WorldWideScience

Sample records for silicate solid phases

  1. Behaviour of Fe4O5-Mg2Fe2O5 solid solutions and their relation to coexisting Mg-Fe silicates and oxide phases

    Science.gov (United States)

    Uenver-Thiele, Laura; Woodland, Alan B.; Miyajima, Nobuyoshi; Ballaran, Tiziana Boffa; Frost, Daniel J.

    2018-03-01

    Experiments at high pressures and temperatures were carried out (1) to investigate the crystal-chemical behaviour of Fe4O5-Mg2Fe2O5 solid solutions and (2) to explore the phase relations involving (Mg,Fe)2Fe2O5 (denoted as O5-phase) and Mg-Fe silicates. Multi-anvil experiments were performed at 11-20 GPa and 1100-1600 °C using different starting compositions including two that were Si-bearing. In Si-free experiments the O5-phase coexists with Fe2O3, hp-(Mg,Fe)Fe2O4, (Mg,Fe)3Fe4O9 or an unquenchable phase of different stoichiometry. Si-bearing experiments yielded phase assemblages consisting of the O5-phase together with olivine, wadsleyite or ringwoodite, majoritic garnet or Fe3+-bearing phase B. However, (Mg,Fe)2Fe2O5 does not incorporate Si. Electron microprobe analyses revealed that phase B incorporates significant amounts of Fe2+ and Fe3+ (at least 1.0 cations Fe per formula unit). Fe-L2,3-edge energy-loss near-edge structure spectra confirm the presence of ferric iron [Fe3+/Fetot = 0.41(4)] and indicate substitution according to the following charge-balanced exchange: [4]Si4+ + [6]Mg2+ = 2Fe3+. The ability to accommodate Fe2+ and Fe3+ makes this potential "water-storing" mineral interesting since such substitutions should enlarge its stability field. The thermodynamic properties of Mg2Fe2O5 have been refined, yielding H°1bar,298 = - 1981.5 kJ mol- 1. Solid solution is complete across the Fe4O5-Mg2Fe2O5 binary. Molar volume decreases essentially linearly with increasing Mg content, consistent with ideal mixing behaviour. The partitioning of Mg and Fe2+ with silicates indicates that (Mg,Fe)2Fe2O5 has a strong preference for Fe2+. Modelling of partitioning with olivine is consistent with the O5-phase exhibiting ideal mixing behaviour. Mg-Fe2+ partitioning between (Mg,Fe)2Fe2O5 and ringwoodite or wadsleyite is influenced by the presence of Fe3+ and OH incorporation in the silicate phases.

  2. Deep-Earth Equilibration between Molten Iron and Solid Silicates

    Science.gov (United States)

    Brennan, M.; Zurkowski, C. C.; Chidester, B.; Campbell, A.

    2017-12-01

    Elemental partitioning between iron-rich metals and silicate minerals influences the properties of Earth's deep interior, and is ultimately responsible for the nature of the core-mantle boundary. These interactions between molten iron and solid silicates were influential during planetary accretion, and persist today between the mantle and liquid outer core. Here we report the results of diamond anvil cell experiments at lower mantle conditions (40 GPa, >2500 K) aimed at examining systems containing a mixture of metals (iron or Fe-16Si alloy) and silicates (peridotite). The experiments were conducted at pressure-temperature conditions above the metallic liquidus but below the silicate solidus, and the recovered samples were analyzed by FIB/SEM with EDS to record the compositions of the coexisting phases. Each sample formed a three-phase equilibrium between bridgmanite, Fe-rich metallic melt, and an oxide. In one experiment, using pure Fe, the quenched metal contained 6 weight percent O, and the coexisting oxide was ferropericlase. The second experiment, using Fe-Si alloy, was highly reducing; its metal contained 10 wt% Si, and the coexisting mineral was stishovite. The distinct mineralogies of the two experiments derived from their different starting metals. These results imply that metallic composition is an important factor in determining the products of mixed phase iron-silicate reactions. The properties of deep-Earth interfaces such as the core-mantle boundary could be strongly affected by their metallic components.

  3. Solid phase radioimmunoassays

    International Nuclear Information System (INIS)

    Wide, L.

    1977-01-01

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

  4. Carbon Monoxide Silicate Reduction System, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — The Carbon Monoxide Silicate Reduction System (COSRS) is an innovative method that for the first time uses the strong reductant carbon monoxide to both reduce iron...

  5. Carbon Monoxide Silicate Reduction System, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — The Carbon Monoxide Silicate Reduction System (COSRS) is a novel technology for producing large quantities of oxygen on the Moon. Oxygen yields of 15 kilograms per...

  6. Copper Containing Silicates as Catalysts for Liquid Phase Cyclohexane Oxidation

    Directory of Open Access Journals (Sweden)

    Cruz Rosenira S. da

    2002-01-01

    Full Text Available Copper containing silicates have been prepared by an acid-catalyzed sol-gel process. The materials were characterized by X-ray diffraction and fluorescence, EPR spectroscopy, elemental analysis, N2-physisorption, thermogravimetry, differential scanning calorimetry, temperature-programmed reduction, FTIR and UV/VIS spectroscopy. The silicates were shown to be efficient catalysts for the oxidation of cyclohexane with tert-butyl hydroperoxide as oxidant. Cyclohexanol and cyclohexanone were obtained as the main products. The metal was shown to be weakly bound to the silicate matrix and metal leaching was observed. Leaching was quantified by X-ray fluorescence and leaching tests showed that the catalytic activity is due to supported copper species. Leached copper showed no activity in the homogeneous phase.

  7. Evaluation of apatite silicates as solid oxide fuel cell electrolytes

    Energy Technology Data Exchange (ETDEWEB)

    Marrero-Lopez, D. [Dpto. de Fisica Aplicada I, Laboratorio de Materiales y Superficies (Unidad Asociada al C.S.I.C.), Universidad de Malaga, 29071 Malaga (Spain); Dpto. de Quimica Inorganica, Universidad de La Laguna, 38200 La Laguna, Tenerife (Spain); Martin-Sedeno, M.C.; Aranda, M.A.G. [Dpto. de Quimica Inorganica, Universidad Malaga, 29071 Malaga (Spain); Pena-Martinez, J. [Dpto. de Quimica Inorganica, Universidad de La Laguna, 38200 La Laguna, Tenerife (Spain); Instituto de Energias Renovables, Parque Tecnologico, Universidad de Castilla La Mancha, 02006 Albacete (Spain); Ruiz-Morales, J.C.; Nunez, P. [Dpto. de Quimica Inorganica, Universidad de La Laguna, 38200 La Laguna, Tenerife (Spain); Ramos-Barrado, J.R. [Dpto. de Fisica Aplicada I, Laboratorio de Materiales y Superficies (Unidad Asociada al C.S.I.C.), Universidad de Malaga, 29071 Malaga (Spain)

    2010-05-01

    Apatite-type silicates have been considered as promising electrolytes for Solid Oxide Fuel Cells (SOFC); however studies on the potential use of these materials in SOFC devices have received relatively little attention. The lanthanum silicate with composition La{sub 10}Si{sub 5.5}Al{sub 0.5}O{sub 26.75} has been evaluated as electrolyte with the electrode materials commonly used in SOFC, i.e. manganite, ferrite and cobaltite as cathode materials and NiO-CGO composite, chromium-manganite and Sr{sub 2}MgMoO{sub 6} as anode materials. Chemical compatibility, area-specific resistance and fuel cell studies have been performed. X-ray powder diffraction (XRPD) analysis did not reveal any trace of reaction products between the apatite electrolyte and most of the aforementioned electrode materials. However, the area-specific polarisation resistance (ASR) of these electrodes in contact with apatite electrolyte increased significantly with the sintering temperature, indicating reactivity at the electrolyte/electrode interface. On the other hand, the ASR values are significantly improved using a ceria buffer layer between the electrolyte and electrode materials to prevent reactivity. Maximum power densities of 195 and 65 mWcm{sup -2} were obtained at 850 and 700 C, respectively in H{sub 2} fuel, using an 1 mm-thick electrolyte, a NiO-Ce{sub 0.8}Gd{sub 0.2}O{sub 1.9} composite as anode and La{sub 0.6}Sr{sub 0.4}Co{sub 0.8}Fe{sub 0.2}O{sub 3-{delta}} as cathode materials. This fuel cell was tested for 100 h in 5%H{sub 2}-Ar atmosphere showing stable performance. (author)

  8. 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)

  9. Understanding the defect chemistry of alkali metal strontium silicate solid solutions: insights from experiment and theory

    KAUST Repository

    Bayliss, Ryan D.

    2014-09-24

    © the Partner Organisations 2014. Recent reports of remarkably high oxide ion conduction in a new family of strontium silicates have been challenged. It has recently been demonstrated that, in the nominally potassium substituted strontium germanium silicate material, the dominant charge carrier was not the oxygen ion, and furthermore that the material was not single phase (R. D. Bayliss et. al., Energy Environ. Sci., 2014, DOI: 10.1039/c4ee00734d). In this work we re-investigate the sodium-doped strontium silicate material that was reported to exhibit the highest oxide ion conductivity in the solid solution, nominally Sr0.55Na0.45SiO2.775. The results show lower levels of total conductivity than previously reported and sub-micron elemental mapping demonstrates, in a similar manner to that reported for the Sr0.8K0.2Si0.5Ge0.5O2.9 composition, an inhomogeneous chemical distribution correlating with a multiphase material. It is also shown that the conductivity is not related to protonic mobility. A density functional theory computational approach provides a theoretical justification for these new results, related to the high energetic costs associated with oxygen vacancy formation. This journal is

  10. Silicate Phases on the Surfaces of Trojan Asteroids

    Science.gov (United States)

    Martin, Audrey; Emery, Joshua P.; Lindsay, Sean S.

    2017-10-01

    Determining the origin of asteroids provides an effective means of constraining the solar system’s dynamic past. Jupiter Trojan asteroids (hereafter Trojans) may help in determining the amount of radial mixing that occurred during giant planet migration. Previous studies aimed at characterizing surface composition show that Trojans have low albedo surfaces and are spectrally featureless in the near infrared. The thermal infrared (TIR) wavelength range has advantages for detecting silicates on low albedo asteroids such as Trojans. The 10 μm region exhibits strong features due to the Si-O fundamental molecular vibrations. Silicates that formed in the inner solar system likely underwent thermal annealing, and thus are crystalline, whereas silicates that accreted in the outer solar system experienced less thermal processing, and therefore are more likely to have remained in an amorphous phase. We hypothesize that the Trojans formed in the outer solar system (i.e., the Kuiper Belt), and therefore will have a more dominant amorphous spectral silicate component. With TIR spectra from the Spitzer Space Telescope, we identify mineralogical features from the surface of 11 Trojan asteroids. Fine-grain mixtures of crystalline pyroxene and olivine exhibit a 10 μm feature with sharp cutoffs between about 9 μm and 12 μm, which create a broad flat plateau. Amorphous phases, when present, smooth the sharp emission features, resulting in a dome-like shape. Preliminary results indicate that the surfaces of analyzed Trojans contain primarily amorphous silicates. Emissivity spectra of asteroids 1986 WD and 4709 Ennomos include small peaks in the 10 μm region, diagnostic of small amounts of crystalline olivine. One explanation is that Trojans formed in the same region as Kuiper Belt objects, and when giant planet migration ensued, they were swept into Jupiter’s stable Lagrange points where they are found today. As such, it is possible that an ancestral group of Kuiper Belt

  11. Solid phase transformations

    CERN Document Server

    Čermák, J

    2008-01-01

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

  12. 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.

  13. Barium silicates as high thermal expansion seals for solid oxide fuel cells studied by high-temperature X-ray diffraction (HT-XRD)

    Science.gov (United States)

    Kerstan, Marita; Rüssel, Christian

    Gas-tight seals between metals and ceramics in solid-oxide fuel cells can be fabricated from glasses which enable the crystallization of phases with high thermal expansion coefficients (mostly barium silicates). This article mainly reports on high-temperature X-ray diffraction studies on these silicates. It is shown that all barium silicates exhibit thermal expansion coefficients in the range from 10.5 to 15.4 × 10 -6 K -1 (100-800 °C). The expansions are strongly dependent on the respective crystallographic axis. The ortho- and metasilicates exhibit the largest thermal expansion coefficients. The coefficient of thermal expansion of a sealing glass is attributed to the thermal expansion of the crystalline phases and the residual glassy phase. The phase formation should carefully be controlled also with respect to aging. Crystalline phases with high coefficients of thermal expansion, such as the barium silicates, are advantageous as components in such sealing glasses.

  14. Solid phases of tenoxicam.

    Science.gov (United States)

    Cantera, Rodrigo G; Leza, María G; Bachiller, Carmen M

    2002-10-01

    In this report we describe the preparation and characterization of four polymorphic forms of tenoxicam; they are, three 1:1 stoichiometric solvates with acetonitrile, dioxane, and N,N-dimethylformamide, and an amorphous phase obtained by recrystallization in various solvents. Polymorph IV and solvates with dioxane and N,N-dimethylformamide are reported for the first time in this paper. In addition, three solvates were crystallized in acetone, ethyl acetate, and isopropyl alcohol. These solid forms were characterized by X-ray powder diffraction, differential scanning calorimetry, infrared spectroscopy, thermogravimetry, optical microscopy, and elemental analysis. Solid-state properties, intrinsic dissolution rate, and dissolution kinetics from formulated tablets are also provided. Copyright 2002 Wiley-Liss Inc. and the American Pharmaceutical Association

  15. 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.

  16. 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

  17. Activity of NaOH buffered by silicate solids in molten sodium acetate-water at 3170C

    International Nuclear Information System (INIS)

    Weres, O.; Tsao, L.

    1988-01-01

    Silica and sodium acetate are present in the steam generator tube sheet crevices of many nuclear power plants. Trace solutes in the condensate are tremendously concentrated in the crevices by boiling. Sparingly soluble sodium silicates and other solids precipitate from the crevice liquid leaving an extremely concentrated molten mixture of water, sodium acetate and other salts. The precipitates buffer the activity of sodium hydroxide in the superheated liquid that remains. The activity of NaOH corresponding to the buffers quartz/sodium disilicate and sodium disilicate/sodium metasilicate at 317 0 C has been determined experimentally. The sodium hydroxide content of a sodium acetate-water melt buffered by these reactions was determined by chemical analysis, and the corresponding activity of NaOH at temperature was calculated using the recently published Pitzer-Simonson Model of molten salt-water mixtures. The molten mixture of sodium acetate and water plays the role solvent in these experiments and calculations. The free energies of formation of solid sodium silicates at 317 0 C were also determined. The activity of NaOH corresponding to other silicate and phosphate buffers was calculated using published thermodynamic data and estimated from phase diagrams

  18. Polymer Derived Rare Earth Silicate Nanocomposite Protective Coatings for Nuclear Thermal Propulsion Systems, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — Leveraging a rapidly evolving state-of-the-art technical base empowered by Phase I NASA SBIR funding, NanoSonic's polymer derived rare earth silicate EBCs will...

  19. Polymer Derived Rare Earth Silicate Nanocomposite Protective Coatings for Nuclear Thermal Propulsion Systems, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — The objective of this Phase I SBIR program is to develop polymer derived rare earth silicate nanocomposite environmental barrier coatings (EBC) for providing...

  20. 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....

  1. Application of spherical silicate to prepare solid dispersion dosage forms with aqueous polymers.

    Science.gov (United States)

    Nagane, Kentaro; Kimura, Susumu; Ukai, Koji; Takahashi, Chisato; Ogawa, Noriko; Yamamoto, Hiromitsu

    2015-09-30

    The objective of this study is to prepare and characterize solid dispersions of nifedipine (NP) using porous spherical silicate micro beads (MB) that were approximately 100 μm in diameter with vinylpyrrolidone/vinyl acetate copolymer (PVP/VA) and a Wurster-type fluidized bed granulator. Compared with previously reported solid dispersion using only MB, the supersaturation of NP dissolved from the proposed system of MB and PVP/VA was maintained during dissolution tests. The proposed system produced a solid dispersion product coated on MB, and morphology was maintained after the coating process to prepare solid dispersion; therefore, the powder characteristics, such as flowability of the proposed solid dispersion product, was tremendously preferable to that of the conventional spray-dried solid dispersions of NP with PVP/VA, expecting to make the consequent manufacturing processes easy for development. Another advantage in the terms of manufacturing is its simple process to prepare solid dispersion by spraying the drug and polymer that were dissolved in an organic solvent onto a MB in a Wurster-type fluidized bed granulator, thus, simplifying the optimization and scale-up with ease. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. 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.

  3. Solid Phase Characterization of Solids Recovered from Failed Sluicer Arm

    Energy Technology Data Exchange (ETDEWEB)

    Cooke, Gary A. [Hanford Site (HNF), Richland, WA (United States)

    2015-03-09

    The Enclosure to this memo discusses the solid phase characterization of a solid sample that was retrieved from the single-shell Tank 241-C-111 extended reach sluicer #2. This sluicer, removed from riser #3 on September 25, 2014, was found to have approximately 0.4 gallons of solid tank waste adhering to the nozzle area.

