Three-phase boundary length in solid-oxide fuel cells: A mathematical model

Energy Technology Data Exchange (ETDEWEB)

Janardhanan, Vinod M. [Institutefor Chemical Technology and Polymer Chemistry, University of Karlsruhe (TH), Kaiserstr. 12, D-76128 Karlsruhe (Germany); Heuveline, Vincent; Deutschmann, Olaf [Institute for Applied and Numerical Mathematics, University of Karlsruhe (TH), Kaiserstr. 12, D-76128 Karlsruhe (Germany)

2008-03-15

A mathematical model to calculate the volume specific three-phase boundary length in the porous composite electrodes of solid-oxide fuel cell is presented. The model is exclusively based on geometrical considerations accounting for porosity, particle diameter, particle size distribution, and solids phase distribution. Results are presented for uniform particle size distribution as well as for non-uniform particle size distribution. (author)

Three-phase boundary length in solid-oxide fuel cells: A mathematical model

Science.gov (United States)

Janardhanan, Vinod M.; Heuveline, Vincent; Deutschmann, Olaf

A mathematical model to calculate the volume specific three-phase boundary length in the porous composite electrodes of solid-oxide fuel cell is presented. The model is exclusively based on geometrical considerations accounting for porosity, particle diameter, particle size distribution, and solids phase distribution. Results are presented for uniform particle size distribution as well as for non-uniform particle size distribution.

Lanthanum gallate and ceria composite as electrolyte for solid oxide fuel cells

Energy Technology Data Exchange (ETDEWEB)

Li Shuai, E-mail: shuail@kth.s [Department of Materials Science and Engineering, School of Industrial Engineering and Management, Royal Institute of Technology, SE 10044 Stockholm (Sweden); Li Zhicheng [School of Materials Science and Engineering, Central South University, 410083 Changsha, Hunan (China); Bergman, Bill [Department of Materials Science and Engineering, School of Industrial Engineering and Management, Royal Institute of Technology, SE 10044 Stockholm (Sweden)

2010-03-04

The composite of doped lanthanum gallate (La{sub 0.9}Sr{sub 0.1}Ga{sub 0.8}Mg{sub 0.2}O{sub 2.85}, LSGM) and doped ceria (Ce{sub 0.8}Sm{sub 0.2}O{sub 1.9}, CSO) was investigated as an electrolyte for solid oxide fuel cell (SOFC). The LSGM-CSO composite was examined by X-ray diffraction (XRD) and impedance spectroscopy. It was found that the sintered LSGM-CSO composite contains mainly fluorite CeO{sub 2} phase and a minority impurity phase, Sm{sub 3}Ga{sub 5}O{sub 12}. The LSGM-CSO composite electrolyte shows a small grain boundary response in the impedance spectroscopy as compared to LSGM and CSO pellets. The composite electrolyte exhibits the highest conductivity in the temperature range of 250-600 {sup o}C, compared to LSGM and CSO. The LSGM-CSO composite can be expected to be an attractive intermediate temperature electrolyte material for solid oxide fuel cells.

The role of solid-solid phase transitions in mantle convection

Science.gov (United States)

Faccenda, Manuele; Dal Zilio, Luca

2017-01-01

With changing pressure and temperature conditions, downwelling and upwelling crustal and mantle rocks experience several solid-solid phase transitions that affect the mineral physical properties owing to structural changes in the crystal lattice and to the absorption or release of latent heat. Variations in density, together with phase boundary deflections related to the non-null reaction slope, generate important buoyancy forces that add to those induced by thermal perturbations. These buoyancy forces are proportional to the density contrast between reactant and product phases, their volume fraction, the slope and the sharpness of the reaction, and affect the style of mantle convection depending on the system composition. In a homogeneous pyrolitic mantle there is little tendency for layered convection, with slabs that may stagnate in the transition zone because of the positive buoyancy caused by post-spinel and post-ilmenite reactions, and hot plumes that are accelerated by phase transformations in the 600-800 km depth range. By adding chemical and mineralogical heterogeneities as on Earth, phase transitions introduce bulk rock and volatiles filtering effects that generate a compositional gradient throughout the entire mantle, with levels that are enriched or depleted in one or more of these components. Phase transitions often lead to mechanical softening or hardening that can be related to a different intrinsic mechanical behaviour and volatile solubility of the product phases, the heating or cooling associated with latent heat, and the transient grain size reduction in downwelling cold material. Strong variations in viscosity would enhance layered mantle convection, causing slab stagnation and plume ponding. At low temperatures and relatively dry conditions, reactions are delayed due to the sluggish kinetics, so that non-equilibrium phase aggregates can persist metastably beyond the equilibrium phase boundary. Survival of low-density metastable olivine

Study on paraffin/expanded graphite composite phase change thermal energy storage material

International Nuclear Information System (INIS)

Zhang Zhengguo; Fang Xiaoming

2006-01-01

A paraffin/expanded graphite composite phase change thermal energy storage material was prepared by absorbing the paraffin into an expanded graphite that has an excellent absorbability. In such a composite, the paraffin serves as a latent heat storage material and the expanded graphite acts as the supporting material, which prevents leakage of the melted paraffin from its porous structure due to the capillary and surface tension forces. The inherent structure of the expanded graphite did not change in the composite material. The solid-liquid phase change temperature of the composite PCM was the same as that of the paraffin, and the latent heat of the paraffin/expanded graphite composite material was equivalent to the calculated value based on the mass ratio of the paraffin in the composite. The heat transfer rate of the paraffin/expanded graphite composite was obviously higher than that of the paraffin due to the combination with the expanded graphite that had a high thermal conductivity. The prepared paraffin/expanded graphite composite phase change material had a large thermal storage capacity and improved thermal conductivity and did not experience liquid leakage during its solid-liquid phase change

Features of solid solutions composition in magnesium with yttrium alloys

International Nuclear Information System (INIS)

Drits, M.E.; Rokhlin, L.L.; Tarytina, I.E.

1983-01-01

Additional data on features of yttrium solid solutions composition in magnesium in the course of their decomposition investigation in the case of aging are obtianed. The investigation has been carried out on the base of a binary magnesium-yttrium alloy the composition of which has been close to maximum solubility (at eutectic temperature) and magnesium-yttrium alloys additionally doped with zinc. It is shown that higher yttrium solubility in solid magnesium than it has been expected, issueing from the difference in atomic radii of these metals indicates electron yttrium-magnesium atoms interaction. In oversaturated magnesium-yttrium solid solutions at earlier decomposition stages Mg 3 Cd type ordering is observed. At aging temperatures up to 250 deg C and long exposures corresponding to highest strengthening in oversaturated magnesium yttrium solid solutions a rhombic crystal lattice phase with three symmetric orientations is formed

Municipal solid waste composition determination supporting the integrated solid waste management system in the island of Crete

International Nuclear Information System (INIS)

Gidarakos, E.; Havas, G.; Ntzamilis, P.

2006-01-01

A one-year survey was conducted in the greater region of Crete (located at the lower region of the Aegean Sea) for the purpose of identifying waste composition (including chemical and physical characterization), as well as any seasonal variation. The investigation was carried out repeatedly at seven landfills and one transfer station in Crete, in four phases. Each sampling phase corresponded to a season (autumn, winter, spring, summer). ASTM D5231-92(2003) standard method and RCRA Waste Sampling Draft Technical Guidance were used. Hand sorting was used for classifying the collected wastes into the following categories: plastics, paper, metals, aluminium, leather-wood-textiles-rubbers, organic wastes, non-combustibles and miscellaneous. Further analysis included proximate and ultimate analysis of combustible materials. Metals such as lead, cadmium and mercury were also investigated. The results show that there has been a significant decrease of organic wastes during the last decade due to the increase of packaging materials, as a result of a change in consumption patterns. Three main waste categories were determined: organic wastes, paper and plastics, which combined represent 76% of the total waste in Crete. Furthermore, a high fraction of glass and a seasonal variation of aluminium indicate a strong correlation of waste composition with certain human activities, such as tourism. There is also a variation between the municipal solid waste (MSW) composition in the region of Crete (2003-2004) and MSW composition suggested in the National Solid Waste Planning (2000) [National Solid Waste Planning, 2000. Completion and particularization of Common Ministerial Act 113944//1944/1997: National Solid Waste Planning, June 2000]. The results of this survey are to be utilized by the regional solid waste authorities in order to establish an integrated waste treatment site, capable of fulfilling the regional waste management demands

Municipal solid waste composition determination supporting the integrated solid waste management system in the island of Crete.

Science.gov (United States)

Gidarakos, E; Havas, G; Ntzamilis, P

2006-01-01

A one-year survey was conducted in the greater region of Crete (located at the lower region of the Aegean Sea) for the purpose of identifying waste composition (including chemical and physical characterization), as well as any seasonal variation. The investigation was carried out repeatedly at seven landfills and one transfer station in Crete, in four phases. Each sampling phase corresponded to a season (autumn, winter, spring, summer). ASTM D5231-92(2003) standard method and RCRA Waste Sampling Draft Technical Guidance were used. Hand sorting was used for classifying the collected wastes into the following categories: plastics, paper, metals, aluminium, leather-wood-textiles-rubbers, organic wastes, non-combustibles and miscellaneous. Further analysis included proximate and ultimate analysis of combustible materials. Metals such as lead, cadmium and mercury were also investigated. The results show that there has been a significant decrease of organic wastes during the last decade due to the increase of packaging materials, as a result of a change in consumption patterns. Three main waste categories were determined: organic wastes, paper and plastics, which combined represent 76% of the total waste in Crete. Furthermore, a high fraction of glass and a seasonal variation of aluminium indicate a strong correlation of waste composition with certain human activities, such as tourism. There is also a variation between the municipal solid waste (MSW) composition in the region of Crete (2003-2004) and MSW composition suggested in the National Solid Waste Planning (2000) [National Solid Waste Planning, 2000. Completion and particularization of Common Ministerial Act 113944//1944/1997: National Solid Waste Planning, June 2000]. The results of this survey are to be utilized by the regional solid waste authorities in order to establish an integrated waste treatment site, capable of fulfilling the regional waste management demands.

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)

New Approaches in Soil Organic Matter Fluorescence; A Solid Phase Fluorescence Approach

Science.gov (United States)

Bowman, M. M.; Sanclements, M.; McKnight, D. M.

2017-12-01

Fluorescence spectroscopy is a well-established technique to investigate the composition of organic matter in aquatic systems and is increasingly applied to soil organic matter (SOM). Current methods require that SOM be extracted into a liquid prior to analysis by fluorescence spectroscopy. Soil extractions introduce an additional layer of complexity as the composition of the organic matter dissolved into solution varies based upon the selected extractant. Water is one of the most commonly used extractant, but only extracts the water-soluble fraction of the SOM with the insoluble soil organic matter fluorescence remaining in the soil matrix. We propose the use of solid phase fluorescence on whole soils as a potential tool to look at the composition of organic matter without the extraction bias and gain a more complete understand of the potential for fluorescence as a tool in terrestrial studies. To date, the limited applications of solid phase fluorescence have ranged from food and agriculture to pharmaceutical with no clearly defined methods and limitations available. We are aware of no other studies that use solid phase fluorescence and thus no clear methods to look at SOM across a diverse set of soil types and ecosystems. With this new approach to fluorescence spectroscopy there are new challenges, such as blank correction, inner filter effect corrections, and sample preparation. This work outlines a novel method for analyzing soil organic matter using solid phase fluorescence across a wide range of soils collected from the National Ecological Observatory Network (NEON) eco-domains. This method has shown that organic matter content in soils must be diluted to 2% to reduce backscattering and oversaturation of the detector in forested soils. In mineral horizons (A) there is observed quenching of the humic-like organic matter, which is likely a result of organo-mineral complexation. Finally, we present preliminary comparisons between solid and liquid phase

Gibbs Energy Modeling of Digenite and Adjacent Solid-State Phases

Science.gov (United States)

Waldner, Peter

2017-08-01

All sulfur potential and phase diagram data available in the literature for solid-state equilibria related to digenite have been assessed. Thorough thermodynamic analysis at 1 bar total pressure has been performed. A three-sublattice approach has been developed to model the Gibbs energy of digenite as a function of composition and temperature using the compound energy formalism. The Gibbs energies of the adjacent solid-state phases covelitte and high-temperature chalcocite are also modeled treating both sulfides as stoichiometric compounds. The novel model for digenite offers new interpretation of experimental data, may contribute from a thermodynamic point of view to the elucidation of the role of copper species within the crystal structure and allows extrapolation to composition regimes richer in copper than stoichiometric digenite Cu2S. Preliminary predictions into the ternary Cu-Fe-S system at 1273 K (1000 °C) using the Gibbs energy model of digenite for calculating its iron solubility are promising.

Recent developments and future trends in solid phase microextraction techniques towards green analytical chemistry.

Science.gov (United States)

Spietelun, Agata; Marcinkowski, Łukasz; de la Guardia, Miguel; Namieśnik, Jacek

2013-12-20

Solid phase microextraction find increasing applications in the sample preparation step before chromatographic determination of analytes in samples with a complex composition. These techniques allow for integrating several operations, such as sample collection, extraction, analyte enrichment above the detection limit of a given measuring instrument and the isolation of analytes from sample matrix. In this work the information about novel methodological and instrumental solutions in relation to different variants of solid phase extraction techniques, solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE) and magnetic solid phase extraction (MSPE) is presented, including practical applications of these techniques and a critical discussion about their advantages and disadvantages. The proposed solutions fulfill the requirements resulting from the concept of sustainable development, and specifically from the implementation of green chemistry principles in analytical laboratories. Therefore, particular attention was paid to the description of possible uses of novel, selective stationary phases in extraction techniques, inter alia, polymeric ionic liquids, carbon nanotubes, and silica- and carbon-based sorbents. The methodological solutions, together with properly matched sampling devices for collecting analytes from samples with varying matrix composition, enable us to reduce the number of errors during the sample preparation prior to chromatographic analysis as well as to limit the negative impact of this analytical step on the natural environment and the health of laboratory employees. Copyright © 2013 Elsevier B.V. All rights reserved.

Solid polymer composite electrolytes for PEMFC

Energy Technology Data Exchange (ETDEWEB)

Zaidi, S M.J.; Mikhailenko, S D; Kaliaguine, S

1998-07-01

Composite electrolyte membranes for fuel cell technology were prepared from solid state proton conductors and polymer binders. The polymers were partially sulfonated and non-sulfonated polysulfone (PS), porous polyetherimide (PEI) and polymethylmethacrylate (PMMA). As proton conductors H-chabazite, tungstophosphoric acid and its Na-salt and non-stoichiometric boron phosphate were employed. All membranes prepared using sulfonated PS as a binder with sulfonation degree higher than 50% were found to be mechanically unstable. They possess however reasonably high conductivity up to 6{times}10{sup {minus}3} S/cm. Introducing the tungstophosphoric acid (TPA) into the nonsulfonated porous PS makes possible to obtain strong and flexible membranes with s=4{times}10{sup {minus}3} S/cm, while use of boron phosphate in that case results in the conductivity of about 10{sup {minus}5} S/cm. Porous PEI impregnated with aqueous solution of TPA retains its original tensile strength and exhibited the conductivity s=2{times}10{sup {minus}4} S/cm. It however fell to 3{times}10{sup {minus}5} S/cm when the binder was modified with 2% of propionic acid, which caused a decrease in polymer pore size. Incorporation of the sodium acid salt of TPA into PEI allows one to obtain a composite with reasonably good mechanical properties and a conductivity of ca 10{sup {minus}5} S/cm for membranes prepared by the cast method. Using the phase inversion technique for preparation of the membranes of the same composition makes possible to increase their conductivity up to 10{sup {minus}4} S/cm. When boron phosphate was used in lieu of TPA salt the conductivity obtained is still higher reaching 3{times}10{sup {minus}5} and 3{times}10{sup {minus}4} S/cm for membranes prepared by cast and phase inversion techniques respectively. The PMMA based membranes were mechanically stable even when a solid content reached 55wt.%. Among PMMA membranes the highest conductivity of 10{sup {minus}3} S/cm was registered for

Phase composition and microstructure of WC-Co alloys obtained by selective laser melting

Science.gov (United States)

Khmyrov, Roman S.; Shevchukov, Alexandr P.; Gusarov, Andrey V.; Tarasova, Tatyana V.

2018-03-01

Phase composition and microstructure of initial WC, BK8 (powder alloy 92 wt.% WC-8 wt.% Co), Co powders, ball-milled powders with four different compositions (1) 25 wt.% WC-75 wt.% Co, (2) 30 wt.% BK8-70 wt.% Co, (3) 50 wt.% WC-50 wt.% Co, (4) 94 wt.% WC-6 wt.% Co, and bulk alloys obtained by selective laser melting (SLM) from as-milled powders in as-melted state and after heat treatment were investigated by scanning electron microscopy and X-ray diffraction analysis. Initial and ball-milled powders consist of WC, hexagonal α-Co and face-centered cubic β-Co. The SLM leads to the formation of major new phases W3Co3C, W4Co2C and face-centered cubic β-Co-based solid solution. During the heat treatment, there occurs partial decomposition of the face-centered cubic β-Co-based solid solution with the formation of W2C and hexagonal α-Co solid solution. The microstructure of obtained bulk samples, in general, corresponds to the observed phase composition.

Final Report For The Initial Solid Phase Characterization Of The 2011 Grab Samples And Composite For The C-109 Hard Heel Study

International Nuclear Information System (INIS)

Page, J.S.; Cooke, G.A.; Pestovich, J.A.

2011-01-01

On May 3, 2011, solid phase characterization subsamples were taken from six of the eight grab samples that had been collected from tank 241-C-109 in April, 2011 and delivered to the 222-S Laboratory. These subsamples were characterized in order to guide the creation of the composite for the C-109 hard heel study. Visual observation showed that there was a large variability in the physical characteristics of the eight individual grab samples. Several of the grab samples consisted of 'stone-like' cobbles (several > 25 mm in diameter) while the other grab samples were of a finer granular composition referred to as 'bulk material'. Half of the six subsamples taken for this initial SPC were of crushed cobbles and half were of the bulk material. Scanning electron microscopy was performed on all six subsamples, and X-ray diffraction was performed on all three of the 'bulk material' samples and one of the crushed cobble samples. The crushed cobbles were found to be composed primarily of gibbsite (Al(OHh) 3 ). Analysis by X-ray diffraction indicated gibbsite to be the only crystalline phase detected, and scanning electron microscopy showed the crushed cobbles to consist primarily of aggregates of euhedral to subhedral gibbsite crystals that were 20 to 100 μm in size. The aggregates, having a moderate amount of pore space, were cemented primarily by recrystallized gibbsite making them resistant to crushing. The bulk material consisted of coarse to fine-grained pebble-sized (2 to 20 mm) particles. The X-ray diffraction analysis showed them to be a mixture of natrophosphate (Na 7 (PO 4 ) 2 F·19(H 2 O)) and gibbsite crystals in varying amounts in each of the three subsamples (i.e., some grab samples were primarily natrophosphate while others were mixed with gibbsite). The scanning electron microscopy analysis of the bulk material showed the crystals to be euhedral to anhedral (rounded) in shape. Trace phases, too minor to be detected by XRD, were observed in the SEM analysis

Structures of the particles of the condensed dispersed phase in solid fuel combustion products plasma

International Nuclear Information System (INIS)

Samaryan, A.A.; Chernyshev, A.V.; Nefedov, A.P.; Petrov, O.F.; Fortov, V.E.; Mikhailov, Yu.M.; Mintsev, V.B.

2000-01-01

The results of experimental investigations of a type of dusty plasma which has been least studied--the plasma of solid fuel combustion products--were presented. Experiments to determine the parameters of the plasma of the combustion products of synthetic solid fuels with various compositions together with simultaneous diagnostics of the degree of ordering of the structures of the particles of the dispersed condensed phase were performed. The measurements showed that the charge composition of the plasma of the solid fuels combustion products depends strongly on the easily ionized alkali-metal impurities which are always present in synthetic fuel in one or another amount. An ordered arrangement of the particles of a condensed dispersed phase in structures that form in a boundary region between the high-temperature and condensation zones was observed for samples of aluminum-coated solid fuels with a low content of alkali-metal impurities

Oxygen exchange and transport in dual phase ceramic composite electrodes.

Science.gov (United States)

Druce, John; Téllez, Helena; Ishihara, Tatsumi; Kilner, John A

2015-01-01

Composites consisting of a perovskite-based electronic or mixed conductor with a fluorite-structured ionic conductor are often used as electrodes in solid oxide electrochemical energy conversion devices. After sintering the materials, there is often evidence for inter-reaction between the two phases, or inter-diffusion of cations or impurities between the two phases. We studied the (18)O exchange properties of a composite consisting of CGO and LSCF in a 50 : 50 ratio. High resolution ToF-SIMS mapping reveals that the (18)O fraction at the very outer surface of grains of the CGO phase is much higher than expected from D* and k* values for the single-phase parent material. Surface compositional analysis by ToF-SIMS and low energy ion scattering (LEIS) spectroscopy suggests that the surfaces of the CGO grains in the composite do not show the impurities which typically segregate to the surface in single-phase CGO. Thus, the "cleaning" of impurities from the CGO surface by dissolution into the perovskite phase may be one explanation for the apparent enhanced surface exchange for CGO in these composites.

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.

Investigation into isomolar series of Al(NO3)3, Na3VO4 solution mixture and composition of solid phases

International Nuclear Information System (INIS)

Chernysh, L.F.; Nakhodnova, A.P.; Makarova, R.A.

1979-01-01

Conducted is investigation of properties of isomolar series of aluminium nitrate and sodiUm vanadate solutions at pH of the latter 12.5; 10.0; 7.0 and the temperature of 25 deg C using the methods of pH-metry, conductometry, ''seeming'' volume of precipitations, residual concentration of aluminium and vanadium. It is shown, that the composition property diagram of the system investigated does not reflect the true composition of solid-phase products of the reaction, which depends on the component ratio in solution. Bottom phases of isomolar series are mainly heterogeneous. At the excess of sodium vanadate solution and its high pH values conditions for the basic salt formation are created. At pH of the Na 3 VO 4 solution of 12.5 and 10.0 and Al(NO 3 ) 3 : Na 3 VO 4 ratios 4:6 and 3:7 respectively obtained are the basic aluminium vanadates of the (AlOH) 3 (VO 4 ) 2 x 7.5H 2 O and (AlOH) 2 V 2 O 7 x5H 2 O composition, some of their physicochemical properties being investigated

A functional form-stable phase change composite with high efficiency electro-to-thermal energy conversion

International Nuclear Information System (INIS)

Wu, Wenhao; Huang, Xinyu; Li, Kai; Yao, Ruimin; Chen, Renjie; Zou, Ruqiang

2017-01-01

Graphical abstract: The thermal conductivity of PU was enhanced to 43 times of the pristine value by encapsulation in a PGF, PU@PGF can be used for highly efficient electro-to-heat energy conversion and storage with the highest energy storage efficiency up to 85%. - Highlights: • The composite exhibits an in-situ solid-solid phase change behavior. • The enthalpy of polyurethane is enhanced within the matrix. • The thermal conductivity of the composite is 43 times as much as that of the polyurethane. • Supercooling of polyurethane is greatly reduced. • The composite is applied to cold protection as a wear layer. - Abstract: A novel solid-to-solid phase change composite brick was prepared by combination of polyurethane (PU) and pitch-based graphite foam (PGF). The carbonaceous support, which can be used for mass production, not only greatly improves the thermal conductivity but promote electro-to-heat conversion efficiency of organic phase change materials (PCMs). Our composite retained the enthalpy of PCM and exhibited a greatly reduced supercooling temperature. The novel composite was investigated by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and scanning electron microscope (SEM). The enthalpy of polyurethane has increased about 8.6% after infiltrating into graphite foam. The composite was very stable during thermal cycle test, and the electro-to-heat conversion efficiency achieves to 85% at lower voltages (1.5–1.8 V), which can vastly reduce energy consumption. The as-prepared composite was used in a wear layer to test its performance comparing with normal fabric.

Fabrication of metal matrix composite by semi-solid powder processing

Energy Technology Data Exchange (ETDEWEB)

Wu, Yufeng [Iowa State Univ., Ames, IA (United States)

2011-01-01

Various metal matrix composites (MMCs) are widely used in the automotive, aerospace and electrical industries due to their capability and flexibility in improving the mechanical, thermal and electrical properties of a component. However, current manufacturing technologies may suffer from insufficient process stability and reliability and inadequate economic efficiency and may not be able to satisfy the increasing demands placed on MMCs. Semi-solid powder processing (SPP), a technology that combines traditional powder metallurgy and semi-solid forming methods, has potential to produce MMCs with low cost and high efficiency. In this work, the analytical study and experimental investigation of SPP on the fabrication of MMCs were explored. An analytical model was developed to understand the deformation mechanism of the powder compact in the semi-solid state. The densification behavior of the Al6061 and SiC powder mixtures was investigated with different liquid fractions and SiC volume fractions. The limits of SPP were analyzed in terms of reinforcement phase loading and its impact on the composite microstructure. To explore adoption of new materials, carbon nanotube (CNT) was investigated as a reinforcing material in aluminum matrix using SPP. The process was successfully modeled for the mono-phase powder (Al6061) compaction and the density and density distribution were predicted. The deformation mechanism at low and high liquid fractions was discussed. In addition, the compaction behavior of the ceramic-metal powder mixture was understood, and the SiC loading limit was identified by parametric study. For the fabrication of CNT reinforced Al6061 composite, the mechanical alloying of Al6061-CNT powders was first investigated. A mathematical model was developed to predict the CNT length change during the mechanical alloying process. The effects of mechanical alloying time and processing temperature during SPP were studied on the mechanical, microstructural and

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

Science.gov (United States)

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

2018-01-01

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

Tetragonal-cubic phase boundary in nanocrystalline ZrO2-Y2O3 solid solutions synthesized by gel-combustion

International Nuclear Information System (INIS)

Fabregas, Ismael O.; Craievich, Aldo F.; Fantini, Marcia C.A.; Millen, Ricardo P.; Temperini, Marcia L.A.; Lamas, Diego G.

2011-01-01

Research highlights: → Gel-combustion synthesis yields compositionally homogeneous, single-phased ZrO 2 -Y 2 O 3 nanopowders, that exhibit the presence at room temperature of three different phases depending on Y 2 O 3 content, namely two tetragonal forms (t' and t'') and the cubic phase. → Phase identification can be achieved by synchrotron XPD (SXPD) and Raman spectroscopy since the tetragonal forms and the cubic phase can be distinguished by these techniques. → The crystallographic features of ZrO 2 -Y 2 O 3 nanopowders were determined by SXPD. They are similar to those reported by Yashima and coworkers for compositionally homogeneous materials containing larger (micro)crystals. However, the lattice parameters are slightly different and the axial ratios c/a of our t' samples are smaller than those reported by these authors. → Compositional t'/t'' and t''/cubic phase boundaries are located at (9 ± 1) and (10.5 ± 0.5) mol% Y 2 O 3 , respectively. → For the whole series of nanocrystalline ZrO 2 -Y 2 O 3 solid solutions studied in the present work, no evidences of the presence of a mixture of phases - as reported by Yashima and coworkers for microcrystalline solid solutions - were detected. - Abstract: By means of synchrotron X-ray powder diffraction (SXPD) and Raman spectroscopy, we have detected, in a series of nanocrystalline and compositionally homogeneous ZrO 2 -Y 2 O 3 solid solutions, the presence at room temperature of three different phases depending on Y 2 O 3 content, namely two tetragonal forms and the cubic phase. The studied materials, with average crystallite sizes within the range 7-10 nm, were synthesized by a nitrate-citrate gel-combustion process. The crystal structure of these phases was also investigated by SXPD. The results presented here indicate that the studied nanocrystalline ZrO 2 -Y 2 O 3 solid solutions exhibit the same phases reported in the literature for compositionally homogeneous materials containing larger (micro

Characterization of rhamnolipids by liquid chromatography/mass spectrometry after solid-phase extraction.

Science.gov (United States)

Behrens, Beate; Engelen, Jeannine; Tiso, Till; Blank, Lars Mathias; Hayen, Heiko

2016-04-01

Rhamnolipids are surface-active agents with a broad application potential that are produced in complex mixtures by bacteria of the genus Pseudomonas. Analysis from fermentation broth is often characterized by laborious sample preparation and requires hyphenated analytical techniques like liquid chromatography coupled to mass spectrometry (LC-MS) to obtain detailed information about sample composition. In this study, an analytical procedure based on chromatographic method development and characterization of rhamnolipid sample material by LC-MS as well as a comparison of two sample preparation methods, i.e., liquid-liquid extraction and solid-phase extraction, is presented. Efficient separation was achieved under reversed-phase conditions using a mixed propylphenyl and octadecylsilyl-modified silica gel stationary phase. LC-MS/MS analysis of a supernatant from Pseudomonas putida strain KT2440 pVLT33_rhlABC grown on glucose as sole carbon source and purified by solid-phase extraction revealed a total of 20 congeners of di-rhamnolipids, mono-rhamnolipids, and their biosynthetic precursors 3-(3-hydroxyalkanoyloxy)alkanoic acids (HAAs) with different carbon chain lengths from C8 to C14, including three rhamnolipids with uncommon C9 and C11 fatty acid residues. LC-MS and the orcinol assay were used to evaluate the developed solid-phase extraction method in comparison with the established liquid-liquid extraction. Solid-phase extraction exhibited higher yields and reproducibility as well as lower experimental effort.

Composition and quantification of phases in the solid-state reduction of chromite using SEM-EDX and EPMA-WDS techniques

International Nuclear Information System (INIS)

Johnston, R.F.; Duong, H.V.

1996-01-01

Phase changes in the solid-state reduction of chromite ore ((Mg,Fe)(Fe,Al,Cr) sub 2 O sub 4) with coal have been studied in the temperature range 1OOO degree C to 1400 degree C and EPMA-WDS techniques. EDX mapping of the reduced chromite gave qualitative chemical composition and structural characteristics of the phases. These phases were then quantified by the EPAM-WDS technique. No significant reduction of the chromite ore was seen at 1OOO degree C and 11OO degree C. At 1200 degree C iron was being reduced, resulting in zoning of chromite particles as reduction proceeded. At higher temperatures, chromium was being reduced simultaneously with the iron in the chromite. This was followed by some silicon reduction. Carbon was not found in the chromite grains which suggested that reduction of chromite ore by coal occurs mostly through carbon monoxide as a reaction intermediate. Various ferroalloy phases containing silicon and/or carbon were found and quantified. The slag was found to contain chromium, iron and carbon

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....

Composition and structure of solid-phase carriers of activity in soils of the exclusion zone.; Stroenie i sostav tverdofaznykh nositelej aktivnosti v pochvakh Zony otchuzhdeniya ChAEhS.

Energy Technology Data Exchange (ETDEWEB)

Bondarenko, G N; Dolin, V V; Val` ter, A A; Tikhanov, Eh K [AN Ukrainskoj SSR, Kiev (Ukraine). Inst. Geokhimii i Fiziki Mineralov; [Nauchno-Proizvodstvennoe Ob` ` edinenie Pripyat` , Chernobyl (Ukraine)

1994-12-31

From four different soils in the exclusion Chernobyl zone 35 << hot >> particles were picked out, their radionuclide and substance composition was investigated. To estimate a specific quantity of solid-phase carriers of activity we have calculated a ratio of activities of {sup 144} Ce and {sup 137} Cs in soils to the particles. Substance composition of the << hot >> particles investigated by the methods of electronic microscopy.

CONDENSED MATTER: STRUCTURE, MECHANICAL AND THERMAL PROPERTIES: Molecular Dynamics Study of Stability of Solid Solutions and Amorphous Phase in the Cu-Al System

Science.gov (United States)

Yang, Bin; Lai, Wen-Sheng

2009-06-01

The relative stability of fcc and bcc solid solutions and amorphous phase with different compositions in the Cu-Al system is studied by molecular dynamics simulations with n-body potentials. For Cu1-xAlx alloys, the calculations show that the fcc solid solution has the lowest energies in the composition region with x 0.72, while the bee solid solution has the lowest energies in the central composition range, in agreement with the ball-milling experiments that a single bcc solid solution with 0.30 < x < 0.70 is obtained. The evolution of structures in solid solutions and amorphous phase is studied by the coordination number (CN) and bond-length analysis so as to unveil the underlying physics. It is found that the energy sequence among three phases is determined by the competition in energy change originating from the bond length and CNs (or the number of bonds).

Volatile composition of peppermint (Mentha piperita L.) commercial teas through solid phase extraction.

Science.gov (United States)

Riachi, L G; Abi-Zaid, I E; Moreira, R F A; De Maria, C A B

2012-12-01

Volatiles from aqueous extract of peppermint commercial sachets were investigated through gas chromatography/flame ionization detection (GC/FID) and GC/mass spectrometry (MS). Samples were prepared under similar conditions as in homemade tea. Volatiles were isolated using solid phase extraction method (SPE) with Porapak Q trap followed by desorption with acetone. Estimated mean values for short and medium chain carboxylic acids (C2-C12) and ketones lay in the range of 50-64 microg kg(-1) whilst aliphatic alcohols and acyclic hydrocarbons had values lower than 6 microg kg(-1). The major volatiles were terpenes (275-382 microg kg(-1)) that reached 89 % of the total composition. A total of 16 compounds, among them dodecane, acetoin, acetol, citral, geraniol and octanoic acid have been described by the first time in peppermint tea. These findings could be attributed to the different analytical approach employed, mainly to the use of different extraction/pre-concentration techniques. Given the apparently lower proportion of terpenes in the aqueous extract it may be that the chemical properties of the peppermint essential oil are not entirely reproduced with homemade tea.

Composite electrolyte with proton conductivity for low-temperature solid oxide fuel cell

Energy Technology Data Exchange (ETDEWEB)

Raza, Rizwan, E-mail: razahussaini786@gmail.com [Department of Physics, COMSATS Institute of Information Technology, Lahore 54000 (Pakistan); Department of Energy Technology, Royal Institute of Technology, KTH, Stockholm 10044 (Sweden); Ahmed, Akhlaq; Akram, Nadeem; Saleem, Muhammad; Niaz Akhtar, Majid; Ajmal Khan, M.; Abbas, Ghazanfar; Alvi, Farah; Yasir Rafique, M. [Department of Physics, COMSATS Institute of Information Technology, Lahore 54000 (Pakistan); Sherazi, Tauqir A. [Department of Chemistry, COMSATS Institute of Information Technology, Abbotabad 22060 (Pakistan); Shakir, Imran [Sustainable Energy Technologies (SET) center, College of Engineering, King Saud University, PO-BOX 800, Riyadh 11421 (Saudi Arabia); Mohsin, Munazza [Department of Physics, Lahore College for Women University, Lahore, 54000 (Pakistan); Javed, Muhammad Sufyan [Department of Physics, COMSATS Institute of Information Technology, Lahore 54000 (Pakistan); Department of Applied Physics, Chongqing University, Chongqing 400044 (China); Zhu, Bin, E-mail: binzhu@kth.se, E-mail: zhubin@hubu.edu.cn [Department of Energy Technology, Royal Institute of Technology, KTH, Stockholm 10044 (Sweden); Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials, Faculty of Physics and Electronic Science/Faculty of Computer and Information, Hubei University, Wuhan, Hubei 430062 (China)

2015-11-02

In the present work, cost-effective nanocomposite electrolyte (Ba-SDC) oxide is developed for efficient low-temperature solid oxide fuel cells (LTSOFCs). Analysis has shown that dual phase conduction of O{sup −2} (oxygen ions) and H{sup +} (protons) plays a significant role in the development of advanced LTSOFCs. Comparatively high proton ion conductivity (0.19 s/cm) for LTSOFCs was achieved at low temperature (460 °C). In this article, the ionic conduction behaviour of LTSOFCs is explained by carrying out electrochemical impedance spectroscopy measurements. Further, the phase and structure analysis are investigated by X-ray diffraction and scanning electron microscopy techniques. Finally, we achieved an ionic transport number of the composite electrolyte for LTSOFCs as high as 0.95 and energy and power density of 90% and 550 mW/cm{sup 2}, respectively, after sintering the composite electrolyte at 800 °C for 4 h, which is promising. Our current effort toward the development of an efficient, green, low-temperature solid oxide fuel cell with the incorporation of high proton conductivity composite electrolyte may open frontiers in the fields of energy and fuel cell technology.

Composite electrolyte with proton conductivity for low-temperature solid oxide fuel cell

Science.gov (United States)

Raza, Rizwan; Ahmed, Akhlaq; Akram, Nadeem; Saleem, Muhammad; Niaz Akhtar, Majid; Sherazi, Tauqir A.; Ajmal Khan, M.; Abbas, Ghazanfar; Shakir, Imran; Mohsin, Munazza; Alvi, Farah; Javed, Muhammad Sufyan; Yasir Rafique, M.; Zhu, Bin

2015-11-01

In the present work, cost-effective nanocomposite electrolyte (Ba-SDC) oxide is developed for efficient low-temperature solid oxide fuel cells (LTSOFCs). Analysis has shown that dual phase conduction of O-2 (oxygen ions) and H+ (protons) plays a significant role in the development of advanced LTSOFCs. Comparatively high proton ion conductivity (0.19 s/cm) for LTSOFCs was achieved at low temperature (460 °C). In this article, the ionic conduction behaviour of LTSOFCs is explained by carrying out electrochemical impedance spectroscopy measurements. Further, the phase and structure analysis are investigated by X-ray diffraction and scanning electron microscopy techniques. Finally, we achieved an ionic transport number of the composite electrolyte for LTSOFCs as high as 0.95 and energy and power density of 90% and 550 mW/cm2, respectively, after sintering the composite electrolyte at 800 °C for 4 h, which is promising. Our current effort toward the development of an efficient, green, low-temperature solid oxide fuel cell with the incorporation of high proton conductivity composite electrolyte may open frontiers in the fields of energy and fuel cell technology.

Composite Solid Fuel: Research of Formation Parameters

Directory of Open Access Journals (Sweden)

Tabakaev Roman

2016-01-01

Full Text Available Involving of local low-grade fuels resources in fuel and energy balance is actual question of research in the present. In this paper the possibility of processing low-grade fuel in the solid fuel composite was considered. The aim of the work is to define the optimal parameters for formation of the solid composite fuel. A result of researches determined that dextrin content in the binder allows to obtain solid composite fuel having the highest strength. The drying temperature for the various fuels was determined: for pellets production was 20-80 °C, for briquettes – 20-40 °C.

Electroplating of nanostructured polyaniline-polypyrrole composite coating in a stainless-steel tube for on-line in-tube solid phase microextraction.

Science.gov (United States)

Asiabi, Hamid; Yamini, Yadollah; Seidi, Shahram; Esrafili, Ali; Rezaei, Fatemeh

2015-06-05

In this work, a novel and efficient on-line in-tube solid phase microextraction method followed by high performance liquid chromatography was developed for preconcentration and determination of trace amounts of parabens. A nanostructured polyaniline-polypyrrole composite was electrochemically deposited on the inner surface of a stainless steel tube and used as the extraction phase. Several important factors that influence the extraction efficiency, including type of solid-phase coating, extraction and desorption times, flow rates of the sample solution and eluent, pH, and ionic strength of the sample solution were investigated and optimized. Under the optimal conditions, the limits of detection were in the range of 0.02-0.04 μg L(-1). This method showed good linearity for parabens in the range of 0.07-50 μg L(-1), with coefficients of determination better than 0.998. The intra- and inter-assay precisions (RSD%, n=3) were in the range of 5.9-7.0% and 4.4-5.7% at three concentration levels of 2, 10, and 20 μg L(-1), respectively. The extraction recovery values for the spiked samples were in the acceptable range of 80.3-90.2%. The validated method was successfully applied for analysis of methyl-, ethyl-, and propyl parabens in some water, milk, and juice samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Ductile-phase toughening in V-V3Si in situ composites

International Nuclear Information System (INIS)

Henshall, G.; Strum, M.J.; Bewlay, B.P.; Sutliff, J.A.

1997-01-01

This article describes the room-temperature fracture behavior of ductile-phase-toughened V-V 3 Si in situ composites that were produced by arc melting (AM), cold-crucible induction melting (IM), and cold-crucible directional solidification (DS). Composites were produced containing a wide range of microstructures, interstitial impurity contents, and volume fractions of the ductile V-Si solid solution phase, denoted (V). The fracture toughness of these composites generally increases as the volume fraction of (V) increases, but is strongly influenced by the microstructure, the mechanical properties of the component phases, and the crystallographic orientation of the (V) phase with respect to the maximum principal stress direction. For eutectic composites that have a (V) volume fraction of about 50 pct, the fracture toughness increases with decreasing ''''effective'''' interstitial impurity concentration, [I] = [N] + 1.33 [O] + 9 [H]. As [I] decreases from 1,400 ppm (AM) to 400 ppm (IM), the fracture toughness of the eutectic composites increases from 10 to 20 MPa √m. Further, the fracture toughness of the DS eutectic composites is greater when the crack propagation direction is perpendicular, rather than parallel, to the composite growth direction. These results are discussed in light of conventional ductile-phase bridging theories, which alone cannot fully explain the fracture toughness of V-Si in situ composites

Theoretical study on phase coexistence in ferroelectric solid solutions near the tricritical point

Energy Technology Data Exchange (ETDEWEB)

Lu, Xiaoyan, E-mail: luxy@hit.edu.cn, E-mail: dzk@psu.edu; Li, Hui [Key Lab of Structures Dynamic Behavior and Control of the Ministry of Education, School of Civil Engineering, Harbin Institute of Technology, Harbin 150001 (China); Zheng, Limei [Condensed Matter Science and Technology Institute, Harbin Institute of Technology, Harbin 150001 (China); Cao, Wenwu [Condensed Matter Science and Technology Institute, Harbin Institute of Technology, Harbin 150001 (China); Department of Mathematics and Materials Research Institute, The Pennsylvania State University, University Park, Pennsylvania 16802 (United States)

2015-04-07

Phase coexistence in ferroelectric solid solutions near the tricritical point has been theoretically analyzed by using the Landau-Devonshire theory. Results revealed that different phases having similar potential wells could coexist in a narrow composition range near the tricritical point in the classical Pb(Zr{sub 1−x}Ti{sub x})O{sub 3} system. The potential barrier between potential wells increases with the decrease of temperature. Coexisting phases or different domains of the same phase can produce adaptive strains to maintain atomic coherency at the interfaces or domain walls. Such compatibility strains have influence on the energy potential as well as the stability of relative phases, leading to the appearance of energetically unfavorable monoclinic phases. Those competing and coexisting phases also construct an easy phase transition path with small energy barrier in between, so that very small stimuli can produce large response in compositions near the morphotropic phase boundary, especially near the tricritical point.

Theoretical study on phase coexistence in ferroelectric solid solutions near the tricritical point

International Nuclear Information System (INIS)

Lu, Xiaoyan; Li, Hui; Zheng, Limei; Cao, Wenwu

2015-01-01

Phase coexistence in ferroelectric solid solutions near the tricritical point has been theoretically analyzed by using the Landau-Devonshire theory. Results revealed that different phases having similar potential wells could coexist in a narrow composition range near the tricritical point in the classical Pb(Zr 1−x Ti x )O 3 system. The potential barrier between potential wells increases with the decrease of temperature. Coexisting phases or different domains of the same phase can produce adaptive strains to maintain atomic coherency at the interfaces or domain walls. Such compatibility strains have influence on the energy potential as well as the stability of relative phases, leading to the appearance of energetically unfavorable monoclinic phases. Those competing and coexisting phases also construct an easy phase transition path with small energy barrier in between, so that very small stimuli can produce large response in compositions near the morphotropic phase boundary, especially near the tricritical point

Study on polyethylene glycol/epoxy resin composite as a form-stable phase change material

International Nuclear Information System (INIS)

Fang Yutang; Kang Huiying; Wang Weilong; Liu Hong; Gao Xuenong

2010-01-01

Form-stable polyethylene glycol (PEG)/epoxy resin (EP) composite as a novel phase change material (PCM) was prepared using casting molding method. In this new material, PEG acts as the latent heat storage material and EP polymer serves as the supporting material, which provides structural strength and prevents the leakage of the melted PEG. The structure and morphology of the novel composite were observed using Fourier transformation infrared spectroscope (FTIR) and scanning electronic microscope (SEM). The thermo-mechanical property and transition behavior were characterized by polarizing optical microscope (POM), static thermo-mechanical analysis (TMA) and differential scanning calorimeter (DSC). The experimental results show that, as a result of the physical tangled function of the epoxy resin carrier to the PEG segment, the composite macroscopically presents the solid-solid phase change characteristic.

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

Directory of Open Access Journals (Sweden)

Ireneusz Sowa

2018-03-01

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

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).

Thermal characterization of polymer matrix composites containing microencapsulated paraffin in solid or liquid state

International Nuclear Information System (INIS)

Sari-Bey, Sana; Fois, Magali; Krupa, Igor; Ibos, Laurent; Benyoucef, Boumédiène

2014-01-01

Highlights: • Thermal characterization of PCL/Micronal composites. • Melting enthalpy and heat capacity measured by DSC. • Interest: have measured thermal properties at different temperatures. • Thermophysical properties measurement temperatures chosen outside phase changes. • Characteristics useful to model composites heat transfer for LHTES applications. - Abstract: This work focuses on the study of heat transfer mechanisms in composites materials which may be used for Latent Heat Thermal Energy Storage applications. These composites contain phase change material (PCM) which can absorb and release energy during thermal cycling. PCM’s used here are paraffins microencapsulated in poly(methylmethacrylate); microencapsulation avoids the flow of paraffin when it is in the liquid state. Samples with different paraffin weight fractions and particles shape and distribution were studied in this work. Scanning Electron Microscopy and Differential Scanning Calorimetry were used to determine morphology and perform measurements of phase changes temperatures, enthalpies and heat capacity respectively. Further, a periodic method (DICO) allowed measuring thermal conductivity (λ) and diffusivity (a) of the composites at temperatures below and above of the paraffin phase change from crystalline solid to isotropic liquid

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.

Multivariate Quantification of the Solid State Phase Composition of Co-Amorphous Naproxen-Indomethacin

Directory of Open Access Journals (Sweden)

Andreas Beyer

2015-10-01

Full Text Available To benefit from the optimized dissolution properties of active pharmaceutical ingredients in their amorphous forms, co-amorphisation as a viable tool to stabilize these amorphous phases is of both academic and industrial interest. Reports dealing with the physical stability and recrystallization behavior of co-amorphous systems are however limited to qualitative evaluations based on the corresponding X-ray powder diffractograms. Therefore, the objective of the study was to develop a quantification model based on X-ray powder diffractometry (XRPD, followed by a multivariate partial least squares regression approach that enables the simultaneous determination of up to four solid state fractions: crystalline naproxen, γ-indomethacin, α-indomethacin as well as co-amorphous naproxen-indomethacin. For this purpose, a calibration set that covers the whole range of possible combinations of the four components was prepared and analyzed by XRPD. In order to test the model performances, leave-one-out cross validation was performed and revealed root mean square errors of validation between 3.11% and 3.45% for the crystalline molar fractions and 5.57% for the co-amorphous molar fraction. In summary, even four solid state phases, involving one co-amorphous phase, can be quantified with this XRPD data-based approach.

Solid phase microbial fuel cell (SMFC) for harnessing bioelectricity from composite food waste fermentation: influence of electrode assembly and buffering capacity.

Science.gov (United States)

Mohan, S Venkata; Chandrasekhar, K

2011-07-01

Solid phase microbial fuel cells (SMFC; graphite electrodes; open-air cathode) were designed to evaluate the potential of bioelectricity production by stabilizing composite canteen based food waste. The performance was evaluated with three variable electrode-membrane assemblies. Experimental data depicted feasibility of bioelectricity generation from solid state fermentation of food waste. Distance between the electrodes and presence of proton exchange membrane (PEM) showed significant influence on the power yields. SMFC-B (anode placed 5 cm from cathode-PEM) depicted good power output (463 mV; 170.81 mW/m(2)) followed by SMFC-C (anode placed 5 cm from cathode; without PEM; 398 mV; 53.41 mW/m(2)). SMFC-A (PEM sandwiched between electrodes) recorded lowest performance (258 mV; 41.8 mW/m(2)). Sodium carbonate amendment documented marked improvement in power yields due to improvement in the system buffering capacity. SMFCs operation also documented good substrate degradation (COD, 76%) along with bio-ethanol production. The operation of SMFC mimicked solid-sate fermentation which might lead to sustainable solid waste management practices. Copyright © 2011 Elsevier Ltd. All rights reserved.

