. The expression involves both the symmetry conserving and the symmetry broken parts of the direct pair correlation function. The theory is used to calculate phase diagram of systems of soft spheres interacting via inverse power potentials u(r)=ε(σ/r)^{n}, where parameter n measures softness of the potential. We find that for 1/nfcc) structure while for 1/n≥0.154 the body-centred-cubic (bcc) structure is preferred. The bcc structure transforms into the fcc structure upon increasing the density. The calculated phase diagram is in good agreement with the one found from molecular simulations.

Source identification of underground fuel spills by solid-phase microextraction/high-resolution gas chromatography/genetic algorithms.

Science.gov (United States)

Lavine, B K; Ritter, J; Moores, A J; Wilson, M; Faruque, A; Mayfield, H T

2000-01-15

Solid-phase microextraction (SPME), capillary column gas chromatography, and pattern recognition methods were used to develop a potential method for typing jet fuels so a spill sample in the environment can be traced to its source. The test data consisted of gas chromatograms from 180 neat jet fuel samples representing common aviation turbine fuels found in the United States (JP-4, Jet-A, JP-7, JPTS, JP-5, JP-8). SPME sampling of the fuel's headspace afforded well-resolved reproducible profiles, which were standardized using special peak-matching software. The peak-matching procedure yielded 84 standardized retention time windows, though not all peaks were present in all gas chromatograms. A genetic algorithm (GA) was employed to identify features (in the standardized chromatograms of the neat jet fuels) suitable for pattern recognition analysis. The GA selected peaks, whose two largest principal components showed clustering of the chromatograms on the basis of fuel type. The principal component analysis routine in the fitness function of the GA acted as an information filter, significantly reducing the size of the search space, since it restricted the search to feature subsets whose variance is primarily about differences between the various fuel types in the training set. In addition, the GA focused on those classes and/or samples that were difficult to classify as it trained using a form of boosting. Samples that consistently classify correctly were not as heavily weighted as samples that were difficult to classify. Over time, the GA learned its optimal parameters in a manner similar to a perceptron. The pattern recognition GA integrated aspects of strong and weak learning to yield a "smart" one-pass procedure for feature selection.

Determination of chlorinated polycyclic aromatic hydrocarbons in water by solid-phase extraction coupled with gas chromatography and mass spectrometry.

Science.gov (United States)

Wang, Xianli; Kang, Haiyan; Wu, Junfeng

2016-05-01

Given the potential risks of chlorinated polycyclic aromatic hydrocarbons, the analysis of their presence in water is very urgent. We have developed a novel procedure for determining chlorinated polycyclic aromatic hydrocarbons in water based on solid-phase extraction coupled with gas chromatography and mass spectrometry. The extraction parameters of solid-phase extraction were optimized in detail. Under the optimal conditions, the proposed method showed wide linear ranges (1.0-1000 ng/L) with correlation coefficients ranging from 0.9952 to 0.9998. The limits of detection and the limits of quantification were in the range of 0.015-0.591 and 0.045-1.502 ng/L, respectively. Recoveries ranged from 82.5 to 102.6% with relative standard deviations below 9.2%. The obtained method was applied successfully to the determination of chlorinated polycyclic aromatic hydrocarbons in real water samples. Most of the chlorinated polycyclic aromatic hydrocarbons were detected and 1-monochloropyrene was predominant in the studied water samples. This is the first report of chlorinated polycyclic aromatic hydrocarbons in water samples in China. The toxic equivalency quotients of chlorinated polycyclic aromatic hydrocarbons in the studied tap water were 9.95 ng the toxic equivalency quotient m(-3) . 9,10-Dichloroanthracene and 1-monochloropyrene accounted for the majority of the total toxic equivalency quotients of chlorinated polycyclic aromatic hydrocarbons in tap water. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Liquid Solution Phase Epitaxial Growth of Al-doped f-SiC for LEDs

DEFF Research Database (Denmark)

Tang, Kai; Ma, Xiang; van der Eijk, Casper

light quality and longer lifespan, compared to the current yellow phosphor based white LEDs. Liquid phase epitaxy technology is able to yield a high crystalline quality in terms of structural perfection owing to the fact that it is a near equilibrium process. In addition, the technological equipment...... are presented and discussed. Since operational temperature of LPE growth is much lower than that currently used in physical vapour transport (PVT) process, it is expected to save the energy consumption for SiC crystal growth....

Molecular structure determination of cyclootane by ab initio and electron diffraction methods in the gas phase

OpenAIRE

De Almeida, Wagner B.

2000-01-01

The determination of the molecular structure of molecules is of fundamental importance in chemistry. X-rays and electron diffraction methods constitute in important tools for the elucidation of the molecular structure of systems in the solid state and gas phase, respectively. The use of quantum mechanical molecular orbital ab initio methods offer an alternative for conformational analysis studies. Comparison between theoretical results and those obtained experimentally in the gas phase can ma...

Determination of the nitrogen concentration in epitaxial layers of GaAs /SUB 1-x/ p /SUB x/ by the optical method

International Nuclear Information System (INIS)

Lupal, M.V.; Klot, B; Nikhter, K.; Pikhtin, A.N.; Trapp, M.

1986-01-01

This paper determines the dependence of the cross section for absorption in the A /SUB N/ line of a bound exciton on the nitrogen content in the solid solution GaAs /SUB 1-x/ P /SUB x/ by comparing the results of optical measurements with the data from secondary ionic mass spectrometry, and these results are used to study the effect of technological factors on the nitrogen concentration epitaxial layers obtained by the gas-transport method. Doping was carried out with nitrogen by injecting ammonia into the reactor zone; the partial pressure of the ammonia was varied from 1 to 25 kPa. Aside from nitrogen, the authors doped the layers with shallow donor Te. It is established that the solubility of nitrogen in the solid solution decreases as the arsenic content increases when the convenient optical method for determining the nitrogen concentration in epitaxial GaAs /SUB 1-x/ P /SUB x/ layers is used

Fixing arsenic contained in a gas phase using solid hematite

International Nuclear Information System (INIS)

Balladares, E.; Gonzalez, A.; Rarra, R.; Sanchez, M.

2004-01-01

Feasibility to obtain ferric arsenate starting from arsenic containing gas in contact with Fe 3 O 3 has been studied. Thermodynamic stability of the system Fe-As-O was analysed in order to verify conditions to form Fe x As y O z type compounds. Experiments were made using a hematite sample suspended in a thermogravimetric device. As 4 O 6 was generated starting from solid As 2 O 3 which was circulating through the iron oxide. Final samples were analysed chemically and by means of DRX, verifying the formation of FeAsO 4 , FeAsO 4 .2h 2 O and FeAsO 4 .(H 2 O) 2 in small quantities. Tests in porous bed and pellets were carried out, studying the effect of: porosity, temperature and oxygen potential. The largest conversion obtained was 10% at 800 degree centigrade, pO 2 =50% and porosity=0.883. (Author) 9 refs

Solid-solid phase change thermal storage application to space-suit battery pack

Science.gov (United States)

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.

The gas phase structure of α -pinene, a main biogenic volatile organic compound

Science.gov (United States)

Neeman, Elias M.; Avilés Moreno, Juan Ramón; Huet, Thérèse R.

2017-12-01

The gas phase structure of the bicyclic atmospheric aerosol precursor α-pinene was investigated employing a combination of quantum chemical calculation and Fourier transform microwave spectroscopy coupled to a supersonic jet expansion. The very weak rotational spectra of the parent species and all singly substituted 13C in natural abundance have been identified, from 2 to 20 GHz, and fitted to Watson's Hamiltonian model. The rotational constants were used together with geometrical parameters from density functional theory and ab initio calculations to determine the rs, r0, and rm(1 ) structures of the skeleton, without any structural assumption in the fit concerning the heavy atoms. The double C=C bond was found to belong to a quasiplanar skeleton structure containing 6 carbon atoms. Comparison with solid phase structure is reported. The significant differences of α-pinene in gas phase and other gas phase bicyclic monoterpene structures (β-pinene, nopinone, myrtenal, and bicyclo[3.1.1]heptane) are discussed.

Solid phase assays

International Nuclear Information System (INIS)

Reese, M.G.; Johnson, L.R.; Ransom, D.K.

1980-01-01

In a solid phase assay for quantitative determination of biological and other analytes, a sample such as serum is contacted with a receptor for the analyte being assayed, the receptor being supported on a solid support. No tracer for the analyte is added to the sample before contacting with the receptor; instead the tracer is contacted with the receptor after unbound analyte has been removed from the receptor. The assay can be otherwise performed in a conventional manner but can give greater sensitivity. (author)

Determination of Benzo(a)pyrene in Malaysian commercialized coffee powder using solid phase extraction and gas chromatography

International Nuclear Information System (INIS)

Noraini Kasim; Rozita Osman; Norashikin Saim; Licaberth Ismail

2012-01-01

Roasting is a critical process in coffee production as it enables the development of flavor and aroma. Benzo[a]pyrene (BaP) is a non desirable product of incomplete combustion at temperatures between 300 and 600 degree Celsius and may be produced during roasting step. In this study, selected samples of roasted coffee powder were analysed for BaP. Extraction of BaP was achieved using C 18 solid phase extraction (SPE) prior to analysis by gas chromatography. Calibration curve prepared with concentrations ranged between 3 - 50 ppm showed good linearity with r = 0.999. The limit of detection (LOD) was 0.25 ppm and the limit of quantification (LOQ) was 0.85 ppm. Recovery of BaP obtained from spiked sample (3 ppm) was 88.7 % with RSD (n=3) of 5.4 %. Benzo[a]pyrene was detected in all samples, at level ranging from 0.14 to 0.62 ppb. (author)

Determination of Lactones in Wines by Headspace Solid-Phase Microextraction and Gas Chromatography Coupled with Mass Spectrometry

Directory of Open Access Journals (Sweden)

S. J. Pérez-Olivero

2014-01-01

Full Text Available Application of headspace solid-phase microextraction (HS-SPME coupled with high-resolution gas chromatographic (HRGC analysis was studied for determining lactones in wines. Six different SPME fibers were tested, and the influence of different factors such as temperature and time of desorption, ionic strength, time of extraction, content of sugar, ethanol, tannins and anthocyanins, and pH and influence of SO2 were studied. The proposed HS-SPME-GC method is an appropriate technique for the quantitative analysis of γ-butyrolactone, γ-hexalactone, trans-whiskey lactone, γ-octalactone, cis-whiskey lactone, γ-nonalactone, γ-decalactone, δ-decalactone, and γ-undecalactone in wines. Method reproducibility and repeatability ranged between 0.6 and 5.2% for all compounds. Detection limit for γ-butyrolactone was 0.17 mg/L and a few μg/L for the rest of the compounds. The optimized method has been applied to several wine samples.

Microextração por fase sólida SPME, Solid Phase Micro-Extration

Directory of Open Access Journals (Sweden)

Antonio Luiz Pires Valente

2000-08-01

Full Text Available Fundamental aspects of Solid Phase Micro-Extraction (SPME are discussed in the present paper. The application of SPME as a microtechnique of sample preparation for gas chromatographic analysis is considered and related to existing theoretical models. Both research prototypes and commercial SPME devices are considered.

Thin film structures and phase stability

International Nuclear Information System (INIS)

Clemens, B.M.; Johnson, W.L.

1990-01-01

This was a two day symposium, with invited and contributed papers as well as an evening poster session. The first day concentrated on solid state reactions with invited talks by Lindsay Greer from the University of Cambridge, King Tu from IBM Yorktown Heights, and Carl Thompson from MIT. Professor Greer observed that the diffusion of Zr is 10 6 times slower than that of Ni in amorphous NiZr, confirming that Ni is the mobile species in solid state amorphization. King Tu explained the formation of metastable phases in this film diffusion couples by the concept of maximum rate of free energy change. Carl Thompson discussed the formation of amorphous phases in metal silicon systems, and discussed a two stage nucleation and growth process. The contributed papers also generated discussion on topics such as phase segregation, amorphous silicide formation, room temperature oxidation of silicon, and nucleation during ion beam irradiation. There was a lively poster session on Monday evening with papers on a wide variety of topics covering the general area of thin film science. The second day had sessions Epitaxy and Multilayer Structure I and II, with the morning focussing on epitaxial and heteroepitaxial growth of thin films. Robin Farrow of IBM Almaden led off with an invited talk where he reported on some remarkable success he and his co-workers have had in growing single crystal epitaxial thin films and superlattices of silver, iron, cobalt and platinum on GaAs. This was followed by several talks on epitaxial growth and characterization. The afternoon focused on interfaces and structure of multilayered materials. A session on possible stress origins of the supermodulus effect was highlighted by lively interaction from the audience. Most of the papers presented at the symposium are presented in this book

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

Science.gov (United States)

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.

Evaluation of solid-phase microextraction conditions for the determination of polycyclic aromatic hydrocarbons in aquatic species using gas chromatography

Energy Technology Data Exchange (ETDEWEB)

Aguinaga, N.; Campillo, N.; Vinas, P.; Hernandez-Cordoba, M. [University of Murcia, Department of Analytical Chemistry, Faculty of Chemistry, Murcia (Spain)

2008-06-15

This paper describes a headspace solid-phase microextraction (HS-SPME) procedure coupled to gas chromatography with mass spectrometric detection (GC-MS) for the determination of eight PAHs in aquatic species. The influence of various parameters on the PAH extraction efficiency was carefully examined. At 75 C and for an extraction time of 60 min, a polydimethylsiloxane-divinylbenzene (PDMS/DVB) fiber coating was found to be most suitable. Under the optimized conditions, detection limits ranged from 8 to 450 pg g{sup -1}, depending on the compound and the sample matrix. The repeatability varied between 7 and 15% (RSD). Accuracy was tested using the NIST SRM 1974b reference material. The method was successfully applied to different samples, and the studied PAHs were detected in several of the samples. (orig.)

Solid phase epitaxy on N-type polysilicon films formed by aluminium induced crystallization of amorphous silicon

Energy Technology Data Exchange (ETDEWEB)

Tuezuen, O., E-mail: Ozge.Tuzun@iness.c-strasbourg.f [InESS, UMR 7163 CNRS-UdS, 23 rue du Loess, F-67037 Strasbourg Cedex 2 (France); Slaoui, A.; Roques, S.; Focsa, A. [InESS, UMR 7163 CNRS-UdS, 23 rue du Loess, F-67037 Strasbourg Cedex 2 (France); Jomard, F.; Ballutaud, D. [GEMaC-UMR 8635 CNRS, 1 place Aristide Briand, F-92195 Meudon (France)

2009-10-01

In this work, undoped amorphous silicon layers were deposited on n-type AIC seed films and then annealed at different temperatures for epitaxial growth. The epitaxy was carried out using halogen lamps (rapid thermal process or RTP) or a tube conventional furnace (CTP). We investigated the morphology of the resulting 2 {mu}m thick epi-layers by means of optical microscopy. An average grain size of about 40 {mu}m is formed after 90 s annealing at 1000 {sup o}C in RTP. The stress and degree of crystallinity of the epi-layers were studied by micro-Raman Spectroscopy and UV-visible spectrometer as a function of annealing time. The presence of compressive stress is observed from the peak position which shifts from 520.0 cm{sup -1} to 521.0 cm{sup -1} and 522.3 cm{sup -1} after CTP annealing for 10 min and 90 min, respectively. It is shown that the full width at half maximum (FWHM) varies from 9.8 cm{sup -1} to 15.6 cm{sup -1}, and the magnitude of stress is changing from 325 MPa to 650 MPa. Finally, the highest crystallinity is achieved after annealing at 1000 {sup o}C for 90 min in a tube furnace exhibiting a crystalline fraction of 81.5%. X-ray diffraction technique was used to determine the preferential orientation of the poly-Si thin films formed by SPE technique on n{sup +} type AIC layer. The preferential orientation is <100> for all annealing times at 1000 {sup o}C.

Effects of anharmonic strain on the phase stability of epitaxial films and superlattices: Applications to noble metals

International Nuclear Information System (INIS)

Ozolins, V.; Wolverton, C.; Zunger, A.

1998-01-01

Epitaxial strain energies of epitaxial films and bulk superlattices are studied via first-principles total-energy calculations using the local-density approximation. Anharmonic effects due to large lattice mismatch, beyond the reach of the harmonic elasticity theory, are found to be very important in Cu/Au (lattice mismatch 12%), Cu/Ag (12%), and Ni/Au (15%). We find that left-angle 001 right-angle is the elastically soft direction for biaxial expansion of Cu and Ni, but it is left-angle 201 right-angle for large biaxial compression of Cu, Ag, and Au. The stability of superlattices is discussed in terms of the coherency strain and interfacial energies. We find that in phase separating systems such as Cu-Ag the superlattice formation energies decrease with superlattice period, and the interfacial energy is positive. Superlattices are formed easiest on (001) and hardest on (111) substrates. For ordering systems, such as Cu-Au and Ag-Au, the formation energy of superlattices increases with period, and interfacial energies are negative. These superlattices are formed easiest on (001) or (110) and hardest on (111) substrates. For Ni-Au we find a hybrid behavior: superlattices along left-angle 111 right-angle and left-angle 001 right-angle behave like phase separating systems, while for left-angle 110 right-angle they behave like ordering systems. Finally, recent experimental results on epitaxial stabilization of disordered Ni-Au and Cu-Ag alloys, immiscible in the bulk form, are explained in terms of destabilization of the phase separated state due to lattice mismatch between the substrate and constituents. copyright 1998 The American Physical Society

Development of Key Technologies for White Lighting Based on Light-Emitting Diodes (LEDs)

Energy Technology Data Exchange (ETDEWEB)

Werner Goetz; Bill Imler; James Kim; Junko Kobayashi; Andrew Kim; Mike Krames; Rick Mann; Gerd Mueller-Mach; Anneli Munkholm; Jonathan Wierer

2004-03-31

This program was organized to focus on materials development issues critical to the acceleration of solid-state lighting, and was split into three major thrust areas: (1) study of dislocation density reduction for GaN grown on sapphire using 'cantilever epitaxy', and the impact of dislocation density on the performance of state-of-the-art high-power LEDs; (2) the evaluation of in situ techniques for monitoring gas phase chemistry and the properties of GaN-based layers during metal-organic vapor phase epitaxy (MOCVD), and (3) feasibility for using semiconductor nanoparticles ('quantum dots') for the down-conversion of blue or ultraviolet light to generate white light. The program included a partnership between Lumileds Lighting (epitaxy and device fabrication for high power LEDs) and Sandia National Laboratories (cantilever epitaxy, gas phase chemistry, and quantum dot synthesis). Key findings included: (1) cantilever epitaxy can provide dislocation density reduction comparable to that of more complicated approaches, but all in one epitaxial growth step; however, further improvements are required to realize significant gains in LED performance at high drive currents, (2) in situ tools can provide detailed knowledge about gas phase chemistry, and can be used to monitor and control epitaxial layer composition and temperature to provide improved yields (e.g., a fivefold increase in color targeting is demonstrated for 540nm LEDs), and (3) quantum efficiency for quantum dots is improved and maintained up to 70% in epoxy thin films, but further work is necessary to increase densification (absorption) and robustness before practical application to LEDs.

Effect of crystal orientation on the phase diagrams, dielectric and piezoelectric properties of epitaxial BaTiO{sub 3} thin films

Energy Technology Data Exchange (ETDEWEB)

Wu, Huaping, E-mail: wuhuaping@gmail.com, E-mail: hpwu@zjut.edu.cn [Key Laboratory of E& M (Zhejiang University of Technology), Ministry of Education & Zhejiang Province, Hangzhou 310014 (China); State Key Laboratory of Structural Analysis for Industrial Equipment, Dalian University of Technology, Dalian 116024 (China); Ma, Xuefu; Zhang, Zheng; Zeng, Jun; Chai, Guozhong [Key Laboratory of E& M (Zhejiang University of Technology), Ministry of Education & Zhejiang Province, Hangzhou 310014 (China); Wang, Jie [Department of Engineering Mechanics, School of Aeronautics and Astronautics, Zhejiang University, Hangzhou 310027 (China)

2016-01-15

The influence of crystal orientations on the phase diagrams, dielectric and piezoelectric properties of epitaxial BaTiO{sub 3} thin films has been investigated using an expanded nonlinear thermodynamic theory. The calculations reveal that crystal orientation has significant influence on the phase stability and phase transitions in the misfit strain-temperature phase diagrams. In particular, the (110) orientation leads to a lower symmetry and more complicated phase transition than the (111) orientation in BaTiO{sub 3} films. The increase of compressive strain will dramatically enhance the Curie temperature T{sub C} of (110)-oriented BaTiO{sub 3} films, which matches well with previous experimental data. The polarization components experience a great change across the boundaries of different phases at room temperature in both (110)- and (111)-oriented films, which leads to the huge dielectric and piezoelectric responses. A good agreement is found between the present thermodynamics calculation and previous first-principles calculations. Our work provides an insight into how to use crystal orientation, epitaxial strain and temperature to tune the structure and properties of ferroelectrics.

Influence of fluid-mechanical characteristics of the system on the volumetric mass transfer coefficient and gas dispersion in three-phase system

Directory of Open Access Journals (Sweden)

Knežević Milena M.

2014-01-01

Full Text Available Distribution of gas bubbles and volumetric mass transfer coefficient, Kla, in a three phase system, with different types of solid particles at different operation conditions were studied in this paper. The ranges of superficial gas and liquid velocities used in this study were 0,03-0,09 m/s and 0-0,1 m/s, respectively. The three different types of solid particles were used as a bed in the column (glass dp=3 mm, dp=6 mm; ceramic dp=6 mm. The experiments were carried out in a 2D plexiglas column, 278 x 20,4 x 500 mm and in a cylindrical plexiglas column, with a diameter of 64 mm and a hight of 2000 mm. The Kla coefficient increased with gas and liquid velocities. Results showed that the volumetric mass transfer coefficient has a higher values in three phase system, with solid particles, compared with two phase system. The particles properties (diameter and density have a major impact on oxygen mass transfer in three phase systems.

FLUIDDYNAMIC ASPECTS OF GAS-PHASE ETHYLENE POLYMERIZATION REACTOR DESIGN

Directory of Open Access Journals (Sweden)

Guardani R.

1998-01-01

Full Text Available The relative importance of design variables affecting the fluiddynamic behavior of a fluidized bed reactor for the gas-phase ethylene polymerization is discussed, based on mathematical modeling. The three-phase bubbling fluidized bed model is based on axially distributed properties for the bubble, cloud and emulsion phases, combined with correlations for population balance and entrainment. Under the operating conditions adopted in most industrial processes, the reactor performance is affected mainly by the reaction rate and solids entrainment. Simulation results indicate that an adequate design of the freeboard and particle collecting equipment is of primary importance in order to produce polymeric particles with the desired size distribution, as well as to keep entrainment and catalyst feed rates at adequate levels.

Comparison of electrical and optical characteristics in gas-phase and gas-liquid phase discharges

Energy Technology Data Exchange (ETDEWEB)

Qazi, H. I. A.; Li, He-Ping, E-mail: liheping@tsinghua.edu.cn; Zhang, Xiao-Fei; Bao, Cheng-Yu [Department of Engineering Physics, Tsinghua University, Beijing 100084 (China); Nie, Qiu-Yue [School of Electrical Engineering and Automation, Harbin Institute of Technology, Harbin, Heilongjiang Province 150001 (China)

2015-12-15

This paper presents an AC-excited argon discharge generated using a gas-liquid (two-phase) hybrid plasma reactor, which mainly consists of a powered needle electrode enclosed in a conical quartz tube and grounded deionized water electrode. The discharges in the gas-phase, as well as in the two-phase, exhibit two discharge modes, i.e., the low current glow-like diffuse mode and the high current streamer-like constrict mode, with a mode transition, which exhibits a negative resistance of the discharges. The optical emission spectral analysis shows that the stronger diffusion of the water vapor into the discharge region in the two-phase discharges boosts up the generation of OH (A–X) radicals, and consequently, leads to a higher rotational temperature in the water-phase plasma plume than that of the gas-phase discharges. Both the increase of the power input and the decrease of the argon flow rate result in the increase of the rotational temperature in the plasma plume of the water-phase discharge. The stable two-phase discharges with a long plasma plume in the water-phase under a low power input and gas flow rate may show a promising prospect for the degradation of organic pollutants, e.g., printing and dyeing wastewater, in the field of environmental protection.

Headspace solid-phase microextraction coupled to gas chromatography for the analysis of aldehydes in edible oils.

Science.gov (United States)

Ma, Chunhua; Ji, Jiaojiao; Tan, Connieal; Chen, Dongmei; Luo, Feng; Wang, Yiru; Chen, Xi

2014-03-01

Oxidation has important effects on the quality of edible oils. In particular, the generation of aldehydes produced by the oxidation of oils is one of the deteriorative factors to their quality. The aim of this study was to develop a method to determine the aldehydes as lipid oxidation markers in edible oils. Seven aldehydes generated from lipid oxidation were studied using headspace solid-phase microextraction coupled to gas chromatography with a flame ionization detector. The extraction efficiency of five commercial fibers was investigated and the influence of extraction temperature, extraction time, desorption temperature, and desorption time were optimized. The best result was obtained with 85 μm carboxen/polydimethylsiloxane, extraction at 50 °C for 15 min and desorption in the gas chromatography injector at 250 °C for 2 min. Under the optimized conditions, the content of hexanal was the highest of the seven aldehydes in all edible oils. The limits of detection for hexanal in the three oils were found to range from 4.6 to 10.2 ng L(-1). The reproducibility of the method was evaluated and the relative standard deviations were less than 8.9%. This developed approach was successfully applied to analyze hexanal in peanut oil, soy oil, and olive oil samples, and these results were compared with those obtained using the thiobarbituric acid-reactive substances (TBARs) method. © 2013 The Authors. Published by Elsevier B.V. All rights reserved.

Characterisation of volatile profiles in 50 native Peruvian chili pepper using solid phase microextraction-gas chromatography mass spectrometry (SPME-GCMS).

Science.gov (United States)

Patel, Kirti; Ruiz, Candy; Calderon, Rosa; Marcelo, Mavel; Rojas, Rosario

2016-11-01

The volatiles were characterised by headspace solid phase micro extraction (HS-SPME), gas chromatography mass spectrometry (GC-FID/MS). A total of 127 compounds were identified with terpenes (including mono terpenes and sesquiterpenes - a total of 45 compounds), esters (31 compounds) and hydrocarbons (20 compounds) were the predominant volatile compounds. Principal component analysis (PCA) of the volatile compounds yielded 2 significant PC's, which together accounted for 90.3% of the total variance in the data set and the scatter plot generated between PC1 and PC2 successfully segregated the 50 chili pepper samples into 7 groups. Clusters of hydrocarbons, esters, terpenes, aldehyde and ketones formed the major determinants of the difference. Copyright © 2016 Elsevier Ltd. All rights reserved.

Experimental-statistical model of liquid-phase epitaxy for InP/InGaAsP/InP heterostructures

International Nuclear Information System (INIS)

Vasil'ev, M.G.; Selin, A.A.; Shelyakin, A.A.

1985-01-01

A mathematic model of the process of liquid-phase epitaxy for double InP/InGaAsP/InP heterostructures is constructed using statistical methods of experiment planning. The analysis of the model shows that the degree of In-P system melt supercooling affects considerably the characteristics of double heterostructures

A parallel solution-adaptive scheme for predicting multi-phase core flows in solid propellant rocket motors

International Nuclear Information System (INIS)

Sachdev, J.S.; Groth, C.P.T.; Gottlieb, J.J.

2003-01-01

The development of a parallel adaptive mesh refinement (AMR) scheme is described for solving the governing equations for multi-phase (gas-particle) core flows in solid propellant rocket motors (SRM). An Eulerian formulation is used to described the coupled motion between the gas and particle phases. A cell-centred upwind finite-volume discretization and the use of limited solution reconstruction, Riemann solver based flux functions for the gas and particle phases, and explicit multi-stage time-stepping allows for high solution accuracy and computational robustness. A Riemann problem is formulated for prescribing boundary data at the burning surface. Efficient and scalable parallel implementations are achieved with domain decomposition on distributed memory multiprocessor architectures. Numerical results are described to demonstrate the capabilities of the approach for predicting SRM core flows. (author)

Nitrogen doping efficiency during vapor phase epitaxy of 4H-SiC

Energy Technology Data Exchange (ETDEWEB)

Rowland, L.B.; Brandt, C.D. [Northrop Grumman Science and Technology Center, Pittsburgh, PA (United States); Burk, A.A. Jr. [Northrop Grumman Advanced Technology Lab., Baltimore, MD (United States)

1998-06-01

This work examines the interrelationships among doping efficiency, mole fraction, and Si/C ratio for intentional doping of 4H-SiC during vapor phase epitaxy using N{sub 2}. For four Si/C ratios, the doping concentration increased linearly as a function of increasing N{sub 2} partial pressure with a slope of 1.0 {+-} 0.03. Variation of propane mole fraction while the SiH{sub 4} and N{sub 2} mole fractions were kept constant revealed two different modes of nitrogen incorporation, corresponding to carbon-rich and silicon-rich conditions. (orig.) 14 refs.

Gas-Solid Reaction Properties of Fluorine Compounds and Solid Adsorbents for Off-Gas Treatment from Semiconductor Facility

Directory of Open Access Journals (Sweden)

Shinji Yasui

2012-01-01

Full Text Available We have been developing a new dry-type off-gas treatment system for recycling fluorine from perfluoro compounds present in off-gases from the semiconductor industry. The feature of this system is to adsorb the fluorine compounds in the exhaust gases from the decomposition furnace by using two types of solid adsorbents: the calcium carbonate in the upper layer adsorbs HF and converts it to CaF2, and the sodium bicarbonate in the lower layer adsorbs HF and SiF4 and converts them to Na2SiF6. This paper describes the fluorine compound adsorption properties of both the solid adsorbents—calcium carbonate and the sodium compound—for the optimal design of the fixation furnace. An analysis of the gas-solid reaction rate was performed from the experimental results of the breakthrough curve by using a fixed-bed reaction model, and the reaction rate constants and adsorption capacity were obtained for achieving an optimal process design.