  4. Physical mineralogy of (Ca,Al)-rich silicate phases of the Earth's mantle. Geodynamic implications

    International Nuclear Information System (INIS)

    Gautron, Laurent

    2008-01-01

    bottom heating of the big domes observed in the cross sections of the mantle obtained by seismic tomography. The possible relation between our results from mineral physics and the volume of 'hot' materials present at the bottom of the mantle, is also discussed. The second silicate phase bearing Ca and Al presented in this thesis is the new high pressure phase named CAS phase of composition CaAl 4 Si 2 O 11 . After many experimental studies performed at high pressure on basaltic crust assemblage, it is now commonly accepted that the CAS phase is one of the main mineral phases present in the oceanic crust (Mid-Ocean Ridge Basalt, MORB) subducted to the lowermost lower mantle. The CAS phase is shown to be one of the last solid residual phases (with Ca-perovskite) when the oceanic crust is partially molten, as expected when this crust reaches the D'' region. Here, we show that the CAS phase bears an iso-symmetrical transition where some silicon atoms adopt a coordination 5, in the trigonal bipyramidal site (2 face-sharing tetrahedra). The implications of such intermediate coordination (between coordinations 4 and 6) is discussed in terms of diffusion processes, diffusion creep deformation, viscosity: it appears that the formation of SiO 5 groups strongly favours the deformation properties of these materials, and then enhances their transport properties. It is clear that the coordination of silicon atoms could have a strong direct effect on the dynamic processes occurring in the deep mantle. With the two studies presented in this thesis, we see that experimental mineral physics can provide essential data for models in geodynamics, thermal behaviour and in seismology. Seismic waves give data about the structure of the deep Earth and the density profile, while experimental geodynamics reproduce the rheological behaviour of the mantle with appropriate fluids and a bottom heating: it is then important to provide complementary data about the Earth materials. The study of the CAS

  5. Effect of phase composition of calcium silicate phosphate component on properties of brushite based composite cements

    Energy Technology Data Exchange (ETDEWEB)

    Sopcak, T., E-mail: tsopcak@imr.saske.sk [Institute of Materials Research of SAS, Watsonova 47, 04001 Kosice (Slovakia); Medvecky, L.; Giretova, M.; Stulajterova, R.; Durisin, J. [Institute of Materials Research of SAS, Watsonova 47, 04001 Kosice (Slovakia); Girman, V. [Institute of Physics, Faculty of Science, P. J. Šafárik University, Park Angelinum 9, 04001 Kosice (Slovakia); Faberova, M. [Institute of Materials Research of SAS, Watsonova 47, 04001 Kosice (Slovakia)

    2016-07-15

    The composite cement mixtures were prepared by mixing brushite (B) with, the amorphous hydrated calcium silicate phosphate (CSPH) or annealed calcium silicate phosphate (CSP composed of Si-saturated hydroxyapatite, wollastonite and silica) phases and water as liquid component. The contents of the silicate-phosphate phase in composites were 10.30 and 50 wt%. The significant effect of both the Ca/P ratio and different solubility of calcium silicate phosphate component in starting cement systems on setting time and phase composition of the final composite cements was demonstrated. The compressive strength of the set cements increased with the filler addition and the highest value (~ 48 MPa) exhibited the 50CSP/B cement composite. The final setting times of the composite cements decreased with the CSPH addition from about 25 to 17 min in 50CSHP/B and setting time of CSP/B composites was around 30 min. The higher content of silica in cements caused the precipitation of fine hydroxyapatite particles in the form of nanoneedles or thin plates perpendicularly oriented to sample surface. The analysis of in vitro cement cytotoxicity demonstrated the strong reduction in cytotoxicity of 10CSPH/B composite with time of cultivation (a low cytotoxicity after 9 days of culture) contrary to cements with higher calcium silicate-phosphate content. These results were attributed to the different surface topography of composite substrates and possible stimulation of cell proliferation by the slow continuously release of ions from 10CSPH/B cement. - Highlights: • Ca/P ratio and solubility of calcium silicate-phosphate components affect the self-setting properties of cements. • Strong relationship between the composite in vitro cytotoxicity and surface microtopography was demonstrated. • Plate-like morphology of coarser particles allowed cells to better adhere and proliferate as compared with nanoneedles.

  6. Thermogravimetric analysis of phase transitions in cement compositions mixed by sodium silicate solution

    Directory of Open Access Journals (Sweden)

    Fedosov Sergey Viktorovich

    2014-01-01

    Full Text Available This paper presents a study of the capability to modify cement by mechanical activation of sodium silicate water solution. Admixtures or blends of binding agents were employed for modifying concrete properties. The liquid glass is applied to protect from chemically or physically unfavorable environmental impacts, such as acidic medium and high temperature. The sodium silicate is a high-capacity setting accelerator. The increasing of the liquid glass proportion in the mix leads to the degradation of the cement paste plasticity and for this reason it is necessary to reduce the amount of liquid glass in the cement paste. The activation of dilute water solution of sodium silicate into rotary pulsating apparatus directly before tempering of the cement paste is an effective way to decrease mass fraction of liquid glass in the cement paste. The results of the combined influence of liquid glass and mechanical activation on physicochemical processes taking place in cement stone are represented in this research. Thermogravimetric analysis was used in order to study cement blends. Thermogravimetric analysis of modified cement stone assays was performed by thermo analyzer SETARAM TGA 92-24. The results of the analysis of phase transition taking place under high-temperature heating of cement stone modified by the mechanical activation of the water solution of the sodium silicate were introduced. Thermograms of cement stone assays were obtained at different hardening age. The comparison of these thermograms allows us to come to a conclusion on the formation and the retention during long time of a more dense structure of the composite matrix mixed by the mechanical activation of sodium silicate water solution. The relation between the concrete composition and its strength properties was stated. Perhaps, the capability of modified concrete to keep calcium ions in sparingly soluble hydrosilicates leads to the increase in its durability and corrosion resistance.

  7. Development of novel tricalcium silicate-based endodontic cements with sintered radiopacifier phase.

    Science.gov (United States)

    Xuereb, M; Sorrentino, F; Damidot, D; Camilleri, Josette

    2016-06-01

    All implants, bone and endodontic cements need to be sufficiently radiopaque to be able to be distinguished from neighbouring anatomical structures post-operatively. For this purpose, radiopacifying materials are added to the cements to render them sufficiently radiopaque. Bismuth oxide has been quite a popular choice of radiopacifier in endodontic materials. It has been shown to cause dental discoloration. The aim of this study was to develop, characterize and assess the properties of tricalcium silicate cement with alternative radiopacifiers, which are either inter-ground or sintered to the tricalcium silicate cement. Custom-made endodontic cements based on tricalcium silicate and 20 % barium, calcium or strontium zirconate, which were either inter-ground or sintered at high temperatures, were produced. The set materials stored for 28 days in Hank's balanced salt solution were characterized by scanning electron microscopy and X-ray diffraction analysis. Assessment of pH, leaching, interaction with physiological solution, radiopacity, setting time, compressive strength and material porosity were investigated. Mineral trioxide aggregate (MTA) Angelus was used as control. Addition of radiopacifying materials improved the radiopacity of the material. The sintered cements exhibited the formation of calcium zirconate together with the respective radiopacifier phase. All materials produced calcium hydroxide on hydration, which interacted with tissue fluids forming hydroxyapatite on the material surface. The physical properties of the tricalcium silicate-based cements were comparable to MTA Angelus. A novel method of producing radiopaque tricalcium silicate-based cements was demonstrated. The novel materials exhibited properties, which were either comparable or else improved over the control. The novel materials can be used to replace MTA for root-end filling, perforation repair and other clinical applications where MTA is indicated.

  8. Carbonate formation in non-aqueous environments by solid-gas carbonation of silicates

    Science.gov (United States)

    Day, S. J.; Thompson, S. P.; Evans, A.; Parker, J. E.

    2012-02-01

    We have produced synthetic analogues of cosmic silicates using the Sol Gel method, producing amorphous silicates of composition Mg(x)Ca(1-x)SiO3. Using synchrotron X-ray powder diffraction on Beamline I11 at the Diamond Light Source, together with a newly-commissioned gas cell, real-time powder diffraction scans have been taken of a range of silicates exposed to CO2 under non-ambient conditions. The SXPD is complemented by other techniques including Raman and Infrared Spectroscopy and SEM imaging.

  9. 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...

  10. Europium doped di-calcium magnesium di-silicate orange–red emitting phosphor by solid state reaction method

    Directory of Open Access Journals (Sweden)

    Ishwar Prasad Sahu

    2015-07-01

    Full Text Available A new orange–red europium doped di-calcium magnesium di-silicate (Ca2MgSi2O7:Eu3+ phosphor was prepared by the traditional high temperature solid state reaction method. The prepared Ca2MgSi2O7:Eu3+ phosphor was characterized by X-ray diffractometer (XRD, transmission electron microscopy (TEM, field emission scanning electron microscopy (FESEM with energy dispersive x-ray spectroscopy (EDX, fourier transform infrared spectra (FTIR, photoluminescence (PL and decay characteristics. The phase structure of sintered phosphor was akermanite type structure which belongs to the tetragonal crystallography with space group P4¯21m, this structure is a member of the melilite group and forms a layered compound. The chemical composition of the sintered Ca2MgSi2O7:Eu3+ phosphor was confirmed by EDX spectra. The PL spectra indicate that Ca2MgSi2O7:Eu3+ can be excited effectively by near ultraviolet (NUV light and exhibit bright orange–red emission with excellent color stability. The fluorescence lifetime of Ca2MgSi2O7:Eu3+ phosphor was found to be 28.47 ms. CIE color coordinates of Ca2MgSi2O7:Eu3+ phosphor is suitable as orange-red light emitting phosphor with a CIE value of (X = 0.5554, Y = 0.4397. Therefore, it is considered to be a new promising orange–red emitting phosphor for white light emitting diode (LED application.

  11. Enhanced enamel benefits from a novel toothpaste and dual phase gel containing calcium silicate and sodium phosphate salts.

    Science.gov (United States)

    Hornby, Kate; Ricketts, Stephen R; Philpotts, Carole J; Joiner, Andrew; Schemehorn, Bruce; Willson, Richard

    2014-06-01

    To investigate the enamel health benefits of a novel toothpaste and a dual phase gel containing calcium silicate, sodium phosphate and fluoride. Enamel demineralisation was assessed using two pH cycling protocols with either lactic acid or citric acid as the acid challenge. Remineralisation of lactic acid softened and citric acid softened enamel was assessed using a number of protocols. All demineralisation and remineralisation evaluation was by surface microhardness measurements. The novel calcium silicate/phosphate fluoride toothpaste inhibited enamel demineralisation to a significantly (pcalcium silicate/phosphate fluoride toothpaste also showed significant (pcalcium silicate/phosphate fluoride dual phase gel provided enhanced remineralisation of citric acid softened enamel compared to fluoride and non-fluoride controls. These studies show that formulations containing calcium silicate, sodium phosphate salts and fluoride provide enhanced enamel demineralisation and remineralisation in vitro benefits. The novel oral care formulations containing calcium silicate, sodium phosphate salts and fluoride is a new approach to the protection of enamel from acid attacks and the repair of demineralised enamel, leading to increased dental hard tissue benefits. © 2014 Elsevier Ltd. All rights reserved.

  12. Mesoporous VN prepared by solid-solid phase separation

    Energy Technology Data Exchange (ETDEWEB)

    Yang Minghui, E-mail: m.yang@cornell.edu [Department of Chemistry, Cornell University, Ithaca, New York 14853-1301 (United States); Ralston, Walter T. [Department of Chemistry, Cornell University, Ithaca, New York 14853-1301 (United States); Tessier, Franck [UMR CNRS 6226 ' Sciences Chimiques de Rennes' , Equipe ' Verres et Ceramiques' , Universite de Rennes 1, F-35042 Rennes cedex (France); Allen, Amy J. [Department of Chemistry, Cornell University, Ithaca, New York 14853-1301 (United States); DiSalvo, Francis J., E-mail: fjd3@cornell.edu [Department of Chemistry, Cornell University, Ithaca, New York 14853-1301 (United States)

    2013-01-15

    We recently reported a simple route to prepare mesoporous, conducting nitrides from Zn containing ternary transition metal oxides. Those materials result from the condensation of atomic scale voids created by the loss of Zn by evaporation, the replacement of 3 oxygen anions by 2 nitrogen anions, and in most cases the loss of oxygen to form water on the reduction of the transition metal. In this report, we present a different route to prepare mesoporous VN from K containing vanadium oxides. In this case, ammonolysis results in a multiphase solid product that contains VN, and other water soluble compounds such as KOH or KNH{sub 2}. On removing the K containing products by washing with degassed water, only mesoporous VN remains. VN materials with different pore sizes (10 nm-20 nm) were synthesized at 600 Degree-Sign C by varying the reaction time, while larger pores are obtained at higher temperatures (50 nm at 800 Degree-Sign C). - Graphical Abstract: The synthesis process of mesoporous VN from solid-solid separation. Highlights: Black-Right-Pointing-Pointer Mesoporous VN has been prepared by solid-solid phase separation. Black-Right-Pointing-Pointer Mesoporous VN was characterized by Rietveld refinement of PXRD, SEM and nitrogen physisorption. Black-Right-Pointing-Pointer VN materials with different pore sizes (10 nm-50 nm) were synthesized.

  13. 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).

  14. 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

  15. Ternary Phase-Separation Investigation of Sol-Gel Derived Silica from Ethyl Silicate 40

    Science.gov (United States)

    Wang, Shengnan; Wang, David K.; Smart, Simon; Diniz da Costa, João C.

    2015-01-01

    A ternary phase-separation investigation of the ethyl silicate 40 (ES40) sol-gel process was conducted using ethanol and water as the solvent and hydrolysing agent, respectively. This oligomeric silica precursor underwent various degrees of phase separation behaviour in solution during the sol-gel reactions as a function of temperature and H2O/Si ratios. The solution composition within the immiscible region of the ES40 phase-separated system shows that the hydrolysis and condensation reactions decreased with decreasing reaction temperature. A mesoporous structure was obtained at low temperature due to weak drying forces from slow solvent evaporation on one hand and formation of unreacted ES40 cages in the other, which reduced network shrinkage and produced larger pores. This was attributed to the concentration of the reactive sites around the phase-separated interface, which enhanced the condensation and crosslinking. Contrary to dense silica structures obtained from sol-gel reactions in the miscible region, higher microporosity was produced via a phase-separated sol-gel system by using high H2O/Si ratios. This tailoring process facilitated further condensation reactions and crosslinking of silica chains, which coupled with stiffening of the network, made it more resistant to compression and densification. PMID:26411484

  16. 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

  17. 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.

  18. Magnetic in-tube solid phase microextraction.

    Science.gov (United States)

    Moliner-Martínez, Y; Prima-Garcia, Helena; Ribera, Antonio; Coronado, Eugenio; Campíns-Falcó, P

    2012-08-21

    We report a new in-tube solid phase microextraction approach named magnetic in-tube solid phase microextraction, magnetic-IT-SPME. Magnetic-IT-SPME has been developed, taking advantage of magnetic microfluidic principles with the aim to improve extraction efficiency of IT-SPME systems. First, a magnetic hybrid material formed by Fe(3)O(4) nanoparticles supported on SiO(2) was synthesized and immobilized in the surface of a bared fused silica capillary column to obtain a magnetic adsorbent extraction phase. The capillary column was placed inside a magnetic coil that allowed the application of a variable magnetic field. Acetylsalicylic acid, acetaminophen, atenolol, diclofenac, and ibuprofen were tested as target analytes. The application of a controlled magnetic field resulted in quantitative extraction efficiencies of the target analytes between 70 and 100%. These results demonstrated that magnetic forces solve the low extraction efficiency (10-30%) of IT-SPME systems, which is one of their main drawbacks.

  19. Mineral CO2 sequestration in basalts and ultra-basic rocks: impact of secondary silicated phases on the carbonation process

    International Nuclear Information System (INIS)

    Sissmann, Olivier

    2013-01-01

    The formation of carbonates constitutes a stable option for carbon dioxide (CO 2 ) geological sequestration, and is prone to play a significant role in reducing emissions of anthropic origin. However, our comprehension of the carbonation mechanism, as well as of the kinetics limitations encountered during this chemical reaction, remains poorly developed. Though there is a large number of studies focusing on the dissolution kinetics of basic silicates and on the precipitation of carbonates, few have inquired about the impact that the formation of non-carbonated secondary phases can have on these reaction's kinetics. It is the approach chosen here, as only solid knowledge of the global carbonation mechanism can make this process predictive and efficient. Experimental data on dissolution and carbonation have therefore been determined in batch reactors, on relevant minerals and rocks. Firstly, we studied the carbonation of olivine (a major phase within peridotites and minor within basalts) at 90 deg. C and under pCO 2 of 280 bars. The dissolution of San Carlos olivine (Mg 1.76 Fe 0.24 SiO 4 ) is slowed down by the formation of a surface silica gel, when the fluid reaches equilibrium with amorphous silica. The transport of species to the reactive medium becomes the limiting step of the process, slowing down the dissolution process of San Carlos olivine by 5 orders of magnitude. However, this passivation doesn't occur during the alteration of Ca-olivine (Ca 2 SiO 4 ), though a surface silica layer does form. This comparison suggests that it isn't the structure of the silicate but its chemical composition, which controls the transport properties through the interfacial layer. The second part explores the effects of organic ligands and of temperature variations on the formation of those phases. The addition of citrate at 90 deg. C increases the kinetics of San Carlos olivine by one order of magnitude, and allows the release of enough Mg in the aqueous medium to form

  20. Solid-phase equilibria on Pluto's surface

    Science.gov (United States)

    Tan, Sugata P.; Kargel, Jeffrey S.