Rapid in situ growth of oriented titanium-nickel oxide composite nanotubes arrays coated on a nitinol wire as a solid-phase microextraction fiber coupled to HPLC-UV.

Science.gov (United States)

Zhen, Qi; Zhang, Min; Song, Wenlan; Wang, Huiju; Wang, Xuemei; Du, Xinzhen

2016-10-01

An oriented titanium-nickel oxide composite nanotubes coating was in situ grown on a nitinol wire by direct electrochemical anodization in ethylene glycol with ammonium fluoride and water for the first time. The morphology and composition of the resulting coating showed that the anodized nitinol wire provided a titania-rich coating. The titanium-nickel oxide composite nanotubes coated fiber was used for solid-phase microextraction of different aromatic compounds coupled to high-performance liquid chromatography with UV detection. The titanium-nickel oxide composite nanotubes coating exhibited high extraction capability, good selectivity, and rapid mass transfer for weakly polar UV filters. Thereafter the important parameters affecting extraction efficiency were investigated for solid-phase microextraction of UV filters. Under the optimized conditions, the calibration curves were linear in the range of 0.1-300 μg/L for target UV filters with limits of detection of 0.019-0.082 μg/L. The intraday and interday precision of the proposed method with the single fiber were 5.3-7.2 and 5.9-7.9%, respectively, and the fiber-to-fiber reproducibility ranged from 6.3 to 8.9% for four fibers fabricated in different batches. Finally, its applicability was evaluated by the extraction and determination of target UV filters in environmental water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

FORMATION REGULARITIES OF PHASE COMPOSITION, STRUCTURE AND PROPERTIES DURING MECHANICAL ALLOYING OF BINARY ALUMINUM COMPOSITES

Directory of Open Access Journals (Sweden)

F. G. Lovshenko

2015-01-01

Full Text Available The paper presents investigation results pertaining to  ascertainment of formation regularities of phase composition and structure during mechanical alloying of binary aluminium composites/substances. The invetigations have been executed while applying a wide range of methods, devices and equipment used in modern material science. The obtained data complement each other. It has been established that presence of oxide and hydro-oxide films on aluminium powder  and introduction of surface-active substance in the composite have significant effect on mechanically and thermally activated phase transformations and properties of semi-finished products.  Higher fatty acids have been used as a surface active substance.The mechanism of mechanically activated solid solution formation has been identified. Its essence is  a formation of  specific quasi-solutions at the initial stage of processing. Mechanical and chemical interaction between components during formation of other phases has taken place along with dissolution  in aluminium while processing powder composites. Granule basis is formed according to the dynamic recrystallization mechanism and possess submicrocrystal structural type with the granule dimension basis less than 100 nm and the grains are divided in block size of not more than 20 nm with oxide inclusions of 10–20 nm size.All the compounds  with the addition of  surface-active substances including aluminium powder without alloying elements obtained by processing in mechanic reactor are disperse hardened. In some cases disperse hardening is accompanied by dispersive and solid solution hardnening process. Complex hardening predetermines a high temperature of recrystallization in mechanically alloyed compounds,  its value exceeds 400 °C.

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.

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)

Magnetic nanoparticles-nylon 6 composite for the dispersive micro solid phase extraction of selected polycyclic aromatic hydrocarbons from water samples.

Science.gov (United States)

Reyes-Gallardo, Emilia M; Lucena, R; Cárdenas, S; Valcárcel, M

2014-06-06

In this article, the easy synthesis of magnetic nanoparticles-nylon 6 composite is presented, characterized and applied in the microextraction field. The one-step synthesis of the composite is performed by a solvent changeover playing with the different solubility of the polymeric network in formic acid and water. The new material has been characterized by different techniques including infrared spectroscopy, transmission and scanning microscopy. The extraction performance of the composite under a dispersive micro solid phase extraction format has been evaluated by determining four polycyclic aromatic hydrocarbons (benzo[b]fluoranthene, fluoranthene, indeno[1,2,3-cd]pyrene and phenanthrene) in water using ultra performance liquid chromatography (UPLC) combined with photo diode array detection. The developed methodology allows the determination of the analytes with limits of detection in the range from 0.05 μg/L (benzo[b]fluoranthene) to 0.58 μg/L (phenanthrene). The repeatability of the method was better than 6.9% at the limit of quantification level. The relative recoveries varied in the interval 80-111%. Copyright © 2014 Elsevier B.V. All rights reserved.

Phase relations and Gibbs energies of spinel phases and solid solutions in the system Mg-Rh-O

Energy Technology Data Exchange (ETDEWEB)

Jacob, K.T., E-mail: katob@materials.iisc.ernet.in [Department of Materials Engineering, Indian Institute of Science, Bangalore 560 012 (India); Prusty, Debadutta [Department of Materials Engineering, Indian Institute of Science, Bangalore 560 012 (India); Kale, G.M. [Institute for Materials Research, University of Leeds, Leeds, LS2 9JT (United Kingdom)

2012-02-05

Highlights: Black-Right-Pointing-Pointer Refinement of phase diagram for the system Mg-Rh-O and thermodynamic data for spinel compounds MgRh{sub 2}O{sub 4} and Mg{sub 2}RhO{sub 4} is presented. Black-Right-Pointing-Pointer A solid-state electrochemical cell is used for thermodynamic measurement. Black-Right-Pointing-Pointer An advanced design of the solid-state electrochemical cell incorporating buffer electrodes is deployed to minimize polarization of working electrode. Black-Right-Pointing-Pointer Regular solution model for the spinel solid solution MgRh{sub 2}O{sub 4} - Mg{sub 2}RhO{sub 4} based on ideal mixing of cations on the octahedral site is proposed. Black-Right-Pointing-Pointer Factors responsible for stabilization of tetravalent rhodium in spinel compounds are identified. - Abstract: Pure stoichiometric MgRh{sub 2}O{sub 4} could not be prepared by solid state reaction from an equimolar mixture of MgO and Rh{sub 2}O{sub 3} in air. The spinel phase formed always contained excess of Mg and traces of Rh or Rh{sub 2}O{sub 3}. The spinel phase can be considered as a solid solution of Mg{sub 2}RhO{sub 4} in MgRh{sub 2}O{sub 4}. The compositions of the spinel solid solution in equilibrium with different phases in the ternary system Mg-Rh-O were determined by electron probe microanalysis. The oxygen potential established by the equilibrium between Rh + MgO + Mg{sub 1+x}Rh{sub 2-x}O{sub 4} was measured as a function of temperature using a solid-state cell incorporating yttria-stabilized zirconia as an electrolyte and pure oxygen at 0.1 MPa as the reference electrode. To avoid polarization of the working electrode during the measurements, an improved design of the cell with a buffer electrode was used. The standard Gibbs energies of formation of MgRh{sub 2}O{sub 4} and Mg{sub 2}RhO{sub 4} were deduced from the measured electromotive force (e.m.f.) by invoking a model for the spinel solid solution. The parameters of the model were optimized using the measured

Tetragonal-cubic phase boundary in nanocrystalline ZrO{sub 2}-Y{sub 2}O{sub 3} solid solutions synthesized by gel-combustion

Energy Technology Data Exchange (ETDEWEB)

Fabregas, Ismael O. [CINSO (Centro de Investigaciones en Solidos), CITEFA-CONICET, J.B. de La Salle 4397, 1603 Villa Martelli, Pcia. de Buenos Aires (Argentina); Craievich, Aldo F.; Fantini, Marcia C.A. [Instituto de Fisica, Universidade de Sao Paulo, Travessa R da Rua do Matao, No. 187, Cidade Universitaria, 05508-900 Sao Paulo (Brazil); Millen, Ricardo P.; Temperini, Marcia L.A. [Instituto de Quimica, Universidade de Sao Paulo, Avenida Prof. Lineu Prestes 748, Cidade Universitaria, 05508-900 Sao Paulo (Brazil); Lamas, Diego G., E-mail: dlamas@uncoma.edu.ar [CINSO (Centro de Investigaciones en Solidos), CITEFA-CONICET, J.B. de La Salle 4397, 1603 Villa Martelli, Pcia. de Buenos Aires (Argentina); Laboratorio de Caracterizacion de Materiales, Facultad de Ingenieria, Universidad Nacional del Comahue, Buenos Aires 1400, (8300) Neuquen Capital, Prov. de Neuquen (Argentina)

2011-04-21

Research highlights: > Gel-combustion synthesis yields compositionally homogeneous, single-phased ZrO{sub 2}-Y{sub 2}O{sub 3} nanopowders, that exhibit the presence at room temperature of three different phases depending on Y{sub 2}O{sub 3} content, namely two tetragonal forms (t' and t'') and the cubic phase. > Phase identification can be achieved by synchrotron XPD (SXPD) and Raman spectroscopy since the tetragonal forms and the cubic phase can be distinguished by these techniques. > The crystallographic features of ZrO{sub 2}-Y{sub 2}O{sub 3} nanopowders were determined by SXPD. They are similar to those reported by Yashima and coworkers for compositionally homogeneous materials containing larger (micro)crystals. However, the lattice parameters are slightly different and the axial ratios c/a of our t' samples are smaller than those reported by these authors. > Compositional t'/t'' and t''/cubic phase boundaries are located at (9 {+-} 1) and (10.5 {+-} 0.5) mol% Y{sub 2}O{sub 3}, respectively. > For the whole series of nanocrystalline ZrO{sub 2}-Y{sub 2}O{sub 3} solid solutions studied in the present work, no evidences of the presence of a mixture of phases - as reported by Yashima and coworkers for microcrystalline solid solutions - were detected. - Abstract: By means of synchrotron X-ray powder diffraction (SXPD) and Raman spectroscopy, we have detected, in a series of nanocrystalline and compositionally homogeneous ZrO{sub 2}-Y{sub 2}O{sub 3} solid solutions, the presence at room temperature of three different phases depending on Y{sub 2}O{sub 3} content, namely two tetragonal forms and the cubic phase. The studied materials, with average crystallite sizes within the range 7-10 nm, were synthesized by a nitrate-citrate gel-combustion process. The crystal structure of these phases was also investigated by SXPD. The results presented here indicate that the studied nanocrystalline ZrO{sub 2}-Y{sub 2}O{sub 3} solid

Solid radiation curable polyene compositions containing liquid polythiols and solid styrene-allyl copolymer based polyenes

International Nuclear Information System (INIS)

Morgan, C.R.

1977-01-01

Novel styrene-allyl alcohol copolymer based solid polyene compositions which when mixed with liquid polythiols can form solid curable polyene-polythiol systems are claimed. These solid polyenes, containing at least two reactive carbon-to-carbon unsaturated bonds, are urethane or ester derivatives of styrene-allyl alcohol copolymers. The solid polyenes are prepared by treating the hydroxyl groups of a styrene-allyl alcohol copolymer with a reactive unsaturated isocyanate, e.g., allyl isocyanate or a reactive unsaturated carboxylic acid, e.g., acrylic acid. Upon exposure to a free radical generator, e.g., actinic radiation, the solid polyene-polythiol compositions cure to solid, insoluble, chemically resistant, cross-linked polythioether products. Since the solid polyene-liquid polythiol composition can be cured in a solid state, such a curable system finds particular use in preparation of coatings, imaged surfaces such as photoresists, particularly solder-resistant photoresists, printing plates, etc

Cu–Co–O nano-catalysts as a burn rate modifier for composite solid propellants

Directory of Open Access Journals (Sweden)

D. Chaitanya Kumar Rao

2016-08-01

Full Text Available Nano-catalysts containing copper–cobalt oxides (Cu–Co–O have been synthesized by the citric acid (CA complexing method. Copper (II nitrate and Cobalt (II nitrate were employed in different molar ratios as the starting reactants to prepare three types of nano-catalysts. Well crystalline nano-catalysts were produced after a period of 3 hours by the calcination of CA–Cu–Co–O precursors at 550 °C. The phase morphologies and crystal composition of synthesized nano-catalysts were examined using Scanning Electron Microscope (SEM, Energy Dispersive Spectroscopy (EDS and Fourier Transform Infrared Spectroscopy (FTIR methods. The particle size of nano-catalysts was observed in the range of 90 nm–200 nm. The prepared nano-catalysts were used to formulate propellant samples of various compositions which showed high reactivity toward the combustion of HTPB/AP-based composite solid propellants. The catalytic effects on the decomposition of propellant samples were found to be significant at higher temperatures. The combustion characteristics of composite solid propellants were significantly improved by the incorporation of nano-catalysts. Out of the three catalysts studied in the present work, CuCo-I was found to be the better catalyst in regard to thermal decomposition and burning nature of composite solid propellants. The improved performance of composite solid propellant can be attributed to the high crystallinity, low agglomeration and lowering the decomposition temperature of oxidizer by the addition of CuCo-I nano-catalyst.

The study of long-term stability in liquid-solid phases for HLW disposal

International Nuclear Information System (INIS)

Wei, Y.Y.; Tseng, C.L.; Yang, J.Y.; Ke, C.H.; Wang, T.H.; Jan, Y.L.; Lee, C.B.; Lan, P.L.; Hsu, C.N.; Tsai, S.C.; Li, M.H.; Teng, S.P.

2005-01-01

Full text of publication follows: This study is conducted to observe changes in both chemical properties of buffer materials and liquid phases over an experimental period of 2 years. In our experiments, bentonite powder and crushed granite are separately mixed with synthetic groundwater, synthetic seawater and de-ionised water at a fixed liquid-solid ratio of 30. A mixed set with both bentonite and granite together as solid phase is also investigated. During this study, aliquots of the liquid phases are sampled every two months and pH and Eh values are measured immediately. Concentrations of Na, Mg, K, Al, Ca, Ti, Mn, Ba, Fe, Sr, Li and Th are analyzed in the liquid phase directly by ICP-AES. After separation by centrifugation followed by freeze drying and digestion, the solid phases are analyzed as well for elemental composition. Alteration of solid phases during the experimental period is discussed. The preliminary results show that the pH values of the three solutions vary considerably in the individual experimental systems containing bentonite, granite or the mixed system. In general, higher pH values are found in DI-water for all solid phases. Eh values fluctuate a lot in the range 100 to 300 mV in all experiment sets. Different to the experiments with granite for which similar Eh values are found in all solutions, a significantly different Eh-value is found in the experiment with bentonite in DI-water as compared to the other solutions. The results from element analysis indicate that equilibrium is achieved after only two months and element concentrations change only slightly thereafter. We conclude from our experiments that both bentonite and granite keep their characteristics as radionuclide sorbents in the vicinity of a nuclear waste repository. Reaction equilibria appear to be attained rapidly. Because there are just a few alterations in this study, it would be a huge error source in analyzing from the inhomogeneous solid phase such as granite and losses

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...

Form-stable paraffin/high density polyethylene composites as solid-liquid phase change material for thermal energy storage: preparation and thermal properties

International Nuclear Information System (INIS)

Sari, Ahmet

2004-01-01

This paper deals with the preparation of paraffin/high density polyethylene (HDPE) composites as form-stable, solid-liquid phase change material (PCM) for thermal energy storage and with determination of their thermal properties. In such a composite, the paraffin (P) serves as a latent heat storage material and the HDPE acts as a supporting material, which prevents leakage of the melted paraffin because of providing structural strength. Therefore, it is named form-stable composite PCM. In this study, two kinds of paraffins with melting temperatures of 42-44 deg. C (type P1) and 56-58 deg. C (type P2) and latent heats of 192.8 and 212.4 J g -1 were used. The maximum weight percentage for both paraffin types in the PCM composites without any seepage of the paraffin in the melted state were found as high as 77%. It is observed that the paraffin is dispersed into the network of the solid HDPE by investigation of the structure of the composite PCMs using a scanning electronic microscope (SEM). The melting temperatures and latent heats of the form-stable P1/HDPE and P2/HDPE composite PCMs were determined as 37.8 and 55.7 deg. C, and 147.6 and 162.2 J g -1 , respectively, by the technique of differential scanning calorimetry (DSC). Furthermore, to improve the thermal conductivity of the form-stable P/HDPE composite PCMs, expanded and exfoliated graphite (EG) by heat treatment was added to the samples in the ratio of 3 wt.%. Thereby, the thermal conductivity was increased about 14% for the form-stable P1/HDPE and about 24% for the P2/HDPE composite PCMs. Based on the results, it is concluded that the prepared form-stable P/HDPE blends as composite type PCM have great potential for thermal energy storage applications in terms of their satisfactory thermal properties and improved thermal conductivity. Furthermore, these composite PCMs added with EG can be considered cost effective latent heat storage materials since they do not require encapsulation and extra cost to enhance

Microstructure and phase composition of sputter-deposited zirconia-yttria films

International Nuclear Information System (INIS)

Knoll, R.W.; Bradley, E.R.

1983-11-01

Thin ZrO 2 -Y 2 O 3 coatings ranging in composition from 3 to 15 mole % Y 2 O 3 were produced by rf sputter deposition. This composition range spanned the region on the equilibrium ZrO 2 -Y 2 O 3 phase diagram corresponding to partially stabilized zirconia (a mixture of tetragonal ZrO 2 and cubic solid solution). Microstructural characteristics and crystalline phase composition of as-deposited and heat treated films (1100 0 C and 1500 0 C) were determined by transmission electron microscopy (TEM) and by x-ray diffraction (XRD). Effects of substrate bias (0 approx. 250 volts), which induced ion bombardment of the film during growth, were also studied. The as-deposited ZrO 2 -Y 2 O 3 films were single phase over the composition range studied, and XRD data indicated considerable local atomic disorder in the lattice. Films produced at low bias contained intergranular voids, pronounced columnar growth, and porosity between columns. At high bias, the microstructure was denser, and films contained high compressive stress. After heat treatment, all deposits remained single phase, therefore a microstructure and precipitate distribution characteristic of toughened, partially stabilized zirconia appear to be difficult to achieve in vapor deposited zirconia coatings

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.

Kinetics of solid-phase in ion exchange on tin hydrogen phosphate

International Nuclear Information System (INIS)

Kislitsyn, M.N.; Ketsko, V.A.; Yaroslavtsev, A.B.

2004-01-01

Solid state reactions in mixture of tin hydrogen phosphate and alkali metal (M=Na, K, Cs) chlorides have been studied both in the mode of polythermal heating and at a fixed temperature, using data of X-ray phase and thermogravimetric analyses. In the range 400-750 Deg C solid state ion exchange reactions occur in the systems studied and yield mono-- and dialkali phosphates MHSn(PO 4 ) 2 and M 2 Sn(PO 4 ) 2 . Counter diffusion coefficients for alkali metal cations and protons in the matrices of compositions MHSn(PO 4 ) 2 and M 2 Sn(PO 4 ) 2 have been determined [ru

Simple material physics experiment for studying phase diagrams and solid state transformations in alloys

Energy Technology Data Exchange (ETDEWEB)

Kaur, S; Kamal, R [Punjabi Univ., Patiala (India). Dept. of Physics

1977-09-01

Study of phase diagram and accompanying solid state transformations is essential to determine the best possible composition, manufacturing techniques and physical properties of an alloy. A simple technique having wide applications in metallurgical industry is to study the temperature--time curve of the alloy undergoing cooling with an uniform rate. An experiment which uses this technique is described. It is widely applicable in the fields of materials science, applied solid state physics, physical metallurgy and physical chemistry.

Solid composite electrolytes for lithium batteries

Science.gov (United States)

Kumar, Binod; Scanlon, Jr., Lawrence G.

2000-01-01

Solid composite electrolytes are provided for use in lithium batteries which exhibit moderate to high ionic conductivity at ambient temperatures and low activation energies. In one embodiment, a ceramic-ceramic composite electrolyte is provided containing lithium nitride and lithium phosphate. The ceramic-ceramic composite is also preferably annealed and exhibits an activation energy of about 0.1 eV.

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...

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

Phases of variable composition in the system Ba3-xSrxEr(BO3)3 (0≤x≤3.0)

International Nuclear Information System (INIS)

Khamaganova, T.N.

2008-01-01

The possibility of preparing two series of solid solutions in the system Ba 3-x Sr x Er(BO 3 ) 3 (0 ≤ x ≤ 3.0), crystallizing in different structural types, was examined. Samples of the phases of variable composition were synthesized by solid-phase reactions over the temperature range 500-1000 deg C, and their X-ray diffraction characteristics were determined. It is found that the triple phases prepared form two series of substitutional solid solutions in the system studied [ru

Relating hydrogen-bonding interactions with the phase behavior of naproxen/PVP K 25 solid dispersions: evaluation of solution-cast and quench-cooled films.

Science.gov (United States)

Paudel, Amrit; Nies, Erik; Van den Mooter, Guy

2012-11-05

In this work, we investigated the relationship between various intermolecular hydrogen-bonding (H-bonding) interactions and the miscibility of the model hydrophobic drug naproxen with the hydrophilic polymer polyvinylpyrrolidone (PVP) across an entire composition range of solid dispersions prepared by quasi-equilibrium film casting and nonequilibrium melt quench cooling. The binary phase behavior in solid dispersions exhibited substantial processing method dependence. The solid state solubility of crystalline naproxen in PVP to form amorphous solid dispersions was 35% and 70% w/w naproxen in solution-cast films and quench-cooled films, respectively. However, the presence of a single mixed phase glass transition indicated the amorphous miscibility to be 20% w/w naproxen for the films, beyond which amorphous-amorphous and/or crystalline phase separations were apparent. This was further supported by the solution state interactions data such as PVP globular size distribution and solution infrared spectral profiles. The borderline melt composition showed cooling rate dependence of amorphization. The glass transition and melting point depression profiles of the system were treated with the analytical expressions based on Flory-Huggins mixing theory to interpolate the equilibrium solid solubility. FTIR analysis and subsequent spectral deconvolution revealed composition and miscibility dependent variations in the strength of drug-polymer intermolecular H-bonding. Two types of H-bonded populations were evidenced from 25% w/w and 35% w/w naproxen in solution-cast films and quench-cooled films, respectively, with the higher fraction of strongly H-bonded population in the drug rich domains of phase separated amorphous film compositions and highly drug loaded amorphous quench-cooled dispersions.

Influence of composition of the raw materials on phase formation in solid compounds based on slag and clay minerals

International Nuclear Information System (INIS)

Galkin, A.V.; Tolebaev, T.; Omarova, V.I.; Burkitbaev, M.; Blynskiy, A.P.; Bachilova, N.V.; Matsynina, V.I.

2003-01-01

Full text: Activation of solidification processes in a compound formed on the basis of slag and clay minerals using sodium hydroxide - the output product from processing the BN-350 sodium coolant it is expedient to form the final product with a phase composition representing (in terms of long term storage) hydro-alumino-silicates incorporating Na-22 and Cs-137 radionuclides, which isomorphly replace other atoms in the crystal lattice sites. Combination of mineral phases, such as alkaline and alkaline-earth hydro-alumino-silicates with zeolite-like structure, providing sorptive properties, and the tobermorite like low-base hydro silicates of calcium defining the physico-mechanical properties of compound is the necessary condition for the compound stability. Investigations of phase formation in the mixtures of Kazakhstan clay, slag materials and alkali have been conducted targeted to control the physico-chemical properties of solid compound. The mixtures of alkali, thermal power plant ashes and clays of various mineralogical genesis (kaolinite, bentonite, Ca-Na-smectite montmorillonite) have been studied. The ashes and phosphorous slag while interacting with alkali are determined to form the non-alkaline hydro-silicates of stavrolite and indianite (anortite) type with free alkali being found in an unbound state. Both alkaline and alkaline-alkaline-earth hydro-silicates of Na 2 Ca 2 Si 2 O 7 H 2 O type are only formed in a compounds containing metallurgical slag. Formation of alkaline hydro-alumino-silicates of NaAlSiO 4 H 2 0 type as well as tomsonite (Na 4 Ca 8 [Al 20S i 20 O 80 ] 24H 2 O) - the zeolite like mineral have been detected in a two-component alkali-clay mixtures. Besides the quantity of tomsonite was determined to be not only dependent on Al 2 O 3 content in clay component but is also defined by stoichiometric composition of the mixture, because zeolite synthesis takes place under conditions of gels co-deposition and high pH value. Maximum quantity of

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....

Theoretical prediction of morphotropic compositions in Na1/2Bi1/2TiO3-based solid solutions from transition pressures

Science.gov (United States)

Gröting, Melanie; Albe, Karsten

2014-02-01

In this article we present a method based on ab initio calculations to predict compositions at morphotropic phase boundaries in lead-free perovskite solid solutions. This method utilizes the concept of flat free energy surfaces and involves the monitoring of pressure-induced phase transitions as a function of composition. As model systems, solid solutions of Na1/2Bi1/2TiO3 with the alkali substituted Li1/2Bi1/2TiO3 and K1/2Bi1/2TiO3 and the alkaline earth substituted CaTiO3 and BaTiO3 are chosen. The morphotropic compositions are identified by determining the composition at which the phase transition pressure equals zero. In addition, we discuss the different effects of hydrostatic pressure (compression and tension) and chemical substitution on the antiphase tilts about the [111] axis (a-a-a-) present in pure Na1/2Bi1/2TiO3 and how they develop in the two solid solutions Na1/2Bi1/2TiO3-CaTiO3 and Na1/2Bi1/2TiO3-BaTiO3. Finally, we discuss the advantages and shortcomings of this simple computational approach.

Effective medium of periodic fluid-solid composites

KAUST Repository

Mei, Jun; Wu, Ying; Liu, Zhengyou

2012-01-01

An analytic solution of the effective mass density and bulk modulus of a periodic fluid-solid composite is obtained by using the multiple-scattering theory in the long-wavelength limit. It is shown that when the concentration of solid inclusions

Computer Simulations of Composite Electrodes in Solid-Oxide Fuel-Cells

Energy Technology Data Exchange (ETDEWEB)

Sunde, Svein

1999-07-01

aspects of structure and composition. The thesis is composed of the five papers: (A) Calculation of conductivity and polarization resistance of composite SOFC-electrodes from random resistor networks, (B) Monte Carlo Simulations of Conductivity of Composite Electrodes for Solid Oxide Fuel Cells, (C) Monte Carlo Simulations of the Polarization Resistance of Composite Electrodes for Solid Oxide Fuel Cells (D) Calculations of Impedance of Composite Modes for Solid Oxide Fuel Cells (E) Simulations of Composite Electrodes in Fuel Cells. The major results are: (1) A Monte Carlo method is constructed for electrochemical applications, (2) The Monte Carlo simulations of conductivity with respect to its dependence on composition and temperature are validated quantitatively with respect to experimental results (papers A, B and E), (3) The Monte Carlo method is validated qualitatively with respect polarisation resistance and its thickness dependence (papers A, C, and E), (Considerable scatter in the experimental results prevents a more strict quantitative evaluation of the model.), (4) A dependence of the percolation threshold on particle size in the composite is suggested as a major reason for electrode deactivation in fuel cells employing composite electrodes in which particle aggregation occur (paper B), (5) The range of compositions within which there will be a thickness dependence of the polarisation resistance is calculated as a function of relative ratio of particle radii (paper C), (6) The shapes of impedance-plane plots for composite electrodes will usually differ significantly from their point-contact counterparts exclusively for reasons related structure (paper D), (7) The macroscopic porous-electrode theory is adapted for composite electrodes (papers C and E), (8) A model for internal reforming of methane at a composite fuel-cell anode is formulated, based on the macroscopic porous-electrode theory (paper E). The model includes a description of gas-phase transport and non

Phase composition of EhK 990-ID steel

International Nuclear Information System (INIS)

Rabinovich, A.V.; Milova, I.M.; Zaslavskij, Yu.B.; Neklyudov, I.M.; Chernyj, B.P.; Vanzha, A.F.; Zejdlits, M.P.; Kurasov, A.N.; Shmelev, Yu.S.

1990-01-01

The microstructure and phase composition of EhK99 steel have been investigated. It is shown that the scandium absolute concentration in solid solution of hot-deformed metal is directly proportional to their total content. It was established that the ratio between the scandium concentration in solid solution and the total content [Sc] ss/[Sc] s is not the function of the latter and constitutes (24.5±5.5) rel.%. The limiting scandium solubility in the EhK99 steel at temperature 1270 deg C was determined. It constitutes 0.07±0.005 mass%. In this paper proposed is the mechanism of intermetallide-and-second phase nucleation and growth during crystallization and homogenizing annealing. The recommendation for regimes of homogenizing annealing (1270 deg C, 12 hours) are given. It is shown that the homogenizing vacuum annealing may have an appreciable influence on the technique plasticity and production of good tubes of EhK99 steel with scandium content no more than 0.07wt%. 2 refs., 10 figs., 2 tabs

Determination of equilibrium phase composition in the Hg-HgTe-CdTe system by ''dew point'' method

International Nuclear Information System (INIS)

Vanyukov, A.V.; Krotov, I.I.; Ermakov, A.I.

1978-01-01

Using the ''dew point'' method a study has been made of the equilibrium composition of the solid and liquid phases in the Hg-HgTe-CdTe system at 404, 435 and 454 deg C. It has been pointed out that crystallization of cadmium-rich solid solutions of Cdsub(x)Hgsub(1-x) Te takes place from a liquid phase with a much higher concentration of Hg. The activity of Hg in the liquid phase increases along the liquidus isotherm in the direction from section Hg-HgTe to section HgCdTe in accordance with the increase of its concentration. An increase in activity of Hg in the solid phase of Cdsub(x)Hgsub(1-x)Te has been noted with the reduction of its concentration

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.

An ordered metallic glass solid solution phase that grows from the melt like a crystal

International Nuclear Information System (INIS)

Chapman, Karena W.; Chupas, Peter J.; Long, Gabrielle G.; Bendersky, Leonid A.; Levine, Lyle E.; Mompiou, Frédéric; Stalick, Judith K.; Cahn, John W.

2014-01-01

We report structural studies of an Al–Fe–Si glassy solid that is a solid solution phase in the classical thermodynamic sense. We demonstrate that it is neither a frozen melt nor nanocrystalline. The glass has a well-defined solubility limit and rejects Al during formation from the melt. The pair distribution function of the glass reveals chemical ordering out to at least 12 Å that resembles the ordering within a stable crystalline intermetallic phase of neighboring composition. Under isothermal annealing at 305 °C the glass first rejects Al, then persists for approximately 1 h with no detectable change in structure, and finally is transformed by a first-order phase transition to a crystalline phase with a structure that is different from that within the glass. It is possible that this remarkable glass phase has a fully ordered atomic structure that nevertheless possesses no long-range translational symmetry and is isotropic

A review of the potential of photoacoustic and photothermal spectroscopy for the characterisation of actinide solid phases

International Nuclear Information System (INIS)

Liezers, M.; McMillan, J.W.; Pollard, P.M.

1988-09-01

As the solid actinide compounds encountered in radioactive wastes have widely differing aqueous solubilities, methods are required to determine their composition. Analytical methods with the potential to characterise solid actinide compounds in equilibrium with an aqueous phase are reviewed. 'Direct', essentially non-invasive methods were sought. The most promising were identified as photoacoustic and photothermal spectroscopies. A programme is suggested for their study and exploitation. (author)

Kinetic modeling of solid-state partitioning phase transformation with simultaneous misfit accommodation

International Nuclear Information System (INIS)

Song, Shaojie; Liu, Feng

2016-01-01

Considering a spherical misfitting precipitate growing into a finite elastic-perfectly plastic supersaturated matrix, a kinetic modeling for such solid-state partitioning phase transformation is presented, where the interactions of interface migration, solute diffusion and misfit accommodation are analyzed. The linkage between interface migration and solute diffusion proceeds through interfacial composition and interface velocity; their effects on misfit accommodation are mainly manifested in an effective transformation strain, which depends on instantaneous composition field and precipitate size. Taking γ to α transformation of a binary Fe-0.5 at.% C alloy under both isothermal and continuous cooling conditions as examples, the effects of misfit accommodation on the coupling interface migration and solute diffusion are well evaluated and discussed. For the isothermal transformation, a counterbalancing influence between mechanical and chemical driving forces is found so that the mixed-mode transformation kinetics is not sensitive with respect to the elastic–plastic accommodation of the effective misfit strain. Different from the isothermal process, during the continuous cooling condition, the effects of misfit accommodation on the kinetics of solid-state partitioning phase transformation are mainly manifested in the great decrease of the transformation starting temperature and the thermodynamic equilibrium composition. The present kinetic modeling was applied to predict the experimentally measured γ/α transformation of Fe-0.47 at.% C alloy conducted with a cooling rate of 10 K min −1 and a good agreement was achieved.

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

Investigation of metal-matrix composite containing liquid-phase dispersion

Czech Academy of Sciences Publication Activity Database

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

2012-01-01

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

Thermal decomposition of solid mixtures of 2-oxy-4,6-dinitramine-s-triazine (DNAM) and phase stabilized ammonium nitrate (PSAN)

OpenAIRE

Simões, P. N.; Pedroso, L. M.; Portugal, A. A.; Campos, J. L.

2000-01-01

The thermal decomposition of solid mixtures of 2-oxy-4,6-dinitramine-s-triazine (DNAM) and phase stabilized ammonium nitrate (PSAN) at different mass ratios has been studied. Simultaneous thermal analysis (DSC/TG) and thermomicroscopy have been used. It was found that PSAN promotes the lowering of the decomposition temperature of DNAM. The beginning of this process occurs when both components are in the solid state irrespective of the composition. However, the composition appears as the main ...

Sintered glass ceramic composites from vitrified municipal solid waste bottom ashes

International Nuclear Information System (INIS)

Aloisi, Mirko; Karamanov, Alexander; Taglieri, Giuliana; Ferrante, Fabiola; Pelino, Mario

2006-01-01

A glass ceramic composite was obtained by sinter-crystallisation of vitrified municipal solid waste bottom ashes with the addition of various percentages of alumina waste. The sintering was investigated by differential dilatometry and the crystallisation of the glass particles by differential thermal analysis. The crystalline phases produced by the thermal treatment were identified by X-ray diffraction analysis. The sintering process was found to be affected by the alumina addition and inhibited by the beginning of the crystal-phase precipitation. Scanning electron microscopy was performed on the fractured sintered samples to observe the effect of the sintering. Young's modulus and the mechanical strength of the sintered glass ceramic and composites were determined at different heating rates. The application of high heating rate and the addition of alumina powder improved the mechanical properties. Compared to the sintered glass ceramic without additives, the bending strength and the Young's modulus obtained at 20 deg. C/min, increased by about 20% and 30%, respectively

Chemically and compositionally modified solid solution disordered multiphase nickel hydroxide positive electrode for alkaline rechargeable electrochemical cells

Science.gov (United States)

Ovshinsky, Stanford R.; Corrigan, Dennis; Venkatesan, Srini; Young, Rosa; Fierro, Christian; Fetcenko, Michael A.

1994-01-01

A high capacity, long cycle life positive electrode for use in an alkaline rechargeable electrochemical cell comprising: a solid solution nickel hydroxide material having a multiphase structure that comprises at least one polycrystalline .gamma.-phase including a polycrystalline .gamma.-phase unit cell comprising spacedly disposed plates with at least one chemical modifier incorporated around the plates, the plates having a range of stable intersheet distances corresponding to a 2.sup.+ oxidation state and a 3.5.sup.+, or greater, oxidation state; and at least one compositional modifier incorporated into the solid solution nickel hydroxide material to promote the multiphase structure.

Investigation into isomolar series of Al(NO/sub 3/)/sub 3/, Na/sub 3/VO/sub 4/ solution mixture and composition of solid phases

Energy Technology Data Exchange (ETDEWEB)

Chernysh, L F; Nakhodnova, A P; Makarova, R A [Donetskij Gosudarstvennyj Univ. (Ukrainian SSR)

1979-11-01

Conducted is investigation of properties of isomolar series of aluminium nitrate and sodium vanadate solutions at pH of the latter 12.5; 10.0; 7.0 and the temperature of 25 deg C using the methods of pH-metry, conductometry, ''seeming'' volume of precipitations, residual concentration of aluminium and vanadium. It is shown, that the composition property diagram of the system investigated does not reflect the true composition of solid-phase products of the reaction, which depends on the component ratio in solution. Bottom phases of isomolar series are mainly heterogeneous. At the excess of sodium vanadate solution and its high pH values conditions for the basic salt formation are created. At pH of the Na/sub 3/VO/sub 4/ solution of 12.5 and 10.0 and Al(NO/sub 3/)/sub 3/: Na/sub 3/VO/sub 4/ ratios 4:6 and 3:7 respectively obtained are the basic aluminium vanadates of the (AlOH)/sub 3/(VO/sub 4/)/sub 2/x 7.5H/sub 2/O and (AlOH)/sub 2/V/sub 2/O/sub 7/x5H/sub 2/O composition, some of their physicochemical properties being investigated.

Morphology, composition, and mixing state of primary particles from combustion sources ? crop residue, wood, and solid waste

OpenAIRE

Liu, Lei; Kong, Shaofei; Zhang, Yinxiao; Wang, Yuanyuan; Xu, Liang; Yan, Qin; Lingaswamy, A. P.; Shi, Zongbo; Lv, Senlin; Niu, Hongya; Shao, Longyi; Hu, Min; Zhang, Daizhou; Chen, Jianmin; Zhang, Xiaoye

2017-01-01

Morphology, composition, and mixing state of individual particles emitted from crop residue, wood, and solid waste combustion in a residential stove were analyzed using transmission electron microscopy (TEM). Our study showed that particles from crop residue and apple wood combustion were mainly organic matter (OM) in smoldering phase, whereas soot-OM internally mixed with K in flaming phase. Wild grass combustion in flaming phase released some Cl-rich-OM/soot particles and cardboard combusti...

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)

Combination of (M)DSC and surface analysis to study the phase behaviour and drug distribution of ternary solid dispersions.

Science.gov (United States)

Meeus, Joke; Scurr, David J; Chen, Xinyong; Amssoms, Katie; Davies, Martyn C; Roberts, Clive J; Van den Mooter, Guy

2015-04-01

Miscibility of the different compounds that make up a solid dispersion based formulation play a crucial role in the drug release profile and physical stability of the solid dispersion as it defines the phase behaviour of the dispersion. The standard technique to obtain information on phase behaviour of a sample is (modulated) differential scanning calorimetry ((M)DSC). However, for ternary mixtures (M)DSC alone is not sufficient to characterize their phase behaviour and to gain insight into the distribution of the active pharmaceutical ingredient (API) in a two-phased polymeric matrix. MDSC was combined with complementary surface analysis techniques, specifically time-of-flight secondary ion mass spectrometry (ToF-SIMS) and atomic force microscopy (AFM). Three spray-dried model formulations with varying API/PLGA/PVP ratios were analyzed. MDSC, TOF-SIMS and AFM provided insights into differences in drug distribution via the observed surface coverage for 3 differently composed ternary solid dispersions. Combining MDSC and surface analysis rendered additional insights in the composition of mixed phases in complex systems, like ternary solid dispersions.

Quantum chemistry of solids and materials technology: solid-phase compounds of d- and f-elements

International Nuclear Information System (INIS)

Gubanov, V.A.

1988-01-01

The results of studies aimed at the development of methods of theoretical calculations of the electronic structure of solid phase compounds of α- and f-elements and the modelling of physicochemical properties of materials developed on their basis, are presented. The possibilities of cluster and zone calculations of the electronic structure of refractory compounds of d-metals with light elements are considered. The regularities of changes in the chemical bond and properties during crystal lattice alloying with metals, metalloids are found. The methods of quantum chemical modeling of optically active and luminescent materials on the base of oxides, fluorides, chalcogenides of d- and f-metals are developed. The compositions of new optically active compositions and protective coatings are suggested. New approaches to the study of magnetic properties of metals, alloys and compounds are developed. The results of calculations of the energy spectra of high-temperature oxide superconductors are given

A Li-Garnet composite ceramic electrolyte and its solid-state Li-S battery

Science.gov (United States)

Huang, Xiao; Liu, Cai; Lu, Yang; Xiu, Tongping; Jin, Jun; Badding, Michael E.; Wen, Zhaoyin

2018-04-01

A high strength Li-Garnet solid electrolyte composite ceramic is successfully prepared via conventional solid state method with Li6.4La3Zr1.4Ta0.6O12 and nano MgO powders. Well sintered ceramic pellets and bars are obtained with 0-9 wt.% MgO. Fracture strength is approximately 135 MPa for composite ceramics with 5-9 wt.% MgO, which is ∼50% higher than that of pure Li6.4La3Zr1.4Ta0.6O12 (90 MPa). Lithium-ion conductivity of the composite is above 5 × 10-4 S cm-1 at room temperature; comparable to the pure Li6.4La3Zr1.4Ta0.6O12 material. SEM cross-sections of the composite ceramic shows a much more uniform microstructure comparing with pure ones, owing to the grain growth inhibition effect of the MgO second phase. A battery cell consisting of Li/composite ceramics/Sulfur-Carbon at 25 °C exhibits a capacity of 685 mAh g-1 at 0.2 C at the 200th cycle, while maintaining a coulombic efficiency of 100%. These results indicate that the composite ceramic Li6.4La3Zr1.4Ta0.6O12-MgO is promising for the production of electrolyte membrane and fabrication of Li-Sulfur batteries.

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.

Axial dispersion of gas and solid phases in a gas—solid packed column at trickle flow

NARCIS (Netherlands)

Roes, A.W.M.; van Swaaij, Willibrordus Petrus Maria

1979-01-01

Axial dispersion of gas and solid phases in a gas—solid packed column at trickle flow, a promising new countercurrent operation, was evaluated using residence time distribution (RTD) experiments. The column was packed with dumped Pall rings, the gas phase was air at ambient conditions and the solid

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.

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.

Simulation of the infiltration process of a ceramic open-pore body with a metal alloy in semi-solid state to design the manufacturing of interpenetrating phase composites

Science.gov (United States)

Schomer, Laura; Liewald, Mathias; Riedmüller, Kim Rouven

2018-05-01

Metal-ceramic Interpenetrating Phase Composites (IPC) belong to a special subcategory of composite materials and reveal enhanced properties compared to conventional composite materials. Currently, IPC are produced by infiltration of a ceramic open-pore body with liquid metal applying high pressure and I or high temperature to avoid residual porosity. However, these IPC are not able to gain their complete potential, because of structural damages and interface reactions occurring during the manufacturing process. Compared to this, the manufacturing of IPC using the semi-solid forming technology offers great perspectives due to relative low processing temperatures and reduced mechanical pressure. In this context, this paper is focusing on numerical investigations conducted by using the FLOW-3D software for gaining a deeper understanding of the infiltration of open-pore bodies with semi-solid materials. For flow simulation analysis, a geometric model and different porous media drag models have been used. They have been adjusted and compared to get a precise description of the infiltration process. Based on these fundamental numerical investigations, this paper also shows numerical investigations that were used for basically designing a semi-solid forming tool. Thereby, the development of the flow front and the pressure during the infiltration represent the basis of the evaluation. The use of an open and closed tool cavity combined with various geometries of the upper die shows different results relating to these evaluation arguments. Furthermore, different overflows were designed and its effects on the pressure at the end of the infiltration process were investigated. Thus, this paper provides a general guideline for a tool design for manufacturing of metal-ceramic IPC using semi-solid forming.

Tribo-electric charging of dielectric solids of identical composition

Science.gov (United States)

Angus, John C.; Greber, Isaac

2018-05-01

Despite its long history and importance in many areas of science and technology, there is no agreement on the mechanisms responsible for tribo-electric charging, including especially the tribo-charging of chemically identical dielectric solids. Modeling of the excitation, diffusional transport, and de-excitation of electrons from hot spots shows that a difference in local surface roughness of otherwise identical solid dielectric objects leads to different transient excited electron concentrations during tribo-processes. The model predicts that excited electron concentrations are lower and concentration gradients higher in solids with rougher rather than smoother surfaces. Consequently, during contact, the flux of charge carriers (electrons or holes) from hot spots will be greater into the rougher solid than into the smoother solid. These predictions are in agreement with current and historical observations of tribo-electric charge transfer between solids of the same composition. This effect can take place in parallel with other processes and may also play a role in the charging of solids of different composition.

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.

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.

A novel poly(deep eutectic solvent)-based magnetic silica composite for solid-phase extraction of trypsin

International Nuclear Information System (INIS)

Xu, Kaijia; Wang, Yuzhi; Li, Yixue; Lin, Yunxuan; Zhang, Haibao; Zhou, Yigang

2016-01-01

Novel poly(deep eutectic solvent) grafted silica-coated magnetic microspheres (Fe 3 O 4 @SiO 2 -MPS@PDES) were prepared by polymerization of choline chloride-itaconic acid (ChCl-IA) and γ-MPS-modified magnetic silica composites, and were characterized by vibrating sample magnetometer (VSM), Fourier transform infrared spectrometry (FT-IR), X-ray photoelectron spectra (XPS), thermal gravimetric analysis (TGA) and transmission electron microscope (TEM). Then the synthetic Fe 3 O 4 @SiO 2 -MPS@PDES microspheres were applied for the magnetic solid-phase extraction (MSPE) of trypsin for the first time. After extraction, the concentration of trypsin in the supernatant was determined by a UV–vis spectrophotometer. Single factor experiments were carried out to investigate the effects of the extraction process, including the concentration of trypsin, the ionic strength, the pH value, the extraction time and the temperature. Experimental results showed the extraction capacity could reach up to 287.5 mg/g under optimized conditions. In comparison with Fe 3 O 4 @SiO 2 -MPS, Fe 3 O 4 @SiO 2 -MPS@PDES displayed higher extraction capacity and selectivity for trypsin. According to the regeneration studies, Fe 3 O 4 @SiO 2 -MPS@PDES microspheres can be recycled six times without significant loss of its extraction capacity, and retained a high extraction capacity of 233 mg/g after eight cycles. Besides, the activity studies also demonstrated that the activity of the extracted trypsin was well retained. Furthermore, the analysis of real sample revealed that the prepared magnetic microspheres can be used to purify trypsin in crude bovine pancreas extract. These results highlight the potential of the proposed Fe 3 O 4 @SiO 2 -MPS@PDES-MSPE method in separation of biomolecules. - Highlights: • A strategy for solid-phase extraction of trypsin based on poly(deep eutectic solvent) modified magnetic silica microspheres. • Fe 3 O 4 @SiO 2 -MPS@PDES showed higher extraction capacity

Iron oxide functionalized graphene nano-composite for dispersive solid phase extraction of chemical warfare agents from aqueous samples.

Science.gov (United States)

Chinthakindi, Sridhar; Purohit, Ajay; Singh, Varoon; Tak, Vijay; Goud, D Raghavender; Dubey, D K; Pardasani, Deepak

2015-05-15

Present study deals with the preparation and evaluation of graphene based magnetic nano-composite for dispersive solid phase extraction of Chemical Weapons Convention (CWC) relevant chemicals from aqueous samples. Nano-composite, Fe3O4@SiO2-G was synthesized by covalently bonding silica coated Fe3O4 onto the graphene sheets. Nerve agents (NA), Sulfur mustard (SM) and their non-toxic environmental markers were the target analytes. Extraction parameters like amount of sorbent, extraction time and desorption conditions were optimized. Dispersion of 20 milligram of sorbent in 200mL of water sample for 20min. followed by methanol/chloroform extraction produced average to good recoveries (27-94%) of targeted analytes. Recoveries of real agents exhibited great dependency upon sample pH and ionic strength. Sarin produced maximum recovery under mild acidic conditions (56% at pH 5) while VX demanded alkaline media (83% at pH 9). Salts presence in the aqueous samples was found to be advantageous, raising the recoveries to as high as 94% for SM. Excellent limits of detection (LOD) for sulphur mustard and VX (0.11ngmL(-1) and 0.19ngmL(-1) respectively) proved the utility of the developed method for the off-site analysis of CWC relevant chemicals. Copyright © 2015 Elsevier B.V. All rights reserved.

Phase diagram of nanoscale alloy particles used for vapor-liquid-solid growth of semiconductor nanowires.

Science.gov (United States)

Sutter, Eli; Sutter, Peter

2008-02-01

We use transmission electron microscopy observations to establish the parts of the phase diagram of nanometer sized Au-Ge alloy drops at the tips of Ge nanowires (NWs) that determine their temperature-dependent equilibrium composition and, hence, their exchange of semiconductor material with the NWs. We find that the phase diagram of the nanoscale drop deviates significantly from that of the bulk alloy, which explains discrepancies between actual growth results and predictions on the basis of the bulk-phase equilibria. Our findings provide the basis for tailoring vapor-liquid-solid growth to achieve complex one-dimensional materials geometries.