Characterization of three agave species by gas chromatography and solid-phase microextraction-gas chromatography-mass spectrometry.

Science.gov (United States)

Peña-Alvarez, Araceli; Díaz, Laura; Medina, Alejandra; Labastida, Carmen; Capella, Santiago; Vera, Luz Elena

2004-02-20

Steam distillation (SD) extraction-solid-phase microextraction coupled to GC-MS was developed for the determination of terpenes and Bligh-Dyer extraction-derivatization coupled with GC for the determination of fatty acids such as ethyl esters were used. It was found that the three different Agave species have the same profile of fatty acids; the quantity of these compounds is different in each Agave variety. On the other hand, different terpenes were identified in the three Agave plants studied: nine in A. salmiana, eight in A. angustifolia and 32 in A. tequilana Weber var. azul.

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

Science.gov (United States)

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 (%) 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).

In silico carbon molecular beam epitaxial growth of graphene on the h-BN substrate: carbon source effect on van der Waals epitaxy

Science.gov (United States)

Lee, Jonghoon; Varshney, Vikas; Park, Jeongho; Farmer, Barry L.; Roy, Ajit K.

2016-05-01

Against the presumption that hexagonal boron-nitride (h-BN) should provide an ideal substrate for van der Waals (vdW) epitaxy to grow high quality graphene films, carbon molecular beam epitaxy (CMBE) techniques using solid carbon sublimation have reported relatively poor quality of the graphene. In this article, the CMBE growth of graphene on the h-BN substrate is numerically studied in order to identify the effect of the carbon source on the quality of the graphene film. The carbon molecular beam generated by the sublimation of solid carbon source materials such as graphite and glassy carbon is mostly composed of atomic carbon, carbon dimers and carbon trimers. Therefore, the graphene film growth becomes a complex process involving various deposition characteristics of a multitude of carbon entities. Based on the study of surface adsorption and film growth characteristics of these three major carbon entities comprising graphite vapour, we report that carbon trimers convey strong traits of vdW epitaxy prone to high quality graphene growth, while atomic carbon deposition is a surface-reaction limited process accompanied by strong chemisorption. The vdW epitaxial behaviour of carbon trimers is found to be substantial enough to nucleate and develop into graphene like planar films within a nanosecond of high flux growth simulation, while reactive atomic carbons tend to impair the structural integrity of the crystalline h-BN substrate upon deposition to form an amorphous interface between the substrate and the growing carbon film. The content of reactive atomic carbons in the molecular beam is suspected to be the primary cause of low quality graphene reported in the literature. A possible optimization of the molecular beam composition towards the synthesis of better quality graphene films is suggested.Against the presumption that hexagonal boron-nitride (h-BN) should provide an ideal substrate for van der Waals (vdW) epitaxy to grow high quality graphene films, carbon

Combinatorial Solid-Phase Synthesis of Balanol Analogues

DEFF Research Database (Denmark)

Nielsen, John; Lyngsø, Lars Ole

1996-01-01

The natural product balanol has served as a template for the design and synthesis of a combinatorial library using solid-phase chemistry. Using a retrosynthetic analysis, the structural analogues have been assembled from three relatively accessible building blocks. The solid-phase chemistry inclu...

Application of solid-phase microextraction with gas chromatography and mass spectrometry for the early detection of active moulds on historical woollen objects.

Science.gov (United States)

Sawoszczuk, Tomasz; Syguła-Cholewińska, Justyna; Del Hoyo-Meléndez, Julio M

2017-02-01

The goal of this work was to determine the microbial volatile organic compounds emitted by moulds growing on wool in search of particular volatiles mentioned in the literature as indicators of active mould growth. The keratinolytically active fungi were inoculated on two types of media: (1) samples of wool placed on broths, and (2) on broths containing amino acids that are elements of the structure of keratin. All samples were prepared inside 20 mL vials (closed system). In the first case (1) the broths did not contain any sources of organic carbon, nitrogen, or sulfur, i.e. wool was the only nutrient for the moulds. A third type of sample was historical wool prepared in a Petri dish without a broth and inoculated with a keratinolytically active mould (open system). The microbial volatiles emitted by moulds were sampled with the headspace solid-phase microextraction method. Volatiles extracted on solid-phase microextraction fibers were analyzed in a gas chromatography with mass spectrometry system. Qualitative and quantitative analyses of chromatograms were carried out in search of indicators of metabolic activity. The results showed that there are three groups of volatiles that can be used for the detection of active forms of moulds on woollen objects. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Non-targeted volatile profiles for the classification of the botanical origin of Chinese honey by solid-phase microextraction and gas chromatography-mass spectrometry combined with chemometrics.

Science.gov (United States)

Chen, Hui; Jin, Linghe; Fan, Chunlin; Wang, Wenwen

2017-11-01

A potential method for the discrimination and prediction of honey samples of various botanical origins was developed based on the non-targeted volatile profiles obtained by solid-phase microextraction with gas chromatography and mass spectrometry combined with chemometrics. The blind analysis of non-targeted volatile profiles was carried out using solid-phase microextraction with gas chromatography and mass spectrometry for 87 authentic honey samples from four botanical origins (acacia, linden, vitex, and rape). The number of variables was reduced from 2734 to 70 by using a series of filters. Based on the optimized 70 variables, 79.12% of the variance was explained by the first four principal components. Partial least squares discriminant analysis, naïve Bayes analysis, and back-propagation artificial neural network were used to develop the classification and prediction models. The 100% accuracy revealed a perfect classification of the botanical origins. In addition, the reliability and practicability of the models were validated by an independent set of additional 20 authentic honey samples. All 20 samples were accurately classified. The confidence measures indicated that the performance of the naïve Bayes model was better than the other two models. Finally, the characteristic volatile compounds of linden honey were tentatively identified. The proposed method is reliable and accurate for the classification of honey of various botanical origins. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Epitaxial Oxide Thin Films Grown by Solid Source Metal-Organic Chemical Vapor Deposition.

Science.gov (United States)

Lu, Zihong

1995-01-01

The conventional liquid source metal-organic chemical vapor deposition (MOCVD) technique is capable of producing large area, high quality, single crystal semiconductor films. However, the growth of complex oxide films by this method has been hampered by a lack of suitable source materials. While chemists have been actively searching for new source materials, the research work reported here has demonstrated the successful application of solid metal-organic sources (based on tetramethylheptanedionate) to the growth of high quality thin films of binary compound cerium dioxide (CeO_2), and two more complex materials, the ternary compound lithium niobate (LiNbO_3), with two cations, and the quaternary compound strontium barium niobate (SBN), with three cations. The growth of CeO_2 thin films on (1012)Al_2O_3 substrates has been used as a model to study the general growth behavior of oxides. Factors affecting deposition rate, surface morphology, out-of-plane mosaic structure, and film orientation have been carefully investigated. A kinetic model based on gas phase prereaction is proposed to account for the substrate temperature dependence of film orientation found in this system. Atomically smooth, single crystal quality cerium dioxide thin films have been obtained. Superconducting YBCO films sputtered on top of solid source MOCVD grown thin cerium dioxide buffer layers on sapphire have been shown to have physical properties as good as those of YBCO films grown on single crystal MgO substrates. The thin film growth of LiNbO_3 and Sr_{1-x}Ba _{x}Nb_2 O_6 (SBN) was more complex and challenging. Phase purity, transparency, in-plane orientation, and the ferroelectric polarity of LiNbO _3 films grown on sapphire substrates was investigated. The first optical quality, MOCVD grown LiNbO _3 films, having waveguiding losses of less than 2 dB/cm, were prepared. An important aspect of the SBN film growth studies involved finding a suitable single crystal substrate material. Mg

Position-controlled epitaxial III-V nanowires on silicon

Energy Technology Data Exchange (ETDEWEB)

Roest, Aarnoud L; Verheijen, Marcel A; Wunnicke, Olaf; Serafin, Stacey; Wondergem, Harry; Bakkers, Erik P A M [Philips Research Laboratories, Professor Holstlaan 4, 5656 AA Eindhoven (Netherlands); Kavli Institute of NanoScience, Delft University of Technology, PO Box 5046, 2600 GA Delft (Netherlands)

2006-06-14

We show the epitaxial integration of III-V semiconductor nanowires with silicon technology. The wires are grown by the VLS mechanism with laser ablation as well as metal-organic vapour phase epitaxy. The hetero-epitaxial growth of the III-V nanowires on silicon was confirmed with x-ray diffraction pole figures and cross-sectional transmission electron microscopy. We show preliminary results of two-terminal electrical measurements of III-V nanowires grown on silicon. E-beam lithography was used to predefine the position of the nanowires.

Position-controlled epitaxial III-V nanowires on silicon

International Nuclear Information System (INIS)

Roest, Aarnoud L; Verheijen, Marcel A; Wunnicke, Olaf; Serafin, Stacey; Wondergem, Harry; Bakkers, Erik P A M

2006-01-01

We show the epitaxial integration of III-V semiconductor nanowires with silicon technology. The wires are grown by the VLS mechanism with laser ablation as well as metal-organic vapour phase epitaxy. The hetero-epitaxial growth of the III-V nanowires on silicon was confirmed with x-ray diffraction pole figures and cross-sectional transmission electron microscopy. We show preliminary results of two-terminal electrical measurements of III-V nanowires grown on silicon. E-beam lithography was used to predefine the position of the nanowires

Hydrodynamic boundary conditions for one-component liquid-gas flows on non-isothermal solid substrates

KAUST Repository

Xu, Xinpeng

2012-01-01

Recently, liquid-gas flows related to droplets, bubbles, and thin films on solid surfaces with thermal and wettability gradients have attracted widespread attention because of the many physical processes involved and their promising potential applications in biology, chemistry, and industry. Various new physical effects have been discovered at fluid-solid interfaces by experiments and molecular dynamics simulations, e.g., fluid velocity slip, temperature slip (Kapitza resistance), mechanical-thermal cross coupling, etc. There have been various models and theories proposed to explain these experimental and numerical observations. However, to the best of our knowledge,a continuum hydrodynamic model capable of predicting the temperature and velocity profiles of liquid-gas flows on non-isothermal, heterogeneous solid substrates is still absent. The purpose of this work is to construct a continuum model for simulating the liquid-gas flows on solid surfaces that are flat and rigid, and may involve wettability gradients and thermal gradients. This model is able to describe fluid velocity slip, temperature slip, and mechanical-thermal coupling that may occur at fluid-solid interfaces. For this purpose, we first employ the diffuse interface modeling to formulate the hydrodynamic equations for one-component liquid-gas flows in the bulk region. This reproduces the dynamic van der Waals theory of Onuki [Phys. Rev. Lett., 94: 054501, 2005]. We then extendWaldmann\\'s method [Z. Naturforsch. A, 22: 1269-1280, 1967] to formulate the boundary conditions at the fluid-solid interface that match the hydrodynamic equations in the bulk. The effects of the solid surface curvature are also briefly discussed in the appendix. The guiding principles of our model derivation are the conservation laws and the positive definiteness of entropy production together with the Onsager reciprocal relation. The derived model is self-consistent in the sense that the boundary conditions are

Creating Ruddlesden-Popper phases by hybrid molecular beam epitaxy

International Nuclear Information System (INIS)

Haislmaier, Ryan C.; Stone, Greg; Alem, Nasim; Engel-Herbert, Roman

2016-01-01

The synthesis of a 50 unit cell thick n = 4 Sr_n_+_1Ti_nO_3_n_+_1 (Sr_5Ti_4O_1_3) Ruddlesden-Popper (RP) phase film is demonstrated by sequentially depositing SrO and TiO_2 layers in an alternating fashion using hybrid molecular beam epitaxy (MBE), where Ti was supplied using titanium tetraisopropoxide (TTIP). A detailed calibration procedure is outlined for determining the shuttering times to deposit SrO and TiO_2 layers with precise monolayer doses using in-situ reflection high energy electron diffraction (RHEED) as feedback. Using optimized Sr and TTIP shuttering times, a fully automated growth of the n = 4 RP phase was carried out over a period of >4.5 h. Very stable RHEED intensity oscillations were observed over the entire growth period. The structural characterization by X-ray diffraction and high resolution transmission electron microscopy revealed that a constant periodicity of four SrTiO_3 perovskite unit cell blocks separating the double SrO rocksalt layer was maintained throughout the entire film thickness with a very little amount of planar faults oriented perpendicular to the growth front direction. These results illustrate that hybrid MBE is capable of layer-by-layer growth with atomic level precision and excellent flux stability.

An Introduction to the Gas Phase

Science.gov (United States)

Vallance, Claire

2017-11-01

'An Introduction to the Gas Phase' is adapted from a set of lecture notes for a core first year lecture course in physical chemistry taught at the University of Oxford. The book is intended to give a relatively concise introduction to the gas phase at a level suitable for any undergraduate scientist. After defining the gas phase, properties of gases such as temperature, pressure, and volume are discussed. The relationships between these properties are explained at a molecular level, and simple models are introduced that allow the various gas laws to be derived from first principles. Finally, the collisional behaviour of gases is used to explain a number of gas-phase phenomena, such as effusion, diffusion, and thermal conductivity.

Structure dynamics. Determination of the coupled relationships in solid-fluid-gas dynamics

International Nuclear Information System (INIS)

Hofmann, H.; Huber, A.; Naehring, T.; Bonakdarzadeh, S.; Faass, E.; Gaschen, J.P.; Kniffka, K.; Pilz, H.

1980-06-01

In the present paper the code concept SAN (Structure ANalysis) is presented. SAN is designed according to the modular principle using describing and coordinating modules. SAN is based on the discreetizing method. It uses compatible forms of description. The method of finite elements is applied. Solid-fluid-gas structures may be described as well as their interrelations in the linear and nonlinear region, including phase transitions with the associated descriptions of material and state. (orig./RW) [de

Growth of CoSi2 on Si(001) by reactive deposition epitaxy

International Nuclear Information System (INIS)

Lim, C.W.; Shin, C.-S.; Gall, D.; Zuo, J.M.; Petrov, I.; Greene, J.E.

2005-01-01

CaF 2 -structure CoSi 2 layers were formed on Si(001) by reactive deposition epitaxy (RDE) and compared with CoSi 2 layers obtained by conventional solid phase growth (SPG). In both sets of experiments, Co was deposited by ultrahigh-vacuum magnetron sputtering and CoSi 2 formed at 600 deg. C. However, in the case of RDE, CoSi 2 formation occurred during Co deposition while for SPG, Co was deposited at 25 deg. C and silicidation took place during subsequent annealing. X-ray diffraction pole figures and transmission electron microscopy results demonstrate that RDE CoSi 2 layers are epitaxial with a cube-on-cube relationship (001) CoSi 2 parallel (001) Si and [100] CoSi 2 parallel[100] Si . In contrast, SPG films are polycrystalline with an average grain size of ≅1000 A and a mixed 111/002/022/112 orientation. We attribute the striking difference to rapid Co diffusion into the Si(001) substrate during RDE for which the high Co/Si reactivity gives rise to a flux-limited reaction resulting in the direct formation of the disilicide phase. In contrast, sequential nucleation and transformation among increasingly Si-rich phases--from orthorhombic Co 2 Si to cubic CoSi to CoSi 2 --during SPG results in polycrystalline layers with a complex texture

Determination of 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in soy sauce by headspace derivatization solid-phase microextraction combined with gas chromatography-mass spectrometry.

Science.gov (United States)

Lee, Maw-Rong; Chiu, Tzu-Chun; Dou, Jianpeng

2007-05-22

This study proposes a method for identifying 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in aqueous matrices by using headspace on-fiber derivatization following solid-phase microextraction combined with gas chromatography-mass spectrometry. The optimized SPME experimental procedures for extracting 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in aqueous solutions involved a 85 microm polyacrylate-coated fiber at pH 6, a sodium chloride concentration of 0.36 g mL(-1), extraction at 50 degrees C for 15 min and desorption of analytes at 260 degrees C for 3 min. Headspace derivatization was conducted in a laboratory-made design with N-methyl-N-(trimethylsilyl)-trifluoroacetamide vapor following solid-phase microextraction by using 3 microL N-methyl-N-(trimethylsilyl)-trifluoroacetamide at an oil bath temperature of 230 degrees C for 40 s. This method had good repeatability (R.S.D.s or = 0.9972) for ultrapure water and soy sauce samples that were spiked with two analytes. Detection limits were obtained at the ng mL(-1). The result demonstrated that headspace on-fiber derivatization following solid-phase microextraction was a simple, fast and accurate technique for identifying trace 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in soy sauce.

Determination of roasted pistachio (Pistacia vera L.) key odorants by headspace solid-phase microextraction and gas chromatography-olfactometry.

Science.gov (United States)

Aceña, Laura; Vera, Luciano; Guasch, Josep; Busto, Olga; Mestres, Montserrat

2011-03-23

Key odorants in roasted pistachio nuts have been determined for the first time. Two different pistachio varieties (Fandooghi and Kerman) have been analyzed by means of headspace solid-phase microextraction (HS-SPME) and gas chromatography-olfactometry (GCO). The aroma extract dilution analyses (AEDA) applied have revealed 46 and 41 odor-active regions with a flavor dilution (FD) factor≥64 for the Fandooghi and the Kerman varieties, respectively, and 39 of them were related to precisely identified compounds. These included esters, pyrazines, aldehydes, acids, furans, and phenols. The results show that the Fandooghi variety presents, not only more odor-active regions but also higher FD factors than the Kerman variety that can lead to the conclusion that the first variety has a richer aromatic profile than the second one. The descriptive sensory analysis (DSA) showed that the roasted, chocolate/coffee, and nutty attributes were rated significantly higher in the Fandooghi variety, whereas the green attribute was significantly higher in the Kerman one.

Identification and fingerprinting of biodiesel blends by solid phase extraction and gas chromatography-mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Yang, Z. [Environment Canada, Ottawa, ON (Canada). Emergencies Science and Technology Section, Emergencies, Operational Analytical Laboratories and Research Support Division; China Univ. of Geosciences, Wuhan (China). School of Environmental Studies; Hollebone, B.; Wang, Z.; Yang, C.; Landriault, M. [Environment Canada, Ottawa, ON (Canada). Emergencies Science and Technology Section, Emergencies, Operational Analytical Laboratories and Research Support Division

2009-07-01

Interest in biodiesel as a replacement for petroleum diesel fuel is growing. In North America, biodiesels are produced by the methyl esterification of plant and animal triglycerides, resulting in complex mixtures composed of fatty acid methyl esters (FAMEs). It is important for both environmental forensic and remediation purposes to determine diesel and biodiesel origins, and the biodiesel content when it is blended with conventional petroleum diesel. This paper reported on a study that combined 2 methods to determine biodiesel levels in blended fuels. Micro-column fractionation of FAMEs involving solid phase extraction (SPE) was combined with gas chromatography-mass spectrometry (GC/MS) to achieve detailed chemical fingerprinting of blends, including the identification and quantification of individual aliphatic hydrocarbons, aromatic hydrocarbons, fatty acid alkyl esters, and free sterols. Fractionation of the fuel samples was optimized for separation of fatty acid esters, free sterols from petroleum hydrocarbons into 4 fractions, notably aliphatic, aromatic, fatty-acid ester and polar components. A sum of the FAME components was used to determine an unknown blend level in freshly-prepared samples. This study showed that this method has great potential for identifying biodiesel in diesel fuel blends and could form the basis of a method for biodiesel-contaminated environmental samples. 28 refs., 5 tabs., 4 figs.

Identification and fingerprinting of biodiesel blends by solid phase extraction and gas chromatography-mass spectrometry

International Nuclear Information System (INIS)

Yang, Z.; China Univ. of Geosciences, Wuhan; Hollebone, B.; Wang, Z.; Yang, C.; Landriault, M.

2009-01-01

Interest in biodiesel as a replacement for petroleum diesel fuel is growing. In North America, biodiesels are produced by the methyl esterification of plant and animal triglycerides, resulting in complex mixtures composed of fatty acid methyl esters (FAMEs). It is important for both environmental forensic and remediation purposes to determine diesel and biodiesel origins, and the biodiesel content when it is blended with conventional petroleum diesel. This paper reported on a study that combined 2 methods to determine biodiesel levels in blended fuels. Micro-column fractionation of FAMEs involving solid phase extraction (SPE) was combined with gas chromatography-mass spectrometry (GC/MS) to achieve detailed chemical fingerprinting of blends, including the identification and quantification of individual aliphatic hydrocarbons, aromatic hydrocarbons, fatty acid alkyl esters, and free sterols. Fractionation of the fuel samples was optimized for separation of fatty acid esters, free sterols from petroleum hydrocarbons into 4 fractions, notably aliphatic, aromatic, fatty-acid ester and polar components. A sum of the FAME components was used to determine an unknown blend level in freshly-prepared samples. This study showed that this method has great potential for identifying biodiesel in diesel fuel blends and could form the basis of a method for biodiesel-contaminated environmental samples. 28 refs., 5 tabs., 4 figs.

Solid phase transformations

CERN Document Server

Čermák, J

2008-01-01

This special-topic book, devoted to ""Solid Phase Transformations"" , covers a broad range of phenomena which are of importance in a number of technological processes. Most commercial alloys undergo thermal treatment after casting, with the aim of imparting desired compositions and/or optimal morphologies to the component phases. In spite of the fact that the topic has lain at the center of physical metallurgy for a long time, there are numerous aspects which are wide open to potential investigative breakthroughs. Materials with new structures also stimulate research in the field, as well as n

Vapor phase epitaxy of silicon on meso porous silicon for deposition on economical substrate and low cost photovoltaic application

International Nuclear Information System (INIS)

Quoizola, S.

2003-01-01

The silicon is more and more used in the industry. Meanwhile the production cost is a problem to solve to develop the photovoltaic cells production. This thesis presents a new technology based on the use of a meso-porous silicon upper layer,to grow the active silicon layer of 50 μm width. The photovoltaic cell is then realized, the device is removed and placed on a low cost substrate. The silicon substrate of beginning can be used again after cleaning. The first chapter presents the operating and the characteristics of the silicon photovoltaic cell. The second chapter is devoted to the growth technique, the vapor phase epitaxy, and the third chapter to the epitaxy layer. The chapter four deals with the porous silicon and the structure chosen in this study. The chapter five is devoted to the characterization of the epitaxy layer on porous silicon. The photovoltaic cells realized on these layers are presented in the last chapter. (A.L.B.)

Application of process tomography in gas-solid fluidised beds in different scales and structures

Science.gov (United States)

Wang, H. G.; Che, H. Q.; Ye, J. M.; Tu, Q. Y.; Wu, Z. P.; Yang, W. Q.; Ocone, R.

2018-04-01

Gas-solid fluidised beds are commonly used in particle-related processes, e.g. for coal combustion and gasification in the power industry, and the coating and granulation process in the pharmaceutical industry. Because the operation efficiency depends on the gas-solid flow characteristics, it is necessary to investigate the flow behaviour. This paper is about the application of process tomography, including electrical capacitance tomography (ECT) and microwave tomography (MWT), in multi-scale gas-solid fluidisation processes in the pharmaceutical and power industries. This is the first time that both ECT and MWT have been applied for this purpose in multi-scale and complex structure. To evaluate the sensor design and image reconstruction and to investigate the effects of sensor structure and dimension on the image quality, a normalised sensitivity coefficient is introduced. In the meantime, computational fluid dynamic (CFD) analysis based on a computational particle fluid dynamic (CPFD) model and a two-phase fluid model (TFM) is used. Part of the CPFD-TFM simulation results are compared and validated by experimental results from ECT and/or MWT. By both simulation and experiment, the complex flow hydrodynamic behaviour in different scales is analysed. Time-series capacitance data are analysed both in time and frequency domains to reveal the flow characteristics.

A novel series of isoreticular metal organic frameworks: Realizing metastable structures by liquid phase epitaxy

KAUST Repository

Liu, Jinxuan; Lukose, Binit; Shekhah, Osama; Arslan, Hasan Kemal; Weidler, Peter; Gliemann, Hartmut; Brä se, Stefan; Grosjean, Sylvain; Godt, Adelheid; Feng, Xinliang; Mü llen, Klaus; Magdau, Ioan-Bogdan; Heine, Thomas; Wö ll, Christof

2012-01-01

A novel class of metal organic frameworks (MOFs) has been synthesized from Cu-acetate and dicarboxylic acids using liquid phase epitaxy. The SURMOF-2 isoreticular series exhibits P4 symmetry, for the longest linker a channel-size of 3 3 nm2 is obtained, one of the largest values reported for any MOF so far. High quality, ab-initio electronic structure calculations confirm the stability of a regular packing of (Cu++) 2-carboxylate paddle-wheel planes with P4 symmetry and reveal, that the SURMOF-2 structures are in fact metastable, with a fairly large activation barrier for the transition to the bulk MOF-2 structures exhibiting a lower, twofold (P2 or C2) symmetry. The theoretical calculations also allow identifying the mechanism for the low-temperature epitaxial growth process and to explain, why a synthesis of this highly interesting, new class of high-symmetry, metastable MOFs is not possible using the conventional solvothermal process.

A novel series of isoreticular metal organic frameworks: Realizing metastable structures by liquid phase epitaxy

KAUST Repository

Liu, Jinxuan

2012-12-04

A novel class of metal organic frameworks (MOFs) has been synthesized from Cu-acetate and dicarboxylic acids using liquid phase epitaxy. The SURMOF-2 isoreticular series exhibits P4 symmetry, for the longest linker a channel-size of 3 3 nm2 is obtained, one of the largest values reported for any MOF so far. High quality, ab-initio electronic structure calculations confirm the stability of a regular packing of (Cu++) 2-carboxylate paddle-wheel planes with P4 symmetry and reveal, that the SURMOF-2 structures are in fact metastable, with a fairly large activation barrier for the transition to the bulk MOF-2 structures exhibiting a lower, twofold (P2 or C2) symmetry. The theoretical calculations also allow identifying the mechanism for the low-temperature epitaxial growth process and to explain, why a synthesis of this highly interesting, new class of high-symmetry, metastable MOFs is not possible using the conventional solvothermal process.

Determination of organotin compounds by headspace solid-phase microextraction-gas chromatography-pulsed flame-photometric detection (HS-SPME-GC-PFPD)

Energy Technology Data Exchange (ETDEWEB)

Bravo, Manuel [Universite de Pau et des Pays de L' Adour, Laboratoire de Chimie Analytique, LCABIE, UMR CNRS 5034, Pau (France); Pontificia Universidad Catolica de Valparaiso, Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Valparaiso (Chile); Lespes, Gaetane; Gautier, Martine Potin [Pontificia Universidad Catolica de Valparaiso, Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Valparaiso (Chile); Gregori, Ida de; Pinochet, Hugo [Universite de Pau et des Pays de L' Adour, Laboratoire de Chimie Analytique, LCABIE, UMR CNRS 5034, Pau (France)

2005-12-01

A method based on Headspace solid-phase microextraction (HS-SPME, with a 100 {mu}m PDMS-fiber) in combination with gas-chromatography and pulsed flame-photometric detection (GC-PFPD) has been investigated for simultaneous determination of eight organotin compounds. Monobutyltin (MBT), dibutyltin (DBT), tributyltin (TBT), monophenyltin (MPhT), and the semi-volatile diphenyltin (DPhT), triphenyltin (TPhT), monooctyltin (MOcT), and dioctyltin (DOcT) were determined after derivatization with sodium tetraethylborate. The conditions used for the extraction and preconcentration step were optimised by experimental design methodology. Tripropyltin (TPrT) and diheptyltin (DHepT) were used as internal standards for quantification of volatile and semi-volatile organotin compounds, respectively. The analytical precision (RSD) for ten successive injections of a standard mixture containing all the organic tin compounds ranged between 2 and 11%. The limits of detection for all the organotin compounds were sub ng (Sn) L{sup -1} in water and close to ng (Sn) kg{sup -1} in sediments. The accuracy of the method was evaluated by analysis of two certified reference material (CRM) sediment samples. The HS-SPME-GC-PFPD was then applied to the analysis of three harbour sediment samples. The results showed that headspace SPME is an attractive tool for analysis of organotin compounds in solid environmental matrices. (orig.)

Determination of chlorophenols in landfill leachate using headspace sampling with ionic liquid-coated solid-phase microextraction fibers combined with gas chromatography–mass spectrometry

International Nuclear Information System (INIS)

Ho, Tse-Tsung; Chen, Chung-Yu; Li Zuguang; Yang, Thomas Ching-Cherng; Lee, Maw-Rong

2012-01-01

Highlights: ► Ionic liquid (IL), ([C 4 MIM][PF 6 ]), was rapid synthesized by microwave radiation. ► Trace chlorophenols in landfill leachate were extract by SPME coated IL. ► The IL-coated SPME-GC/MS method is low-cost, solvent-free and sensitive. - Abstract: A new microextraction technique based on ionic liquid solid-phase microextraction (IL-SPME) was developed for determination of trace chlorophenols (CPs) in landfill leachate. The synthesized ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate ([C 4 MIM][PF 6 ]), was coated onto the spent fiber of SPME for extraction of trace CPs. After extraction, the absorbed analytes were desorbed and quantified using gas chromatography–mass spectrometry (GC/MS). The term of the proposed method is as ionic liquid-coated of solid-phase microextraction combined with gas chromatography–mass spectrometry (IL-SPME-GC/MS). No carryover effect was found, and every laboratory-made ionic liquids-coated-fiber could be used for extraction at least eighty times without degradation of efficiency. The chlorophenols studied were 2,4-dichlorophenol (2,4-DP), 2,4,6-trichlorophenol (2,4,6-TCP), 2,3,4,6-tetrachlorophenol (2,3,4,6-TeCP), and pentachlorophenol (PCP). The best results of chlorophenols analysis were obtained with landfill leachate at pH 2, headspace extraction for 4 min, and thermal desorption with the gas chromatograph injector at 240 °C for 4 min. Linearity was observed from 0.1 to 1000 μg L −1 with relative standard deviations (RSD) less than 7% and recoveries were over 87%. The limit of detection (LOD) for pentachlorophenol was 0.008 μg L −1 . The proposed method was tested by analyzing landfill leachate from a sewage farm. The concentrations of chlorophenols were detected to range from 1.1 to 1.4 μg L −1 . The results demonstrate that the IL-SPME-GC/MS method is highly effective in analyzing trace chlorophenols in landfill leachate.