    2018-03-01

    Pluto's surface is covered by volatile ices that are in equilibrium with the atmosphere. Multicomponent phase equilibria may be calculated using a thermodynamic equation of state and, without additional assumptions, result in methane-rich and nitrogen-rich solid phases. The former is formed at temperature range between the atmospheric pressure-dependent sublimation and condensation points, while the latter is formed at temperatures lower than the sublimation point. The results, calculated for the observed 11 μbar atmospheric pressure and composition, are consistent with recent work derived from observations by New Horizons.

  1. Solid phase synthesis of purines from pyrimidines.

    Science.gov (United States)

    Di Lucrezia, R; Gilbert, I H; Floyd, C D

    2000-01-01

    In this paper the solid phase synthesis of various substituted purines is described starting from 4,6-dichloro-5-nitropyrimidine. The 4,6-dichloro-5-nitropyrimidine was coupled to Rink amide resin followed by displacement of the second chloride by an amino compound. Reduction of the nitro compound proved to be problematic but was achieved using lithium aluminum hydride/aluminum trichloride. The diamines (13) were then elaborated to purines by three different routes.

  2. DNA Extraction: Organic and Solid-Phase.

    Science.gov (United States)

    Altayari, Wafa

    2016-01-01

    DNA extraction remains a critical step in DNA profiling of biological material recovered from scenes of crime. In the forensic community several methods have gained popularity, including Chelex(®), organic extraction, and solid-phase extraction. While some laboratories streamlined their processes and only use one method we have retained several methods and continue to use these for different sample types. In this chapter we present three methods that have been used for several years in our laboratory.

  3. 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)

  4. Solid-state autocatalysis and oscillatory reactions in silicate glass systems

    DEFF Research Database (Denmark)

    Canning, John; Sørensen, Henrik Rokkjær; Kristensen, Martin

    2006-01-01

    We report the first demonstration of autocatalysis and oscillatory behaviour in the solid-state where no decomposition process is involved. Our material system is solid-state silica glass impregnated with hydrogen. It is at the heart of photosensitivity in glass-based optical waveguides and devic...

  5. The role of medium range order on phase transitions in chain silicates upon compression

    International Nuclear Information System (INIS)

    Serghiou, G; Chopelas, A; Boehler, R

    2004-01-01

    Raman spectroscopic measurements of the tetrahedrally coordinated crystal MnSiO 3 (rhodonite) in an argon pressure medium show that it becomes amorphous above 33 GPa. This observation consolidates our findings and explanation for the global structural trends exhibited by the extended chain silicate family AA'BO 3 (AA': Mg, Ca, Mn, Fe; B: Si) upon compression. In particular, crystals of this family are made of two types of building blocks coined P and C. Those crystals comprised solely of P blocks transform to dense higher coordinated crystalline phases; those comprised of P and C blocks, such as MnSiO 3 rhodonite, become amorphous; whereas those comprised solely of C blocks show both crystalline and amorphous regions upon compression. The reason that this medium range order length scale (building block scale) classification is correlated with the type of transitions taking place upon compression is due to the instability of C blocks and C-P interfaces with respect to P blocks and P-P interfaces at high pressures

  6. Polymer Derived Yttrium Silicate Ablative TPS Materials for Next-Generation Exploration Missions, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Through the proposed NASA SBIR program, NanoSonic will optimize its HybridSil® derived yttrium silicates to serve as next-generation reinforcement for carbon and...

  7. Analyses and predictions of the thermodynamic properties and phase diagrams of silicate systems

    Energy Technology Data Exchange (ETDEWEB)

    Blander, M. [Argonne National Lab., IL (United States); Pelton, A.; Eriksson, G. [Ecole Polytechnique, Montreal, PQ (Canada). Dept. of Metallurgy and Materials Engineering

    1992-07-01

    Molten silicates are ordered solutions which can not be well represented by the usual polynomial representation of deviations from ideal solution behavior (i.e. excess free energies of mixing). An adaptation of quasichemical theory which is capable of describing the properties of ordered solutions represents the measured properties of binary silicates over broad ranges of composition and temperature. For simple silicates such as the MgO-FeO-SiO{sub 2} ternary system, in which silica is the only acid component, a combining rule generally leads to good predictions of ternary solutions from those of the binaries. In basic solutions, these predictions are consistent with those of the conformal ionic solution theory. Our results indicate that our approach could provide a potentially powerful tool for representing and predicting the properties of multicomponent molten silicates.

  8. Analyses and predictions of the thermodynamic properties and phase diagrams of silicate systems

    Energy Technology Data Exchange (ETDEWEB)

    Blander, M. (Argonne National Lab., IL (United States)); Pelton, A.; Eriksson, G. (Ecole Polytechnique, Montreal, PQ (Canada). Dept. of Metallurgy and Materials Engineering)

    1992-01-01

    Molten silicates are ordered solutions which can not be well represented by the usual polynomial representation of deviations from ideal solution behavior (i.e. excess free energies of mixing). An adaptation of quasichemical theory which is capable of describing the properties of ordered solutions represents the measured properties of binary silicates over broad ranges of composition and temperature. For simple silicates such as the MgO-FeO-SiO{sub 2} ternary system, in which silica is the only acid component, a combining rule generally leads to good predictions of ternary solutions from those of the binaries. In basic solutions, these predictions are consistent with those of the conformal ionic solution theory. Our results indicate that our approach could provide a potentially powerful tool for representing and predicting the properties of multicomponent molten silicates.

  9. Directed gas phase formation of silicon dioxide and implications for the formation of interstellar silicates.

    Science.gov (United States)

    Yang, Tao; Thomas, Aaron M; Dangi, Beni B; Kaiser, Ralf I; Mebel, Alexander M; Millar, Tom J

    2018-02-22

    Interstellar silicates play a key role in star formation and in the origin of solar systems, but their synthetic routes have remained largely elusive so far. Here we demonstrate in a combined crossed molecular beam and computational study that silicon dioxide (SiO 2 ) along with silicon monoxide (SiO) can be synthesized via the reaction of the silylidyne radical (SiH) with molecular oxygen (O 2 ) under single collision conditions. This mechanism may provide a low-temperature path-in addition to high-temperature routes to silicon oxides in circumstellar envelopes-possibly enabling the formation and growth of silicates in the interstellar medium necessary to offset the fast silicate destruction.

  10. 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.

  11. 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...

  12. Orange-red emitting europium doped strontium ortho-silicate phosphor prepared by a solid state reaction method.

    Science.gov (United States)

    Sahu, Ishwar Prasad

    2017-05-01

    In the present article we report europium-doped strontium ortho-silicates, namely Sr 2 SiO 4 :xEu 3+ (x = 1.0, 1.5, 2.0, 2.5 or 3.0 mol%) phosphors, prepared by solid state reaction method. The crystal structures of the sintered phosphors were consistent with orthorhombic crystallography with a Pmna space group. The chemical compositions of the sintered phosphors were confirmed by energy dispersive X-ray spectroscopy (EDS). Thermoluminescence (TL) kinetic parameters such as activation energy, order of kinetics and frequency factors were calculated by the peak shape method. Orange-red emission originating from the 5 D 0 - 7 F J (J = 0, 1, 2, 3) transitions of Eu 3+ ions could clearly be observed after samples were excited at 395 nm. The combination of these emissions constituted orange-red light as indicated on the Commission Internationale de l'Eclairage (CIE) chromaticity diagram. Mechanoluminescence (ML) intensity of the prepared phosphor increased linearly with increasing impact velocity of the moving piston that suggests that these phosphors can also be used as sensors to detect the stress of an object. Thus, the present investigation indicates that the piezo-electricity was responsible for producing ML in the prepared phosphor. Copyright © 2016 John Wiley & Sons, Ltd.

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

    African Journals Online (AJOL)

    aminopropyl-modified silica SPE cartridge, and thereafter determined by reverse phase high ... Keywords: Synthetic colors, Food, Fruit flavored drinks, Solid phase extraction, RP-HPLC ..... by thin-layer chromatography-fast atom bombardment.

  14. Thermal properties and application of potential lithium silicate breeder materials

    International Nuclear Information System (INIS)

    Skokan, A.; Wedemeyer, H.; Vollath, D.; Gunther, E.

    1987-01-01

    Phase relations, thermal stability and preparation methods of the Li 2 O-rich silicates Li 8 SiO 6 and ''Li 6 SiO 5 '' have been investigated experimentally, the application of these compounds as solid breeder materials is discussed. In the second part of this contribution, the results of thermal expansion measurements on the silicates Li 2 SiO 3 , Li 4 SiO 4 and Li 8 SiO 6 are presented

  15. Thermal properties and application of potential lithium silicate breeder materials

    International Nuclear Information System (INIS)

    Skokan, A.; Wedemeyer, H.; Vollath, D.; Guenther, E.

    1986-01-01

    Phase relations, thermal stability and preparation methods of the Li 2 O-rich silicates Li 8 SiO 6 and 'Li 6 SiO 5 ' have been investigated experimentally, the application of these compounds as solid breeder materials is discussed. In the second part of this contribution, the results of thermal expansion measurements on the silicates Li 2 SiO 3 , Li 4 SiO 4 and Li 8 SiO 6 are presented. (author)

  16. Study on the Solid Phase Extraction and Spectrophotometric ...

    African Journals Online (AJOL)

    NJD

    By solid phase extraction of the. Hg(II)-ABTR chelate with a C18 disk, an enrichment factor of 50 was achieved. Combining the new reagent with solid phase extraction allowed the development of a highly sensitive, selective and rapid method for the determination of mercury in water and biological samples. 2. Experimental.

  17. 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 ... Solid phase extraction is recognized as the most common sample pre- treatment technique to enhance the concentration of a target in biological samples. [17]. The aim ... pure water (solvent B) in HPLC experiment. The.

  18. Petrophysical Analysis of Siliceous Ooze Sediments, Ormen Lange Field, Norway

    DEFF Research Database (Denmark)

    Awedalkarim, Ahmed; Fabricius, Ida Lykke

    structure is complex and the solids are mechanically fragile and hydrous. Normal petrophysical methods used in formation evaluation might not be suitable for interpreting siliceous ooze. For example, density and neutron logging tools are calibrated to give correct porosity readings in a limestone formation...... present in the solid. Some minerals of siliceous ooze, such as opal, have hydrogen in their structures which influences the measured hydrogen index (HI). The neutron tool obtains the combined signal of the HI of the solid phase and of the water that occupies the true porosity. The HI is equal to true...

  19. Obtaining calcium silicates by using solid residues as precursors. Influence of water in the process of mixing reagents; Obtencin de silicatos de calcio empleando como precursores residuos solidos. Influencia del mezclado de reactivos en fase seca o fase humeda

    Energy Technology Data Exchange (ETDEWEB)

    Felipe-Sese, M.; Eliche-Quesada, D.; Corpas-Iglesias, F. A.

    2011-07-01

    The suitability of re-using residues marble, remaining from cutting marble, as a source of calcium-oxide, as well as the resultant ashes from the combustion of the wastes generated in the process of manufacturing boards from derivates of wood, as a source of silica, as raw material for the production of calcium silicate products has been determined. First of all, the influence of water has been studied in the initial phase of mixing residues. Marble and ashes have been mixed in molar relation CaO:SiO{sub 2} of 1:1 using two different ways: using a planetary ball mill (while in solid state) or agitating at 90 degree centigrade (2 h) using a 60 wt% of water (while in humid state). Later, both mixtures were sintered at 1100 degree centigrade (24 h). In order to use the obtained calcium-silicates as ceramic insulating thermal materials, the samples were compressed at 15 Tm obtaining bricks from which the technological properties have been studied. The ceramic materials obtained from mixing the residues in dry phase, as well as those obtained in the wet phase, can be used as thermal insulators, showing values of conductivity of 0.18 and 0.12 w/m{sup 2}K, with an elevated resistance to compressive strength. (Author) 14 refs.

  20. Air sampling with solid phase microextraction

    Science.gov (United States)

    Martos, Perry Anthony

    There is an increasing need for simple yet accurate air sampling methods. The acceptance of new air sampling methods requires compatibility with conventional chromatographic equipment, and the new methods have to be environmentally friendly, simple to use, yet with equal, or better, detection limits, accuracy and precision than standard methods. Solid phase microextraction (SPME) satisfies the conditions for new air sampling methods. Analyte detection limits, accuracy and precision of analysis with SPME are typically better than with any conventional air sampling methods. Yet, air sampling with SPME requires no pumps, solvents, is re-usable, extremely simple to use, is completely compatible with current chromatographic equipment, and requires a small capital investment. The first SPME fiber coating used in this study was poly(dimethylsiloxane) (PDMS), a hydrophobic liquid film, to sample a large range of airborne hydrocarbons such as benzene and octane. Quantification without an external calibration procedure is possible with this coating. Well understood are the physical and chemical properties of this coating, which are quite similar to those of the siloxane stationary phase used in capillary columns. The log of analyte distribution coefficients for PDMS are linearly related to chromatographic retention indices and to the inverse of temperature. Therefore, the actual chromatogram from the analysis of the PDMS air sampler will yield the calibration parameters which are used to quantify unknown airborne analyte concentrations (ppb v to ppm v range). The second fiber coating used in this study was PDMS/divinyl benzene (PDMS/DVB) onto which o-(2,3,4,5,6- pentafluorobenzyl) hydroxylamine (PFBHA) was adsorbed for the on-fiber derivatization of gaseous formaldehyde (ppb v range), with and without external calibration. The oxime formed from the reaction can be detected with conventional gas chromatographic detectors. Typical grab sampling times were as small as 5 seconds

  1. Solid oxide fuel cells with apatite-type lanthanum silicate-based electrolyte films deposited by radio frequency magnetron sputtering

    Science.gov (United States)

    Liu, Yi-Xin; Wang, Sea-Fue; Hsu, Yung-Fu; Wang, Chi-Hua

    2018-03-01

    In this study, solid oxide fuel cells (SOFCs) containing high-quality apatite-type magnesium doped lanthanum silicate-based electrolyte films (LSMO) deposited by RF magnetron sputtering are successfully fabricated. The LSMO film deposited at an Ar:O2 ratio of 6:4 on an anode supported NiO/Sm0.2Ce0·8O2-δ (SDC) substrate followed by post-annealing at 1000 °C reveals a uniform and dense c-axis oriented polycrystalline structure, which is well adhered to the anode substrate. A composite SDC/La0·6Sr0·4Co0·2Fe0·8O3-δ cathode layer is subsequently screen-printed on the LSMO deposited anode substrate and fired. The SOFC fabricated with the LSMO film exhibits good mechanical integrity. The single cell with the LSMO layer of ≈2.8 μm thickness reports a total cell resistance of 1.156 and 0.163 Ωcm2, open circuit voltage of 1.051 and 0.982 V, and maximum power densities of 0.212 and 1.490 Wcm-2 at measurement temperatures of 700 and 850 °C, respectively, which are comparable or superior to those of previously reported SOFCs with yttria stabilized zirconia electrolyte films. The results of the present study demonstrate the feasibility of deposition of high-quality LSMO films by RF magnetron sputtering on NiO-SDC anode substrates for the fabrication of SOFCs with good cell performance.

  2. 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.

  3. Solid lubrication design methodology, phase 2

    Science.gov (United States)

    Pallini, R. A.; Wedeven, L. D.; Ragen, M. A.; Aggarwal, B. B.

    1986-01-01

    The high temperature performance of solid lubricated rolling elements was conducted with a specially designed traction (friction) test apparatus. Graphite lubricants containing three additives (silver, phosphate glass, and zinc orthophosphate) were evaluated from room temperature to 540 C. Two hard coats were also evaluated. The evaluation of these lubricants, using a burnishing method of application, shows a reasonable transfer of lubricant and wear protection for short duration testing except in the 200 C temperature range. The graphite lubricants containing silver and zinc orthophosphate additives were more effective than the phosphate glass material over the test conditions examined. Traction coefficients ranged from a low of 0.07 to a high of 0.6. By curve fitting the traction data, empirical equations for slope and maximum traction coefficient as a function of contact pressure (P), rolling speed (U), and temperature (T) can be developed for each lubricant. A solid lubricant traction model was incorporated into an advanced bearing analysis code (SHABERTH). For comparison purposes, preliminary heat generation calculations were made for both oil and solid lubricated bearing operation. A preliminary analysis indicated a significantly higher heat generation for a solid lubricated ball bearing in a deep groove configuration. An analysis of a cylindrical roller bearing configuration showed a potential for a low friction solid lubricated bearing.