Thermal conductivity and latent heat thermal energy storage properties of LDPE/wax as a shape-stabilized composite phase change material

International Nuclear Information System (INIS)

Trigui, Abdelwaheb; Karkri, Mustapha; Krupa, Igor

2014-01-01

Highlights: • This study deals with the comparison of experimental results for different PCM composite to be used in passive solar walls. • This paper reports on the successful use of a specific experimental method in order to characterize the phase change effects. • The results have shown that most important thermal properties of these composites at the solid and liquid states. • Results indicate the thermal effectiveness of phase change material and significant amount of energy saving can be achieved. • Heat flux measurements are a very interesting experimental source of data which comes to complete the calorimetric device (DSC). - Abstract: Phase change material (PCM) composites based on low-density polyethylene (LDPE) with paraffin waxes were investigated in this study. The composites were prepared using a meltmixing method with a Brabender-Plastograph. The LDPE as the supporting matrix kept the molten waxes in compact shape during its phase transition from solid to liquid. Immiscibility of the PCMs (waxes) and the supporting matrix (LDPE) is a necessary property for effective energy storage. Therefore, this type paraffin can be used in a latent heat storage system without encapsulation. The objective of this research is to use PCM composite as integrated components in a passive solar wall. The proposed composite TROMBE wall allows daily storage of the solar energy in a building envelope and restitution in the evening, with a possible control of the air flux in a ventilated air layer. An experimental set-up was built to determine the thermal response of these composites to thermal solicitations. In addition, a DSC analysis was carried out. The results have shown that most important thermal properties of these composites at the solid and liquid states, like the “apparent” thermal conductivity, the heat storage capacity and the latent heat of fusion. Results indicate the performance of the proposed system is affected by the thermal effectiveness of

Diffusion relaxation times of nonequilibrium isolated small bodies and their solid phase ensembles to equilibrium states

Science.gov (United States)

Tovbin, Yu. K.

2017-08-01

The possibility of obtaining analytical estimates in a diffusion approximation of the times needed by nonequilibrium small bodies to relax to their equilibrium states based on knowledge of the mass transfer coefficient is considered. This coefficient is expressed as the product of the self-diffusion coefficient and the thermodynamic factor. A set of equations for the diffusion transport of mixture components is formulated, characteristic scales of the size of microheterogeneous phases are identified, and effective mass transfer coefficients are constructed for them. Allowing for the developed interface of coexisting and immiscible phases along with the porosity of solid phases is discussed. This approach can be applied to the diffusion equalization of concentrations of solid mixture components in many physicochemical systems: the mutual diffusion of components in multicomponent systems (alloys, semiconductors, solid mixtures of inert gases) and the mass transfer of an absorbed mobile component in the voids of a matrix consisting of slow components or a mixed composition of mobile and slow components (e.g., hydrogen in metals, oxygen in oxides, and the transfer of molecules through membranes of different natures, including polymeric).

KAJIAN ADSORPSI ION LOGAM Cr(VI OLEH ADSORBEN KOMBINASI ARANG AKTIF SEKAM PADI DAN ZEOLIT MENGGUNAKAN METODE SOLID-PHASE SPECTROPHOTOMETRY (SPS

Directory of Open Access Journals (Sweden)

Sulistyo Saputro

2016-10-01

  This study aims to study the use of activated rice husk charcoal and zeolite as combination adsorbents to adsorb Cr(VI metal ions; the effect of the combination adsorbents of activated rice husk charcoal and zeolite’s compositions to adsorb Cr(VI metal ions; and the sensitivity of solid-phase spectrophotometry (SPS as a method to determine the reduced levels of Cr(VI metal ions in the level of 15μ"> g/L. The activated rice husk charcoal used were obtained through the activation process by soaking in a solution of ZnCl2 10% while the zeolite with a solution of H2SO4 10%. The contacting process of the adsorbents with Cr(VI metal ions was done by varying the compositions of the activated rice husk charcoal and zeolite adsorbent, 1:1, 1:2, 1:3, and 2:1. The data analysis of the Cr(VI level used solid-phase spectrophotometry (SPS method. Characterization of activated rice husk charcoal and zeolite used FTIR. The results showed that: (1 a combination of activated rice husk charcoal and zeolite can be used as adsorbent to adsorb Cr(VI metal ions with the adsorption capacity was 0,28 15μ"> g/g; (2 the optimum composition of adsorbents was 1:2 with the percentage of absorption was 40,99%; (3 solid-phase spectrophotometry (SPS is a sensitive method to determine the reduced levels of Cr(VI in the level of 15μ"> g/L with the limit of detection (LOD was 0,021 15μ"> g/L.   Keywords: adsorption, Cr(VI,  activated  rice husk charcoal,  zeolite, solid-phase spectrophotometry

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

Analytical study of solids-gas two phase flow

International Nuclear Information System (INIS)

Hosaka, Minoru

1977-01-01

Fundamental studies were made on the hydrodynamics of solids-gas two-phase suspension flow, in which very small solid particles are mixed in a gas flow to enhance the heat transfer characteristics of gas cooled high temperature reactors. Especially, the pressure drop due to friction and the density distribution of solid particles are theoretically analyzed. The friction pressure drop of two-phase flow was analyzed based on the analytical result of the single-phase friction pressure drop. The calculated values of solid/gas friction factor as a function of solid/gas mass loading are compared with experimental results. Comparisons are made for Various combinations of Reynolds number and particle size. As for the particle density distribution, some factors affecting the non-uniformity of distribution were considered. The minimum of energy dispersion was obtained with the variational principle. The suspension density of particles was obtained as a function of relative distance from wall and was compared with experimental results. It is concluded that the distribution is much affected by the particle size and that the smaller particles are apt to gather near the wall. (Aoki, K.)

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.

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.

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.

Tribological properties of solid lubricants filled glass fiber reinforced polyamide 6 composites

International Nuclear Information System (INIS)

Li, Du-Xin; You, Yi-Lan; Deng, Xin; Li, Wen-Juan; Xie, Ying

2013-01-01

Highlights: ► The tribological properties of GF/PA6 improved by the incorporation of PTFE. ► PTFE and UHMWPE exhibited a synergism effect on reducing friction coefficient. ► Solid lubricants enlarged the range of applied velocity for GF/PA6 composite. - Abstract: The main purpose of this paper is to further optimize the tribological properties of the glass fiber reinforced PA6 (GF/PA6,15/85 by weight) for high performance friction materials using single or combinative solid lubricants such as Polytetrafluroethylene (PTFE), ultra-high molecular weight polyethylene (UHMWPE) and the combination of both of them. Various polymer blends, where GF/PA6 acts as the polymer matrix and solid lubricants as the dispersed phase were prepared by injection molding. The tribological properties of these materials and the synergism as a result of the incorporation of both PTFE and UHMWPE were investigated. The results showed that, at a load of 40 N and a velocity of 200 rpm, PTFE was effective in improving the tribological capabilities of matrix material. On the contrary, UHMWPE was not conductive to maintain the structure integrity of GF/PA6 composite and harmful to the friction and wear properties. The combination of PTFE and UHMWPE showed synergism on further reducing the friction coefficient of the composites filled with either PTFE or UHMWPE only. Effects of load and velocity on tribological behavior were also discussed. To further understand the wear mechanism, the worn surfaces were examined by scanning electron microscopy

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.

Ni-Based Solid Oxide Cell Electrodes

DEFF Research Database (Denmark)

Mogensen, Mogens Bjerg; Holtappels, Peter

2013-01-01

This paper is a critical review of the literature on nickel-based electrodes for application in solid oxide cells at temperature from 500 to 1000 _C. The applications may be fuel cells or electrolyser cells. The reviewed literature is that of experimental results on both model electrodes...... and practical composite cermet electrodes. A substantially longer three-phase boundary (TPB) can be obtained per unit area of cell in such a composite of nickel and electrolyte material, provided that two interwoven solid networks of the two solid and one gaseous phases are obtained to provide a three...

Composition control of low-volatile solids through chemical vapor transport reactions. III. The example of gallium monoselenide: Control of the polytypic structure, non-stoichiometry and properties

International Nuclear Information System (INIS)

Zavrazhnov, A.; Naumov, A.; Sidey, V.; Pervov, V.

2012-01-01

Highlights: ► This work is devoted to the composition control of solids with selective CVT method. ► Phase identity and non-stoichiometry of solids (GaSe, etc.) depend on CVT-temperatures. ► The interrelation between the properties of GaSe and CVT conditions is also found. ► For iodide transporting system the diagram of phase stability of solids is adjusted. ► High temperatures and Se-rich non-stoichiometry are necessary for γ-GaSe stability. - Abstract: By means of particular examples, the present work demonstrates the possibility of directed delicate non-destructive control of structure, composition and properties of inorganic solids using the method of selective chemical vapor transport (SCVT). Gallium monoselenide GaSe is the main model object. Additional, though less detailed, explanation is given by the example of gallium monosulfide GaS. Experimental evidences on the possibility of the control of polytypic structure, non-stoichiometry and properties of gallium monoselenide were obtained in non-isothermal variant of selective chemical vapor transport which has non-destructive character. Diagnostics of the phase (polytypic) composition and non-stoichiometry of GaSe was performed with the use of X-ray diffractometry as well as with the use of cathode luminescence spectra. It was experimentally found that there exists a connection of non-stoichiometry and the properties of gallium selenides with the determining conditions of selective chemical vapor transport: temperature of controlled sample (T 2 ) and the difference of temperatures between the hot and cold zones (ΔT). It is shown that the phase diagram of Ga–Se system needs to be partially revised near the composition of Ga 1 Se 1 . The reason for such revision is the fact that two polytypes (ε-GaSe and γ-GaSe) exist on this phase diagram as independent phases.

Solid-phase photocatalytic degradation of polyethylene film with manganese oxide OMS-2

Science.gov (United States)

Liu, Guanglong; Liao, Shuijiao; Zhu, Duanwei; Cui, Jingzhen; Zhou, Wenbing

2011-01-01

Solid-phase photocatalytic degradation of polyethylene (PE) film with cryptomelane-type manganese oxide (OMS-2) as photocatalyst was investigated in the ambient air under ultraviolet and visible light irradiation. The properties of the composite films were compared with those of the pure PE film through performing weight loss monitoring, IR spectroscopy, scanning electron microscopic (SEM) and X-ray photoelectron spectroscopy (XPS). The photoinduced degradation of PE-OMS-2 composite films was higher than that of the pure films, while there has been little change under the visible light irradiation. The weight loss of PE-OMS-2 (1.0 wt%) composite films steadily decreased and reached 16.5% in 288 h under UV light irradiation. Through SEM observation there were some cavities on the surface of composite films, but few change except some surface chalking phenomenon occurred in pure PE film. The degradation rate with ultraviolet irradiation is controllable by adjusting the content of OMS-2 particles in PE plastic. Finally, the mechanism of photocatalytic degradation of the composite films was briefly discussed.

Microencapsulated Phase Change Composite Materials for Energy Efficient Buildings

Science.gov (United States)

Thiele, Alexander

This study aims to elucidate how phase change material (PCM)-composite materials can be leveraged to reduce the energy consumption of buildings and to provide cost savings to ratepayers. Phase change materials (PCMs) can store thermal energy in the form of latent heat when subjected to temperatures exceeding their melting point by undergoing a phase transition from solid to liquid state. Reversibly, PCMs can release this thermal energy when the system temperature falls below their solidification point. The goal in implementing composite PCM walls is to significantly reduce and time-shift the maximum thermal load on the building in order to reduce and smooth out the electricity demand for heating and cooling. This Ph.D. thesis aims to develop a set of thermal design methods and tools for exploring the use of PCM-composite building envelopes and for providing design rules for their practical implementation. First, detailed numerical simulations were used to show that the effective thermal conductivity of core-shell-matrix composites depended only on the volume fraction and thermal conductivity of the constituent materials. The effective medium approximation reported by Felske (2004) was in very good agreement with numerical predictions of the effective thermal conductivity. Second, a carefully validated transient thermal model was used to simulate microencapsulated PCM-composite walls subjected to diurnal or annual outdoor temperature and solar radiation flux. It was established that adding microencapsulated PCM to concrete walls both substantially reduced and delayed the thermal load on the building. Several design rules were established, most notably, (i) increasing the volume fraction of microencapsulated PCM within the wall increases the energy savings but at the potential expense of mechanical properties [1], (ii) the phase change temperature leading to the maximum energy and cost savings should equal the desired indoor temperature regardless of the climate

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.

Phase Relations in Ternary Systems in the Subsolidus Region: Methods to Formulate Solid Solution Equations and to Find Particular Compositions

Science.gov (United States)

Alvarez-Montan~o, Victor E.; Farías, Mario H.; Brown, Francisco; Mun~oz-Palma, Iliana C.; Cubillas, Fernando; Castillon-Barraza, Felipe F.

2017-01-01

A good understanding of ternary phase diagrams is required to advance and/or to reproduce experimental research in solid-state and materials chemistry. The aim of this paper is to describe the solutions to problems that appear when studying or determining ternary phase diagrams. A brief description of the principal features shown in phase diagrams…

Physicochemical investigation of Bi2MoO6 solid-phase interaction with Sm2MoO6

International Nuclear Information System (INIS)

Khajkina, E.G.; Kovba, L.M.; Bazarova, Zh.G.; Khal'baeva, K.M.; Khakhinov, V.V.; Mokhosoev, M.V.

1986-01-01

Bi 2 MoO 6 -Sm 2 MoO 6 interaction in the temperature range of 700-1000 deg C is studied using X-ray phase analysis and vibrational spectroscopy. Formation of monoclinic solid solutions based on γ'-Bi 2 MoO 6 and B 2-x Sm x MoO 6 varied composition phase with α-Ln 2 MoO 6 structure which homogeneity region extent at 1000 deg C constitutes ∼ 50 mol % (0.7≤x≤1.7) is stated. Crystallographic characteristics of the synthesized phases are determined

Composition of municipal solid waste in Denmark

DEFF Research Database (Denmark)

Edjabou, Vincent Maklawe Essonanawe; Petersen, Claus; Scheutz, Charlotte

2014-01-01

Data for the composition of municipal solid waste is a critical basis for any assessment of waste technologies and waste management systems. The detailed quantification of waste fractions is absolutely needed for a better technological development of waste treatment. The current waste composition...... comparability to characterize municipal solid waste. This methodology was applied to residual waste collected from 1,442 households in three municipalities in Denmark. The main fractions contributing to the residual household waste were food waste and miscellaneous waste. Statistical analysis suggested...... of standardised and commonly accepted waste characterization methodologies, various approaches have been reported in literature. This limits both comparability and applicability of the results. The purpose of this study was to introduce a consistent methodology that reduces uncertainties and ensures data...

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...

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.

Comparison of the solid-phase extraction efficiency of a bounded and an included cyclodextrin-silica microporous composite for polycyclic aromatic hydrocarbons determination in water samples.

Science.gov (United States)

Mauri-Aucejo, Adela; Amorós, Pedro; Moragues, Alaina; Guillem, Carmen; Belenguer-Sapiña, Carolina

2016-08-15

Solid-phase extraction is one of the most important techniques for sample purification and concentration. A wide variety of solid phases have been used for sample preparation over time. In this work, the efficiency of a new kind of solid-phase extraction adsorbent, which is a microporous material made from modified cyclodextrin bounded to a silica network, is evaluated through an analytical method which combines solid-phase extraction with high-performance liquid chromatography to determine polycyclic aromatic hydrocarbons in water samples. Several parameters that affected the analytes recovery, such as the amount of solid phase, the nature and volume of the eluent or the sample volume and concentration influence have been evaluated. The experimental results indicate that the material possesses adsorption ability to the tested polycyclic aromatic hydrocarbons. Under the optimum conditions, the quantification limits of the method were in the range of 0.09-2.4μgL(-1) and fine linear correlations between peak height and concentration were found around 1.3-70μgL(-1). The method has good repeatability and reproducibility, with coefficients of variation under 8%. Due to the concentration results, this material may represent an alternative for trace analysis of polycyclic aromatic hydrocarbons in water trough solid-phase extraction. Copyright © 2016 Elsevier B.V. All rights reserved.

Changes in volatile compound composition of Antrodia camphorata during solid state fermentation.

Science.gov (United States)

Xia, Yongjun; Zhang, Baorong; Li, Weijiang; Xu, Ganrong

2011-10-01

Although the volatiles present in mushrooms and fungi have been investigated by many researchers, including Antrodia camphorata in submerged fermentation, there are few data available regarding changes in volatile compounds during fermentation. Our research has revealed that solid state fermentation of A. camphorata is highly odiferous compared with submerged cultures and the odor changed with increasing culture time. Therefore the aim of this study was to investigate the changes in volatile compound composition of A. camphorata during solid state fermentation. Altogether, 124 major volatile compounds were identified. The volatile compounds produced by A. camphorata during growth in solid state fermentation were quite different. Oct-1-en-3-ol, octan-3-one and methyl 2-phenylacetate were predominant in exponential growth phase production, while the dominant volatiles produced in stationary phase were octan-3-one and methyl 2-phenylacetate. In stationary phase, lactone compounds in A. camphorata, such as 5-butyloxolan-2-one, 5-heptyloxolan-2-one, 6-heptyloxan-2-one, contributed greatly to peach and fruit-like flavor. Terpene and terpene alcohol compounds, such as 1-terpineol, L-linalool, T-cadinol, (E, E)-farnesol, β-elemene, cis-α-bisabolene and α-muurolene, made different contributions to herbal fresh aroma in A. camphorata. Nineteen volatile sesquiterpenes were detected from solid state fermentation of A. camphorata. The compounds 5-n-butyl-5H-furan-2-one, β-ionone, (-)-caryophyllene oxide, aromadendrene oxide, diepi-α-cedrene epoxide, β-elemene, α-selinene, α-muurolene, azulene, germacrene D, γ-cadinene and 2-methylpyrazine have not hitherto been reported in A. camphorata. The preliminary results suggest that the aroma-active compounds produced by A camphorata in solid state fermentation might serve as an important source of natural aroma compounds for the food and cosmetic industries or antibiotic activity compounds. The sesquiterpenes could be

A simplified radiometabolite analysis procedure for PET radioligands using a solid phase extraction with micellar medium

International Nuclear Information System (INIS)

Nakao, Ryuji; Halldin, Christer

2013-01-01

A solid phase extraction method has been developed for simple and high-speed direct determination of PET radioligands in plasma. Methods: This methodology makes use of a micellar medium and a solid-phase extraction cartridge for displacement of plasma protein bound radioligand and separation of PET radioligands from their radiometabolites without significant preparation. The plasma samples taken from monkey or human during PET measurements were mixed with a micellar eluent containing an anionic surfactant sodium dodecyl sulphate and loaded onto SPE cartridges. The amount of radioactivity corresponding to parent radioligand (retained on the cartridge) and its radioactive metabolites (eluted with micellar eluent) was measured. Results: Under the optimized conditions, excellent separation of target PET radioligands from their radiometabolites was achieved with a single elution and short run-time of 1 min. This method was successfully applied to study the metabolism for 11 C-labelled radioligands in human or monkey plasma. The amount of parent PET radioligands estimated by micellar solid phase extraction strongly corresponded with that determined by radio-LC. The improved throughput permitted the analysis of a large number of plasma samples (up to 13 samples per one PET study) for accurate estimation of metabolite-corrected input function during quantitative PET imaging studies. Conclusion: Solid phase extraction together with micellar medium is fast, sensitive and easy to use, and therefore it is an attractive alternative method to determine relative composition of PET radioligands in plasma

A novel poly(deep eutectic solvent)-based magnetic silica composite for solid-phase extraction of trypsin

Energy Technology Data Exchange (ETDEWEB)

Xu, Kaijia [State Key Laboratory of Chemo/Biosensing and Chemometrics, College of Chemistry and Chemical Engineering, Hunan University, Changsha, 410082 (China); Wang, Yuzhi, E-mail: wyzss@hnu.edu.cn [State Key Laboratory of Chemo/Biosensing and Chemometrics, College of Chemistry and Chemical Engineering, Hunan University, Changsha, 410082 (China); Li, Yixue; Lin, Yunxuan; Zhang, Haibao [State Key Laboratory of Chemo/Biosensing and Chemometrics, College of Chemistry and Chemical Engineering, Hunan University, Changsha, 410082 (China); Zhou, Yigang [Department of Microbiology, College of Basic Medicine, Central South University, Changsha, 410083 (China)

2016-11-23

Novel poly(deep eutectic solvent) grafted silica-coated magnetic microspheres (Fe{sub 3}O{sub 4}@SiO{sub 2}-MPS@PDES) were prepared by polymerization of choline chloride-itaconic acid (ChCl-IA) and γ-MPS-modified magnetic silica composites, and were characterized by vibrating sample magnetometer (VSM), Fourier transform infrared spectrometry (FT-IR), X-ray photoelectron spectra (XPS), thermal gravimetric analysis (TGA) and transmission electron microscope (TEM). Then the synthetic Fe{sub 3}O{sub 4}@SiO{sub 2}-MPS@PDES microspheres were applied for the magnetic solid-phase extraction (MSPE) of trypsin for the first time. After extraction, the concentration of trypsin in the supernatant was determined by a UV–vis spectrophotometer. Single factor experiments were carried out to investigate the effects of the extraction process, including the concentration of trypsin, the ionic strength, the pH value, the extraction time and the temperature. Experimental results showed the extraction capacity could reach up to 287.5 mg/g under optimized conditions. In comparison with Fe{sub 3}O{sub 4}@SiO{sub 2}-MPS, Fe{sub 3}O{sub 4}@SiO{sub 2}-MPS@PDES displayed higher extraction capacity and selectivity for trypsin. According to the regeneration studies, Fe{sub 3}O{sub 4}@SiO{sub 2}-MPS@PDES microspheres can be recycled six times without significant loss of its extraction capacity, and retained a high extraction capacity of 233 mg/g after eight cycles. Besides, the activity studies also demonstrated that the activity of the extracted trypsin was well retained. Furthermore, the analysis of real sample revealed that the prepared magnetic microspheres can be used to purify trypsin in crude bovine pancreas extract. These results highlight the potential of the proposed Fe{sub 3}O{sub 4}@SiO{sub 2}-MPS@PDES-MSPE method in separation of biomolecules. - Highlights: • A strategy for solid-phase extraction of trypsin based on poly(deep eutectic solvent) modified magnetic silica

Carbon nanotube-based benzyl polymethacrylate composite monolith as a solid phase extraction adsorbent and a stationary phase material for simultaneous extraction and analysis of polycyclic aromatic hydrocarbon in water.

Science.gov (United States)

Al-Rifai, Asma'a; Aqel, Ahmad; Wahibi, Lamya Al; ALOthman, Zeid A; Badjah-Hadj-Ahmed, Ahmed-Yacine

2018-02-02

A composite of multi-walled carbon nanotubes incorporated into a benzyl methacrylate-co-ethylene dimethacrylate porous monolith was prepared, characterized and used as solid phase adsorbent and as stationary phase for simultaneous extraction and separation of ten polycyclic aromatic hydrocarbons, followed by nano-liquid chromatography analysis. The extraction and chromatographic parameters were optimized with regard to the extraction efficiency and the quality of chromatographic analytes separation. Under the optimized conditions, all PAHs were separated in 13 min with suitable resolution values (Rs = 1.74-3.98). Addition of a small amount of carbon nanotubes (0.1% with respect to monomers) to the polymerization mixture increased the efficiency for the separation column to over 41,700 plates m -1 for chrysene at flow rate of 0.5 μL min -1 . The method showed a wide linear range (1-500 μg L -1 with R 2 more than 0.9938), acceptable extraction repeatability (RSDs extraction cartridges) and satisfactory detection limits (0.02-0.22 μg L -1 ). Finally, the proposed method was successfully applied to the detection of polycyclic aromatic hydrocarbons in environmental water samples. After a simple extraction procedure with preconcentration factor equal to 100, the average recovery values in ultra-pure, tap and sea water samples were found to be in the range 81.3-95.4% with %RSD less than 6.4. Again, the presence of carbon nanotubes (0.3% relatively to monomers) in native polymer enhanced the extraction performance for the solid phase adsorbent up to 78.4%. The application of the monoliths modified with CNTs in extraction and nano-scale liquid chromatography for analysis of environmental samples offered several advantages; it demonstrated an acceptable precision, low detection limits, good reproducibility, satisfying recoveries and wide dynamic linear ranges. Copyright © 2018. Published by Elsevier B.V.

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.

Phase Composition Maps integrate mineral compositions with rock textures from the micro-meter to the thin section scale

Science.gov (United States)

Willis, Kyle V.; Srogi, LeeAnn; Lutz, Tim; Monson, Frederick C.; Pollock, Meagen

2017-12-01

Textures and compositions are critical information for interpreting rock formation. Existing methods to integrate both types of information favor high-resolution images of mineral compositions over small areas or low-resolution images of larger areas for phase identification. The method in this paper produces images of individual phases in which textural and compositional details are resolved over three orders of magnitude, from tens of micrometers to tens of millimeters. To construct these images, called Phase Composition Maps (PCMs), we make use of the resolution in backscattered electron (BSE) images and calibrate the gray scale values with mineral analyses by energy-dispersive X-ray spectrometry (EDS). The resulting images show the area of a standard thin section (roughly 40 mm × 20 mm) with spatial resolution as good as 3.5 μm/pixel, or more than 81 000 pixels/mm2, comparable to the resolution of X-ray element maps produced by wavelength-dispersive spectrometry (WDS). Procedures to create PCMs for mafic igneous rocks with multivariate linear regression models for minerals with solid solution (olivine, plagioclase feldspar, and pyroxenes) are presented and are applicable to other rock types. PCMs are processed using threshold functions based on the regression models to image specific composition ranges of minerals. PCMs are constructed using widely-available instrumentation: a scanning-electron microscope (SEM) with BSE and EDS X-ray detectors and standard image processing software such as ImageJ and Adobe Photoshop. Three brief applications illustrate the use of PCMs as petrologic tools: to reveal mineral composition patterns at multiple scales; to generate crystal size distributions for intracrystalline compositional zones and compare growth over time; and to image spatial distributions of minerals at different stages of magma crystallization by integrating textures and compositions with thermodynamic modeling.

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.

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.

Continuous solid-state phase transitions in energy storage materials with orientational disorder – Computational and experimental approach

International Nuclear Information System (INIS)

Singh, Harpreet; Talekar, Anjali; Chien, Wen-Ming; Shi, Renhai; Chandra, Dhanesh; Mishra, Amrita; Tirumala, Muralidhar; Nelson, Daryl J.

2015-01-01

We report on TES (thermal energy storage) in new CT (continuous phase transitions) in multicomponent tetrahederally configured (orientationally disordered) crystals of NPG-neopentylglycol-C 5 H 12 O 2 , PG-pentaglycerine-C 5 H 12 O 3 , and PE-pentaerythritol-C 5 H 12 O 4 . This discovery is applicable in thermal energy storage in many systems which do not require conventional isothermal first-order phase transition energy storage. The above compounds exhibit polymorphs of orientationally disordered phases in which O–H…O bond rotation around the C–C bond stores significant amount of energy; for example, in PE 41.26 kJ/mol are absorbed isothermally during solid–solid transitions. In this paper we show, anisothermal continuous phase transitions (CT), due to compositional changes with changes in temperature, associated with a measurable amount of energy, not reported earlier. The correlation of phase stability regions in pseudo-binaries, calculated from ternary NPG–PG–PE phase diagrams, is validated by experimental ternary DSC (differential scanning calorimetry) and in-situ x-ray diffraction data. We established equations for determining the CT in a temperature range, and their respective enthalpies of transitions for any composition of the ternaries. Thermodynamic calculations of the Gibbs energies of the solution phases are modeled as substitutional solid solutions, in which the excess Gibbs energies are expressed by the Redlich–Kister–Muggianu polynomial. There is excellent agreement between the experimental and CALPHAD calculated data. - Highlights: • Continuous phase transition (CT) thermal energy storage in organic ternary system. • Anisothermal temperature ramping leads to CT transitions as per lever rule. • Orientationally disordered phases store energy in O–H…O bond rotation/oscillation. • Validated calculated data with measured thermodynamic properties in ternary system. • Used CALPHAD methodology to calculate Gibbs energies of

Martensitic transformation between competing phases in Ti–Ta alloys: a solid-state nudged elastic band study

International Nuclear Information System (INIS)

Chakraborty, Tanmoy; Rogal, Jutta; Drautz, Ralf

2015-01-01

A combined density functional theory and solid-state nudged elastic band study is presented to investigate the martensitic transformation between β → (α″, ω) phases in the Ti–Ta system. The minimum energy paths along the transformation are calculated and the transformation mechanisms as well as relative stabilities of the different phases are discussed for various compositions. The analysis of the transformation paths is complemented by calculations of phonon spectra to determine the dynamical stability of the β, α″, and ω phase. Our theoretical results confirm the experimental findings that with increasing Ta concentration there is a competition between the destabilisation of the α″ and ω phase and the stabilisation of the high-temperature β phase. (paper)

Preparation and characterization of form-stable paraffin/polyurethane composites as phase change materials for thermal energy storage

International Nuclear Information System (INIS)

Chen, Keping; Yu, Xuejiang; Tian, Chunrong; Wang, Jianhua

2014-01-01

Highlights: • Paraffin/polyurethane composite as form-stable phase change material was prepared by bulk polymerization. • Paraffin/polyurethane composite possesses typical character of dual phase transition. • Total latent heat of n-eicosane/PUPCM is as high as 141.2 J/g. • Maximum encapsulation ratio for n-octadecane/PUPCM composites is 25% w/w. - Abstract: Polyurethane phase change material (PUPCM) has been demonstrated to be effective solid–solid phase change material for thermal energy storage. However, the high cost and complex process on preparation of PUPCMs with high enthalpy and broad phase transition temperature range can prohibit industrial-scale applications. In this work, a series of novel form-stable paraffin/PUPCMs composites (n-octadecane/PUPCM, n-eicosane/PUPCM and paraffin wax/PUPCM) with high enthalpy and broad phase transition temperature range (20–65 °C) were directly synthesized via bulk polymerization. The composites were prepared at different mass fractions of n-octadecane (10, 20, 25, 30% w/w). The results indicated that the maximum encapsulation ratio for n-octadecane/PUPCM10000 composites was around 25% w/w. The chemical structure and crystalline properties of these composites were characterized by Fourier transform infrared spectroscopy (FT-IR), polarizing optical microscopy (POM), wide-angle X-ray diffraction (WAXD). Thermal properties and thermal reliability of the composites were determined using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). From DSC analysis, the composites showed a typical dual phase change temperature. The enthalpy for the composite with 25% w/w n-eicosane was as high as 141.2 J/g. TGA analysis indicated that the composites degraded at considerably high temperatures. The process of preparation of PUPCMs and their composites was very simple, inexpensive, environmental friendly and easy to process into desired shapes, which could find the promising applications in solar

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.

Mathematical micro-model of a solid oxide fuel cell composite cathode

International Nuclear Information System (INIS)

Kenney, B.; Karan, K.

2004-01-01

In a solid oxide fuel cell (SOFC), the cathode processes account for a majority of the overall electrochemical losses. A composite cathode comprising a mixture of ion-conducting electrolyte and electron-conducting electro-catalyst can help minimize cathode losses provided microstructural parameters such as particle-size, composition, and porosity are optimized. The cost of composite cathode research can be greatly reduced by incorporating mathematical models into the development cycle. Incorporated with reliable experimental data, it is possible to conduct a parametric study using a model and the predicted results can be used as guides for component design. Many electrode models treat the cathode process simplistically by considering only the charge-transfer reaction for low overpotentials or the gas-diffusion at high overpotentials. Further, in these models an average property of the cathode internal microstructure is assumed. This paper will outline the development of a 1-dimensional SOFC composite cathode micro-model and the experimental procedures for obtaining accurate parameter estimates. The micro-model considers the details of the cathode microstructure such as porosity, composition and particle-size of the ionic and electronic phases, and their interrelationship to the charge-transfer reaction and mass transport processes. The micro-model will be validated against experimental data to determine its usefulness for performance prediction. (author)

A New Class of Ternary Compound for Lithium-Ion Battery: from Composite to Solid Solution.

Science.gov (United States)

Wang, Jiali; Wu, Hailong; Cui, Yanhua; Liu, Shengzhou; Tian, Xiaoqing; Cui, Yixiu; Liu, Xiaojiang; Yang, Yin

2018-02-14

Searching for high-performance cathode materials is a crucial task to develop advanced lithium-ion batteries (LIBs) with high-energy densities for electrical vehicles (EVs). As a promising lithium-rich material, Li 2 MnO 3 delivers high capacity over 200 mAh g -1 but suffers from poor structural stability and electronic conductivity. Replacing Mn 4+ ions by relatively larger Sn 4+ ions is regarded as a possible strategy to improve structural stability and thus cycling performance of Li 2 MnO 3 material. However, large difference in ionic radii of Mn 4+ and Sn 4+ ions leads to phase separation of Li 2 MnO 3 and Li 2 SnO 3 during high-temperature synthesis. To prepare solid-solution phase of Li 2 MnO 3 -Li 2 SnO 3 , a buffer agent of Ru 4+ , whose ionic radius is in between that of Mn 4+ and Sn 4+ ions, is introduced to assist the formation of a single solid-solution phase. The results show that the Li 2 RuO 3 -Li 2 MnO 3 -Li 2 SnO 3 ternary system evolves from mixed composite phases into a single solid-solution phase with increasing Ru content. Meanwhile, discharge capacity of this ternary system shows significantly increase at the transformation point which is ascribed to the improvement of Li + /e - transportation kinetics and anionic redox chemistry for solid-solution phase. The role of Mn/Sn molar ratio of Li 2 RuO 3 -Li 2 MnO 3 -Li 2 SnO 3 ternary system has also been studied. It is revealed that higher Sn content benefits cycling stability of the system because Sn 4+ ions with larger sizes could partially block the migration of Mn 4+ and Ru 4+ from transition metal layer to Li layer, thus suppressing structural transformation of the system from layered-to-spinel phase. These findings may enable a new route for exploring ternary or even quaternary lithium-rich cathode materials for LIBs.

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

Anti-perovskite solid electrolyte compositions

Science.gov (United States)

Zhao, Yusheng; Daemen, Luc Louis

2015-12-26

Solid electrolyte antiperovskite compositions for batteries, capacitors, and other electrochemical devices have chemical formula Li.sub.3OA, Li.sub.(3-x)M.sub.x/2OA, Li.sub.(3-x)N.sub.x/3OA, or LiCOX.sub.zY.sub.(1-z), wherein M and N are divalent and trivalent metals respectively and wherein A is a halide or mixture of halides, and X and Y are halides.

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

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

Kinetic study of solid phase demineralization by weak acids in one-step enzymatic bio-refinery of shrimp cuticles

OpenAIRE

Baron, Regis; Socol, Marius; Arhaliass, A.; Bruzac, Sandrine; Le Roux, Karine; Del Pino, J. Rodriguez; Berge, Jean-pascal; Kaas, Raymond

2015-01-01

We describe a one-step bio-refinery process for shrimp composites by-products. Its originality lies in a simple rapid (6 h) biotechnological cuticle fragmentation process that recovers all major compounds (chitins, peptides and minerals in particular calcium). The process consists of a controlled exogenous enzymatic proteolysis in a food-grade acidic medium allowing chitin purification (solid phase), and recovery of peptides and minerals (liquid phase). At a pH of between 3.5 and 4, protease ...

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.

Design of Low-Melting Point Compositions Suitable for Transient Liquid Phase Sintering of PM Steels Based on a Thermodynamic and Kinetic Study

Science.gov (United States)

Bernardo, Elena; de Oro, Raquel; Campos, Mónica; Torralba, José Manuel

2014-04-01

The possibility of tailoring the characteristics of a liquid metal is an important asset in a wide number of processing techniques. For most of these processes, the nature and degree of the interaction between liquid and solid phases are usually a focus of interest since they determine liquid properties such as wettability and infiltration capacity. Particularly, within the powder metallurgy (PM) technology, it is considered one of the key aspects to obtain high performance steels through liquid phase sintering. In this work, it is proved how thermodynamic and kinetics software is a powerful tool to study the liquid/solid interactions. The assessment of different liquid phase promoters for transient liquid phase sintering is addressed through the use of ThermoCalc and DICTRA calculations. Besides melting temperatures, particular attention is given to the solubility phenomena between the phases and the kinetics of these processes. Experimental validation of thermodynamic results is carried out by wetting and infiltration experiments at high temperatures. Compositions presenting different liquid/solid solubility are evaluated and directly correlated to the behavior of the liquid during a real sintering process. Therefore, this work opens the possibility to optimize liquid phase compositions and predict the liquid behavior from the design step, which is considered of high technological value for the PM industry.

The influence of precipitation temperature on the properties of ceria–zirconia solid solution composites

International Nuclear Information System (INIS)

Cui, Yajuan; Fang, Ruimei; Shang, Hongyan; Shi, Zhonghua; Gong, Maochu; Chen, Yaoqiang

2015-01-01

Highlights: • The crystallite size of precipitate increases as the precipitation temperature rises. • The stack of large crystallite can form nanoparticles with big pore size. • Big pore sizes are advantageous to improve the thermal stability. • Phase segregation is restricted in CZ solid solution precipitated at 70 °C. • The reducibility and OSC of the solid solution precipitated at 70 °C are improved. - Abstract: The ceria–zirconia composites (CZ) with a Ce/Zr mass ratio of 1/1 were synthesized by a back-titration method, in which the influence of precipitation temperature on the properties of ceria–zirconia precipitates was investigated. The resulting precipitation and mixed oxides at different precipitation temperatures were then characterized by a range of techniques, including textural properties, X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscope (SEM), X-ray photoelectron spectroscopy (XPS), H 2 -temperature programmed reduction (H 2 -TPR) as well as oxygen storage capacity (OSC) measurement. The results revealed that ceria–zirconia composites were formed as solid solution and such structure is favored of thermostability and texture properties. In particular, the composite CZ-70 synthesized at 70 °C exhibited prominent thermostability with a surface area of 32 m 2 /g as well as a pore volume of 0.15 cc/g after aging treatment at 1000 °C for 5 h. And this was found to be associated with the wider pore size distribution which maybe owed to the formation of large crystal at the primary stage of precipitation. Additionally, the composite CZ-70 showed excellent reduction property and OSC benefiting from stable texture and structure

Liquid-solid phase transition of Ge-Sb-Te alloy observed by in-situ transmission electron microscopy

Energy Technology Data Exchange (ETDEWEB)

Berlin, Katja, E-mail: katja.berlin@pdi-berlin.de; Trampert, Achim

2017-07-15

Melting and crystallization dynamics of the multi-component Ge-Sb-Te alloy have been investigated by in-situ transmission electron microscopy (TEM). Starting point of the phase transition study is an ordered hexagonal Ge{sub 1}Sb{sub 2}Te{sub 4} thin film on Si(111) where the crystal structure and the chemical composition are verified by scanning TEM and electron energy-loss spectroscopy, respectively. The in-situ observation of the liquid phase at 600°C including the liquid-solid and liquid-vacuum interfaces and their movements was made possible due to an encapsulation of the TEM sample. The solid-liquid interface during melting displays a broad and diffuse transition zone characterized by a vacancy induced disordered state. Although the velocities of interface movements are measured to be in the nanometer per second scale, both, for crystallization and solidification, the underlying dynamic processes are considerably different. Melting reveals linear dependence on time, whereas crystallization exhibits a non-linear time-dependency featuring a superimposed start-stop motion. Our results may provide valuable insight into the atomic mechanisms at interfaces during the liquid-solid phase transition of Ge-Sb-Te alloys. - Highlights: • In-situ TEM observation of liquid Ge-Sb-Te phase transition due to encapsulation. • During melting: Observation of non-ordered interface transition due to premelting. • During solidification: Observation of non-linear time-dependent crystallization.

Liquid-solid phase transition of Ge-Sb-Te alloy observed by in-situ transmission electron microscopy

International Nuclear Information System (INIS)

Berlin, Katja; Trampert, Achim

2017-01-01

Melting and crystallization dynamics of the multi-component Ge-Sb-Te alloy have been investigated by in-situ transmission electron microscopy (TEM). Starting point of the phase transition study is an ordered hexagonal Ge 1 Sb 2 Te 4 thin film on Si(111) where the crystal structure and the chemical composition are verified by scanning TEM and electron energy-loss spectroscopy, respectively. The in-situ observation of the liquid phase at 600°C including the liquid-solid and liquid-vacuum interfaces and their movements was made possible due to an encapsulation of the TEM sample. The solid-liquid interface during melting displays a broad and diffuse transition zone characterized by a vacancy induced disordered state. Although the velocities of interface movements are measured to be in the nanometer per second scale, both, for crystallization and solidification, the underlying dynamic processes are considerably different. Melting reveals linear dependence on time, whereas crystallization exhibits a non-linear time-dependency featuring a superimposed start-stop motion. Our results may provide valuable insight into the atomic mechanisms at interfaces during the liquid-solid phase transition of Ge-Sb-Te alloys. - Highlights: • In-situ TEM observation of liquid Ge-Sb-Te phase transition due to encapsulation. • During melting: Observation of non-ordered interface transition due to premelting. • During solidification: Observation of non-linear time-dependent crystallization.

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

Science.gov (United States)

Benson, D. K.; Christensen, C.

1983-11-01

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

Phase separation in biopolymer gels: a low- to high-solid exploration of structural morphology and functionality.

Science.gov (United States)

Kasapis, Stefan

2008-04-01

Phase separation in protein and polysaccharide gels remains one of the basic tools of achieving the required structural properties and textural profile in food product formulations. As ever, the industrialist is faced with the challenge of innovation in an increasingly competitive market in terms of ingredient cost, product added-value, and expectations of a healthy life-style to mention but a few. It appears, however, that a gap persists between the fundamental knowledge and a direct application to food related concepts with a growing need for scientific input. Furthermore, within the context of materials science, there is a tendency to examine research findings in either low- or high-solid systems without considering synergistic insights/benefits to contemporary needs, spanning the full range of relevant time-, length-, and concentration scales. This review highlights the latest attempts made to utilize and further develop fundamental protocols from the advanced synthetic polymer research as a source of inspiration for contemporary bio-related applications in low- and intermediate-solid composite gels. Then, it takes advantage of this school of thought to "force a passage" through the phase topology and molecular dynamics of binary biopolymer mixtures at high levels of co-solute. It is hoped that these phenomenological and fundamental tools should be able to bridge the divide in the analysis of the two "types" of composite materials (from low to high solids) thus dealing effectively with the specific and often intricate problems of their science and applications.

Manganese oxalate nanorods as ballistic modifier for composite solid propellants

Energy Technology Data Exchange (ETDEWEB)

Singh, Supriya [Department of Chemistry, DDU Gorakhpur University, Gorakhpur 273009, U.P. (India); Chawla, Mohit [School of Basic Sciences, Indian Institute of Technology Mandi, Mandi 175005, H.P. (India); Siril, Prem Felix, E-mail: prem@iitmandi.ac.in [School of Basic Sciences, Indian Institute of Technology Mandi, Mandi 175005, H.P. (India); Singh, Gurdip [Department of Chemistry, DDU Gorakhpur University, Gorakhpur 273009, U.P. (India)

2014-12-10

Highlights: • Manganese oxalate nanorods were prepared using mild thermal precipitation and aging. • The nanorods were found to be efficient ballistic modifier for solid propellants. • The nanorods sensitized the thermolysis of ammonium perchlorate. • Controlled thermal decomposition of nanorods yielded manganese oxide nanoparticles. • MnO nanoparticles formed insitu in the condensed phase enhance the burning rates. - Abstract: Rod-shaped nanostructures of manganese oxalate (MnC{sub 2}O{sub 4}) were synthesized via mild thermal precipitation and aging process. Chemical composition of the MnC{sub 2}O{sub 4} nanorods was confirmed using Fourier transform infra-red (FTIR) spectroscopy and energy dispersive X-ray spectroscopy (EDS). X-ray diffraction (XRD) and selected area electron diffraction (SAED) studies revealed the crystal structure. Field emission scanning electron microscopy (FE-SEM) imaging and high resolution transmission electron microscopy (HR-TEM) were employed to study the structural features of the nanorods. The MnC{sub 2}O{sub 4} nanorods were found to be efficient ballistic modifier for the burning rate enhancement of composite solid propellants (CSPs). Thermal analysis using TGA-DSC showed that MnC{sub 2}O{sub 4} nanorods sensitized the thermal decomposition of ammonium perchlorate (AP) and the CSPs. Controlled thermal decomposition of the MnC{sub 2}O{sub 4} nanorods resulted in the formation of managanese oxide nanoparticles with mesoporosity. A plausible mechanism for the burning rate enhancement using MnC{sub 2}O{sub 4} nanorods was proposed.

Solid polymer electrolyte composite membrane comprising plasma etched porous support

Science.gov (United States)

Liu, Han; LaConti, Anthony B.

2010-10-05

A solid polymer electrolyte composite membrane and method of manufacturing the same. According to one embodiment, the composite membrane comprises a rigid, non-electrically-conducting support, the support preferably being a sheet of polyimide having a thickness of about 7.5 to 15 microns. The support has a plurality of cylindrical pores extending perpendicularly between opposing top and bottom surfaces of the support. The pores, which preferably have a diameter of about 0.1 to 5 microns, are made by plasma etching and preferably are arranged in a defined pattern, for example, with fewer pores located in areas of high membrane stress and more pores located in areas of low membrane stress. The pores are filled with a first solid polymer electrolyte, such as a perfluorosulfonic acid (PFSA) polymer. A second solid polymer electrolyte, which may be the same as or different than the first solid polymer electrolyte, may be deposited over the top and/or bottom of the first solid polymer electrolyte.

Solid polymer electrolyte composite membrane comprising laser micromachined porous support

Science.gov (United States)

Liu, Han [Waltham, MA; LaConti, Anthony B [Lynnfield, MA; Mittelsteadt, Cortney K [Natick, MA; McCallum, Thomas J [Ashland, MA

2011-01-11

A solid polymer electrolyte composite membrane and method of manufacturing the same. According to one embodiment, the composite membrane comprises a rigid, non-electrically-conducting support, the support preferably being a sheet of polyimide having a thickness of about 7.5 to 15 microns. The support has a plurality of cylindrical pores extending perpendicularly between opposing top and bottom surfaces of the support. The pores, which preferably have a diameter of about 5 microns, are made by laser micromachining and preferably are arranged in a defined pattern, for example, with fewer pores located in areas of high membrane stress and more pores located in areas of low membrane stress. The pores are filled with a first solid polymer electrolyte, such as a perfluorosulfonic acid (PFSA) polymer. A second solid polymer electrolyte, which may be the same as or different than the first solid polymer electrolyte, may be deposited over the top and/or bottom of the first solid polymer electrolyte.

Separation of oils from solids

International Nuclear Information System (INIS)

Van Slyke, D.C.

1992-01-01

This patent describes a method for cleaning oil-contaminated particulate solids. It comprises: contacting contaminated solids with a non-aqueous liquid composition comprising a carboxylic acid; then contacting the solids with an aqueous wash containing a reagent for converting the carboxylic acid to a water-soluble carboxylate salt; and removing an aqueous phase containing carboxylate salt and entrained oil

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.

Composite Repair System, Phase I

Data.gov (United States)

National Aeronautics and Space Administration — GTL has developed an innovative composite repair methodology known as the Composite Repair System (CRS). In this phase I effort, CRS is being developed for the...

Liquid-phase and solid-phase radioimmunoassay with herpes simplex virus type 1 nucleocapsids

International Nuclear Information System (INIS)

Bystricka, M.; Rajcani, J.; Libikova, H.; Sabo, A.; Foeldes, O.; Sadlon, J.

1985-01-01

Liquid-phase radioimmunoassay and solid-phase radioimmunoassay are described using 125 I-labelled or immobilized nucleocapsids (NC) of herpes simplex virus (HSV) type1. These techniques appeared sensitive and specific for quantitation of HSV-NC antigens and corresponding antibodies. (author)

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

Science.gov (United States)

Cassidy, Daniel H.; Irvine, Robert L.