Determination of chlorophenols in landfill leachate using headspace sampling with ionic liquid-coated solid-phase microextraction fibers combined with gas chromatography-mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Ho, Tse-Tsung; Chen, Chung-Yu [Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan (China); Li Zuguang [Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan (China); College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310014, Zhejiang (China); Yang, Thomas Ching-Cherng [Department of Chemistry, National Kaohsiung Normal University, Kaohsiung 82444, Taiwan (China); Lee, Maw-Rong, E-mail: mrlee@dragon.nchu.edu.tw [Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan (China)

2012-01-27

Highlights: Black-Right-Pointing-Pointer Ionic liquid (IL), ([C{sub 4}MIM][PF{sub 6}]), was rapid synthesized by microwave radiation. Black-Right-Pointing-Pointer Trace chlorophenols in landfill leachate were extract by SPME coated IL. Black-Right-Pointing-Pointer The IL-coated SPME-GC/MS method is low-cost, solvent-free and sensitive. - Abstract: A new microextraction technique based on ionic liquid solid-phase microextraction (IL-SPME) was developed for determination of trace chlorophenols (CPs) in landfill leachate. The synthesized ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate ([C{sub 4}MIM][PF{sub 6}]), was coated onto the spent fiber of SPME for extraction of trace CPs. After extraction, the absorbed analytes were desorbed and quantified using gas chromatography-mass spectrometry (GC/MS). The term of the proposed method is as ionic liquid-coated of solid-phase microextraction combined with gas chromatography-mass spectrometry (IL-SPME-GC/MS). No carryover effect was found, and every laboratory-made ionic liquids-coated-fiber could be used for extraction at least eighty times without degradation of efficiency. The chlorophenols studied were 2,4-dichlorophenol (2,4-DP), 2,4,6-trichlorophenol (2,4,6-TCP), 2,3,4,6-tetrachlorophenol (2,3,4,6-TeCP), and pentachlorophenol (PCP). The best results of chlorophenols analysis were obtained with landfill leachate at pH 2, headspace extraction for 4 min, and thermal desorption with the gas chromatograph injector at 240 Degree-Sign C for 4 min. Linearity was observed from 0.1 to 1000 {mu}g L{sup -1} with relative standard deviations (RSD) less than 7% and recoveries were over 87%. The limit of detection (LOD) for pentachlorophenol was 0.008 {mu}g L{sup -1}. The proposed method was tested by analyzing landfill leachate from a sewage farm. The concentrations of chlorophenols were detected to range from 1.1 to 1.4 {mu}g L{sup -1}. The results demonstrate that the IL-SPME-GC/MS method is highly effective in

Gas Source Techniques for Molecular Beam Epitaxy of Highly Mismatched Ge Alloys

OpenAIRE

Chad A. Stephenson; Miriam Gillett-Kunnath; William A. O’Brien; Robert Kudrawiec; Mark A. Wistey

2016-01-01

Ge and its alloys are attractive candidates for a laser compatible with silicon integrated circuits. Dilute germanium carbide (Ge1−xCx) offers a particularly interesting prospect. By using a precursor gas with a Ge4C core, C can be preferentially incorporated in substitutional sites, suppressing interstitial and C cluster defects. We present a method of reproducible and upscalable gas synthesis of tetrakis(germyl)methane, or (H3Ge)4C, followed by the design of a hybrid gas/solid-source molecu...

Slurried solid media for simultaneous water purification and carbon dioxide removal from gas mixtures

Science.gov (United States)

Aines, Roger D.; Bourcier, William L.; Viani, Brian

2013-01-29

A slurried solid media for simultaneous water purification and carbon dioxide removal from gas mixtures includes the steps of dissolving the gas mixture and carbon dioxide in water providing a gas, carbon dioxide, water mixture; adding a porous solid media to the gas, carbon dioxide, water mixture forming a slurry of gas, carbon dioxide, water, and porous solid media; heating the slurry of gas, carbon dioxide, water, and porous solid media producing steam; and cooling the steam to produce purified water and carbon dioxide.

Solid-Solid Vacuum Regolith Heat-Exchanger for Oxygen Production, Phase I

Data.gov (United States)

National Aeronautics and Space Administration — This SBIR Phase-1 project will demonstrate the feasibility of using a novel coaxial counterflow solid-solid heat exchanger to recover heat energy from spent regolith...

Methodology for the determination of residues of organophosphorous pesticides in milk of domestic consumption by means of gas chromatography and extraction in solid phase

International Nuclear Information System (INIS)

Romero Blanco, Eric; Meza Nunez, Humberto; Poveda Calvo, Vanessa

2005-01-01

A new method oriented to the detection and quantification of 15 organophosphate pesticide in raw milk samples for national consumption has been developed by using a gas chromatograph equipped with polydimethylsiloxane capillary column and a nitrogen-phosphorus detector (NPD), in combination with the extraction technique in solid phase (SPE) for the sample cleaning process and pesticide extraction. Recovery percentages obtained were close to 100% and the detection limits obtained were lower than 20 μg/L for 13 of the organophosphates analyzed. Overall, the method showed important improvement as compared to conventional liquid/liquid extraction methodologies. (Author) [es

Epitaxial thin film growth of LiH using a liquid-Li atomic template

International Nuclear Information System (INIS)

Oguchi, Hiroyuki; Ikeshoji, Tamio; Orimo, Shin-ichi; Ohsawa, Takeo; Shiraki, Susumu; Hitosugi, Taro; Kuwano, Hiroki

2014-01-01

We report on the synthesis of lithium hydride (LiH) epitaxial thin films through the hydrogenation of a Li melt, forming abrupt LiH/MgO interface. Experimental and first-principles molecular dynamics studies reveal a comprehensive microscopic picture of the crystallization processes, which sheds light on the fundamental atomistic growth processes that have remained unknown in the vapor-liquid-solid method. We found that the periodic structure that formed, because of the liquid-Li atoms at the film/MgO-substrate interface, serves as an atomic template for the epitaxial growth of LiH crystals. In contrast, films grown on the Al 2 O 3 substrates indicated polycrystalline films with a LiAlO 2 secondary phase. These results and the proposed growth process provide insights into the preparation of other alkaline metal hydride thin films on oxides. Further, our investigations open the way to explore fundamental physics and chemistry of metal hydrides including possible phenomena that emerge at the heterointerfaces of metal hydrides

EDITORIAL: Epitaxial graphene Epitaxial graphene

Science.gov (United States)

de Heer, Walt A.; Berger, Claire

2012-04-01

Graphene is widely regarded as an important new electronic material with interesting two-dimensional electron gas properties. Not only that, but graphene is widely considered to be an important new material for large-scale integrated electronic devices that may eventually even succeed silicon. In fact, there are countless publications that demonstrate the amazing applications potential of graphene. In order to realize graphene electronics, a platform is required that is compatible with large-scale electronics processing methods. It was clear from the outset that graphene grown epitaxially on silicon carbide substrates was exceptionally well suited as a platform for graphene-based electronics, not only because the graphene sheets are grown directly on electronics-grade silicon carbide (an important semiconductor in its own right), but also because these sheets are oriented with respect to the semiconductor. Moreover, the extremely high temperatures involved in production assure essentially defect-free and contamination-free materials with well-defined interfaces. Epitaxial graphene on silicon carbide is not a unique material, but actually a class of materials. It is a complex structure consisting of a reconstructed silicon carbide surface, which, for planar hexagonal silicon carbide, is either the silicon- or the carbon-terminated face, an interfacial carbon rich layer, followed by one or more graphene layers. Consequently, the structure of graphene films on silicon carbide turns out to be a rich surface-science puzzle that has been intensively studied and systematically unravelled with a wide variety of surface science probes. Moreover, the graphene films produced on the carbon-terminated face turn out to be rotationally stacked, resulting in unique and important structural and electronic properties. Finally, in contrast to essentially all other graphene production methods, epitaxial graphene can be grown on structured silicon carbide surfaces to produce graphene

Solid-phase spectrophotometry

International Nuclear Information System (INIS)

Brykina, G.D.; Marchenko, D.Yu.; Shpigun, O.A.

1995-01-01

Solid-phase spectrophotometry (SPS), which is based on the direct measurement of light absorption of an ion exchanger containing a substance of interest, was reviewed. Since 1976, it has been known that aborbance of an ion exchanger is directly proportional to the concentration of a particular ion in solution. A similar dependence can also be followed for other sorbents, as well as for foams, membranes, films, etc., which do not exhibit ion exchange properties. One can use absorption, diffuse reflection, and luminescence spectra parameters as an analytical signal. Thus, SPS of ion exchangers is among the analytical techniques that combine the sorption concentration and surface determination of the substance of interest. This review summarizes the advancements in SPS over the last six years and demonstrates the prospects for its development. Special attention is paid to experimental methods for measuring solid-phase absorption and to the basic procedures of sample preparation, including new ones. These two facets are of great importance for obtaining precise results and extending the capabilities of SPS

Influence of epitaxial strain on multiple-mode compounds: The case of SrBi.sub.2./sub.Nb.sub.2./sub.O.sub.9./sub.

Czech Academy of Sciences Publication Activity Database

Petralanda, U.; Hlinka, Jiří; Extebarria, I.

2017-01-01

Roč. 96, č. 14 (2017), s. 1-7, č. článku 144112. ISSN 2469-9950 R&D Projects: GA ČR GA15-04121S Grant - others:AV ČR(CZ) PAN-17-04 Program:Bilaterální spolupráce Institutional support: RVO:68378271 Keywords : ferroelectrics * thin films * epitaxy * ab-initio methods * phase transitions Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 3.836, year: 2016

Selected Topics on Mass Transport in Gas-solid Interactions

DEFF Research Database (Denmark)

Somers, Marcel A.J.

2004-01-01

The present article is a short review containing examples of the role of mass transport in the solid state during gas-solid interactions. Examples are taken from the authors' research on the interaction of carbon and/or nitrogen with iron-based metals. Topics dealt with are diffusion-controlled d......The present article is a short review containing examples of the role of mass transport in the solid state during gas-solid interactions. Examples are taken from the authors' research on the interaction of carbon and/or nitrogen with iron-based metals. Topics dealt with are diffusion...... on the kinetics of phenomena in the solid state. Various experimental techniques were applied to investigate these phenomena; it is however beyond the scope of the present article to treat experimental conditions in detail. The interested reader is referred to the original work for in depth discussions...

Visualizing Gas Adsorption on Porous Solids: Four Simple, Effective Demonstrations

Science.gov (United States)

Cheung, Ocean

2014-01-01

Gas adsorption on porous solids is a topic that is often discussed in an undergraduate chemistry or chemical engineering course. The idea of porosity and gas adsorption on a porous solid is usually discussed with adsorption isotherms recorded using commercially available equipment. This discussion can be rather abstract and can be difficult for…

Application of head-space solid-phase microextraction for the analysis of volatile metabolites emitted by Penicillium species

DEFF Research Database (Denmark)

Nilsson, Torben; Larsen, Thomas Ostenfeld; Montanarella, Luca

1996-01-01

Head-space solid-phase microextraction (HS-SPME) has been used to collect volatile organic compounds (VOCs) emitted from fungi of the genus Penicillium. Gas chromatography combined with mass spectrometry (GC-MS) was employed for the analysis of the profiles of volatile metabolites characteristic...

InAs/GaAs quantum dot lasers with InGaP cladding layer grown by solid-source molecular-beam epitaxy

International Nuclear Information System (INIS)

Yeh, N.-T.; Liu, W.-S.; Chen, S.-H.; Chiu, P.-C.; Chyi, J.-I.

2002-01-01

This letter presents the lasing properties of InAs/GaAs quantum dot lasers with InGaP cladding layers grown by solid-source molecular-beam epitaxy. These Al-free lasers exhibit a threshold current density of 138 A/cm 2 , an internal loss of 1.35 cm -1 , and an internal quantum efficiency of 31% at room temperature. At a low temperature, a very high characteristic temperature of 425 K and very low threshold current density of 30 A/cm 2 are measured

Metalorganic vapor phase epitaxy of AlN on sapphire with low etch pit density

Science.gov (United States)

Koleske, D. D.; Figiel, J. J.; Alliman, D. L.; Gunning, B. P.; Kempisty, J. M.; Creighton, J. R.; Mishima, A.; Ikenaga, K.

2017-06-01

Using metalorganic vapor phase epitaxy, methods were developed to achieve AlN films on sapphire with low etch pit density (EPD). Key to this achievement was using the same AlN growth recipe and only varying the pre-growth conditioning of the quartz-ware. After AlN growth, the quartz-ware was removed from the growth chamber and either exposed to room air or moved into the N2 purged glove box and exposed to H2O vapor. After the quartz-ware was exposed to room air or H2O, the AlN film growth was found to be more reproducible, resulting in films with (0002) and (10-12) x-ray diffraction (XRD) rocking curve linewidths of 200 and 500 arc sec, respectively, and EPDs < 100 cm-2. The EPD was found to correlate with (0002) linewidths, suggesting that the etch pits are associated with open core screw dislocations similar to GaN films. Once reproducible AlN conditions were established using the H2O pre-treatment, it was found that even small doses of trimethylaluminum (TMAl)/NH3 on the quartz-ware surfaces generated AlN films with higher EPDs. The presence of these residual TMAl/NH3-derived coatings in metalorganic vapor phase epitaxy (MOVPE) systems and their impact on the sapphire surface during heating might explain why reproducible growth of AlN on sapphire is difficult.

Solid Organic Deposition During Gas Injection Studies

DEFF Research Database (Denmark)

Dandekar, Abhijit Y.; Andersen, Simon Ivar; Stenby, Erling Halfdan

2000-01-01

Recently a series of first contact miscibility (swelling) experiments have been performed on undersaturated light and heavy oils using LPG rich and methane rich injection gases, in which solid organic deposition was observed. A compositional gradient in the oils during the gas injection process....... The asphaltene content of the different oil samples were determined by the TP 143 method. The standard asphaltenes and the solid organic deposit recovered from the swelling tests were analyzed using FTIR, HPLC-SEC and H-1 NMR. The aim of these analyses is to reveal the molecular nature of the deposits formed...... during the gas injection process in comparison with the standard asphaltenes in order to understand the mechanisms involved in asphaltene deposition....

Coefficient of solid-gas heat transfer in particle fixed bed; Coeficiente de transferencia de calor gas-solido em leito fixo de particulas

Energy Technology Data Exchange (ETDEWEB)

Fernandes Filho, Francisco

1991-03-01

The work presents a study on heat transfer between gas and solid phases for fixed beds in the absence of mass transfer and chemical reactions. Mathematical models presented in the literature were analyzed concerning to the assumptions made on axial dispersion in the fluid phase and interparticle thermal conductivity. Heat transfer coefficients and their dependency on flow conditions, particles and packed bed characteristics were experimentally determined through the solution of the previous mathematical models. Pressure drop behaviour for the packed beds used for the heat transfer study was also included. (author) 32 refs., 12 figs.

Development of a simple and sensitive method for the characterization of odorous waste gas emissions by means of solid-phase microextraction (SPME) and GC-MS/olfactometry.

Science.gov (United States)

Kleeberg, K K; Liu, Y; Jans, M; Schlegelmilch, M; Streese, J; Stegmann, R

2005-01-01

A solid-phase microextraction (SPME) method has been developed for the extraction of odorous compounds from waste gas. The enriched compounds were characterized by gas chromatography-mass spectrometry (GC-MS) and gas chromatography followed by simultaneous flame ionization detection and olfactometry (GC-FID/O). Five different SPME fiber coatings were tested, and the carboxen/polydimethylsiloxane (CAR/PDMS) fiber showed the highest ability to extract odorous compounds from the waste gas. Furthermore, parameters such as exposure time, desorption temperature, and desorption time have been optimized. The SPME method was successfully used to characterize an odorous waste gas from a fat refinery prior to and after waste gas treatment in order to describe the treatment efficiency of the used laboratory scale plant which consisted of a bioscrubber/biofilter combination and an activated carbon adsorber. The developed method is a valuable approach to provide detailed information of waste gas composition and complements existing methods for the determination of odors. However, caution should be exercised if CAR/PDMS fibers are used for the quantification of odorous compounds in multi-component matrices like waste gas emissions since the relative affinity of each analyte was shown to differ according to the total amount of analytes present in the sample.

A novel poly(3,4-ethylenedioxythiophene)-ionic liquid composite coating for the headspace solid-phase microextraction and gas chromatography determination of several alcohols in soft drinks.

Science.gov (United States)

Wu, Mian; Zhang, Haibo; Zhao, Faqiong; Zeng, Baizhao

2014-11-19

A novel poly(3,4-ethylenedioxythiophene)-ionic liquid (i.e., 1-hydroxyethyl-3-methyl imidazolium-bis[(trifluoromethyl)sulfonyl]imide) composite film was electrodeposited on a Pt wire for headspace solid-phase microextraction. The film showed nodular structure and had large specific surface. In addition, it displayed high thermal stability (up to 300°C) and durable property (could be used for more than 200 times). Coupled with gas chromatography-flame ionization detection, the resulting fiber was applied to the headspace solid-phase microextraction and determination of several alcohols (i.e., linalool, nonanol, terpineol, geraniol, decanol and dodecanol). It presented higher extraction capability in comparison with the poly(3,4-ethylenedioxythiophene) and commercial polydimethylsiloxane/divinylbenzene fiber. Under the optimized conditions, the linear ranges exceeded three magnitudes with correlation coefficients above 0.9952 and the low limits of detection were 34.2-81.3ng L(-1). For different alcohols the repeatabilities (defined as RSD) were alcohols in real samples with acceptable recoveries from 81.1% to 106.6%. Copyright © 2014 Elsevier B.V. All rights reserved.

GaN/NbN epitaxial semiconductor/superconductor heterostructures

Science.gov (United States)

Yan, Rusen; Khalsa, Guru; Vishwanath, Suresh; Han, Yimo; Wright, John; Rouvimov, Sergei; Katzer, D. Scott; Nepal, Neeraj; Downey, Brian P.; Muller, David A.; Xing, Huili G.; Meyer, David J.; Jena, Debdeep

2018-03-01

Epitaxy is a process by which a thin layer of one crystal is deposited in an ordered fashion onto a substrate crystal. The direct epitaxial growth of semiconductor heterostructures on top of crystalline superconductors has proved challenging. Here, however, we report the successful use of molecular beam epitaxy to grow and integrate niobium nitride (NbN)-based superconductors with the wide-bandgap family of semiconductors—silicon carbide, gallium nitride (GaN) and aluminium gallium nitride (AlGaN). We apply molecular beam epitaxy to grow an AlGaN/GaN quantum-well heterostructure directly on top of an ultrathin crystalline NbN superconductor. The resulting high-mobility, two-dimensional electron gas in the semiconductor exhibits quantum oscillations, and thus enables a semiconductor transistor—an electronic gain element—to be grown and fabricated directly on a crystalline superconductor. Using the epitaxial superconductor as the source load of the transistor, we observe in the transistor output characteristics a negative differential resistance—a feature often used in amplifiers and oscillators. Our demonstration of the direct epitaxial growth of high-quality semiconductor heterostructures and devices on crystalline nitride superconductors opens up the possibility of combining the macroscopic quantum effects of superconductors with the electronic, photonic and piezoelectric properties of the group III/nitride semiconductor family.

Molecular structure determination of cyclooctane by Ab Initio and electron diffraction methods in the gas phase

International Nuclear Information System (INIS)

Almeida, Wagner B. de

2000-01-01

The determination of the molecular structure of molecules is of fundamental importance in chemistry. X-rays and electron diffraction methods constitute in important tools for the elucidation of the molecular structure of systems in the solid state and gas phase, respectively. The use of quantum mechanical molecular orbital ab initio methods offer an alternative for conformational analysis studies. Comparison between theoretical results and those obtained experimentally in the gas phase can make a significant contribution for an unambiguous determination of the geometrical parameters. In this article the determination for an unambiguous determination of the geometrical parameters. In this article the determination of the molecular structure of the cyclooctane molecule by electron diffraction in the gas phase an initio calculations will be addressed, providing an example of a comparative analysis of theoretical and experimental predictions. (author)

Solid phase microextraction capillary gas chromatography combined with furnace atomization plasma emission spectrometry for speciation of mercury in fish tissues

International Nuclear Information System (INIS)

Grinberg, Patricia; Campos, Reinaldo C.; Mester, Zoltan; Sturgeon, Ralph E.

2003-01-01

The use of solid phase microextraction in conjunction with tandem gas chromatography-furnace atomization plasma emission spectrometry (SPME-GC-FAPES) was evaluated for the determination of methylmercury and inorganic mercury in fish tissue. Samples were digested with methanolic potassium hydroxide, derivatized with sodium tetraethylborate and extracted by SPME. After the SPME extraction, species were separated by GC and detected by FAPES. All experimental parameters were optimized for best separation and analytical response. A repeatability precision of typically 2% can be achieved with long-term (3 months) reproducibility precision of 4.3%. Certified Reference Materials DORM-2, DOLT-2 and TORT-2 from the National Research Council of Canada were analyzed to verify the accuracy of this technique. Detection limits of 1.5 ng g -1 for methylmercury and 0.7 ng g -1 for inorganic mercury in biological tissues were obtained

Wax Precipitation Modeled with Many Mixed Solid Phases

DEFF Research Database (Denmark)

Heidemann, Robert A.; Madsen, Jesper; Stenby, Erling Halfdan

2005-01-01

The behavior of the Coutinho UNIQUAC model for solid wax phases has been examined. The model can produce as many mixed solid phases as the number of waxy components. In binary mixtures, the solid rich in the lighter component contains little of the heavier component but the second phase shows sub......-temperature and low-temperature forms, are pure. Model calculations compare well with the data of Pauly et al. for C18 to C30 waxes precipitating from n-decane solutions. (C) 2004 American Institute of Chemical Engineers....

Solid-phase microextraction gas chromatography-mass spectrometry determination of fragrance allergens in baby bathwater.

Science.gov (United States)

Lamas, J Pablo; Sanchez-Prado, Lucia; Garcia-Jares, Carmen; Llompart, Maria

2009-07-01

A method based on solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) has been optimized for the determination of fragrance allergens in water samples. This is the first study devoted to this family of cosmetic ingredients performed by SPME. The influence of parameters such as fibre coating, extraction and desorption temperatures, salting-out effect and sampling mode on the extraction efficiency has been studied by means of a mixed-level factorial design, which allowed the study of the main effects as well as two-factor interactions. Excluding desorption temperature, the other parameters were, in general, very important for the achievement of high response. The final procedure was based on headspace sampling at 100 degrees C, using polydimethylsiloxane/divinylbenzene fibres. The method showed good linearity and precision for all compounds, with detection limits ranging from 0.001 to 0.3 ng mL(-1). Reliability was demonstrated through the evaluation of the recoveries in different real water samples, including baby bathwater and swimming pool water. The absence of matrix effects allowed the use of external standard calibration to quantify the target compounds in the samples. The proposed procedure was applied to the determination of allergens in several real samples. All the target compounds were found in the samples, and, in some cases, at quite high concentrations. The presence and the levels of these chemicals in baby bathwater should be a matter of concern.

Characterization of low Al content Al{sub x}Ga{sub 1-x}N epitaxial films grown by atmospheric-pressure MOVPE

Energy Technology Data Exchange (ETDEWEB)

Toure, A.; Halidou, I.; Benzarti, Z.; Bchetnia, A.; El Jani, B. [Faculte des Sciences, Unite de Recherche sur les Hetero-Epitaxies et Applications, 5019 Monastir (Tunisia); Fouzri, A. [Laboratoire Physico-Chimie des Materiaux, Faculte des Sciences de Monastir, Unite de Service Commun de Recherche ' ' High Resolution X-ray Diffractometer' ' , 5019 Monastir (Tunisia)

2012-05-15

Al{sub x}Ga{sub 1-x}N epitaxial films grown on GaN/sapphire by atmospheric-pressure metalorganic vapor phase epitaxy (AP-MOVPE) using trimethylgallium (TMG) and trimethylaluminum (TMA) as group III precursors have been studied. Two groups of samples were grown. The aluminum (Al) solid composition of Al{sub x}Ga{sub 1-x}N was varied in the range from 0.03 to 0.20 by changing the molar flow ratio [TMA/(TMA + TMG)]. The effect of TMA flow rate, respectively, TMG flow rate, on the growth rate, and Al solid composition is discussed. The structural properties of the alloys have been investigated by high-resolution X-ray diffraction (HRXRD). The optical properties of these samples were investigated by photoluminescence (PL). It is found that on increasing Al solid composition, via an increase of the TMA flow rate, the structural quality is deteriorated and the growth efficiency decreases. On the other hand, when the TMG flow rate is reduced, a decrease of the full width at half-maximum (FWHM) is observed with Al content. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

In situ TEM observation of solid-gas reactions

International Nuclear Information System (INIS)

Kishita, K; Kamino, T; Watabe, A; Kuroda, K; Saka, H

2008-01-01

Under a gaseous atmosphere at high temperatures, almost all the materials (metal, catalysts, etc.) change their structures and properties. For the research and development of materials, it is of vital importance to clarify mechanisms of solid-gas and liquid-gas reactions. Recently an in situ TEM system combined with an environmental holder, which has a gas injection nozzle close to a specimen-heating element, has been developed. The gas injection nozzle permits gas to flow around the specimens sitting on the heating element made of a fine W filament. The newly developed in situ TEM has a differential pumping system; therefore, the pressure in the specimen chamber is maintained in the range of higher than 1 Pa, while the pressure in the electron gun chamber can be kept in the range of 10 -5 Pa. This system was applied to in situ observation of chemical reactions of metals with gases: Observation of oxidation and reduction under a gas pressure ranging from 10 -5 Pa to 1 Pa at high temperatures (room temperature to ∼1473 K) were successfully carried out on pure metal and rare metal catalysts at near-atomic resolution. This in situ environmental TEM system is promising for clarifying mechanisms of many solid-gas and liquid-gas reactions that take place at high temperatures under a gas atmosphere.

Land application uses for dry flue gas desulfurization by-products: Phase 3

Energy Technology Data Exchange (ETDEWEB)

Dick, W.; Bigham, J.; Forster, R.; Hitzhusen, F.; Lal, R.; Stehouwer, R.; Traina, S.; Wolfe, W.; Haefner, R.; Rowe, G.

1999-01-31

New flue gas desulfurization (FGD) scrubbing technologies create a dry, solid by-product material consisting of excess sorbent, reaction product that contains sulfate and sulfite, and coal fly ash. Generally, dry FGD by-products are treated as solid wastes and disposed in landfills. However, landfill sites are becoming scarce and tipping fees are constantly increasing. Provided the environmental impacts are socially and scientifically acceptable, beneficial uses via recycling can provide economic benefits to both the producer and the end user of the FGD. A study titled ''Land Application Uses for Dry Flue Gas Desulfurization By-Products'' was initiated in December, 1990 to develop and demonstrate large volume, beneficial uses of FGD by-products. Phase 1 and Phase 2 reports have been published by the Electric Power Research Institute (EPRI), Palo Alto, CA. Phase 3 objectives were to demonstrate, using field studies, the beneficial uses of FGD by-products (1) as an amendment material on agricultural lands and on abandoned surface coal mine land, (2) as an engineering material for soil stabilization and raid repair, and (3) to assess the environmental and economic impacts of such beneficial uses. Application of dry FGD by-product to three soils in place of agricultural limestone increased alfalfa (Medicago sativa L.) and corn (Zea may L.) yields. No detrimental effects on soil and plant quality were observed.

Solid - solid and solid - liquid phase transitions of iron and iron alloys under laser shock compression

Science.gov (United States)

Harmand, M.; Krygier, A.; Appel, K.; Galtier, E.; Hartley, N.; Konopkova, Z.; Lee, H. J.; McBride, E. E.; Miyanishi, K.; Nagler, B.; Nemausat, R.; Vinci, T.; Zhu, D.; Ozaki, N.; Fiquet, G.

2017-12-01

An accurate knowledge of the properties of iron and iron alloys at high pressures and temperatures is crucial for understanding and modelling planetary interiors. While Earth-size and Super-Earth Exoplanets are being discovered in increasingly large numbers, access to detailed information on liquid properties, melting curves and even solid phases of iron and iron at the pressures and temperatures of their interiors is still strongly limited. In this context, XFEL sources coupled with high-energy lasers afford unique opportunities to measure microscopic structural properties at far extreme conditions. Also the achievable time resolution allows the shock history and phase transition mechanisms to be followed during laser compression, improving our understanding of the high pressure and high strain experiments. Here we present recent studies devoted to investigate the solid-solid and solid-liquid transition in laser-shocked iron and iron alloys (Fe-Si, Fe-C and Fe-O alloys) using X-ray diffraction and X-ray diffuse scattering. Experiment were performed at the MEC end-station of the LCLS facility at SLAC (USA). Detection of the diffuse scattering allowed the identification of the first liquid peak position along the Hugoniot, up to 4 Mbar. The time resolution shows ultrafast (between several tens and several hundreds of picoseconds) solid-solid and solid-liquid phase transitions. Future developments at XFEL facilities will enable detailed studies of the solid and liquid structures of iron and iron alloys as well as out-of-Hugoniot studies.