  4. Nanorod Array Solid State Neutron Detectors, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — In this Phase I SBIR project, Synkera proposes to develop and commercialize solid-state neutron detectors of a unique architecture that will enable sensor modules...

  5. Headspace Solid-Phase Microextraction Coupled with Gas ...

    African Journals Online (AJOL)

    contact temperature measurement system (ONTMS). Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was used to analyze the volatile composition of raw FCP and its various ...

  6. Insight into solid-liquid phase transfer catalyzed synthesis of ...

    Indian Academy of Sciences (India)

    Insight into solid-liquid phase transfer catalyzed synthesis of Mecoprop ester using K₂CO₃ as base and development of new kinetic model involving liquid product and two solid co-products. GANAPATI D YADAV GUNJAN P DESHMUKH. REGULAR ARTICLE Volume 129 Issue 11 November 2017 pp 1677-1685 ...

  7. 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...

  8. 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...... including MSNT-mediated esterification of both support-bound alcohols and carboxylic acids has been implemented successfully. Copyright (C) 1996 Elsevier Science Ltd....

  9. The Structural Phase Transition in Solid DCN

    DEFF Research Database (Denmark)

    Dietrich, O. W.; Mackenzie, Gordon A.; Pawley, G. S.

    1975-01-01

    Neutron scattering measurements on deuterated hydrogen cyanide have shown that the structural phase change from a tetragonal to an orthorhombic form at 160K is a first-order transition. A transverse acoustic phonon mode, which has the symmetry of the phase change, was observed at very low energies...

  10. Magnetic Solid Phase Extraction Applied to Food Analysis

    Directory of Open Access Journals (Sweden)

    Israel S. Ibarra

    2015-01-01

    Full Text Available Magnetic solid phase extraction has been used as pretreatment technique for the analysis of several compounds because of its advantages when it is compared with classic methods. This methodology is based on the use of magnetic solids as adsorbents for preconcentration of different analytes from complex matrices. Magnetic solid phase extraction minimizes the use of additional steps such as precipitation, centrifugation, and filtration which decreases the manipulation of the sample. In this review, we describe the main procedures used for synthesis, characterization, and application of this pretreatment technique which were applied in food analysis.

  11. 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.

  12. Study of cements silicate phases hydrated under high pressure and high temperature; Etude des phases silicatees du ciment hydrate sous haute pression et haute temperature

    Energy Technology Data Exchange (ETDEWEB)

    Meducin, F.

    2001-10-01

    This study concerns the durability of oil-well cementing. Indeed, in oil well cementing a cement slurry is pumped down the steel casing of the well up the annular space between it and the surrounding rock to support and protect the casing. The setting conditions of pressure and temperature may be very high (up to 1000 bar and 250 deg C at the bottom of the oil-well). In this research, the hydration of the main constituent of cement, synthetic tri-calcium silicate Ca{sub 3}SiO{sub 2}, often called C{sub 3}S (C = CaO; S = SiO{sub 2} and H H{sub 2}O), is studied. Calcium Silicate hydrates are prepared in high-pressure cells to complete their phase diagram (P,T) and obtain the stability conditions for each species. Indeed, the phases formed in these conditions are unknown and the study consists in the hydration of C{sub 3}S at different temperatures, pressures, and during different times to simulate the oil-well conditions. In a first step (until 120 deg C at ambient pressure) the C-S-H, a not well crystallized and non-stoichiometric phase, is synthesized: it brings adhesion and mechanical properties., Then, when pressure and temperature increase, crystallized phases appear such as jaffeite (Ca{sub 6}(Si{sub 2}O{sub 7})(OH){sub 6}) and hillebrandite (Ca{sub 2}(SiO{sub 3})(OH){sub 2}). Silicon {sup 29}Si Nuclear Magnetic Resonance (using standard sequences MAS, CPMAS) allow us to identify all the silicates hydrates formed. Indeed, {sup 29}Si NMR is a valuable tool to determine the structure of crystallized or not-well crystallized phases of cement. The characterization of the hydrated samples is completed by other techniques: X- Ray Diffraction and Scanning Electron Microscopy. The following results are found: jaffeite is the most stable phase at C/S=3. To simulate the hydration of real cement, hydration of C{sub 3}S with ground quartz and with or without super-plasticizers is done. In those cases, new phases appear: kilchoanite mainly, and xonotlite. A large amount of

  13. Incorporation of phosphorus guest ions in the calcium silicate phases of Portland cement from 31P MAS NMR spectroscopy.

    Science.gov (United States)

    Poulsen, Søren L; Jakobsen, Hans J; Skibsted, Jørgen

    2010-06-21

    Portland cements may contain small quantities of phosphorus (typically below 0.5 wt % P(2)O(5)), originating from either the raw materials or alternative sources of fuel used to heat the cement kilns. This work reports the first (31)P MAS NMR study of anhydrous and hydrated Portland cements that focuses on the phase and site preferences of the (PO(4))(3-) guest ions in the main clinker phases and hydration products. The observed (31)P chemical shifts (10 to -2 ppm), the (31)P chemical shift anisotropy, and the resemblance of the lineshapes in the (31)P and (29)Si MAS NMR spectra strongly suggest that (PO(4))(3-) units are incorporated in the calcium silicate phases, alite (Ca(3)SiO(5)) and belite (Ca(2)SiO(4)), by substitution for (SiO(4))(4-) tetrahedra. This assignment is further supported by a determination of the spin-lattice relaxation times for (31)P in alite and belite, which exhibit the same ratio as observed for the corresponding (29)Si relaxation times. From simulations of the intensities, observed in inversion-recovery spectra for a white Portland cement, it is deduced that 1.3% and 2.1% of the Si sites in alite and belite, respectively, are replaced by phosphorus. Charge balance may potentially be achieved to some extent by a coupled substitution mechanism where Ca(2+) is replaced by Fe(3+) ions, which may account for the interaction of the (31)P spins with paramagnetic Fe(3+) ions as observed for the ordinary Portland cements. A minor fraction of phosphorus may also be present in the separate phase Ca(3)(PO(4))(2), as indicated by the observation of a narrow resonance at delta((31)P) = 3.0 ppm for two of the studied cements. (31)P{(1)H} CP/MAS NMR spectra following the hydration of a white Portland cement show that the resonances from the hydrous phosphate species fall in the same spectral range as observed for (PO(4))(3-) incorporated in alite. This similarity and the absence of a large (31)P chemical shift ansitropy indicate that the hydrous (PO(4

  14. Small angle X-ray scattering from hydrating tricalcium silicate

    International Nuclear Information System (INIS)

    Vollet, D.

    1983-01-01

    The small-angle X-ray scattering technique was used to study the structural evolution of hydrated tricalcium silicate at room temperature. The changes in specific area of the associated porosity and the evolution of density fluctuations in the solid hydrated phase were deduced from the scattering data. A correlation of these variations with the hydration mechanism is tried. (Author) [pt

  15. 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...

  16. 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

  17. Phase transitions in crystalline solids 1

    International Nuclear Information System (INIS)

    Walker, J.R.

    1993-09-01

    Many crystalline materials of interest to the Canadian Nuclear Program have the potential to undergo phase transitions in their range of application. During such phase transitions, a representation of the space group of the higher symmetry polymorph softens to induce the transition. This report is the first in a series of reports concerned with the group-theoretic properties of phase transitions in crystalline materials. The object of the research is to identify all spectroscopically-active soft modes for the 230 three-dimensional space groups. Identification of these soft modes will enable a detailed examination of phase transitions in materials of interest to the Canadian Nuclear Program and aid in the optimization of material properties. In this report, the group-theoretic properties of crystal structures and phase transitions are reviewed. It is demonstrated that the problem of extending a group reduces to that of determining its automorphisms. The automorphism groups of the crystallographic and icosahedral point groups are derived using a consistent presentation

  18. Spectral properties of porphyrins in the systems with layered silicates

    International Nuclear Information System (INIS)

    Ceklovsky, A.

    2009-03-01

    This work is focused on investigation of hybrid materials based on layered silicates, representing host inorganic component, and porphyrin dyes as organic guest. Aqueous colloidal dispersions, as well as thin solid films of layered silicate/porphyrin systems were studied. Modification of photophysical properties, such as absorption and fluorescence of molecules, adsorbed or incorporated in layered silicate hosts, were studied mainly to spread the knowledge about the environments suitable for incorporating aromatic compounds, providing photoactive properties of potential technological interest. TMPyP cations interact with the surfaces of layered silicates via electrostatic interactions. The extent of dye adsorption on colloidal particles of the silicates is influenced by the CEC values and swelling ability of silicates. Interaction of porphyrins with layered silicate hosts leads to significant changes of dye spectral properties. One of the key parameters that has a crucial impact on this interaction is the layer charge of silicate template. Other factors influence the resulting spectral properties of hybrid systems, such as the method of hybrid material preparation, the material's type (colloid, film), and the modification of the silicate host. Molecular orientation studies using linearly-polarized spectroscopies in VIS and IR regions revealed that TMPyP molecules were oriented in almost parallel fashion with respect to the silicate surface plane. Slightly higher values of the orientation angle of TMPyP transition moment were observed for the TMPyP/FHT system. Thus, flattening of the guest TMPyP molecules is the next important factor (mainly in the systems with lower layer charge), influencing its spectral properties upon the interaction with layered silicates. Fluorescence was effectively quenched in the systems based on solid films prepared from the high concentration of the dye (10-3 mol.dm-3). The quenching is most probably related to the structure of the

  19. Heterogeneous Ferroelectric Solid Solutions Phases and Domain States

    CERN Document Server

    Topolov, Vitaly

    2012-01-01

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

  20. The Structural Phase Transition in Solid DCN

    DEFF Research Database (Denmark)

    Dietrich, O. W.; Mackenzie, Gordon A.; Pawley, G. S.

    1976-01-01

    Neutron scattering measurements on deuterated hydrogen cyanide have shown that the structural phase transition from a tetragonal to an orthorhombic form at 160 K is a first order transition. A transverse acoustic phonon mode, which has the symmetry of the transition was observed at very low...

  1. 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.

  2. 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.

  3. Solid-phase synthesis of piperazinones via disrupted Ugi condensation.

    Science.gov (United States)

    Treder, Adam P; Tremblay, Marie-Claude; Yudin, Andrei K; Marsault, Eric

    2014-09-05

    The first application of aziridine aldehyde dimers in solid-phase synthesis is reported. The solid-supported disrupted Ugi condensation between an aziridine aldehyde dimer, isonitrile, and backbone-anchored amino acids delivered N-acyl aziridine intermediates, which were reacted with nucleophiles to yield the corresponding piperazinones. Subsequent cleavage from the resin provided a diverse set of 2,3,6-trisubstituted piperazinones starting from various amino acids, aziridine aldehydes, and nucleophiles.

  4. High temperature gas-solid reactions in calc-silicate Cu-Au skarn formation; Ertsberg, Papua Province, Indonesia

    Science.gov (United States)

    Henley, Richard W.; Brink, Frank J.; King, Penelope L.; Leys, Clyde; Ganguly, Jibamitra; Mernagh, Terrance; Middleton, Jill; Renggli, Christian J.; Sieber, Melanie; Troitzsch, Ulrike; Turner, Michael

    2017-12-01

    The 2.7-3 Ma Ertsberg East Skarn System (Indonesia), adjacent to the giant Grasberg Porphyry Copper deposit, is part of the world's largest system of Cu -Au skarn deposits. Published fluid inclusion and stable isotope data show that it formed through the flux of magma-derived fluid through contact metamorphosed carbonate rock sequences at temperatures well above 600° C and pressures of less than 50 MPa. Under these conditions, the fluid has very low density and the properties of a gas. Combining a range of micro-analytical techniques, high-resolution QEMSCAN mineral mapping and computer-assisted X-ray micro-tomography, an array of coupled gas-solid reactions may be identified that controlled reactive mass transfer through the 1 km3 hydrothermal skarn system. Vacancy-driven mineral chemisorption reactions are identified as a new type of reactive transport process for high-temperature skarn alteration. These gas-solid reactions are maintained by the interaction of unsatisfied bonds on mineral surfaces and dipolar gas-phase reactants such as SO2 and HCl that are continuously supplied through open fractures and intergranular diffusion. Principal reactions are (a) incongruent dissolution of almandine-grossular to andradite and anorthite (an alteration mineral not previously recognized at Ertsberg), and (b) sulfation of anorthite to anhydrite. These sulfation reactions also generate reduced sulfur with consequent co-deposition of metal sulfides. Diopside undergoes similar reactions with deposition of Fe-enriched pyroxene in crypto-veins and vein selvedges. The loss of calcium from contact metamorphic garnet to form vein anhydrite necessarily results in Fe-enrichment of wallrock, and does not require Fe-addition from a vein fluid as is commonly assumed.

  5. Combinatorial solid-phase synthesis of hapalosin mimetics

    DEFF Research Database (Denmark)

    Olsen, Jacob A.; Jensen, Knud J.; Nielsen, John

    2000-01-01

    The solid-phase synthesis of a small library of mimetics of the cyclic depsipeptide hapalosin is described. 3-Amino-4-hydroxy-5-nitrobenzoic acid was anchored through the anilino moiety to a backbone amide linker (BAL) handle support. Using chemoselective reactions and without the need for protec......The solid-phase synthesis of a small library of mimetics of the cyclic depsipeptide hapalosin is described. 3-Amino-4-hydroxy-5-nitrobenzoic acid was anchored through the anilino moiety to a backbone amide linker (BAL) handle support. Using chemoselective reactions and without the need...

  6. Solid-phase synthesis of complex and pharmacologically interesting heterocycles

    DEFF Research Database (Denmark)

    Nielsen, Thomas Eiland

    2009-01-01

    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......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...

  7. Solid-phase synthesis of multivalent metal phosphates

    International Nuclear Information System (INIS)

    Konstant, Z.A.

    1984-01-01

    Some multivalent metals (Mg, Zn, Mn, Co, Ni, Sc, Ti, V, Cr, Fe, Ce) are used as examples for considering certain general problems (mechanism, phase formation) of solid-phase synthesis of phosphates from metal oxides and ammonium dihydrophosphate (t=200-1500 deg C). It is noted that the observed phenomena, such as parallel reactionS, formation of several modifications of one compound is characteristic of solid-phase synthesis of condensed phosphates when condensation is determined by the metal-phosphorus ratio, potential cation coordination and thermodynamic characteristics of polymers being prepared. The possibility of oxidation-reduction reactions with multiple changes in the valence of elements is also very important. Complex schemes of interactions, phase diagrams of the systems are presented

  8. 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.)

  9. Solid-phase synthesis of complex and pharmacologically interesting heterocycles

    DEFF Research Database (Denmark)

    Nielsen, Thomas Eiland

    2009-01-01

    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...

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

    Energy Technology Data Exchange (ETDEWEB)

    Ely, T. M. [Washington River Protection Solutions LLC, Richland, WA (United States); LaMothe, M. E. [Washington River Protection Solutions LLC, Richland, WA (United States); Lachut, J. S. [Washington River Protection Solutions LLC, Richland, WA (United States)

    2016-01-11

    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.

  11. Insight into solid-liquid phase transfer catalyzed synthesis of ...

    Indian Academy of Sciences (India)

    Ganapati D Yadav

    2017-11-16

    Nov 16, 2017 ... https://doi.org/10.1007/s12039-017-1368-1. REGULAR ARTICLE. Special Issue on Recent Trends in the Design and Development of Catalysts and their Applications. Insight into solid-liquid phase transfer catalyzed synthesis of. Mecoprop ester using K2CO3 as base and development of new kinetic model ...

  12. Extraction of Pesticides from Plants using Solid Phase ...

    African Journals Online (AJOL)

    NICO

    Extraction of Pesticides from Plants using Solid Phase. Microextraction and QuEChERS. Veronica C. Obusenga*, Beauty M. Mookantsaa, Harriet Okatcha,. Ketlhatlogile Mosepeleb and NelsonTortoc. aDepartment of Chemistry. University of Botswana, Private Bag UB 00704, Gaborone, Botswana. bUniversity of Botswana ...

  13. 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...

  14. Headspace solid-phase microextraction and gas chromatography ...

    African Journals Online (AJOL)

    Purpose: To extract and analyze the volatile components of Chrysanthemum morifolium Ramat. 'huaiju' by headspace solid-phase microextraction (HS-SPME) and gas chromatography–mass spectrometry. (GC–MS). Methods: Volatile components were extracted by HS-SPME and identified by GC–MS. The relative contents ...

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

    African Journals Online (AJOL)

    performance liquid chromatography–tandem mass spectrometry for the blood quantification of thirty-four toxic principles of plant origin. Application to forensic toxicology. J Chromatogr B 2015; 975: 65-76. 16. Żwir-Ferenc A, Biziuk M. Solid phase extraction technique - Trends, opportunities and applications. Polish J Environ ...