1995-10-01

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

Study of crystalline morphology and phase structure in poly(styrene-b-ethylene oxide-b-styrene) triblock copolymers bu solid state RMN spin diffusion

International Nuclear Information System (INIS)

Mantovani, Gerson L.; Phan, Trang; Bertin, Denis; Azevedo, Eduardo R. de; Bonagamba, Tito J.

2009-01-01

The phase structure and crystalline morphology of a series of polystyrene-b-polyethylene oxide-b-polystyrene (PS-b- PEO-b-PS) triblock copolymers, with different compositions and molecular weights, has been studied by solid-state NMR. WAXS and DSC measurements were used to detect the presence of crystalline domains of polyethylene oxide (PEO) blocks at room temperature as a function of the copolymer composition. 1 H NMR spin diffusion analyses provided an estimation of the size of the dispersed phases of the nano structured copolymers. (author)

The Pictet-Spengler reaction in solid-phase combinatorial chemistry

DEFF Research Database (Denmark)

Nielsen, Thomas E; Diness, Frederik; Meldal, Morten

2003-01-01

The Pictet-Spengler reaction is an important reaction for the generation of tetrahydro-beta-carbolines and tetrahydroisoquinoline ring systems, which exhibit a range of biological and pharmacological properties. This review covers the solid-phase Pictet-Spengler reaction, as employed in solid...

A sol-gel based solid phase microextraction fiber for the analysis of aliphatic alcohols in apple juices.

Science.gov (United States)

Farhadi, Khalil; Maleki, Ramin; Tahmasebi, Raheleh

2010-01-01

A new fiber based on titania-chitin sol-gel coated on a silver wire for the headspace solid phase microextraction of aliphatic alcohols from apple juice samples was developed. The influences of fiber coating composition and microextraction conditions (extraction temperature, extraction time, and ionic strength of the sample matrix) on the fiber performance were investigated. Also, the influence of temperature and time on desorption of analytes from fiber were studied. Under the optimized conditions, a porous fiber with a high extraction capacity and good thermal stability (up to 250 degrees C) was obtained. The proposed headspace solid-phase microextraction-GC method was successfully used for the analysis of aliphatic alcohols in apple juice and concentrate samples. The recovery values were from 92.8 to 98.6%. The RSD (n=5) for all analytes were below 7.8%.

Phase 2, Solid waste retrieval strategy

International Nuclear Information System (INIS)

Johnson, D.M.

1994-01-01

Solid TRU retrieval, Phase 1 is scheduled to commence operation in 1998 at 218W-4C-T01 and complete recovery of the waste containers in 2001. Phase 2 Retrieval will recover the remaining buried TRU waste to be retrieved and provide the preliminary characterization by non-destructive means to allow interim storage until processing for disposal. This document reports on researching the characterization documents to determine the types of wastes to be retrieved and where located, waste configurations, conditions, and required methods for retrieval. Also included are discussions of wastes encompassed by Phase 2 for which there are valid reasons to not retrieve

Phase 2, Solid waste retrieval strategy

Energy Technology Data Exchange (ETDEWEB)

Johnson, D.M.

1994-09-29

Solid TRU retrieval, Phase 1 is scheduled to commence operation in 1998 at 218W-4C-T01 and complete recovery of the waste containers in 2001. Phase 2 Retrieval will recover the remaining buried TRU waste to be retrieved and provide the preliminary characterization by non-destructive means to allow interim storage until processing for disposal. This document reports on researching the characterization documents to determine the types of wastes to be retrieved and where located, waste configurations, conditions, and required methods for retrieval. Also included are discussions of wastes encompassed by Phase 2 for which there are valid reasons to not retrieve.

Phase transitions in solids under high pressure

CERN Document Server

Blank, Vladimir Davydovich

2013-01-01

Phase equilibria and kinetics of phase transformations under high pressureEquipment and methods for the study of phase transformations in solids at high pressuresPhase transformations of carbon and boron nitride at high pressure and deformation under pressurePhase transitions in Si and Ge at high pressure and deformation under pressurePolymorphic α-ω transformation in titanium, zirconium and zirconium-titanium alloys Phase transformations in iron and its alloys at high pressure Phase transformations in gallium and ceriumOn the possible polymorphic transformations in transition metals under pressurePressure-induced polymorphic transformations in АIBVII compoundsPhase transformations in AIIBVI and AIIIBV semiconductor compoundsEffect of pressure on the kinetics of phase transformations in iron alloysTransformations during deformation at high pressure Effects due to phase transformations at high pressureKinetics and hysteresis in high-temperature polymorphic transformations under pressureHysteresis and kineti...

The Importance of Phonons with Negative Phase Quotient in Disordered Solids.

Science.gov (United States)

Seyf, Hamid Reza; Lv, Wei; Rohskopf, Andrew; Henry, Asegun

2018-02-08

Current understanding of phonons is based on the phonon gas model (PGM), which is best rationalized for crystalline materials. However, most of the phonons/modes in disordered materials have a different character and thus may contribute to heat conduction in a fundamentally different way than is described by PGM. For the modes in crystals, which have sinusoidal character, one can separate the modes into two primary categories, namely acoustic and optical modes. However, for the modes in disordered materials, such designations may no longer rigorously apply. Nonetheless, the phase quotient (PQ) is a quantity that can be used to evaluate whether a mode more so shares a distinguishing property of acoustic vibrations manifested as a positive PQ, or a distinguishing property of an optical vibrations manifested as negative PQ. In thinking about this characteristic, there is essentially no intuition regarding the role of positive vs. negative PQ vibrational modes in disordered solids. Given this gap in understanding, herein we studied the respective contributions to thermal conductivity for several disordered solids as a function of PQ. The analysis sheds light on the importance of optical like/negative PQ modes in structurally/compositionally disordered solids, whereas in crystalline materials, the contributions of optical modes are usually small.

Solid Particle Erosion Behaviors of Carbon-Fiber Epoxy Composite and Pure Titanium

Science.gov (United States)

Cai, Feng; Gao, Feng; Pant, Shashank; Huang, Xiao; Yang, Qi

2016-01-01

Rotor blades of Bell CH-146 Griffon helicopter experience excessive solid particle erosion at low altitudes in desert environment. The rotor blade is made of an advanced light-weight composite which, however, has a low resistance to solid particle erosion. Coatings have been developed and applied to protect the composite blade. However, due to the influence of coating process on composite material, the compatibility between coating and composite base, and the challenges of repairing damaged coatings as well as the inconsistency between the old and new coatings, replaceable thin metal shielding is an alternative approach; and titanium, due to its high-specific strength and better formability, is an ideal candidate. This work investigates solid particle erosion behaviors of carbon-fiber epoxy composite and titanium in order to assess the feasibility of titanium as a viable candidate for erosion shielding. Experiment results showed that carbon-fiber epoxy composite showed a brittle erosion behavior, whereas titanium showed a ductile erosion mode. The erosion rate on composite was 1.5 times of that on titanium at impingement angle 15° and increased to 5 times at impact angle 90°.

Structural, electrical conductivity and dielectric behavior of Na2SO4–LDT composite solid electrolyte

Directory of Open Access Journals (Sweden)

Mohd Z. Iqbal

2016-01-01

Full Text Available A series of composite materials of general molecular formula (1 − x Na2SO4 − (x LDT was prepared by solid state reaction method. The phase structure and functionalization of these materials were defined by X-ray diffraction (XRD and Fourier-transform infrared spectroscopy (FT-IR respectively. Differential thermal analysis (DTA revealed that the hump of phase transition at 250 °C has decreased while its thermal stability was enhanced. Scanning electron microscopy signifies the presence of improved rigid surfaces and interphases that are accountable for the high ionic conduction due to dispersion of LDT particles in the composite systems. Arrhenius plots of the conductance show the maximum conductivity, σ = 4.56 × 10−4 S cm−1 at 500 °C for the x = 0.4 composition with the lowest activation energy 0.34 eV in the temperature range of 573–773 K. The value of dielectric constant was decreased with increasing frequency and follows the usual trend.

Solid state reaction in alumina nanoparticles/LZSA glass-ceramic composites

International Nuclear Information System (INIS)

Montedo, O.K.; Oliveira, A.N. de; Raupp-Pereira, F.

2016-01-01

Full text: The aim of this work is to present results related to solid state reactions on LZSA glass-ceramic composites containing alumina reinforcement nano-particles. A LZSA (Li2O-ZrO2-SiO2-Al2O3) glass-ceramic has been prepared by sintering of powders and characterized. Composites containing 0 to 77 vol.% of alumina nanoparticles (27-43 nm APS, 35 m2.g-1 SSA) and a 16.9Li2O•5.0ZrO2•65.1SiO2•8.6Al2O3 glass-ceramic matrix have been prepared. X-ray diffractometry studies have been performed in order of investigating the solid state reactions occurring in LZSA-based composites. Results of the XRD patterns have been related to the coefficient of thermal expansion (CTE), Young modulus, and dielectric constant, showing that, in comparison with the glass-ceramic composition, the composites showed a decrease of CTE with the alumina concentration increasing, due to the increasing of beta-spodumeness formation (solid solution of beta-spodumene, Li2O.Al2O3.4-10SiO2). The performance of the glass-ceramic was improved with the alumina nano-particles addition, showing potential of using in the preparation of Low Thermal Co-fired Ceramics (LTCC). (author)

Structure-phase composition and nano hardness of chrome-fullerite-chrome films irradiated by boron ions

International Nuclear Information System (INIS)

Baran, L.V.

2015-01-01

By methods of atomic force microscopy, X-ray diffraction and nano indentation the research of change of structure phase composition and nano hardness of the chrome - fullerite - chrome films, subjected to implantation by B + ions (E = 80 keV, F = 5*10 17 ions/cm 2 ) are submitted. It is established, that as a result of Boron ion implantation of the chrome - fullerite - chrome films, chrome and fullerite inter fusion on sues, that is the solid-phase interaction and as a result of which forms the heterophase with increased nano hardness. (authors)

Composite cathode materials development for intermediate temperature solid oxide fuel cell systems

Science.gov (United States)

Qin, Ya

Solid oxide fuel cell (SOFC) systems are of particular interest as electrochemical power systems that can operate on various hydrocarbon fuels with high fuel-to-electrical energy conversion efficiency. Within the SOFC stack, La0.8Sr 0.2Ga0.8Mg0.115Co0.085O3-delta (LSGMC) has been reported as an optimized composition of lanthanum gallate based electrolytes to achieve higher oxygen ionic conductivity at intermediate temperatures, i.e., 500-700°C. The electrocatalytic properties of interfaces between LSGMC electrolytes and various candidate intermediate-temperature SOFC cathodes have been investigated. Sm0.5Sr0.5CoO 3-delta (SSC), and La0.6Sr0.4Co0.2Fe 0.8O3-delta (LSCF), in both pure and composite forms with LSGMC, were investigated with regards to both oxygen reduction and evolution, A range of composite cathode compositions, having ratios of SSC (in wt.%) with LSGMC (wt.%) spanning the compositions 9:1, 8:2, 7:3, 6:4 and 5:5, were investigated to determine the optimal cathode-electrolyte interface performance at intermediate temperatures. All LSGMC electrolyte and cathode powders were synthesized using the glycine-nitrate process (GNP). Symmetrical electrochemical cells were investigated with three-electrode linear dc polarization and ac impedance spectroscopy to characterize the kinetics of the interfacial reactions in detail. Composite cathodes were found to perform better than the single phase cathodes due to significantly reduced polarization resistances. Among those composite SSC-LSGMC cathodes, the 7:3 composition has demonstrated the highest current density at the equivalent overpotential values, indicating that 7:3 is an optimal mixing ratio of the composite cathode materials to achieve the best performance. For the composite SC-LSGMC cathode/LSGMC interface, the cathodic overpotential under 1 A/cm2 current density was as low as 0.085 V at 700°C, 0.062V at 750°C and 0.051V at 800°C in air. Composite LSCF-LSGMC cathode/LSGMC interfaces were found to have

Solid Phase Extraction and Spectrophotometric Determination of ...

African Journals Online (AJOL)

NJD

2005-04-15

Apr 15, 2005 ... to the economy and has significant industrial applications. The development of a ... Waters Solid Phase Extraction (SPE) device (the device can carry out twenty ... HPLC grade dimethyl formamide (DMF) (Fisher. Corporation ...

Pressure Effects on Solid State Phase Transformation of Aluminium Bronze in Cooling Process

International Nuclear Information System (INIS)

Hai-Yan, Wang; Jian-Hua, Liu; Gui-Rong, Peng; Yan, Chen; Yu-Wen, Liu; Fei, Li; Wen-Kui, Wang

2009-01-01

Effects of high pressure (6 GPa) on the solid state phase transformation kinetic parameters of aluminum bronze during the cooling process are investigated, based on the measurement and calculation of its solid state phase transformation temperature, duration and activation energy and the observation of its microstructures. The results show that high pressure treatment can reduce the solid phase transformation temperature and activation energy in the cooling process and can shorten the phase transformation duration, which is favorable when forming fine-grained aluminum bronze

Solid phase extraction method for determination of mitragynine in ...

African Journals Online (AJOL)

All rights reserved. ... 1Department of Pharmacology, 2Department of Applied Science, 3Police Forensic Science Center 10, Yala 95000, 4Natural ... Purpose: To develop a solid phase extraction (SPE) method that utilizes reverse-phase high.

Modification of polydopamine-coated Fe3O4 nanoparticles with multi-walled carbon nanotubes for magnetic-μ-dispersive solid-phase extraction of antiepileptic drugs in biological matrices.

Science.gov (United States)

Zhang, Ruiqi; Wang, Siming; Yang, Ye; Deng, Yulan; Li, Di; Su, Ping; Yang, Yi

2018-06-01

In this study, multi-walled carbon nanotubes were coated on the surface of magnetic nanoparticles modified by polydopamine. The synthesized composite was characterized and applied to magnetic-μ-dispersive solid-phase extraction of oxcarbazepine (OXC), phenytoin (PHT), and carbamazepine (CBZ) from human plasma, urine, and cerebrospinal fluid samples prior to analysis by a high-performance liquid chromatography-photodiode array detector. The extraction parameters were investigated and the optimum condition was obtained when the variables were set to the following: sorbent type, Fe 3 O 4 @polyDA-MWCNTs (length Graphical abstract Magnetic multi-walled carbon nanotube core-shell composites were applied as magnetic-μ-dispersive solid-phase extraction adsorbents for determination of antiepileptic drugs in biological matrices.

A multi-phase equation of state for solid and liquid lead

International Nuclear Information System (INIS)

Robinson, C.M.

2004-01-01

This paper considers a multi-phase equation of state for solid and liquid lead. The thermodynamically consistent equation of state is constructed by calculating separate equations of state for the solid and liquid phases. The melt curve is the curve in the pressure, temperature plane where the Gibb's free energy of the solid and liquid phases are equal. In each phase a complete equation of state is obtained using the assumptions that the specific heat capacity is constant and that the Grueneisen parameter is proportional to the specific volume. The parameters for the equation of state are obtained from experimental data. In particular they are chosen to match melt curve and principal Hugoniot data. Predictions are made for the shock pressure required for melt to occur on shock and release

High-temperature x-ray diffraction study of HfTiO4-HfO2 solid solutions

International Nuclear Information System (INIS)

Carpenter, D.A.

1975-01-01

High-temperature x-ray diffraction techniques were used to determine the axial thermal expansion curves of HfTiO 4 -HfO 2 solid solutions as a function of composition. Data show increasing anisotropy with increasing HfO 2 content. An orthorhombic-to-monoclinic phase transformation was detected near room temperature for compositions near the high HfO 2 end of the orthorhombic phase field and for compositions within the two-phase region (HfTiO 4 solid solution plus HfO 2 solid solution). An orthorhombic-to-cubic phase transformation is indicated by data from oxygen-deficient materials at greater than 1873 0 K. (U.S.)

Hybrid Composite Material and Solid Particle Erosion Studies

Science.gov (United States)

Chellaganesh, D.; Khan, M. Adam; Ashif, A. Mohamed; Ragul Selvan, T.; Nachiappan, S.; Winowlin Jappes, J. T.

2018-04-01

Composite is one of the predominant material for most challenging engineering components. Most of the components are in the place of automobile structure, aircraft structures, and wind turbine blade and so on. At the same all the components are indulged to mechanical loading. Recent research on composite material are machinability, wear, tear and corrosion studies. One of the major issue on recent research was solid particle air jet erosion. In this paper hybrid composite material with and without filler. The fibre are in the combination of hemp – kevlar (60:40 wt.%) as reinforcement using epoxy as a matrix. The natural material palm and coconut shell are used as filler materials in the form of crushed powder. The process parameter involved are air jet velocity, volume of erodent and angle of impingement. Experiment performed are in eight different combinations followed from 2k (k = 3) factorial design. From the investigation surface morphology was studied using electron microscope. Mass change with respect to time are used to calculate wear rate and the influence of the process parameters. While solid particle erosion the hard particle impregnates in soft matrix material. Influence of filler material has reduced the wear and compared to plain natural composite material.

Mechanism and microstructures in Ga2O3 pseudomartensitic solid phase transition.

Science.gov (United States)

Zhu, Sheng-Cai; Guan, Shu-Hui; Liu, Zhi-Pan

2016-07-21

Solid-to-solid phase transition, although widely exploited in making new materials, challenges persistently our current theory for predicting its complex kinetics and rich microstructures in transition. The Ga2O3α-β phase transformation represents such a common but complex reaction with marked change in cation coordination and crystal density, which was known to yield either amorphous or crystalline products under different synthetic conditions. Here we, via recently developed stochastic surface walking (SSW) method, resolve for the first time the atomistic mechanism of Ga2O3α-β phase transformation, the pathway of which turns out to be the first reaction pathway ever determined for a new type of diffusionless solid phase transition, namely, pseudomartensitic phase transition. We demonstrate that the sensitivity of product crystallinity is caused by its multi-step, multi-type reaction pathway, which bypasses seven intermediate phases and involves all types of elementary solid phase transition steps, i.e. the shearing of O layers (martensitic type), the local diffusion of Ga atoms (reconstructive type) and the significant lattice dilation (dilation type). While the migration of Ga atoms across the close-packed O layers is the rate-determining step and yields "amorphous-like" high energy intermediates, the shearing of O layers contributes to the formation of coherent biphase junctions and the presence of a crystallographic orientation relation, (001)α//(201[combining macron])β + [120]α//[13[combining macron]2]β. Our experiment using high-resolution transmission electron microscopy further confirms the theoretical predictions on the atomic structure of biphase junction and the formation of (201[combining macron])β twin, and also discovers the late occurrence of lattice expansion in the nascent β phase that grows out from the parent α phase. By distinguishing pseudomartensitic transition from other types of mechanisms, we propose general rules to predict the

Solid-phase synthesis of complex and pharmacologically interesting heterocycles

DEFF Research Database (Denmark)

Nielsen, Thomas Eiland

2009-01-01

Efficient routes for the creation of heterocycles continue to be one of the primary goals for solid-phase synthesis. Recent advances in this field rely most notably on transition-metal-catalysis and N-acyliminium chemistry to mediate a range of cyclization processes for the generation of compounds...... with significant structural complexity and diversity. This review describes some of the most systematic solid-phase approaches that are potentially suited for pharmaceutical applications, that is, the methods described are useful for the synthesis of compound collections, and exhibit tunable stereochemistry...

Liquid-phase epitaxy of InGaAsP solid solutions on profiled substrates of InP(100)

International Nuclear Information System (INIS)

Dvoryankin, V.F.; Kaevitser, L.R.; Komarov, A.A.; Telegin, A.A.; Khusid, L.B.; Chernushin, M.D.

1990-01-01

Peculiarities of selective growth of InGaAsP solid solutions under liquid-phase epitaxy in shallow grooves are considered. InGaAsP crystals grown in grooves oriented along crystallografic [110] and [011] directions are determined to trend to equilibrium form under two-phase epitaxy, while wedge-shaped form of In 0.77 Ga 0.23 As 0.53 P 0.45 and In 0.53 P o.45 and IN 0.59 Ga 0.41 As 0.83 P 0.12 epitaxial layers obtained in grooves is determined by their composition only and does not depend on groove configuration

Indigenous microbial capability in solid manure residues to start-up solid-phase anaerobic digesters.

Science.gov (United States)

Yap, S D; Astals, S; Jensen, P D; Batstone, D J; Tait, S

2017-06-01

Batch solid-phase anaerobic digestion is a technology for sustainable on-farm treatment of solid residues, but is an emerging technology that is yet to be optimised with respect to start-up and inoculation. In the present study, spent bedding from two piggeries (site A and B) were batch digested at total solids (TS) concentration of 5, 10 and 20% at mesophilic (37°C) and thermophilic (55°C) temperatures, without adding an external inoculum. The results showed that the indigenous microbial community present in spent bedding was able to recover the full methane potential of the bedding (140±5 and 227±6L CH 4 kgVS fed -1 for site A and B, respectively), but longer treatment times were required than for digestion with an added external inoculum. Nonetheless, at high solid loadings (i.e. TS level>10%), the digestion performance was affected by chemical inhibition due to ammonia and/or humic acid. Thermophilic temperatures did not influence digestion performance but did increase start-up failure risk. Further, inoculation of residues from the batch digestion to subsequent batch enhanced start-up and achieved full methane potential recovery of the bedding. Inoculation with liquid residue (leachate) was preferred over a solid residue, to preserve treatment capacity for fresh substrate. Overall, the study highlighted that indigenous microbial community in the solid manure residue was capable of recovering full methane potential and that solid-phase digestion was ultimately limited by chemical inhibition rather than lack of suitable microbial community. Copyright © 2017 Elsevier Ltd. All rights reserved.

Supercooling suppression of microencapsulated phase change materials by optimizing shell composition and structure

International Nuclear Information System (INIS)

Cao, Fangyu; Yang, Bao

2014-01-01

Highlights: • A new method for supercooling suppression of microPCMs by optimizing the structure of the microcapsule shell. • Large effective latent heat (up to 213 J/g) of the microPCMs, much higher than those using additive as nucleating agents. • Change of shell composition and structure significantly affects the phase transition processes of the encapsulated PCMs. • The latent heat of the shell-induced phase transition is maximized, reaching 83.7% of the latent heat of bulk octadecane. • Hollow spheres with porous rather than solid resin shell are also formed when the SDS concentration is very high. - Abstract: A new method for supercooling suppression of microencapsulated phase change materials (PCMs) has been developed by optimizing the composition and structure of the microcapsule resin shell. The microcapsules comprising paraffin octadecane encapsulated in melamine–formaldehyde resin shell were synthesized with the use the oil-in-water emulsion technique. These PCM microcapsules are 5–15 μm in diameter. The supercooling of these octadecane microcapsules can be as large as 13.6 °C, when the homogeneous nucleation is dominant during the melt crystallization into the thermodynamically stable triclinic phase. It is discovered that the homogeneous nucleation can be mediated by shell-induced nucleation of the triclinic phase and the metastable rotator phase when the shell composition and structure are optimized, without need of any nucleating additives. The effects of synthesis parameters, such as ratio of melamine to formaldehyde, pH of pre-polymer, and pH of emulsion, on the phase transition properties of the octadecane microcapsules have been investigated systemically. The optimum synthesis conditions have been identified in terms of minimizing the supercooling while maintaining heat capacity. Potential applications of this type of phase changeable microcapsules include high heat capacity thermal fluids, thermal management in smart buildings

On the study of the solid-solid phase transformation of TlBiTe2

International Nuclear Information System (INIS)

Chrissafis, K.; Vinga, E.S.; Paraskevopoulos, K.M.; Polychroniadis, E.K.

2003-01-01

The narrow gap semiconductor TlBiTe 2 undergoes a solid-solid phase transformation from the rhombohedral (D 3d ) to the cubic (O h ) phase. The present paper deals with the study of this phase transformation combining the results of Differential Scanning Calorimetry (DSC) and Transmission Electron Microscopy (TEM). It has been found that during heating the transformation is an athermal activated process, which can be described only by a combination of more than one processes while during cooling it exhibits an expectable thermal hysteresis due to the volume difference. The results of the kinetic analysis combined with the electron microscopy findings, supported also by the Fourier Transform Infrared (FTIR) spectroscopy ones, lead to the conclusion that TlBiTe 2 undergoes a multiple-step, displacive, martensitic type transformation. (Abstract Copyright [2003], Wiley Periodicals, Inc.)

Solid phase radioimmunoassays for human C-reactive protein

International Nuclear Information System (INIS)

Shine, B.; Beer, F.C. de; Pepys, M.B.

1981-01-01

Two new, rapid and sensitive radioimmunoassays for human C-reactive protein (CRP) have been established using antiserum coupled to magnetizable cellulose particles, which facilitate phase separation. A single antibody method, using solid phase anti-CRP, provides a sensitivity of 50 μg/l with a 1-h incubation time and intra- and inter-assay coefficients of variation of 10%. A double antibody method, using fluid phase rabbit anti-CRP serum and solid phase sheep anti-rabbit IgG serum, provides a sensitivity of 3 μg/l with an overnight incubation and intra- and inter-assay coefficients of variation of 10%. Among 468 sera from normal adult volunteer blood donors the median CRP concentration was 800 μg/l, interquartile range 340-1700 μg/l and range 70-29,000 μg/l. Ninety percent of samples contained less than 3 mg/l and 99% less than 10 mg/l. Low levels (14-650 μg/l) of CRP were detected both in amniotic fluids and in cerebrospinal fluids. (Auth.)

Gamma camera system with composite solid state detector

International Nuclear Information System (INIS)

Gerber, M.S.; Miller, D.W.

1977-01-01

A composite solid-state detector is described for utilization within gamma cameras. The detector's formed of an array of detector crystals, the opposed surfaces of each of which are formed incorporating an impedance-derived configuration for determining one coordinate of the location of discrete impinging photons upon the detector. A combined read-out for all detectors within the composite array is achieved through a row and column interconnection of the impedance configurations. Utilizing the read-outs for respective sides of the discrete crystals, a resultant time-constant characteristic for the composite detector crystal array remains essentially that of individual crystal detectors

SOLID-PHASE PEPTIDE SYNTHESIS OF ISOTOCIN WITH AMIDE ...

African Journals Online (AJOL)

SOLID-PHASE PEPTIDE SYNTHESIS OF ISOTOCIN WITH AMIDE OF ASPARAGINE PROTECTED WITH 1-TETRALINYL. TRIFLUOROMETHANESULPHONIC ACID (TFMSA) DEPROTECTION, CLEAVAGE AND AIR OXIDATION OF MERCAPTO GROUPS TO DISULPHIDE.

Solid-State NMR Investigation of Drug-Excipient Interactions and Phase Behavior in Indomethacin-Eudragit E Amorphous Solid Dispersions.

Science.gov (United States)

Lubach, Joseph W; Hau, Jonathan

2018-02-20

To investigate the nature of drug-excipient interactions between indomethacin (IMC) and methacrylate copolymer Eudragit® E (EE) in the amorphous state, and evaluate the effects on formulation and stability of these amorphous systems. Amorphous solid dispersions containing IMC and EE were spray dried with drug loadings from 20% to 90%. PXRD was used to confirm the amorphous nature of the dispersions, and DSC was used to measure glass transition temperatures (T g ). 13 C and 15 N solid-state NMR was utilized to investigate changes in local structure and protonation state, while 1 H T 1 and T 1ρ relaxation measurements were used to probe miscibility and phase behavior of the dispersions. T g values for IMC-EE solid dispersions showed significant positive deviations from predicted values in the drug loading range of 40-90%, indicating a relatively strong drug-excipient interaction. 15 N solid-state NMR exhibited a change in protonation state of the EE basic amine, with two distinct populations for the EE amine at -360.7 ppm (unprotonated) and -344.4 ppm (protonated). Additionally, 1 H relaxation measurements showed phase separation at high drug load, indicating an amorphous ionic complex and free IMC-rich phase. PXRD data showed all ASDs up to 90% drug load remained physically stable after 2 years. 15 N solid-state NMR experiments show a change in protonation state of EE, indicating that an ionic complex indeed forms between IMC and EE in amorphous solid dispersions. Phase behavior was determined to exhibit nanoscale phase separation at high drug load between the amorphous ionic complex and excess free IMC.

Bioinspired magnetite synthesis via solid precursor phases

NARCIS (Netherlands)

Lenders, J.J.M.; Mirabello, G.; Sommerdijk, N.A.J.M.

2016-01-01

Living organisms often exploit solid but poorly ordered mineral phases as precursors in the biomineralization of their inorganic body parts. Generally speaking, such precursor-based approaches allow the organisms-without the need of high supersaturation levels-to accumulate significant quantities of

On Inclusion-Matrix Interfacial Stresses in Composites Containing Phase-Transforming Phases

International Nuclear Information System (INIS)

Wang, Y.-C.; Ko, C.-C.

2010-01-01

Recent development in composites containing phase-transforming particles, such as vanadium dioxide or barium titanate, reveals the overall stiffness and viscoelastic damping of the composites may be unbounded. Negative stiffness is induced from phase transformation predicted by the Landau phase transformation theory. Although this unbounded phenomenon is theoretically supported with the composite homogenization theory, detailed stress analyses of the composites are still lacking. In this work, we analyze the two-dimensional plane stress elasticity problem of a square plate containing a circular inclusion, under the assumption that the Young's modulus of the inclusion is negative. Assumption of negative stiffness is a priori in the present analysis. A static loading condition is adopted to estimate the effective modulus of the composites by the ratio of applied stress to averaged strain on the loading edges. It is found that the interfacial stresses between the circular inclusion and matrix increase dramatically when the negative stiffness is so tuned that overall stiffness is unbounded. Furthermore, it is found that stress distributions in the inclusion are not uniform, contrary to Eshelby's theorem, which states, for two-phase, infinite composites, the inclusion's stress distribution is uniform when the shape of the inclusion has higher symmetry than an ellipse. The rationale for this nonuniform stress distributions is due to nonlocal effects induced from negative stiffness.

Investigation of binary solid phases by calorimetry and kinetic modelling

OpenAIRE

Matovic, M.

2007-01-01

The traditional methods for the determination of liquid-solid phase diagrams are based on the assumption that the overall equilibrium is established between the phases. However, the result of the crystallization of a liquid mixture will typically be a non-equilibrium or metastable state of the solid. For a proper description of the crystallization process the equilibrium approach is insufficient and a kinetic approach is actually required. In this work, we show that during slow crystallizatio...

Evaluation of natural toxicity on MICROTOX solid-phase test. The pelitic normalization

International Nuclear Information System (INIS)

Onorati, F.; Pellegrini, D.; Ausili, A.

1999-01-01

In sediment toxicity testing Microtox solid-phase test (SPT) is one of the most used and standardised bioassay. Nevertheless, its real sensitivity and discriminatory power is still unclear, because of several interferences principally related to the matrix composition. Using reference sediments, characterised with chemical and physical analysis, it was possible to find a significant relationship between their natural toxicity and the pelitic fraction that allows to estimate the natural component of the acute toxicity in contaminated samples. This relationship arrows a more sensitive and valid interpretation than raw data and it is used to develop a sediment toxicity index (STI) based on radio to reference (RTR) concept, applicable to harbour contaminated samples [it

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

Solid-phase route to Fmoc-protected cationic amino acid building blocks

DEFF Research Database (Denmark)

Clausen, Jacob Dahlqvist; Linderoth, Lars; Nielsen, Hanne Mørck

2012-01-01

Diamino acids are commonly found in bioactive compounds, yet only few are commercially available as building blocks for solid-phase peptide synthesis. In the present work a convenient, inexpensive route to multiple-charged amino acid building blocks with varying degree of hydrophobicity...... was developed. A versatile solid-phase protocol leading to selectively protected amino alcohol intermediates was followed by oxidation to yield the desired di- or polycationic amino acid building blocks in gram-scale amounts. The synthetic sequence comprises loading of (S)-1-(p-nosyl)aziridine-2-methanol onto...... of simple neutral amino acids as well as analogs displaying high bulkiness or polycationic side chains was prepared. Two building blocks were incorporated into peptide sequences using microwave-assisted solid-phase peptide synthesis confirming their general utility....

End-Member Formulation of Solid Solutions and Reactive Transport

Energy Technology Data Exchange (ETDEWEB)

Lichtner, Peter C. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

2015-09-01

A model for incorporating solid solutions into reactive transport equations is presented based on an end-member representation. Reactive transport equations are solved directly for the composition and bulk concentration of the solid solution. Reactions of a solid solution with an aqueous solution are formulated in terms of an overall stoichiometric reaction corresponding to a time-varying composition and exchange reactions, equivalent to reaction end-members. Reaction rates are treated kinetically using a transition state rate law for the overall reaction and a pseudo-kinetic rate law for exchange reactions. The composition of the solid solution at the onset of precipitation is assumed to correspond to the least soluble composition, equivalent to the composition at equilibrium. The stoichiometric saturation determines if the solid solution is super-saturated with respect to the aqueous solution. The method is implemented for a simple prototype batch reactor using Mathematica for a binary solid solution. Finally, the sensitivity of the results on the kinetic rate constant for a binary solid solution is investigated for reaction of an initially stoichiometric solid phase with an undersaturated aqueous solution.

Unitized solid phase immunoassay kit and method

International Nuclear Information System (INIS)

1975-01-01

A unitized solid phase kit for radioimmunoassay is disclosed. All of the necessary assay reagents are incorporated into a single tube wherein all phases of the assay procedure are performed, requiring only the addition of the patient's sample. Antibody is bound to the tube surface while labelled antigen is also present but unbound. Storage in the absence of air and water results in the stabilization of the reagents such that the system can be stored for long periods

Analysis of semi-solid processing for metal matrix composite synthesis using factorial design

Directory of Open Access Journals (Sweden)

Kratus Ranieri

2012-02-01

Full Text Available The main goal in this work is to conduct a quantitative analysis of the mechanical stir casting process for obtaining particulate metal matrix composites. A combined route of stirring at semi-solid state followed by stirring at liquid state is proposed. A fractional factorial design was developed to investigate the influence and interactions of factors as: time, rotation, initial fraction and particle size, on the incorporated fraction. The best incorporations were obtained with all factors at high levels, as well as that very long stirring periods have no strong influence being particle size and rotation the most important factors on the incorporated fraction. Particle wetting occurs during stirring at semi-solid state, highlighting the importance of the interactions between particles and the alloy globularized phase. The role of the alloying element Mg as a wettability-promoting agent is discussed. The shear forces resulting from the stirring system is emphasized and understood as the effect of rotation itself added to the propeller blade geometry.

Solid-phase microextraction

DEFF Research Database (Denmark)

Nilsson, Torben

The objective of this study has been to develop new analytical methods using the rapid, simple and solvent-free extraction technique solid-phase microextraction (SPME) for the quantitative analysis of organic pollutants at trace level in drinking water and environmental samples. The dynamics...... of SPME were examined for halogenated and non-halogenated volatile hydrocarbons, and a standard method for their quantitative analysis in aqueous samples was developed and validated in inter-laboratory studies on the basis of reference material and in comparison with the traditional methods....... The influences of some possible interferences on the SPME process were examined, and new SPME probes were tested for the in situ monitoring of groundwater pollutants. Inter-laboratory studies were carried out also for the validation of SPME for the quantitative analysis of organochlorine, organonitrogen...

Phase segregation in cerium-lanthanum solid solutions

NARCIS (Netherlands)

Belliere, V.; Joorst, G; Stephan, O; de Groot, FMF; Weckhuysen, BM

2006-01-01

Electron energy-loss spectroscopy (EELS) in combination with scanning transmission electron microscopy ( STEM) reveals that the La enrichment at the surface of cerium-lanthanum solid solutions is an averaged effect and that segregation occurs in a mixed oxide phase. This separation occurs within a

Nutritional composition of bioproducts generated from semi-solid ...

African Journals Online (AJOL)

Nutritional composition of bioproducts generated from semi-solid fermentation of pineapple peel by edible mushrooms. Raiane Áila Teixeira Souza, Tamiris Rio Branco da Fonseca, Larissa de Souza Kirsch, Larissa Svetlana Cavalcante Silva, Mircella Marialva Alecrim, Raimundo Felipe da Cruz Filho, Maria Francisca ...

Complement fixation by solid phase immune complexes. Reduced capacity in SLE sera

DEFF Research Database (Denmark)

Baatrup, G; Jonsson, H; Sjöholm, A

1988-01-01

We describe an ELISA for assessment of complement function based on the capacity of serum to support fixation of complement components to solid phase immune complexes (IC). Microplates were coated with aggregated bovine serum albumin (BSA) followed by rabbit anti-BSA IgG. The solid phase IC were...

Biological nitrate removal from water and wastewater by solid-phase denitrification process.

Science.gov (United States)

Wang, Jianlong; Chu, Libing

2016-11-01

Nitrate pollution in receiving waters has become a serious issue worldwide. Solid-phase denitrification process is an emerging technology, which has received increasing attention in recent years. It uses biodegradable polymers as both the carbon source and biofilm carrier for denitrifying microorganisms. A vast array of natural and synthetic biopolymers, including woodchips, sawdust, straw, cotton, maize cobs, seaweed, bark, polyhydroxyalkanoate (PHA), polycaprolactone (PCL), polybutylene succinate (PBS) and polylactic acid (PLA), have been widely used for denitrification due to their good performance, low cost and large available quantities. This paper presents an overview on the application of solid-phase denitrification in nitrate removal from drinking water, groundwater, aquaculture wastewater, the secondary effluent and wastewater with low C/N ratio. The types of solid carbon source, the influencing factors, the microbial community of biofilm attached on the biodegradable carriers, the potential adverse effect, and the cost of denitrification process are introduced and evaluated. Woodchips and polycaprolactone are the popular and competitive natural plant-like and synthetic biodegradable polymers used for denitrification, respectively. Most of the denitrifiers reported in solid-phase denitrification affiliated to the family Comamonadaceae in the class Betaproteobacteria. The members of genera Diaphorobacter, Acidovorax and Simplicispira were mostly reported. In future study, more attention should be paid to the simultaneous removal of nitrate and toxic organic contaminants such as pesticide and PPCPs by solid-phase denitrification, to the elucidation of the metabolic and regulatory relationship between decomposition of solid carbon source and denitrification, and to the post-treatment of the municipal secondary effluent. Solid-phase denitrification process is a promising technology for the removal of nitrate from water and wastewater. Copyright © 2016

Solid-solid synthesis and structural phase transition process of SmF3

Science.gov (United States)

Yan, Qi-Cao; Guo, Xing-Min

2018-04-01

Mazes of contradictory conclusions have been obtained by previous researches about structural phase transition process of SmF3. In this paper, the single crystals of SmF3 (hexagonal and orthorhombic) were prepared by solid-solid synthesis, which have shown gradual changes in crystal growth modes with the increase temperature and holding time. Furthermore, we propose the phase transition process of in SmF3. Hexagonal symmetry of SmF3 (space group Pnma) was prepared firstly by heating Sm2O3 and NH4HF2 over 40 min at 270 °C. And then orthorhombic symmetry of SmF3 (space group P63mc) was obtained by heating hexagonal symmetry over 10 h at 650 °C. The reaction of SmF3 (hexagonal) = SmF3 (orthorhombic) is extremely sluggish at a low temperature (less than 650 °C), which was seen as a Mixed Grown Region.

Thermodynamic phase behavior of API/polymer solid dispersions.

Science.gov (United States)

Prudic, Anke; Ji, Yuanhui; Sadowski, Gabriele

2014-07-07

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

The conductivity and stability of polymer composite solid electrolyte upon addition of graphene

Science.gov (United States)

Hamid, Farzana Abd.; Salleh, Fauzani Md.; Mohamed, Nor Sabirin

2017-12-01

The effect of graphene composition on the conductivity and stability of polymer composite solid electrolyte was studied. These polymer composite solid electrolytes were synthesized by sol gel method and prepared via the solution-casting technique. The compositions of graphene were varied between 10 wt% to 70 wt%. The changes in the functional group of polymer composite after the addition of graphene were characterized by Fourier Transform InfraRed spectroscopy. Electrochemical impedance spectroscopy was conducted at ambient temperature in the frequency range of 10 Hz to 1 MHz to study the conductivity of the polymer composite. The highest conductivity was obtained at 60 wt% graphene with the value of 2.85×10-4 Scm-1. Sample without the addition of graphene showed the lowest conductivity value of 1.77×10-7 Scm-1 and acts as an insulator. The high conductivity at 60 wt% graphene loading is related to dehydration of cellulose. This is supported by the FTIR spectrum where the absorption peaks of C-O stretching vibrations of polymer composite is weakened and the hydroxyl group is slightly shifted compared to the FTIR spectrum without the addition of graphene. Linear sweep voltammetry results demonstrated that the polymer composite solid electrolyte exhibited electrochemical stability up to 3.2 V.

Solid Amalgam Composite Electrode as a New Sensor for the Determination of Biologically Active Compounds

Czech Academy of Sciences Publication Activity Database

Josypčuk, Bohdan; Navrátil, Tomáš; Lukina, A.; Pecková, K.; Barek, J.

2007-01-01

Roč. 52, č. 6 (2007), s. 897-910 ISSN 0009-2223 R&D Projects: GA ČR GA203/07/1195; GA MŠk(CZ) LC06035 Institutional research plan: CEZ:AV0Z40400503 Keywords : solid composite electrode * solid amalgam electrodes * solid amalgam composite electrode * voltammetry Subject RIV: CG - Electrochemistry Impact factor: 0.529, year: 2007

Solid-phase microextraction for bioconcentration studies according to OECD TG 305

Energy Technology Data Exchange (ETDEWEB)

Duering, Rolf-Alexander; Boehm, Leonard [Land Use and Nutrition (IFZ) Justus Liebig University Giessen, Institute of Soil Science and Soil Conservation, Research Centre for BioSystems, Giessen (Germany); Schlechtriem, Christian [Fraunhofer Institute for Molecular Biology and Applied Ecology (IME), Schmallenberg (Germany)

2012-12-15

An important aim of the European Community Regulation on chemicals and their safe use is the identification of (very) persistent, (very) bioaccumulative, and toxic substances. In other regulatory chemical safety assessments (pharmaceuticals, biocides, pesticides), the identification of such (very) persistent, (very) bioaccumulative, and toxic substances is of increasing importance. Solid-phase microextraction is especially capable of extracting total water concentrations as well as the freely dissolved fraction of analytes in the water phase, which is available for bioconcentration in fish. However, although already well established in environmental analyses to determine and quantify analytes mainly in aqueous matrices, solid-phase microextraction is still a rather unusual method in regulatory ecotoxicological research. Here, the potential benefits and drawbacks of solid-phase microextraction are discussed as an analytical routine approach for aquatic bioconcentration studies according to OECD TG 305, with a special focus on the testing of hydrophobic organic compounds characterized by log K{sub OW}> 5. (orig.)

Effective medium of periodic fluid-solid composites

KAUST Repository

Mei, Jun

2012-05-24

An analytic solution of the effective mass density and bulk modulus of a periodic fluid-solid composite is obtained by using the multiple-scattering theory in the long-wavelength limit. It is shown that when the concentration of solid inclusions is high, the effective mass density is structure dependent and differs significantly from the leading-order dipole solution, whereas Wood\\'s formula is accurately valid, independently of the structures. Numerical evaluations from the analytic solution are shown to be in excellent agreement with finite-element simulations. In the vicinity of the tight-packing limit, the critical behavior of the effective mass density is also studied and it is independent of the lattice symmetry. © 2012 Europhysics Letters Association.

Simulating Solid-Solid Phase Transition in Shape-Memory Alloy Microstructure by Face-Offsetting Method

International Nuclear Information System (INIS)

Bellur Ramaswamy, Ravi S.; Tortorelli, Daniel A.; Fried, Eliot; Jiao Xiangmin

2008-01-01

Advances in the understanding of martensitic transformations (diffusionless, solid-solid phase transformations) have been instrumental to the recent discovery of new low hysteresis alloys. However, some key fundamental issues must be better understood to design still better alloys. Restricting attention to antiplane shear, we use finite element analysis to model the shape-memory alloy microstructure within the Abeyaratne-Knowles continuum thermomechanical framework and use an interface kinetic relation of the kind proposed by Rosakis and Tsai. Geometric singularities and topological changes associated with microstructural evolution pose significant numerical challenges. We address such challenges with a recently developed front-tracking scheme called the face-offsetting method (FOM) to explicitly model phase interfaces. Initial results demonstrate the effectiveness of FOM in resolving needle-like twinned microstructures

Two-dimensional solid-phase extraction strategy for the selective enrichment of aminoglycosides in milk.

Science.gov (United States)

Shen, Aijin; Wei, Jie; Yan, Jingyu; Jin, Gaowa; Ding, Junjie; Yang, Bingcheng; Guo, Zhimou; Zhang, Feifang; Liang, Xinmiao

2017-03-01

An orthogonal two-dimensional solid-phase extraction strategy was established for the selective enrichment of three aminoglycosides including spectinomycin, streptomycin, and dihydrostreptomycin in milk. A reversed-phase liquid chromatography material (C 18 ) and a weak cation-exchange material (TGA) were integrated in a single solid-phase extraction cartridge. The feasibility of two-dimensional clean-up procedure that experienced two-step adsorption, two-step rinsing, and two-step elution was systematically investigated. Based on the orthogonality of reversed-phase and weak cation-exchange procedures, the two-dimensional solid-phase extraction strategy could minimize the interference from the hydrophobic matrix existing in traditional reversed-phase solid-phase extraction. In addition, high ionic strength in the extracts could be effectively removed before the second dimension of weak cation-exchange solid-phase extraction. Combined with liquid chromatography and tandem mass spectrometry, the optimized procedure was validated according to the European Union Commission directive 2002/657/EC. A good performance was achieved in terms of linearity, recovery, precision, decision limit, and detection capability in milk. Finally, the optimized two-dimensional clean-up procedure incorporated with liquid chromatography and tandem mass spectrometry was successfully applied to the rapid monitoring of aminoglycoside residues in milk. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Gastric emptying scintigraphy: choice by in vitro test, of a new 99mTc marker to label solid phase and further analysis with the better radiopharmaceuticals

International Nuclear Information System (INIS)

Blanc, F.

2005-05-01

The study of gastric emptying by isotopic method occurs regularly in Brest nuclear medicine department. It consists in eating radiolabelled omelette with rhenium sulphide macro-colloid and in drinking radiolabelled water with 111 In-DTPA. The two phases are followed in stomach with gamma-camera. Rhenium sulphide macro-colloid have been taken off the market in january 2004 and no radiopharmaceutical has replaced them. in vitro test permitted us to test solid phase radiolabeling stability with 5 99m Tc-vectors used in nuclear medicine. Two of them are suitable for gastric emptying solid phase labelling: the tin fluoride colloids and the sodium phytate but tin fluoride colloids give better labelling stability than sodium phytate. In order to define solid phase marker properties, studies of medium composition by X fluorescence, size by laser granulometry, structure by NMR (nuclear magnetic resonance), TLC (thin layer chromatography) and by centrifugation are done either with the two vectors or only with sodium phytate. Structural properties of tin fluoride colloids are known. Results of this study indicate that phytates can be colloids. Finally, the good gastric emptying solid phase marker must be a colloid with a size of about 200 nm. (author)

Evaluation of a solid-phase RIA technique and a solid-phase ELISA technique for demonstrating hepatitis-B surface antigen

International Nuclear Information System (INIS)

Vranckx, R.; Cole, J.; Peetermans, M.

1978-01-01

The sensitivities of a solid-phase radioimmunoassay (RIA), a solid-phase enzyme immunoassay (ELISA) and a haemagglutination test (RPHA) for the detection of the hepatitis-B surface antigen (HBsAg) were compared (1) by screening a panel of 300 sera (97 positives and 203 negatives), and (2) by titrating serial dilutions of 10 positive sera. Ninety-seven sera were positive by RIA, 95% were detected by ELISA and 81% were detected by RPHA. In the serial dilutions, the average end-points of the titrations were 0.005ng/ml for RIA, 0.01ng/ml for ELISA and 0.04 ng/ml for RPHA. It can be concluded that the sensitivity of the ELISA test is intermediate between that of the RIA and the RPHA. The ELISA and the RPHA tests seem to be a little more sensitive for the detection of subtype ay than for the detection of subtype ad. (author)

First-principles thermodynamics study of phase stability in inorganic halide perovskite solid solutions

Science.gov (United States)

Bechtel, Jonathon S.; Van der Ven, Anton

2018-04-01

Halide substitution gives rise to a tunable band gap as a function of composition in halide perovskite materials. However, photoinduced phase segregation, observed at room temperature in mixed halide A Pb (IxBr1-x) 3 systems, limits open circuit voltages and decreases photovoltaic device efficiencies. We investigate equilibrium phase stability of orthorhombic P n m a γ -phase CsM (XxY1-x) 3 perovskites where M is Pb or Sn, and X and Y are Br, Cl, or I. Finite-temperature phase diagrams are constructed using a cluster expansion effective Hamiltonian parameterized from first-principles density-functional-theory calculations. Solid solution phases for CsM (IxBr1-x) 3 and CsM (BrxCl1-x) 3 are predicted to be stable well below room temperature while CsM (IxCl1-x) 3 systems have miscibility gaps that extend above 400 K. The height of the miscibility gap correlates with the difference in volume between end members. Also layered ground states are found on the convex hull at x =2 /3 for CsSnBr2Cl ,CsPbI2Br , and CsPbBrCl2. The impact of these ground states on the finite temperature phase diagram is discussed in the context of the experimentally observed photoinduced phase segregation.