Epitaxial strain-engineered self-assembly of magnetic nanostructures in FeRh thin films

International Nuclear Information System (INIS)

Witte, Ralf; Kruk, Robert; Molinari, Alan; Wang, Di; Brand, Richard A; Hahn, Horst; Schlabach, Sabine; Provenzano, Virgil

2017-01-01

In this paper we introduce an innovative bottom–up approach for engineering self-assembled magnetic nanostructures using epitaxial strain-induced twinning and phase separation. X-ray diffraction, 57 Fe Mössbauer spectroscopy, scanning tunneling microscopy, and transmission electron microscopy show that epitaxial films of a near-equiatomic FeRh alloy respond to the applied epitaxial strain by laterally splitting into two structural phases on the nanometer length scale. Most importantly, these two structural phases differ with respect to their magnetic properties, one being paramagnetic and the other ferromagnetic, thus leading to the formation of a patterned magnetic nanostructure. It is argued that the phase separation directly results from the different strain-dependence of the total energy of the two competing phases. This straightforward relation directly enables further tailoring and optimization of the nanostructures’ properties. (paper)

Creating Ruddlesden-Popper phases by hybrid molecular beam epitaxy

Energy Technology Data Exchange (ETDEWEB)

Haislmaier, Ryan C.; Stone, Greg; Alem, Nasim; Engel-Herbert, Roman, E-mail: rue2@psu.edu [Department of Materials Science and Engineering, The Pennsylvania State University, University Park, Pennsylvania 16802 (United States)

2016-07-25

The synthesis of a 50 unit cell thick n = 4 Sr{sub n+1}Ti{sub n}O{sub 3n+1} (Sr{sub 5}Ti{sub 4}O{sub 13}) Ruddlesden-Popper (RP) phase film is demonstrated by sequentially depositing SrO and TiO{sub 2} layers in an alternating fashion using hybrid molecular beam epitaxy (MBE), where Ti was supplied using titanium tetraisopropoxide (TTIP). A detailed calibration procedure is outlined for determining the shuttering times to deposit SrO and TiO{sub 2} layers with precise monolayer doses using in-situ reflection high energy electron diffraction (RHEED) as feedback. Using optimized Sr and TTIP shuttering times, a fully automated growth of the n = 4 RP phase was carried out over a period of >4.5 h. Very stable RHEED intensity oscillations were observed over the entire growth period. The structural characterization by X-ray diffraction and high resolution transmission electron microscopy revealed that a constant periodicity of four SrTiO{sub 3} perovskite unit cell blocks separating the double SrO rocksalt layer was maintained throughout the entire film thickness with a very little amount of planar faults oriented perpendicular to the growth front direction. These results illustrate that hybrid MBE is capable of layer-by-layer growth with atomic level precision and excellent flux stability.

Growth of Ba1-zSrzBiO3-y single crystals and the prospects for its application for liquid phase epitaxy of Ba1-xKxBiO3-δ superconductor

International Nuclear Information System (INIS)

Soldatov, A.G.; Barilo, S.N.; Shiryaev, S.V.; Finskaya, V.M.

2002-01-01

In order to get a substrate for liquid phase epitaxy of the Ba 1-x K x BiO 3-δ (BKBO) superconducting films a possibility to grow single crystals of the Ba 1-z Sr z BiO 3-y (BSBO) solid solution series was investigated. The BSBO crystals with z = 0; 0.2; 0.29; 0.45; 0.49; 0.50; 0.54; 0.58 were obtained by crystallization from melt. The temperature versus composition phase diagram of the BaO · 1/2Bi 2 O 3 -SrO · 1/2Bi 2 O 3 system was constructed. A comparative analysis of the effect of cation composition and oxygen nonstoichiometry on the BSBO lattice parameters was carried out. The growth features of superconducting BKBO films onto BSBO substrates are discussed [ru

Two-phase air-solid stationary turbulent flow in a cylindrical tube, with a high massive concentration

International Nuclear Information System (INIS)

Fortier, Andre; Chen, Che Pen

1976-01-01

The momentum theorem, applied separately to the two phases (fluid and solid particles), together with the equations of continuity, gives two differential equations by which the pressure and the concentration along the longitudinal profile x can be computed. These equations can be obtained by introduction of several averaging procedures of physical significance. These quantities are defined in a simple manner for the general case. Using experimental measurements of solid particle velocities in a horizontal tube by radio-tracers, it is shown how to determine the three average coefficients: Λsub(g) friction coefficient of gas, Λsub(s) momentum loss coefficient of solid particles by impacts, against the wall, and Csub(D) drag coefficient due to the velocity difference between the two phases. This determination is based on the numerical solution of the two differential equations conveniently simplified [fr

Crystallization engineering as a route to epitaxial strain control

Directory of Open Access Journals (Sweden)

Andrew R. Akbashev

2015-10-01

Full Text Available The controlled synthesis of epitaxial thin films offers opportunities for tuning their functional properties via enabling or suppressing strain relaxation. Examining differences in the epitaxial crystallization of amorphous oxide films, we report on an alternate, low-temperature route for strain engineering. Thin films of amorphous Bi–Fe–O were grown on (001SrTiO3 and (001LaAlO3 substrates via atomic layer deposition. In situ X-ray diffraction and X-ray photoelectron spectroscopy studies of the crystallization of the amorphous films into the epitaxial (001BiFeO3 phase reveal distinct evolution profiles of crystallinity with temperature. While growth on (001SrTiO3 results in a coherently strained film, the same films obtained on (001LaAlO3 showed an unstrained, dislocation-rich interface, with an even lower temperature onset of the perovskite phase crystallization than in the case of (001SrTiO3. Our results demonstrate how the strain control in an epitaxial film can be accomplished via its crystallization from the amorphous state.

Multiple solid-phase microextraction

NARCIS (Netherlands)

Koster, EHM; de Jong, GJ

2000-01-01

Theoretical aspects of multiple solid-phase microextraction are described and the principle is illustrated with the extraction of lidocaine from aqueous solutions. With multiple extraction under non-equilibrium conditions considerably less time is required in order to obtain an extraction yield that

Chirality-Controlled Growth of Single-Wall Carbon Nanotubes Using Vapor Phase Epitaxy: Mechanistic Understanding and Scalable Production

Science.gov (United States)

2016-09-15

AFRL-AFOSR-VA-TR-2016-0319 Chirality -Controlled Growth of Single-Wall Carbon Nanotubes Using Vapor Phase Epitaxy: Mechanistic Understanding and...TELEPHONE NUMBER (Include area code) DISTRIBUTION A: Distribution approved for public release. 15-06-2016 final Jun 2014 - Jun 2016 Chirality ...for Public Release; Distribution is Unlimited. In this report, we present our efforts in establishing a novel and effective approach for chirality

Applications of Solid-Phase Microextraction and Gas Chromatography/Mass Spectrometry (SPME-GC/MS in the Study of Grape and Wine Volatile Compounds

Directory of Open Access Journals (Sweden)

Annarita Panighel

2014-12-01

Full Text Available Volatile compounds are responsible for the wine “bouquet”, which is perceived by sniffing the headspace of a glass, and of the aroma component (palate-aroma of the overall flavor, which is perceived on drinking. Grape aroma compounds are transferred to the wine and undergo minimal alteration during fermentation (e.g., monoterpenes and methoxypyrazines; others are precursors of aroma compounds which form in winemaking and during wine aging (e.g., glycosidically-bound volatile compounds and C13-norisoprenoids. Headspace solid phase microextraction (HS-SPME is a fast and simple technique which was developed for analysis of volatile compounds. This review describes some SPME methods coupled with gas chromatography/mass spectrometry (GC/MS used to study the grape and wine volatiles.

Trace-level determination of polar flavour compounds in butter by solid-phase extraction and gas chromatography-mass spectrometry.

NARCIS (Netherlands)

Adahchour, M.; Vreuls, J.J.; van der Heijden, A.; Brinkman, U.A.T.

1999-01-01

Volatile compounds are responsible for the aromas of butter. A simple technique for the determination of these components is described which is based on solid-phase extraction (SPE) after melting of the butter and separation of the aqueous phase from the fat. Volatile flavours present in the water

Aberration corrected STEM of defects in epitaxial n=4 Ruddlesden-Popper phase Can+1MnnO3n+1

International Nuclear Information System (INIS)

Wang, P; Bleloch, A L; Goodhew, P J; Yan, L; Niu, H J; Rosseinsky, M J; Chalker, P R

2008-01-01

Defects in Ruddlesden-Popper phase CaO·[(CaMnO 3 )] 4 epitaxial films grown on SrTiO 3 (001) by pulsed laser deposition have been investigated using high angle annular dark field imaging in an aberration-corrected STEM. The stacking faults perpendicular and parallel to the substrate formed during the growth are discussed in detail. The desired n = 4 RP phase is imaged and chemically analyzed at the atomic scale using electron energy loss spectroscopy.

Method for improved gas-solids separation

Science.gov (United States)

Kusik, C.L.; He, B.X.

1990-11-13

Methods are disclosed for the removal of particulate solids from a gas stream at high separation efficiency, including the removal of submicron size particles. The apparatus includes a cyclone separator type of device which contains an axially mounted perforated cylindrical hollow rotor. The rotor is rotated at high velocity in the same direction as the flow of an input particle-laden gas stream to thereby cause enhanced separation of particulate matter from the gas stream in the cylindrical annular space between the rotor and the sidewall of the cyclone vessel. Substantially particle-free gas passes through the perforated surface of the spinning rotor and into the hollow rotor, from where it is discharged out of the top of the apparatus. Separated particulates are removed from the bottom of the vessel. 4 figs.

Determination of selected UV filters in indoor dust by matrix solid-phase dispersion and gas chromatography-tandem mass spectrometry.

Science.gov (United States)

Negreira, N; Rodríguez, I; Rubí, E; Cela, R

2009-07-31

A simple, inexpensive sample preparation procedure, based on the matrix solid-phase dispersion (MSPD) technique, for the determination of six UV filters: 2-ethylhexyl salicylate (EHS), 3,3,5-trimethylcyclohexyl salicylate (Homosalate, HMS), 3-(4-methylbenzylidene) camphor (4-MBC), isoamyl-p-methoxycinnamate (IAMC), 2-ethylhexyl-p-methoxycinnamate (EHMC) and octocrylene (OCR), in dust from indoor environments is presented and the influence of several operational parameters on the extraction performance discussed. Under the final working conditions, sieved samples (0.5 g) were mixed with the same amount of anhydrous sodium sulphate and dispersed with 2 g of octadecyl bonded silica (C18) in a mortar with a pestle. This blend was transferred to a polypropylene solid-phase extraction cartridge containing 2 g of activated silica, as the clean-up co-sorbent. The cartridge was first rinsed with 5 mL of n-hexane and the analytes were then recovered with 4 mL of acetonitrile. This extract was adjusted to 1 mL, filtered and the compounds were determined by gas chromatography combined with tandem mass spectrometry (GC-MS/MS). Recoveries for samples spiked at two different concentrations ranged between 77% and 99%, and the limits of quantification (LOQs) of the method between 10 and 40 ng g(-1). Analysis of settled dust from different indoor areas, including private flats, public buildings and vehicle cabins, showed that EHMC and OCR were ubiquitous in this matrix, with maximum concentrations of 15 and 41 microg g(-1), respectively. Both UV filters were also quantified in dust reference material SRM 2585 for first time. EHS, 4-MBC and IAMC were detected in some of the analyzed samples, although at lower concentrations than EHMC and OCR.

Effect of solids, caloric content on dual-phase gastric emptying

Energy Technology Data Exchange (ETDEWEB)

Van Den Maegdenbergh, V.; Urbain, J.L.; Siegel, J.A.; Mortelmans, L.; De Roo, M. (Univ. Hospital Gasthuisberg, Leuven (Belgium) Temple Univ. Hospital, Philadelphia, PA (USA))

1990-03-01

The dual-phase gastric emptying technique is routinely employed to determine the differential emptying of solids and liquids in a wide spectrum of gastrointestinal diseases. Composition, acidity, volume, caloric density, physical form and viscosity of the test means have been shown to be important determinants for the quantitative evaluation of gastric emptying. In this study, the authors have evaluated the effect of increasing the caloric content of the solid portion of a physiologic test mean on both solid and liquid emptying kinetics in health male volunteers. They observed that increasing solid caloric content delayed emptying of both solids and liquids. For the solid phase, the delay was accounted for by a longer lag phase and decrease in emptying rate; for liquids a longer emptying rate was also obtained. They conclude that modification of the caloric content of the solid portion of a meal not only affects the emptying of the solid phase but also alters the emptying of the liquid component of the meal.

Simultaneous analysis of amphetamine-type stimulants in plasma by solid-phase microextraction and gas chromatography-mass spectrometry.

Science.gov (United States)

Mariotti, Kristiane de Cássia; Schuh, Roselena S; Ferranti, Priscila; Ortiz, Rafael S; Souza, Daniele Z; Pechansky, Flavio; Froehlich, Pedro E; Limberger, Renata P

2014-09-01

Brazil is considered one of the countries with the highest number of amphetamine-type stimulant (ATS) users worldwide, mainly diethylpropion (DIE) and fenproporex (FEN). The use of ATS is mostly linked to diverted prescription stimulants and this misuse is widely associated with (ab)use by drivers. A validated method was developed for the simultaneous analysis of amphetamine (AMP), DIE and FEN in plasma samples employing direct immersion-solid-phase microextraction, and gas chromatographic/mass spectrometric analysis. Trichloroacetic acid 10% was used for plasma deproteinization. In situ derivatization with propylchloroformate was employed. The linear range of the method covered from 5.0 to 100 ng/mL. The detection limits were 1.0 (AMP), 1.5 (DIE) and 2.0 ng/mL (FEN). The accuracy assessment of the control samples was within 85.58-108.33% of the target plasma concentrations. Recoveries ranged from 46.35 to 84.46% and precision was <15% of the value of relative standard deviation. This method is appropriate for screening and confirmation in plasma forensic toxicology analyses of these basic drugs. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Liquid Phase Epitaxial Growth of Al-doped f-SiC for White Light-Emitting Diodes

DEFF Research Database (Denmark)

Tang, Kai; Ma, Xiang; can der Eijk, Casper

efficiency, better light quality and longer lifespan, compared to the current yellow phosphor based white LEDs.Liquid phase epitaxy technology can yield a high crystalline quality in terms of structural perfection owing to the fact that it is a near equilibrium crystalline growth process. In addition....... The experimental results are presented and discussed. Since operational temperature of LPE growth is much lower than that currently used in physical vapour transport (PVT) process, it is expected to save the energy consumption for SiC crystal growth....

Development of Production PVD-AIN Buffer Layer System and Processes to Reduce Epitaxy Costs and Increase LED Efficiency

Energy Technology Data Exchange (ETDEWEB)

Cerio, Frank

2013-09-14

The DOE has set aggressive goals for solid state lighting (SSL) adoption, which require manufacturing and quality improvements for virtually all process steps leading to an LED luminaire product. The goals pertinent to this proposed project are to reduce the cost and improve the quality of the epitaxial growth processes used to build LED structures. The objectives outlined in this proposal focus on achieving cost reduction and performance improvements over state-of-the-art, using technologies that are low in cost and amenable to high efficiency manufacturing. The objectives of the outlined proposal focus on cost reductions in epitaxial growth by reducing epitaxy layer thickness and hetero-epitaxial strain, and by enabling the use of larger, less expensive silicon substrates and would be accomplished through the introduction of a high productivity reactive sputtering system and an effective sputtered aluminum-nitride (AlN) buffer/nucleation layer process. Success of the proposed project could enable efficient adoption of GaN on-silicon (GaN/Si) epitaxial technology on 150mm silicon substrates. The reduction in epitaxy cost per cm{sup 2} using 150mm GaN-on-Si technology derives from (1) a reduction in cost of ownership and increase in throughput for the buffer deposition process via the elimination of MOCVD buffer layers and other throughput and CoO enhancements, (2) improvement in brightness through reductions in defect density, (3) reduction in substrate cost through the replacement of sapphire with silicon, and (4) reduction in non-ESD yield loss through reductions in wafer bow and temperature variation. The adoption of 150mm GaN/Si processing will also facilitate significant cost reductions in subsequent wafer fabrication manufacturing costs. There were three phases to this project. These three phases overlap in order to aggressively facilitate a commercially available production GaN/Si capability. In Phase I of the project, the repeatability of the performance

Extração em fase sólida (SPE e micro extração em fase sólida (SPME de piretróides em água Solid-phase extraction (SPE and solid-phase microextraction of pyrethroids in water

Directory of Open Access Journals (Sweden)

Wilma Regina Barrionuevo

2001-04-01

Full Text Available The pyrethroids bifenthrin, permethrin, cypermethrin and deltamethrin were extracted by solid phase extraction (SPE and solid phase microextraction (SPME. The analysis were performed on a gas chromatograph with electron capture detection (GC-ECD. Octadecil Silano-C18, Florisil and Silica stationary phases were studied for SPE. Better results were obtained for Florisil which gave recoveries from 80% to 108%. Pyrethroids extraction by SPME showed a linear response and a detection limit of 10 pg ml-1. Although the data showed that the two extraction methods were able to isolate the pesticide residues from water samples, the best results were obtained by using SPME which is more sensitive, faster, cheeper, being a more useful technique for the analysis of pyrethroids in drinking water.

Molecular simulation of excess isotherm and excess enthalpy change in gas-phase adsorption.

Science.gov (United States)

Do, D D; Do, H D; Nicholson, D

2009-01-29

We present a new approach to calculating excess isotherm and differential enthalpy of adsorption on surfaces or in confined spaces by the Monte Carlo molecular simulation method. The approach is very general and, most importantly, is unambiguous in its application to any configuration of solid structure (crystalline, graphite layer or disordered porous glass), to any type of fluid (simple or complex molecule), and to any operating conditions (subcritical or supercritical). The behavior of the adsorbed phase is studied using the partial molar energy of the simulation box. However, to characterize adsorption for comparison with experimental data, the isotherm is best described by the excess amount, and the enthalpy of adsorption is defined as the change in the total enthalpy of the simulation box with the change in the excess amount, keeping the total number (gas + adsorbed phases) constant. The excess quantities (capacity and energy) require a choice of a reference gaseous phase, which is defined as the adsorptive gas phase occupying the accessible volume and having a density equal to the bulk gas density. The accessible volume is defined as the mean volume space accessible to the center of mass of the adsorbate under consideration. With this choice, the excess isotherm passes through a maximum but always remains positive. This is in stark contrast to the literature where helium void volume is used (which is always greater than the accessible volume) and the resulting excess can be negative. Our definition of enthalpy change is equivalent to the difference between the partial molar enthalpy of the gas phase and the partial molar enthalpy of the adsorbed phase. There is no need to assume ideal gas or negligible molar volume of the adsorbed phase as is traditionally done in the literature. We illustrate this new approach with adsorption of argon, nitrogen, and carbon dioxide under subcritical and supercritical conditions.

Phase stability in wear-induced supersaturated Al-Ti solid solution

Energy Technology Data Exchange (ETDEWEB)

Watanabe, Y.; Yokoyama, K. [Dept. of Functional Machinery Mechanics Shinshu Univ., Ueda (Japan); Hosoda, H. [Precision and Intelligence Lab., Tokyo Inst. of Tech., Nagatsuta, Midori-ku, Yokohama (Japan)

2002-07-01

Al-Ti supersaturated solid solutions were introduced by wear testing and the rapid quenching of an Al/Al{sub 3}Ti composite (part of an Al/Al{sub 3}Ti functionally graded material) that was fabricated using the centrifugal method. The phase stability of the supersaturated solid solution was studied through systematic annealing of the supersaturated solid solution. It was found that the Al-Ti supersaturated solid solution decomposed into Al and Al{sub 3}Ti intermetallic compound phases during the heat treatment. The Al-Ti supersaturated solid solutions fabricated were, therefore, not an equilibrium phase, and thus decomposed into the equilibrium phases during heat treatment. It was also found that heat treatment leads to a significant hardness increase for the Al-Ti supersaturated solid solution. Finally, it was concluded that formation of the wear-induced supersaturated solid solution layer was a result of severe plastic deformation. (orig.)

Possibility of the use of intermediate carbidsiliconoxide nanolayers on polydiamond substrates for gallium nitride layers epitaxy

Energy Technology Data Exchange (ETDEWEB)

Averichkin, P. A., E-mail: P-Yugov@mail.ru; Donskov, A. A. [State Research and Design Institute of Rare-Metal Industry Giredmet AO (Russian Federation); Dukhnovsky, M. P. [R & D Enterprise Istok (Russian Federation); Knyazev, S. N. [State Research and Design Institute of Rare-Metal Industry Giredmet AO (Russian Federation); Kozlova, Yu. P. [Russian Academy of Sciences, Institute for Nuclear Research (Russian Federation); Yugova, T. G.; Belogorokhov, I. A. [State Research and Design Institute of Rare-Metal Industry Giredmet AO (Russian Federation)

2016-04-15

The results of using carbidsiliconoxide (a-C:SiO1{sub .5}) films with a thickness of 30–60 nm, produced by the pyrolysis annealing of oligomethylsilseskvioksana (CH{sub 3}–SiO{sub 1.5}){sub n} with cyclolinear (staircased) molecular structure, as intermediate films in the hydride vapor phase epitaxy of gallium nitride on polycrystalline CVD-diamond substrates are presented. In the pyrolysis annealing of (CH{sub 3}–SiO{sub 1.5}){sub n} films in an atmosphere of nitrogen at a temperature of 1060°C, methyl radicals are carbonized to yield carbon atoms chemically bound to silicon. In turn, these atoms form a SiC monolayer on the surface of a-C:SiO{sub 1.5} films via covalent bonding with silicon. It is shown that GaN islands grow on such an intermediate layer on CVD-polydiamond substrates in the process of hydride vapor phase epitaxy in a vertical reactor from the GaCl–NH{sub 3}–N{sub 2} gas mixture.

Stochastic four-way coupling of gas-solid flows for Large Eddy Simulations

Science.gov (United States)

Curran, Thomas; Denner, Fabian; van Wachem, Berend

2017-11-01

The interaction of solid particles with turbulence has for long been a topic of interest for predicting the behavior of industrially relevant flows. For the turbulent fluid phase, Large Eddy Simulation (LES) methods are widely used for their low computational cost, leaving only the sub-grid scales (SGS) of turbulence to be modelled. Although LES has seen great success in predicting the behavior of turbulent single-phase flows, the development of LES for turbulent gas-solid flows is still in its infancy. This contribution aims at constructing a model to describe the four-way coupling of particles in an LES framework, by considering the role particles play in the transport of turbulent kinetic energy across the scales. Firstly, a stochastic model reconstructing the sub-grid velocities for the particle tracking is presented. Secondly, to solve particle-particle interaction, most models involve a deterministic treatment of the collisions. We finally introduce a stochastic model for estimating the collision probability. All results are validated against fully resolved DNS-DPS simulations. The final goal of this contribution is to propose a global stochastic method adapted to two-phase LES simulation where the number of particles considered can be significantly increased. Financial support from PetroBras is gratefully acknowledged.

The injection of inert gas ions into solids: their trapping and escape

International Nuclear Information System (INIS)

Carter, G.; Armour, D.G.; Donnelly, S.E.; Ingram, D.C.; Webb, R.P.

1980-01-01

Basic information is required to understand fission gas generation and its consequence for swelling and embrittlement in fission reactors, for understanding and controlling first wall problems in fusion reactors and for attempting to design storage for active gas waste. In all of these areas the rare gas atoms are generated with kinetic energy and may thus interact differently, during their slowing down, with the solid than if they had been introduced more gently (e.g. via diffusion) into the solid. An important method of simulating the behaviour of such energetic rare gas atoms in solids is via external irradiation of the solid with rare gas ions of appropriate species and energies and it is the purpose of this review to evaluate studies of this nature. The review is divided into three parts. The first describes experimental techniques, discusses the results of measurements of how ions penetrate into and may be retained in a solid, and outlines theoretical interpretations of the data. The mechanisms of gas atom dissolution and thermal transport in solids are of profound importance and so, in the second part of this review, attention is devoted to how the technique of post-implantation thermal evolution spectrometry can be employed to attempt to understand some of these processes. Particular attention is paid to the difficulties of unique interpretation of evolution spectra. In the final section, consideration will be given to the processes which lead to the inevitable saturation of solids undergoing continued irradiation with rare gas ions and experimental measurements and their probable interpretation will be discussed. Since many materials are of importance in the context of this symposium, reference will be made to as broad a range of studies as possible. (author)

The international symposium on 'chemical engineering of gas-liquid-solid catalyst reactions'

Energy Technology Data Exchange (ETDEWEB)

Hammer, H

1978-06-01

A report on the International Symposium on ''Chemical Engineering of Gas-Liquid-Solid Catalyst Reactions'', sponsored by the University of Liege (3/2-3/78), covers papers on the hydrodynamics, modeling and simulation, operating behavior, and chemical kinetics of trickle-bed reactors; scale-up of a trickle-bed reactor for hydrotreating Kuwait vacuum distillate; experimental results obtained in trickle-bed reactors for hydroprocessing atmospheric residua, hydrogenation of methylstyrene, hydrogenation of butanone, and hydrodemetallization of petroleum residua; advantages and disadvantages of various three-phase reactor types (e.g., for the liquid-phase hydrogenation of carbon monoxide to benzene, SNG, or methanol) and hydrodynamics, mass and heat transfer, and modeling of bubble columns with suspended catalysts (slurry reactors), and their applications (e.g., in SNG and fermentation processes).

Epitaxial Graphene: A New Material for Electronics

Science.gov (United States)

de Heer, Walt A.

2007-10-01

Graphene multilayers are grown epitaxially on single crystal silicon carbide. This system is composed of several graphene layers of which the first layer is electron doped due to the built-in electric field and the other layers are essentially undoped. Unlike graphite the charge carriers show Dirac particle properties (i.e. an anomalous Berry's phase, weak anti-localization and square root field dependence of the Landau level energies). Epitaxial graphene shows quasi-ballistic transport and long coherence lengths; properties that may persists above cryogenic temperatures. Paradoxically, in contrast to exfoliated graphene, the quantum Hall effect is not observed in high mobility epitaxial graphene. It appears that the effect is suppressed due to absence of localized states in the bulk of the material. Epitaxial graphene can be patterned using standard lithography methods and characterized using a wide array of techniques. These favorable features indicate that interconnected room temperature ballistic devices may be feasible for low dissipation high-speed nano-electronics.

Molecular-beam epitaxial growth of insulating AlN on surface-controlled 6H-SiC substrate by HCl gas etching

International Nuclear Information System (INIS)

Onojima, Norio; Suda, Jun; Matsunami, Hiroyuki

2002-01-01

Insulating AlN layers were grown on surface-controlled 6H-SiC subtrates by molecular-beam epitaxy (MBE) using elemental Al and rf plasma-excited nitrogen (N*). HCl gas etching was introduced as an effective pretreatment method of substrate for MBE growth of AlN. 6H-SiC substrates pretreated by HCl gas etching had no surface polishing scratches and an atomically flat surface. In addition, evident ( 3 √x 3 √)R30 deg. surface reconstruction was observed even before thermal cleaning. AlN layers grown on this substrate had no defects related to surface polishing scratches and excellent insulating characteristics

Innovative in-line separators: removal of water or sand in oil/water and gas/liquid/solid pipelines

Energy Technology Data Exchange (ETDEWEB)

Jepson, Paul; Cheolho Kang; Gopal, Madan [CC Technologies, Dublin, OH (United States)

2003-07-01

In oil and gas production, multiphase mixtures are often separated before downstream processing. The separators are large, often 20 - 40 feet long and large diameter and use sophisticated internals. The costs are in the millions of dollars. Further, the sand and water in the flow can cause severe internal erosion and corrosion respectively before the flow reaches the separators. The CC Technologies/MIST In line Separation System is a cost-effective, efficient device for use in multiphase environments. The device is applicable for gas/solid, gas/liquid/solid and oil/water systems and offers exceptional separation between phases for a fraction of the cost of expensive gravity separators and hydro cyclones. The System contains no moving parts and is designed to be of the same diameter as the pipe, and experiences low shear forces. It can be fabricated with standard pipes. The efficiency of the separator has been determined in an industrial scale, pilot plant test facility at CC Technologies in 4-inch diameter pipes and has been found to be in excess of 98-99% for the removal of sand. Two phase oil/water separation effectiveness is in excess of 90% in 1-stage and 95% in 2 - stage. (author)

Gas phase ion chemistry

CERN Document Server

Bowers, Michael T

1979-01-01

Gas Phase Ion Chemistry, Volume 1 covers papers on the advances of gas phase ion chemistry. The book discusses the advances in flow tubes and the measurement of ion-molecule rate coefficients and product distributions; the ion chemistry of the earth's atmosphere; and the classical ion-molecule collision theory. The text also describes statistical methods in reaction dynamics; the state selection by photoion-photoelectron coincidence; and the effects of temperature and pressure in the kinetics of ion-molecule reactions. The energy distribution in the unimolecular decomposition of ions, as well

Rapid determination of the volatile components in tobacco by ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction with gas chromatography-mass spectrometry.

Science.gov (United States)

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.

Deposition and characterisation of epitaxial oxide thin films for SOFCs

KAUST Repository

Santiso, José ; Burriel, Mó nica

2010-01-01

This paper reviews the recent advances in the use of thin films, mostly epitaxial, for fundamental studies of materials for solid oxide fuel cell (SOFC) applications. These studies include the influence of film microstructure, crystal orientation

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

Science.gov (United States)

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.

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

Energy Technology Data Exchange (ETDEWEB)

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

1997-06-24

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

A Model of Solid State Gas Sensors

Science.gov (United States)

Woestman, J. T.; Brailsford, A. D.; Shane, M.; Logothetis, E. M.