  16. after solid phase extraction on modified sawdust s

    African Journals Online (AJOL)

    Preferred Customer

    detection limit and selectivity [1]. Various methods have been used for the ..... The equation of the line was A = 0.0098C + 0.0022 with a regression coefficient of r = 0.9977 (n = 10). The limit of ... In order to evaluate the selectivity of the method, the effects of different ions on the solid phase extraction and determination of ...

  17. 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

  18. 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

  19. Kinetics of solid state phase transformations: Measurement and ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 122; Issue 1. Kinetics of solid state phase transformations: Measurement and modelling of some basic issues. S Raju E ... are enumerated. A simple and general modelling methodology for understanding the kinetics of non-isothermal transformations is outlined.

  20. 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...

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

    DEFF Research Database (Denmark)

    Lyngsø, Lars O.; Nielsen, John

    1998-01-01

    The development of a solid-phase synthesis of 3-amino-2-pyrazolines is described. Conjugate addition of hydrazines to α,β-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- pyrazolines....

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

    African Journals Online (AJOL)

    Recovery was 94.2 % for Brilliant blue in jelly powder. Conclusion: This method was successfully applied to determine colorants in various (30) water-soluble foods, including fruit flavored drinks, sugar confectionery, sweets, etc. Keywords: Synthetic colors, Food, Fruit flavored drinks, Solid phase extraction, RP-HPLC ...

  3. Headspace solid-phase microextraction and gas chromatography ...

    African Journals Online (AJOL)

    Purpose: To extract and analyze the volatile components of Chrysanthemum morifolium Ramat. 'huaiju' by headspace solid-phase microextraction (HS-SPME) and gas chromatography–mass spectrometry (GC–MS). Methods: Volatile components were extracted by HS-SPME and identified by GC–MS. The relative contents ...

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

    African Journals Online (AJOL)

    ... analysis of 14 multiclass pesticide residues in fruits and vegetable samples. The gas chromatography mass spectrometry parameters (desorption temperature and time, column flow rate, interface temperature) and solid phase microextraction parameters (fiber coating type, extraction temperature and time, pH, salt addition ...

  5. Insight into solid-liquid phase transfer catalyzed synthesis of ...

    Indian Academy of Sciences (India)

    2-Methyl-4-chlorophenoxy propionic acid (Mecoprop) is a widely used household herbicide. In the current work, a simple synthetic method is developed for Mecoprop methyl ester using solid-liquid phase transfer catalysis (S-L PTC) with K₂CO₃ as mild base and toluene as solvent. Conversion of 95% was achieved with ...

  6. 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

  7. 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 ...

  8. The study of actinide solubility limiting solid phases

    International Nuclear Information System (INIS)

    Thomason, H.P.

    1988-01-01

    The literature has been surveyed for information on the identification and ageing of actinide solubility limiting solid phases. References include identification and ageing of actinide solids which do not necessarily relate to the control of solubility or the conditions found in the near-field of a repository. Methods which have been used to characterise actinide solids include X-ray diffraction, electron microscopy, Raman spectroscopy, X-ray photoelectron spectroscopy, electrochemistry and chemical analysis. The techniques most widely used are X-ray and electron diffraction. As well as characterisation, diffraction patterns have been used to monitor changes in the crystallinity of a solid with time. The ageing of alpha active actinide solids involves two conflicting processes. An amorphous actinide precipitate will, like most solids, become more crystalline with time. The recoil energy from the alpha decay of actinides will displace some of the atoms from their lattice sites and cause a decrease in crystallinity. The crystallinity of actinide solids affects solubility and is therefore an important parameter to study. Recommendations have been made for further environmental work. (author)

  9. Uranium-iron-silicate phases from the Balkan Metallogenic Zone and the Lenz im Kaltenegg (Styria, Austria) deposit

    International Nuclear Information System (INIS)

    Simova, F.G.

    1985-01-01

    The newly-found mineral phases of U 4+ of the UO 2 -FeO - SiO 2 homologuos series are reported. They have been established in a deposit of remobilized veinlet-disseminated type, falling within the scope of West-Balkan Metallogenic Zone and of the slightly metamorphized sedimentary type deposit, within the scope of the Semmering - Wechsel Massif, the Eastern Alpes. The presence of pyrite, hematite and peroxides, as well as uranium oxides and U-Fe silicates as small crystals determines the high iron content and radioactivity of the altered rocks. A complex of physical and chemical methods of investigation, radiography, scanning electron microscopy and X-ray microspectral analysis were employed to study the ore mineralization. Rour U-Fe-Si minerals, new to science, have been identified, one coming from Austria and three from the West-Balkan Metallogenic Zone of Bulgaria. The specific composition of the uranium mineralization made it possible to determine the Alpine and recent ages of the hydrothermal mineralization

  10. Phase field modeling of flexoelectricity in solid dielectrics

    Science.gov (United States)

    Chen, H. T.; Zhang, S. D.; Soh, A. K.; Yin, W. Y.

    2015-07-01

    A phase field model is developed to study the flexoelectricity in nanoscale solid dielectrics, which exhibit both structural and elastic inhomogeneity. The model is established for an elastic homogeneous system by taking into consideration all the important non-local interactions, such as electrostatic, elastic, polarization gradient, as well as flexoelectric terms. The model is then extended to simulate a two-phase system with strong elastic inhomogeneity. Both the microscopic domain structures and the macroscopic effective piezoelectricity are thoroughly studied using the proposed model. The results obtained show that the largest flexoelectric induced polarization exists at the interface between the matrix and the inclusion. The effective piezoelectricity is greatly influenced by the inclusion size, volume fraction, elastic stiffness, and the applied stress. The established model in the present study can provide a fundamental framework for computational study of flexoelectricity in nanoscale solid dielectrics, since various boundary conditions can be easily incorporated into the phase field model.

  11. Distribution of Dechlorinating Bacteria between the Aqueous and Solid Phases

    Science.gov (United States)

    Cápiro, N. L.; Hatt, J. K.; Wang, Y.; Loeffler, F. E.; Pennell, K. D.

    2010-12-01

    Microbial monitoring of aquifers relies on nucleic acid biomarker analysis, which is typically performed with biomass recovered from groundwater samples; however, it is unclear what fraction of the target population(s) is associated with groundwater (i.e., planktonic cells) or is attached to solid phases (i.e., biofilms). Understanding how the titer of target organism(s) in groundwater correlates with the true cell titers of the target organism in the aquifer (i.e., planktonic plus attached cells) is critical for a meaningful interpretation of the data, the prediction of bioremediation performance, and the implementation of site management strategies. To evaluate the distribution of active cells between resident solid phase and the aqueous phase, one-dimensional columns were packed under water-saturated conditions with Bio-Dechlor INOCULUM, a PCE-to ethene-dechlorinating bacterial consortium containing both multiple Dehalococcoides (Dhc) strains and Geobacter lovleyi strain SZ (GeoSZ). The columns were packed with two distinct solid matrices: a low organic content sandy Federal Fine Ottawa soil or Appling soil with higher organic matter content. Influent reduced mineral salts medium supplied at a groundwater pore-water velocity of 0.3 m/day contained both 10 mM lactate as electron donor and 0.33 mM PCE as electron acceptor. Routine collection of biomass from column side ports and effluent samples measured the titers of target cells in the aqueous phase and determined when steady state conditions had been reached. A second set of column experiments evaluated delivery and filtration effects by the solid matrix (i.e., Federal Fine Ottawa sand versus Appling soil) under the same conditions except that electron donor or acceptor were omitted (no growth conditions). Quantitative real-time PCR (qPCR) analysis using Dhc and GeoSZ 16S rRNA gene-targeted primer and probe sets determined the planktonic cell counts, and destructive sampling of the columns allowed measurement

  12. 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.

  13. Semi-automated microwave assisted solid-phase peptide synthesis

    DEFF Research Database (Denmark)

    Pedersen, Søren Ljungberg

    measurements during microwave heating. Then we developed protocols for on-resin reductive amination for anchoring of the first amino acids to a BAL handle. Finally, we used the new instrument and the optimized protocols to assist in the synthesis of a range of difficult and long sequences. We believe...... 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...

  14. 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...

  15. Addition of amines to naphthoquinone in water and solid phase

    International Nuclear Information System (INIS)

    Martinez, Sabrina T.; Silva, Barbara V.; Pinto, Angelo C.; Ferreira, Vitor F.; Silva, Fernando de Carvalho da

    2012-01-01

    Considering all the aspects of the principles of green chemistry, we present herein the addition reactions of amines to 1,4-naphthoquinone in water as solvent and also in solid phase. These reactions resulted in very colorful products that were easily monitored by thin layer chromatography and consequently easy to separate. Therefore, they are interesting experiments for experimental organic chemistry in the classrooms or in the laboratories. (author)

  16. Binding of properdin to solid-phase immune complexes

    DEFF Research Database (Denmark)

    Junker, A; Baatrup, G; Svehag, S E

    1998-01-01

    The capacity of serum to support deposition of C3, properdin and factor B was studied by enzyme-linked immunosorbent assay using solid-phase immune complexes (IC) for activation of complement. Deposition of C3 and properdin occurred in fairly dilute normal human serum (NHS), but factor B uptake...... fixed to IC was the principal ligand for properdin in the assay. The findings could have biological implications relating to complement-mediated modification of immune complexes in disease....

  17. A solid-phase radioimmunoassay for detection of tetanus antibodies

    International Nuclear Information System (INIS)

    Dow, B.C.; Barr, A.; Crawford, R.J.; Mitchell, R.

    1983-01-01

    A solid-phase radioimmunoassay has been developed as a screening technique for tetanus antibodies in blood plasma. It is based on the principle of a commercial test for Hepatitis B antibody. Compared to previous screening techniques, the radioimmunoassay showed better stability with no apparent loss of sensitivity over a 2 month period. This technique has proved useful in determining tetanus immunity and in monitoring free antibody level in treated cases of clinical tetanus. (U.K.)

  18. An on-line monitor for cation exchange elution chromatography using lithium silicate glass beads as solid scintillator

    International Nuclear Information System (INIS)

    Zhu Rongbao; Yang Liucheng; Wei Liansheng; Ji Liqiang; Zhang Zengrui

    1988-03-01

    A new type of on-line monitoring system used to monitor radioactive nuclides with α or soft β radiation in the effluent from a high pressure ion exchange column is described. The beads made of cerium-impregnated lithium silicate glass are used as scientillation material. They are filled into a quartz glass tube to form a flow cell. By reducing the diameter of glass beads to more closly approximate the average range of α or soft β radiation in solution, the absolute counting efficiency for 241 Am, 242 Cm α radiation have reached and 85.8% and 92.8% respectively, for 14 C, 90 Sr- 90 Y β radiation, 62.1% and 88.6% respectively. These values can be comparable to those achieved with on-line liquid scientillation technique. When the total amount of 241 Am added into column is decreased to 7.4 Bq it is still possible to obtain a clear chromatography peak (half peak width = 0.22 mL)

  19. THE ALUMINA-SILICATES IN STABILIZATION PROCESSES IN FLUIDIZED-BED ASH

    Directory of Open Access Journals (Sweden)

    IVANA PERNA

    2011-03-01

    Full Text Available Presented study of coal fluidized-bed ash solidification was accompanied with specific studies of alumino-silicates residues in ashes. The specific technology of fluid coal burning and its relatively low temperature combustion combines coal burning and decomposition of calcium carbonate added to the fluid layer in the main endeavor to capture all sulfur oxides. The burning temperature seems be decisive to the behavior of clayed residues and calcium carbonate decomposition in connection for the future solidification of fluidized bed ash. The calcareous substances in combination with alumino-silicate residues form solid bodies where silicates play decisive role of long-term stability and insolubility of obtained solids. The position of aluminum ions in clayed residues of burned coal were studied by MAS-NMR with attention on aluminum ion coordination to oxygen and formation of roentgen amorphous phase of poly-condensed calcium alumina-silicate.

  20. Encapsulation, solid-phases identification and leaching of toxic metals in cement systems modified by natural biodegradable polymers.

    Science.gov (United States)

    Lasheras-Zubiate, M; Navarro-Blasco, I; Fernández, J M; Alvarez, J I

    2012-09-30

    Cement mortars loaded with Cr, Pb and Zn were modified by polymeric admixtures [chitosans with low (LMWCH), medium (MMWCH) and high (HMWCH) molecular weight and hydroxypropylchitosan (HPCH)]. The influence of the simultaneous presence of the heavy metal and the polymeric additive on the fresh properties (consistency, water retention and setting time) and on the compressive strength of the mortars was assessed. Leaching patterns as well as properties of the cement mortars were related to the heavy metals-bearing solid phases. Chitosan admixtures lessened the effect of the addition of Cr and Pb on the setting time. In all instances, chitosans improved the compressive strength of the Zn-bearing mortars yielding values as high as 15 N mm(-2). A newly reported Zn phase, dietrichite (ZnAl(2)(SO(4))(4)·22H(2)O) was identified under the presence of LMWCH: it was responsible for an improvement by 24% in Zn retention. Lead-bearing silicates, such as plumalsite (Pb(4)Al(2)(SiO(3))(7)), were also identified by XRD confirming that Pb was mainly retained as a part of the silicate network after Ca ion exchange. Also, the presence of polymer induced the appearance and stabilization of some Pb(IV) species. Finally, diverse chromate species were identified and related to the larger leaching values of Cr(VI). Copyright © 2012 Elsevier B.V. All rights reserved.

  1. 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.)

  2. 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

  3. 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.

  4. Thermoset polymer-layered silicic acid nanocomposites

    Science.gov (United States)

    Wang, Zhen

    Nanocomposites are formed when phase mixing occurs on a nanometer length scale. Due to the improved phase morphology and interfacial properties, nanocomposites exhibit mechanical properties superior to conventional composites. Toyota researchers first demonstrated that organoclay could be exfoliated in a nylon-6 matrix to greatly improve the thermal and mechanical properties of the polymer, which has resulted in a practical application in the automobile industry. A great deal of research has been conducted on organic-inorganic hybrid composites in which smectite clays are used as reinforcement agents. However, little work has been devoted to derivatives of other layered inorganic solids. In the present work, the first examples of organic polymer-layered silicic acid nanocomposites have been prepared by formation of a cured epoxy polymer network in the presence of organo cation exchange forms of magadiite. The exfoliation of silicate nanolayers in the epoxy matrix was achieved by in-situ intragallery polymerization during the thermosetting process. In general, the tensile properties, solvent resistance, barrier properties and chemical stability of the polymer matrix are greatly improved by the embedded silicate nanolayers when the matrix is flexible (sub-ambient Tg). The improvement of properties are dependent on the silicate loading, the degree of nanolayer separation and interfacial properties. Interestingly, the exfoliation also affects the polymer elasticity in a favorable way. The mechanism leading to nanocomposite formation is proposed. One exfoliated epoxy-magadiite nanocomposite/composition possessed unique transparent optical properties. The exfoliation chemistry was successfully extended to the other members of the layered silicic acid family. A new approach also was developed to prepare thermoset epoxy polymer-layered silicate nanocomposites in which curing agents can be directly intercalated into the intragallery without the need for alkylammonium ions

  5. Solid State NMR Studies of the Aluminum Hydride Phases

    Science.gov (United States)

    Hwang, Son-Jong; Bowman, R. C., Jr.; Graetz, Jason; Reilly, J. J.

    2006-01-01

    Several solid state NMR techniques including magic-angle-spinning (MAS) and multiple-quantum (MQ) MAS experiments have been used to characterize various AlH3 samples. MAS-NMR spectra for the 1H and 27Al nuclei have been obtained on a variety of AlH3 samples that include the (beta)- and (gamma)- phases as well as the most stable (alpha)-phase. While the dominant components in these NMR spectra correspond to the aluminum hydride phases, other species were found that include Al metal, molecular hydrogen (H2), as well as peaks that can be assigned to Al-O species in different configurations. The occurrence and concentration of these extraneous components are dependent upon the initial AlH3 phase composition and preparation procedures. Both the (beta)-AlH3 and (gamma)-AlH3 phases were found to generate substantial amounts of Al metal when the materials were stored at room temperature while the (alpha)-phase materials do not exhibit these changes.

  6. Novel solidsolid 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.

  7. Studies of solid-state electrochromic devices based on Peo/siliceous hybrids doped with lithium perchlorate

    International Nuclear Information System (INIS)

    Barbosa, P.C.; Silva, M.M.; Smith, M.J.; Goncalves, A.; Fortunato, E.