C18, C8, and perfluoro reversed phases on diamond for solid-phase extraction.

Science.gov (United States)

Saini, Gaurav; Wiest, Landon A; Herbert, David; Biggs, Katherine N; Dadson, Andrew; Vail, Michael A; Linford, Matthew R

2009-04-17

In spite of advances in solid-phase extraction (SPE) technology there are certain disadvantages to current SPE silica-based, column packings. The pH range over which extraction can occur is limited and each column is generally only used once. New diamond-based reversed SPE phases (C(18), C(8), and perfluorinated) were developed in our laboratories. Studies were done which show that these phases do not have the same limitations as traditional silica-based stationary phases. The synthesis and properties of these diamond-based phases are presented, and the stability, percent recovery, and column capacity are given for the C(18) phase.

Influence of Calcium on Microbial Reduction of Solid Phase Uranium (VI)

International Nuclear Information System (INIS)

Liu, Chongxuan; Jeon, Byong-Hun; Zachara, John M.; Wang, Zheming

2007-01-01

The effect of calcium on microbial reduction of a solid phase U(VI), sodium boltwoodite (NaUO2SiO3OH · 1.5H2O), was evaluated in a culture of a dissimilatory metal-reducing bacterium (DMRB), Shewanella oneidensis strain MR-1. Batch experiments were performed in a non-growth bicarbonate medium with lactate as electron donor at pH 7 buffered with PIPES. Calcium increased both the rate and extent of Na-boltwoodite dissolution by increasing its solubility through the formation of a ternary aqueous calcium-uranyl-carbonate species. The ternary species, however, decreased the rates of microbial reduction of aqueous U(VI). Laser-induced fluorescence spectroscopy (LIFS) and transmission electron microscopy (TEM) revealed that microbial reduction of solid phase U(VI) is a sequentially coupled process of Na-boltwoodite dissolution, U(VI) aqueous speciation, and microbial reduction of dissolved U(VI) to U(IV) that accumulated on bacterial surfaces/periplasm. The overall rates of microbial reduction of solid phase U(VI) can be described by the coupled rates of dissolution and microbial reduction that were both influenced by calcium. The results demonstrated that dissolved U(VI) concentration during microbial reduction was a complex function of solid phase U(VI) dissolution kinetics, aqueous U(VI) speciation, and microbial activity

Nuclear prehistory influence on irradiated metallic iron phase composition

International Nuclear Information System (INIS)

Alekseev, I.E.

2007-01-01

With application of different Moessbauer spectroscopy applications the phase composition of metallic iron after irradiation by both neutrons and charged particles were studied. Irradiation conditions, method of targets examination and phase composition of samples after irradiation were presented in tabular form. It is shown, that phase composition of irradiated metal is defined by nuclear prehistory. So, in a number of cases abnormals (stabilization of high- and low-temperature structural phases of iron at room temperature after irradiation end) were revealed

Chemically and geographically distinct solid-phase iron pools in the Southern Ocean.

Science.gov (United States)

von der Heyden, B P; Roychoudhury, A N; Mtshali, T N; Tyliszczak, T; Myneni, S C B

2012-11-30

Iron is a limiting nutrient in many parts of the oceans, including the unproductive regions of the Southern Ocean. Although the dominant fraction of the marine iron pool occurs in the form of solid-phase particles, its chemical speciation and mineralogy are challenging to characterize on a regional scale. We describe a diverse array of iron particles, ranging from 20 to 700 nanometers in diameter, in the waters of the Southern Ocean euphotic zone. Distinct variations in the oxidation state and composition of these iron particles exist between the coasts of South Africa and Antarctica, with different iron pools occurring in different frontal zones. These speciation variations can result in solubility differences that may affect the production of bioavailable dissolved iron.

Solid phase tube radioimmunoassay for digoxin detection

International Nuclear Information System (INIS)

Stellner, K.; Glatz, C.; Linke, R.

1975-01-01

A solid phase radioimmunoassay with 125 I is described for cardiac patients. The test for the digoxin determination and the poisoning due to cardiac glycosides can be measured very accurately and carried out easily. In addition, the test determination can be automatically performed in connection with other tests. (GSE/LH) [de

Heat transfer characteristics of thermal energy storage of a composite phase change materials: Numerical and experimental investigations

International Nuclear Information System (INIS)

Aadmi, Moussa; Karkri, Mustapha; El Hammouti, Mimoun

2014-01-01

In the present study, phase change materials based on epoxy resin paraffin wax with the melting point 27 °C were used as a new energy storage system. Thermophysical properties and the process of melting of a PCM (phase change material) composite were investigated numerically and experimentally. DSC (differential scanning calorimetry) has been used for measurement of melting enthalpy and determination of PCM heat capacity. The thermophysical properties of the prepared composite have been characterized by using a new transient hot plate apparatus. The results have shown that the most important thermal properties of these composites at the solid and liquid states are like the “apparent” thermal conductivity, the heat storage capacity and the latent heat of fusion. These experimental results have been simulated by using numerical Comsol ® Multiphysiques 4.3 based models with success. The results of the experimental investigation compare favorably with the numerical results and thus serve to validate the numerical approach. - Highlights: • Phase change materials based on paraffin spheres used as new energy storage system. • Thermophysical properties and the melting process of composites were investigated. • All experimental results have been simulated using Comsol ® Multiphysiques. • The ability to store and release the thermal energy were investigated. • A very thin molten PCM (phase change material) exists which is apparently visible in the spheres

Experimental (solid + liquid) or (liquid + liquid) phase equilibria of (amine + nitrile) binary mixtures

International Nuclear Information System (INIS)

Domanska, Urszula; Marciniak, Malgorzata

2007-01-01

(Solid + liquid) phase diagrams have been determined for (hexylamine, or octylamine, or 1,3-diaminopropane + acetonitrile) mixtures. Simple eutectic systems have been observed in these mixtures. (Liquid + liquid) phase diagrams have been determined for (octylamine, or decylamine + propanenitrile, or + butanenitrile) mixtures. Mixtures with propanenitrile and butanenitrile show immiscibility in the liquid phase with an upper critical solution temperature, UCST. (Solid + liquid) phase diagrams have been correlated using NRTL, NRTL 1, Wilson and UNIQUAC equations. (Liquid + liquid) phase diagrams have been correlated using NRTL equation

Improved detection limits for phthalates by selective solid-phase micro-extraction

KAUST Repository

Zia, Asif I.; Afsarimanesh, Nasrin; Xie, Li; Nag, Anindya; Al-Bahadly, I. H.; Yu, P. L.; Kosel, Jü rgen

2016-01-01

Presented research reports on an improved method and enhanced limits of detection for phthalates; a hazardous additive used in the production of plastics by solid-phase micro-extraction (SPME) polymer in comparison to molecularly imprinted solid

Elementary excitations and phase transformations in solids

International Nuclear Information System (INIS)

Cowley, R.A.

1985-01-01

Neutron scattering is and will continue to be a uniquely powerful tool for the study of elementary excitations and phase transformations in solids. The paper examines a few recent experiments on molecular crystals, superionic materials, paramagnetic scattering and phase transitions to see what experimental features made these experiments possible, and hence to make suggestions about future needs. It is concluded that new instruments will extend the scope of neutron scattering studies to new excitations, that there is a need for higher resolution, particularly for phase transition studies, and that it will be important to use intensity information, discrimination against unwanted inelastic processes and polarization analysis to reliably measure the excitations in new materials. (author)

Semi-automated microwave assisted solid-phase peptide synthesis

DEFF Research Database (Denmark)

Pedersen, Søren Ljungberg

with microwaves for SPPS has gained in popularity as it for many syntheses has provided significant improvement in terms of speed, purity, and yields, maybe especially in the synthesis of long and "difficult" peptides. Thus, precise microwave heating has emerged as one new parameter for SPPS, in addition...... to coupling reagents, resins, solvents etc. We have previously reported on microwave heating to promote a range of solid-phase reactions in SPPS. Here we present a new, flexible semi-automated instrument for the application of precise microwave heating in solid-phase synthesis. It combines a slightly modified...... Biotage Initiator microwave instrument, which is available in many laboratories, with a modified semi-automated peptide synthesizer from MultiSynTech. A custom-made reaction vessel is placed permanently in the microwave oven, thus the reactor does not have to be moved between steps. Mixing is achieved...

Investigation of solid-phase hydrogenation of amino acids and peptides

International Nuclear Information System (INIS)

Zolotarev, Yu.A.; Myasoedov, N.F.; Zajtsev, D.A.; Lubnin, M.Yu.; Tatur, V.Yu.; Kozik, V.S.; Dorokhova, E.M.; Rozenberg, S.N.

1990-01-01

The possibility of synthesizing amino acids and peptides multiply labelled with tritium or deuterium by the method of solid-phase isotopic exchange with gaseous hydrogen isotopes was verified. Establishment of the isotopic hydrogen equilibrium between the gaseous phase and the solid phase formed by the amino acid molecules was found experimentally. The activation energy of the isotopic exchange is 13 kcal/mol. A mathematical model was set up for the isotopic exchange with a probable substitution of hydrogen atoms. Uniformly labelled amino acids were obtained in a high optical purity and with 80 to 90% hydrogen substitution by deuterium and tritium. Tritiated peptides were prepared in high yields at molar activities of 1.5 to 3.7 TBq/mmol. (author). 4 tabs

The use of solid sorbents for direct accumulation of organic compounds from water matrices : a review of solid-phase extraction techniques

NARCIS (Netherlands)

Liska, I.; Krupcik, J.; Leclercq, P.A.

1989-01-01

The main principles of solid-phase extraction techniques are reviewed in this paper. Various solid sorbents can be used as a suitable trap for direct accumulation of organic compounds from aqueous solutions. The trapped analytes can be desorbed by elution with suitably chosen liquid phases. These

Geotechnical properties of municipal solid waste at different phases of biodegradation

International Nuclear Information System (INIS)

Reddy, Krishna R.; Hettiarachchi, Hiroshan; Gangathulasi, Janardhanan; Bogner, Jean E.

2011-01-01

Highlights: → Degraded synthetic municipal solid waste (MSW) anaerobically in controlled bench-scale reactors. → Performed laboratory tests to determine geotechnical properties of MSW at different phases of degradation. → Hydraulic conductivity decreased by two orders of magnitude due to degradation. → Compression ratio reduced from 0.34 for initial fresh waste to 0.15 for the mostly degraded waste. → Friction angle reduced, but cohesion increased with degradation. - Abstract: This paper presents the results of laboratory investigation conducted to determine the variation of geotechnical properties of synthetic municipal solid waste (MSW) at different phases of degradation. Synthetic MSW samples were prepared based on the composition of MSW generated in the United States and were degraded in bioreactors with leachate recirculation. Degradation of the synthetic MSW was quantified based on the gas composition and organic content, and the samples exhumed from the bioreactor cells at different phases of degradation were tested for the geotechnical properties. Hydraulic conductivity, compressibility and shear strength of initial and degraded synthetic MSW were all determined at constant initial moisture content of 50% on wet weight basis. Hydraulic conductivity of synthetic MSW was reduced by two orders of magnitude due to degradation. Compression ratio was reduced from 0.34 for initial fresh waste to 0.15 for the mostly degraded waste. Direct shear tests showed that the fresh and degraded synthetic MSW exhibited continuous strength gain with increase in horizontal deformation, with the cohesion increased from 1 kPa for fresh MSW to 16-40 kPa for degraded MSW and the friction angle decreased from 35 o for fresh MSW to 28 o for degraded MSW. During the triaxial tests under CU condition, the total strength parameters, cohesion and friction angle, were found to vary from 21 to 57 kPa and 1 o to 9 o , respectively, while the effective strength parameters, cohesion

Zinc composite anode for batteries with solid electrolyte

Science.gov (United States)

Tedjar, F.; Melki, T.; Zerroual, L.

A new negative composite anode for batteries with a solid electrolyte is studied. Using a complex of zinc ammonium chloride mixed with zinc metal powder, the advantage of the Zn/Zn 2+ electrode ( e = -760 mV) is kept while the energy density and the shelf-life of the battery are increased.

Municipal Solid Waste Composition Study of Selected Area in Gambang, Pahang

International Nuclear Information System (INIS)

Mokhtar, Nadiah; Romali, Noor Suraya; Osmi, Siti Fatimah Che; Ishak, Wan Faizal Wan; Samah, Mohd Armi Abu

2013-01-01

The amount of municipal solid waste (MSW) generated continue to increase in response to rapid growth in population, change in life style and accelerated urbanization and industrialization process. The study on MSW is important in order to determine the composition further seeks an immediate remedy to minimize the waste generated at the early stage. As most of the MSW goes to the landfill or dumping sites, particularly in Malaysia, closure of filled-up landfill may become an alarm clock for an immediate action of proper solid waste management. This research aims to determine the waste composition generated from selected residential area at Gambang, Kuantan, Pahang which represent Old residential area (ORA), Intermediate residential area (IRA) and New residential area (NRA). The study was conducted by segregating and weighing solid waste in the residential area into 6 main components ie., food waste, paper, plastic, glass, metal and others. In a period of four weeks, samples from the residential unit were taken and analyzed. The MSW generation rates were recorded vary from 0.217 to 0.388 kg person −1 day −1 . Food waste has become the major solid waste component generated daily which mounted up to 50%. From this research, the result revealed that the recyclable composition of waste generated by residents have a potential to be reuse, recycle and reduce at the point sources.

Municipal Solid Waste Composition Study of Selected Area in Gambang, Pahang

Science.gov (United States)

Mokhtar, Nadiah; Ishak, Wan Faizal Wan; Suraya Romali, Noor; Fatimah Che Osmi, Siti; Armi Abu Samah, Mohd

2013-06-01

The amount of municipal solid waste (MSW) generated continue to increase in response to rapid growth in population, change in life style and accelerated urbanization and industrialization process. The study on MSW is important in order to determine the composition further seeks an immediate remedy to minimize the waste generated at the early stage. As most of the MSW goes to the landfill or dumping sites, particularly in Malaysia, closure of filled-up landfill may become an alarm clock for an immediate action of proper solid waste management. This research aims to determine the waste composition generated from selected residential area at Gambang, Kuantan, Pahang which represent Old residential area (ORA), Intermediate residential area (IRA) and New residential area (NRA). The study was conducted by segregating and weighing solid waste in the residential area into 6 main components ie., food waste, paper, plastic, glass, metal and others. In a period of four weeks, samples from the residential unit were taken and analyzed. The MSW generation rates were recorded vary from 0.217 to 0.388 kg person-1day-1. Food waste has become the major solid waste component generated daily which mounted up to 50%. From this research, the result revealed that the recyclable composition of waste generated by residents have a potential to be reuse, recycle and reduce at the point sources.

Solid particle erosion of polymers and composites

Science.gov (United States)

Friedrich, K.; Almajid, A. A.

2014-05-01

After a general introduction to the subject of solid particle erosion of polymers and composites, the presentation focusses more specifically on the behavior of unidirectional carbon fiber (CF) reinforced polyetheretherketone (PEEK) composites under such loadings, using different impact conditions and erodents. The data were analyzed on the basis of a newly defined specific erosive wear rate, allowing a better comparison of erosion data achieved under various testing conditions. Characteristic wear mechanisms of the CF/PEEK composites consisted of fiber fracture, matrix cutting and plastic matrix deformation, the relative contribution of which depended on the impingement angles and the CF orientation. The highest wear rates were measured for impingement angles between 45 and 60°. Using abrasion resistant neat polymer films (in this case PEEK or thermoplastic polyurethane (TPU) ones) on the surface of a harder substrate (e.g. a CF/PEEK composite plate) resulted in much lower specific erosive wear rates. The use of such polymeric films can be considered as a possible method to protect composite surfaces from damage caused by minor impacts and erosion. In fact, they are nowadays already successfully applied as protections for wind energy rotor blades.

Estimated D2--DT--T2 phase diagram in the three-phase region

International Nuclear Information System (INIS)

Souers, P.C.; Hickman, R.G.; Tsugawa, R.T.

1976-01-01

A composite of experimental eH 2 -D 2 phase-diagram data at the three-phase line is assembled from the literature. The phase diagram is a smooth cigar shape without a eutectic point, indicating complete miscibility of liquid and solid phases. Additional data is used to estimate the D 2 -T 2 , D 2 DT, and DT-T 2 binary phase diagrams. These are assembled into the ternary D 2 -DT-T 2 phase diagram. A surface representing the chemical equilibrium of the three species is added to the phase diagram. At chemical equilibrium, it is estimated that 50-50 liquid D-T at 19.7 0 K is in equilibrium with 42 mole percent T vapor and 54 percent T solid. Infrared spectroscopy is suggested as a means of component analysis of liquid and solid mixtures

A reactor/separator device for use in automated solid phase immunoassay

International Nuclear Information System (INIS)

Farina, P.R.; Ordonez, K.P.; Siewers, I.J.

1979-01-01

A reactor/separator device is described for use in automated solid phase immunoassay, including radioimmunoassays. The device is a column fitted at the bottom portion with a water impermeable disc which can hold, for example, immunoabsorbents, immobilized antisera or ion exchange resins. When the contents of the column supported by the disc are brought into contact with an aqueous phase containing reagents or reactants, a chemical reaction is initiated. After the reaction, centrifugally applied pressure forces the aqueous phase through the filter disc making it water permeable and separating a desired component for subsequent analysis. The reactor/separator device of the present invention permits kinetic solid phase assays (non-equilibrium conditions) to be carried out which would be difficult to perform by other conventional methods. (author)

Solid-phase photocatalytic degradation of polystyrene plastic with goethite modified by boron under UV-vis light irradiation

International Nuclear Information System (INIS)

Liu Guanglong; Zhu Duanwei; Zhou Wenbing; Liao Shuijiao; Cui Jingzhen; Wu Kang; Hamilton, David

2010-01-01

A novel photodegradable polyethylene-boron-goethite (PE-B-goethite) composite film was prepared by embedding the boron-doped goethite into the commercial polyethylene. The goethite catalyst was modified by boron in order to improve its photocatalytic efficiency under the ultraviolet and visible light irradiation. Solid-phase photocatalytic degradation of the PE-B-goethite composite film was carried out in an ambient air at room temperature under ultraviolet and visible light irradiation. The properties of composite films were compared with those of the pure PE films and the PE-goethite composite films through performing weight loss monitoring, scanning electron microscope (SEM) analysis, FT-IR spectroscopy and X-ray photoelectron spectroscopy (XPS). The photo-induced degradation of PE-B-goethite composite films was higher than that of the pure PE films and the PE-goethite composite films under the UV-irradiation, while there has been little change under the visible light irradiation. The weight loss of the PE-B-goethite (0.4 wt.%) composite film reached 12.6% under the UV-irradiation for 300 h. The photocatalytic degradation mechanism of the composite films was briefly discussed.

Solid oxide fuel cell having a glass composite seal

Science.gov (United States)

De Rose, Anthony J.; Mukerjee, Subhasish; Haltiner, Jr., Karl Jacob

2013-04-16

A solid oxide fuel cell stack having a plurality of cassettes and a glass composite seal disposed between the sealing surfaces of adjacent cassettes, thereby joining the cassettes and providing a hermetic seal therebetween. The glass composite seal includes an alkaline earth aluminosilicate (AEAS) glass disposed about a viscous glass such that the AEAS glass retains the viscous glass in a predetermined position between the first and second sealing surfaces. The AEAS glass provides geometric stability to the glass composite seal to maintain the proper distance between the adjacent cassettes while the viscous glass provides for a compliant and self-healing seal. The glass composite seal may include fibers, powders, and/or beads of zirconium oxide, aluminum oxide, yttria-stabilized zirconia (YSZ), or mixtures thereof, to enhance the desirable properties of the glass composite seal.

Faults of solid-phase welding in titanium joints and their effect on strength

International Nuclear Information System (INIS)

Matyushkin, B.A.; Redchits, V.V.

1982-01-01

A possibility of the usage of thermal arc energy for the determination of the kinetics of solid-phase joint formation of the VT20 titanium alloy is found out experimentally. Positive action of diffusion annealing upon mechanical properties. of solid-phase joints is explained by the defect elimination

Towards the improvement of the oxidation resistance of Nb-silicides in situ composites: A solid state diffusion approach

International Nuclear Information System (INIS)

Mathieu, S.; Knittel, S.; François, M.; Portebois, L.; Mathieu, S.; Vilasi, M.

2014-01-01

Highlights: •Local equilibrium is attained during oxidation at phase boundaries (steady state conditions). •A solid state diffusion model explains the oxidation mechanism of Nb-silicides composites. •The Nb ss fraction is not the only parameters governing the oxidation rate of Nb-silicides. •Aluminium increases the thermodynamic activity of Si in the Nb-silicides composites. •The results indicate the need to develop a Nb–Ti–Hf–Al–Cr–Si thermodynamic database. -- Abstract: The present study focuses on the oxidation mechanism of Nb-silicide composites and on the effect of the composition on the oxidation rate at 1100 °C. A theoretical approach is proposed based on experimental results and used to optimise the oxidation resistance. The growth model based on multiphase diffusion was experimentally tested and confirmed by manufacturing seven composites with different compositions. It was also found that the effect of the composition has to be evaluated at 1100 °C within a short time duration (50 h), where the oxide scale and the internal oxidation zone both grow according to parabolic kinetics

Method for calculating solid-solid phase transitions at high temperature: An application to N2O

International Nuclear Information System (INIS)

Kuchta, B.; Etters, R.D.

1992-01-01

Two similar techniques for calculating solid-solid phase transitions at high temperatures are developed, where the contribution of the entropy may be a decisive factor. They utilize an artificial reversible path from one phase to another by application of a control parameter. Thermodynamic averages are calculated using constant-volume and constant-pressure Monte Carlo techniques. An application to N 2 O at room temperature shows that the cubic Pa3 to orthorhombic Cmca transition occurs near 4.9-GPa pressure, very close to the value calculated at very low temperatures. These results support experimental evidence that the transition pressure is virtually independent of temperature

Zinc composite anode for batteries with solid electrolyte

Energy Technology Data Exchange (ETDEWEB)

Tedjar, F.; Melki, T.; Zerroual, L. (Setif Univ. (Algeria). Unite de Recherche Electrochimie)

1992-05-01

A new negative composite anode for batteries with a solid electrolyte is studied. Using a complex of zinc ammonium chloride mixed with zinc metal powder, the advantage of the Zn/Zn[sup 2+] electrode (e = -760 mV) is kept while the energy density and the shelf-life of the battery are increased. (orig.).

Comprehensive profiling of ribonucleosides modification by affinity zirconium oxide-silica composite monolithic column online solid-phase microextraction - Mass spectrometry analysis.

Science.gov (United States)

Jiang, Han-Peng; Chu, Jie-Mei; Lan, Meng-Dan; Liu, Ping; Yang, Na; Zheng, Fang; Yuan, Bi-Feng; Feng, Yu-Qi

2016-09-02

More than 140 modified ribonucleosides have been identified in RNA. Determination of endogenous modified ribonucleosides in biological fluids may serve as non-invasive disease diagnostic strategy. However, detection of the modified ribonucleosides in biological fluids is challenging, especially for the low abundant modified ribonucleosides due to the serious matrix interferences of biological fluids. Here, we developed a facile preparation strategy and successfully synthesized zirconium oxide-silica (ZrO2/SiO2) composite capillary monolithic column that exhibited excellent performance for the selective enrichment of cis-diol-containing compounds. Compared with the boronate-based affinity monolith, the ZrO2/SiO2 monolith showed ∼2 orders of magnitude higher extraction capacity and can be used under physiological pH (pH 6.5-7.5). Using the prepared ZrO2/SiO2 composite monolith as the trapping column and reversed-phase C18 column as the analytical column, we further established an online solid-phase microextraction (SPME) in combination with liquid chromatography-mass spectrometry (online SPME-LC-MS/MS) analysis for the comprehensive profiling of ribonucleosides modification in human urine. Our results showed that 68 cis-diol-containing ribosylated compounds were identified in human urine, which is, to the best of our knowledge, the highest numbers of cis-diol-containing compounds were determined in a single analysis. It is worth noting that four modified ribonucleosides were discovered in the human urine for the first time. In addition, the quantification results from the pooled urine samples showed that compared to healthy controls, the contents of sixteen ribose conjugates in the urine of gastric cancer, eleven in esophagus cancer and seven in lymphoma increased more than two folds. Among these ribose conjugates, four ribose conjugates increased more than two folds in both gastric cancer and esophagus cancer; three ribose conjugates increased more than two

A review of solid-fluid selection options for optical-based measurements in single-phase liquid, two-phase liquid-liquid and multiphase solid-liquid flows

Science.gov (United States)

Wright, Stuart F.; Zadrazil, Ivan; Markides, Christos N.

2017-09-01

Experimental techniques based on optical measurement principles have experienced significant growth in recent decades. They are able to provide detailed information with high-spatiotemporal resolution on important scalar (e.g., temperature, concentration, and phase) and vector (e.g., velocity) fields in single-phase or multiphase flows, as well as interfacial characteristics in the latter, which has been instrumental to step-changes in our fundamental understanding of these flows, and the development and validation of advanced models with ever-improving predictive accuracy and reliability. Relevant techniques rely upon well-established optical methods such as direct photography, laser-induced fluorescence, laser Doppler velocimetry/phase Doppler anemometry, particle image/tracking velocimetry, and variants thereof. The accuracy of the resulting data depends on numerous factors including, importantly, the refractive indices of the solids and liquids used. The best results are obtained when the observational materials have closely matched refractive indices, including test-section walls, liquid phases, and any suspended particles. This paper reviews solid-liquid and solid-liquid-liquid refractive-index-matched systems employed in different fields, e.g., multiphase flows, turbomachinery, bio-fluid flows, with an emphasis on liquid-liquid systems. The refractive indices of various aqueous and organic phases found in the literature span the range 1.330-1.620 and 1.251-1.637, respectively, allowing the identification of appropriate combinations to match selected transparent or translucent plastics/polymers, glasses, or custom materials in single-phase liquid or multiphase liquid-liquid flow systems. In addition, the refractive indices of fluids can be further tuned with the use of additives, which also allows for the matching of important flow similarity parameters such as density and viscosity.

All-solid state flexible supercapacitors based on graphene/polymer composites

Energy Technology Data Exchange (ETDEWEB)

Kim, Jung Won; Choi, Bong Gill, E-mail: bgchoi@kangwon.ac.kr

2015-06-01

Recent advances in lightweight, flexible, and wearable electronic equipment has led to advancements in the development of sufficiently compact and flexible energy storage. A challenge remains to integrate the storage elements as closely as possible within a fully flexible device. Here, we demonstrate the fabrication of all-solid state flexible supercapacitors with the integration of two electrodes that consist of graphene/polymer composites. Robust conductive free-standing thin graphene/polymer composite electrodes were prepared through a simple “physical grinding” process. As-prepared composite electrodes store energy up to a reversible gravimetric capacitance of 90.6 F/g, at a constant current density of 0.5 A/g while also delivering long-term durability (90% retention) for excess of five-thousands of cycles. Notably, the enhancement of mechanical properties of supercapacitors enables them to maintain their electrochemical performance even when twisted or folded. This straightforward approach to the fabrication of fully flexible supercapacitors provides new design opportunities within wearable electronics and electrochemical applications. - Highlights: • All solid-sate supercapacitors were fabricated using graphene/polymer composite electrodes. • Supercapacitor devices show an excellent mechanical flexibility. • High electrochemical performances were demonstrated.

All-solid state flexible supercapacitors based on graphene/polymer composites

International Nuclear Information System (INIS)

Kim, Jung Won; Choi, Bong Gill

2015-01-01

Recent advances in lightweight, flexible, and wearable electronic equipment has led to advancements in the development of sufficiently compact and flexible energy storage. A challenge remains to integrate the storage elements as closely as possible within a fully flexible device. Here, we demonstrate the fabrication of all-solid state flexible supercapacitors with the integration of two electrodes that consist of graphene/polymer composites. Robust conductive free-standing thin graphene/polymer composite electrodes were prepared through a simple “physical grinding” process. As-prepared composite electrodes store energy up to a reversible gravimetric capacitance of 90.6 F/g, at a constant current density of 0.5 A/g while also delivering long-term durability (90% retention) for excess of five-thousands of cycles. Notably, the enhancement of mechanical properties of supercapacitors enables them to maintain their electrochemical performance even when twisted or folded. This straightforward approach to the fabrication of fully flexible supercapacitors provides new design opportunities within wearable electronics and electrochemical applications. - Highlights: • All solid-sate supercapacitors were fabricated using graphene/polymer composite electrodes. • Supercapacitor devices show an excellent mechanical flexibility. • High electrochemical performances were demonstrated

A novel poly(deep eutectic solvent)-based magnetic silica composite for solid-phase extraction of trypsin.

Science.gov (United States)

Xu, Kaijia; Wang, Yuzhi; Li, Yixue; Lin, Yunxuan; Zhang, Haibao; Zhou, Yigang

2016-11-23

Novel poly(deep eutectic solvent) grafted silica-coated magnetic microspheres (Fe 3 O 4 @SiO 2 -MPS@PDES) were prepared by polymerization of choline chloride-itaconic acid (ChCl-IA) and γ-MPS-modified magnetic silica composites, and were characterized by vibrating sample magnetometer (VSM), Fourier transform infrared spectrometry (FT-IR), X-ray photoelectron spectra (XPS), thermal gravimetric analysis (TGA) and transmission electron microscope (TEM). Then the synthetic Fe 3 O 4 @SiO 2 -MPS@PDES microspheres were applied for the magnetic solid-phase extraction (MSPE) of trypsin for the first time. After extraction, the concentration of trypsin in the supernatant was determined by a UV-vis spectrophotometer. Single factor experiments were carried out to investigate the effects of the extraction process, including the concentration of trypsin, the ionic strength, the pH value, the extraction time and the temperature. Experimental results showed the extraction capacity could reach up to 287.5 mg/g under optimized conditions. In comparison with Fe 3 O 4 @SiO 2 -MPS, Fe 3 O 4 @SiO 2 -MPS@PDES displayed higher extraction capacity and selectivity for trypsin. According to the regeneration studies, Fe 3 O 4 @SiO 2 -MPS@PDES microspheres can be recycled six times without significant loss of its extraction capacity, and retained a high extraction capacity of 233 mg/g after eight cycles. Besides, the activity studies also demonstrated that the activity of the extracted trypsin was well retained. Furthermore, the analysis of real sample revealed that the prepared magnetic microspheres can be used to purify trypsin in crude bovine pancreas extract. These results highlight the potential of the proposed Fe 3 O 4 @SiO 2 -MPS@PDES-MSPE method in separation of biomolecules. Copyright © 2016 Elsevier B.V. All rights reserved.

Phase transitions of amorphous solid acetone in confined geometry investigated by reflection absorption infrared spectroscopy.

Science.gov (United States)

Shin, Sunghwan; Kang, Hani; Kim, Jun Soo; Kang, Heon

2014-11-26

We investigated the phase transformations of amorphous solid acetone under confined geometry by preparing acetone films trapped in amorphous solid water (ASW) or CCl4. Reflection absorption infrared spectroscopy (RAIRS) and temperature-programmed desorption (TPD) were used to monitor the phase changes of the acetone sample with increasing temperature. An acetone film trapped in ASW shows an abrupt change in the RAIRS features of the acetone vibrational bands during heating from 80 to 100 K, which indicates the transformation of amorphous solid acetone to a molecularly aligned crystalline phase. Further heating of the sample to 140 K produces an isotropic solid phase, and eventually a fluid phase near 157 K, at which the acetone sample is probably trapped in a pressurized, superheated condition inside the ASW matrix. Inside a CCl4 matrix, amorphous solid acetone crystallizes into a different, isotropic structure at ca. 90 K. We propose that the molecularly aligned crystalline phase formed in ASW is created by heterogeneous nucleation at the acetone-water interface, with resultant crystal growth, whereas the isotropic crystalline phase in CCl4 is formed by homogeneous crystal growth starting from the bulk region of the acetone sample.

Enhanced ionic conductivity with Li{sub 7}O{sub 2}Br{sub 3} phase in Li{sub 3}OBr anti-perovskite solid electrolyte

Energy Technology Data Exchange (ETDEWEB)

Zhu, Jinlong, E-mail: jlzhu04@physics.unlv.edu, E-mail: yusheng.zhao@unlv.edu, E-mail: zhaoys@sustc.edu.cn; Li, Shuai; Zhang, Yi; Howard, John W.; Wang, Yonggang; Kumar, Ravhi S.; Wang, Liping [High Pressure Science and Engineering Center, University of Nevada, Las Vegas, Nevada 89154 (United States); Lü, Xujie [Center for Integrated Nanotechnologies and Earth and Environmental Sciences Division, Los Alamos National Laboratory, Los Alamos, New Mexico 87545 (United States); Li, Yutao [Materials Research Program and The Texas Materials Institute, University of Texas at Austin, Texas 78712 (United States); Zhao, Yusheng, E-mail: jlzhu04@physics.unlv.edu, E-mail: yusheng.zhao@unlv.edu, E-mail: zhaoys@sustc.edu.cn [High Pressure Science and Engineering Center, University of Nevada, Las Vegas, Nevada 89154 (United States); Department of Physics, South University of Science and Technology of China, Guangdong 518055 (China)

2016-09-05

Cubic anti-perovskites with general formula Li{sub 3}OX (X = Cl, Br, I) were recently reported as superionic conductors with the potential for use as solid electrolytes in all-solid-state lithium ion batteries. These electrolytes are nonflammable, low-cost, and suitable for thermoplastic processing. However, the primary obstacle of its practical implementation is the relatively low ionic conductivity at room temperature. In this work, we synthesized a composite material consisting of two anti-perovskite phases, namely, cubic Li{sub 3}OBr and layered Li{sub 7}O{sub 2}Br{sub 3,} by solid state reaction routes. The results indicate that with the phase fraction of Li{sub 7}O{sub 2}Br{sub 3} increasing to 44 wt. %, the ionic conductivity increased by more than one order of magnitude compared with pure phase Li{sub 3}OBr. Formation energy calculations revealed the meta-stable nature of Li{sub 7}O{sub 2}Br{sub 3}, which supports the great difficulty in producing phase-pure Li{sub 7}O{sub 2}Br{sub 3} at ambient pressure. Methods of obtaining phase-pure Li{sub 7}O{sub 2}Br{sub 3} will continue to be explored, including both high pressure and metathesis techniques.

Solid-phase micro-extraction in bioanalysis, exemplified by lidocaine determination

NARCIS (Netherlands)

de Jong, GJ; Koster, EHM

2000-01-01

Solid-phase micro-extraction (SPME) is a never sample preparation technique that can be used for gaseous, liquid or solid samples in conjunction with GC, HPLC or CE (e.g. [1]). The use of SPME for the analysis of drugs in biofluids is also becoming popular (e.g. [2]). The principle is that a fused

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 ...

Solid phase separation technique for use in radioimmunoassays

International Nuclear Information System (INIS)

Tu, J.I.

1979-01-01

A radioimmunoassay procedure, and article of manufacture for carrying out that procedure, are disclosed herein. The solid phase separation technique utilized in the radioimmunoassay of this invention utilizes a test tube, the internal surface of which has been coated with two antibody layers

Studies in Solid Phase Peptide Synthesis: A Personal Perspective

Energy Technology Data Exchange (ETDEWEB)

Mitchell, A R

2007-06-01

By the early 1970s it had became apparent that the solid phase synthesis of ribonuclease A could not be generalized. Consequently, virtually every aspect of solid phase peptide synthesis (SPPS) was reexamined and improved during the decade of the 1970s. The sensitive detection and elimination of possible side reactions (amino acid insertion, N{sup {alpha}}-trifluoroacetylation, N{sup {alpha}{var_epsilon}}-alkylation) was examined. The quantitation of coupling efficiency in SPPS as a function of chain length was studied. A new and improved support for SPPS, the 'PAM-resin', was prepared and evaluated. These and many other studies from the Merrifield laboratory and elsewhere increased the general acceptance of SPPS leading to the 1984 Nobel Prize in Chemistry for Bruce Merrifield.

Anodic stripping voltammetry using graphite composite solid electrode

Czech Academy of Sciences Publication Activity Database

Navrátil, Tomáš; Barek, J.; Kopanica, Miloslav

2009-01-01

Roč. 74, 11-12 (2009), s. 1807-1826 ISSN 0010-0765 R&D Projects: GA AV ČR IAA400400806; GA ČR GA203/07/1195; GA MŠk(CZ) LC06035 Institutional research plan: CEZ:AV0Z40400503 Keywords : Graphite composite solid electrode * voltammetry * metals Subject RIV: CG - Electrochemistry Impact factor: 0.856, year: 2009

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.

Investigation of binary solid phases by calorimetry and kinetic modelling

NARCIS (Netherlands)

Matovic, M.

2007-01-01

The traditional methods for the determination of liquid-solid phase diagrams are based on the assumption that the overall equilibrium is established between the phases. However, the result of the crystallization of a liquid mixture will typically be a non-equilibrium or metastable state of the

Development and Application of Solid Phase Extraction Method for ...

African Journals Online (AJOL)

NICO

for the addition of organic modifier, sample load volume, conditioning solvent, washing solvent and ... Solid phase extraction, polycyclic aromatic hydrocarbons, water samples, ... such as polymeric, activated carbon or silica modified with.

Ion-selective solid-phase electrode sensitive to ammonium ions

International Nuclear Information System (INIS)

Vlasov, Yu.G.; Milonova, M.S.; Antonov, P.P.; Bychkov, E.A.; Ehfa, A.Ya.

1983-01-01

Ammonium phosphomolybdate is investigated for the purpose of using it as membrane material of ammonium-selective solid-phase electrodes. Estimation of proton mobility and ion conductivity of ammonium phosphomolybdate is performed

Graphene oxide-TiO2 composite solid phase extraction combined with graphite furnace atomic absorption spectrometry for the speciation of inorganic selenium in water samples.

Science.gov (United States)

Zhang, Yanan; Chen, Beibei; Wu, Shaowei; He, Man; Hu, Bin

2016-07-01

In this paper, a method of graphene oxide (GO)-TiO2 composite solid phase extraction followed by graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the speciation of inorganic selenium in environmental waters. The adsorption behavior of inorganic Se(IV) and Se(VI) on the GO-TiO2(1:1) composite was investigated. It was found that Se(IV) was quantitatively retained on the GO-TiO2 composites within a wide pH range of 0.5-10, while Se(VI) was quantitatively adsorbed on GO-TiO2(1:1) composite at pH 0.5-2, and no obvious adsorption of Se(VI) within the pH range of 4-10 was found. By selecting pH 6.0, Se(IV) could be easily determined. After reduction of Se(VI), total Se was determined by the proposed method, and Se(VI) was calculated as the difference between the total Se and Se(IV). The factors affecting the separation/preconcentration of Se(IV) and Se(VI) were studied. Under the optimum conditions, the isothermal adsorption of Se(IV) on the GO-TiO2(1:1) composite fitted Langmuir model; a linear range over 0.1-12ngmL(-1) was obtained. The limit of detection (LOD) and precision of the method for Se(IV) was 0.04ngmL(-1) and 9.4% (cSe(IV)=0.5ngmL(-1), n=7), respectively. In order to verify the accuracy of the method, a standard water sample (GSBZ50031-94) was analyzed, and the determined value was in a good agreement to the certified value. The established method was applied to inorganic Se speciation in environmental water samples and the recovery of 87.4-102% was obtained for the spiked samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Fabrication and characterization of dual-functional ultrafine composite fibers with phase-change energy storage and luminescence properties.

Science.gov (United States)

Xi, Peng; Zhao, Tianxiang; Xia, Lei; Shu, Dengkun; Ma, Menjiao; Cheng, Bowen

2017-01-09

Ultrafine composite fibers consisting of a thermoplastic polyurethane solid-solid phase-change material and organic lanthanide luminescent materials were prepared through a parallel electrospinning technique as an innovative type of ultrafine, dual-functional fibers containing phase-change and luminescent properties. The morphology and structure, thermal energy storage, and luminescent properties of parallel electrospun ultrafine fibers were investigated. Scanning electron microscopy (SEM) images showed that the parallel electrospun ultrafine fibers possessed the desired morphologies with smaller average fiber diameters than those of traditional mixed electrospun ultrafine fibers. Transmission electron microscopy (TEM) images revealed that the parallel electrospun ultrafine fibers were composed of two parts. Polymeric phase-change materials, which can be directly produced and spun, were used to provide temperature stability, while a mixture of polymethyl methacrylate and an organic lanthanide complex acted as the luminescent unit. Differential scanning calorimetry (DSC) and luminescence measurements indicated that the unique structure of the parallel electrospun ultrafine fibers provides the products with good thermal energy storage and luminescence properties. The fluorescence intensity and the phase-change enthalpy values of the ultrafine fibers prepared by parallel electrospinning were respectively 1.6 and 2.1 times those of ultrafine fibers prepared by mixed electrospinning.

Copper-substituted perovskite compositions for solid oxide fuel cell cathodes and oxygen reduction electrodes in other electrochemical devices

Science.gov (United States)

Rieke, Peter C [Pasco, WA; Coffey, Gregory W [Richland, WA; Pederson, Larry R [Kennewick, WA; Marina, Olga A [Richland, WA; Hardy, John S [Richland, WA; Singh, Prabhaker [Richland, WA; Thomsen, Edwin C [Richland, WA

2010-07-20

The present invention provides novel compositions that find advantageous use in making electrodes for electrochemical cells. Also provided are electrochemical devices that include active oxygen reduction electrodes, such as solid oxide fuel cells, sensors, pumps and the like. The compositions comprises a copper-substituted ferrite perovskite material. The invention also provides novel methods for making and using the electrode compositions and solid oxide fuel cells and solid oxide fuel cell assemblies having cathodes comprising the compositions.

Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction of herbicides in peanuts.

Science.gov (United States)

Li, Na; Wang, Zhibing; Zhang, Liyuan; Nian, Li; Lei, Lei; Yang, Xiao; Zhang, Hanqi; Yu, Aimin

2014-10-01

Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction was developed and applied to the extraction of pesticides in high fatty matrices. The herbicides were ultrasonically extracted from peanut using ethyl acetate as extraction solvent. The separation of the analytes from a large amount of co-extractive fat was achieved by dispersive solid-phase extraction using MIL-101(Cr) as sorbent. In this step, the analytes were adsorbed on MIL-101(Cr) and the fat remained in bulk. The herbicides were separated and determined by high-performance liquid chromatography. The experimental parameters, including type and volume of extraction solvent, ultrasonication time, volume of hexane and eluting solvent, amount of MIL-101(Cr) and dispersive solid phase extraction time, were optimized. The limits of detection for herbicides range from 0.98 to 1.9 μg/kg. The recoveries of the herbicides are in the range of 89.5-102.7% and relative standard deviations are equal or lower than 7.0%. The proposed method is simple, effective and suitable for treatment of the samples containing high content of fat. Copyright © 2014 Elsevier B.V. All rights reserved.

Facile synthesis of aliphatic isothiocyanates and thioureas on solid phase using peptide coupling reagents

DEFF Research Database (Denmark)

Boas, Ulrik; Andersen, Heidi Gertz; Christensen, Jørn B.

2004-01-01

Peptide coupling reagents can be used as versatile reagents for the formation of aliphatic isothiocyanates and thioureas on solid phase from the corresponding solid-phase anchored aliphatic primary amines. The formation of the thioureas is fast and highly chemoselective, and proceeds via formatio...

Tetraphenylimidodiphosphinate as solid phase extractant for preconcentrative separation of thorium from aqueous solution

International Nuclear Information System (INIS)

Na Liu; Yanfei Wang; Chuhua He

2016-01-01

A simple and reliable method for solid phase extraction of thorium using tetraphenylimidodiphosphinate is presented. The solid phase extraction process was optimized at equilibrium time 3 h, pH = 4.5, initial concentration 30 mg L -1 and extractant dosage 0.01 g with 98.95 % of removal efficiency and 29.68 mg g -1 of adsorption capacity. The interfering ions experiments indicated that it had almost no effect on thorium adsorption. Kinetics data follow the pseudo-first-order model and equilibrium data agreed with the Langmuir isotherm model very well. FT-IR analysis indicated that imino group and phosphoryl acted as the significant roles in the solid phase extraction process. (author)

Investigation of a nanoconfined, ceramic composite, solid polymer electrolyte

International Nuclear Information System (INIS)

Jayasekara, Indumini; Poyner, Mark; Teeters, Dale

2017-01-01

The challenges for further development of lithium rechargeable batteries are finding electrolyte materials that are safe, have mechanical and thermal stability and have sufficiently high ionic conduction. Polymer electrolytes have many of these advantages, but suffer with low ionic conduction. This study involves the use of anodic aluminum oxide (AAO) membranes having nanochannels filled with polymer electrolyte to make composite solid electrolytes having ionic conductivity several orders of magnitude higher (10 −4 Ω ‐1 cm −1 ) than non-confined polymer. SEM, ac impedance spectroscopy, temperature dependence studies, XRD, ATR- FTIR and DSC studies were done in order to characterize and understand the behavior of nanoconfined polymer electrolytes. The composite polymer electrolyte was found to be more amorphous with polymer chains aligned in the direction of the nanochannels, which is felt to promote ion conduction. The electrolyte systems, confined in nanoporous membranes, can be used as electrolytes for the fabrication of a room temperature all solid state battery.

Electrophoretic deposition of 9-YSZ solid electrolyte on Ni- YSZ composite

International Nuclear Information System (INIS)

Santos, F.S.; Yoshito, W.K.; Lazar, D.R.R.; Ussui, V.

2010-01-01

9-YSZ ceramic and Ni-YSZ metal/ceramic composite are the more commonly used materials for the fabrication of solid oxide fuel cell electrolyte and anode, respectively. The main challenges for these applications are the forming of both materials as superposed double thin layers. In the present work ceramic powder of 9- YSZ was synthesized by a coprecipitation technique and the Ni O-YSZ composite by a combustion technique. The later was formed by uniaxial pressing as cylindrical pellets of 15 mm diameter. Thin ceramic layers of 9-YSZ were deposited on composite pellets from a suspension with 10% solid content by an Electrophoretic Deposition technique. Applied voltage varied in the range of 30 to 200 V and deposition time from 15 to 90 seconds, evaluating the deposited mass, porosity on the interface and adhesion of layers. Resulted ceramics were characterized by X-ray diffraction and were observed in a scanning electron microscope. Results showed that deposited layers are thin (∼20μm), dense and have good adhesion on the surface of composite substrate. (author)

Zirconium determination in rocks by solid-phase spectrophotometry

International Nuclear Information System (INIS)

Brykina, G.D.; Lebedeva, G.G.; Agapova, G.F.; AN SSSR, Moscow

1990-01-01

A method was developed for determination of zirconium in rocks by solid-phase spectrophotometry using AV-17x8-Cl anion exchanger modified with xylenol orange. Relative standard deviation at the level of (2-4.9)x10 -3 % ZrO 2 was about 0.245

Solid Phase Radioimmunoassay for Measuring Serum Prolactin Using Antibody Coupled Magnetizable Particles

International Nuclear Information System (INIS)

El-Bayoumy, A.S.A.