1997-03-01

Solid state gas sensors are widely used to measure the concentrations of gases such as CO, CH_4, C_3H_6, H_2, C_3H8 and O2 The applications of these sensors range from air-to-fuel ratio control in combustion processes including those in automotive engines and industrial furnaces to leakage detection of inflammable and toxic gases in domestic and industrial environments. As the need increases to accurately measure smaller and smaller concentrations, problems such as poor selectivity, stability and response time limit the use of these sensors. In an effort to overcome some of these limitations, a theoretical model of the transient behavior of solid state gas sensors has been developed. In this presentation, a model for the transient response of an electrochemical gas sensor to gas mixtures containing O2 and one reducing species, such as CO, is discussed. This model accounts for the transport of the reactive species to the sampling electrode, the catalyzed oxidation/reduction reaction of these species and the generation of the resulting electrical signal. The model will be shown to reproduce the results of published steady state models and to agree with experimental steady state and transient data.

Methanol synthesis in a countercurrent gas-solid-solid trickle flow reactor. An experimental study

NARCIS (Netherlands)

Kuczynski, M.; Oyevaar, M.H.; Pieters, R.T.; Westerterp, K.R.

1987-01-01

The synthesis of methanol from CO and H2 was executed in a gas-solid-solid trickle flow reactor. The reactor consisted of three tubular reactor sections with cooling sections in between. The catalyst was Cu on alumina, the adsorbent was a silica-alumina powder and the experimental range 498–523 K,

Detachment of CVD-grown graphene from single crystalline Ni films by a pure gas phase reaction

Science.gov (United States)

Zeller, Patrick; Henß, Ann-Kathrin; Weinl, Michael; Diehl, Leo; Keefer, Daniel; Lippmann, Judith; Schulz, Anne; Kraus, Jürgen; Schreck, Matthias; Wintterlin, Joost

2016-11-01

Despite great previous efforts there is still a high need for a simple, clean, and upscalable method for detaching epitaxial graphene from the metal support on which it was grown. We present a method based on a pure gas phase reaction that is free of solvents and polymer supports and avoids mechanical transfer steps. The graphene was grown on 150 nm thick, single crystalline Ni(111) films on Si(111) wafers with YSZ buffer layers. Its quality was monitored by using low energy electron diffraction and scanning tunneling microscopy. The gas phase etching uses a chemical transport reaction, the so-called Mond process, based on the formation of gaseous nickel tetracarbonyl in 1 bar of CO at 75 °C and by adding small amounts of sulfide catalysts. X-ray photoelectron spectroscopy, Raman spectroscopy and scanning electron microscopy were used to characterize the detached graphene. It was found that the method successfully removes the nickel from underneath the graphene layer, so that the graphene lies on the insulating oxide buffer layer. Small residual particles of nickel sulfide and cracks in the obtained graphene layer were identified. The defect concentrations were comparable to graphene samples obtained by wet chemical etching and by the bubbling transfer.

Low-temperature liquid-phase epitaxy and optical waveguiding of rare-earth-ion-doped KY(WO4)2 thin layers

NARCIS (Netherlands)

Romanyuk, Y.E.; Utke, I.; Ehrentraut, D.; Apostolopoulos, V.; Pollnau, Markus; Garcia-Revilla, S.; Valiente, B.

2004-01-01

Crystalline $KY(WO_{4})_{2}$ thin layers doped with different rare-earth ions were grown on b-oriented, undoped $KY(WO_{4})_{2}$ substrates by liquid-phase epitaxy employing a low-temperature flux. The ternary chloride mixture of NaCl, KCl, and CsCl with a melting point of 480°C was used as a

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

Science.gov (United States)

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

2007-11-15

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

Determination of parathion in biological fluids by means of direct Solid Phase Microextraction.

OpenAIRE

Gallardo, Eugenia; Barroso, Mário; Margalho, C.; Cruz, Angelines; Vieira, Duarte Nuno; López-Rivadulla, Manuel

2010-01-01

A new and simple procedure for the determination of parathion in human whole blood and urine using direct immersion (DI) solid-phase microextraction (SPME) and gas chromatography/mass spectrometry (GC/MS) is presented. This technique was developed using only 100 ìL of sample, and ethion was used as internal standard (IS). A 65-ìm Carbowax/divinylbenzene (CW/DVB) SPME fibre was selected for sampling, and the main parameters affecting the SPME process such as extraction ...

Application of novel activated carbon fiber solid-phase, microextraction to the analysis of chlorinated hydrocarbons in water by gas chromatography-mass spectrometry

International Nuclear Information System (INIS)

Sun Tonghua; Jia Jinping; Fang Nenghu; Wang Yalin

2005-01-01

This paper presents a study on the performance of activated carbon fiber (ACF) used as extraction fiber for solid-phase microextraction (SPME) and its application for analysis of chlorinated hydrocarbons in water. By means of evaluating scanning electron microscope (SEM) images, specific surface area, pore volume, pore distribution, and properties of adsorption and desorption, the optimal active concentration of phosphoric acid has been determined. Coupled with gas chromatograph-mass spectrometry (GC-MS), ACF-SPME is suitable for determination chlorinated hydrocarbons in water with headspace. Experimental parameters such as adsorption and desorption conditions were studied. The optimized method has an acceptable linearity, good precision, with R.S.D. values <10% for each compound. Compared with commercial fibers, ACF has many advantages such as better resistance to organic solvents, better endurance to high temperature and longer lifetime

Determination of steroids, caffeine and methylparaben in water using solid phase microextraction-comprehensive two dimensional gas chromatography-time of flight mass spectrometry.

Science.gov (United States)

Lima Gomes, Paulo C F; Barnes, Brian B; Santos-Neto, Álvaro J; Lancas, Fernando M; Snow, Nicholas H

2013-07-19

Analysis of several emerging contaminants (steroids, caffeine and methylparaben) in water using automated solid-phase microextraction with comprehensive two dimensional gas chromatography coupled to time of flight mass spectrometry (SPME-GCxGC-ToF/MS) is presented. Experimental design was used to determine the best SPME extraction conditions and the steroids were not derivatized prior to injection. SPME-GCxGC-ToF/MS provided linear ranges from 0.6 to 1200μgL(-1) and limits of detection and quantitation from 0.02 to 100μgL(-1). A series of river water samples obtained locally were subjected to analysis. SPME-GCxGC-ToF/MS is readily automated, straightforward and competitive with other methods for low level analysis of emerging contaminants. Copyright © 2013 Elsevier B.V. All rights reserved.

Phase coexistence in ferroelectric solid solutions: Formation of monoclinic phase with enhanced piezoelectricity

Directory of Open Access Journals (Sweden)

Xiaoyan Lu

2016-10-01

Full Text Available Phase morphology and corresponding piezoelectricity in ferroelectric solid solutions were studied by using a phenomenological theory with the consideration of phase coexistence. Results have shown that phases with similar energy potentials can coexist, thus induce interfacial stresses which lead to the formation of adaptive monoclinic phases. A new tetragonal-like monoclinic to rhombohedral-like monoclinic phase transition was predicted in a shear stress state. Enhanced piezoelectricity can be achieved by manipulating the stress state close to a critical stress field. Phase coexistence is universal in ferroelectric solid solutions and may provide a way to optimize ultra-fine structures and proper stress states to achieve ultrahigh piezoelectricity.

Epitaxial thin film growth of LiH using a liquid-Li atomic template

Energy Technology Data Exchange (ETDEWEB)

Oguchi, Hiroyuki, E-mail: oguchi@nanosys.mech.tohoku.ac.jp [Department of Nanomechanics, Tohoku University, Sendai 980-8579 (Japan); Micro System Integration Center (muSIC), Tohoku University, Sendai 980-0845 (Japan); Ikeshoji, Tamio; Orimo, Shin-ichi [Institute for Materials Research, Tohoku University, Sendai 980-8577 (Japan); Advanced Institute for Materials Research (AIMR), Tohoku University, Sendai 980-8577 (Japan); Ohsawa, Takeo; Shiraki, Susumu; Hitosugi, Taro [Advanced Institute for Materials Research (AIMR), Tohoku University, Sendai 980-8577 (Japan); Kuwano, Hiroki [Department of Nanomechanics, Tohoku University, Sendai 980-8579 (Japan)

2014-11-24

We report on the synthesis of lithium hydride (LiH) epitaxial thin films through the hydrogenation of a Li melt, forming abrupt LiH/MgO interface. Experimental and first-principles molecular dynamics studies reveal a comprehensive microscopic picture of the crystallization processes, which sheds light on the fundamental atomistic growth processes that have remained unknown in the vapor-liquid-solid method. We found that the periodic structure that formed, because of the liquid-Li atoms at the film/MgO-substrate interface, serves as an atomic template for the epitaxial growth of LiH crystals. In contrast, films grown on the Al{sub 2}O{sub 3} substrates indicated polycrystalline films with a LiAlO{sub 2} secondary phase. These results and the proposed growth process provide insights into the preparation of other alkaline metal hydride thin films on oxides. Further, our investigations open the way to explore fundamental physics and chemistry of metal hydrides including possible phenomena that emerge at the heterointerfaces of metal hydrides.

Using reweighting and free energy surface interpolation to predict solid-solid phase diagrams

Science.gov (United States)

Schieber, Natalie P.; Dybeck, Eric C.; Shirts, Michael R.

2018-04-01

Many physical properties of small organic molecules are dependent on the current crystal packing, or polymorph, of the material, including bioavailability of pharmaceuticals, optical properties of dyes, and charge transport properties of semiconductors. Predicting the most stable crystalline form at a given temperature and pressure requires determining the crystalline form with the lowest relative Gibbs free energy. Effective computational prediction of the most stable polymorph could save significant time and effort in the design of novel molecular crystalline solids or predict their behavior under new conditions. In this study, we introduce a new approach using multistate reweighting to address the problem of determining solid-solid phase diagrams and apply this approach to the phase diagram of solid benzene. For this approach, we perform sampling at a selection of temperature and pressure states in the region of interest. We use multistate reweighting methods to determine the reduced free energy differences between T and P states within a given polymorph and validate this phase diagram using several measures. The relative stability of the polymorphs at the sampled states can be successively interpolated from these points to create the phase diagram by combining these reduced free energy differences with a reference Gibbs free energy difference between polymorphs. The method also allows for straightforward estimation of uncertainties in the phase boundary. We also find that when properly implemented, multistate reweighting for phase diagram determination scales better with the size of the system than previously estimated.

Heterogeneous Ferroelectric Solid Solutions Phases and Domain States

CERN Document Server

Topolov, Vitaly

2012-01-01

The book deals with perovskite-type ferroelectric solid solutions for modern materials science and applications, solving problems of complicated heterophase/domain structures near the morphotropic phase boundary and applications to various systems with morphotropic phases. In this book domain state–interface diagrams are presented for the interpretation of heterophase states in perovskite-type ferroelectric solid solutions. It allows to describe the stress relief in the presence of polydomain phases, the behavior of unit-cell parameters of coexisting phases and the effect of external electric fields. The novelty of the book consists in (i) the first systematization of data about heterophase states and their evolution in ferroelectric solid solutions (ii) the general interpretation of heterophase and domain structures at changing temperature, composition or electric field (iii) the complete analysis of interconnection domain structures, unit-cell parameters changes, heterophase structures and stress relief.

Epitaxial growth of mixed conducting layered Ruddlesden–Popper Lan+1NinO3n+1 (n = 1, 2 and 3) phases by pulsed laser deposition

International Nuclear Information System (INIS)

Wu, Kuan-Ting; Soh, Yeong-Ah; Skinner, Stephen J.

2013-01-01

Graphical abstract: - Highlights: • High quality epitaxial thin films of layered Ruddlesden–Popper nickelates were prepared. • For the first time this has been achieved by the PLD process. • n = 1, 2 and 3 films were successfully deposited on SrTiO 3 and NdGaO 3 substrates. • c-Axis oriented films were confirmed by XRD analysis. • In-plane and out-of-plane strain effects on lattice are discussed. - Abstract: Layered Ruddlesden–Popper phases of composition La n+1 Ni n O 3n+1 (n = 1, 2 and 3) have been epitaxially grown on SrTiO 3 (0 0 1) or NdGaO 3 (1 1 0) single crystal substrates using the pulsed laser deposition technique. X-ray diffraction analyses (θ/2θ, rocking curves, and φ-scans) and atomic force microscopy confirms the high-quality growth of the series of films with low surface roughness values (less than 1 nm). In particular, epitaxial growth of the higher order phases (n = 2 and 3) of lanthanum nickelate have been demonstrated for the first time

Solid-phase microextraction for gas chromatographic/mass spectrometric analysis of dimethoate in human biological samples.

Science.gov (United States)

Gallardo, E; Barroso, M; Margalho, C; Cruz, A; Vieira, D N; López-Rivadulla, M

2006-01-01

A new, simple and rapid procedure for the determination of dimethoate in urine and blood samples was developed using direct immersion solid-phase microextraction and gas chromatography/mass spectrometry. This technique required only 0.1 mL of sample, and ethion was used as internal standard. Two types of coated fibre were compared (100 microm polydimethylsiloxane, and 65 microm Carbowax/divinylbenzene). Other parameters, such as extraction temperature, adsorption and desorption time, salt addition, agitation and pH, were optimized to enhance the sensitivity of the method. Limits of detection (LODs) and quantitation (LOQs) were 50 and 100 ng/mL for urine and 200 and 500 ng/mL for blood, respectively. The method was found to be linear between the LOQ and 40 microg/mL for urine, and between the LOQ and 50 microg/mL for blood, with correlation coefficients ranging from 0.9923-0.9996. Precision (intra- and interday) and accuracy were in conformity with the criteria normally accepted in bioanalytical method validation. The mean absolute recoveries of dimethoate were 1.24 and 0.50% for urine and blood, respectively. Because of its simplicity and the fact that small volumes of sample are used, the described method can be successfully used in the diagnosis of poisoning by this pesticide, namely in those situations where the sample volume is limited, as frequently occurs in forensic toxicology. Copyright 2006 John Wiley & Sons, Ltd.

Optical effects induced by epitaxial tension in lead titanate

Czech Academy of Sciences Publication Activity Database

Dejneka, Alexandr; Chvostová, Dagmar; Pacherová, Oliva; Kocourek, Tomáš; Jelínek, Miroslav; Tyunina, Marina

2018-01-01

Roč. 112, č. 3 (2018), s. 1-5, č. článku 031111. ISSN 0003-6951 R&D Projects: GA ČR GA15-13778S; GA ČR GA15-15123S Institutional support: RVO:68378271 Keywords : epitaxy * inorganic compounds * optical properties * ferroelectric materials * optical metrology Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics , supercond.) Impact factor: 3.411, year: 2016

Properties of ZrN films as substrate masks in liquid phase epitaxial lateral overgrowth of compound semiconductors

International Nuclear Information System (INIS)

Dobosz, D.; Zytkiewicz, Z.R.; Jakiela, R.; Golaszewska, K.; Kaminska, E.; Piotrowska, A.; Piotrowski, T.T.; Barcz, A.

2005-01-01

The usefulness of ZrN films as masks for epitaxial lateral overgrowth of GaAs and GaSb by liquid phase epitaxy is studied. It was observed that during the growth process ZrN masks are mechanically stable, they adhere strongly to the substrate and do not show any signs of degradation even at the growth temperature as high as 750 C. Moreover, perfect selectivity of GaAs and GaSb epitaxy was obtained on ZrN masked substrates ensuring the growth wide and thin layers. To study the influence of growth conditions on electrical resistivity of the mask, ZrN films deposited on GaAs substrates were annealed in various atmospheres. It was found that at temperatures higher than about 580 C the ZrN masks become highly resistive when heat-treated in hydrogen flow employed during growth. Usually, LPE growth temperature for GaAs is higher. Thus, ELO growth of GaAs by LPE becomes more difficult, though still possible, if ZrN masks are to be applied as buried electrical contacts. For GaSb ELO layers however, typical LPE growth temperature is about 480 C. This allows us to grow high quality GaSb ELO layers by LPE still preserving high electrical conductivity of ZrN mask. (copyright 2005 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Misfit strain-film thickness phase diagrams and related electromechanical properties of epitaxial ultra-thin lead zirconate titanate films

Energy Technology Data Exchange (ETDEWEB)

Qiu, Q.Y.; Mahjoub, R. [School of Materials Science and Engineering, University of New South Wales, Sydney, NSW 2052 (Australia); Alpay, S.P. [Materials Science and Engineering Program and Institute of Materials Science, University of Connecticut, Storrs, CT 06269 (United States); Nagarajan, V., E-mail: nagarajan@unsw.edu.au [School of Materials Science and Engineering, University of New South Wales, Sydney, NSW 2052 (Australia)

2010-02-15

The phase stability of ultra-thin (0 0 1) oriented ferroelectric PbZr{sub 1-x}Ti{sub x}O{sub 3} (PZT) epitaxial thin films as a function of the film composition, film thickness, and the misfit strain is analyzed using a non-linear Landau-Ginzburg-Devonshire thermodynamic model taking into account the electrical and mechanical boundary conditions. The theoretical formalism incorporates the role of the depolarization field as well as the possibility of the relaxation of in-plane strains via the formation of microstructural features such as misfit dislocations at the growth temperature and ferroelastic polydomain patterns below the paraelectric-ferroelectric phase transformation temperature. Film thickness-misfit strain phase diagrams are developed for PZT films with four different compositions (x = 1, 0.9, 0.8 and 0.7) as a function of the film thickness. The results show that the so-called rotational r-phase appears in a very narrow range of misfit strain and thickness of the film. Furthermore, the in-plane and out-of-plane dielectric permittivities {epsilon}{sub 11} and {epsilon}{sub 33}, as well as the out-of-plane piezoelectric coefficients d{sub 33} for the PZT thin films, are computed as a function of misfit strain, taking into account substrate-induced clamping. The model reveals that previously predicted ultrahigh piezoelectric coefficients due to misfit-strain-induced phase transitions are practically achievable only in an extremely narrow range of film thickness, composition and misfit strain parameter space. We also show that the dielectric and piezoelectric properties of epitaxial ferroelectric films can be tailored through strain engineering and microstructural optimization.

Classification of bacteria by simultaneous methylation-solid phase microextraction and gas chromatography/mass spectrometry analysis of fatty acid methyl esters.

Science.gov (United States)

Lu, Yao; Harrington, Peter B

2010-08-01

Direct methylation and solid-phase microextraction (SPME) were used as a sample preparation technique for classification of bacteria based on fatty acid methyl ester (FAME) profiles. Methanolic tetramethylammonium hydroxide was applied as a dual-function reagent to saponify and derivatize whole-cell bacterial fatty acids into FAMEs in one step, and SPME was used to extract the bacterial FAMEs from the headspace. Compared with traditional alkaline saponification and sample preparation using liquid-liquid extraction, the method presented in this work avoids using comparatively large amounts of inorganic and organic solvents and greatly decreases the sample preparation time as well. Characteristic gas chromatography/mass spectrometry (GC/MS) of FAME profiles was achieved for six bacterial species. The difference between Gram-positive and Gram-negative bacteria was clearly visualized with the application of principal component analysis of the GC/MS data of bacterial FAMEs. A cross-validation study using ten bootstrap Latin partitions and the fuzzy rule building expert system demonstrated 87 +/- 3% correct classification efficiency.

Comparative study on the roles of anisotropic epitaxial strain and chemical doping in inducing the antiferromagnetic insulator phase in manganite films

Science.gov (United States)

Jin, Feng; Feng, Qiyuan; Guo, Zhuang; Lan, Da; Wang, Lingfei; Gao, Guanyin; Xu, Haoran; Chen, Binbin; Chen, Feng; Lu, Qingyou; Wu, Wenbin

2017-11-01

Epitaxial strain and chemical doping are two different methods that are commonly used to tune the physical properties of epitaxial perovskite oxide films, but their cooperative effects are less addressed. Here we try to tune the phase separation (PS) in (La1-xP rx) 2 /3C a1 /3Mn O3 (0 ≤x ≤0.4 , LPCMO) films via cooperatively controlling the anisotropic epitaxial strain (AES) and the Pr doping. These films are grown simultaneously on NdGa O3(110 ) ,(LaAlO3) 0.3(SrAl0.5Ta0.5O3 ) 0.7(001 ) , and NdGa O3(001 ) substrates with progressively increased in-plane AES, and probed by x-ray diffraction, magnetotransport, and magnetic force microscopy (MFM) measurements. Although it is known that for x =0 the AES can enhance the orthorhombicity of the films yielding a phase diagram with the antiferromagnetic charge-ordered insulator (AF-COI) state induced, which is quite different from the bulk one, we illustrate that the Pr doping can further drive the films towards a more robust COI state. This cooperative effect is reflected by the increasing magnetic fields needed to melt the COI phase as a function of AES and the doping level. More strikingly, by directly imaging the phase competition morphology of the LPCMO /NdGa O3(001 ) films via MFM, we find that during COI melting the PS domain structure is subject to both AES and the quenched disorder. However, in the reverse process, as the magnetic field is decreased, the COI phase reappears and the AES dominates leaving a crystalline-orientation determined self-organized microstructure. This finding suggests that the PS states and the domain configurations can be selectively controlled by the AES and/or the quenched disorder, which may shed some light on the engineering of PS domains for device fabrications.

Thermodynamic Modeling of Natural Gas Systems Containing Water

DEFF Research Database (Denmark)

Karakatsani, Eirini K.; Kontogeorgis, Georgios M.

2013-01-01

As the need for dew point specifications remains very urgent in the natural gas industry, the development of accurate thermodynamic models, which will match experimental data and will allow reliable extrapolations, is needed. Accurate predictions of the gas phase water content in equilibrium...... with a heavy phase were previously obtained using cubic plus association (CPA) coupled with a solid phase model in the case of hydrates, for the binary systems of water–methane and water–nitrogen and a few natural gas mixtures. In this work, CPA is being validated against new experimental data, both water...... content and phase equilibrium data, and solid model parameters are being estimated for four natural gas main components (methane, ethane, propane, and carbon dioxide). Different tests for the solid model parameters are reported, including vapor-hydrate-equilibria (VHE) and liquid-hydrate-equilibria (LHE...

Methanol ice co-desorption as a mechanism to explain cold methanol in the gas-phase

Science.gov (United States)

Ligterink, N. F. W.; Walsh, C.; Bhuin, R. G.; Vissapragada, S.; van Scheltinga, J. Terwisscha; Linnartz, H.

2018-05-01

Context. Methanol is formed via surface reactions on icy dust grains. Methanol is also detected in the gas-phase at temperatures below its thermal desorption temperature and at levels higher than can be explained by pure gas-phase chemistry. The process that controls the transition from solid state to gas-phase methanol in cold environments is not understood. Aims: The goal of this work is to investigate whether thermal CO desorption provides an indirect pathway for methanol to co-desorb at low temperatures. Methods: Mixed CH3OH:CO/CH4 ices were heated under ultra-high vacuum conditions and ice contents are traced using RAIRS (reflection absorption IR spectroscopy), while desorbing species were detected mass spectrometrically. An updated gas-grain chemical network was used to test the impact of the results of these experiments. The physical model used is applicable for TW Hya, a protoplanetary disk in which cold gas-phase methanol has recently been detected. Results: Methanol release together with thermal CO desorption is found to be an ineffective process in the experiments, resulting in an upper limit of ≤ 7.3 × 10-7 CH3OH molecules per CO molecule over all ice mixtures considered. Chemical modelling based on the upper limits shows that co-desorption rates as low as 10-6 CH3OH molecules per CO molecule are high enough to release substantial amounts of methanol to the gas-phase at and around the location of the CO thermal desorption front in a protoplanetary disk. The impact of thermal co-desorption of CH3OH with CO as a grain-gas bridge mechanism is compared with that of UV induced photodesorption and chemisorption.

Multivariate analysis of the volatile components in tobacco based on infrared-assisted extraction coupled to headspace solid-phase microextraction and gas chromatography-mass spectrometry.

Science.gov (United States)

Yang, Yanqin; Pan, Yuanjiang; Zhou, Guojun; Chu, Guohai; Jiang, Jian; Yuan, Kailong; Xia, Qian; Cheng, Changhe

2016-11-01

A novel infrared-assisted extraction coupled to headspace solid-phase microextraction followed by gas chromatography with mass spectrometry method has been developed for the rapid determination of the volatile components in tobacco. The optimal extraction conditions for maximizing the extraction efficiency were as follows: 65 μm polydimethylsiloxane-divinylbenzene fiber, extraction time of 20 min, infrared power of 175 W, and distance between the infrared lamp and the headspace vial of 2 cm. Under the optimum conditions, 50 components were found to exist in all ten tobacco samples from different geographical origins. Compared with conventional water-bath heating and nonheating extraction methods, the extraction efficiency of infrared-assisted extraction was greatly improved. Furthermore, multivariate analysis including principal component analysis, hierarchical cluster analysis, and similarity analysis were performed to evaluate the chemical information of these samples and divided them into three classifications, including rich, moderate, and fresh flavors. The above-mentioned classification results were consistent with the sensory evaluation, which was pivotal and meaningful for tobacco discrimination. As a simple, fast, cost-effective, and highly efficient method, the infrared-assisted extraction coupled to headspace solid-phase microextraction technique is powerful and promising for distinguishing the geographical origins of the tobacco samples coupled to suitable chemometrics. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Determination of 3-monochloropropane-1,2-diol in grease food by solid phase extraction-derivatization-gas chromatography-mass spectrometry].

Science.gov (United States)

Xiang, Xiaoling; Wang, Liyuan; Shen, Xianghong; Li, Chunsong; Shen, Jianfu; Wu, Pinggu

2017-09-01

To establish the method of determination of 3-monochloropropane-1,2-diol( 3-MCPD) in grease food by gas chromatography-mass spectrometry( GC-MS). 3-MCPD in grease food represented by bean paste was extracted by ultrasound,purified by alkaline earth solid phase extraction column,derivatived using phenylboronic acid( PBA) and detected by GC-MS. The linearity of 3-MCPD ranged from 1-100 ng/mL,with correlation coefficient at 0. 9993.The limits of quantitation( LOQ) in soy sauce,bean paste,pepper oil were 0. 6,0. 5 and7. 0 μg/kg and limits of detection( LOD) were 1. 9,1. 6 and 18. 8 μg/kg,respectively.Average recovery rate and relative standard deviation was 78. 3%-106. 7% and 1. 9%-11. 6%( n = 6), when 3-MCPD was added in grease food at 2. 5-1000 μg/kg. The method has good purification effect and the detection sensitivity and accuracy,and can be used for the determination of 3-MCPD in grease food.

For progress in natural science: Materials international investigations of structural phase transformation and THz properties across metal–insulator transition in VO2/Al2O3 epitaxial films

Directory of Open Access Journals (Sweden)

Mengmeng Yang

2015-10-01

Full Text Available Vanadium dioxide (VO2 epitaxial thin films on (0001-oriented Al2O3 substrates were prepared using radio frequency (RF magnetron sputtering techniques. To study the metal-insulator-transition (MIT mechanism and extend the applications of VO2 epitaxial films at terahertz (THz band, temperature-dependent X-ray diffraction (XRD and THz time domain spectroscopy of the VO2 epitaxial films were performed. Both the lattice constants and THz transmission exhibited a similar and sharp transition that was similar to that observed for the electrical resistance. Consequently, the MIT of the VO2/Al2O3 epitaxial films should be co-triggered by the structural phase transition and electronic transition. Moreover, the very large resistance change (on the order of ~103 and THz response (with a transmission modulation ratio of ~87% in the VO2/Al2O3 epitaxial heterostructures are promising for electrical switch and electro-optical device applications.

The Gaseous Phase as a Probe of the Astrophysical Solid Phase Chemistry

Energy Technology Data Exchange (ETDEWEB)

Abou Mrad, Ninette; Duvernay, Fabrice; Isnard, Robin; Chiavassa, Thierry; Danger, Grégoire, E-mail: gregoire.danger@univ-amu.fr [Aix-Marseille Université, PIIM UMR-CNRS 7345, F-13397 Marseille (France)

2017-09-10

In support of space missions and spectroscopic observations, laboratory experiments on ice analogs enable a better understanding of organic matter formation and evolution in astrophysical environments. Herein, we report the monitoring of the gaseous phase of processed astrophysical ice analogs to determine if the gaseous phase can elucidate the chemical mechanisms and dominant reaction pathways occurring in the solid ice subjected to vacuum ultra-violet (VUV) irradiation at low temperature and subsequently warmed. Simple (CH{sub 3}OH), binary (H{sub 2}O:CH{sub 3}OH, CH{sub 3}OH:NH{sub 3}), and ternary ice analogs (H{sub 2}O:CH{sub 3}OH:NH{sub 3}) were VUV-processed and warmed. The evolution of volatile organic compounds in the gaseous phase shows a direct link between their relative abundances in the gaseous phase, and the radical and thermal chemistries modifying the initial ice composition. The correlation between the gaseous and solid phases may play a crucial role in deciphering the organic composition of astrophysical objects. As an example, possible solid compositions of the comet Lovejoy are suggested using the abundances of organics in its comae.