    2007-01-01

    Sol-gel hybrid organic-inorganic networks, doped with a lithium salt, have been used as electrolytes in prototype smart windows. The work described in this presentation is focused on the application of these networks as dual-function electrolyte/adhesive components in solid-state electrochromic devices. The performance of multi-layer electrochromic devices was characterized as a function of the choice of precursor used to prepare the polymer electrolyte component and the guest salt concentration. The prototype devices exhibited good open-circuit memory, coloration efficiency, optical contrast and stability

  8. Potassium Silicate Foliar Fertilizer Grade from Geothermal Sludge and Pyrophyllite

    Directory of Open Access Journals (Sweden)

    Muljani Srie

    2016-01-01

    Full Text Available Potassium silicate fertilizer grade were successfully produced by direct fusion of silica (SiO2 and potasium (KOH and K2CO3 in furnaces at temperatures up to melting point of mixture. The geothermal sludge (98% SiO2 and the pyrophyllite (95% SiO2 were used as silica sources. The purposes of the study was to synthesise potassium silicate fertilizer grade having solids concentrations in the range of 31-37% K2O, and silica in the range of 48-54% SiO2. The weight ratio of silicon dioxide/potasium solid being 1:1 to 5:1. Silica from geothermal sludge is amorphous, whereas pyrophylite is crystalline phase. The results showed that the amount of raw materials needed to get the appropriate molar ratio of potassium silicate fertilizer grade are different, as well as the fusion temperature of the furnace. Potassium silicate prepared from potassium hydroxide and geothermal sludge produced a low molar ratio (2.5: 1 to 3: 1. The potassium required quite small (4:1 in weight ratio, and on a fusion temperature of about 900 °C. Meanwhile, the potassium silicate prepared from pyrophyllite produced a high molar ratio (1.4 - 9.4 and on a fusion temperature of about 1350 °C, so that potassium needed large enough to meet the required molar ratio for the fertilizer grade. The product potassium silicate solid is amorphous with a little trace of crystalline.

  9. Sensitive and fast mutation detection by solid phase chemical cleavage

    DEFF Research Database (Denmark)

    Hansen, Lise Lotte; Justesen, Just; Kruse, Torben A

    1996-01-01

    We have developed a solid phase chemical cleavage method (SpCCM) for screening large DNA fragments for mutations. All reactions can be carried out in microtiterwells from the first amplification of the patient (or test) DNA through the search for mutations. The reaction time is significantly...... reduced compared to the conventional chemical cleavage method (CCM), and even by using a uniformly labelled probe, the exact position and nature of the mutation can be revealed. The SpCCM is suitable for automatization using a workstation to carry out the reactions and a fluorescent detection-based DNA...

  10. Advances in solid-phase extraction disks for environmental chemistry

    Science.gov (United States)

    Thurman, E.M.; Snavely, K.

    2000-01-01

    The development of solid-phase extraction (SPE) for environmental chemistry has progressed significantly over the last decade to include a number of new sorbents and new approaches to SPE. One SPE approach in particular, the SPE disk, has greatly reduced or eliminated the use of chlorinated solvents for the analysis of trace organic compounds. This article discusses the use and applicability of various SPE disks, including micro-sized disks, prior to gas chromatography-mass spectrometry for the analysis of trace organic compounds in water. Copyright (C) 2000 Elsevier Science B.V.

  11. Powder metallurgy: Solid and liquid phase sintering of copper

    Science.gov (United States)

    Sheldon, Rex; Weiser, Martin W.

    1993-01-01

    Basic powder metallurgy (P/M) principles and techniques are presented in this laboratory experiment. A copper based system is used since it is relatively easy to work with and is commercially important. In addition to standard solid state sintering, small quantities of low melting metals such as tin, zinc, lead, and aluminum can be added to demonstrate liquid phase sintering and alloy formation. The Taguchi Method of experimental design was used to study the effect of particle size, pressing force, sintering temperature, and sintering time. These parameters can be easily changed to incorporate liquid phase sintering effects and some guidelines for such substitutions are presented. The experiment is typically carried out over a period of three weeks.

  12. Measurement of the efficacy of calcium silicate for the protection and repair of dental enamel.

    Science.gov (United States)

    Parker, Alexander S; Patel, Anisha N; Al Botros, Rehab; Snowden, Michael E; McKelvey, Kim; Unwin, Patrick R; Ashcroft, Alexander T; Carvell, Mel; Joiner, Andrew; Peruffo, Massimo

    2014-06-01

    To investigate the formation of hydroxyapatite (HAP) from calcium silicate and the deposition of calcium silicate onto sound and acid eroded enamel surfaces in order to investigate its repair and protective properties. Calcium silicate was mixed with phosphate buffer for seven days and the resulting solids analysed for crystalline phases by Raman spectroscopy. Deposition studies were conducted on bovine enamel surfaces. Acid etched regions were produced on the enamel surfaces using scanning electrochemical cell microscopy (SECCM) with acid filled pipettes and varying contact times. Following treatment with calcium silicate, the deposition was visualised with FE-SEM and etch pit volumes were measured by AFM. A second set of bovine enamel specimens were pre-treated with calcium silicate and fluoride, before acid exposure with the SECCM. The volumes of the resultant acid etched pits were measured using AFM and the intrinsic rate constant for calcium loss was calculated. Raman spectroscopy confirmed that HAP was formed from calcium silicate. Deposition studies demonstrated greater delivery of calcium silicate to acid eroded than sound enamel and that the volume of acid etched enamel pits was significantly reduced following one treatment (pcalcium loss from enamel was 0.092 ± 0.008 cm/s. This was significantly reduced, 0.056 ± 0.005 cm/s, for the calcium silicate treatments (pCalcium silicate can transform into HAP and can be deposited on acid eroded and sound enamel surfaces. Calcium silicate can provide significant protection of sound enamel from acid challenges. Calcium silicate is a material that has potential for a new approach to the repair of demineralised enamel and the protection of enamel from acid attacks, leading to significant dental hard tissue benefits. © 2014 Elsevier Ltd. All rights reserved.

  13. Thorium silicate compound as a solid-state target for production of isomeric thorium-229 nuclei by electron beam irradiation

    Directory of Open Access Journals (Sweden)

    P. V. Borisyuk

    2016-09-01

    Full Text Available In this paper, we discuss an idea of the experiment for excitation of the isomeric transition in thorium-229 nuclei by irradiating with electron beam targets with necessary physical characteristics. The chemical composition and bandgap of ThSi10O22 were determined by X-ray photoelectron spectroscopy and reflection electron energy loss spectroscopy. It was found that the energy gap is equal to 7.7 eV and does not change when the target is exposed to a medium energy electron beam for a long time. This indicates that the compound possesses high electron-beam resistance. A quantitative estimation of the output function of isomeric thorium-229 nuclei generated by interaction of nuclei with the secondary electron flow formed by irradiating the solid-state ThSi10O22-based target is given. The estimation shows that ThSi10O22 is a promising thorium-containing target for investigating excitation of the nuclear low-lying isomeric transition in the thorium-229 isotope using medium-energy electrons.

  14. Critical Regimes of Two-Phase Flows with a Polydisperse Solid Phase

    CERN Document Server

    Barsky, Eugene

    2010-01-01

    This book brings to light peculiarities of the formation of critical regimes of two-phase flows with a polydisperse solid phase. A definition of entropy is formulated on the basis of statistical analysis of these peculiarities. The physical meaning of entropy and its correlation with other parameters determining two-phase flows are clearly defined. The interrelations and main differences between this entropy and the thermodynamic one are revealed. The main regularities of two-phase flows both in critical and in other regimes are established using the notion of entropy. This parameter serves as a basis for a deeper insight into the physics of the process and for the development of exhaustive techniques of mass exchange estimation in such flows. The book is intended for graduate and postgraduate students of engineering studying two-phase flows, and to scientists and engineers engaged in specific problems of such fields as chemical technology, mineral dressing, modern ceramics, microelectronics, pharmacology, po...

  15. System for exchange of hydrogen between liquid and solid phases

    Science.gov (United States)

    Reilly, J.J.; Grohse, E.W.; Johnson, J.R.; Winsche, W.E.

    1985-02-22

    The reversible reaction M + x/2 H/sub 2/ reversible MH/sub x/, wherein M is a reversible metal hydride former that forms a hydride MH/sub x/ in the presence of H/sub 2/, generally used to store and recall H/sub 2/, is found to proceed under an inert liquid, thereby reducing contamination, providing better temperature control, providing in situ mobility of the reactants, and increasing flexibility in process design. Thus, a slurry of particles of a metal hydride former with an inert solvent is subjected to a temperature and pressure controlled atmosphere containing H/sub 2/, to store hydrogen and to release previously stored hydrogen. The direction of the flow of the H/sub 2/ through the liquid is dependent upon the H/sub 2/ pressure in the gas phase at a given temperature. When the actual H/sub 2/ pressure is above the equilibrium absorption pressure of the respective hydride the reaction proceeds to the right, i.e., the metal hydride is formed and hydrogen is stored in the solid particle. When the actual pressure in the gas phase is below the equilibrium dissociation pressure of the respective hydride the reaction proceeds to the left, the metal hydride is decomposed and hydrogen is released into the gas phase.

  16. Investigation of the kinetics and microscopic mechanism of solid-solid phase transitions in HMX

    Science.gov (United States)

    Bowlan, Pamela; Suvorova, Natalya; Oschwald, Dave; Bowlan, John; Rector, Kirk; Henson, Bryan; Smilowitz, Laura

    2017-06-01

    Although studied intensely in the 2000's, a number of important questions about solid-solid phase transitions in the energetic organic material octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) remain. The mechanism by which one of the four isomorphs, known as δ, γ, α and β, transforms into another, and the conditions (i.e. temperature and pressure) and rates at which these transitions take place are still not fully known, yet important for predicting and controlling energy release phenomena in HMX such as detonation. The theory of virtual melting, by which a liquid forms at the interface of a nucleation site, is necessary to explain transformations between certain of the four different phases of HMX, such as the β to δ transition. However the existence of this disordered intermediate state has never been directly proven due to the need for both spatial (HMX using X-ray diffraction and confocal Raman and near-field infrared microscopy.

  17. 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.

  18. Evaluation of stability of enalapril maleate in solid phase.

    Science.gov (United States)

    Stanisz, Beata

    2003-02-26

    The influence of temperature (from 383 to 348 K) and relative humidity (from 25.0 to 76.4%) on the stability of enalapril maleate in the solid phase was investigated. Changes in the concentration enalapril maleate were followed by a HPLC method with UV detection. The kinetic and thermodynamic parameters [E(a) (kJ mol(-1))=168.5+/-27 for RH=0% and 149.1+/-48 for RH=76.4%; deltaH(not equal ) (kJ mol(-1))=166.1+/-30 for RH=0% and 146.6+/-50 for RH=76.4%; deltaS(not equal) (J (K(-1) mol(-1)))=120.3+/-169 for RH=0% and 82.1+/-110 for RH=76.4%) of the decomposition reaction were calculated.

  19. Selectivity of solid-phase extraction phases in the determination of biodegradation products.

    Science.gov (United States)

    Bielicka, K; Voelkel, A

    2001-05-18

    The extraction techniques connected with gas chromatography were used to describe quantitatively and qualitatively the biodegradation process. We investigated the biodegradation of hydrocarbons and non-ionic surfactants. Solid-phase extraction (SPE) and liquid-liquid extraction were used for the isolation of the non-degraded compounds and their degradation products. The selectivity of SPE has a significant influence on the isolation and preconcentration of organic compounds from water.

  20. Municipal solid waste development phases: Evidence from EU27.

    Science.gov (United States)

    Vujić, Goran; Gonzalez-Roof, Alvaro; Stanisavljević, Nemanja; Ragossnig, Arne M

    2015-12-01

    Many countries in the European Union (EU) have very developed waste management systems. Some of its members have managed to reduce their landfilled waste to values close to zero during the last decade. Thus, European Union legislation is very stringent regarding waste management for their members and candidate countries, too. This raises the following questions: Is it possible for developing and developed countries to comply with the European Union waste legislation, and under what conditions? How did waste management develop in relation to the economic development in the countries of the European Union? The correlation between waste management practices and economic development was analysed for 27 of the European Union Member States for the time period between 1995 and 2007. In addition, a regression analysis was performed to estimate landfilling of waste in relation to gross domestic product for every country. The results showed a strong correlation between the waste management variables and the gross domestic product of the EU27 members. The definition of the municipal solid waste management development phases followed a closer analysis of the relation between gross domestic product and landfilled waste. The municipal solid waste management phases are characterised by high landfilling rates at low gross domestic product levels, and landfilling rates near zero at high gross domestic product levels. Hence the results emphasize the importance of wider understanding of what is required for developing countries to comply with the European Union initiatives, and highlight the importance of allowing developing countries to make their own paths of waste management development. © The Author(s) 2015.

  1. Synchrotron x-ray spectroscopy of EuHN O3 aqueous solutions at high temperatures and pressures and Nb-bearing silicate melt phases coexisting with hydrothermal fluids using a modified hydrothermal diamond anvil cell and rail assembly

    Science.gov (United States)

    Mayanovic, Robert A.; Anderson, Alan J.; Bassett, William A.; Chou, I.-Ming

    2007-01-01

    A modified hydrothermal diamond anvil cell (HDAC) rail assembly has been constructed for making synchrotron x-ray absorption spectroscopy, x-ray fluorescence, and x-ray mapping measurements on fluids or solid phases in contact with hydrothermal fluids up to ???900??C and 700 MPa. The diamond anvils of the HDAC are modified by laser milling grooves or holes, for the reduction of attenuation of incident and fluorescent x rays and sample cavities. The modified HDAC rail assembly has flexibility in design for measurement of light elements at low concentrations or heavy elements at trace levels in the sample and the capability to probe minute individual phases of a multiphase fluid-based system using focused x-ray microbeam. The supporting rail allows for uniform translation of the HDAC, rotation and tilt stages, and a focusing mirror, which is used to illuminate the sample for visual observation using a microscope, relative to the direction of the incident x-ray beam. A structure study of Eu(III) aqua ion behavior in high-temperature aqueous solutions and a study of Nb partitioning and coordination in a silicate melt in contact with a hydrothermal fluid are described as applications utilizing the modified HDAC rail assembly. ?? 2007 American Institute of Physics.

  2. Application of solid-phase microextraction in analytical toxicology.

    Science.gov (United States)

    Pragst, Fritz

    2007-08-01

    Solid-phase microextraction (SPME) is a miniaturized and solvent-free sample preparation technique for chromatographic-spectrometric analysis by which the analytes are extracted from a gaseous or liquid sample by absorption in, or adsorption on, a thin polymer coating fixed to the solid surface of a fiber, inside an injection needle or inside a capillary. In this paper, the present state of practical performance and of applications of SPME to the analysis of blood, urine, oral fluid and hair in clinical and forensic toxicology is reviewed. The commercial coatings for fibers or needles have not essentially changed for many years, but there are interesting laboratory developments, such as conductive polypyrrole coatings for electrochemically controlled SPME of anions or cations and coatings with restricted-access properties for direct extraction from whole blood or immunoaffinity SPME. In-tube SPME uses segments of commercial gas chromatography (GC) capillaries for highly efficient extraction by repeated aspiration-ejection cycles of the liquid sample. It can be easily automated in combination with liquid chromatography but, as it is very sensitive to capillary plugging, it requires completely homogeneous liquid samples. In contrast, fiber-based SPME has not yet been performed automatically in combination with high-performance liquid chromatography. The headspace extractions on fibers or needles (solid-phase dynamic extraction) combined with GC methods are the most advantageous versions of SPME because of very pure extracts and the availability of automatic samplers. Surprisingly, substances with quite high boiling points, such as tricyclic antidepressants or phenothiazines, can be measured by headspace SPME from aqueous samples. The applicability and sensitivity of SPME was essentially extended by in-sample or on-fiber derivatization. The different modes of SPME were applied to analysis of solvents and inhalation narcotics, amphetamines, cocaine and metabolites

  3. Development of novel solid-phase protein formulations

    Science.gov (United States)

    Montalvo Ortiz, Brenda Liz

    Proteins are the next-generation drugs for the treatment of several diseases. However, the number of protein drugs is still limited due to the physical or chemical instability of proteins during processing, formulation, storage, and delivery. The formulation of proteins at the solid state has advantages over liquid state, such as improved stability during long-term storage and delivery and decreases transportation costs. In this dissertation, we developed new solid-phase protein formulations in which the integrity of the protein was not compromised. The long term goal of this research was to use these protein formulations to improve protein stability in drug delivery devices, such as poly(lactic-co-glycolic) acid (PLGA). The first solid-phase protein formulation developed in this investigation was named "glassification". We proposed glassification as an alternative protein dehydration technique to the common used one, lyophilization, because this last method involves a series of steps which are detrimental to protein structure and stability. The glassification method consisted on protein dehydration by the use of organic solvents. As a result of the glassification process a small (micrometer size range) protein solid bead was obtained. The proteins used to study the glassification process were lysozyme (LYS), alpha-chymotrypsin (CHYMO) and horseradish peroxidase (HRP). These studies revealed that the glassification process itself did not alter protein structure and the activity was preserved. Ethyl acetate was the most effective organic solvent for protein glassification because it led to the highest protein residual activity, no insoluble aggregate formation and is a relatively non-toxic solvent, which allow the incorporation of these protein microparticles in PLGA microspheres. The incorporation of spherical HRP microparticles into PLGA microspheres resulted in superior properties when compared with encapsulated lyophilized HRP powder, such as improved release

  4. 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.