2012-01-01

The objective of the present work was to prepare solid phase radioimmunoassay (RIA) reagents. Development as well as optimization and validation of RIA system using solid phase magnetic particles for the measurement of prolactin (PRL) in human serum are described. The production of polyclonal antibodies was carried out by immunizing three Balb/C mice intraperitoneal through primary injection and two booster doses. Low density magnetizable cellulose iron oxide particles have been used to couple covalently to the IgG fraction of polyclonal anti-prolactin using carbonyl diimidazole activation method and applied as a solid phase separating agent for RIA of serum prolactin. Preparation of 125 I-PRL tracer was prepared using lactoperoxidase method and it was purified by gel filtration using sephadex G-100. The PRL standards were prepared using a highly purified PRL antigen with assay buffer as standard matrix. Optimization and validation of the assay were carried out. The results obtained provide a low cost, simple, sensitive, specific and accurate RIA system of prolactin based on magnetizable solid phase separation. These magnetic particles retain their characteristics during storage for 6 months at 4 degree C. In conclusion, this assay could be used as a useful diagnostic tool for pituitary dysfunction and possible reproductive disability.

Microwave assisted solid phase extraction for separation preconcentration sulfamethoxazole in wastewater using tyre based activated carbon as solid phase material prior to spectrophotometric determination

Science.gov (United States)

Mogolodi Dimpe, K.; Mpupa, Anele; Nomngongo, Philiswa N.

2018-01-01

This work was chiefly encouraged by the continuous consumption of antibiotics which eventually pose harmful effects on animals and human beings when present in water systems. In this study, the activated carbon (AC) was used as a solid phase material for the removal of sulfamethoxazole (SMX) in wastewater samples. The microwave assisted solid phase extraction (MASPE) as a sample extraction method was employed to better extract SMX in water samples and finally the analysis of SMX was done by the UV-Vis spectrophotometer. The microwave assisted solid phase extraction method was optimized using a two-level fractional factorial design by evaluating parameters such as pH, mass of adsorbent (MA), extraction time (ET), eluent ratio (ER) and microwave power (MP). Under optimized conditions, the limit of detection (LOD) and limit of quantification (LOQ) were 0.5 μg L- 1 and 1.7 μg L- 1, respectively, and intraday and interday precision expressed in terms of relative standard deviation were > 6%.The maximum adsorption capacity was 138 mg g- 1 for SMX and the adsorbent could be reused eight times. Lastly, the MASPE method was applied for the removal of SMX in wastewater samples collected from a domestic wastewater treatment plant (WWTP) and river water.

Bridging phases at the morphotropic boundaries of lead oxide solid solutions

NARCIS (Netherlands)

Noheda, Beatriz; Cox, DE

2006-01-01

Ceramic solid solutions of PbZr1-xTixO3 (PZT) with compositions x similar or equal to 0.50 are well-known for their extraordinarily large piezoelectric responses. The latter are highly anisotropic, and it was recently shown that, for the rhombohedral compositions (x less than or similar to 0.5), the

Solid-state phase equilibria in the Fe-Pt-Pr ternary system at 1173 K

International Nuclear Information System (INIS)

Ren Jing; Gu Zhengfei; Cheng Gang; Zhou Huaiying

2005-01-01

The solid-state phase equilibria in the Fe-Pt-Pr ternary system at 1173 K (Pr ≤ 70%) were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersion spectroscopy (EDS) techniques. The 1173 K isothermal section consists of 13 single-phase regions, 22 two-phase regions and 10 three-phase regions. At 1173 K, we have observed that the maximum solid solubility of Pt in α-Fe is below 1.5 at.% and the solid solution region of Pt in γ-Fe is from 2 to 35 at.%; the maximum solid solubility of Fe in Pt is 18 at.%. The maximum solubility of Fe in PrPt 5 , PrPt 3 , PrPt 2 , Pr 3 Pt 4 , PrPt, Pr 3 Pt 2 and Pr 7 Pt 3 is below 1 at.%. The maximum solubility of Pr in α-(Fe, Pt), γ-(Fe, Pt), FePt, FePt 3 and (Pt, Fe) (the solid solution of Fe in Pt) is 6, 2, 4, 4.5 and 1.5 at.%, respectively. In this work, it is found that the phase Pr 3 Pt 4 does not exist in the ternary system. The binary compounds Fe 7 Pr and Fe 2 Pr and any new ternary compounds were not observed

Practical solid and liquid phase markers for studying gastric emptying in man

International Nuclear Information System (INIS)

Thomforde, G.M.; Brown, M.L.; Malagelada, J.R.

1985-01-01

This paper presents a method used to evaluate solid and liquid phase markers for radionuclide gastric emptying studies. The authors conducted in vitro and in vivo comparative experiments employing several radiolabeled markers. Among the solid phase markers tested, Tc-99m-sulfur colloid in vivo-labeled liver and I-131-fiber performed optimally. However, Tc-99M sulfur colloid in scrambled egg showed very acceptable performance and it is significantly easier to prepare. Among liquid phase markers, they found In-111-DTPA stabilized with 1% albumin to be a good agent and appropriate for dual isotope emptying studies

Radiation-induced segregation on defect clusters in single-phase concentrated solid-solution alloys

International Nuclear Information System (INIS)

Lu, Chenyang; Yang, Taini; Jin, Ke; Gao, Ning; Xiu, Pengyuan; Zhang, Yanwen; Gao, Fei; Bei, Hongbin; Weber, William J.; Sun, Kai; Dong, Yan; Wang, Lumin

2017-01-01

A group of single-phase concentrated solid-solution alloys (SP-CSAs), including NiFe, NiCoFe, NiCoFeCr, as well as a high entropy alloy NiCoFeCrMn, was irradiated with 3 MeV Ni"2"+ ions at 773 K to a fluence of 5 × 10"1"6 ions/cm"2 for the study of radiation response with increasing compositional complexity. Advanced transmission electron microscopy (TEM) with electron energy loss spectroscopy (EELS) was used to characterize the dislocation loop distribution and radiation-induced segregation (RIS) on defect clusters in the SP-CSAs. The results show that a higher fraction of faulted loops exists in the more compositionally complex alloys, which indicate that increasing compositional complexity can extend the incubation period and delay loop growth. The RIS behaviors of each element in the SP-CSAs were observed as follows: Ni and Co tend to enrich, but Cr, Fe and Mn prefer to deplete near the defect clusters. RIS level can be significantly suppressed by increasing compositional complexity due to the sluggish atom diffusion. According to molecular static (MS) simulations, “disk” like segregations may form near the faulted dislocation loops in the SP-CSAs. Segregated elements tend to distribute around the whole faulted loop as a disk rather than only around the edge of the loop.

Composition and solubility of precipitated copper(II) arsenates

Energy Technology Data Exchange (ETDEWEB)

Nelson, Hanna; Shchukarev, Andrey; Sjoeberg, Staffan [Department of Chemistry, Umea University, SE-901 87 Umea (Sweden); Loevgren, Lars, E-mail: lars.lovgren@chem.umu.se [Department of Chemistry, Umea University, SE-901 87 Umea (Sweden)

2011-05-15

Research Highlights: > By mixing solutions of Cu{sup 2+} and HAsO{sub 4}{sup 2-} solid phases are formed in a wide pH range. > Five different stoichiometric compositions were found. > Two of the solid phases formed in 0.1 M NaCl contained Na{sup +}. > Stability constants for all solid phases have been determined. > Aqueous complexes containing Cu{sup 2+} and AsO{sub 4}{sup 3-} ions could not be detected. - Abstract: Equilibrium reactions involving Cu(II) and As(V) have been studied with respect to formation of complexes in aqueous solutions as well as formation of solid phases. Potentiometric titrations performed at 25 deg. C (I = 0.1 M Na(Cl)) and at different Cu to As ratios gave no evidence for the existence of Cu(II) arsenate complexes in solution below the pH of the precipitation boundaries (pH {approx} 4), irrespective of the Cu to As ratio and pH. Mixing of solutions of Cu(II) and As(V) at different proportions and adjusting pH to values ranging from 4 to 9 resulted in precipitation of five different solid phases. The elemental composition of the solids was determined using X-ray Photoelectron Spectroscopy, and Environmental Scanning Microscopy-Field Emission Gun equipped with an energy dispersive spectroscopy detector. The average Cu/As ratio was determined by dissolving the solids. Total soluble concentrations of the components Cu(II) and As(V), as well as the basicity of the solid phases were determined by analysis of aqueous solutions. Based upon these experimental data the stoichiometric composition of the solid phases and their stability were determined. The resulting equilibrium model includes the solid phases Cu{sub 3}(AsO{sub 4}){sub 2}, Cu{sub 3}(AsO{sub 4})(OH){sub 3}, Cu{sub 2}(AsO{sub 4})(OH), Cu{sub 5}Na(HAsO{sub 4})(AsO{sub 4}){sub 3} and Cu{sub 5}Na{sub 2}AsO{sub 4}){sub 4}, where Cu{sub 5}Na(HAsO{sub 4})(AsO{sub 4}){sub 3} and Cu{sub 5}Na{sub 2}(AsO{sub 4}){sub 4} have not been reported previously. In 0.1 M Na(Cl), Na{sup +} was found to be

Pyrolytic in situ magnetization of metal-organic framework MIL-100 for magnetic solid-phase extraction.

Science.gov (United States)

Huo, Shu-Hui; An, Hai-Yan; Yu, Jing; Mao, Xue-Feng; Zhang, Zhe; Bai, Lei; Huang, Yan-Feng; Zhou, Peng-Xin

2017-09-29

In this study, we report a facile, environmental friendly fabrication of a type of magnetic metal-organic framework (MOF) MIL-100 that can be used for magnetic solid-phase extraction (MSPE). The magnetic MOF composites were fabricated using in situ calcination method. The as-synthesized materials exhibited both high porosity and magnetic characteristics. They used for the MSPE of polycyclic aromatic hydrocarbons (PAHs) from water samples. Such MOF-based magnetic solid-phase extraction in combination with gas chromatography equipped with a flame ionization detector (GC-FID), exhibited wide linearity (0.02-250μgL -1 ), low detection limits (4.6-8.9ngL -1 ), and high enrichment factors (452-907) for PAHs. The relative standard deviations (RSDs) for intra- and inter-day extractions of PAHs were ranging from 1.7% to 9.8% and 3.8% to 9.2%, respectively. The recoveries for spiked PAHs (1μgL -1 ) in water samples were in the range of 88.5% to 106.6%. The results showed that the special anion-π orbital (electron donor-acceptor) interaction and π-π stacking between magnetic MIL-100 and PAHs play an important role in the adsorption of PAHs. Copyright © 2017. Published by Elsevier B.V.

Phase transition in Smsub(1-x)Gdsub(x)S and Smsub(1-x)Tmsub(x)S solid solutions under pressure

International Nuclear Information System (INIS)

Kaminskij, V.V.; Stepanov, N.N.; Romanova, M.V.

1985-01-01

Experiments are conducted on studying the effect of the n quantity on Psub(pt) (phase transition pressure) for SmS and systems of solid solutions Smsub(1-x)Gdsub(x)S and Smsub(1-x)Tmsub(x)S with conductivity electron concentrations approximately 10 19 -10 21 cm -3 corresponding to the semiconducting phase of these solutions. The investigated monocrystal samples have been prepared by the method of planar crystallization from the melt, have been chipped off over the cleavage planes [100], their characteristic sizes not exceeding 2 mm. Samples of the Smsub(1-x)Tmsub(x)S system were polycrystalline and they had characteristic dimensions of approximately 3mm. Concentration of conductivity electrons has been determined from measurements of the Hall constant. Hydrostatic compression of the samples has been exercised in a piston high-pressure chamber at T=300 K. The observed electric conductivity jump determined by the standard d.c. compensation technique was a criterion of the presence of the phase transition to the metal state. Dependences of Psub(pt) in SmS base solid solutions with approximately 10 19 -10 21 cm -3 concentration of conductivity electrons have similar tendency in behaviour: a certain increase in the phase transition pressure with n growth and then its drop at n approaching concentrations corresponding to compositions close to critical ones for the semiconductor-metal phase transition in any system of solid solutions. If the first mechanism prevails at small as then further on the second mechanism swelling by a power law with a high index plays the main role

Solid-phase synthesis of 3-amino-2-pyrazolines

DEFF Research Database (Denmark)

Nielsen, John

1998-01-01

The development of a solid-phase synthesis of 3-amino-2-pyrazolines is described. Conjugate addition of hydrazines to alpha,beta-unsaturated nitriles followed by cyclization yields 3-amino-2-pyrazolines. Acylation or sulfonation of the free amino-group yields a 24 member library of 3-amino-2...

Solid-Phase Extraction Combined with High Performance Liquid ...

African Journals Online (AJOL)

Methods: Solid-phase extraction method was employed for the extraction of the estrogen from milk and high performance liquid chromatography-diode array detector (HPLC-DAD) was used for the determination of estrogen. Results: Optimal chromatographic conditions were achieved on an Eclipse XDB-C18 column at a ...

Co-pyrolysis of coal with organic solids

Energy Technology Data Exchange (ETDEWEB)

Straka, P.; Buchtele, J. [Inst. of Rock Structure and Mechanics, Prague (Czechoslovakia)

1995-12-01

The co-pyrolysis of high volatile A bituminous coal with solid organic materials (proteins, cellulose, polyisoprene, polystyrene, polyethylene-glycolterephtalate-PEGT) at a high temperature conditions was investigated. Aim of the work was to evaluate, firstly, the changes of the texture and of the porous system of solid phase after high temperature treatment in presence of different types of macromolecular solids, secondly, properties and composition of the tar and gas. Considered organic solids are important waste components. During their co-pyrolysis the high volatile bituminous coal acts as a hydrogen donor in the temperature rank 220-480{degrees}C. In the rank 500- 1000{degrees}C the solid phase is formed. The co-pyrolysis was carried out at heating rate 3 K/min. It was found that an amount of organic solid (5-10%) affects important changes in the optical texture forms of solid phase, in the pore distribution and in the internal surface area. Transport large pores volume decreases in presence of PEGT, polystyrene and cellulose and increases in presence of proteins and polyisoprene. (image analysis measurements show that the tendency of coal to create coarse pores during co-pyrolysis is very strong and increases with increasing amount of organic solid in blend). An addition of considered materials changes the sorption ability (methylene blue test, iodine adsorption test), moreover, the reactivity of the solid phase.

Flow Strength of Shocked Aluminum in the Solid-Liquid Mixed Phase Region

Science.gov (United States)

Reinhart, William

2011-06-01

Shock waves have been used to determine material properties under high shock stresses and very-high loading rates. The determination of mechanical properties such as compressive strength under shock compression has proven to be difficult and estimates of strength have been limited to approximately 100 GPa or less in aluminum. The term ``strength'' has been used in different ways. For a Von-Mises solid, the yield strength is equal to twice the shear strength of the material and represents the maximum shear stress that can be supported before yield. Many of these concepts have been applied to materials that undergo high strain-rate dynamic deformation, as in uni-axial strain shock experiments. In shock experiments, it has been observed that the shear stress in the shocked state is not equal to the shear strength, as evidenced by elastic recompressions in reshock experiments. This has led to an assumption that there is a yield surface with maximum (loading)and minimum (unloading), shear strength yet the actual shear stress lies somewhere between these values. This work provides the first simultaneous measurements of unloading velocity and flow strength for transition of solid aluminum to the liquid phase. The investigation describes the flow strength observed in 1100 (pure), 6061-T6, and 2024 aluminum in the solid-liquid mixed phase region. Reloading and unloading techniques were utilized to provide independent data on the two unknowns (τc and τo) , so that the actual critical shear strength and the shear stress at the shock state could be estimated. Three different observations indicate a change in material response for stresses of 100 to 160 GPa; 1) release wave speed (reloading where applicable) measurements, 2) yield strength measurements, and 3) estimates of Poisson's ratio, all of which provide information on the melt process including internal consistency and/or non-equilibrium and rate-dependent melt behavior. The study investigates the strength properties

Fatty acids polymorphism and solid-state miscibility

Energy Technology Data Exchange (ETDEWEB)

Gbabode, Gabin [Centre de Physique Moleculaire Optique et Hertzienne, Universite Bordeaux I, 33405 Talence (France)], E-mail: ggbabode@ulb.ac.be; Negrier, Philippe; Mondieig, Denise [Centre de Physique Moleculaire Optique et Hertzienne, Universite Bordeaux I, 33405 Talence (France); Moreno, Evelyn; Calvet, Teresa; Cuevas-Diarte, Miquel Angel [Departament de Cristallografia, Mineralogia i Diposits Minerals, Universitat de Barcelona, 08028 Barcelona (Spain)

2009-02-05

The pentadecanoic acid-hexadecanoic acid (C{sub 15}H{sub 29}OOH-C{sub 16}H{sub 31}OOH) binary system is dealt with in this article. The polymorphism of 20 mixed materials has been investigated combining calorimetric measurements, isothermal and versus temperature X-ray powder diffraction and also FTIR spectroscopy. In particular, the cell parameters of the stable forms, temperatures and heats of phase changes for the two constituents and a proposal of phase diagram are given in this article. Three solid forms are created by mixing in addition with the four solid forms of the pure components. All these solid forms are stabilized on narrow domains of composition, implying a reduced solid-state miscibility of the pentadecanoic and hexadecanoic acids.

Solid polymer electrolyte composite membrane comprising a porous support and a solid polymer electrolyte including a dispersed reduced noble metal or noble metal oxide

Science.gov (United States)

Liu, Han; Mittelsteadt, Cortney K; Norman, Timothy J; Griffith, Arthur E; LaConti, Anthony B

2015-02-24

A solid polymer electrolyte composite membrane and method of manufacturing the same. According to one embodiment, the composite membrane comprises a thin, rigid, dimensionally-stable, non-electrically-conducting support, the support having a plurality of cylindrical, straight-through pores extending perpendicularly between opposing top and bottom surfaces of the support. The pores are unevenly distributed, with some or no pores located along the periphery and more pores located centrally. The pores are completely filled with a solid polymer electrolyte, the solid polymer electrolyte including a dispersed reduced noble metal or noble metal oxide. The solid polymer electrolyte may also be deposited over the top and/or bottom surfaces of the support.

Microwave-assisted solid-phase Ugi four-component condensations

DEFF Research Database (Denmark)

Nielsen, John

1999-01-01

An 18-member library was constructed from 2 isocyanides, 3 aldehydes and 3 carboxylic acids via microwave-assisted solid-phase Ugi reactions on TentaGel S RAM. Products of high purity were obtained in moderate to excellent yields after reaction times of 5 minutes or less (irradiation at 60W). (C...

Development of a solid-phase assay for measurement of proteolytic enzyme activity

International Nuclear Information System (INIS)

Varani, J.; Johnson, K.; Kaplan, J.

1980-01-01

A solid-phase, plate assay was developed for the measurement of proteolytic enzyme activity. In this assay procedure, radiolabeled substrates were dried onto the surface of microtiter wells. Following drying, the wells were washed two times with saline to remove the nonadherent substrate. When proteolytic enzymes were added to the wells, protein hydrolysis occurred, releasing radioactivity into the supernatant fluid. The amount of protein hydrolysis that occurred was reflected by the amount of radioactivity in the supernatant fluid. When 125 I-hemoglobin was used as the substrate, it was as susceptible to hydrolysis by trypsin in the solid-phase assay as it was in solution in a standard assay procedure. Protease activity from a variety of sources (including from viable cells as well as from extracellular sources) were also able to hydrolyze the hemoglobin on the plate. 125 I-Labeled serum albumen, fibrinogen, and rat pulmonary basement membrane were also susceptible to hydrolysis by trypsin in the solid phase. When [ 14 C]elastin was dried onto the plate, it behaved in a similar manner to elastin in solution. It was resistant to hydrolysis by nonspecific proteases such as trypsin and chymotrypsin but was highly susceptible to hydrolysis by elastase. The solid-phase plate assay has several features which recommended it for routine use. It is as sensitive as standard tube assays (and much more sensitive than routinely used colormetric assays). It is quick and convenient; there are no precipitation, centrifugation, or filtration steps. In addition, very small volumes of radioactive wastes are generated. Another advantage of the solid-phase plate assay is the resistance of the dried substrates to spontaneous breakdown and to microbial contamination. Finally, this assay is suitable for use with viable cells as well as for extracellular proteases

Method of non-interacting thermodynamic calculation of binary phase diagrams containing p disordered phases with variable composition and q phases with constant composition at (p, q) ≤ 10

International Nuclear Information System (INIS)

Udovskij, A.L.; Karpushkin, V.N.; Nikishina, E.A.

1991-01-01

Method of non-interacting thermodynamic calculation of state diagram of binary systems contacting p disordered phases with variable composition and q phases with constant composition for (p, q) ≤ 10 case is developed. Determination of all possible solutions of phase equilibrium equations is realized in the method. Certain application examples of computer-realized method of T-x thermodynamic calculation using PC for Cr-W, Ni-W, Ni-Al, Ni-Re binary systems are given

Assessment of all-solid-state lithium-ion batteries

Science.gov (United States)

Braun, P.; Uhlmann, C.; Weiss, M.; Weber, A.; Ivers-Tiffée, E.

2018-07-01

All-solid-state lithium-ion batteries (ASSBs) are considered as next generation energy storage systems. A model might be very useful, which describes all contributions to the internal cell resistance, enables an optimization of the cell design, and calculates the performance of an open choice of cell architectures. A newly developed one-dimensional model for ASSBs is presented, based on a design concept which employs the use of composite electrodes. The internal cell resistance is calculated by linking two-phase transmission line models representing the composite electrodes with an ohmic resistance representing the solid electrolyte (separator). Thereby, electrical parameters, i.e. ionic and electronic conductivity, electrochemical parameters, i.e. charge-transfer resistance at interfaces and lithium solid-state diffusion, and microstructure parameters, i.e. electrode thickness, particle size, interface area, phase composition and tortuosity, are considered as the most important material and design parameters. Subsequently, discharge curves are simulated, and energy- and power-density characteristics of all-solid-state cell architectures are calculated. These model calculations are discussed and compared with experimental data from literature for a high power LiCoO2-Li10GeP2S12/Li10GeP2S12/Li4Ti5O12-Li10GeP2S12 cell.

Salt Composition Derived from Veazey Composition by Thermodynamic Modeling and Predicted Composition of Drum Contents

Energy Technology Data Exchange (ETDEWEB)

Weisbrod, Kirk Ryan [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Veirs, Douglas Kirk [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Funk, David John [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Clark, David Lewis [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

2016-03-11

This report describes the derivation of the salt composition from the Veazey salt stream analysis. It also provides an estimate of the proportions of the kitty litter, nitrate salt and neutralizer that was contained in drum 68660. While the actinide content of waste streams was judiciously followed in the 1980s in TA-55, no record of the salt composition could be found. Consequently, a salt waste stream produced from 1992 to 1994 and reported by Gerry Veazey provided the basis for this study. While chemical analysis of the waste stream was highly variable, an average analysis provided input to the Stream Analyzer software to calculate a composition for a concentrated solid nitrate salt and liquid waste stream. The calculation predicted the gas / condensed phase compositions as well as solid salt / saturated liquid compositions. The derived composition provides an estimate of the nitrate feedstream to WIPP for which kinetic measurements can be made. The ratio of salt to Swheat in drum 68660 contents was estimated through an overall mass balance on the parent and sibling drums. The RTR video provided independent confirmation concerning the volume of the mixture. The solid salt layer contains the majority of the salt at a ratio with Swheat that potentially could become exothermic.

Salt Composition Derived from Veazey Composition by Thermodynamic Modeling and Predicted Composition of Drum Contents

International Nuclear Information System (INIS)

Weisbrod, Kirk Ryan; Veirs, Douglas Kirk; Funk, David John; Clark, David Lewis

2016-01-01

This report describes the derivation of the salt composition from the Veazey salt stream analysis. It also provides an estimate of the proportions of the kitty litter, nitrate salt and neutralizer that was contained in drum 68660. While the actinide content of waste streams was judiciously followed in the 1980s in TA-55, no record of the salt composition could be found. Consequently, a salt waste stream produced from 1992 to 1994 and reported by Gerry Veazey provided the basis for this study. While chemical analysis of the waste stream was highly variable, an average analysis provided input to the Stream Analyzer software to calculate a composition for a concentrated solid nitrate salt and liquid waste stream. The calculation predicted the gas / condensed phase compositions as well as solid salt / saturated liquid compositions. The derived composition provides an estimate of the nitrate feedstream to WIPP for which kinetic measurements can be made. The ratio of salt to Swheat in drum 68660 contents was estimated through an overall mass balance on the parent and sibling drums. The RTR video provided independent confirmation concerning the volume of the mixture. The solid salt layer contains the majority of the salt at a ratio with Swheat that potentially could become exothermic.

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

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

Aqueous Microwave-Assisted Solid-Phase Synthesis Using Boc-Amino Acid Nanoparticles

Directory of Open Access Journals (Sweden)

Yoshinobu Fukumori

2013-07-01

Full Text Available We have previously developed water-based microwave (MW-assisted peptide synthesis using Fmoc-amino acid nanopaticles. It is an organic solvent-free, environmentally friendly method for peptide synthesis. Here we describe water-based MW-assisted solid-phase synthesis using Boc-amino acid nanoparticles. The microwave irradiation allowed rapid solid-phase reaction of nanoparticle reactants on the resin in water. We also demonstrated the syntheses of Leu-enkephalin, Tyr-Gly-Gly-Phe-Leu-OH, and difficult sequence model peptide, Val-Ala-Val-Ala-Gly-OH, using our water-based MW-assisted protocol with Boc-amino acid nanoparticles.

Solid phase radioimmunoassay for HBe Ag and anti-HBe

Energy Technology Data Exchange (ETDEWEB)

Froesner, G G; Deinhardt, F [Muenchen Univ. (Germany, F.R.). Inst. fuer Hygiene und Medizinische Mikrobiologie; Sugg, U [Tuebingen Univ. (Germany, F.R.). Abt. fuer Transfusionswesen mit Blutbank; Haas, H [Staedtische Krankenanstalten Esslingen (Germany, F.R.). Zentrallabor; Overby, R L [Abbott Labs., North Chicago, IL (USA)

1978-04-01

A highly sensitive solid phase radioimmunoassay for the detection of hepatitis Be-antigen (HBeAg) and anti-HBe is described. Iodine-125 labelled anti-HBe is used as a tracer. The assay is about 500 foLd more sensitive than immunodiffusion.

Solid phase extraction-electrospray ionization mass spectrometric method for the determination of palladium

International Nuclear Information System (INIS)

Pranaw Kumar; Telmore, Vijay M.; Jaison, P.G.; Sarkar, Arnab; Alamelu, D.; Aggarwal, S.K.

2015-01-01

Platinum group of element (PGEs) are extensively used as a catalyst and anticancer reagent. Due to the soft nature of PGEs, sulphur based donar ligands are used for the separation of these elements. Studies on the formation of different species are helpful for obtaining the ideas about separation of these elements from the complex matrices. Palladium (Pd) is studied as a representative element which is also formed by nuclear fission of fissile nuclides. In view of the relatively small amount of solvent required for separation, solid phase extraction is preferred over most of the separation methods. Solid phase extraction method using DPX as a stationary phase was previously reported for the separation of Pd in SHLLW using benzoylthiourea as a ligand. However, in case of large volume samples manual extraction by DPX is tedious task. In the present studies, the feasibility of extraction using benzoylthiourea on automated solid phase extraction system was carried out for the extraction of Pd

One pot synthesis of magnetic graphene/carbon nanotube composites as magnetic dispersive solid-phase extraction adsorbent for rapid determination of oxytetracycline in sewage water.

Science.gov (United States)

Sun, Yunyun; Tian, Jing; Wang, Lu; Yan, Hongyuan; Qiao, Fengxia; Qiao, Xiaoqiang

2015-11-27

A simple and time-saving one pot synthesis of magnetic graphene/carbon nanotube composites (M-G/CNTs) was developed that could avoid the tedious drying process of graphite oxide, and G/CNTs were modified by Fe3O4 nanoparticles in the reduction procedure. It contributed to a shorten duration of the synthesis process of M-G/CNTs. The obtained M-G/CNTs were characterized and the results indicated that CNTs and Fe3O4 nanoparticles were served as spacer distributing to the layers of graphene, which was beneficial for enlarging surface area and improving extraction efficiency. Moreover, M-G/CNTs showed good magnetic property and outstanding thermal stability. Then M-G/CNTs were applied as adsorbent of magnetic dispersive solid-phase extraction for rapid extraction and determination of oxytetracycline in sewage water. Under the optimum conditions, good linearity was obtained in the range of 20-800ngmL(-1) and the recoveries were ranged from 95.5% to 112.5% with relative standard deviations less than 5.8%. Copyright © 2015 Elsevier B.V. All rights reserved.

Phase transition of solid bismuth under high pressure

International Nuclear Information System (INIS)

Chen Hai-Yan; Xiang Shi-Kai; Yan Xiao-Zhen; Zhang Yi; Liu Sheng-Gang; Bi Yan; Zheng Li-Rong

2016-01-01

As a widely used pressure calibrator, the structural phase transitions of bismuth from phase I, to phase II, to phase III, and then to phase V with increasing pressure at 300 K have been widely confirmed. However, there are different structural versions for phase III, most of which are determined by x-ray diffraction (XRD) technology. Using x-ray absorption fine structure (XAFS) measurements combined with ab initio calculations, we show that the proposed incommensurate composite structure of bismuth of the three configurations is the best option. An abnormal continuous increase of the nearest-neighbor distance of phase III with elevated pressure is also observed. The electronic structure transformation from semimetal to metal is responsible for the complex behavior of structure transformation. (paper)

Solid-solid phase transformation via internal stress-induced virtual melting, significantly below the melting temperature. Application to HMX energetic crystal.

Science.gov (United States)

Levitas, Valery I; Henson, Bryan F; Smilowitz, Laura B; Asay, Blaine W

2006-05-25

We theoretically predict a new phenomenon, namely, that a solid-solid phase transformation (PT) with a large transformation strain can occur via internal stress-induced virtual melting along the interface at temperatures significantly (more than 100 K) below the melting temperature. We show that the energy of elastic stresses, induced by transformation strain, increases the driving force for melting and reduces the melting temperature. Immediately after melting, stresses relax and the unstable melt solidifies. Fast solidification in a thin layer leads to nanoscale cracking which does not affect the thermodynamics or kinetics of the solid-solid transformation. Thus, virtual melting represents a new mechanism of solid-solid PT, stress relaxation, and loss of coherence at a moving solid-solid interface. It also removes the athermal interface friction and deletes the thermomechanical memory of preceding cycles of the direct-reverse transformation. It is also found that nonhydrostatic compressive internal stresses promote melting in contrast to hydrostatic pressure. Sixteen theoretical predictions are in qualitative and quantitative agreement with experiments conducted on the PTs in the energetic crystal HMX. In particular, (a) the energy of internal stresses is sufficient to reduce the melting temperature from 551 to 430 K for the delta phase during the beta --> delta PT and from 520 to 400 K for the beta phase during the delta --> beta PT; (b) predicted activation energies for direct and reverse PTs coincide with corresponding melting energies of the beta and delta phases and with the experimental values; (c) the temperature dependence of the rate constant is determined by the heat of fusion, for both direct and reverse PTs; results b and c are obtained both for overall kinetics and for interface propagation; (d) considerable nanocracking, homogeneously distributed in the transformed material, accompanies the PT, as predicted by theory; (e) the nanocracking does not

Progress in Dual (Piezoelectric-Magnetostrictive Phase Magnetoelectric Sintered Composites

Directory of Open Access Journals (Sweden)

Rashed Adnan Islam

2012-01-01

Full Text Available The primary aims of this review article are (a to develop the fundamental understanding of ME behavior in perovskite piezoelectric-spinel magnetostrictive composite systems, (b to identify the role of composition, microstructural variables, phase transformations, composite geometry, and postsintering heat treatment on ME coefficient, and (c to synthesize, characterize, and utilize the high ME coefficient composite. The desired range of ME coefficient in the sintered composite is 0.5–1 V/cm⋅Oe. The studies showed that the soft piezoelectric phase quantified by smaller elastic modulus, large grain size of piezoelectric phase (~1 μm, and layered structures yields higher magnitude of ME coefficient. It is also found that postsintering thermal treatment such as annealing and aging alters the magnitude of magnetization providing an increase in the magnitude of ME coefficient. A trilayer composite was synthesized using pressure-assisted sintering with soft phase [0.9 PZT–0.1 PZN] having grain size larger than 1 μm and soft ferromagnetic phase of composition Ni0.8Cu0.2Zn0.2Fe2O4 [NCZF]. The composite showed a high ME coefficient of 412 and 494 mV/cm⋅Oe after sintering and annealing, respectively. Optimized ferrite to PZT thickness ratio was found to be 5.33, providing ME coefficient of 525 mV/cm⋅Oe. The ME coefficient exhibited orientation dependence with respect to applied magnetic field. Multilayering the PZT layer increased the magnitude of ME coefficient to 782 mV/cm⋅Oe. Piezoelectric grain texturing and nanoparticulate assembly techniques were incorporated with the layered geometry. It was found that with moderate texturing, d33 and ME coefficient reached up to 325 pC/N and 878 mV/cm⋅Oe, respectively. Nanoparticulate core shell assembly shows the promise for achieving large ME coefficient in the sintered composites. A systematic relationship between composition, microstructure, geometry, and properties is

Solid-phase oligosaccharide and glycopeptide synthesis using glycosynthases

DEFF Research Database (Denmark)

Tolborg, Jakob Fjord; Petersen, Lars; Jensen, Knud Jørgen

2002-01-01

and the prospect of automatability. Here, we report the first application of glycosynthases to solid-phase oligosaccharide synthesis by use of the 51 kDa serine and glycine mutants of Agrobacterium sp. beta-glucosidase, Abg E358S and E358G. Acceptors were linked to PEGA resin through a backbone amide linker (BAL...

Effective Mechanical Property Estimation of Composite Solid Propellants Based on VCFEM

Directory of Open Access Journals (Sweden)

Liu-Lei Shen

2018-01-01

Full Text Available A solid rocket motor is one of the critical components of solid missiles, and its life and reliability mostly depend on the mechanical behavior of a composite solid propellant (CSP. Effective mechanical properties are critical material constants to analyze the structural integrity of propellant grain. They are estimated by a numerical method that combines the Voronoi cell finite element method (VCFEM and the homogenization method in the present paper. The correctness of this combined method has been validated by comparing with a standard finite element method and conventional theoretical models. The effective modulus and the effective Poisson’s ratio of a CSP varying with volume fraction and component material properties are estimated. The result indicates that the variations of the volume fraction of inclusions and the properties of the matrix have obvious influences on the effective mechanical properties of a CSP. The microscopic numerical analysis method proposed in this paper can also be used to provide references for the design and the analysis of other large volume fraction composite materials.

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

Solid-Phase Synthesis of Smac Peptidomimetics Incorporating Triazoloprolines and Biarylalanines

DEFF Research Database (Denmark)

Le Quement, Sebastian T.; Ishoey, Mette; Petersen, Mette T.

2011-01-01

by deactivating proteolytic caspases. The Smac protein has an antagonistic effect on IAPs, thus providing structural clues for the synthesis of new pro-apoptotic compounds. Herein, we report a solid-phase approach for the synthesis of Smac-derived tetrapeptide libraries. On the basis of a common (N......-Me)AVPF sequence, peptides incorporating triazoloprolines and biarylalanines were synthesized by means of Cu(I)-catalyzed azide–alkyne cycloaddition and Pd-catalyzed Suzuki cross-coupling reactions. Solid-phase procedures were optimized to high efficiency, thus accessing all products in excellent crude purities...... and yields (both typically above 90%). The peptides were subjected to biological evaluation in a live/dead cellular assay which revealed that structural decorations on the AVPF sequence indeed are highly important for cytotoxicity toward HeLa cells....

Multigrid Finite Element Method in Calculation of 3D Homogeneous and Composite Solids

Directory of Open Access Journals (Sweden)

A.D. Matveev

2016-12-01

Full Text Available In the present paper, a method of multigrid finite elements to calculate elastic three-dimensional homogeneous and composite solids under static loading has been suggested. The method has been developed based on the finite element method algorithms using homogeneous and composite three-dimensional multigrid finite elements (MFE. The procedures for construction of MFE of both rectangular parallelepiped and complex shapes have been shown. The advantages of MFE are that they take into account, following the rules of the microapproach, heterogeneous and microhomogeneous structures of the bodies, describe the three-dimensional stress-strain state (without any simplifying hypotheses in homogeneous and composite solids, as well as generate small dimensional discrete models and numerical solutions with a high accuracy.

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

NARCIS (Netherlands)

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

2001-01-01

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

Flexible poly(ethylene carbonate)/garnet composite solid electrolyte reinforced by poly(vinylidene fluoride-hexafluoropropylene) for lithium metal batteries

Science.gov (United States)

He, Zijian; Chen, Long; Zhang, Bochen; Liu, Yongchang; Fan, Li-Zhen

2018-07-01

Solid-state electrolytes with high ionic conductivities, great flexibility, and easy processability are needed for high-performance solid-state rechargeable lithium batteries. In this work, we synthesize nanosized cubic Li6.25Al0.25La3Zr2O12 (LLZO) by solution combustion method and develop a flexible garnet-based composite solid electrolyte composed of LLZO, poly(ethylene carbonate) (PEC), poly(vinylidene fluoride-hexafluoropropylene) (P(VdF-HFP) and lithium bis(fluorosulfonyl)imide (LiFSI)). In the flexible composite solid electrolytes, LLZO nanoparticles, as ceramic matrix, have a positive effect on ionic conductivities and lithium ion transference number (tLi+). PEC, as a fast ion-conducting polymer, possesses high tLi+ inherently. P(VdF-HFP), as a binder, can strengthen mechanical properties. Consequently, the as-prepared composite solid electrolyte demonstrates high tLi+ (0.82) and superb thermal stability (remaining LLZO matrix after burning). All-solid-state LiFePO4|Li cells assembled with the flexible composite solid electrolyte deliver a high initial discharge specific capacity of 121.4 mAh g-1 and good cycling stability at 55 °C.

A Variational Model for Two-Phase Immiscible Electroosmotic Flow at Solid Surfaces

KAUST Repository

Shao, Sihong

2012-01-01

We develop a continuum hydrodynamic model for two-phase immiscible flows that involve electroosmotic effect in an electrolyte and moving contact line at solid surfaces. The model is derived through a variational approach based on the Onsager principle of minimum energy dissipation. This approach was first presented in the derivation of a continuum hydrodynamic model for moving contact line in neutral two-phase immiscible flows (Qian, Wang, and Sheng, J. Fluid Mech. 564, 333-360 (2006)). Physically, the electroosmotic effect can be formulated by the Onsager principle as well in the linear response regime. Therefore, the same variational approach is applied here to the derivation of the continuum hydrodynamic model for charged two-phase immiscible flows where one fluid component is an electrolyte exhibiting electroosmotic effect on a charged surface. A phase field is employed to model the diffuse interface between two immiscible fluid components, one being the electrolyte and the other a nonconductive fluid, both allowed to slip at solid surfaces. Our model consists of the incompressible Navier-Stokes equation for momentum transport, the Nernst-Planck equation for ion transport, the Cahn-Hilliard phase-field equation for interface motion, and the Poisson equation for electric potential, along with all the necessary boundary conditions. In particular, all the dynamic boundary conditions at solid surfaces, including the generalized Navier boundary condition for slip, are derived together with the equations of motion in the bulk region. Numerical examples in two-dimensional space, which involve overlapped electric double layer fields, have been presented to demonstrate the validity and applicability of the model, and a few salient features of the two-phase immiscible electroosmotic flows at solid surface. The wall slip in the vicinity of moving contact line and the Smoluchowski slip in the electric double layer are both investigated. © 2012 Global-Science Press.

Finite element modeling for integrated solid-solid PCM-building material with varying phase change temperatures

Energy Technology Data Exchange (ETDEWEB)

Zhang, D.; Fung, A.S.; Siddiqui, O. [Ryerson Polytechnic Univ., Toronto, ON (Canada). Dept. of Mechanical and Industrial Engineering

2008-08-15

Solid-solid phase change materials (SSPCMs) are used to enhance thermal storage performance and reduce indoor temperature fluctuations in buildings. In this study, a finite element model (FEM) was used to investigate the thermal properties of different types of SSPCMs. An effective heat capacity method was used to develop the model. An integrated PCM-building material was analyzed in relation to temperature and heat flux profiles. Governing equations for the heat transfer process were composed of Navier-Stokes momentum equations; a mass conservation equation; and an energy conservation equation. Effective heat capacity was described as a linear function of the latent heat of fusion on both the heating and cooling processes. Data from the simulation were then compared with an experiment suing drywall, concrete and gypcrete samples. Heat flux across the surfaces and temperatures on the surfaces of the materials were measured. Data were used to validate the finite element model (FEM). Results of the study suggested that heat flux profiles are an effective means of understanding phase change processes. It was concluded that PCMs with lower phase change temperatures lengthened energy releases and improved thermal comfort in the building. 12 refs., 2 tabs., 14 figs.

New Solid Phases for Estimation of Hormones by Radioimmunoassay Technique

International Nuclear Information System (INIS)

Sheha, R.R.; Ayoub, H.S.M.; Shafik, M.

2013-01-01

The efforts in this study were initiated to develop and validate new solid phases for estimation of hormones by radioimmunoassay (RIA). The study argued the successful application of different hydroxy apatites (HAP) as new solid phases for estimation of Alpha fetoprotein (AFP), Thyroid Stimulating hormone (TSH) and Luteinizing hormone (LH) in human serum. Hydroxy apatites have different alkali earth elements were successfully prepared by a well-controlled co-precipitation method with stoichiometric ratio value 1.67. The synthesized barium and calcium hydroxy apatites were characterized using XRD and Ftir and data clarified the preparation of pure structures of both BaHAP and CaHAP with no evidence on presence of other additional phases. The prepared solid phases were applied in various radioimmunoassay systems for separation of bound and free antigens of AFP, TSH and LH hormones. The preparation of radiolabeled tracer for these antigens was carried out using chloramine-T as oxidizing agent. The influence of different parameters on the activation and coupling of the used apatite particles with the polyclonal antibodies was systematically investigated and the optimum conditions were determined. The assay was reproducible, specific and sensitive enough for regular estimation of the studied hormones. The intra-and inter-assay variation were satisfactory and also the recovery and dilution tests indicated an accurate calibration. The reliability of these apatite particles had been validated by comparing the results that obtained by using commercial kits. The results finally authenticates that hydroxyapatite particles would have a great potential to address the emerging challenge of accurate quantitation in laboratory medical application

A solid-phase-radioimmunoassay for total serum thyroxine

International Nuclear Information System (INIS)

Moedder, G.; Sokolowski, G.

1978-01-01

A new solid phase radioimmunoassay for total serum thyroxine was evaluated over a longer time under clinical routine conditions and compared with an established test system. The results show up that the T 4 values are precise, reliable and reproducible, the is incomplicate to handle and well suitable for semiautomatic pipetting systems. (orig.) 891 MG [de

Melting along the Hugoniot and solid phase transition for Sn via sound velocity measurements

Science.gov (United States)

Song, Ping; Cai, Ling-cang; Tao, Tian-jiong; Yuan, Shuai; Chen, Hong; Huang, Jin; Zhao, Xin-wen; Wang, Xue-jun

2016-11-01

It is very important to determine the phase boundaries for materials with complex crystalline phase structures to construct their corresponding multi-phase equation of state. By measuring the sound velocity of Sn with different porosities, different shock-induced melting pressures along the solid-liquid phase boundary could be obtained. The incipient shock-induced melting of porous Sn samples with two different porosities occurred at a pressure of about 49.1 GPa for a porosity of 1.01 and 45.6 GPa for a porosity of 1.02, based on measurements of the sound velocity. The incipient shock-induced melting pressure of solid Sn was revised to 58.1 GPa using supplemental measurements of the sound velocity. Trivially, pores in Sn decreased the shock-induced melting pressure. Based on the measured longitudinal sound velocity data, a refined solid phase transition and the Hugoniot temperature-pressure curve's trend are discussed. No bcc phase transition occurs along the Hugoniot for porous Sn; further investigation is required to understand the implications of this finding.

Determination of organophosphorus pesticides using molecularly imprinted polymer solid phase extraction

International Nuclear Information System (INIS)

Mohd Marsin Sanagi; Syairah Salleh; Wan Aini Wan Ibrahim

2011-01-01

Molecularly imprinted polymer solid phase extraction (MIP-SPE) method has been developed for the determination of organophosphorus pesticides (OPPs) in water samples. The MIP was prepared by thermo-polymerization method using methacrylic acid (MAA) as functional monomer, ethylene glycol dimethacrylate (EGDMA) as crosslinker, acetonitrile as porogenic solvent and quinalphos as the template molecule. The three OPPs (diazinon, quinalphos and chloropyrifos) were selected as target analytes as they are widely used in agriculture sector. Various parameters affecting the extraction efficiency of the imprinted polymers have been evaluated to optimize the selective preconcentration of OPPs from aqueous samples. The characteristics of the MIP-SPE method were validated by high performance liquid chromatography (HPLC). The accuracy and selectivity of the MIP-SPE process developed were verified using non-imprinted polymer solid phase extraction (NIP-SPE) and a commercial C 18 -SPE was used for comparison. The recoveries of the target analytes obtained using the MIPs as the solid phase sorbent ranged from 83% to 98% (RSDs 1.05 - 1.98 %; n=3) for water sample. The developed MIP-SPE method demonstrates that it could be applied for the determination of OPPs in water samples. (author)

Municipal solid waste composition: Sampling methodology, statistical analyses, and case study evaluation

International Nuclear Information System (INIS)

Edjabou, Maklawe Essonanawe; Jensen, Morten Bang; Götze, Ramona; Pivnenko, Kostyantyn; Petersen, Claus; Scheutz, Charlotte; Astrup, Thomas Fruergaard

2015-01-01

Highlights: • Tiered approach to waste sorting ensures flexibility and facilitates comparison of solid waste composition data. • Food and miscellaneous wastes are the main fractions contributing to the residual household waste. • Separation of food packaging from food leftovers during sorting is not critical for determination of the solid waste composition. - Abstract: Sound waste management and optimisation of resource recovery require reliable data on solid waste generation and composition. In the absence of standardised and commonly accepted waste characterisation methodologies, various approaches have been reported in literature. This limits both comparability and applicability of the results. In this study, a waste sampling and sorting methodology for efficient and statistically robust characterisation of solid waste was introduced. The methodology was applied to residual waste collected from 1442 households distributed among 10 individual sub-areas in three Danish municipalities (both single and multi-family house areas). In total 17 tonnes of waste were sorted into 10–50 waste fractions, organised according to a three-level (tiered approach) facilitating comparison of the waste data between individual sub-areas with different fractionation (waste from one municipality was sorted at “Level III”, e.g. detailed, while the two others were sorted only at “Level I”). The results showed that residual household waste mainly contained food waste (42 ± 5%, mass per wet basis) and miscellaneous combustibles (18 ± 3%, mass per wet basis). The residual household waste generation rate in the study areas was 3–4 kg per person per week. Statistical analyses revealed that the waste composition was independent of variations in the waste generation rate. Both, waste composition and waste generation rates were statistically similar for each of the three municipalities. While the waste generation rates were similar for each of the two housing types (single

Municipal solid waste composition: Sampling methodology, statistical analyses, and case study evaluation

Energy Technology Data Exchange (ETDEWEB)

Edjabou, Maklawe Essonanawe, E-mail: vine@env.dtu.dk [Department of Environmental Engineering, Technical University of Denmark, 2800 Kgs. Lyngby (Denmark); Jensen, Morten Bang; Götze, Ramona; Pivnenko, Kostyantyn [Department of Environmental Engineering, Technical University of Denmark, 2800 Kgs. Lyngby (Denmark); Petersen, Claus [Econet AS, Omøgade 8, 2.sal, 2100 Copenhagen (Denmark); Scheutz, Charlotte; Astrup, Thomas Fruergaard [Department of Environmental Engineering, Technical University of Denmark, 2800 Kgs. Lyngby (Denmark)

2015-02-15

Highlights: • Tiered approach to waste sorting ensures flexibility and facilitates comparison of solid waste composition data. • Food and miscellaneous wastes are the main fractions contributing to the residual household waste. • Separation of food packaging from food leftovers during sorting is not critical for determination of the solid waste composition. - Abstract: Sound waste management and optimisation of resource recovery require reliable data on solid waste generation and composition. In the absence of standardised and commonly accepted waste characterisation methodologies, various approaches have been reported in literature. This limits both comparability and applicability of the results. In this study, a waste sampling and sorting methodology for efficient and statistically robust characterisation of solid waste was introduced. The methodology was applied to residual waste collected from 1442 households distributed among 10 individual sub-areas in three Danish municipalities (both single and multi-family house areas). In total 17 tonnes of waste were sorted into 10–50 waste fractions, organised according to a three-level (tiered approach) facilitating comparison of the waste data between individual sub-areas with different fractionation (waste from one municipality was sorted at “Level III”, e.g. detailed, while the two others were sorted only at “Level I”). The results showed that residual household waste mainly contained food waste (42 ± 5%, mass per wet basis) and miscellaneous combustibles (18 ± 3%, mass per wet basis). The residual household waste generation rate in the study areas was 3–4 kg per person per week. Statistical analyses revealed that the waste composition was independent of variations in the waste generation rate. Both, waste composition and waste generation rates were statistically similar for each of the three municipalities. While the waste generation rates were similar for each of the two housing types (single

Solid phase extraction of copper(II) by fixed bed procedure on cation exchange complexing resins.