Cork as a new (green) coating for solid-phase microextraction: Determination of polycyclic aromatic hydrocarbons in water samples by gas chromatography–mass spectrometry

International Nuclear Information System (INIS)

Dias, Adriana Neves; Simão, Vanessa; Merib, Josias; Carasek, Eduardo

2013-01-01

Highlights: ► Cork as a new coating for solid-phase microextraction was proposed. ► Good results were achieved, demonstrating the applicability of the cork as coating for SPME. ► The efficiency of cork fiber was very similar to commercially available fibers. -- Abstract: A new fiber for solid-phase microextraction (SPME) was prepared employing cork as a coating. The morphology and composition of the cork fiber was evaluated by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR), respectively. The proposed fiber was used for the determination of polycyclic aromatic hydrocarbons (PAHs) in river water samples by gas chromatography–selected ion monitoring–mass spectrometry (GC–SIM–MS). A central composite design was used for optimization of the variables involved in the extraction of PAHs from water samples. The optimal extraction conditions were extraction time and temperature of 60 min and 80 °C, respectively. The detection and quantification limits were 0.03 and 0.1 μg L −1 , respectively. The recovery values were between 70.2 and 103.2% and the RSD was ≤15.7 (n = 3). The linear range was 0.1–10 μg L −1 with r ≥ 0.96 and the fiber-to-fiber reproducibility showed RSD ≤ 18.6% (n = 5). The efficiency of the cork fiber was compared with commercially available fibers and good results were achieved, demonstrating the applicability and great potential of cork as a coating for SPME

Photovoltaic X-ray detectors based on epitaxial GaAs structures

Energy Technology Data Exchange (ETDEWEB)

Achmadullin, R.A. [Institute of Radio Engineering and Electronics, Russian Academy of Sciences, 1 Ac. Vvedenski square, Fryazino 141190, Moscow region (Russian Federation); Artemov, V.V. [Shubnikov Institute of Crystallography, Russian Academy of Sciences, 59 Leninski pr., Moscow B-333, 117333 (Russian Federation); Dvoryankin, V.F. [Institute of Radio Engineering and Electronics, Russian Academy of Sciences, 1 Ac. Vvedenski square, Fryazino 141190, Moscow region (Russian Federation)]. E-mail: vfd217@ire216.msk.su; Dvoryankina, G.G. [Institute of Radio Engineering and Electronics, Russian Academy of Sciences, 1 Ac. Vvedenski square, Fryazino 141190, Moscow region (Russian Federation); Dikaev, Yu.M. [Institute of Radio Engineering and Electronics, Russian Academy of Sciences, 1 Ac. Vvedenski square, Fryazino 141190, Moscow region (Russian Federation); Ermakov, M.G. [Institute of Radio Engineering and Electronics, Russian Academy of Sciences, 1 Ac. Vvedenski square, Fryazino 141190, Moscow region (Russian Federation); Ermakova, O.N. [Institute of Radio Engineering and Electronics, Russian Academy of Sciences, 1 Ac. Vvedenski square, Fryazino 141190, Moscow region (Russian Federation); Chmil, V.B. [Scientific State Center, High Energy Physics Institute, Protvino, Moscow region (Russian Federation); Holodenko, A.G. [Scientific State Center, High Energy Physics Institute, Protvino, Moscow region (Russian Federation); Kudryashov, A.A.; Krikunov, A.I.; Petrov, A.G.; Telegin, A.A. [Institute of Radio Engineering and Electronics, Russian Academy of Sciences, 1 Ac. Vvedenski square, Fryazino 141190, Moscow region (Russian Federation); Vorobiev, A.P. [Scientific State Center, High Energy Physics Institute, Protvino, Moscow region (Russian Federation)

2005-12-01

A new type of the photovoltaic X-ray detector based on epitaxial p{sup +}-n-n'-n{sup +} GaAs structures which provides a high efficiency of charge collection in the non-bias operation mode at room temperature is proposed. The GaAs epitaxial structures were grown by vapor-phase epitaxy on heavily doped n{sup +}-GaAs(1 0 0) substrates. The absorption efficiency of GaAs X-ray detector is discussed. I-V and C-V characteristics of the photovoltaic X-ray detectors are analyzed. The built-in electric field profiles in the depletion region of epitaxial structures are measured by the EBIC method. Charge collection efficiency to {alpha}-particles and {gamma}-radiation are measured. The application of X-ray detectors is discussed.

Characterization of the volatile profiles of beer using headspace solid-phase microextraction and gas chromatography-mass spectrometry.

Science.gov (United States)

Rossi, Serena; Sileoni, Valeria; Perretti, Giuseppe; Marconi, Ombretta

2014-03-30

The objective of this study was a multivariate characterization of the volatile profile of beers. Such a characterization is timely considering the increasing worldwide consumption of beer, the continuous growth of microbreweries and the importance of volatile compounds to beer flavour. A method employing solid-phase microextraction and gas chromatography-mass spectrometry (SPME-GC-MS) was optimized and then applied to a sample set of 36 industrial and craft beers of various styles and fermentation types. The volatile profiles of different beer styles is described, with particular attention paid to the volatile compounds characteristic of a spontaneously fermented lambic raspberry framboise beer. Furthermore, it was also possible to identify which specific volatile compounds are principally responsible for the differences in the volatile profiles of top- and bottom-fermented beers. Moreover, a volatile fingerprint of the craft top-fermented Italian beers was defined, as they show a very similar volatile profile. Finally, the volatile compounds that are characteristic of the bock-style beers are described. The SPME-GC-MS analytical method optimized in this study is suitable for characterizing the volatile fingerprint of different beers, especially on the basis of the kind of fermentation (top, bottom or spontaneous), the method of production and the style of the beer. © 2013 Society of Chemical Industry.

Graphene oxide bonded fused-silica fiber for solid-phase microextraction-gas chromatography of polycyclic aromatic hydrocarbons in water.

Science.gov (United States)

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

2012-01-01

A novel chemically bonded graphene oxide/fused-silica fiber was prepared and applied in solid-phase microextraction of six polycyclic aromatic hydrocarbons from water samples coupled with gas chromatography. It exhibited high extraction efficiency and excellent stability. Effects of extraction time, extraction temperature, ionic strength, stirring rate and desorption conditions were investigated and optimized in our work. Detection limits to the six polycyclic aromatic hydrocarbons were less than 0.08 μg/L, and their calibration curves were all linear (R(2)≥0.9954) in the range from 0.05 to 200 μg/L. Single fiber repeatability and fiber-to-fiber reproducibility were less than 6.13 and 15.87%, respectively. This novel fiber was then utilized to analyze two real water samples from the Yellow River and local waterworks, and the recoveries of samples spiked at 1 and 10 μg/L ranged from 84.48 to 118.24%. Compared with other coating materials, this graphene oxide-coated fiber showed many advantages: wide linear range, low detection limit, and good stability in acid, alkali, organic solutions and at high temperature. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Rapid Determination of Clenbuterol in Pork by Direct Immersion Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry.

Science.gov (United States)

Ye, Diru; Wu, Susu; Xu, Jianqiao; Jiang, Ruifen; Zhu, Fang; Ouyang, Gangfeng

2016-02-01

Direct immersion solid-phase microextraction (DI-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was developed for rapid analysis of clenbuterol in pork for the first time. In this work, a low-cost homemade 44 µm polydimethylsiloxane (PDMS) SPME fiber was employed to extract clenbuterol in pork. After extraction, derivatization was performed by suspending the fiber in the headspace of the 2 mL sample vial saturated with a vapor of 100 µL hexamethyldisilazane. Lastly, the fiber was directly introduced to GC-MS for analysis. All parameters that influenced absorption (extraction time), derivatization (derivatization reagent, time and temperature) and desorption (desorption time) were optimized. Under optimized conditions, the method offered a wide linear range (10-1000 ng g(-1)) and a low detection limit (3.6 ng g(-1)). Finally, the method was successfully applied in the analysis of pork from the market, and recoveries of the method for spiked pork were 97.4-105.7%. Compared with the traditional solvent extraction method, the proposed method was much cheaper and fast. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Multivariate study of parameters in the determination of pesticide residues in apple by headspace solid phase microextraction coupled to gas chromatography-mass spectrometry using experimental factorial design.

Science.gov (United States)

Abdulra'uf, Lukman Bola; Tan, Guan Huat

2013-12-15

Solid-phase microextraction (SPME) is a solvent-less sample preparation method which combines sample preparation, isolation, concentration and enrichment into one step. In this study, multivariate strategy was used to determine the significance of the factors affecting the solid phase microextraction of pesticide residues (fenobucarb, diazinon, chlorothalonil and chlorpyrifos) using a randomised factorial design. The interactions and effects of temperature, time and salt addition on the efficiency of the extraction of the pesticide residues were evaluated using 2(3) factorial designs. The analytes were extracted with 100 μm PDMS fibres according to the factorial design matrix and desorbed into a gas chromatography-mass spectrometry detector. The developed method was applied for the analysis of apple samples and the limits of detection were between 0.01 and 0.2 μg kg(-)(1), which were lower than the MRLs for apples. The relative standard deviations (RSD) were between 0.1% and 13.37% with average recovery of 80-105%. The linearity ranges from 0.5-50 μg kg(-)(1) with correlation coefficient greater than 0.99. Copyright © 2013 Elsevier Ltd. All rights reserved.

Contribution to the modelling of gas-solid reactions and reactors

International Nuclear Information System (INIS)

Patisson, F.

2005-09-01

Gas-solid reactions control a great number of major industrial processes involving matter transformation. This dissertation aims at showing that mathematical modelling is a useful tool for both understanding phenomena and optimising processes. First, the physical processes associated with a gas-solid reaction are presented in detail for a single particle, together with the corresponding available kinetic grain models. A second part is devoted to the modelling of multiparticle reactors. Different approaches, notably for coupling grain models and reactor models, are illustrated through various case studies: coal pyrolysis in a rotary kiln, production of uranium tetrafluoride in a moving bed furnace, on-grate incineration of municipal solid wastes, thermogravimetric apparatus, nuclear fuel making, steel-making electric arc furnace. (author)

Epitaxial Integration of Nanowires in Microsystems by Local Micrometer Scale Vapor Phase Epitaxy

DEFF Research Database (Denmark)

Mølhave, Kristian; Wacaser, Brent A.; Petersen, Dirch Hjorth

2008-01-01

deposition (CVD) or metal organic VPE (MOVPE). However, VPE of semiconducting nanowires is not compatible with several microfabrication processes due to the high synthesis temperatures and issues such as cross-contamination interfering with the intended microsystem or the VPE process. By selectively heating...... a small microfabricated heater, growth of nanowires can be achieved locally without heating the entire microsystem, thereby reducing the compatibility problems. The first demonstration of epitaxial growth of silicon nanowires by this method is presented and shows that the microsystem can be used for rapid...

Comparative solution and solid-phase glycosylations toward a disaccharide library

DEFF Research Database (Denmark)

Agoston, K.; Kröger, Lars; Agoston, Agnes

2009-01-01

A comparative study on solution-phase and solid-phase oligosaccharide synthesis was performed. A 16-member library containing all regioisomers of Glc-Glc, Glc-Gal, Gal-Glc, and Gal-Gal disaccharides was synthesized both in solution and on solid phase. The various reaction conditions for different...

Role of nanoparticles in analytical solid phase microextraction (SPME)

NARCIS (Netherlands)

Zielinska, K.; Leeuwen, van H.P.

2013-01-01

Solid phase microextraction (SPME) is commonly used to measure the free concentration of fairly hydrophobic substances in aqueous media on the basis of their partitioning between sample solution and a solid phase. Here we study the role of nanoparticles that may sorb the analyte in the sample

Harsh-Environment Solid-State Gamma Detector for Down-hole Gas and Oil Exploration

International Nuclear Information System (INIS)

Peter Sandvik; Stanislav Soloviev; Emad Andarawis; Ho-Young Cha; Jim Rose; Kevin Durocher; Robert Lyons; Bob Pieciuk; Jim Williams; David O'Connor

2007-01-01

The goal of this program was to develop a revolutionary solid-state gamma-ray detector suitable for use in down-hole gas and oil exploration. This advanced detector would employ wide-bandgap semiconductor technology to extend the gamma sensor's temperature capability up to 200 C as well as extended reliability, which significantly exceeds current designs based on photomultiplier tubes. In Phase II, project tasks were focused on optimization of the final APD design, growing and characterizing the full scintillator crystals of the selected composition, arranging the APD device packaging, developing the needed optical coupling between scintillator and APD, and characterizing the combined elements as a full detector system preparing for commercialization. What follows is a summary report from the second 18-month phase of this program

Lattice-Symmetry-Driven Epitaxy of Hierarchical GaN Nanotripods

KAUST Repository

Wang, Ping

2017-01-18

Lattice-symmetry-driven epitaxy of hierarchical GaN nanotripods is demonstrated. The nanotripods emerge on the top of hexagonal GaN nanowires, which are selectively grown on pillar-patterned GaN templates using molecular beam epitaxy. High-resolution transmission electron microscopy confirms that two kinds of lattice-symmetry, wurtzite (wz) and zinc-blende (zb), coexist in the GaN nanotripods. Periodical transformation between wz and zb drives the epitaxy of the hierarchical nanotripods with N-polarity. The zb-GaN is formed by the poor diffusion of adatoms, and it can be suppressed by improving the ability of the Ga adatoms to migrate as the growth temperature increased. This controllable epitaxy of hierarchical GaN nanotripods allows quantum dots to be located at the phase junctions of the nanotripods and nanowires, suggesting a new recipe for multichannel quantum devices.

Materials research for passive solar systems: Solid-state phase-change materials

Science.gov (United States)

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.

The liquid phase epitaxy method for the construction of oriented ZIF-8 thin films with controlled growth on functionalized surfaces

KAUST Repository

Shekhah, Osama; Eddaoudi, Mohamed

2013-01-01

Highly-oriented ZIF-8 thin films with controllable thickness were grown on an -OH-functionalized Au substrate using the liquid phase epitaxy method at room temperature, as evidenced by SEM and PXRD. The adsorption-desorption properties of the resulting ZIF-8 thin film were investigated for various VOCs using the QCM technique. © The Royal Society of Chemistry 2013.

Solid-phase reductive amination for glycomic analysis.

Science.gov (United States)

Jiang, Kuan; Zhu, He; Xiao, Cong; Liu, Ding; Edmunds, Garrett; Wen, Liuqing; Ma, Cheng; Li, Jing; Wang, Peng George

2017-04-15

Reductive amination is an indispensable method for glycomic analysis, as it tremendously facilitates glycan characterization and quantification by coupling functional tags at the reducing ends of glycans. However, traditional in-solution derivatization based approach for the preparation of reductively aminated glycans is quite tedious and time-consuming. Here, a simpler and more efficient strategy termed solid-phase reductive amination was investigated. The general concept underlying this new approach is to streamline glycan extraction, derivatization, and purification on non-porous graphitized carbon sorbents. Neutral and sialylated standard glycans were utilized to test the feasibility of the solid-phase method. As results, almost complete labeling of those glycans with four common labels of aniline, 2-aminobenzamide (2-AB), 2-aminobenzoic acid (2-AA) and 2-amino-N-(2-aminoethyl)-benzamide (AEAB) was obtained, and negligible desialylation occurred during sample preparation. The labeled glycans derived from glycoproteins showed excellent reproducibility in high performance liquid chromatography (HPLC) and matrix assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) analysis. Direct comparisons based on fluorescent absorbance and relative quantification using isotopic labeling demonstrated that the solid-phase strategy enabled 20-30% increase in sample recovery. In short, the solid-phase strategy is simple, reproducible, efficient, and sensitive for glycan analysis. This method was also successfully applied for N-glycan profiling of HEK 293 cells with MALDI-TOF MS, showing its attractive application in the high-throughput analysis of mammalian glycome. Published by Elsevier B.V.

Concurrent bandgap narrowing and polarization enhancement in epitaxial ferroelectric nanofilms

Czech Academy of Sciences Publication Activity Database

Tyunina, Marina; Yao, L.; Chvostová, Dagmar; Dejneka, Alexandr; Kocourek, Tomáš; Jelínek, Miroslav; Trepakov, Vladimír; van Dijken, S.

2015-01-01

Roč. 16, č. 2 (2015), 026002 ISSN 1468-6996 R&D Projects: GA ČR GAP108/12/1941 Institutional support: RVO:68378271 Keywords : epitaxial growth * ferroelectric nanofilms Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 3.433, year: 2015

Suppression of metastable-phase inclusion in N-polar (0001¯) InGaN/GaN multiple quantum wells grown by metalorganic vapor phase epitaxy

International Nuclear Information System (INIS)

Shojiki, Kanako; Iwabuchi, Takuya; Kuboya, Shigeyuki; Choi, Jung-Hun; Tanikawa, Tomoyuki; Hanada, Takashi; Katayama, Ryuji; Matsuoka, Takashi; Usami, Noritaka

2015-01-01

The metastable zincblende (ZB) phase in N-polar (0001 ¯ ) (−c-plane) InGaN/GaN multiple quantum wells (MQWs) grown by metalorganic vapor phase epitaxy is elucidated by the electron backscatter diffraction measurements. From the comparison between the −c-plane and Ga-polar (0001) (+c-plane), the −c-plane MQWs were found to be suffered from the severe ZB-phase inclusion, while ZB-inclusion is negligible in the +c-plane MQWs grown under the same growth conditions. The ZB-phase inclusion is a hurdle for fabricating the −c-plane light-emitting diodes because the islands with a triangular shape appeared on a surface in the ZB-phase domains. To improve the purity of stable wurtzite (WZ)-phase, the optimum conditions were investigated. The ZB-phase is dramatically eliminated with decreasing the V/III ratio and increasing the growth temperature. To obtain much-higher-quality MQWs, the thinner InGaN wells and the hydrogen introduction during GaN barriers growth were tried. Consequently, MQWs with almost pure WZ phase and with atomically smooth surface have been demonstrated

A multi-residue method for the analysis of pesticides and pesticide degradates in water using HLB solid-phase extraction and gas chromatography-ion trap mass spectrometry

Science.gov (United States)

Hladik, M.L.; Smalling, K.L.; Kuivila, K.M.

2008-01-01

A method was developed for the analysis of over 60 pesticides and degradates in water by HLB solid-phase extraction and gas-chromatography/mass spectrometry. Method recoveries and detection limits were determined using two surface waters with different dissolved organic carbon (DOC) concentrations. In the lower DOC water, recoveries and detection limits were 80%-108% and 1-12 ng/L, respectively. In the higher DOC water, the detection limits were slightly higher (1-15 ng/L). Additionally, surface water samples from four sites were analyzed and 14 pesticides were detected with concentrations ranging from 4 to 1,200 ng/L. ?? 2008 Springer Science+Business Media, LLC.

Study on confirmation of Solid-Meal Lag Phase of Gastric Emptying

International Nuclear Information System (INIS)

Lee, Ji Young; Lee, Kyoung Soo; Kim, Chang Guhn; Juhng, Seon Kwan; Won, Jong Jin; Nah, Yong Ho

1991-01-01

The purpose of this study was to examine the existence of a lag phase of gastric emptying of solid meals. We studied solid phase gastric emptying in 26 normal subject using continuous data acquisition for 30 minutes. Each ingested a 300 g meal containing 99m Tc-labeled scrambled egg (solid 150 g, milk 150 ml). Lag phase was determined by 1) inspection of the gastric emptying curve 2) time to a 2% decrease in stomach activity 3) the time of visual appearance of duodenal activity on computer image. We concluded that solid meal lag phase exist.

Study on confirmation of Solid-Meal Lag Phase of Gastric Emptying

Energy Technology Data Exchange (ETDEWEB)

Lee, Ji Young; Lee, Kyoung Soo; Kim, Chang Guhn; Juhng, Seon Kwan; Won, Jong Jin; Nah, Yong Ho [Wonkwang University School of Medicine, Iksan (Korea, Republic of)

1991-07-15

The purpose of this study was to examine the existence of a lag phase of gastric emptying of solid meals. We studied solid phase gastric emptying in 26 normal subject using continuous data acquisition for 30 minutes. Each ingested a 300 g meal containing {sup 99m}Tc-labeled scrambled egg (solid 150 g, milk 150 ml). Lag phase was determined by 1) inspection of the gastric emptying curve 2) time to a 2% decrease in stomach activity 3) the time of visual appearance of duodenal activity on computer image. We concluded that solid meal lag phase exist.

Studies of matrix diffusion in gas phase

International Nuclear Information System (INIS)

Hartikainen, K.; Timonen, J.; Vaeaetaeinen, K.; Pietarila, H.

1994-03-01

The diffusion of solutes from fractures into rock matrix is an important factor in the safety analysis of disposal of radioactive waste. Laboratory measurements are needed to complement field investigations for a reliable determination of the necessary transport parameters. Measurements of diffusion coefficients in tight rock samples are usually time consuming because the diffusion processes are slow. On the other hand it is well known that diffusion coefficients in the gas phase are roughly four orders of magnitude larger than those in the liquid phase. Therefore, for samples whose structures do not change much upon drying, it is possible to estimate the diffusion properties of the liquid phase when the properties of the gas phase are known. Advantages of the gas method are quick and easy measurements. In the measurements nitrogen was used as the carrier gas and helium as the tracer gas, and standard techniques have been used for helium detection. Techniques have been developed for both channel flow and through-diffusion measurements. The breakthrough curves have been measured in every experiment and all measurements have been modelled by using appropriate analytical models. As a result matrix porosities and effective diffusion coefficients in the gas phase have been determined. (12 refs., 21 figs., 6 tabs.)

Epitaxial engineering of polar ɛ-Ga2O3 for tunable two-dimensional electron gas at the heterointerface

Science.gov (United States)

Cho, Sung Beom; Mishra, Rohan

2018-04-01

We predict the formation of a polarization-induced two-dimensional electron gas (2DEG) at the interface of ɛ-Ga2O3 and CaCO3, wherein the density of the 2DEG can be tuned by reversing the spontaneous polarization in ɛ-Ga2O3, for example, with an applied electric field. ɛ-Ga2O3 is a polar and metastable ultra-wide band-gap semiconductor. We use density-functional theory (DFT) calculations and coincidence-site lattice model to predict the region of epitaxial strain under which ɛ-Ga2O3 can be stabilized over its other competing polymorphs and suggest promising substrates. Using group-theoretical methods and DFT calculations, we show that ɛ-Ga2O3 is a ferroelectric material where the spontaneous polarization can be reversed through a non-polar phase by using an electric field. Based on the calculated band alignment of ɛ-Ga2O3 with various substrates, we show the formation of a 2DEG with a high sheet charge density of 1014 cm-2 at the interface with CaCO3 due to the spontaneous and piezoelectric polarization in ɛ-Ga2O3, which makes the system attractive for high-power and high-frequency applications.

Novel solid – solid phase change material based on polyethylene glycol and cellulose used for temperature stabilisation

Directory of Open Access Journals (Sweden)

Wojda Marta

2014-01-01

Full Text Available Thermal management is one of crucial issues in the development of modern electronic devices. In the recent years interest in phase change materials (PCMs as alternative cooling possibility has increased significantly. Preliminary results concerning the research into possibility of the use of solid-solid phase change materials (S-S PCMs for stabilisation temperature of electronic devices has been presented in the paper. Novel solid-solid phase change material based on polyethylene glycol and cellulose has been synthesized. Attempt to improve its thermal conductivity has been taken. Material has been synthesized for the purpose of stabilisation of temperature of electronic devices.

InAs film grown on Si(111) by metal organic vapor phase epitaxy

International Nuclear Information System (INIS)

Caroff, P; Jeppsson, M; Mandl, B; Wernersson, L-E; Wheeler, D; Seabaugh, A; Keplinger, M; Stangl, J; Bauer, G

2008-01-01

We report the successful growth of high quality InAs films directly on Si(111) by Metal Organic Vapor Phase Epitaxy. A nearly mirror-like and uniform InAs film is obtained at 580 0 C for a thickness of 2 μm. We measured a high value of the electron mobility of 5100 cm 2 /Vs at room temperature. The growth is performed using a standard two-step procedure. The influence of the nucleation layer, group V flow rate, and layer thickness on the electrical and morphological properties of the InAs film have been investigated. We present results of our studies by Atomic Force Microscopy, Scanning Electron Microscopy, electrical Hall/van der Pauw and structural X-Ray Diffraction characterization

Composition-induced structural, electrical, and magnetic phase transitions in AX-type mixed-valence cobalt oxynitride epitaxial thin films

Energy Technology Data Exchange (ETDEWEB)

Takahashi, Jumpei; Oka, Daichi [Department of Chemistry, School of Science, The University of Tokyo, 7-3-1 Hongo, Bunkyo, Tokyo 113-0033 (Japan); Kanagawa Academy of Science and Technology (KAST), 3-2-1 Sakado, Takatsu, Kawasaki 213-0012 (Japan); Hirose, Yasushi, E-mail: hirose@chem.s.u-tokyo.ac.jp; Yang, Chang; Fukumura, Tomoteru; Hasegawa, Tetsuya [Department of Chemistry, School of Science, The University of Tokyo, 7-3-1 Hongo, Bunkyo, Tokyo 113-0033 (Japan); Kanagawa Academy of Science and Technology (KAST), 3-2-1 Sakado, Takatsu, Kawasaki 213-0012 (Japan); CREST, Japan Science and Technology Agency, 7-3-1 Hongo, Bunkyo, Tokyo 113-0033 (Japan); Nakao, Shoichiro [Kanagawa Academy of Science and Technology (KAST), 3-2-1 Sakado, Takatsu, Kawasaki 213-0012 (Japan); CREST, Japan Science and Technology Agency, 7-3-1 Hongo, Bunkyo, Tokyo 113-0033 (Japan); Harayama, Isao; Sekiba, Daiichiro [University of Tsukuba Tandem Accelerator Complex (UTTAC), 1-1-1 Tennoudai, Tsukuba, Ibaraki 305-8577 (Japan)

2015-12-07

Synthesis of mid- to late-transition metal oxynitrides is generally difficult by conventional thermal ammonolysis because of thermal instability. In this letter, we synthesized epitaxial thin films of AX-type phase-pure cobalt oxynitrides (CoO{sub x}N{sub y}) by using nitrogen-plasma-assisted pulsed laser deposition and investigated their structural, electrical, and magnetic properties. The CoO{sub x}N{sub y} thin films with 0 ≤ y/(x + y) ≤ 0.63 grown on MgO (100) substrates showed a structural phase transition from rock salt (RS) to zinc blend at the nitrogen content y/(x + y) ∼ 0.5. As the nitrogen content increased, the room-temperature electrical resistivity of the CoO{sub x}N{sub y} thin films monotonically decreased from the order of 10{sup 5} Ω cm to 10{sup −4} Ω cm. Furthermore, we observed an insulator-to-metal transition at y/(x + y) ∼ 0.34 in the RS-CoO{sub x}N{sub y} phase, which has not yet been reported in Co{sup 2+}/Co{sup 3+} mixed-valence cobalt oxides with octahedral coordination. The low resistivity in the RS-CoO{sub x}N{sub y} phase, on the 10{sup −3} Ω cm order, may have originated from the intermediate spin state of Co{sup 3+} stabilized by the lowered crystal field symmetry of the CoO{sub 6−n}N{sub n} octahedra (n = 1, 2,…5). Magnetization measurements suggested that a magnetic phase transition occurred in the RS-CoO{sub x}N{sub y} films during the insulator-to-metal transition. These results demonstrate that low-temperature epitaxial growth is a promising approach for exploring novel electronic functionalities in oxynitrides.

Composition-induced structural, electrical, and magnetic phase transitions in AX-type mixed-valence cobalt oxynitride epitaxial thin films

International Nuclear Information System (INIS)

Takahashi, Jumpei; Oka, Daichi; Hirose, Yasushi; Yang, Chang; Fukumura, Tomoteru; Hasegawa, Tetsuya; Nakao, Shoichiro; Harayama, Isao; Sekiba, Daiichiro

2015-01-01

Synthesis of mid- to late-transition metal oxynitrides is generally difficult by conventional thermal ammonolysis because of thermal instability. In this letter, we synthesized epitaxial thin films of AX-type phase-pure cobalt oxynitrides (CoO x N y ) by using nitrogen-plasma-assisted pulsed laser deposition and investigated their structural, electrical, and magnetic properties. The CoO x N y thin films with 0 ≤ y/(x + y) ≤ 0.63 grown on MgO (100) substrates showed a structural phase transition from rock salt (RS) to zinc blend at the nitrogen content y/(x + y) ∼ 0.5. As the nitrogen content increased, the room-temperature electrical resistivity of the CoO x N y thin films monotonically decreased from the order of 10 5  Ω cm to 10 −4  Ω cm. Furthermore, we observed an insulator-to-metal transition at y/(x + y) ∼ 0.34 in the RS-CoO x N y phase, which has not yet been reported in Co 2+ /Co 3+ mixed-valence cobalt oxides with octahedral coordination. The low resistivity in the RS-CoO x N y phase, on the 10 −3  Ω cm order, may have originated from the intermediate spin state of Co 3+ stabilized by the lowered crystal field symmetry of the CoO 6−n N n octahedra (n = 1, 2,…5). Magnetization measurements suggested that a magnetic phase transition occurred in the RS-CoO x N y films during the insulator-to-metal transition. These results demonstrate that low-temperature epitaxial growth is a promising approach for exploring novel electronic functionalities in oxynitrides

Probing the liquid and solid phases in closely spaced two-dimensional systems

Energy Technology Data Exchange (ETDEWEB)

Zhang, Ding

2014-03-06

Gas, liquid and solid phases are the most common states of matter in our daily encountered 3-dimensional space. The school example is the H{sub 2}O molecule with its phases vapor, water and ice. Interestingly, electrons - with their point-like nature and negative charges - can also organize themselves under certain conditions to bear properties of these three common phases. At relatively high temperature, where Boltzmann statistics prevails, the ensemble of electrons without interactions can be treated as a gas of free particles. Cooling down the system, this electron gas condenses into a Fermi liquid. Finally, as a result of the repulsive Coulomb forces, electrons try to avoid each other by maximizing their distances. When the Coulomb interaction becomes sufficiently strong, a regular lattice emerges - an electron solid. The story however does not end here. Nature has much more in store for us. Electronic systems in fact exhibit a large variety of phases induced by spatial confinement, an external magnetic field, Coulomb interactions, or interactions involving degrees of freedom other than charge such as spin and valley. Here in this thesis, we restrict ourselves to the study of electrons in a 2-dimenisonal (2D) plane. Already in such a 2D electron system (2DES), several distinct states of matter appear: integer and fractional quantum Hall liquids, the 2D Wigner solid, stripe and bubble phases etc. In 2DES it is sufficient to sweep the perpendicular magnetic field to pass from one of these phases into another. Experimentally, many of these phases can be revealed by simply measuring the resistance. For a quantum Hall state, the longitudinal resistance vanishes, while the Hall resistance exhibits a plateau. The quantum Hall plateau is a manifestation of localization induced by the inevitable sample disorder. Coulomb interaction can also play an important role to localize charges. Even in the disorder-free case, electrons - more precisely quasi-particles in the

Probing the liquid and solid phases in closely spaced two-dimensional systems

International Nuclear Information System (INIS)

Zhang, Ding

2014-01-01

Gas, liquid and solid phases are the most common states of matter in our daily encountered 3-dimensional space. The school example is the H 2 O molecule with its phases vapor, water and ice. Interestingly, electrons - with their point-like nature and negative charges - can also organize themselves under certain conditions to bear properties of these three common phases. At relatively high temperature, where Boltzmann statistics prevails, the ensemble of electrons without interactions can be treated as a gas of free particles. Cooling down the system, this electron gas condenses into a Fermi liquid. Finally, as a result of the repulsive Coulomb forces, electrons try to avoid each other by maximizing their distances. When the Coulomb interaction becomes sufficiently strong, a regular lattice emerges - an electron solid. The story however does not end here. Nature has much more in store for us. Electronic systems in fact exhibit a large variety of phases induced by spatial confinement, an external magnetic field, Coulomb interactions, or interactions involving degrees of freedom other than charge such as spin and valley. Here in this thesis, we restrict ourselves to the study of electrons in a 2-dimenisonal (2D) plane. Already in such a 2D electron system (2DES), several distinct states of matter appear: integer and fractional quantum Hall liquids, the 2D Wigner solid, stripe and bubble phases etc. In 2DES it is sufficient to sweep the perpendicular magnetic field to pass from one of these phases into another. Experimentally, many of these phases can be revealed by simply measuring the resistance. For a quantum Hall state, the longitudinal resistance vanishes, while the Hall resistance exhibits a plateau. The quantum Hall plateau is a manifestation of localization induced by the inevitable sample disorder. Coulomb interaction can also play an important role to localize charges. Even in the disorder-free case, electrons - more precisely quasi-particles in the partially

Layered growth model and epitaxial growth structures for SiCAlN alloys

International Nuclear Information System (INIS)

Liu Zhaoqing; Ni Jun; Su Xiaoao; Dai Zhenhong

2009-01-01

Epitaxial growth structures for (SiC) 1-x (AlN) x alloys are studied using a layered growth model. First-principle calculations are used to determine the parameters in the layered growth model. The phase diagrams of epitaxial growth are given. There is a rich variety of the new metastable polytype structures at x=1/6 ,1/5 ,1/4 ,1/3 , and 1/2 in the layered growth phase diagrams. We have also calculated the electronic properties of the short periodical SiCAlN alloys predicted by our layered growth model. The results show that various ordered structures of (SiC) 1-x (AlN) x alloys with the band gaps over a wide range are possible to be synthesized by epitaxial growth.