  5. Microencapsulated Comb-Like Polymeric Solid-Solid Phase Change Materials via In-Situ Polymerization

    Directory of Open Access Journals (Sweden)

    Wei Li

    2018-02-01

    Full Text Available To enhance the thermal stability and permeability resistance, a comb-like polymer with crystallizable side chains was fabricated as solid-solid phase change materials (PCMs inside the cores of microcapsules and nanocapsules prepared via in-situ polymerization. In this study, the effects on the surface morphology and microstructure of micro/nanocapsules caused by microencapsulating different types of core materials (i.e., n-hexadecane, ethyl hexadecanoate, hexadecyl acrylate and poly(hexadecyl acrylate were systematically studied via field emission scanning electron microscope (FE-SEM and transmission electron microscope (TEM. The confined crystallization behavior of comb-like polymer PCMs cores was investigated via differential scanning calorimeter (DSC. Comparing with low molecular organic PCMs cores, the thermal stability of PCMs microencapsulated comb-like polymer enhanced significantly, and the permeability resistance improved obviously as well. Based on these resultant analysis, the microencapsulated comb-like polymeric PCMs with excellent thermal stability and permeability resistance showed promising foreground in the field of organic solution spun, melt processing and organic coating.

  6. Silicate glasses

    International Nuclear Information System (INIS)

    Lutze, W.

    1988-01-01

    Vitrification of liquid high-level radioactive wastes has received the greatest attention, world-wide, compared to any other HLW solidification process. The waste form is a borosilicate-based glass. The production of phosphate-based glass has been abandoned in the western world. Only in the Soviet Union are phosphate-based glasses still being developed. Vitrification techniques, equipment and processes and their remote operation have been developed and studied for almost thirty years and have reached a high degree of technical maturity. Industrial demonstration of the vitrification process has been in progress since 1978. This chapter is a survey of world-wide research and development efforts in nuclear waste glasses and its production technology. The principal glasses considered are silicate glasses which contain boron, i.e., borosilicate glasses

  7. Microwave Enhanced Freeze Drying of Solid Waste, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Development of technology for Microwave Enhanced Freeze Drying of Solid Waste (MEFDSW) is proposed. The present state of the art for solid waste stabilization using...

  8. Solid-phase microextraction and the human fecal VOC metabolome.

    Directory of Open Access Journals (Sweden)

    Emma Dixon

    2011-04-01

    Full Text Available The diagnostic potential and health implications of volatile organic compounds (VOCs present in human feces has begun to receive considerable attention. Headspace solid-phase microextraction (SPME has greatly facilitated the isolation and analysis of VOCs from human feces. Pioneering human fecal VOC metabolomic investigations have utilized a single SPME fiber type for analyte extraction and analysis. However, we hypothesized that the multifarious nature of metabolites present in human feces dictates the use of several diverse SPME fiber coatings for more comprehensive metabolomic coverage. We report here an evaluation of eight different commercially available SPME fibers, in combination with both GC-MS and GC-FID, and identify the 50/30 µm CAR-DVB-PDMS, 85 µm CAR-PDMS, 65 µm DVB-PDMS, 7 µm PDMS, and 60 µm PEG SPME fibers as a minimal set of fibers appropriate for human fecal VOC metabolomics, collectively isolating approximately 90% of the total metabolites obtained when using all eight fibers. We also evaluate the effect of extraction duration on metabolite isolation and illustrate that ex vivo enteric microbial fermentation has no effect on metabolite composition during prolonged extractions if the SPME is performed as described herein.

  9. Headspace solid-phase microextraction for wine volatile analysis.

    Science.gov (United States)

    Azzi-Achkouty, Samar; Estephan, Nathalie; Ouaini, Naïm; Rutledge, Douglas N

    2017-07-03

    The most commonly used technique to prepare samples for the analysis of wine volatile is the headspace solid-phase microextraction (HS-SPME). This method has gained popularity in last few years, as it is a unique solventless preparation technique. In this paper, a summary of recently published studies using HS-SPME for the analysis of wine aromas, with special emphasis on the method developed, has been compiled. Several papers are discussed in detail, mainly with respect to the SPME conditions used. A brief summary of the reviews related to HS-SPME analysis is given and discussed. Several parameters affecting the HS-SPME, such as the salt concentration and the agitation conditions, are used in the same way as used in several papers. The HS-SPME extraction proved to be sufficiently sensitive to satisfy legislative requirements related to low detection and quantification limits as well as method accuracy and precision requirements. However, in order to achieve the best performance and precision, the protocol needs to be optimized for each case. The effect of different parameters must be well characterized to ensure correct extraction and desorption to ensure the transfer of extracted compounds into the analytical system. The operating parameters, such as time, temperature, and agitation, must then be kept constant for all the samples.

  10. Automated solid-phase peptide synthesis to obtain therapeutic peptides

    Directory of Open Access Journals (Sweden)

    Veronika Mäde

    2014-05-01

    Full Text Available The great versatility and the inherent high affinities of peptides for their respective targets have led to tremendous progress for therapeutic applications in the last years. In order to increase the drugability of these frequently unstable and rapidly cleared molecules, chemical modifications are of great interest. Automated solid-phase peptide synthesis (SPPS offers a suitable technology to produce chemically engineered peptides. This review concentrates on the application of SPPS by Fmoc/t-Bu protecting-group strategy, which is most commonly used. Critical issues and suggestions for the synthesis are covered. The development of automated methods from conventional to essentially improved microwave-assisted instruments is discussed. In order to improve pharmacokinetic properties of peptides, lipidation and PEGylation are described as covalent conjugation methods, which can be applied by a combination of automated and manual synthesis approaches. The synthesis and application of SPPS is described for neuropeptide Y receptor analogs as an example for bioactive hormones. The applied strategies represent innovative and potent methods for the development of novel peptide drug candidates that can be manufactured with optimized automated synthesis technologies.

  11. 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...

  12. 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...... experiments revealed that histamine adsorbed onto a solid-phase could bind the antiserum. However, neither free histamine nor histamine coupled to unrelated carriers could inhibit the binding of antiserum to the solid-phase histamine. Cross-reactivity was demonstrated between HSA and solid-phase bound...... histamine, as the immunoradiometric assay was inhibited by HSA. This unexpected cross-reactivity was established, as a commercially available antiserum with specificity to HSA without histamine also bound to the solid-phase bound histamine. It is suggested that preparations of antibodies against histamine...

  13. 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.

  14. 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

  15. Multiphase Modeling of Solid Rocket Motor Internal Environment, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Solid rocket motor (SRM) design requires thorough understanding of the slag accumulation process in order to: predict thrust continuity, optimize propellant...

  16. Highly Efficient, Durable Regenerative Solid Oxide Stack, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Precision Combustion, Inc. (PCI) proposes to develop a highly efficient regenerative solid oxide stack design. Novel structural elements allow direct internal...

  17. Ultrarapid mutation detection by multiplex, solid-phase chemical cleavage

    Energy Technology Data Exchange (ETDEWEB)

    Rowley, G.; Saad, S.; Giannelli, F.; Green, P.M. [Guy`s & St. Thomas`s Hospitals, London (United Kingdom)

    1995-12-10

    The chemical cleavage of mismatches in heteroduplexes formed by probe and test DNA detects and locates any sequence change in long DNA segments ({approximately}1.8 kb), and its efficiency has been well tested in the analysis of both average (e.g., coagulation factor IX) and large, complex genes (e.g., coagulation factor VIII and dystrophin). In the latter application RT/PCR products allow the examination of all essential sequences of the gene in a minimum number of reactions. We use two specific chemical reactants (hydroxylamine and osmium tetroxide) and piperidine cleavage of the above procedure to develop a very fast mutation screening method. This is based on: (1) 5{prime} or internal fluorescent labeling to allow concurrent screening of three to four DNA fragments and (2) solid-phase chemistry to use a microliter format and reduce the time required for the procedure, from amplification of sequence to gel loading inclusive, to one person-working-day. We test the two variations of the method, one entailing 5{prime} labeling of probe DNA and the other uniform labeling of both probe and target DNA, by detecting 114 known hemophilia B (coagulation factor IX) mutations and by analyzing 129 new patients. Uniform labeling of both probe and target DNA prior to formation of the heteroduplexes leads to almost twofold redundancy in the ability to detect mutations. Alternatively, the latter procedure may offer very efficient though less than 100% screening for sequence changes with only hydroxylamine. The full method with two chemical reactions (hydroxylamine and osmium tetroxide) should allow one person to screen with virtually 100% accuracy more than 300 kb of sequence in three ABI 373 gels in 1 day. 26 refs., 7 figs., 1 tab.

  18. Solid phase exchange labeling of I-123-HIPDM

    International Nuclear Information System (INIS)

    Mangner, T.; Rogers, W.L.; Wieland, D.; Clinthorne, N.; Juni, J.; Koral, K.; Mayans, R.; Swanson, D.

    1984-01-01

    Reported brain uptake of the I-123 diamine, HIPDM, ranges from 3.5% to 8.5% of the injected dose. This variability has been attributed to varying purity of the labeled compound produced by published methods. The authors have obtained excellent radioiodide incorporation into HIPDM using a simple, 5-minute, solid-phase exchange reaction in the presence of ammonium sulfate or bisulfate. However, when ammonium sulfate was used, HPLC analysis (μBodapak-phenyl; 1% ammonium acetate (pH 5.5)/methanol, 30/70) revealed the presence of, in addition to labeled HIPDM and unreacted radioiodide, two additional labeled compounds, each comprising 4% of the total activity. Lowering the initial pH of the reaction by the use of ammonium bisulfate resulted in quantitative radioiodide incorporation to give chromatographically pure HIPDM. To date, this preparation has been tested in one normal human. Percent uptake in brain was determined by tomographic imaging with both a single photon ring tomograph (SPRINT) and rotating Anger camera (GE 400-T). In each case high energy background was determined by acquiring data with lead shielding over the collimator. This background was then subtracted from the images. Calibration was performed by imaging a 19 cm diameter uniform cylindrical phantom filled with I-123. Both sets of images were attenuation corrected with the Sorenson method. Total uptake in the brain was between 6.7% and 7.2% depending upon selection of the brain outline. This agrees with values reported previously and is quite comparable to those measured for iodoamphetamine

  19. Determination of Thermal Conductivity of Silicate Matrix for Applications in Effective Media Theory

    Science.gov (United States)

    Fiala, Lukáš; Jerman, Miloš; Reiterman, Pavel; Černý, Robert

    2018-02-01

    Silicate materials have an irreplaceable role in the construction industry. They are mainly represented by cement-based- or lime-based materials, such as concrete, cement mortar, or lime plaster, and consist of three phases: the solid matrix and air and water present in the pores. Therefore, their effective thermal conductivity depends on thermal conductivities of the involved phases. Due to the time-consuming experimental determination of the effective thermal conductivity, its calculation by means of homogenization techniques presents a reasonable alternative. In the homogenization theory, both volumetric content and particular property of each phase need to be identified. For porous materials the most problematic part is to accurately identify thermal conductivity of the solid matrix. Due to the complex composition of silicate materials, the thermal conductivity of the matrix can be determined only approximately, based on the knowledge of thermal conductivities of its major compounds. In this paper, the thermal conductivity of silicate matrix is determined using the measurement of a sufficiently large set of experimental data. Cement pastes with different open porosities are prepared, dried, and their effective thermal conductivity is determined using a transient heat-pulse method. The thermal conductivity of the matrix is calculated by means of extrapolation of the effective thermal conductivity versus porosity functions to zero porosity. Its practical applicability is demonstrated by calculating the effective thermal conductivity of a three-phase silicate material and comparing it with experimental data.

  20. The contact angle of wetting of the solid phase of soil before and after chemical modification

    Directory of Open Access Journals (Sweden)

    Tyugai Zemfira

    2015-07-01

    Full Text Available Wettability of soil affects a wide variety of processes including infiltration, preferential flow and surface runoff. Wettability of surface is usually expressed in terms of contact angle (CA measurement. If the CA between liquid and solid surface is less than 90°, the surface is called hydrophilic, otherwise the surface is called hydrophobic. If the CA of water droplet on hydrophilic surface is in a range of 0-30° this surface is called superhydrophilic. In case of superhydrophobic surfaces the CA exceeds 150° that means that these surfaces are extremely difficult to wet. CA of wetting of mineral soil particles depends on the overlying organic and iron compounds. The object of study is a sample of the humus-accumulative horizon of typical chernozem (Kursk, Russia and two samples (horizons A1, B2 of red ferrallitic soils (Fr. Norfolk, NE Oceania. The soil samples were analyzed for organic carbon, forms of non-silicate iron and hydrophobic-hydrophilic composition of humic substances. CA of wetting was determined in the intact samples and after removal of organic matter (H2O2 treatment, amorphous and crystallized forms of iron. Static contact angles were determined with the sessile drop method using a digital goniometer (Drop Shape Analysis System, DSA100, Krüss GmbH, Hamburg, Germany. The contact angle was calculated by the Young–Laplace method (fitting of Young–Laplace equation to the drop shape. The measurements were repeated 10-15 times for every sample. Oxidation of organic matter (H2O2 treatment causes an increase in the values of CA of wetting (in chernozem from 9.3 to 28,0-29.5º, in ferrallitic soil from 18.0 − 27.3 to 22.4 − 33.4º. CA remained constant for chernozem and slightly decreased in the case of ferrallitic soil, when the removal of amorphous and crystallized forms of iron was performed on samples pretreated with H2O2. CA increase occurs after successive removal of nonsilicate forms of iron from soil samples of

  1. Materials research for passive solar systems: solid-state phase-change materials

    Energy Technology Data Exchange (ETDEWEB)

    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 (C/sub 5/H/sub 12/O/sub 4/), pentaglycerinve (C/sub 5/H/sub 12/O/sub 3/), and neopentyl glycol (C/sub 5/H/sub 12/O/sub 2/). Solid solution mixtures of these compounds can be tailored so that they exhibit solid-to-solid phase transformations at any desired temperature betweeen 25/sup 0/C and 188/sup 0/C, and have latent heats of transformation between 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. Nevertheless, a higher cost of the phase-change materials (approx. =$0.70 per pound) is likely to limit their applicability in passive solar systems unless their performance can be significantly improved through further research.

  2. Solid State MEMS Thrusters Using Electrically Controlled Extinguishable Solid Propellant, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — ET Materials, LLC developed the first ever electrically controlled extinguishable solid propellant (ECESP). The original propellant developed under Air Force SBIR...

  3. Insight into solid-liquid phase transfer catalyzed synthesis of ...

    Indian Academy of Sciences (India)

    Ganapati D Yadav

    2017-11-16

    TEAB) were screened ..... ion-pair with phenoxide species leading to the formation of potassium salt with K and KHCO3. The ..... on solid potassium carbonate surface under PTC circum- stances Heteroatom Chem. 15 447. 15.

  4. Microwave Enhanced Freeze Drying of Solid Waste, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — The development of advanced methods for Microwave Enhanced Freeze Drying of Solid Waste (MEFDSW) is proposed. Methods for the recovery of relatively pure water as a...

  5. Solid State Oxygen Concentrator and Compressor, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Sustainable Innovations has developed a novel solid state technology for gas separation and will be applying it for the first time to meet a critical life support...

  6. Mineralogical characterization of municipal solid waste incineration bottom ash with an emphasis on heavy metal-bearing phases.

    Science.gov (United States)

    Wei, Yunmei; Shimaoka, Takayuki; Saffarzadeh, Amirhomayoun; Takahashi, Fumitake

    2011-03-15

    Municipal solid waste incineration (MSWI) bottom ash contains a considerable amount of heavy metals. The occurrence and uneven distribution of these heavy metals in bottom ash can increase the complexity of such residues in terms of long-term behavior upon landfilling or recycling. Bottom ashes sampled from three stoker-type incinerators in Japan were analyzed in this paper. This study presents detailed information on the mineralogical characterization of bottom ash constituents and the weathering behavior of these constituents by means of optical microscopy and scanning electron microscopy. It was revealed that bottom ash mainly consists of assorted silicate-based glass phases (48-54 wt% of ash) and mineral phases including melilites, pseudowollastonite, spinels, and metallic inclusions (Fe-P, Fe-S, Fe-Cu, Cu-Sn, Cu-Zn, Cu-S, and Cu-Pb dominated phases), as melt products formed during the incineration process. The compounds embedded in the glass matrix, e.g. spinels and metallic inclusions, played the most important role in concentration of heavy metals (Pb, Zn, Cu, Cr, Mn, Ni, etc.). Other phases such as refractory minerals and ceramics, frequently found in ash, were of less significance in terms of their influence on the involvement of heavy metals. Analysis of lab-scale artificially weathered and 10-year landfilled bottom ash samples revealed that secondary mineralization/alteration of the bottom ash constituents principally carbonation and glass evolution substantially decreased the potential risk of the heavy metals to the surrounding environment. Copyright © 2011 Elsevier B.V. All rights reserved.