Science.gov (United States)

Pesavento, Maria; Sturini, Michela; D'Agostino, Girolamo; Biesuz, Raffaela

2010-02-19

The efficiency of the metal ion recovery by solid phase extraction (SPE) in complexing resins columns is predicted by a simple model based on two parameters reflecting the sorption equilibria and kinetics of the metal ion on the considered resin. The parameter related to the adsorption equilibria was evaluated by the Gibbs-Donnan model, and that related to the kinetics by assuming that the ion exchange is the adsorption rate determining step. The predicted parameters make it possible to evaluate the breakthrough volume of the considered metal ion, Cu(II), from different kinds of complexing resins, and at different conditions, such as acidity and ionic composition. Copyright 2009. Published by Elsevier B.V.

Effects of deep cryogenic treatment on the solid-state phase transformation of Cu-Al alloy in cooling process

Science.gov (United States)

Wang, Yuhui; Liao, Bo; Liu, Jianhua; Chen, Shuqing; Feng, Yu; Zhang, Yanyan; Zhang, Ruijun

2012-07-01

The solid-state phase transformation temperature and duration of deep cryogenic treated and untreated Cu-Al alloys in cooling process were measured by differential scanning calorimetry measurement. The solid-state phase transformation activation energy and Avrami exponent were calculated according to these measurements. The effects of deep cryogenic treatment on the solid-state phase transformation were investigated based on the measurement and calculation as well as the observation of alloy's microstructure. The results show that deep cryogenic treatment can increase the solid-phase transformation activation energy and shorten the phase transformation duration, which is helpful to the formation of fine grains in Cu-Al alloy.

Recent Application of Solid Phase Based Techniques for Extraction and Preconcentration of Cyanotoxins in Environmental Matrices.

Science.gov (United States)

Mashile, Geaneth Pertunia; Nomngongo, Philiswa N

2017-03-04

Cyanotoxins are toxic and are found in eutrophic, municipal, and residential water supplies. For this reason, their occurrence in drinking water systems has become a global concern. Therefore, monitoring, control, risk assessment, and prevention of these contaminants in the environmental bodies are important subjects associated with public health. Thus, rapid, sensitive, selective, simple, and accurate analytical methods for the identification and determination of cyanotoxins are required. In this paper, the sampling methodologies and applications of solid phase-based sample preparation methods for the determination of cyanotoxins in environmental matrices are reviewed. The sample preparation techniques mainly include solid phase micro-extraction (SPME), solid phase extraction (SPE), and solid phase adsorption toxin tracking technology (SPATT). In addition, advantages and disadvantages and future prospects of these methods have been discussed.

Solid phase microextraction speciation analysis of triclosan in aqueous mediacontaining sorbing nanoparticles

NARCIS (Netherlands)

Zielinska, K.

2014-01-01

Solid phase microextraction (SPME) is applied in the speciation analysis of the hydrophobic compound triclosan in an aqueous medium containing sorbing SiO2 nanoparticles (NPs). It is found that these NPs, as well as their complexes with triclosan, partition between the bulk medium and the solid

Solid-phase microextraction for the analysis of biological samples

NARCIS (Netherlands)

Theodoridis, G; Koster, EHM; de Jong, GJ

2000-01-01

Solid-phase microextraction (SPME) has been introduced for the extraction of organic compounds from environmental samples. This relatively new extraction technique has now also gained a lot of interest in a broad field of analysis including food, biological and pharmaceutical samples. SPME has a

Estrogenic and AhR activities in dissolved phase and suspended solids from wastewater treatment plants.

Science.gov (United States)

Dagnino, Sonia; Gomez, Elena; Picot, Bernadette; Cavaillès, Vincent; Casellas, Claude; Balaguer, Patrick; Fenet, Hélène

2010-05-15

The distribution of estrogen receptor (ERalpha) and Aryl Hydrocarbon Receptor (AhR) activities between the dissolved phase and suspended solids were investigated during wastewater treatment. Three wastewater treatment plants with different treatment technologies (waste stabilization ponds (WSPs), trickling filters (TFs) and activated sludge supplemented with a biofilter system (ASB)) were sampled. Estrogenic and AhR activities were detected in both phases in influents and effluents. Estrogenic and AhR activities in wastewater influents ranged from 41.8 to 79 ng/L E(2) Eq. and from 37.9 to 115.5 ng/L TCDD Eq. in the dissolved phase and from 5.5 to 88.6 ng/g E(2) Eq. and from 15 to 700 ng/g TCDD Eq. in the suspended solids. For both activities, WSP showed greater or similar removal efficiency than ASB and both were much more efficient than TF which had the lowest removal efficiency. Moreover, our data indicate that the efficiency of removal of ER and AhR activities from the suspended solid phase was mainly due to removal of suspended solids. Indeed, ER and AhR activities were detected in the effluent suspended solid phase indicating that suspended solids, which are usually not considered in these types of studies, contribute to environmental contamination by endocrine disrupting compounds and should therefore be routinely assessed for a better estimation of the ER and AhR activities released in the environment. Copyright 2010 Elsevier B.V. All rights reserved.

Determination of 8 Synthetic Food Dyes by Solid Phase Extraction ...

African Journals Online (AJOL)

Keywords: Synthetic colors, Food, Fruit flavored drinks, Solid phase extraction, RP-HPLC. Tropical Journal of ..... food dyes by thin-layer chromatography-fast atom bombardment ... food dyes in soft drinks containing natural pigments by.

Vapour-phase method in the synthesis of polymer-ibuprofen sodium-silica gel composites.

Science.gov (United States)

Kierys, Agnieszka; Krasucka, Patrycja; Grochowicz, Marta

2017-11-01

The study discusses the synthesis of polymer-silica composites comprising water soluble drug (ibuprofen sodium, IBS). The polymers selected for this study were poly(TRIM) and poly(HEMA- co -TRIM) produced in the form of permanently porous beads via the suspension-emulsion polymerization method. The acid and base set ternary composites were prepared by the saturation of the solid dispersions of drug (poly(TRIM)-IBS and/or poly(HEMA- co -TRIM)-IBS) with TEOS, and followed by their exposition to the vapour mixture of water and ammonia, or water and hydrochloric acid, at autogenous pressure. The conducted analyses reveal that the internal structure and total porosity of the resulting composites strongly depend on the catalyst which was used for silica precursor gelation. The parameters characterizing the porosity of both of the acid set composites are much lower than the parameters of the base set composites. Moreover, the basic catalyst supplied in the vapour phase does not affect the ibuprofen sodium molecules, whereas the acid one causes transformation of the ibuprofen sodium into the sodium chloride and a derivative of propanoic acid, which is poorly water soluble. The release profiles of ibuprofen sodium from composites demonstrate that there are differences in the rate and efficiency of drug desorption from them. They are mainly affected by the chemical character of the polymeric carrier but are also associated with the restricted swelling of the composites in the buffer solution after precipitation of silica gel.

Vapour-phase method in the synthesis of polymer-ibuprofen sodium-silica gel composites

Directory of Open Access Journals (Sweden)

Agnieszka Kierys

2017-11-01

Full Text Available The study discusses the synthesis of polymer-silica composites comprising water soluble drug (ibuprofen sodium, IBS. The polymers selected for this study were poly(TRIM and poly(HEMA-co-TRIM produced in the form of permanently porous beads via the suspension-emulsion polymerization method. The acid and base set ternary composites were prepared by the saturation of the solid dispersions of drug (poly(TRIM-IBS and/or poly(HEMA-co-TRIM-IBS with TEOS, and followed by their exposition to the vapour mixture of water and ammonia, or water and hydrochloric acid, at autogenous pressure. The conducted analyses reveal that the internal structure and total porosity of the resulting composites strongly depend on the catalyst which was used for silica precursor gelation. The parameters characterizing the porosity of both of the acid set composites are much lower than the parameters of the base set composites. Moreover, the basic catalyst supplied in the vapour phase does not affect the ibuprofen sodium molecules, whereas the acid one causes transformation of the ibuprofen sodium into the sodium chloride and a derivative of propanoic acid, which is poorly water soluble. The release profiles of ibuprofen sodium from composites demonstrate that there are differences in the rate and efficiency of drug desorption from them. They are mainly affected by the chemical character of the polymeric carrier but are also associated with the restricted swelling of the composites in the buffer solution after precipitation of silica gel.

Immobilization and functional reconstitution of antibody Fab fragment by solid-phase refolding.

Science.gov (United States)

Kumada, Yoichi; Hamasaki, Kyoto; Nakagawa, Aya; Sasaki, Eiju; Shirai, Tatsunori; Okumura, Masahiro; Inoue, Manami; Kishimoto, Michimasa

2013-12-31

In this study, we demonstrated the successful preparation of a Fab antibody-immobilized hydrophilic polystyrene (phi-PS) plate via one- and two-step solid-phase refolding methods. Both polystyrene-binding peptide (PS-tag)-fused Fd fragment of heavy chain (Fab H-PS) and full-length of light-chain (Fab L-PS) were individually produced in insoluble fractions of Escherichia coli cells, and they were highly purified in the presence of 8M of urea. Antigen-binding activities of Fab antibody immobilized were correctly recovered by the one-step solid-phase refolding method that a mixture of Fab H-PS and Fab L-PS was immobilized in the presence of 0.5-2M urea, followed by surface washing of the phi-PS plate with PBST. These results indicate that by genetic fusion of a PS-tag, a complex between Fab H and Fab L was efficiently immobilized on the surface of a phi-PS plate even in the presence of a low concentration of urea, and was then correctly refolded to retain its high antigen-binding activity via removal of the urea. A two-step solid-phase refolding method whereby Fab H-PS and Fab L-PS were successively refolded on the surface of a phi-PS plate also resulted in Fab antibody formation on the plate. Furthermore, both the binding affinity and the specificity of the Fab antibody produced by the two-step method were highly maintained, according to the results of sandwich ELISA and competitive ELISA using Fab antibody-immobilized plate via two-step solid-phase refolding. Thus, the solid-phase refolding method demonstrated in this study should be quite useful for the preparation of a Fab antibody-immobilized PS surface with high efficiency from individually produced Fab H-PS and Fab L-PS. This method will be applicable to the preparation of a large Fab antibody library on the surface of a PS plate for use in antibody screening. © 2013. Published by Elsevier B.V. All rights reserved.

Microstructure characterization of multi-phase composites and utilization of phase change materials and recycled rubbers in cementitious materials

Science.gov (United States)

Meshgin, Pania

2011-12-01

This research focuses on two important subjects: (1) Characterization of heterogeneous microstructure of multi-phase composites and the effect of microstructural features on effective properties of the material. (2) Utilizations of phase change materials and recycled rubber particles from waste tires to improve thermal properties of insulation materials used in building envelopes. Spatial pattern of multi-phase and multidimensional internal structures of most composite materials are highly random. Quantitative description of the spatial distribution should be developed based on proper statistical models, which characterize the morphological features. For a composite material with multi-phases, the volume fraction of the phases as well as the morphological parameters of the phases have very strong influences on the effective property of the composite. These morphological parameters depend on the microstructure of each phase. This study intends to include the effect of higher order morphological details of the microstructure in the composite models. The higher order statistics, called two-point correlation functions characterize various behaviors of the composite at any two points in a stochastic field. Specifically, correlation functions of mosaic patterns are used in the study for characterizing transport properties of composite materials. One of the most effective methods to improve energy efficiency of buildings is to enhance thermal properties of insulation materials. The idea of using phase change materials and recycled rubber particles such as scrap tires in insulation materials for building envelopes has been studied.

A development of multi-Species mass transport model considering thermodynamic phase equilibrium

DEFF Research Database (Denmark)

Hosokawa, Yoshifumi; Yamada, Kazuo; Johannesson, Björn

2008-01-01

) variation in solid-phase composition when using different types of cement, (ii) physicochemical evaluation of steel corrosion initiation behaviour by calculating the molar ratio of chloride ion to hydroxide ion [Cl]/[OH] in pore solution, (iii) complicated changes of solid-phase composition caused......In this paper, a multi-species mass transport model, which can predict time dependent variation of pore solution and solid-phase composition due to the mass transport into the hardened cement paste, has been developed. Since most of the multi-species models established previously, based...... on the Poisson-Nernst-Planck theory, did not involve the modeling of chemical process, it has been coupled to thermodynamic equilibrium model in this study. By the coupling of thermodynamic equilibrium model, the multi-species model could simulate many different behaviours in hardened cement paste such as: (i...

Double-antibody solid-phase radioimmunoassay: a simplified phase-separation procedure applied to various ligands

International Nuclear Information System (INIS)

Tevaarwerk, G.J.M.; Boyle, D.A.; Hurst, C.J.; Anguish, I.; Uksik, P.

1980-01-01

The purpose was to develop a simplified and reliable method of separating free from antibody-bound ligand using a precipitating antibody linked to a cellulose derivative. Dose-response curves and control sera were set up in parallel for various pituitary and placental polypeptides, steroid hormones, insulin, glucagon, triiodothyronine, thyroxine, angiotensin I, calcitonin, gastrin, cyclic AMP, and digoxin. After first-antibody reactions had reached equilibrium, free and bound ligand were separated using a double-antibody solid-phase system in parallel with conventional methods, including dextran-coated charcoal, double-antibody precipitation, single-antibody solid phase, organic solvents, salt precipitation, and anion-exchange resins. The effect of variations in temperature, incubation time, protein content, pH, and amount of separating material added were studied. The results showed that separation was complete within 1 hr for small ligand molecules and within 2 hr for larger ones. Dose-response curves and control-sera results closely paralleled those obtained with conventional methods. The method was not affected by moderate variations in incubation variables. Nonspecific binding was less than 3% in all assays, while intra-assay and interassay coefficients of variation were similar to those obtained with conventional phase-separation methods. It is concluded that the method is a simple and rapid alternative phase-separation system. It has the advantage of being free from common nonspecific intersample variations, and can be applied to any assay system based on rabbit or guinea pig antibodies without preliminay time- or reagent-consuming titration or adjustments to establish optimum phase-separating conditions

Sampling and analytical procedures for the determination of VOCs released into air from natural and anthropogenic sources: A comparison between SPME (Solid Phase Micro Extraction) and ST (Solid Trap) methods

International Nuclear Information System (INIS)

Tassi, F.; Capecchiacci, F.; Buccianti, A.; Vaselli, O.

2012-01-01

In the present study, two sampling and analytical methods for VOC determination in fumarolic exhalations related to hydrothermal-magmatic reservoirs in volcanic and geothermal areas and biogas released from waste landfills were compared: (a) Solid Traps (STs), consisting of three phase (Carboxen B, Carboxen C and Carbosieve S111) absorbent stainless steel tubes and (b) Solid Phase Micro Extraction (SPME) fibers, composed of DiVinylBenzene (DVB), Carboxen and PolyDimethylSiloxane. These techniques were applied to pre-concentrate VOCs discharged from: (i) low-to-high temperature fumaroles collected at Vulcano Island, Phlegrean Fields (Italy), and Nisyros Island (Greece), (ii) recovery wells in a solid waste disposal site located near Florence (Italy). A glass condensing system cooled with water was used to collect the dry fraction of the fumarolic gases, in order to allow more efficient VOC absorption avoiding any interference by water vapor and acidic gases, such as SO 2 , H 2 S, HF and HCl, typically present at relatively high concentrations in these fluids. Up to 37 organic species, in the range of 40–400 m/z, were determined by coupling gas chromatography to mass spectrometry (GC–MS). This study shows that the VOC compositions of fumaroles and biogas determined via SPME and ST are largely consistent and can be applied to the analysis of VOCs in gases released from different natural and anthropogenic environments. The SPME method is rapid and simple and more appropriate for volcanic and geothermal emissions, where VOCs are present at relatively high concentrations and prolonged gas sampling may be hazardous for the operator. The ST method, allowing the collection of large quantities of sample, is to be preferred to analyze the VOC composition of fluids from diffuse emissions and air, where these compounds are present at relatively low concentrations.

Modeling and Analysis of a Three-Phase Solid-State Var ...

African Journals Online (AJOL)

Modeling and Analysis of a Three-Phase Solid-State Var Compensator (SSVC) ... Nigerian Journal of Technology. Journal Home ... The problems associated with the flow of reactive power in transmission and distribution lines are well known.

Preparation of molybdenum borides by combustion synthesis involving solid-phase displacement reactions

International Nuclear Information System (INIS)

Yeh, C.L.; Hsu, W.S.

2008-01-01

Preparation of molybdenum borides of five different phases in the Mo-B binary system (including Mo 2 B, MoB, MoB 2 , Mo 2 B 5 , and MoB 4 ) was performed by self-propagating high-temperature synthesis (SHS) with two kinds of the reactant samples. When elemental powder compacts with an exact stoichiometry corresponding to the boride phase were employed, self-sustaining reaction was only achieved in the sample with Mo:B = 1:1 and nearly single-phase MoB was yielded. Therefore, the other four boride compounds were prepared from the reactant compacts composed of MoO 3 , Mo, and B powders, within which the displacement reaction of MoO 3 with boron was involved in combustion synthesis. Experimental evidence shows that the extent of displacement reaction in the overall reaction has a significant impact on sustainability of the synthesis reaction, combustion temperature, reaction front velocity, and composition of the end product. An increase in the solid-phase displacement reaction taking place during the SHS process contributes more heat flux to the synthesis reaction, thus resulting in the increase of combustion temperature and enhancement of the reaction front velocity. Based upon the XRD analysis, formation of Mo 2 B, MoB 2 , and Mo 2 B 5 as the dominant boride phase in the end product was successful through the SHS reaction with powder compacts under appropriate stoichiometries between MoO 3 , Mo, and B. However, a poor conversion was observed in the synthesis of MoB 4 . The powder compact prepared for the production of MoB 4 yielded mostly Mo 2 B 5

Role of Precursor-Conversion Chemistry in the Crystal-Phase Control of Catalytically Grown Colloidal Semiconductor Quantum Wires.

Science.gov (United States)

Wang, Fudong; Buhro, William E

2017-12-26

Crystal-phase control is one of the most challenging problems in nanowire growth. We demonstrate that, in the solution-phase catalyzed growth of colloidal cadmium telluride (CdTe) quantum wires (QWs), the crystal phase can be controlled by manipulating the reaction chemistry of the Cd precursors and tri-n-octylphosphine telluride (TOPTe) to favor the production of either a CdTe solute or Te, which consequently determines the composition and (liquid or solid) state of the Bi x Cd y Te z catalyst nanoparticles. Growth of single-phase (e.g., wurtzite) QWs is achieved only from solid catalysts (y ≪ z) that enable the solution-solid-solid growth of the QWs, whereas the liquid catalysts (y ≈ z) fulfill the solution-liquid-solid growth of the polytypic QWs. Factors that affect the precursor-conversion chemistry are systematically accounted for, which are correlated with a kinetic study of the composition and state of the catalyst nanoparticles to understand the mechanism. This work reveals the role of the precursor-reaction chemistry in the crystal-phase control of catalytically grown colloidal QWs, opening the possibility of growing phase-pure QWs of other compositions.

Radioimmuoassay study of antidigitoxin antibodies in liquid phase and after coupling on a solid phase

International Nuclear Information System (INIS)

Collignon, A.; German, A.; Scherrmann, J.M.; Bourdon, R.

1983-01-01

Antidigitoxin antibodies prepared by immunizing rabbits with a digitoxin-bovine serum albumin conjugate have been studied by radioimmunoassay in the native serum (homogeneous phase antibodies) and after coupling on glass beads (heterogeneous phase antibodies). Homogeneous phase antibodies present a satisfactory titer and affinity constant and react very specifically with digitoxin. Fixation of antibodies on a solid phase induce a loss of their immunoreactivity as it is showed by modification of the inhibition curves, by a greater sensitivity to the chemical structure of the tracer and by a decrease of the affinity constant. Reactionnal kinetic and sensitivity to the incubation temperature are not modified. Heterogeneous phase antibodies present a greater stability. Both antibodies types can be used for a digitoxin radioimmunoassay [fr

Studies on composite solid propellant with tri-modal ammonium perchlorate containing an ultrafine fraction

Directory of Open Access Journals (Sweden)

K.V. Suresh Babu

2017-08-01

Full Text Available Composite solid propellant is prepared using tri-modal Ammonium perchlorate (AP containing coarse, fine and ultrafine fractions of AP with average particle size (APS 340, 40 and 5 μm respectively, in various compositions and their rheological, mechanical and burn rate characteristics are evaluated. The optimum combination of AP coarse to fine to ultrafine weight fraction was obtained by testing of series of propellant samples by varying the AP fractions at fixed solid loading. The concentration of aluminium was maintained constant throughout the experiments for ballistics requirement. The propellant formulation prepared using AP with coarse to fine to ultrafine ratio of 67:24:9 has lowest viscosity for the propellant paste and highest tensile strength due to dense packing as supported by the literature. A minimum modulus value was also observed at 9 wt. % of ultrafine AP concentration indicates the maximum solids packing density at this ratio of AP fractions. The burn rate is evaluated at different pressures to obtain pressure exponent. Incorporation of ultrafine fraction of AP in propellant increased burn rate without adversely affecting the pressure exponent. Higher solid loading propellants are prepared by increased AP concentration from 67 to 71 wt. % using AP with coarse to fine to ultrafine ratio of 67:24:9. Higher solid content up to 89 wt. % was achieved and hence increased solid motor performance. The unloading viscosity showed a trend with increased AP content and the propellant couldn't able to cast beyond 71 wt. % of AP. Mechanical properties were also studied and from the experiments noticed that % elongation decreased with increased AP content from 67 to 71 wt.%, whereas tensile strength and modulus increased. Burn rate increased with increased AP content and observed that pressure exponent also increased and it is high for the propellant containing with 71 wt.% of AP due to increased oxidiser to fuel ratio. Catalysed

Phase characteristics of solid-state amplifiers in sub-harmonic bunchers

International Nuclear Information System (INIS)

Liu Rong; Ma Xinpeng; Zhao Fengli; Wang Xiangjian; Wang Guangwei; Huang Yongqing; Zhang Donghui

2009-01-01

To study the phase characteristics of solid-state amplifiers(20 kW/142.8 MHz,10 kW/571.2 MHz) in sub-harmonic bunchers(SHBs) of the BEPC II linear accelerator, phase shift in pulse and phase stability are measured using a digital measurement method based on field programmable gate array(FPGA). The hardware of the measurement system includes the frequency synthesizer, digital signal processing board(FPGA) and PC, and the software includes an internal algorithm on FPGA, communication procedures and PC client interface procedures. The measurement results of phase characteristics are consistent with the actual situation, which is the basis for the further implement of phase compensation in SHBs. (authors)

Development of hydrazinium nitroformate based solid propellants

NARCIS (Netherlands)

Schöyer, H.F.R.; Schnorhk, A.J.; Korting, P.A.O.G.; Lit, P.J. van; Mul, J.M.; Gadiot, G.; Meulenbrugge, J.J.

1995-01-01

The development of new high-performance propellant combinations requires the establishment of safety and handling characteristics and thermodynamic decomposition and explosive properties. This paper addresses the early development phases of a new composite solid propellant based on HNF as oxidizer

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

DEFF Research Database (Denmark)

Hansen, Martin; Poulsen, Rikke; Luong, Xuan

2014-01-01

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

Solid phase extraction and metabolic profiling of exudates from living copepods

DEFF Research Database (Denmark)

Selander, Erik; Heuschele, Jan; Nylund, Göran M.

2016-01-01

describe the development of a closed loop solid phase extraction setup that allows for extraction of exuded metabolites from live copepods. We captured exudates from male and female Temora longicornis and analyzed the content with high resolution LC-MS. Chemometric methods revealed 87 compounds...... that solid phase extraction in combination with metabolic profiling of exudates is a useful tool to develop our understanding of the chemical interplay between pelagic organisms....... Copepodamide G, known to induce defensive responses in phytoplankton, was among the ten compounds of highest relative abundance in both male and female extracts. The presence of copepodamide G shows that the method can be used to capture and analyze chemical signals from living source organisms. We conclude...

Comparison of solid and liquid-phase bioassays using ecoscores to assess contaminated soils

Energy Technology Data Exchange (ETDEWEB)

Lors, Christine [Universite Lille Nord de France, 1bis rue Georges Lefevre, 59044 Lille Cedex (France); Ecole des Mines de Douai, LGCgE-MPE-GCE, 941 rue Charles-Bourseul, 59500 Douai (France); Centre National de Recherche sur les Sites et Sols Pollues, 930 Boulevard Lahure, BP 537, 59505 Douai Cedex (France); Ponge, Jean-Francois, E-mail: ponge@mnhn.fr [Museum National d' Histoire Naturelle, Departement Ecologie et Gestion de la Biodiversite, CNRS UMR 7179, 4 Avenue du Petit-Chateau, 91800 Brunoy (France); Martinez Aldaya, Maite [Museum National d' Histoire Naturelle, Departement Ecologie et Gestion de la Biodiversite, CNRS UMR 7179, 4 Avenue du Petit-Chateau, 91800 Brunoy (France); Damidot, Denis [Universite Lille Nord de France, 1bis rue Georges Lefevre, 59044 Lille Cedex (France); Ecole des Mines de Douai, LGCgE-MPE-GCE, 941 rue Charles-Bourseul, 59500 Douai (France)

2011-10-15

Bioassays on aqueous and solid phases of contaminated soils were compared, belonging to a wide array of trophic and response levels and using ecoscores for evaluating ecotoxicological and genotoxicological endpoints. The method was applied to four coke factory soils contaminated mainly with PAHs, but also to a lesser extent by heavy metals and cyanides. Aquatic bioassays do not differ from terrestrial bioassays when scaling soils according to toxicity but they are complementary from the viewpoint of ecological relevance. Both aquatic and terrestrial endpoints are strongly correlated with concentrations of 3-ring PAHs. This evaluation procedure allows us to propose a cost-effective battery which embraces a wide array of test organisms and response levels: it includes two rapid bioassays (Microtox) and springtail avoidance), a micronucleus test and three bioassays of a longer duration (algal growth, lettuce germination and springtail reproduction). This battery can be recommended for a cost-effective assessment of polluted/remediated soils. - Highlights: > Comparison of liquid- and solid-phase bioassays on contaminated soils, using ecoscores. > Complementarity of liquid- and solid-phase bioassays for the evaluation of environmental hazards. > Proposal for a restricted battery of 5 most sensitive tests. > Use of this restricted battery for a cost-effective assessment of polluted/remediated soils. - Aqueous and solid phases of contaminated soils give similar results in terms of toxicity but are complementary for the evaluation of environmental hazards by ecoscores.

A study of the oxidation of nickel-titanium intermetallics. II. Phase composition of the scale

Energy Technology Data Exchange (ETDEWEB)

Chuprina, V G [Institut Problem Materialovedeniia, Kiev (Ukrainian SSR)

1989-06-01

The phase composition of the scale formed on NiTi during oxidation in air in the temperature range 600-1000 C was investigated by X-ray diffraction and layer-by-layer metallographic analyses. The scale was found to contain NiO, NiO.TiO2, TiO2, Ti2O3, Ti3O5, Ni, and Ni(Ti) solid solution; an Ni3Ti sublayer was present at the scale-alloy boundary. Oxygen diffusion in the scale toward the sublayer and counterdiffusion of Ni(+2) were found to be the principal processes responsible for NiTi oxidation. 8 refs.

Phase and Microstructural Correlation of Spark Plasma Sintered HfB2-ZrB2 Based Ultra-High Temperature Ceramic Composites

Directory of Open Access Journals (Sweden)

Ambreen Nisar

2017-07-01

Full Text Available The refractory diborides (HfB2 and ZrB2 are considered as promising ultra-high temperature ceramic (UHTCs where low damage tolerance limits their application for the thermal protection system in re-entry vehicles. In this regard, SiC and CNT have been synergistically added as the sintering aids and toughening agents in the spark plasma sintered (SPS HfB2-ZrB2 system. Herein, a novel equimolar composition of HfB2 and ZrB2 has shown to form a solid-solution which then allows compositional tailoring of mechanical properties (such as hardness, elastic modulus, and fracture toughness. The hardness of the processed composite is higher than the individual phase hardness up to 1.5 times, insinuating the synergy of SiC and CNT reinforcement in HfB2-ZrB2 composites. The enhanced fracture toughness of CNT reinforced composite (up to a 196% increment surpassing that of the parent materials (ZrB2/HfB2-SiC is attributed to the synergy of solid solution formation and enhanced densification (~99.5%. In addition, the reduction in the analytically quantified interfacial residual tensile stress with SiC and CNT reinforcements contribute to the enhancement in the fracture toughness of HfB2-ZrB2-SiC-CNT composites, mandatory for aerospace applications.

Tethered Nanoparticle–Polymer Composites: Phase Stability and Curvature

KAUST Repository

Srivastava, Samanvaya; Agarwal, Praveen; Archer, Lynden A.

2012-01-01

different small-angle X-ray scattering signatures in comparison to phase-separated composites comprised of bare or sparsely grafted nanoparticles. A general diagram for the dispersion state and phase stability of polymer tethered nanoparticle-polymer

Effects of calcination temperature on phase formation and particle size of Zn{sub 2}Nb{sub 34}O{sub 87} powder synthesized by solid-state reaction

Energy Technology Data Exchange (ETDEWEB)

Amonpattaratkit, Penphitcha, E-mail: p.amonpattaratkit@gmail.com [Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Ananta, Supon, E-mail: suponananta@yahoo.com [Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand)

2013-05-15

The solid-state mixed oxide method via a rapid vibro-milling technique was explored for the preparation of single-phase Zn{sub 2}Nb{sub 34}O{sub 87} nanopowders. Phase formation of zinc niobate was investigated as a function of calcination temperature by using a combination of thermogravimetric/differential thermal analyzer (TG/DTA) and X-ray diffraction (XRD) techniques. Morphology, particle size and chemical composition of the powders were determined by scanning electron microscopy (SEM) and energy-dispersive X-ray (EDX) technique. The obtained results clearly revealed the influences of calcination temperature on phase formation and particle size of Zn{sub 2}Nb{sub 34}O{sub 87} nanopowder. - Highlights: ► Single phase Zn{sub 2}Nb{sub 34}O{sub 87} was firstly prepared by solid-state mixed oxide method via a rapid vibro-milling technique. ► The influences of calcination temperature on phase formation and particle size were investigated. ► Zn{sub 2}Nb{sub 34}O{sub 87} powders were characterized by TG–DTA, XRD, SEM and EDX.

Composition-microstructure-property relationships in dual phase bulk magnetoelectric composite

Science.gov (United States)

Islam, Rashed Adnan

The coexistence of coupled electrical and magnetic properties in the "magnetoelectric" material has led to the possibility of developing smarter and smaller electronic components. In order to make this possibility a reality, significant efforts are required to understand the science of magnetoelectric (ME) behavior and apply this understanding to develop higher sensitivity material. The primary aims of this thesis are to identify the role of composition, microstructural variables, composite geometry, texturing, post sintering heat treatment, and nanoscale assembly on ME coefficient. The overall objective is to synthesize, characterize and utilize a high ME coefficient composite. The desired range of ME coefficient in the sintered composite is more than 1.5 V/cm.Oe. At first, a piezoelectric composition in the system of Pb(Zr,Ti)O 3 - Pb[(Zn,Ni)1/3Nb2/3]O3 was designed and synthesized which has high energy density (d.g) parameter of 18456.2 x 10-15m2/N and high g constant of 83.1 V-m/N in order to use it as the matrix in piezoelectric---magnetostrictive composite. Secondly it was found that soft piezoelectric phase shows much better magnetoelectric response. The magnetoelectric coefficient for Pb(Zr 0.52Ti0.48)O3 - 15% Pb(Zn1/3Nb 2/3)O3 [PZT - 15 PZN] - 20% Ni0.8Zn 0.2Fe2O4 was found to be around 186 mV/cm.Oe. Thridly, soft magnetic phase with lower coercivity and higher magnetization was found to be suitable for high ME coefficient. Zinc doped Ni-ferrite has higher resistivity, permeability, magnetization and it was found that with increasing Zn concentration the ME coefficient increases exhibiting maxima near 30 at% Zn (138 mV/cm.Oe). Fourthly, if the connectivity was changed from (0-3) to (2-2) which is a bilayer geometry, improved piezoelectric (d33 ˜ 80 pC/N), ferroelectric (polarization = 60 muC/cm2), magnetization (25 emu/gm) and lower coercive field (2.8 Oe) were measured. The bilayer shows an enhancement of 67% increase in ME coefficient compared to bulk

A Photolabile Linker for the Solid-Phase Synthesis of Peptide Hydrazides and Heterocycles

DEFF Research Database (Denmark)

Qvortrup, Katrine; Komnatnyy, Vitaly V.; Nielsen, Thomas Eiland

2014-01-01

A photolabile hydrazine linker for the solid-phase synthesis of peptide hydrazides and hydrazine-derived heterocycles is presented. The developed protocols enable the efficient synthesis of structurally diverse peptide hydrazides derived from the standard amino adds, including those with side......-chain protected residues at the C-terminal of the resulting peptide hydrazide, and are useful for the synthesis of dihydropyrano[2,3-c]pyrazoles. The linker is compatible with most commonly used coupling reagents and protecting groups for solid-phase peptide synthesis....

Poly(ethylene glycol)/carbon quantum dot composite solid films exhibiting intense and tunable blue–red emission

International Nuclear Information System (INIS)

Hao, Yanling; Gan, Zhixing; Xu, Jiaqing; Wu, Xinglong; Chu, Paul K.

2014-01-01

Highlights: • Poly(ethylene glycol)/carbon quantum dots (PEG/CQDs) composite solid films exhibiting strong and tunable blue–red emission were prepared. Successful preparation of tunable emitting CQDs solid films can extend the application of carbon quantum dots in photoelectric devices. • The mechanism of the tunable emission from the PEG/CQDs composite solid films was discussed. • On the basis of the characteristics of the PL from solid films in this work, the complex PL origins of CQDs were further defined. The PL mechanism provides insights into the fluorescence mechanism of CQDs and may promotes their applications. • Poly(ethylene glycol); carbon quantum dots; Strong and tunable blue-red emission; The fluorescent quantum yield of 12.6%. - Abstract: Although carbon quantum dots (CQDs) possess excellent luminescence properties, it is a challenge to apply water-soluble CQDs to tunable luminescent devices. Herein, quaternary CQDs are incorporated into poly(ethylene glycol) to produce poly(ethylene glycol)/CQD composite solid films which exhibit strong and tunable blue–red emission. The fluorescent quantum yield reaches 12.6% which is comparable to that of many liquid CQDs and the photoluminescence characteristics are determined to elucidate the fluorescence mechanism. The CQD solid films with tunable optical properties bode well for photoelectric devices especially displays

Influence of process parameters to composite interface organization and performance of liquid/solid bimetal

International Nuclear Information System (INIS)

Rong, S F; Zhu, Y C; Wu, Y H; Yang, P H; Duan, X L; Zhou, H T

2015-01-01

The liquid-solid composite technique was used to prepare the high carbon high chromium steel (HCHCS) and low alloy steel (LCS) bimetal composite materials by means of insert casting method. The influence of some process parameters such as liquid-solid ratio, preheat temperature, pouring temperature on the interface microstructure and mechanical properties were studied. Interface microstructure and element distribution were analyzed. The results show that the interface microstructure becomes better, and bonding area becomes thicker with the increase of the volume of liquid to solid ratio, preheating temperature and pouring temperature. When the liquid-solid ratio is 8:1, the preheating temperature is 300 °C and the pouring temperature is 1565 °C, a good metallurgical bonding area without any hole can be obtained with the interface combination of diffusion and fusion. The composite interface structure was composed of a core material diffusion layer, a cooling solidification layer, a direction growth layer and some cell particles. The elements of C, Cr and Mn diffuse from the HCHCS side to the alloy steel side. The microhardness increased in the gradient from the LCS side to the HCHCS. The microhardness of the interface is significantly higher than that of LCS. (paper)

Solid phase crystallisation of HfO2 thin films

International Nuclear Information System (INIS)

Modreanu, M.; Sancho-Parramon, J.; O'Connell, D.; Justice, J.; Durand, O.; Servet, B.

2005-01-01

In this paper, we report on the solid phase crystallisation of carbon-free HfO 2 thin films deposited by plasma ion assisted deposition (PIAD). After deposition, the HfO 2 films were annealed in N 2 ambient for 3 h at 350, 550 and 750 deg. C. Several characterisation techniques including X-ray reflectometry (XRR), X-ray diffraction (XRD), spectroscopic ellipsometry (SE) and atomic force microscopy (AFM) were used for the physical characterisation of as-deposited and annealed HfO 2 . XRD has revealed that the as-deposited HfO 2 film is in an amorphous-like state with only traces of crystalline phase and that the annealed films are in a highly crystalline state. These results are in good agreement with the SE results showing an increase of refractive index by increasing the annealing temperature. XRR results show a significant density gradient over the as-deposited film thickness, which is characteristic of the PIAD method. The AFM measurements show that the HfO 2 layers have a smooth surface even after annealing at 750 deg. C. The present study demonstrates that the solid phase crystallisation of HfO 2 PIAD thin films starts at a temperature as low as 550 deg. C

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

Science.gov (United States)

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

2013-08-01

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

The constitutive distributed parameter model of multicomponent chemical processes in gas, fluid and solid phase

International Nuclear Information System (INIS)

Niemiec, W.

1985-01-01

In the literature of distributed parameter modelling of real processes is not considered the class of multicomponent chemical processes in gas, fluid and solid phase. The aim of paper is constitutive distributed parameter physicochemical model, constructed on kinetics and phenomenal analysis of multicomponent chemical processes in gas, fluid and solid phase. The mass, energy and momentum aspects of these multicomponent chemical reactions and adequate phenomena are utilized in balance operations, by conditions of: constitutive invariance for continuous media with space and time memories, reciprocity principle for isotropic and anisotropic nonhomogeneous media with space and time memories, application of definitions of following derivative and equation of continuity, to the construction of systems of partial differential constitutive state equations, in the following derivative forms for gas, fluid and solid phase. Couched in this way all physicochemical conditions of multicomponent chemical processes in gas, fluid and solid phase are new form of constitutive distributed parameter model for automatics and its systems of equations are new form of systems of partial differential constitutive state equations in sense of phenomenal distributed parameter control

Multifilamentary superconducting (NbTa)-Sn composite wire by solid-liquid reaction for possible application above 20 tesla

International Nuclear Information System (INIS)

Hong, M.; Hull, G.W. Jr.; Fuchs, E.O.; Holthuis, J.T.

1983-01-01

Nb alloyed with Ta was employed in fabricating multifilamentary composite wires of (NbTa)-Sn using the liquid-infiltration process. The superconducting A15 phase was formed with subsequent heat treatments at 800-950 0 C by the solid-liquid reaction. High inductive Tsub(c)'s of 18.2 K with sharp transition width ( 4 A/cm 2 at 2O T and 4.2 K were obtained. It was found that 2 wt.% Ta in the Nb was sufficient in the enhancement of the overall Jsub(c) at the high fields and in increasing the Hsub(c2) (4.2 K) to 25 T. (Auth.)

Multifilamentary superconducting (NbTa)-Sn composite wire by solid-liquid reaction for possible application above 20 tesla

International Nuclear Information System (INIS)

Hong, M.; Hull, G.W. Jr.; Fuchs, E.O.; Holthuis, J.T.

1983-01-01

Nb alloyed with Ta was employed in fabricating multifilamentary composite wires of (NbTa)-Sn using the liquid-infiltration process. The superconducting A15 phase was formed with subsequent heat treatments at 800-950 0 C by the solid-liquid reaction. High inductive Tsub(c)'s of 18.2 K with sharp transition width ( 4 A/cm 2 at 20 T and 4.2 K were obtained. It was found that 2 wt.% Ta in the Nb was sufficient in the enhancement of the overall Jsub(c) at the high fields and in increasing the Hsub(c2) (4.2 K) to 25 T. (orig.)

Prediction of transport phenomena in near and far field: interaction solid phase/fluid phase

International Nuclear Information System (INIS)

Mingarro, E.

1995-01-01

The prediction of transport phenomena in near and far field is presented in the present report. The study begins with the analysis of solid phases stability: solubility of storage waste: UO 2 and solubility of radionuclides the redox and sorption-desorption conditions are the last aspects studied to predict the transport phenomena

Application of mercapto-silica polymerized high internal phase emulsions for the solid-phase extraction and preconcentration of trace lead(II).

Science.gov (United States)

Su, Rihui; Ruan, Guihua; Chen, Zhengyi; Du, Fuyou; Li, Jianping

2015-12-01

A new class of solid-phase extraction column prepared with grafted mercapto-silica polymerized high internal phase emulsion particles was used for the preconcentration of trace lead. First, mercapto-silica polymerized high internal phase emulsion particles were synthesized by using high internal phase emulsion polymerization and carefully assembled in a polyethylene syringe column. The influences of various parameters including adsorption pH value, adsorption and desorption solvents, flow rate of the adsorption and desorption procedure were optimized, respectively, and the suitable uploading sample volumes, adsorption capacity, and reusability of solid phase extraction column were also investigated. Under the optimum conditions, Pb(2+) could be preconcentrated quantitatively over a wide pH range (2.0-5.0). In the presence of foreign ions, such as Na(+) , K(+) , Ca(2+) , Zn(2+) , Mg(2+) , Cu(2+) , Fe(2+) , Cd(2+) , Cl(-) and NO3 (-) , Pb(2+) could be recovered successfully. The prepared solid-phase extraction column performed with high stability and desirable durability, which allowed more than 100 replicate extractions without measurable changes of performance. The feasibility of the developed method was further validated by the extraction of Pb(2+) in rice samples. At three spiked levels of 40.0, 200 and 800 μg/kg, the average recoveries for Pb(2+) in rice samples ranged from 87.3 to 105.2%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Literature survey on phase composition of hardened cement paste containing fly ash

International Nuclear Information System (INIS)

Otsuka, Taku; Yamamoto, Takeshi

2015-01-01

The purpose of this literature survey is to collect the knowledge on the effect of fly ash in hardened cement paste and the information about evaluation of physicochemical performance based on phase composition of hardened cement paste. The performance of hardened cement paste containing fly ash is affected by the property of fly ash, hydration of cement and pozzolanic reaction of fly ash. Some properties of fly ash such as density and chemical composition are reflected in phase composition, showing the progress of cement hydration and pozzolanic reaction. Therefore clarification of the relationship of phase composition and performance will lead to appropriate evaluation of the property of fly ash. The amount of pore, chemical shrinkage, pore solution, compressive strength, Young modulus and alkali silica reaction have relations to the phase composition of hardened cement paste. It is considered as future subject to clarify the relationship of phase composition and performance for various properties of fly ash. (author)

A photolabile linker for the solid-phase synthesis of 4-substituted NH-1,2,3-triazoles

DEFF Research Database (Denmark)

Qvortrup, Katrine; Nielsen, Thomas Eiland

2011-01-01

A novel photolabile linker for solid-phase synthesis is presented. The linker displays an azido handle for copper-catalyzed azide–alkyne cycloaddition reactions with a variety of alkynes, remains intact under typical solid-phase reaction conditions, and enables a mild photolytic release of 4...

Copper welding in solid phase; Svarka medi v tverdoj faze

Energy Technology Data Exchange (ETDEWEB)

Avagyan, V Sh

1993-12-31

An analysis of the publications on the technology of diffusion welding of copper in solid phase is carried out. The aspects of diffusion welding of copper with silver, aluminium, nickels, chromium, titanium, stainless steel and refractory metals are considered 35 refs.

Comparison of solid-phase and eluate assays to gauge the ecotoxicological risk of organic wastes on soil organisms

International Nuclear Information System (INIS)

Domene, Xavier; Alcaniz, Josep M.; Andres, Pilar

2008-01-01

Development of methodologies to assess the safety of reusing polluted organic wastes in soil is a priority in Europe. In this study, and coupled with chemical analysis, seven organic wastes were subjected to different aquatic and soil bioassays. Tests were carried out with solid-phase waste and three different waste eluates (water, methanol, and dichloromethane). Solid-phase assays were indicated as the most suitable for waste testing not only in terms of relevance for real situations, but also because toxicity in eluates was generally not representative of the chronic effects in solid-phase. No general correlations were found between toxicity and waste pollutant burden, neither in solid-phase nor in eluate assays, showing the inability of chemical methods to predict the ecotoxicological risks of wastes. On the contrary, several physicochemical parameters reflecting the degree of low organic matter stability in wastes were the main contributors to the acute toxicity seen in collembolans and daphnids. - Comparison of solid-phase and eluate bioassays for organic waste testing

Heat and Mass Transfer during Solid-Liquid Phase Transition of n-Alkanes in the C{sub 16} to C{sub 19} Range

Energy Technology Data Exchange (ETDEWEB)

Holmen, Rune

2002-07-01

The main goal of this project has been to study heat and mass transfer during solid-liquid phase transition of n-alkanes in the in the C{sub 16} to C{sub 19} range. Phase transitions of both mixtures and pure components have been investigated. All experiments and simulations have been performed without any convection. Thermal conductivities have been determined at the melting point for solid and liquid unbranched alkanes ranging from C{sub 16} to C{sub 19}. An assessment of the error of the method has been performed. The measurements of solid conductivities are in accordance with measurements reported previously and confirm the applicability of the method. Liquid conductivities are higher than extrapolated values from the literature. The enhanced conductivity is believed to be caused by structural changes close to the melting point which is not taken into account when extrapolating values from the literature. Experiments have been performed for the purpose of investigating the freezing of mixtures of n-alkanes in the C{sub 16}-C{sub 19} range. The positions of the solid-liquid interfaces have been measured as freezing occurred. Calculations of the ratio of liquid and solid conductivities show that the solid structure of mixtures of the investigated n-alkanes is predominantly in a rotator structure at the temperatures investigated. There are indications of a transformation into an orthorhombic structure at lower temperatures. The temperatures on the solid-liquid interface have been measured, and compared with calculated values from chapter 4. The temperature of the interface is represented better by the measured interfacial temperatures than by the calculated interfacial temperatures. The experimental results indicate that the diffusion of heat is the limiting mechanism of phase transition. This result in a homogeneous liquid composition. A numerical model has been developed in order to simulate the experimental freezing of mixtures. The model represents the results

Solid solution and amorphous phase in Ti–Nb–Ta–Mn systems synthesized by mechanical alloying

Energy Technology Data Exchange (ETDEWEB)

Aguilar, C., E-mail: claudio.aguilar@usm.cl [Departamento de Ingeniería Metalúrgica y Materiales, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Guzman, P. [Departamento de Ingeniería Metalúrgica y Materiales, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Lascano, S. [Departamento de Ingeniería Mecánica, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Parra, C. [Departamento de Física, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Bejar, L. [Instituto de Investigaciones Metalúrgicas, Universidad Michoacana de San Nicolás de Hidalgo, Ciudad Universitaria, Morelia C.P. 58000, Michoacán (Mexico); Medina, A. [Facultad de Ingeniería Mecánica, Universidad Michoacana de San Nicolás de Hidalgo, Ciudad Universitaria, C.P. 58000, Michoacán (Mexico); Guzman, D. [Departamento de Metalurgia, Universidad de Atacama, Av. España 485, Copiapó (Chile)

2016-06-15

This work discusses the formation of Ti–30Nb–13Ta–xMn (x: 2, 4 and 6 wt%) solid solution by mechanical alloying using a shaker mill. A solid solution was formed after 15 h of milling and an amorphous phase was formed after 30 h of milling, according to X-ray diffraction results. Disappearance of strongest X-ray diffraction peaks of Nb, Ta and Mn indicated the formation of solid solution, while, X-ray diffraction patterns of powders milled for 30 h showed an amorphous hump with crystalline peaks in the angular range of 35–45° in 2θ. TEM image analysis showed the presence of nanocrystalline intermetallic compounds embedded in an amorphous matrix. Mn{sub 2}Ti, MnTi and NbTi{sub 4} intermetallic compounds were detected and revealed crystallites with size ranging from 3 to 20 nm. The Gibbs free energy for the formation of solid solution and amorphous phase of three ternary systems (Ti–Nb–Ta, Ti–Nb–Mn and Ti–Ta–Mn) was calculated using extended Miedema's model. Experimental and thermodynamic data confirmed that solid solution was first formed in the alloy with 6wt% Mn followed by the formation of an amorphous phase as milling time increases. The presence of Mn promoted the formation of amorphous phase because the atomic radius difference between Mn with Ti, Nb and Ta. - Highlights: • Thermodynamics analysis of extension of solid solution of the Ti–Nb–Ta–Mn system. • Formation of amorphous phase and intermetallic compounds were observed. • Nanocrystalline intermetallic compounds were formed with the sizes between 3 and 20 nm.