A numerical study of three-dimensional flame propagation over thin solids in purely forced concurrent flow including gas-phase radiation

Science.gov (United States)

Feier, Ioan I., Jr.

The effect of flame radiation on concurrent-flow flame spread over a thin solid sample of finite width in a low-speed wind tunnel is modeled using three-dimensional full Navier-Stokes equations and three-dimensional flame radiation transfer equations. The formulation includes the conservation of mass, momentum, energy, and species: fuel vapor, oxygen, carbon dioxide and water vapor. The SN discrete ordinates method is used to solve the radiation transfer equation with a mean absorption coefficient kappa = Ckappa p, where kappap is the Planck mean absorption coefficient of the gas mixture. The varying parameter C has a value between 0 and 1; C represents the strength of flame radiation. In addition, the solid fuel absorptivity alpha is varied to ascertain the effect of flame radiation heat feedback to the solid. The flow tunnel modeled has a dimension of 10x10x30 cm, the solid fuel has a width of 6-cm with two 1-cm inert strips as edges. Incoming forced flow velocity (5 cm/s) of 21% oxygen is assumed. For comparison with the three-dimensional results, corresponding two-dimensional computations are also performed. Detailed spatial flame profiles, solid surface profiles, and heat fluxes are presented. Increasing the flame radiation strength decreases the flame length. Although flame radiation provides an additional heat transfer mechanism to preheat the solid, it is insufficient to offset the decreased convective heating due to the shorter flame; the net effect is a slower spread rate. The percentage of unreacted fuel vapor that escapes from the flame is under 2%. It is theorized that some of the pyrolyzed fuel vapor diffuses sideway and reacts at the flame edges. A radiative energy balance is analyzed also. Flame radiative feedback to the solid plays a more important role in two-dimensional flames. With high solid fuel absorptivity, a peak in the flame spread rate occurs at an intermediate value of flame radiation strength---due to the competition between two

Gas Phase Vibrational Spectroscopy of Weakly Volatil Safe Taggants Using a Synchrotron Source

Science.gov (United States)

Cuisset, Arnaud; Hindle, Francis; Mouret, Gael; Gruet, Sebastien; Pirali, Olivier; Roy, Pascale

2013-06-01

The high performances of the AILES beamline of SOLEIL allow to study at medium resolution (0.5 cm^{-1}) the gas phase THz vibrational spectra of weakly volatil compounds. Between 2008 and 2010 we recorded and analyzed the THz/Far-IR spectra of phosphorous based nerve agents thanks to sufficient vapour pressures from liquid samples at room temperature. Recently, we extended these experiments towards the vibrational spectroscopy of vapour pressures from solid samples. This project is quite challenging since we target lower volatile compounds, and so requires very high sensitive spectrometers. Moreover a specially designed heated multipass-cell have been developped for the gas phase study of very weak vapor pressures. Thanks to skills acquired during initial studies and recent experiments performed on AILES with solid PAHs, we have recorded and assigned the gas phase vibrational fingerprints from the THz to the NIR spectral domain (10-4000 cm-1) of a set of targeted nitro-derivatives. The study was focused onto the para, ortho-mononitrotoluene (p-NT, o-NT), the 1,4 Dinitrobenzene (1,4 DNB), the 2,3-dimethyl-2,3-dinitrobutane (DMNB), and 2,4 and 2,6-dinitrotoluene (2,4-2,6 DNT), which are safe taggants widely used for the detection of commercial explosives. These taggants are usually added to plastic explosives in order to facilitate their vapour detection. Therefore, there is a continuous interest for their detection and identification in realistic conditions via optical methods. A first step consists in the recording of their gas phase vibrational spectra. These expected spectra focused onto molecules involved into defence and security domains are not yet available to date and will be very useful for the scientific community. This work is supported by the contract ANR-11-ASTR-035-01. A. Cuisset, G. Mouret, O. Pirali, P. Roy, F. Cazier, H. Nouali, J. Demaison, J. Phys. Chem. B, 2008, 112:, 12516-12525 I. Smirnova, A. Cuisset, R. Bocquet, F. Hindle, G. Mouret, O

Epitaxial Growth and Cracking Mechanisms of Thermally Sprayed Ceramic Splats

Science.gov (United States)

Chen, Lin; Yang, Guan-jun

2018-02-01

In the present study, the epitaxial growth and cracking mechanisms of thermally sprayed ceramic splats were explored. We report, for the first time, the epitaxial growth of various splat/substrate combinations at low substrate temperatures (100 °C) and large lattice mismatch (- 11.26%). Our results suggest that thermal spray deposition was essentially a liquid-phase epitaxy, readily forming chemical bonding. The interface temperature was also estimated. The results convincingly demonstrated that atoms only need to diffuse and rearrange over a sufficiently short range during extremely rapid solidification. Concurrently, severe cracking occurred in the epitaxial splat/substrate systems, which indicated high tensile stress was produced during splat deposition. The origin of the tensile stress was attributed to the strong constraint of the locally heated substrate by its cold surroundings.

A star-shaped polythiophene dendrimer coating for solid-phase microextraction of triazole agrochemicals.

Science.gov (United States)

Abolghasemi, Mir Mahdi; Habibiyan, Rahim; Jaymand, Mehdi; Piryaei, Marzieh

2018-02-14

A nanostructured star-shaped polythiophene dendrimer was prepared and used as a fiber coating for headspace solid phase microextraction of selected triazolic pesticides (tebuconazole, hexaconazole, penconazole, diniconazole, difenoconazole, triticonazole) from water samples. The dendrimer with its large surface area was characterized by thermogravimetric analysis, UV-Vis spectroscopy and field emission scanning electron microscopy. It was placed on a stainless steel wire for use in SPME. The experimental conditions for fiber coating, extraction, stirring rate, ionic strength, pH value, desorption temperature and time were optimized. Following thermal desorption, the pesticides were quantified by GC-MS. Under optimum conditions, the repeatability (RSD) for one fiber (for n = 3) ranges from 4.3 to 5.6%. The detection limits are between 8 and 12 pg mL -1 . The method is fast, inexpensive (in terms of equipment), and the fiber has high thermal stability. Graphical abstract Schematic presentation of a nanostructured star-shaped polythiophene dendrimer for use in headspace solid phase microextraction of the triazolic pesticides (tebuconazole, hexaconazole, penconazole, diniconazole, difenoconazole, triticonazole). They were then quantified by gas chromatography-mass spectrometry.

Amino-modified diamond as a durable stationary phase for solid-phase extraction.

Science.gov (United States)

Saini, Gaurav; Yang, Li; Lee, Milton L; Dadson, Andrew; Vail, Michael A; Linford, Matthew R

2008-08-15

We report the formation of a highly stable amino stationary phase on diamond and demonstrate its use in solid-phase extraction (SPE). This process consists of spontaneous and self-limiting adsorption of polyallylamine (PAAm) from aqueous solution onto oxidized diamond. Thermal curing under reduced pressure or chemical cross-linking with a diepoxide was shown to fix the polymer to the particles. The resulting adsorbents are stable under even extreme pH conditions (from at least pH 0-14) and significantly more stable than a commercially available amino SPE adsorbent. Coated diamond particles were characterized by X-ray photoelectron spectroscopy (XPS) and diffuse reflectance Fourier transform-infrared spectroscopy (DRIFT). Model silicon surfaces were characterized by spectroscopic ellipsometry and wetting. Solid-phase extraction was demonstrated using cholesterol, hexadecanedioic acid, and palmitoyloleoylphosphatidylcholine as analytes, and these results were compared to those obtained with commercially available materials. Breakthrough curves indicate that, as expected, porous diamond particles have higher analyte capacity than nonporous solid particles.

Adsorption-controlled growth of BiMnO3 films by molecular-beam epitaxy

International Nuclear Information System (INIS)

Lee, J. H.; Ke, X.; Misra, R.; Schiffer, P.; Ihlefeld, J. F.; Mei, Z. G.; Liu, Z. K.; Xu, X. S.; Musfeldt, J. L.; Heeg, T.; Schlom, D. G.; Roeckerath, M.; Schubert, J.

2010-01-01

We have developed the means to grow BiMnO 3 thin films with unparalleled structural perfection by reactive molecular-beam epitaxy and determined its band gap. Film growth occurs in an adsorption-controlled growth regime. Within this growth window bounded by oxygen pressure and substrate temperature at a fixed bismuth overpressure, single-phase films of the metastable perovskite BiMnO 3 may be grown by epitaxial stabilization. X-ray diffraction reveals phase-pure and epitaxial films with ω rocking curve full width at half maximum values as narrow as 11 arc sec (0.003 deg. ). Optical absorption measurements reveal that BiMnO 3 has a direct band gap of 1.1±0.1 eV.

Automated solid-phase extraction of herbicides from water for gas chromatographic-mass spectrometric analysis

Science.gov (United States)

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

1993-01-01

An automated solid-phase extraction (SPE) method was developed for the pre-concentration of chloroacetanilide and triazine herbicides, and two triazine metabolites from 100-ml water samples. Breakthrough experiments for the C18 SPE cartridge show that the two triazine metabolites are not fully retained and that increasing flow-rate decreases their retention. Standard curve r2 values of 0.998-1.000 for each compound were consistently obtained and a quantitation level of 0.05 ??g/l was achieved for each compound tested. More than 10,000 surface and ground water samples have been analyzed by this method.

Determination of six pesticides in the medicinal herb Cordia salicifolia by matrix solid-phase dispersion and gas chromatography/mass spectrometry.

Science.gov (United States)

de Carvalho, Pedro Henrique Viana; Prata, Vanessa de Menezes; Alves, Péricles Barreto; Navickiene, Sandro

2009-01-01

A simple and effective extraction method based on matrix solid-phase dispersion was developed for acephate, chlorpropham, pyrimicarb, bifenthrin, tetradifon, and phosalone in leaves of the medicinal plant Cordia salicifolia, whose extracts are commercialized in Brazil as diuretic, appetite suppressant, and weight loss products. The determination method was GC/MS with selected-ion monitoring. Different parameters of the method were evaluated, such as type of solid phase (C18, alumina, silica gel, and Florisil) and the amount of solid phase and eluent (dichloromethane, ethyl acetate, chloroform, and cyclohexane). The best results were obtained using 0.5 g herb sample, 0.5 g neutral alumina as the dispersant sorbent, 0.5 g C18 as the cleanup sorbent, and cyclohexane-dichloromethane (3 + 1, v/v) as the eluting solvent. The method was validated using herb samples fortified with pesticides at different concentration levels (0.3, 0.5, and 1.0 mg/kg). Average recoveries (seven replicates) ranged from 67.7 to 129.9%, with relative standard deviations between 6.3 and 26%. Detection and quantitation limits for the herb ranged from 0.10 to 0.15 and 0.15 to 0.25 mg/kg, respectively.

Matrix solid-phase dispersion followed by gas chromatography tandem mass spectrometry for the determination of benzotriazole UV absorbers in sediments.

Science.gov (United States)

Carpinteiro, I; Abuín, B; Ramil, M; Rodríguez, I; Cela, R

2012-01-01

A cost-effective and low solvent consumption method, based on the matrix solid-phase dispersion (MSPD) technique, for the determination of six benzotriazole UV absorbers in sediments is presented. Sieved samples (0.5 g) were first mixed in a mortar with a solid sorbent and then transferred to a polypropylene syringe containing a layer of clean-up co-sorbent. Analytes were eluted with a suitable solvent and further determined by gas chromatography with tandem mass spectrometry (GC-MS/MS). Under final conditions, diatomaceous earth and silica, deactivated to 10%, were used as inert dispersant and clean-up co-sorbent, respectively. Analytes were recovered using just 5 mL of dichloromethane, and this extract was concentrated and exchanged to 1 mL of isooctane. Further removal of co-extracted sulphur was achieved adding activated copper powder to final extracts, which were stored overnight, before injection in the GC-MS/MS system. The accuracy of the method was assessed with river and marine sediment samples showing different carbon contents and spiked at different concentrations in the range from 40 to 500 ng g(-1). Recoveries varied between 78% and 110% with associated standard deviations below 14%. The limits of quantification of the method stayed between 3 and 15 ng g(-1). Levels of target compounds in sediment samples ranged from not detected up to a maximum of 56 ng g(-1) for Tinuvin 328.

Synchrotron radiation excited silicon epitaxy using disilane

International Nuclear Information System (INIS)

Akazawa, Housei; Utsumi, Yuichi

1995-01-01

Synchrotron radiation (SR) excited chemical reactions provide new crystal growth methods suitable for low-temperature Si epitaxy. The growth kinetics and film properties were investigated by atomic layer epitaxy (ALE) and photochemical vapor deposition (CVD) modes using Si 2 H 6 . SR-ALE, isolating the surface growth channel mediated by photon stimulated hydrogen desorption, achieves digital growth independent of gas exposure time, SR irradiation time, and substrate temperature. On the other hand in SR-CVD, photolysis of Si 2 H 6 is predominant. In the nonirradiated region, Eley-Rideal type reaction between the photofragments and the surface deposit Si adatoms in a layer-by-layer fashion. In the irradiated region, however, multi-layer photolysis and rebounding occurs within the condensed Si 2 H 6 layer. The pertinent elementary processes were identified by using the high-resolution time-of-flight mass spectroscopy. The SR-CVD can grow a uniform and epitaxial Si film down to 200degC. The surface morphology is controlled by the surfactant effect of hydrogen atoms. (author)

Epitaxial growth of GaN/AlN/InAlN heterostructures for HEMTs in horizontal MOCVD reactors with different designs

Energy Technology Data Exchange (ETDEWEB)

Tsatsulnikov, A. F., E-mail: andrew@beam.ioffe.ru; Lundin, W. V.; Sakharov, A. V.; Zavarin, E. E.; Usov, S. O.; Nikolaev, A. E.; Yagovkina, M. A.; Ustinov, V. M. [Russian Academy of Sciences, Ioffe Physical–Technical Institute (Russian Federation); Cherkashin, N. A. [CEMES–CNRS—Université de Toulouse (France)

2016-09-15

The epitaxial growth of InAlN layers and GaN/AlN/InAlN heterostructures for HEMTs in growth systems with horizontal reactors of the sizes 1 × 2', 3 × 2', and 6 × 2' is investigated. Studies of the structural properties of the grown InAlN layers and electrophysical parameters of the GaN/AlN/InAlN heterostructures show that the optimal quality of epitaxial growth is attained upon a compromise between the growth conditions for InGaN and AlGaN. A comparison of the epitaxial growth in different reactors shows that optimal conditions are realized in small-scale reactors which make possible the suppression of parasitic reactions in the gas phase. In addition, the size of the reactor should be sufficient to provide highly homogeneous heterostructure parameters over area for the subsequent fabrication of devices. The optimal compositions and thicknesses of the InAlN layer for attaining the highest conductance in GaN/AlN/InAlN transistor heterostructures.

The investigation of exposure to benzene, toluene, ethylbenzene and xylene (BTEX with Solid Phase Microextr action Method in gas station in Yazd province

Directory of Open Access Journals (Sweden)

Mohammad Hossein Mosaddegh Mehrjerdi

2014-01-01

Full Text Available Abstract Background: Benzene, toluene, ethylbenzene and xylene (BTEX are volatile organic compounds which their physical and chemical characteristics are similar. Evaporation of BTEX from gasoline in petrol station into the air causes gasoline station attendants expose to them. A new extraction method of volatile organic compounds is solid phase microextraction (SPME. The aim of this study is to optimize extraction conditions of BTEX from air samples and then determination of gasoline station air contamination with BTEX in Yazd. Material and Methods: In this study air samples were collected using Tedlar bags and then extracted and analyzed with SPME fiber and gas chromatography equipped with a flame ionization detector. Results: Our results indicate that PDMS/CAR has the best peak area in comparison with two other fibers The Optimized extraction and desorption times are estimated 3 and 1 minutes, respectively Mean concentration of benzene, toluene, ethyl benzene and xylene in gas station’s air were 1932±807, 667±405, 148±89, 340±216 µg/m3 respectively. Conclusion: Benzene mean concentration is above threshold limit value (0.5PPM. Whereas, toluene, ethylbenzene and xylene mean concentration are lower than threshold limit values.

N-Acyliminium Intermediates in Solid-Phase Synthesis

DEFF Research Database (Denmark)

Quement, Sebastian Thordal le; Petersen, Rico; Meldal, M.

2010-01-01

N-Acyliminium ions are powerful intermediates in synthetic organic chemistry. Examples of their use are numerous in solution-phase synthesis, but there are unmerited few reports on these highly reactive electrophiles in solid-phase synthesis. The present review covers the literature to date and i...

Harsh-Environment Solid-State Gamma Detector for Down-hole Gas and Oil Exploration

Energy Technology Data Exchange (ETDEWEB)

Peter Sandvik; Stanislav Soloviev; Emad Andarawis; Ho-Young Cha; Jim Rose; Kevin Durocher; Robert Lyons; Bob Pieciuk; Jim Williams; David O' Connor

2007-08-10

The goal of this program was to develop a revolutionary solid-state gamma-ray detector suitable for use in down-hole gas and oil exploration. This advanced detector would employ wide-bandgap semiconductor technology to extend the gamma sensor's temperature capability up to 200 C as well as extended reliability, which significantly exceeds current designs based on photomultiplier tubes. In Phase II, project tasks were focused on optimization of the final APD design, growing and characterizing the full scintillator crystals of the selected composition, arranging the APD device packaging, developing the needed optical coupling between scintillator and APD, and characterizing the combined elements as a full detector system preparing for commercialization. What follows is a summary report from the second 18-month phase of this program.

Solid-phase synthesis of molecularly imprinted nanoparticles.

Science.gov (United States)

Canfarotta, Francesco; Poma, Alessandro; Guerreiro, Antonio; Piletsky, Sergey

2016-03-01

Molecularly imprinted polymers (MIPs) are synthetic materials, generally based on acrylic or methacrylic monomers, that are polymerized in the presence of a specific target molecule called the 'template' and capable of rebinding selectively to this target molecule. They have the potential to be low-cost and robust alternatives to biomolecules such as antibodies and receptors. When prepared by traditional synthetic methods (i.e., with free template in solution), their usefulness has been limited by high binding site heterogeneity, the presence of residual template and the fact that the production methods are complex and difficult to standardize. To overcome some of these limitations, we developed a method for the synthesis of MIP nanoparticles (nanoMIPs) using an innovative solid-phase approach, which relies on the covalent immobilization of the template molecules onto the surface of a solid support (glass beads). The obtained nanoMIPs are virtually free of template and demonstrate high affinity for the target molecule (e.g., melamine and trypsin in our published work). Because of an affinity separation step performed on the solid phase after polymerization, poor binders and unproductive polymer are removed, so the final product has more uniform binding characteristics. The overall protocol, starting from the immobilization of the template onto the solid phase and including the purification and characterization of the nanoparticles, takes up to 1 week.

Radiation-induced transformations of isolated organic molecules in solid rare gas matrices

International Nuclear Information System (INIS)

Feldman, V.I.

1998-01-01

Complete text of publication follows. The studies of radiation-chemical behaviour of isolated organic molecules in rigid inert media are of considerable interest for radiation chemistry and general structural chemistry. Previous efforts were limited to the ESR studies of radicals resulting from some small hydrocarbon molecules in frozen rare gas solutions. Recently, we developed an approach to the radiation chemistry of isolated organic molecules using classic matrix isolation procedure for sample preparation and a combination of ESR and IR spectroscopy for characterization of paramagnetic and diamagnetic species resulting form electron irradiation or organic molecules in solid rare gas matrices at 10-15 K. The results obtained reveal high efficiency of energy transfer from rare gas matrix to organic molecules. The total radiation-chemical yields of degradation of organic molecules in argon and xenon matrices were measured directly by IR spectroscopy. The studies of the effect of electron scavengers on the radiolysis of organic molecules in solid rare gases show that the main primary process is positive hole transfer from matrix to additive molecule. ESR spectra of a number of radical cations (alkanes, ethers, arenes) were first characterized in a low-disturbing environment. It was found that the electronic characteristics (IP, polarizability) of the matrix used had crucial effect on trapping and degradation of primary organic radical cations. Using matrices with various IP provides an unique possibility to examine the chemical meaning of excess energy resulting from exothermic positive hole transfer, that is, to follow the fate of excited cations in condensed phase

Correlation dimension estimate and its potential use in analysis of gas-solid flows

DEFF Research Database (Denmark)

Yin, Chungen; Rosendahl, Lasse Aistrup; Kær, Søren Knudsen

2005-01-01

Gas-solid flows are nonlinear systems. Therefore state-space analysis, a tool developed within the framework of nonlinear dynamics, could provide more useful insights into complex gas-solid flows. One of the positive aspects of state-space analysis is that the major properties of a system can be ...

Reactive solid surface morphology variation via ionic diffusion.

Science.gov (United States)

Sun, Zhenchao; Zhou, Qiang; Fan, Liang-Shih

2012-08-14

In gas-solid reactions, one of the most important factors that determine the overall reaction rate is the solid morphology, which can be characterized by a combination of smooth, convex and concave structures. Generally, the solid surface structure varies in the course of reactions, which is classically noted as being attributed to one or more of the following three mechanisms: mechanical interaction, molar volume change, and sintering. Here we show that if a gas-solid reaction involves the outward ionic diffusion of a solid-phase reactant then this outward ionic diffusion could eventually smooth the surface with an initial concave and/or convex structure. Specifically, the concave surface is filled via a larger outward diffusing surface pointing to the concave valley, whereas the height of the convex surface decreases via a lower outward diffusion flux in the vertical direction. A quantitative 2-D continuum diffusion model is established to analyze these two morphological variation processes, which shows consistent results with the experiments. This surface morphology variation by solid-phase ionic diffusion serves to provide a fourth mechanism that supplements the traditionally acknowledged solid morphology variation or, in general, porosity variation mechanisms in gas-solid reactions.

Gas-Phase Thermolyses

DEFF Research Database (Denmark)

Carlsen, Lars; Egsgaard, Helge

1982-01-01

The unimolecular gas-phase thermolyses of the four methyl and ethyl monothioacetates (5)–(8) have been studied by the flash vacuum thermolysis–field ionization mass spectrometry technique in the temperature range 883–1 404 K. The types of reactions verified were keten formation, thiono–thiolo rea...

Rapid estimate of solid volume in large tuff cores using a gas pycnometer

International Nuclear Information System (INIS)

Thies, C.; Geddis, A.M.; Guzman, A.G.

1996-09-01

A thermally insulated, rigid-volume gas pycnometer system has been developed. The pycnometer chambers have been machined from solid PVC cylinders. Two chambers confine dry high-purity helium at different pressures. A thick-walled design ensures minimal heat exchange with the surrounding environment and a constant volume system, while expansion takes place between the chambers. The internal energy of the gas is assumed constant over the expansion. The ideal gas law is used to estimate the volume of solid material sealed in one of the chambers. Temperature is monitored continuously and incorporated into the calculation of solid volume. Temperature variation between measurements is less than 0.1 degrees C. The data are used to compute grain density for oven-dried Apache Leap tuff core samples. The measured volume of solid and the sample bulk volume are used to estimate porosity and bulk density. Intrinsic permeability was estimated from the porosity and measured pore surface area and is compared to in-situ measurements by the air permeability method. The gas pycnometer accommodates large core samples (0.25 m length x 0.11 m diameter) and can measure solid volume greater than 2.20 cm 3 with less than 1% error

Solid phase extraction membrane

Science.gov (United States)

Carlson, Kurt C [Nashville, TN; Langer, Roger L [Hudson, WI

2002-11-05

A wet-laid, porous solid phase extraction sheet material that contains both active particles and binder and that possesses excellent wet strength is described. The binder is present in a relatively small amount while the particles are present in a relatively large amount. The sheet material is sufficiently strong and flexible so as to be pleatable so that, for example, it can be used in a cartridge device.

FORTRAN program for calculating liquid-phase and gas-phase thermal diffusion column coefficients

International Nuclear Information System (INIS)

Rutherford, W.M.

1980-01-01

A computer program (COLCO) was developed for calculating thermal diffusion column coefficients from theory. The program, which is written in FORTRAN IV, can be used for both liquid-phase and gas-phase thermal diffusion columns. Column coefficients for the gas phase can be based on gas properties calculated from kinetic theory using tables of omega integrals or on tables of compiled physical properties as functions of temperature. Column coefficients for the liquid phase can be based on compiled physical property tables. Program listings, test data, sample output, and users manual are supplied for appendices

Method for removing heavy metal and nitrogen oxides from flue gas, device for removing heavy metal and nitrogen oxides from flue gas

Energy Technology Data Exchange (ETDEWEB)

Huang, Hann-Sheng; Livengood, Charles David

1997-12-01

A method for the simultaneous removal of oxides and heavy metals from a fluid is provided comprising combining the fluid with compounds containing alkali and sulfur to create a mixture; spray drying the mixture to create a vapor phase and a solid phase; and isolating the vapor phase from the solid phase. A device is also provided comprising a means for spray-drying flue gas with alkali-sulfide containing liquor at a temperature sufficient to cause the flue gas to react with the compounds so as to create a gaseous fraction and a solid fraction and a means for directing the gaseous fraction to a fabric filter.

Determination of amphetamine-type stimulants in oral fluid by solid-phase microextraction and gas chromatography-mass spectrometry.

Science.gov (United States)

Souza, Daniele Z; Boehl, Paula O; Comiran, Eloisa; Mariotti, Kristiane C; Pechansky, Flavio; Duarte, Paulina C A V; De Boni, Raquel; Froehlich, Pedro E; Limberger, Renata P

2011-06-24

A method for the simultaneous identification and quantification of amphetamine (AMP), methamphetamine (MET), fenproporex (FEN), diethylpropion (DIE) and methylphenidate (MPH) in oral fluid collected with Quantisal™ device has been developed and validated. Thereunto, in-matrix propylchloroformate derivatization followed by direct immersion solid-phase microextraction and gas chromatography-mass spectrometry were employed. Deuterium labeled AMP was used as internal standard for all the stimulants and analysis was performed using the selected ion monitoring mode. The detector response was linear for the studied drugs in the concentration range of 2-256 ng mL(-1) (neat oral fluid), except for FEN, whereas the linear range was 4-256 ng mL(-1). The detection limits were 0.5 ng mL(-1) (MET), 1 ng mL(-1) (MPH) and 2 ng mL(-1) (DIE, AMP, FEN), respectively. Accuracy of quality control samples remained within 98.2-111.9% of the target concentrations, while precision has not exceeded 15% of the relative standard deviation. Recoveries with Quantisal™ device ranged from 77.2% to 112.1%. Also, the goodness-of-fit concerning the ordinary least squares model in the statistical inference of data has been tested through residual plotting and ANOVA. The validated method can be easily automated and then used for screening and confirmation of amphetamine-type stimulants in drivers' oral fluid. Copyright © 2011 Elsevier B.V. All rights reserved.

Improvements in or relating to process for the production of fuel gas from a carbonaceous solid

Energy Technology Data Exchange (ETDEWEB)

1952-12-03

A process was designed for the generation of fuel gas from a solid carbonaceous fuel containing volatilizable constituents, which comprises admixing the solid carbonaceous fuel in particle form with sufficient water to form a fluid suspension, passing the suspension through a heating zone at an elevated temperature such that substantially all of the water is vaporized, thereby forming a dispersion of coal in steam and causing the dispersion to attain a velocity of at least 60 ft. per second to shatter the particles of coal by collision, passing the resulting dispersion into a fluidized bed of solid carbonaceous material in a methanization zone into contact with carbon monoxide and hydrogen at a temperature within the range of from 900/sup 0/ to 1,800/sup 0/F whereby carbon monoxide and hydrogen are converted to methane and volatilizable constituents of the solid carbonaceous material are distilled therefrom, withdrawing carbonaceous material from the methanization zone and passing it into contact with oxygen and steam in dilute phase in a gasification zone maintained at a temperature within the range of 2,000/sup 0/ to about 3,000/sup 0/F, passing the resulting gases comprising carbon monoxide and hydrogen from the gasification zone into the methanization zone as the source of carbon monoxide and hydrogen, and discharging the gaseous products of the methanization zone as the raw-product fuel gas.

Magnetic solid phase extraction and static headspace gas chromatography-mass spectrometry method for the analysis of polycyclic aromatic hydrocarbons.

Science.gov (United States)

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

2016-01-15

A magnetic solid phase extraction (MSPE) protocol combining a static headspace gas chromatography coupled to mass spectrometry (HS-GC-MS) method has been developed for extraction, and determination of 16 polycyclic aromatic hydrocarbons (PAHs) in drinking water samples. Magnetic nanoparticles (MNPs) were coated with 3-aminopropyltriethoxysilane and modified by cholesterol chloroformate. Transmission electron microscope, vibrating sample magnetometer, Fourier transform infrared spectrometry and X-ray photoelectron spectroscopy were used to characterize the cholesterol-functionalized sorbents, and the main parameters affecting the extraction as well as HS sampling, such as sorbent amount, extraction time, oven temperature and equilibration time have been investigated and established. Combination with HS sampling, the MSPE procedure was simple, fast and environmentally friendly, without need of any organic solvent. Method validation proved the feasibility of the developed sorbents for the quantitation of the investigated analytes at trace levels obtaining the limit of detection (S/N=3) ranging from 0.20 to 7.8 ng/L. Good values for intra and inter-day precision were obtained (RSDs ≤ 9.9%). The proposed method was successfully applied to drinking water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Gas flow headspace liquid phase microextraction.

Science.gov (United States)

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

2009-11-06

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

Solid phase syntheses of oligoureas

Energy Technology Data Exchange (ETDEWEB)

Burgess, K.; Linthicum, D.S.; Russell, D.H.; Shin, H.; Shitangkoon, A.; Totani, R.; Zhang, A.J.; Ibarzo, J. [Texas A& M Univ., College Station, TX (United States)

1997-02-19

Isocyanates 7 were formed from monoprotected diamines 3 or 6, which in turn can be easily prepared from commercially available N-BOC- or N-FMOC-protected amino acid derivatives. Isocyanates 7, formed in situ, could be coupled directly to a solid support functionalized with amine groups or to amino acids anchored on resins using CH{sub 2}Cl{sub 2} as solvent and an 11 h coupling time at 25 {degree}C. Such couplings afforded peptidomimetics with an N-phthaloyl group at the N-terminus. The optimal conditions identified for removal of the N-phthaloyl group were to use 60% hydrazine in DMF for 1-3 h. Several sequences of amino acids coupled to ureas (`peptidic ureas`) and of sequential urea units (`oligoureas`) were prepared via solid phase syntheses and isolated by HPLC. Partition coefficients were measured for two of these peptidomimetics, and their water solubilities were found to be similar to the corresponding peptides. A small library of 160 analogues of the YGGFL-amide sequence was prepared via Houghten`s tea bag methodology. This library was tested for binding to the anti-{beta}-endorphin monoclonal antibody. Overall, this paper describes methodology for solid phase syntheses of oligourea derivatives with side chains corresponding to some of the protein amino acids. The chemistry involved is ideal for high-throughput syntheses and screening operations. 51 refs., 3 figs., 2 tabs.

Simultaneous solution algorithms for Eulerian-Eulerian gas-solid flow models: Stability analysis and convergence behaviour of a point and a plane solver

International Nuclear Information System (INIS)

Wilde, Juray de; Vierendeels, Jan; Heynderickx, Geraldine J.; Marin, Guy B.

2005-01-01

Simultaneous solution algorithms for Eulerian-Eulerian gas-solid flow models are presented and their stability analyzed. The integration algorithms are based on dual-time stepping with fourth-order Runge-Kutta in pseudo-time. The domain is solved point or plane wise. The discretization of the inviscid terms is based on a low-Mach limit of the multi-phase preconditioned advection upstream splitting method (MP-AUSMP). The numerical stability of the simultaneous solution algorithms is analyzed in 2D with the Fourier method. Stability results are compared with the convergence behaviour of 3D riser simulations. The impact of the grid aspect ratio, preconditioning, artificial dissipation, and the treatment of the source terms is investigated. A particular advantage of the simultaneous solution algorithms is that they allow a fully implicit treatment of the source terms which are of crucial importance for the Eulerian-Eulerian gas-solid flow models and their solution. The numerical stability of the optimal simultaneous solution algorithm is analyzed for different solids volume fractions and gas-solid slip velocities. Furthermore, the effect of the grid resolution on the convergence behaviour and the simulation results is investigated. Finally, simulations of the bottom zone of a pilot-scale riser with a side solids inlet are experimentally validated

Volatile organo-selenium speciation in biological matter by solid phase microextraction-moderate temperature multicapillary gas chromatography with microwave induced plasma atomic emission spectrometry detection

Energy Technology Data Exchange (ETDEWEB)

Dietz, C.; Sanz Landaluze, J.; Ximenez-Embun, P.; Madrid-Albarran, Y.; Camara, C

2004-01-16

Microwave induced plasma atomic emission spectrometry (MIP-AES) in combination with multicapillary (MC) gas chromatography could be proven to be useful for element specific detection of volatile species. Solid phase microextraction (SPME) was used for preconcentration and sample-matrix separation. The fiber desorption unit as well as the heating control for the MC column were in-house developed and multicapillary column was operated at moderate temperatures (30-100 deg. C). The method was optimized for organo-selenium species (dimethylselenide (DMSe), diethylselenide (DEtSe) and dimethyldiselenide (DMDSe)), using a chemometric approach. Stationary phases for the separation column were optimized using a conventional GC and contrasted with the results obtained with the MC. Application was focussed on selenium accumulating biological matter, such as lupine, yeast, Indian mustard and garlic. These samples were grown in hydroponic solution containing inorganic selenium (Na{sub 2}SeO{sub 3} and Na{sub 2}SeO{sub 4}). SPME sampling was carried out in fixed volume flow boxes in headspace above the living plants and in vials using treated samples. Results demonstrate inorganic selenium transformation into volatile organic species during metabolism. Separation is fast, a chromatogram can be obtained in less than 3 min and detection limits were at sub-ppb level for all investigated species. The system is independent from the use of a conventional gas chromatographic oven and can be used as a versatile alternative to highly cost intensive methods such as GC-ICP-MS.

Structural, electrical and luminescent characteristics of ultraviolet light emitting structures grown by hydride vapor phase epitaxy

Directory of Open Access Journals (Sweden)

A.Y. Polyakov

2017-03-01

Full Text Available Electrical and luminescent properties of near-UV light emitting diode structures (LEDs prepared by hydride vapor phase epitaxy (HVPE were studied. Variations in photoluminescence and electroluminescence efficiency observed for LEDs grown under nominally similar conditions could be attributed to the difference in the structural quality (dislocation density, density of dislocations agglomerates of the GaN active layers, to the difference in strain relaxation achieved by growth of AlGaN/AlGaN superlattice and to the presence of current leakage channels in current confining AlGaN layers of the double heterostructure.

Multiple headspace-solid-phase microextraction: An application to quantification of mushroom volatiles

Energy Technology Data Exchange (ETDEWEB)

Costa, Rosaria; Tedone, Laura; De Grazia, Selenia [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Dugo, Paola [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Centro Integrato di Ricerca (C.I.R.), Università Campus-Biomedico, Via Álvaro del Portillo, 21, 00128 Roma (Italy); Mondello, Luigi, E-mail: lmondello@unime.it [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Centro Integrato di Ricerca (C.I.R.), Università Campus-Biomedico, Via Álvaro del Portillo, 21, 00128 Roma (Italy)

2013-04-03

Highlights: ► Multiple headspace extraction-solid phase microextraction (MHS-SPME) has been applied to the analysis of Agaricus bisporus. ► Mushroom flavor is characterized by the presence of compounds with a 8-carbon atoms skeleton. ► Formation of 8-carbon compounds involves a unique fungal biochemical pathway. ► The MHS-SPME allowed to determine quantitatively 5 target analytes of A. bisporus for the first time. -- Abstract: Multiple headspace-solid phase microextraction (MHS-SPME) followed by gas chromatography/mass spectrometry (GC–MS) and flame ionization detection (GC–FID) was applied to the identification and quantification of volatiles released by the mushroom Agaricus bisporus, also known as champignon. MHS-SPME allows to perform quantitative analysis of volatiles from solid matrices, free of matrix interferences. Samples analyzed were fresh mushrooms (chopped and homogenized) and mushroom-containing food dressings. 1-Octen-3-ol, 3-octanol, 3-octanone, 1-octen-3-one and benzaldehyde were common constituents of the samples analyzed. Method performance has been tested through the evaluation of limit of detection (LoD, range 0.033–0.078 ng), limit of quantification (LoQ, range 0.111–0.259 ng) and analyte recovery (92.3–108.5%). The results obtained showed quantitative differences among the samples, which can be attributed to critical factors, such as the degree of cell damage upon sample preparation, that are here discussed. Considerations on the mushrooms biochemistry and on the basic principles of MHS analysis are also presented.

Multiple headspace-solid-phase microextraction: An application to quantification of mushroom volatiles

International Nuclear Information System (INIS)

Costa, Rosaria; Tedone, Laura; De Grazia, Selenia; Dugo, Paola; Mondello, Luigi

2013-01-01

Highlights: ► Multiple headspace extraction-solid phase microextraction (MHS-SPME) has been applied to the analysis of Agaricus bisporus. ► Mushroom flavor is characterized by the presence of compounds with a 8-carbon atoms skeleton. ► Formation of 8-carbon compounds involves a unique fungal biochemical pathway. ► The MHS-SPME allowed to determine quantitatively 5 target analytes of A. bisporus for the first time. -- Abstract: Multiple headspace-solid phase microextraction (MHS-SPME) followed by gas chromatography/mass spectrometry (GC–MS) and flame ionization detection (GC–FID) was applied to the identification and quantification of volatiles released by the mushroom Agaricus bisporus, also known as champignon. MHS-SPME allows to perform quantitative analysis of volatiles from solid matrices, free of matrix interferences. Samples analyzed were fresh mushrooms (chopped and homogenized) and mushroom-containing food dressings. 1-Octen-3-ol, 3-octanol, 3-octanone, 1-octen-3-one and benzaldehyde were common constituents of the samples analyzed. Method performance has been tested through the evaluation of limit of detection (LoD, range 0.033–0.078 ng), limit of quantification (LoQ, range 0.111–0.259 ng) and analyte recovery (92.3–108.5%). The results obtained showed quantitative differences among the samples, which can be attributed to critical factors, such as the degree of cell damage upon sample preparation, that are here discussed. Considerations on the mushrooms biochemistry and on the basic principles of MHS analysis are also presented

Solid-Phase S-Alkylation Promoted by Molecular Sieves.

Science.gov (United States)

Calce, Enrica; Leone, Marilisa; Mercurio, Flavia Anna; Monfregola, Luca; De Luca, Stefania

2015-11-20

A solid-phase S-alkylation procedure to introduce chemical modification on the cysteine sulfhydryl group of a peptidyl resin is reported. The reaction is promoted by activated molecular sieves and consists of a solid-solid process, since both the catalyst and the substrate are in a solid state. The procedure was revealed to be efficient and versatile, particularly when used in combination with the solution S-alkylation approach, allowing for the introduction of different molecular diversities on the same peptide molecule.

Effects of gas periodic stimulation on key enzyme activity in gas double-dynamic solid state fermentation (GDD-SSF).

Science.gov (United States)

Chen, Hongzhang; Shao, Meixue; Li, Hongqiang

2014-03-05

The heat and mass transfer have been proved to be the important factors in air pressure pulsation for cellulase production. However, as process of enzyme secretion, the cellulase formation has not been studied in the view of microorganism metabolism and metabolic key enzyme activity under air pressure pulsation condition. Two fermentation methods in ATPase activity, cellulase productivity, weight lose rate and membrane permeability were systematically compared. Results indicated that gas double-dynamic solid state fermentation had no obviously effect on cell membrane permeability. However, the relation between ATPase activity and weight loss rate was linearly dependent with r=0.9784. Meanwhile, the results also implied that gas periodic stimulation had apparently strengthened microbial metabolism through increasing ATPase activity during gas double-dynamic solid state fermentation, resulting in motivating the production of cellulase by Trichoderma reesei YG3. Therefore, the increase of ATPase activity would be another crucial factor to strengthen fermentation process for cellulase production under gas double-dynamic solid state fermentation. Copyright © 2013 Elsevier Inc. All rights reserved.

Gas phase dispersion in a small rotary kiln

International Nuclear Information System (INIS)

Spencer, B.B.

1981-07-01

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

Linkage of biomolecules to solid phases for immunoassay

International Nuclear Information System (INIS)

Chapman, R.S.

1998-01-01

Topics covered by this lecture include a brief review of the principal methods of linkage of biomolecules to solid phase matrices. Copies of the key self explanatory slides are presented as figures together with reprints of two publications by the author dealing with a preferred chemistry for the covalent linkage of antibodies to hydroxyl and amino functional groups and the effects of changes in solid phase matrix and antibody coupling chemistry on the performance of a typical excess reagent immunoassay for thyroid stimulating hormone

Hydrodynamic boundary conditions for one-component liquid-gas flows on non-isothermal solid substrates

KAUST Repository

Xu, Xinpeng; Liu, Chun; Qian, Tiezheng

2012-01-01

profiles of liquid-gas flows on non-isothermal, heterogeneous solid substrates is still absent. The purpose of this work is to construct a continuum model for simulating the liquid-gas flows on solid surfaces that are flat and rigid, and may involve

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.

Science.gov (United States)

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.

Adsorption of gas mixtures on heterogeneous solid surfaces

Energy Technology Data Exchange (ETDEWEB)

Jaroniec, M; Rudzinski, W

1977-01-01

A review of theoretical studies on the physical adsorption from gas mixtures on heterogeneous solid surfaces, mainly by Jaroniec and coworkers, covers the vector notation used in the calculations; adsorption isotherms for multicomponent gases; the generalized integral equation for adsorption of gas mixtures, its numerical and analytical solutions, applied, (e.g., to interpret the experimental adsorption isotherms of ethane/ethylene on Nuxit-AL); thermodynamic relations, applied, (e.g., to calculating isosteric adsorption heats from experimental parameters for the adsorption of propylene from propane/propylene mixtures on Nuxit-AL); and the derivation and use of a simplified integral equation for describing the adsorption from gas mixtures on heterogeneous surfaces. 75 references.

Molecular-beam epitaxy growth of high-performance midinfrared diode lasers

International Nuclear Information System (INIS)

Turner, G.W.; Choi, H.K.; Calawa, D.R.

1994-01-01

Recent advances in the performance of GaInAsSb/AlGaAsSb quantum-well diode lasers have been directly related to improvements in the quality of the molecular-beam epitaxy (MBE)-grown epitaxial layers. These improvements have been based on careful measurement and control of lattice matching and intentional strain, changes in shutter sequencing at interfaces, and a generally better understanding of the growth of Sb-based epitaxial materials. By using this improved MBE-grown material, significantly enhanced performance has been obtained for midinfrared lasers. These lasers, which are capable of ∼2-μm emission at room temperature, presently exhibit threshold current densities of 143 A/cm 2 , continuous wave powers of 1.3 W, and diffraction-limited powers of 120 mW. Such high-performance midinfrared diode lasers are of interest for a wide variety of applications, including eye-safe laser radar, remote sensing of atmospheric contaminants and wind turbulence, laser surgery, and pumping of solid-state laser media. 12 refs., 3 figs

Phase diagram of a Lennard-Jones solid

International Nuclear Information System (INIS)

Choi, Y.; Ree, T.; Ree, F.H.

1993-01-01

A phase diagram of a Lennard-Jones solid at kT/ε≥0.8 is constructed by our recent perturbation theory. It shows the stability of the face-centered-cubic phase except within a small pressure and temperature domain, where the hexagonal-close packed phase may occur. The theory predicts anharmonic contributions to the Helmholtz free energy (important to the crystal stability) in good agreement with Monte Carlo data

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

International Nuclear Information System (INIS)

Cassidy, D.P.; Irvine, R.L.

1995-01-01

Both slurry-phase and solid-phase bioremediation are effective ex situ soil decontamination methods. Slurry 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 bioslurry 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 load 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 ate and 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

One unit-cell seed layer induced epitaxial growth of heavily nitrogen doped anatase TiO{sub 2} films

Energy Technology Data Exchange (ETDEWEB)

Chen, T L; Hirose, Y; Hitosugi, T; Hasegawa, T [Kanagawa Academy of Science and Technology (KAST), Kawasaki 213-0012 (Japan)], E-mail: chen@ksp.or.jp

2008-03-21

We present a novel way to obtain heavily nitrogen doped anatase TiO{sub 2} films by using a solid-state nitrogen source. Epitaxial growth of the films was realized by introducing one unit-cell seed layer, which was indicated by reflection high-energy electron diffraction as intensity oscillation. Results of x-ray diffraction and x-ray photoelectron spectroscopy confirmed that the films were in the anatase phase heavily doped with nitrogen of {approx}15 at%. The films obtained exhibited considerable narrowing of the optical bandgap, resulting in an enhancement of absorption in the visible-light region. (fast track communication)

MOLECULARLY IMPRINTED SOLID PHASE EXTRACTION FOR TRACE ANALYSIS OF DIAZINON IN DRINKING WATER

Directory of Open Access Journals (Sweden)

M. Rahiminejad ، S. J. Shahtaheri ، M. R. Ganjali ، A. Rahimi Forushani ، F. Golbabaei

2009-04-01

Full Text Available Amongst organophosphate pesticides, the one most widely used and common environmental contaminant is diazinon; thus methods for its trace analysis in environmental samples must be developed. Use of diazinon imprinted polymers such as sorbents in solid phase extraction, is a prominent and novel application area of molecular imprinted polymers. For diazinon extraction, high performance liquid chromatography analysis was demonstrated in this study. During optimization of the molecular imprinted solid phase extraction procedure for efficient solid phase extraction of diazinon, Plackett-Burman design was conducted. Eight experimental factors with critical influence on molecular imprinted solid phase extraction performance were selected, and 12 different experimental runs based on Plackett-Burman design were carried out. The applicability of diazinon imprinted polymers as the sorbent in solid phase extraction, presented obtained good recoveries of diazinon from LC-grade water. An increase in pH caused an increase in the recovery on molecular imprinted solid phase extraction. From these results, the optimal molecular imprinted solid phase extraction procedure was as follows: solid phase extraction packing with 100 mg diazinon imprinted polymers; conditioning with 5 mL of methanol and 6 mL of LC-grade water; sample loading containing diazinon (pH=10; washing with 1 mL of LC-grade water, 1 mL LC- grade water containing 30% acetonitrile and 0.5 mL of acetonitrile, respectively; eluting with 1 mL of methanol containing 2% acetic acid. The percentage recoveries obtained by the optimized molecular imprinted solid phase extraction were more than 90% with drinking water spiked at different trace levels of diazinon. Generally speaking, the molecular imprinted solid phase extraction procedure and subsequent high performance liquid chromatography analysis can be a relatively fast and proper approach for qualitative and quantitative analysis of diazinon in

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

Science.gov (United States)

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

Evaluation of volatile profiles obtained for minimally-processed pineapple fruit samples during storage by headspace-solid phase microextraction gas chromatography-mass spectrometry

Directory of Open Access Journals (Sweden)

Francielle Crocetta TURAZZI

Full Text Available Abstract This paper describes the application of the solid-phase microextraction (SPME technique for the determination and monitoring of the volatile profile of minimally-processed pineapple fruit stored at various temperatures (-12 °C, 4 °C and 25 °C for different periods (1, 4 and 10 days. The SPME fiber coating composed of Car/PDMS presented the best performance. The optimal extraction conditions obtained through a Doehlert design were 60 min at 35 °C. The profiles for the volatile compounds content of the fruit at each stage of storage were determined by gas chromatography-mass spectrometry (GC-MS. The variation in the volatile profile over time was greater when the fruit samples were stored at 25 °C and at -12 °C compared to 4 °C. Thus, according to the volatile profiles associated with the storage conditions evaluated in this study, packaged pineapple retains best its fresh fruit aroma when stored at 4 °C.

Speciation analysis of organotin compounds in human urine by headspace solid-phase micro-extraction and gas chromatography with pulsed flame photometric detection.

Science.gov (United States)

Valenzuela, Aníbal; Lespes, Gaëtane; Quiroz, Waldo; Aguilar, Luis F; Bravo, Manuel A

2014-07-01

A new headspace solid-phase micro-extraction (HS-SPME) method followed by gas chromatography with pulsed flame photometric detection (GC-PFPD) analysis has been developed for the simultaneous determination of 11 organotin compounds, including methyl-, butyl-, phenyl- and octyltin derivates, in human urine. The methodology has been validated by the analysis of urine samples fortified with all analytes at different concentration levels, and recovery rates above 87% and relative precisions between 2% and 7% were obtained. Additionally, an experimental-design approach has been used to model the storage stability of organotin compounds in human urine, demonstrating that organotins are highly degraded in this medium, although their stability is satisfactory during the first 4 days of storage at 4 °C and pH=4. Finally, this methodology was applied to urine samples collected from harbor workers exposed to antifouling paints; methyl- and butyltins were detected, confirming human exposure in this type of work environment. Copyright © 2014 Elsevier B.V. All rights reserved.

Solid phase microextraction.

Science.gov (United States)

Pawliszyn, J

2001-01-01

Solid Phase Microextraction (SPME) uses a small volume of sorbent dispersed typically on the surface of small fibres, to isolate and concentrate analytes from sample matrix. After contact with sample, analytes are absorbed or adsorbed by the fibre phase (depending on the nature of the coating) until an equilibrium is reached in the system. The amount of an analyte extracted by the coating at equilibrium is determined by the magnitude of the partition coefficient of the analyte between the sample matrix and the coating material. After the extraction step, the fibres are transferred, with the help of a syringe-like handling device, to analytical instrument, for separation and quantitation of target analytes. This technique integrates sampling, extraction and sample introduction and is a simple way of facilitating on-site monitoring. Applications of this technique include environmental monitoring, industrial hygiene, process monitoring, clinical, forensic, food, flavour, fragrance and drug analyses, in laboratory and on-site analysis.

Phase equilibria of carbon dioxide and methane gas-hydrates predicted with the modified analytical S-L-V equation of state

Directory of Open Access Journals (Sweden)

Span Roland

2012-04-01

Full Text Available Gas-hydrates (clathrates are non-stoichiometric crystallized solutions of gas molecules in the metastable water lattice. Two or more components are associated without ordinary chemical union but through complete enclosure of gas molecules in a framework of water molecules linked together by hydrogen bonds. The clathrates are important in the following applications: the pipeline blockage in natural gas industry, potential energy source in the form of natural hydrates present in ocean bottom, and the CO2 separation and storage. In this study, we have modified an analytical solid-liquid-vapor equation of state (EoS [A. Yokozeki, Fluid Phase Equil. 222–223 (2004] to improve its ability for modeling the phase equilibria of clathrates. The EoS can predict the formation conditions for CO2- and CH4-hydrates. It will be used as an initial estimate for a more complicated hydrate model based on the fundamental EoSs for fluid phases.

Characterization of van der Waals type bimodal,- lambda,- meta- and spinodal phase transitions in liquid mixtures, solid suspensions and thin films.

Science.gov (United States)

Rosenholm, Jarl B

2018-03-01

The perfect gas law is used as a reference when selecting state variables (P, V, T, n) needed to characterize ideal gases (vapors), liquids and solids. Van der Waals equation of state is used as a reference for models characterizing interactions in liquids, solids and their mixtures. Van der Waals loop introduces meta- and unstable states between the observed gas (vapor)-liquid P-V transitions at low T. These intermediate states are shown to appear also between liquid-liquid, liquid-solid and solid-solid phase transitions. First-order phase transitions are characterized by a sharp discontinuity of first-order partial derivatives (P, S, V) of Helmholtz and Gibbs free energies. Second-order partial derivatives (K T , B, C V , C P , E) consist of a static contribution relating to second-order phase transitions and a relaxation contribution representing the degree of first-order phase transitions. Bimodal (first-order) and spinodal (second-order) phase boundaries are used to separate stable phases from metastable and unstable phases. The boundaries are identified and quantified by partial derivatives of molar Gibbs free energy or chemical potentials with respect to P, S, V and composition (mole fractions). Molecules confined to spread Langmuir monolayers or adsorbed Gibbs monolayers are characterized by equation of state and adsorption isotherms relating to a two-dimensional van der Waals equation of state. The basic work of two-dimensional wetting (cohesion, adsorption, spreading, immersion), have to be adjusted by a horizontal surface pressure in the presence of adsorbed vapor layers. If the adsorption is extended to liquid films a vertical surface pressure (Π) may be added to account for the lateral interaction, thus restoring PV = ΠAh dependence of thin films. Van der Waals attraction, Coulomb repulsion and structural hydration forces contribute to the vertical surface pressure. A van der Waals type coexistence of ordered (dispersed) and disordered

Development of Epitaxial GaN Films for RF Communications, Phase I

Data.gov (United States)

National Aeronautics and Space Administration — The primary objective of this SBIR is to develop epitaxial GaN films with threading dislocation density less than 10^6 cm^-2. We propose an innovative approach...

Rapid estimate of solid volume in large tuff cores using a gas pycnometer

Energy Technology Data Exchange (ETDEWEB)

Thies, C. [ed.; Geddis, A.M.; Guzman, A.G. [and others

1996-09-01

A thermally insulated, rigid-volume gas pycnometer system has been developed. The pycnometer chambers have been machined from solid PVC cylinders. Two chambers confine dry high-purity helium at different pressures. A thick-walled design ensures minimal heat exchange with the surrounding environment and a constant volume system, while expansion takes place between the chambers. The internal energy of the gas is assumed constant over the expansion. The ideal gas law is used to estimate the volume of solid material sealed in one of the chambers. Temperature is monitored continuously and incorporated into the calculation of solid volume. Temperature variation between measurements is less than 0.1{degrees}C. The data are used to compute grain density for oven-dried Apache Leap tuff core samples. The measured volume of solid and the sample bulk volume are used to estimate porosity and bulk density. Intrinsic permeability was estimated from the porosity and measured pore surface area and is compared to in-situ measurements by the air permeability method. The gas pycnometer accommodates large core samples (0.25 m length x 0.11 m diameter) and can measure solid volume greater than 2.20 cm{sup 3} with less than 1% error.

Greenhouse gas emissions from solid waste in Beijing: The rising trend and the mitigation effects by management improvements.

Science.gov (United States)

Yu, Yongqiang; Zhang, Wen

2016-04-01

Disposal of solid waste poses great challenges to city managements. Changes in solid waste composition and disposal methods, along with urbanisation, can certainly affect greenhouse gas emissions from municipal solid waste. In this study, we analysed the changes in the generation, composition and management of municipal solid waste in Beijing. The changes of greenhouse gas emissions from municipal solid waste management were thereafter calculated. The impacts of municipal solid waste management improvements on greenhouse gas emissions and the mitigation effects of treatment techniques of greenhouse gas were also analysed. Municipal solid waste generation in Beijing has increased, and food waste has constituted the most substantial component of municipal solid waste over the past decade. Since the first half of 1950s, greenhouse gas emission has increased from 6 CO2-eq Gg y(-1)to approximately 200 CO2-eq Gg y(-1)in the early 1990s and 2145 CO2-eq Gg y(-1)in 2013. Landfill gas flaring, landfill gas utilisation and energy recovery in incineration are three techniques of the after-emission treatments in municipal solid waste management. The scenario analysis showed that three techniques might reduce greenhouse gas emissions by 22.7%, 4.5% and 9.8%, respectively. In the future, if waste disposal can achieve a ratio of 4:3:3 by landfill, composting and incineration with the proposed after-emission treatments, as stipulated by the Beijing Municipal Waste Management Act, greenhouse gas emissions from municipal solid waste will decrease by 41%. © The Author(s) 2016.

Gas-Phase Thermolyses

DEFF Research Database (Denmark)

Carlsen, Lars; Egsgaard, Helge

1982-01-01

The unimolecular gas-phase thermolyses of 1,2,3-oxadithiolan 2-oxide and thiiran 1-oxide have been studied by the flash vacuum thermolysis–field ionization mass spectrometry (f.v.t.–f.i.m.s.) technique in the temperature range from 1 043 to 1 404 K. The reactions are rationalized in terms of sulp...

A headspace solid-phase microextraction procedure coupled with gas chromatography-mass spectrometry for the analysis of volatile polycyclic aromatic hydrocarbons in milk samples

Energy Technology Data Exchange (ETDEWEB)

Aguinaga, N.; Campillo, N.; Vinas, P.; Hernandez-Cordoba, M. [University of Murcia, Department of Analytical Chemistry, Faculty of Chemistry, Murcia (Spain)

2008-06-15

A sensitive and solvent-free method for the determination of ten polycyclic aromatic hydrocarbons, namely, naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo[a]anthracene and chrysene, with up to four aromatic rings, in milk samples using headspace solid-phase microextraction and gas chromatography-mass spectrometry detection has been developed. A polydimethylsiloxane-divinylbenzene fiber was chosen and used at 75 C for 60 min. Detection limits ranging from 0.2 to 5 ng L{sup -1} were attained at a signal-to-noise ratio of 3, depending on the compound and the milk sample under analysis. The proposed method was applied to ten different milk samples and the presence of six of the analytes studied in a skimmed milk with vegetal fiber sample was confirmed. The reliability of the procedure was verified by analyzing two different certified reference materials and by recovery studies. (orig.)