Extended solid solubility of a Co–Cr system by mechanical alloying

International Nuclear Information System (INIS)

Betancourt-Cantera, J.A.; Sánchez-De Jesús, F.; Torres-Villaseñor, G.; Bolarín-Miró, A.M.; Cortés-Escobedo, C.A.

2012-01-01

Highlights: ► Solubility of the Co–Cr system is modified by means of Mechanical Alloying (MA). ► MA induces the formation of new solid solutions of Co–Cr system in non-equilibrium. ► MA promote the formation of metastable Co–Cr phases with greater solubility. - Abstract: Mechanical alloying, MA, has been successfully used to extend the limits of solid solubility in many commercially important metallic systems. The aim of this work is to demonstrate that MA modifies the solid solubility of the Co–Cr system. Co and Cr elemental powders were used as precursors and mixed in an adequate weight ratio to obtain Co 100−x Cr x (0 ≤ x ≤ 100, Δx = 10) to study the effect of mechanical processing in the solubility of the Co–Cr system. Processing was carried out at room temperature in a shaker mixer mill using vials and balls of hardened steel as milling media with a ball:powder weight ratio of 10:1. Crystalline structure characterization of the milled powders was conducted using X-ray diffraction, and phase transformations as a function of composition were analyzed. Thermal analysis confirmed structural changes occurred in the mechanically alloyed powders. The evolution of the phase transformations with composition is reported for each composition. The results showed that after high energy ball milling for 7 h, the solid solubility between Co and Cr could be evidently extended, despite the low solid solubility at the equilibrium conditions of this system. Additionally, the micrographs of the milled powders showed that increasing composition of chromium changes the shape and size of the particles while simultaneously reducing their agglomeration; this effect is possibly attributed to the brittleness of elemental chrome.

Extended solid solubility of a Co-Cr system by mechanical alloying

Energy Technology Data Exchange (ETDEWEB)

Betancourt-Cantera, J.A. [Area Academica de Ciencias de la Tierra y Materiales, UAEH Carr. Pachuca-Tulancingo Km. 4.5, Pachuca, Hidalgo 42184 (Mexico); Sanchez-De Jesus, F., E-mail: fsanchez@uaeh.edu.mx [Area Academica de Ciencias de la Tierra y Materiales, UAEH Carr. Pachuca-Tulancingo Km. 4.5, Pachuca, Hidalgo 42184 (Mexico); Torres-Villasenor, G. [Instituto de Investigaciones en Materiales-UNAM, Apdo. Postal 70-360, 04510 Mexico, DF (Mexico); Bolarin-Miro, A.M. [Area Academica de Ciencias de la Tierra y Materiales, UAEH Carr. Pachuca-Tulancingo Km. 4.5, Pachuca, Hidalgo 42184 (Mexico); Cortes-Escobedo, C.A. [Centro de Investigacion e Innovacion Tecnologica del IPN Cda. CECATI S/N, Col. Sta. Catarina, Azcapotzalco, 02250 Mexico, DF (Mexico)

2012-07-15

Highlights: Black-Right-Pointing-Pointer Solubility of the Co-Cr system is modified by means of Mechanical Alloying (MA). Black-Right-Pointing-Pointer MA induces the formation of new solid solutions of Co-Cr system in non-equilibrium. Black-Right-Pointing-Pointer MA promote the formation of metastable Co-Cr phases with greater solubility. - Abstract: Mechanical alloying, MA, has been successfully used to extend the limits of solid solubility in many commercially important metallic systems. The aim of this work is to demonstrate that MA modifies the solid solubility of the Co-Cr system. Co and Cr elemental powders were used as precursors and mixed in an adequate weight ratio to obtain Co{sub 100-x}Cr{sub x} (0 {<=} x {<=} 100, {Delta}x = 10) to study the effect of mechanical processing in the solubility of the Co-Cr system. Processing was carried out at room temperature in a shaker mixer mill using vials and balls of hardened steel as milling media with a ball:powder weight ratio of 10:1. Crystalline structure characterization of the milled powders was conducted using X-ray diffraction, and phase transformations as a function of composition were analyzed. Thermal analysis confirmed structural changes occurred in the mechanically alloyed powders. The evolution of the phase transformations with composition is reported for each composition. The results showed that after high energy ball milling for 7 h, the solid solubility between Co and Cr could be evidently extended, despite the low solid solubility at the equilibrium conditions of this system. Additionally, the micrographs of the milled powders showed that increasing composition of chromium changes the shape and size of the particles while simultaneously reducing their agglomeration; this effect is possibly attributed to the brittleness of elemental chrome.

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.

Ti2Al(C, N) Solid Solution Reinforcing TiAl-Based Composites: Evolution of a Core-Shell Structure, Interfaces, and Mechanical Properties.

Science.gov (United States)

Song, Xiaojie; Cui, Hongzhi; Han, Ye; Ding, Lei; Song, Qiang

2018-05-16

In this work, Ti 2 Al(C, N) solid solution with lamellar structure-enhanced TiAl matrix composites was synthesized by vacuum arc melting, using bulk g-C 3 N 4 , Ti, and Al powders as raw materials. The phases, microstructures, interfaces, and mechanical properties were investigated. MAX phase of Ti 2 Al(C, N) solid solution with lamellar structure was formed. During the melting process, first, C 3 N 4 reacted with Ti to form Ti(C, N) by Ti + C 3 N 4 → Ti(C, N). Then Ti 2 Al(C, N) was formed by a peritectic reaction of TiAl(l) + Ti(C, N)(s) → Ti 2 Al(C, N). C 3 N 4 is the single reactant that provides C and N simultaneously to final product of Ti 2 Al(C, N). The interfaces of TiAl//Ti 2 Al(C, N) and Ti 2 Al(C, N)//Ti(C, N) display perfect orientation relationships with low misfit values. The microhardness, compressive strength, and strain of best-performing TiAl-10 mol % Ti 2 Al(C, N) composite were improved by 45%, 55.7%, and 50% compared with the TiAl alloy, respectively. Uniformly distributed Ti 2 Al(C, N) and unreacted Ti(C, N) particles contributed to the grain refinement and reinforcement of the TiAl matrix. Laminated tearing, particle pull-out, and the crack-arresting of Ti 2 Al(C, N) are crucial for the improvement in compressive strength and plasticity of the composites.

The Systematics of Activity-Composition Relations in Mg-Fe2+ Oxide and Silicate Solid Solutions

Science.gov (United States)

O'Neill, H. S.

2006-12-01

The need to quantify activity-composition relations of mineral solid solutions for petrologic modelling has prompted many experimental studies, but different studies on the same system often appear to show a startling lack of consistency. A good example is Mg-Fe2+ mixing in garnet (the pyrope-almandine join). This is understandable because the energies of mixing in solid solutions are often obtained experimentally as small difference between large numbers. In particular, the fallacy of using a sequential approach to data fitting to a thermodynamic model leads to the accumulated errors being artificially concentrated onto the last step of the fitting process, which is usually that part of the model dealing with the excess energies of mixing. This gives rise to erroneous activity-composition relations, often apparently showing complex deviations from ideality. Systemizing the results of many studies can reveal underlying patterns of behaviour while also identifying outliers and anomalies that may be worth reinvestigating. Davies and Navrotsky [1] showed that the energies of mixing of many different pairs of ions with the same charge correlated well with the difference in molar volumes of the end-members, within a particular crystal structure. This empirical work is now supported by theoretical calculations. It underlies the modern approach to melt/crystal trace-element partitioning. Provided an internally consistent dataset is used, an analogous correlation may be demonstrated across different crystal structures for the mixing of one pair of ions, such as Mg and Fe2+. Activity-composition relations in MgO-"FeO" magnesiowuestite solutions in equilibrium with iron metal were used to obtain the properties of Mg-Fe olivine solutions from magnesiowuestite/olivine partitioning [2]. New results at 1400 K, 1 bar and 1473 K, 25 kb (O'Neill and Pownceby, in prep.) confirm previous work that mixing in Mg-Fe olivine is regular (symmetrical) with W Mg-Fe = 2.5 kJ/mol, with an

Isostructural solid-solid phase transition in monolayers of soft core-shell particles at fluid interfaces: structure and mechanics.

Science.gov (United States)

Rey, Marcel; Fernández-Rodríguez, Miguel Ángel; Steinacher, Mathias; Scheidegger, Laura; Geisel, Karen; Richtering, Walter; Squires, Todd M; Isa, Lucio

2016-04-21

We have studied the complete two-dimensional phase diagram of a core-shell microgel-laden fluid interface by synchronizing its compression with the deposition of the interfacial monolayer. Applying a new protocol, different positions on the substrate correspond to different values of the monolayer surface pressure and specific area. Analyzing the microstructure of the deposited monolayers, we discovered an isostructural solid-solid phase transition between two crystalline phases with the same hexagonal symmetry, but with two different lattice constants. The two phases corresponded to shell-shell and core-core inter-particle contacts, respectively; with increasing surface pressure the former mechanically failed enabling the particle cores to come into contact. In the phase-transition region, clusters of particles in core-core contacts nucleate, melting the surrounding shell-shell crystal, until the whole monolayer moves into the second phase. We furthermore measured the interfacial rheology of the monolayers as a function of the surface pressure using an interfacial microdisk rheometer. The interfaces always showed a strong elastic response, with a dip in the shear elastic modulus in correspondence with the melting of the shell-shell phase, followed by a steep increase upon the formation of a percolating network of the core-core contacts. These results demonstrate that the core-shell nature of the particles leads to a rich mechanical and structural behavior that can be externally tuned by compressing the interface, indicating new routes for applications, e.g. in surface patterning or emulsion stabilization.

Comparison of solid and liquid-phase bioassays using ecoscores to assess contaminated soils

International Nuclear Information System (INIS)

Lors, Christine; Ponge, Jean-Francois; Martinez Aldaya, Maite; Damidot, Denis

2011-01-01

Bioassays on aqueous and solid phases of contaminated soils were compared, belonging to a wide array of trophic and response levels and using ecoscores for evaluating ecotoxicological and genotoxicological endpoints. The method was applied to four coke factory soils contaminated mainly with PAHs, but also to a lesser extent by heavy metals and cyanides. Aquatic bioassays do not differ from terrestrial bioassays when scaling soils according to toxicity but they are complementary from the viewpoint of ecological relevance. Both aquatic and terrestrial endpoints are strongly correlated with concentrations of 3-ring PAHs. This evaluation procedure allows us to propose a cost-effective battery which embraces a wide array of test organisms and response levels: it includes two rapid bioassays (Microtox) and springtail avoidance), a micronucleus test and three bioassays of a longer duration (algal growth, lettuce germination and springtail reproduction). This battery can be recommended for a cost-effective assessment of polluted/remediated soils. - Highlights: → Comparison of liquid- and solid-phase bioassays on contaminated soils, using ecoscores. → Complementarity of liquid- and solid-phase bioassays for the evaluation of environmental hazards. → Proposal for a restricted battery of 5 most sensitive tests. → Use of this restricted battery for a cost-effective assessment of polluted/remediated soils. - Aqueous and solid phases of contaminated soils give similar results in terms of toxicity but are complementary for the evaluation of environmental hazards by ecoscores.

Controlling the alloy composition of PtNi nanocrystals using solid-state dewetting of bilayer films

Energy Technology Data Exchange (ETDEWEB)

Seo, Okkyun; Oh, Se An; Lee, Ji Yeon; Ha, Sung Soo; Kim, Jae Myung; Choi, Jung Won; Kim, Jin-Woo [Department of Physics and Photon Science & School of Materials Science and Engineering, Gwangju Institute of Science and Technology, Gwangju 61005 (Korea, Republic of); Kang, Hyon Chol [Department of Materials and Science Engineering, Chosun University, Gwangju 61542 (Korea, Republic of); Noh, Do Young, E-mail: dynoh@gist.ac.kr [Department of Physics and Photon Science & School of Materials Science and Engineering, Gwangju Institute of Science and Technology, Gwangju 61005 (Korea, Republic of)

2016-05-15

We demonstrate that solid-state dewetting of bilayer films is an effective way for obtaining bimetallic alloy nanocrystals of controlled composition. When a Pt–Ni bilayer film were annealed near 700 °C, Pt and Ni atoms inter-diffused to form a PtNi bimetallic alloy film. Upon annealing at higher temperatures, the bilayer films transformed into <111> oriented PtNi alloy nanocrystals in small-rhombicuboctahedron shape through solid-state dewetting process. The Pt content of the nanocrystals and the alloy films, estimated by applying the Vegard's law to the relaxed lattice constant, was closely related to the thickness of each layer in the as-grown bilayer films which can be readily controlled during bilayer deposition. - Highlights: • Composition control of PtNi nanoparticles using solid state dewetting is proposed. • PtNi alloy composition was controlled by thickness ratio of Pt–Ni bilayer films. • PtNi alloy nanocrystals were obtained in small-rhombicuboctahedron shape.

Investigation of impurity-helium solid phase decomposition

International Nuclear Information System (INIS)

Boltnev, R.E.; Gordon, E.B.; Krushinskaya, I.N.; Martynenko, M.V.; Pel'menev, A.A.; Popov, E.A.; Khmelenko, V.V.; Shestakov, A.F.

1997-01-01

The element composition of the impurity-helium solid phase (IHSP), grown by injecting helium gas jet, involving Ne, Ar, Kr, and Xe atoms and N 2 molecules, into superfluid helium, has been studied. The measured stoichiometric ratios, S = N H e / N I m, are well over the values expected from the model of frozen together monolayer helium clusters. The theoretical possibility for the freezing of two layers helium clusters is justified in the context of the model of IHSP helium subsystem, filled the space between rigid impurity centers. The process of decomposition of impurity-helium (IH)-samples taken out of liquid helium in the temperature range 1,5 - 12 K and the pressure range 10-500 Torr has been studied. It is found that there are two stages of samples decomposition: a slow stage characterized by sample self cooling and a fast one accompanied by heat release. These results suggest, that the IHSP consists of two types of helium - weakly bound and strongly bound helium - that can be assigned to the second and the first coordination helium spheres, respectively, formed around heavy impurity particles. A tendency for enhancement of IHSP thermo stability with increasing the impurity mass is observed. Increase of helium vapor pressure above the sample causes the improvement of IH sample stability. Upon destruction of IH samples, containing nitrogen atoms, a thermoluminescence induced by atom recombination has been detected in the temperature region 3-4,5 K. This suggests that numerous chemical reactions may be realized in solidified helium

Solid-phase synthesis of polyfunctional polylysine dendrons using aldehyde linkers

DEFF Research Database (Denmark)

Svenssen, Daniel K.; Mirsharghi, Sahar; Boas, Ulrik

2014-01-01

A straightforward method for the solid-phase synthesis of C-terminally modified polylysine dendrons has been developed by applying bisalkoxybenzaldehyde and trisalkoxybenzaldehyde linkers. The method has been used for the synthesis of polylysine dendrons with a variety of C-terminal ‘tail groups’...

Graft-copolymerization of styrene on polypropylene in the solid phase

NARCIS (Netherlands)

Beenen, W.; VanderWal, D.; Janssen, L.P.B.M.; Buijtenhuijs, A.; Hogt, A.H.; Wal, Douwe J. v.d.

The graft-copolymerization of styrene on PP in the solid phase has been studied under various reaction conditions using a radical initiator. Polymerization kinetics were investigated by DSC experiments and reactions in glass ampoules. The conversion rate and grafting efficiency of styrene appeared

Immunochemical cross-reactivity between albumin and solid-phase adsorbed histamine

DEFF Research Database (Denmark)

Poulsen, L K; Nolte, H; Søndergaard, I

1990-01-01

For production of an antibody against histamine, this was coupled to human serum albumin (HSA) and used for immunization of rabbits. To test the antiserum, an immunoradiometric assay was developed comprising solid-phase bound histamine, antisera and radiolabelled protein A. Titration and inhibition...

The phase diagram and magnetic properties of Co and Ti co-doped (1−x)BiFeO_3–xLaFeO_3 solid solutions

International Nuclear Information System (INIS)

Wu, Jiangtao; Xu, Jun; Li, Nan; Jiang, Yaqi; Xie, Zhaoxiong

2015-01-01

Single phase Co and Ti co-doped Bi_1_−_xFeO_3−La_xFeO_3 (x = 0–1) solid solutions were prepared by the sol–gel method. Room temperature x-ray powder diffraction (XRD) patterns showed that the structures of as-prepared Bi_1_−_xLa_xFe_0_._9_0Co_0_._0_5Ti_0_._0_5O_3 solid solutions transformed from rhombohedral R3c to tetragonal P4mm and then to orthorhombic Pnma, with increasing La concentration from 0 to 1. In situ high-temperature XRD (HTXRD) analysis further revealed that rhombohedral structure R3c (x ≤ 0.16) and tetragonal structure P4mm (0.17 ≤ x ≤ 0.40) changed to orthorhombic Pnma along with increasing temperature, and the phase transition temperature decreased with the increase of La doping concentration. However, the orthorhombic structure Pnma (x ≥ 0.41) kept stable even when the temperature reached 850 °C. The phase diagram of as-prepared binary solid solutions of Bi_1_−_xLa_xFe_0_._9_0Co_0_._0_5Ti_0_._0_5O_3(x = 0–1) was drawn on the basis of XRD and HTXRD analysis. Magnetic measurement revealed that the magnetic properties are greatly enhanced with the increase of La content. - Highlights: • Single phase Co and Ti co-doped (1−x)BiFeO_3–xLaFeO_3 (x = 0–1) solid solutions were synthesized. • The phase transitions were investigated by tuning composition and temperature. • Phase diagram was constructed according to the results of XRD for the first time. • The magnetization of solid solution can be enhanced when increasing La content.

Numerical simulation analysis of four-stage mutation of solid-liquid two-phase grinding

Science.gov (United States)

Li, Junye; Liu, Yang; Hou, Jikun; Hu, Jinglei; Zhang, Hengfu; Wu, Guiling

2018-03-01

In order to explore the numerical simulation of solid-liquid two-phase abrasive grain polishing and abrupt change tube, in this paper, the fourth order abrupt change tube was selected as the research object, using the fluid mechanics software to simulate,based on the theory of solid-liquid two-phase flow dynamics, study on the mechanism of AFM micromachining a workpiece during polishing.Analysis at different inlet pressures, the dynamic pressure distribution pipe mutant fourth order abrasive flow field, turbulence intensity, discuss the influence of the inlet pressure of different abrasive flow polishing effect.

Solid phase 125I labelled radioimmunoassay for spermidine

International Nuclear Information System (INIS)

Zhao Shimin

1991-01-01

Using 125 I labelled monoclonal antibody against spermidine and solid phase antigen spermidine-bovine serum albumin conjugate, the radioimmunoassay for spermidine was developed. The sensitivity of this method was about 8 times higher than that of liquid phase 14 C labelled spermidine radioimmunoassay, reaching detection limit of 10 ng/ml (0.5 ng/tube). The working range of standard curve was 0-10 5 ng/ml. The new method was suitable for spermidine measurements in saliva, stomach fluid, and cerebrospinal fluid. The coefficients of variation (CV) of within and between-assay were 4% and 13%, respectively. Preliminary clinical measurements showed that the spermidine levels in saliva of cancer patients and in cerebrospinal fluid of leukemia patients were significantly elevated

Microstructural effects of ductile phase toughening of Nb-Nb silicide composites

International Nuclear Information System (INIS)

Lewandowski, J.J.; Dimiduk, D.; Kerr, W.; Menddiratta, M.G.

1988-01-01

In the Nb-Si system, the terminal Nb phase and Nb 5 Si 3 phase are virtually immiscible up to approximately 2033k. This system offers the potential of producing composites consisting of a ductile refractory metal phase and a strong intermetallic phase. In-situ composites containing different volume fractions of the ductile Nb phase were produced via vacuum arc-casting. Microhardness testing as well as smooth bend bar testing was conducted at temperatures ranging from 298k to 1673k in an attempt to determine microstructural effects on the yield strength and smooth bar fracture strength. Notched bend specimens were similarly tested to determine the effects of the ductile phase (i.e. Nb) on enhancing the notched bend toughness. It is shown that Nb phase often behaves in a ductile manner during testing, thereby toughening the in-situ composite. The mechanism of toughening appears to be due to crack bridging

Microstructures and room temperature fracture toughness of Nb/Nb5Si3 composites alloyed with W, Mo and W–Mo fabricated by spark plasma sintering

International Nuclear Information System (INIS)

Xiong, Bowen; Cai, Changchun; Wang, Zhenjun

2014-01-01

Highlights: • Microstructure of Nb/Nb 5 Si 3 composite alloyed with W and Mo is change obviously. • W and Mo elements can solid solution in Nb and Nb 5 Si 3 phase respectively. • Alloyed with W and Mo together, the solid solubility of Nb 5 Si 3 phases is undetected. • The Nb/Nb 5 Si 3 composite alloyed with W and Mo together has high fracture toughness. - Abstract: Microstructures and room temperature fracture toughness of Nb/Nb 5 Si 3 composites alloyed with W, Mo and W–Mo fabricated by spark plasma sintering were investigated. The microstructures were examined using scanning electron microscope (SEM). X-ray diffraction (XRD) was performed on the bulk specimens for identification of phases. The chemical species were analyzed using electron-probe micro-analysis (EPMA). Results indicated that the microstructures of Nb/Nb 5 Si 3 composites alloyed with W or Mo is unaltered, including primary Nb and eutectic mixtures of Nb and Nb 5 Si 3 , and the coarse and fine eutectic mixtures. The W and Mo elements solid solution in Nb and Nb 5 Si 3 phase are detected. But that alloyed with W and Mo together, The microstructures are change obviously, including Nb phase, the solid solubility phases of W and Mo atoms in Nb, and the solid solubility phases of Nb atoms in W are also found, but the solid solubility phenomenon of Nb 5 Si 3 phases is not detected. The microhardness of Nb and Nb 5 Si 3 phases increases obviously because of solid solution strengthening. The Nb/Nb 5 Si 3 composite alloyed with W and Mo together hashing high fracture toughness is attributable to the big eutectic Nb and interface of eutectic phases, which can bear large deformation to absorb the crack energy and form the decohesion between eutectic phases

Size effect for phase stability on Au–Cd–Ag of phase boundary composition

International Nuclear Information System (INIS)

Matsuoka, Yuki; Suzuki, Keiko; Kudo, Natsuko

2013-01-01

Highlights: ► Size and heat treatment effects of phase boundary composition Au 52.5−x Cd 47.5 Ag x were studied. ► The transformation temperature T 0 increases by quench. It is investigated that disordering of atoms and lattice defects make β-phase unstable. ► Downsizing sample decreased T 0 in β-phase, showed a tendency of increase in coexistent phase. ► Downsizing is supposed to make difficult nucleation for martensitic transformation. ► Increasing of surface ratio by downsizing of powder sample is estimated to make easy to transform from unstable β-phase to martensite phase. -- Abstract: Size and heat treatment effects on martensitic transformation of phase boundary composition Au 52.5−x Cd 47.5 Ag x were studied. Au 52.5−x Cd 47.5 Ag x has coexistent phase of β-phase and α-phase of fcc structure at x > 42 at.%. The transformation temperature T 0 decreases as Au is substituted on Ag over phase boundary. T 0 increases by quench in both case of bulk and powder. This behavior is investigated that disordering of atoms and lattice defects make β-phase (L2 1 , B2 or bcc) unstable. Size effect was also inspected. Downsizing sample decreased the transformation temperature in β-phase. On the contrary, the transformation temperature of the coexistent phase showed a tendency of increase. Downsizing is supposed to make difficult nucleation for martensitic transformation because of reduction of β-phase ordered volume. Increasing of surface (disorder structure) ratio by downsizing of powder sample is estimated to make easy to transform from unstable β-phase to martensite phase

Solid gas reaction phase diagram under high gas pressure

International Nuclear Information System (INIS)

Ishizaki, K.

1992-01-01

This paper reports that to evaluate which are the stable phases under high gas pressure conditions, a solid-gas reaction phase diagram under high gas pressure (HIP phase diagram) has been proposed by the author. The variables of the diagram are temperature, reactant gas partial pressure and total gas pressure. Up to the present time the diagrams have been constructed using isobaric conditions. In this work, the stable phases for a real HIP process were evaluated assuming an isochoric condition. To understand the effect of the total gas pressure on stability is of primary importance. Two possibilities were considered and evaluated, those are: the total gas pressure acts as an independent variable, or it only affects the fugacity values. The results of this work indicate that the total gas pressure acts as an independent variable, and in turn also affects the fugacity values

Geological constraints on the thermodynamic properties of the stilbite - stellerite solid solution in low-grade metabasalts

Science.gov (United States)

Fridriksson, Thráinn; Neuhoff, Philip S.; Arnórsson, Stefán; Bird, Dennis K.

2001-11-01

Standard state thermodynamic data for stilbite (Ca2NaAl5Si13O36∗16H2O) and stellerite (Ca2Al4Si14O36∗14H2O), together with mixing properties of the stilbite -stellerite solid solution (stilbite SS) are derived through assessment of geological observations of stilbite SS compositions in metabasalts, experimental phase equilibria, and calorimetric observations. Measured compositions of stilbite SS in Tertiary metabasalts in Iceland and Icelandic geothermal systems change systematically towards the stellerite endmember with increasing stratigraphic depth and temperature. Standard molal volumes, heat capacities, and entropies for the endmembers of the solid solution are derived through critical review of published crystallographic and calorimetric data for natural stilbite SS. Standard molal Gibbs energies of formation at 298.15 K and 1 bar for stilbite (-4,946,475cal mol-1) and stellerite (-4,762,036 cal mol-1) and the mixing properties of the solid solution are retrieved from observed phase- and compositional-relations in metabasalts at Berufjördur, Iceland, measured temperatures of zeolite mineral distribution in active geothermal systems, and published observations of reversed phase equilibria. Mixing in stilbite SS can be described with an athermal solid solution model. Thermodynamic data resulting from our analysis provide close correlation between compositions of stilbite SS in Icelandic geothermal systems predicted from compositions of geothermal solutions and observed compositions of these minerals in low-grade metabasalts of Iceland, as well as the observed temperature of the stilbite SS to laumontite (leonhardite) transition in Icelandic geothermal systems. Stilbite SS composition in metabasalts is a sensitive function of temperature, fluid composition, coexisting minerals (especially silica polymorphs) and geothermal gradient.

Tethered Nanoparticle–Polymer Composites: Phase Stability and Curvature

KAUST Repository

Srivastava, Samanvaya

2012-04-17

Phase behavior of poly(ethylene glycol) (PEG) tethered silica nanoparticles dispersed in PEG hosts is investigated using small-angle X-ray scattering. Phase separation in dispersions of densely grafted nanoparticles is found to display strikingly different small-angle X-ray scattering signatures in comparison to phase-separated composites comprised of bare or sparsely grafted nanoparticles. A general diagram for the dispersion state and phase stability of polymer tethered nanoparticle-polymer composites incorporating results from this as well as various other contemporary studies is presented. We show that in the range of moderate to high grafting densities the dispersion state of nanoparticles in composites is largely insensitive to the grafting density of the tethered chains and chemistry of the polymer host. Instead, the ratio of the particle diameter to the size of the tethered chain and the ratio of the molecular weights of the host and tethered polymer chains (P/N) are shown to play a dominant role. Additionally, we find that well-functionalized nanoparticles form stable dispersions in their polymer host beyond the P/N limit that demarcates the wetting/dewetting transition in polymer brushes on flat substrates interacting with polymer melts. A general strategy for achieving uniform nanoparticle dispersion in polymers is proposed. © 2012 American Chemical Society.

Thermal properties and heat storage analysis of palmitic acid-TiO_2 composite as nano-enhanced organic phase change material (NEOPCM)

International Nuclear Information System (INIS)

Sharma, R.K.; Ganesan, P.; Tyagi, V.V.; Metselaar, H.S.C.; Sandaran, S.C.

2016-01-01

Highlights: • Novel composite of palmitic acid and TiO_2 nanoparticles with enhanced thermal energy storage capabilities • The composite is thermally reliable and chemically stable. • Thermal conductivity of the composite increases significantly with the loading. - Graphical Abstract: - Abstract: In the present study, the phase change behavior of prepared novel composites of palmitic acid and solid nanoparticles of titanium dioxide (TiO_2) for thermal energy storage has been investigated. The nanoparticles are dispersed into the base fluid in various mass fractions (0.5, 1, 3, and 5%), and their effects on the thermo-physical properties have been investigated. Structural analysis has been carried out by using FESEM, and crystallography was checked by XRD technique. The chemical/functional groups of the base fluid and composite PCMs have been analyzed by using FT-IR spectrum. The observations showed that the TiO_2 nanoparticles do not affect the chemical structure of palmitic acid; however they improve the chemical stability. The phase transition temperature and latent heat of fusion has shown the significant stability with the increase in nanoparticle weight fractions. The accelerated thermal cycle test of the composite shows good thermal reliability for 1500 melt/freeze cycles. Thermal conductivity of palmitic acid increased gradually by 12.7, 20.6, 46.6, and 80% for the nanoparticle weight fractions of 0.5, 1, 3, and 5% respectively. Based on the results, it can be mentioned that the prepared palmitic acid based nano-enhanced organic phase change composite materials can be very well used as potential solar thermal energy storage materials.

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

Morphology, composition, and mixing state of primary particles from combustion sources - crop residue, wood, and solid waste.

Science.gov (United States)

Liu, Lei; Kong, Shaofei; Zhang, Yinxiao; Wang, Yuanyuan; Xu, Liang; Yan, Qin; Lingaswamy, A P; Shi, Zongbo; Lv, Senlin; Niu, Hongya; Shao, Longyi; Hu, Min; Zhang, Daizhou; Chen, Jianmin; Zhang, Xiaoye; Li, Weijun

2017-07-11

Morphology, composition, and mixing state of individual particles emitted from crop residue, wood, and solid waste combustion in a residential stove were analyzed using transmission electron microscopy (TEM). Our study showed that particles from crop residue and apple wood combustion were mainly organic matter (OM) in smoldering phase, whereas soot-OM internally mixed with K in flaming phase. Wild grass combustion in flaming phase released some Cl-rich-OM/soot particles and cardboard combustion released OM and S-rich particles. Interestingly, particles from hardwood (pear wood and bamboo) and softwood (cypress and pine wood) combustion were mainly soot and OM in the flaming phase, respectively. The combustion of foam boxes, rubber tires, and plastic bottles/bags in the flaming phase released large amounts of soot internally mixed with a small amount of OM, whereas the combustion of printed circuit boards and copper-core cables emitted large amounts of OM with Br-rich inclusions. In addition, the printed circuit board combustion released toxic metals containing Pb, Zn, Sn, and Sb. The results are important to document properties of primary particles from combustion sources, which can be used to trace the sources of ambient particles and to know their potential impacts in human health and radiative forcing in the air.

A silica fiber coated with a ZnO-graphene oxide nanocomposite with high specific surface for use in solid phase microextraction of the antiepileptic drugs diazepam and oxazepam.

Science.gov (United States)

Alizadeh, Reza; Salami, Maryam; Seidi, Shahram

2018-06-02

A novel ZnO-graphene oxide nanocomposite was prepared and is shown to be a viable coating on fused silica fibers for use in solid phase microextraction (SPME) of diazepam and oxazepam from urine, this followed by thermal desorption and gas chromatographic quantitation using a flame ionization detector. A central composite design was used to optimize extraction time, salt percentage, sample pH and desorption time. Limits of detection are 0.5 μg·L -1 for diazepam and 1.0 μg·L -1 for oxazepam. Repeatability and reproducibility for one fiber (n = 4), expressed as the relative standard deviation at a concentration of 50 μg·L -1 , are 8.3 and 11.3% for diazepam, and 6.7 and 10.1% for oxazepam. The fiber-to-fiber reproducibility is Graphical abstract A hydrothermal method was introduced for preparation of ZnO- GO nano composite on a fused silica fiber as solid phase microextraction with high mechanical, chemical stability and long service life.

Gold catalyzed nickel disilicide formation: a new solid-liquid-solid phase growth mechanism.

Science.gov (United States)

Tang, Wei; Picraux, S Tom; Huang, Jian Yu; Liu, Xiaohua; Tu, K N; Dayeh, Shadi A

2013-01-01

The vapor-liquid-solid (VLS) mechanism is the predominate growth mechanism for semiconductor nanowires (NWs). We report here a new solid-liquid-solid (SLS) growth mechanism of a silicide phase in Si NWs using in situ transmission electron microcopy (TEM). The new SLS mechanism is analogous to the VLS one in relying on a liquid-mediating growth seed, but it is fundamentally different in terms of nucleation and mass transport. In SLS growth of Ni disilicide, the Ni atoms are supplied from remote Ni particles by interstitial diffusion through a Si NW to the pre-existing Au-Si liquid alloy drop at the tip of the NW. Upon supersaturation of both Ni and Si in Au, an octahedral nucleus of Ni disilicide (NiSi2) forms at the center of the Au liquid alloy, which thereafter sweeps through the Si NW and transforms Si into NiSi2. The dissolution of Si by the Au alloy liquid mediating layer proceeds with contact angle oscillation at the triple point where Si, oxide of Si, and the Au alloy meet, whereas NiSi2 is grown from the liquid mediating layer in an atomic stepwise manner. By using in situ quenching experiments, we are able to measure the solubility of Ni and Si in the Au-Ni-Si ternary alloy. The Au-catalyzed mechanism can lower the formation temperature of NiSi2 by 100 °C compared with an all solid state reaction.

Heat transfer in multi-phase materials

CERN Document Server

Öchsner, Andreas

2011-01-01

This book provides a profound understanding, which physical processes and mechanisms cause the heat transfer in composite and cellular materials. It shows models for all important classes of composite materials and introduces into the latest advances. In three parts, the book covers Composite Materials (Part A), Porous and Cellular Materials (Part B) and the appearance of a conjoint solid phase and fluid aggregate (Part C).

Strong work-hardening behavior induced by the solid solution strengthening of dendrites in TiZr-based bulk metallic glass matrix composites

Energy Technology Data Exchange (ETDEWEB)

Ma, D.Q. [State Key Laboratory of Metastable Materials Science and Technology, Yanshan University, Qinhuangdao 066004 (China); Jiao, W.T. [College of Education, Hebei Normal University of Science and Technology, Qinhuangdao 066004 (China); Zhang, Y.F. [State Key Laboratory of Metastable Materials Science and Technology, Yanshan University, Qinhuangdao 066004 (China); Hebei Vocational and Technical College of Building Materials, Qinhuangdao 066004 (China); Wang, B.A.; Li, J.; Zhang, X.Y. [State Key Laboratory of Metastable Materials Science and Technology, Yanshan University, Qinhuangdao 066004 (China); Ma, M.Z., E-mail: mz550509@ysu.edu.cn [State Key Laboratory of Metastable Materials Science and Technology, Yanshan University, Qinhuangdao 066004 (China); Liu, R.P. [State Key Laboratory of Metastable Materials Science and Technology, Yanshan University, Qinhuangdao 066004 (China)

2015-03-05

Highlights: • Hardness of dendrite of TiZr-based BMGMCs increases. • Strong work-hardening behavior is obtained after solid solution strengthening. • Lattice distortions of dendrite suffering from rapid cooling are detected. - Abstract: A series of TiZr-based bulk metallic glass matrix composites (BMGMCs) with distinguished mechanical properties are successfully fabricated by adding different volume fractions of Ta (Ti{sub 38.8}Zr{sub 28.8}Cu{sub 6.2}Be{sub 16.2}Nb{sub 10} as the basic composition, denoted as Ta{sub 0.0}–Ta{sub 8.0}). Along with the growth of precipitated phase, typical dendritic morphology is fully developed in the TiZr-based BMGMCs of Ta{sub 8.0}. Energy-dispersive spectrometry analysis of the dendrites and glass matrix indicates that the metallic elements of Nb and Ta should preferentially form solid solution into dendrites. The chaotic structure of high-temperature precipitate phase is trapped down by the rapid cooling of the copper-mould. The detected lattice distortions in the dendrites are attributed to the strong solid solution strengthening of the metallic elements of Ti, Zr, Nb, and Ta. These lattice distortions increase the resistance of the dislocation motion and pin the dislocations, thus the strength and hardness of dendrite increase. Dendrites create a strong barrier for the shear band propagation and generate multiple shear bands after solid solution strengthening, thereby providing the TiZr-based BMGMCs with greatly improved capacity to sustain plastic deformation and resistance to brittle fracture. Thus, the TiZr-based BMGMCs possess distinguished work-hardening capability. Among these TiZr-based BMGMCs, the sample Ta{sub 0.5} possesses the largest plastic strain (ε{sub p}) at 20.3% and ultimate strength (σ{sub max}) of 2613 MPa during compressive loading. In addition, the sample of Ta{sub 0.5} exhibits work-hardening up to an ultrahigh tensile strength of 1680 MPa during the tensile process, and then progressively

Solid-state quantum chemistry and materials science: Solid compounds of the d and f elements

International Nuclear Information System (INIS)

Gubanov, V.A.

1989-01-01

Methods have been developed for calculating electron structures for solid compounds of d and f elements and for simulating physicochemical properties of materials based on them. Cluster and band calculations are considered for refractory compounds of d metals formed with light elements. There are bond and property regularities in doping by meals and metalloids, and defects and impurities have certain effects, where studies have been made on the electron structures for disordered phases and solid solutions in relation to sublattice compositions. Quantum-chemical simulation methods have been developed for optically active and fluorescent materials based on d and f metal oxides, fluorides, and chalcogenides, and compositions have been proposed for new optically active composites and protective coatings. New approaches have been defined to the magnetic parameters of metals, alloys, and compounds; these can be applied in simulating new magnetic materials. Calculations are given on energy spectra for high-temperature oxide superconductors. There is interesting scope for quantum-chemical methods in application to many topics in materials science

Constitutive modeling of two-phase metallic composites with application to tungsten-based composite 93W–4.9Ni–2.1Fe

International Nuclear Information System (INIS)

Lu, W.R.; Gao, C.Y.; Ke, Y.L.

2014-01-01

The two-phase metallic composites, composed by the metallic particulate reinforcing phase and the metallic matrix phase, have attracted a lot of attention in recent years for their excellent material properties. However, the constitutive modeling of two-phase metallic composites is still lacking currently. Most used models for them are basically oriented for single-phase homogeneous metallic materials, and have not considered the microstructural evolution of the components in the composite. This paper develops a new constitutive model for two-phase metallic composites based on the thermally activated dislocation motion mechanism and the volume fraction evolution. By establishing the relation between microscopic volume fraction and macroscopic state variables (strain, strain rate and temperature), the evolution law of volume fraction during the plastic deformation in two-phase composites is proposed for the first time and introduced into the new model. Then the new model is applied to a typical two-phase tungsten-based composite – 93W–4.9Ni–2.1Fe tungsten heavy alloy. It has been found that our model can effectively describe the plastic deformation behaviors of the tungsten-based composite, because of the introduction of volume fraction evolution and the connecting of macroscopic state variables and micromechanical characteristics in the constitutive model. The model's validation by experimental data indicates that our new model can provide a satisfactory prediction of flow stress for two-phase metallic composites, which is better than conventional single-phase homogeneous constitutive models including the Johnson–Cook (JC), Khan–Huang–Liang (KHL), Nemat-Nasser–Li (NNL), Zerilli–Armstrong (ZA) and Voyiadjis–Abed (VA) models

Impact of co-landfill proportion of bottom ash and municipal solid waste composition on the leachate characteristics during the acidogenesis phase.

Science.gov (United States)

He, Pin-Jing; Pu, Hong-Xia; Shao, Li-Ming; Zhang, Hua

2017-11-01

Incineration has become an important municipal solid waste (MSW) treatment strategy, and generates a large amount of bottom ash (BA). Although some BA is reused, much BA and pretreatment residues from BA recycling are disposed in landfill. When BA and MSW are co-landfilled together, acid neutralization capacity and alkaline earth metal dissolution of BA, as well as different components of MSW may change environmental conditions within the landfill, so the degradation of organic matter and the physical and chemical properties of leachate would be affected. In this study, the effect of co-landfilled BA and MSW on the leachate characteristics during the hydrolysis and acidogenesis phase was studied using different BA/MSW ratios and MSW compositions. The results showed that the co-landfill system increased leachate pH, electric conductivity and alkalinity. For MSW with a high content of degradable components, the release and degradation of total organic carbon (TOC) and volatile fatty acids (VFA) from MSW were promoted when the BA ratio by wet weight was less than 50%, and the biodegradability of leachate was improved. When the BA ratio exceeded 50%, the degradation of organic matters was inhibited. For MSW with low content of degradable components, when the proportion of BA was less than 20%, the release and degradation of TOC and VFA from MSW were promoted and alkalinity increased. When the BA ratio exceeded 20%, the degradation of organic matters was inhibited. The 50% BA ratio could improve the bio-treatability of leachate indicated by the leachate pH and C/N ratio. However, BA inhibited the release of nitrogen (TN and NH 4 + -N) at all BA ratios and MSW compositions. At the same time, the addition of BA increased the risk of leachate collection system clogging due to the dissolution and re-precipitation of alkaline earth metals contained in BA. Copyright © 2017 Elsevier Ltd. All rights reserved.

Double antibody solid-phase radioimmunoassay for staphylococcal enterotoxin A

International Nuclear Information System (INIS)

Lindroth, S.; Niskanen, A.

1977-01-01

A double antibody solid-phase (DASP) radioimmunoassay for staphylococcal enterotoxin A is described. In the assay the antigen-antibody complex is precipitated by anti-rabbit serum which is adsorbed onto a solid carrier (cellulose). The method is sensitive to 200 pg of enterotoxin. It was possible to detect a little as 2-5 ng of enterotoxin A/ml food extract from minced meat and sausage. Enterotoxins B and C were not found to inhibit the uptake of labled enterotoxin A at a level which might distort the results of the enterotoxin A assay. The DASP technique is sensitive, rapid, and easy to perform and thus compares favorably with other radioimmunoassays for enterotoxin. (orig.) [de

Solid Phase Characterization of Tank 241-C-105 Grab Samples

International Nuclear Information System (INIS)

Ely, T. M.; LaMothe, M. E.; Lachut, J. S.

2016-01-01

The solid phase characterization (SPC) of three grab samples from single-shell Tank 241-C-105 (C-105) that were received at the laboratory the week of October 26, 2015, has been completed. The three samples were received and broken down in the 11A hot cells.

Local structure, composition, and crystallization mechanism of a model two-phase “composite nanoglass”

Energy Technology Data Exchange (ETDEWEB)

Chattopadhyay, Soma; Shibata, Tomohiro [CSRRI-IIT, MRCAT, Sector 10, Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Kelly, S. D. [EXAFS Analysis, Bolingbrook, Illinois 60440 (United States); Balasubramanian, M. [Sector 20 XOR, Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Srinivasan, S. G.; Du, Jincheng; Banerjee, Rajarshi [Department of Materials Science and Engineering, University of North Texas, Denton, Texas 76203-5017 (United States); Ayyub, Pushan, E-mail: pushan@tifr.res.in [Department of Condensed Matter Physics and Materials Science, Tata Institute of Fundamental Research, Mumbai 400005 (India)

2016-02-14

We report a detailed study of the local composition and structure of a model, bi-phasic nanoglass with nominal stoichiometry Cu{sub 55}Nb{sub 45}. Three dimensional atom probe data suggest a nanoscale-phase-separated glassy structure having well defined Cu-rich and Nb-rich regions with a characteristic length scale of ≈3 nm. However, extended x-ray absorption fine structure analysis indicates subtle differences in the local environments of Cu and Nb. While the Cu atoms displayed a strong tendency to cluster and negligible structural order beyond the first coordination shell, the Nb atoms had a larger fraction of unlike neighbors (higher chemical order) and a distinctly better-ordered structural environment (higher topological order). This provides the first experimental indication that metallic glass formation may occur due to frustration arising from the competition between chemical ordering and clustering. These observations are complemented by classical as well as ab initio molecular dynamics simulations. Our study indicates that these nanoscale phase-separated glasses are quite distinct from the single phase nanoglasses (studied by Gleiter and others) in the following three respects: (i) they contain at least two structurally and compositionally distinct, nanodispersed, glassy phases, (ii) these phases are separated by comparatively sharp inter-phase boundaries, and (iii) thermally induced crystallization occurs via a complex, multi-step mechanism. Such materials, therefore, appear to constitute a new class of disordered systems that may be called a composite nanoglass.

[Determination of patulin in fruits and jam by solid phase extraction-ultra performance liquid chromatography].

Science.gov (United States)

Lü, Weichao; Shen, Shuchang; Wang, Chao

2017-11-08

With magnesium silicate, silica gel, diatomite and calcium sulfate as raw materials, a new solid phase extraction column was prepared through a series of processes of grinding to ethanol homogenate, drying and packing into polypropylene tube. The sample was hydrolyzed by pectinase, extracted by acetonitrile and purified by solid phase extraction. The target compounds were separated on a C18 column (100 mm×2.1 mm, 1.8 μm), using 0.8% (v/v) tetrahydrofuran solution as mobile phase with a flow rate of 0.5 mL/min. The detection wavelength was 276 nm. The effect of pectinase on extraction yield and purification effect of solid-phase extraction column were investigated. The optimum chromatographic conditions were selected. There was a good linear relationship between the peak heights and the mass concentrations of patulin in the range of 0.1 to 10 mg/L with the correlation coefficient ( R 2 ) of 1. The limit of detection for this method was 10.22 μg/kg. The spiked recoveries of samples were 86.58%-94.84% with the relative standard deviations (RSDs) of 1.45%-2.28%. The results indicated that the self-made solid phase extraction column had a good purification efficiency, and the UPLC had a high separation efficiency. The method is simple, accurate and of great significance for the quality and safety control of fruit products.

Identification of sigma and OMEGA phases in AA2009/SiC composites

Energy Technology Data Exchange (ETDEWEB)

Rodrigo, P., E-mail: pilar.rodrigo@urjc.e [Departamento de Ciencia e Ingenieria de Materiales, Escuela Superior de Ciencias Experimentales y Tecnologia, Universidad Rey Juan Carlos, c/Tulipan s/n, 28933 Mostoles, Madrid (Spain); Poza, P.; Utrilla, M.V.; Urena, A. [Departamento de Ciencia e Ingenieria de Materiales, Escuela Superior de Ciencias Experimentales y Tecnologia, Universidad Rey Juan Carlos, c/Tulipan s/n, 28933 Mostoles, Madrid (Spain)

2009-08-12

The microstructure evolution during ageing treatment at 170 and 190 deg. C of AA2009/SiC composites, reinforced with 15 vol.% particulates and whiskers, was studied by transmission electron microscopy. Besides theta' and S' phases, the typical hardening precipitates on Al-Cu-Mg alloys, it was found the presence of OMEGA and sigma (Al{sub 5}Cu{sub 6}Mg{sub 2}) phases in the matrix. sigma phase was only found in the matrix of particulate composite, while OMEGA phase appeared in both. This phase has not been previously observed in Al matrix composites based on conventional Al-Cu-Mg alloys.

Detection and specifity of class specific antibodies to whole bacteria cells using a solid phase radioimmunoassay

Energy Technology Data Exchange (ETDEWEB)