  7. Solid Phase Equilibrium Relations in the CaO-SiO2-Nb2O5-La2O3 System at 1273 K

    Science.gov (United States)

    Qiu, Jiyu; Liu, Chengjun

    2018-02-01

    Silicate slag system with additions Nb and RE formed in the utilization of REE-Nb-Fe ore deposit resources in China has industrial uses as a metallurgical slag system. The lack of a phase diagram, theoretical, and thermodynamic information for the multi-component system restrict the comprehensive utilization process. In the current work, solid phase equilibrium relations in the CaO-SiO2-Nb2O5-La2O3 quaternary system at 1273 K (1000 °C) were investigated experimentally by the high-temperature equilibrium experiment followed by X-ray diffraction, scanning electron microscope, and energy dispersive spectrometer. Six spatial independent tetrahedron fields in the CaO-SiO2-Nb2O5-La2O3 system phase diagram were determined by the Gibbs Phase Rule. The current work combines the mass fraction of equilibrium phase and corresponding geometric relation. A determinant method was deduced to calculate the mass fraction of equilibrium phase in quaternary system according to the Mass Conservation Law, the Gibbs Phase Rule, the Lever's Rule, and the Cramer Law.

  8. Na/Ca Intermixing around Silicate and Phosphate Groups in Bioactive Phosphosilicate Glasses Revealed by Heteronuclear Solid-State NMR and Molecular Dynamics Simulations.

    Science.gov (United States)

    Mathew, Renny; Stevensson, Baltzar; Edén, Mattias

    2015-04-30

    We characterize the intermixing of network-modifying Na(+)/Ca(2+) ions around the silicate (QSi(n)) and phosphate (QP(n)) tetrahedra in a series of 16 Na2O–CaO–SiO2–P2O5 glasses, whose P content and silicate network connectivity were varied independently. The set includes both bioactive and bioinactive compositions and also encompasses two soda-lime-silicate members devoid of P, as well as two CaO–SiO2 glasses and one Na2O–SiO2–P2O5 glass. The various Si/P↔Na/Ca contacts were probed by molecular dynamics (MD) simulations together with heteronuclear magic-angle-spinning (MAS) nuclear magnetic resonance (NMR) experimentation utilizing (23)Na{(31)P} and (23)Na{(29)Si} REDOR, as well as (31)P{ (23)Na} and (29)Si{(23)Na} REAPDOR. We introduce an approach for quantifying the extent of Na(+)/Ca(2+) ordering around a given QP(n) or QSi(n) group, encoded by the preference factor 0⩽ PM ⩽ 1 conveying the relative weights of a random cation intermixing (PM = 0) and complete preference/ordering (PM = 1) for one of the species M, which represents either Na(+) or Ca(2+). The MD-derived preference factors reveal phosphate and silicate species surrounded by Na(+)/Ca(2+) ions intermixed nearly randomly (PM ≲ 0.15), except for the QSi(4) and QSi(1) groups, which manifest more significant cation ordering with preference for Na+ and Ca2+, respectively. The overall weak preferences are essentially independent of the Si and P contents of the glass, whereas PM primarily correlates with the total amount of network modifiers: as the latter is increased, the Na/Ca distribution around the {QP(0), QSi(1), QSi(2)} groups with preference for Ca2(+ )tend to randomize (i.e., PCa decreases), while the PNa-values grow slightly for the {QP(1), QSi(3), QSi(4)} species already preferring coordination of Na. The set of experimental preference factors {PCa} for the orthophosphate (QP(0)) groups extracted from (31)P{(23)Na} REAPDOR NMR-derived M2(P–Na) dipolar second moments agrees

  9. Studies of neo-formed phases occurring during spent nuclear fuel dissolution in geological repository: influence of silicate ions; Etude des phases neoformees lors de la dissolution du combustible nucleaire en condition de stockage geologique: influence des ions silicate

    Energy Technology Data Exchange (ETDEWEB)

    Robit-Pointeau, V

    2005-12-15

    Spent nuclear fuel alteration in deep storage conditions may proceed by local oxidising conditions at the fuel / water interface under influence of alpha irradiation. However, due to the strong redox buffer capacity of the near-field materials (especially the canister and the geological media), most of the near-field environment will remain reducing. Due to the relative high concentration in silica in such system, coffinite USiO{sub 4}.n(H{sub 2}O) may be a relevant phase to consider as it has been suggested from the natural analogues observations (Oklo). The aim of this work was to assess the relevance of coffinitisation of the spent fuel phenomena. The results of the experimental work contest the thermodynamic predictions. Instead of coffinite, a new U(IV)-Si phase has been observed in water simulating storage conditions. The thermodynamic data on coffinite validated by OECD are based on the average concentration of dissolved silica present in natural system containing uraninite and quartz. As the silica concentration in natural groundwaters is more probably controlled by minerals like chalcedony or silica gel, the coffinite present with uraninite in such systems, is probably not in equilibrium even in 2-billion years- old geological sites. Based on the results of this study, coffinitisation of the spent nuclear fuel in deep geological disposal is not anticipated to be a dominant short term process. (author)

  10. Utilizing ion-pairing hydrophilic interaction chromatography solid phase extraction for efficient glycopeptide enrichment in glycoproteomics

    DEFF Research Database (Denmark)

    Mysling, Simon; Palmisano, Giuseppe; Højrup, Peter

    2010-01-01

    Glycopeptide enrichment is a prerequisite to enable structural characterization of protein glycosylation in glycoproteomics. Here we present an improved method for glycopeptide enrichment based on zwitter-ionic hydrophilic interaction chromatography solid phase extraction (ZIC-HILIC SPE...

  11. Evaluation of a Solid Phase DNA Binding Matrix for Downstream PCR Analysis

    National Research Council Canada - National Science Library

    Bader, Douglas E; Fisher, Glen R; Stratilo, Chad W

    2005-01-01

    A commercially available solid-phase DNA binding matrix (FTA cards) was evaluated for its ability to capture and release DNA for downstream gene amplification and detection assays using polymerase chain reaction (PCR...

  12. Solid phase extraction of β-N-methylamino-L-alanine (BMAA) from ...

    African Journals Online (AJOL)

    2011-01-25

    N-methylamino-L-alanine, BMAA, cyanobacterial bloom, solid phase extraction. Introduction. The isolation of the neurotoxin BMAA from freshwater and marine cyanobacteria (Cox et al., 2005; Banack et al., 2007;. Esterhuizen ...

  13. 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

  14. Solid Phase Peptide Synthesis of Antimicrobial Peptides for cell Binding Studies: Characterization Using Mass Spectrometry

    National Research Council Canada - National Science Library

    Vouros, Paul

    2002-01-01

    ...) in order to determine their anti-microbial activity. To expedite this goal, mass spectrometry was used to identify products of the solid phase synthesis and thereby optimize synthetic conditions...

  15. 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...

  16. 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

  17. The study of actinide solubility limiting solid phases - a literature survey

    International Nuclear Information System (INIS)

    Thomason, H.P.

    1988-03-01

    It is important to identify the solid phases which control the solubilities of the actinides in a cementitious repository and to determine the effect of ageing on these solid phases. This literature survey contains information on the identification and ageing of actinide solubility limiting solid phases and includes references which do not necessarily relate to the control of solubility or the conditions found in the near-field of a repository of the methods which have been used to characterise actinide solids. The techniques most widely used are X-ray and electron diffraction, although they require a solid to be crystalline in order to identify it. As well as characterisation, diffraction patterns have been used to monitor changes in the crystallinity of a solid with time. The ageing of alpha active actinide solids involves two conflicting processes. An amorphous actinide precipitate will, like most solids, become more crystalline with time. However, the recoil energy from the alpha decay of actinides will displace some of the atoms from their lattice sites and cause a decrease in crystallinity. The crystallinity of actinide solids affects solubility and is therefore an important parameter to study. Recommendations have been made for further experimental work. (author)

  18. Resin Capsules: Permeable Containers for Parallel/Combinatorial Solid-Phase Organic Synthesis

    OpenAIRE

    Bouillon, Isabelle; Soural, Miroslav; Krchňák, Viktor

    2008-01-01

    A resin capsule is a permeable container for resin beads designed for multiple/combinatorial solid-phase organic synthesis. Resin capsules consist of a high density polyethylene ring sealed with peek mesh on both sides. The cylindrical shape of resin capsules enabled space-saving packing into plastic column-like reaction vessels commonly used for solid-phase organic synthesis. Resin capsules have been evaluated for their use in combinatorial synthesis, and a set of model compounds with excell...

  19. 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...... of the intermediate isothiocyanate. The isothiocyanate and subsequent thiourea formation take place under standard peptide coupling conditions using carbon disulfide as the 'amino acid'. The thioureas are released from the resin and isolated in moderate to high yields....

  20. Experimental investigation of Cs 137 distribution in a system of aquatic solution - solid phase - plant

    International Nuclear Information System (INIS)

    Marchiulioniene, D.; Kiponas, D.; Lukshiene, B.

    2005-01-01

    Investigation of Cs 137 accumulation in the plant Lepidium sativum L. (seeds, roots, aboveground part) and in the solid phase from the aquatic solution under laboratory conditions was performed. According to the obtained results, evaluation of Cs 137 distribution in the system aquatic solution - solid phase - plant and transfer of this radionuclide from the root system to the plant aboveground part during the plant growth process was done. (authors)

  1. Three magnetic particles solid phase radioimmunoassay for T4: Comparison of their results with established methods

    International Nuclear Information System (INIS)

    Bashir, T.

    1996-01-01

    The introduction of solid phase separation techniques is an important improvement in radioimmunoassays and immunoradiometric assays. Magnetic particle solid phase method has additional advantages over others, as the separation is rapid and centrifugation is not required. Three types of magnetic particles have been studied in T 4 RIA and the results have been compared with commercial kits and other established methods. (author). 4 refs, 9 figs, 2 tabs

  2. Expedient protocol for solid-phase synthesis of secondary and tertiary amines

    DEFF Research Database (Denmark)

    Olsen, Christian A; Witt, Matthias; Jaroszewski, Jerzy W

    2004-01-01

    [reaction: see text] An expedient solid-phase synthetic approach to secondary and tertiary amines was developed. The protocol employs conversion of resin-bound amino alcohols to the corresponding iodides, followed by iodide displacement with primary or secondary amines or with unprotected amino a...... alcohols. This two-step procedure, affording products in good to excellent yields, is suitable for solid-phase synthesis of polyamines....

  3. Modeling of liquid phase formation due to the solid zircaloy-4/solid stainless steel interaction

    Energy Technology Data Exchange (ETDEWEB)

    San Martin, G.E.; Piotrkowski, R. [Comision Nacional de Energia Atomica, Buenos Aires (Argentina). Dept. de Combustibles Nucleares; Moyano, E. [Comision Nacional de Energia Atomica, Buenos Aires (Argentina). Centro de Calculo Cientifico; Garcia, E.A. [Ente Nacional Regulador Nuclear, Buenos Aires (Argentina). Centro Atomico Ezeiza

    1995-12-31

    A diffusion model that describes the eutectic interaction between both as received and oxidized Zry-4 and AISI 316 stainless steel at temperatures between 1000 to 1300{sup 0} C is presented. The instantaneous positions of the two solid/liquid interfaces, are input data. The interdiffusion coefficients are calculated in the melt and the solid/liquid interfaces concentration values for different temperatures. (author). 7 refs., 3 figs., 1 tab.

  4. Vapour phase synthesis of salol over solid acids via transesterification

    Indian Academy of Sciences (India)

    Administrator

    salicylic acid in phenol is very low, this method requires the use of the latter in higher molar ratios. Hence, the method of transesterification of methyl salicylate with phenol is employed wherein the reac- tants, being mutually soluble in one another, can be mixed in different molar ratios. Also, the solid acid catalysts that have ...

  5. Solid-Phase Synthesis of PEGylated Lipopeptides Using Click Chemistry

    DEFF Research Database (Denmark)

    Jølck, Rasmus Irming; Berg, Rolf Henrik; Andresen, Thomas Lars

    2010-01-01

    A versatile methodology for efficient synthesis of PEGylated lipopeptides via CuAAC “Click” conjugation between alkyne-bearing solid-supported lipopeptides and azido-functionalized PEGs is described. This new and very robust method offers a unique platform for synthesizing PEGylated lipopeptides...

  6. Kinetics of solid state phase transformations: Measurement and ...

    Indian Academy of Sciences (India)

    Administrator

    in the realm of metals and alloys. While thermody- namics classifies phase changes in terms of the nature of .... structural change in uranium. 9. It is interesting to note that the temperature interval of the two phase ... diagram for the α → β transformation in uranium is shown. The dotted lines represent various heating rates,.

  7. 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.

  8. Formation of soft magnetic high entropy amorphous alloys composites containing in situ solid solution phase

    Science.gov (United States)

    Wei, Ran; Sun, Huan; Chen, Chen; Tao, Juan; Li, Fushan

    2018-03-01

    Fe-Co-Ni-Si-B high entropy amorphous alloys composites (HEAACs), which containing high entropy solid solution phase in amorphous matrix, show good soft magnetic properties and bending ductility even in optimal annealed state, were successfully developed by melt spinning method. The crystallization phase of the HEAACs is solid solution phase with body centered cubic (BCC) structure instead of brittle intermetallic phase. In addition, the BCC phase can transformed into face centered cubic (FCC) phase with temperature rise. Accordingly, Fe-Co-Ni-Si-B high entropy alloys (HEAs) with FCC structure and a small amount of BCC phase was prepared by copper mold casting method. The HEAs exhibit high yield strength (about 1200 MPa) and good plastic strain (about 18%). Meanwhile, soft magnetic characteristics of the HEAs are largely reserved from HEAACs. This work provides a new strategy to overcome the annealing induced brittleness of amorphous alloys and design new advanced materials with excellent comprehensive properties.

  9. Phase transition of solid bismuth under high pressure

    Science.gov (United States)

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

    2016-10-01

    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. Project supported by the National Natural Science Foundation of China (Grant Nos. 10904133, 11304294, 11274281, 11404006, and U1230201), the Development Foundation of China Academy of Engineering Physics (Grant Nos. 2015B0101004, 2013B0401062, and 2012A0101001), the Research Foundation of the Laboratory of Shock Wave and Detonation, China (Grant No. 9140C670201140C67282).

  10. Solid phase transport in series fluidised bed reactors

    International Nuclear Information System (INIS)

    Hayes, M.R.

    1980-01-01

    In a multistage counter-current fluidised bed column, fluidised bed material is recycled within each stage and a fraction is continuously withdrawn to the next lower stage at a rate dependent only on the rate of removal of the fluidised bed material from the base of the column. It has a particular application to the ion exchange treatment of liquids containing suspended solids, for example leach solutions from uranium ores. (author)

  11. Improvements to solid phase phosphotriester synthesis of deoxyoligonucleotides.

    OpenAIRE

    Patel, T P; Millican, T A; Bose, C C; Titmas, R C; Mock, G A; Eaton, M A

    1982-01-01

    A solution of benzenesulphonic acid (3%, w/v) in a dimethylformamide and dichloromethane mixture (9:1, v/v) is shown to be a very effective reagent for the detritylation of deoxyoligonucleotides attached to a solid support. The levels of depurination with this reagent were lower than those observed with other reagents such as trichloroacetic acid. Coupling reactions are described using above ambient temperatures with no detectable increase in side products. Both procedures have been successfu...

  12. Torrefaction Processing for Human Solid Waste Management, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — The NASA SBIR Phase I project addressed the technical feasibility of an innovative torrefaction (mild pyrolysis) processing system that can be used to sterilize...

  13. Non-collinear wave mixing for a bulk wave phase velocity measurement in an isotropic solid

    NARCIS (Netherlands)

    Demcenko, A.

    2013-01-01

    A measurement method is presented to estimate the bulk wave phase velocity in an isotropic solid when longitudinal or shear wave velocity is known. This method is based on the non-collinear plane wave interaction theory and it does not need to estimate the phase time-of-flight and wave propagation

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

    African Journals Online (AJOL)

    This paper examines the performance of a three-phase solid-state var compensator employed in the power system for reactive power compensation. The principal component of this device is a three-phase pulse-width-modulated voltage source inverter. A mathematical model of the inverter is derived and then used for the ...

  15. Stability Analysis of a Three-Phase Solid-State Var Compensator ...

    African Journals Online (AJOL)

    One of the modern devices employed in reactive power compensation is the three-phase solid-statevar compensator (SSVC). The principal component of this device is a three-phase pulse-width-modulated voltage source inverter. A mathematical model of the inverter is derived in d-q referenceframe and then used to ...

  16. Wave propagation in a condensed medium with N transforming phases: application to solid-I--solid-II-liquid bismuth

    International Nuclear Information System (INIS)

    Hayes, D.B.

    1975-01-01

    Constitutive assumptions of local thermal and pressure equilibrium in a mixture of N transforming phases allow construction of a constitutive equation of a generalized Maxwellian form suitable for studying the kinetics of phase transformations induced by shock-wave loading. This equation relates the pressure rate to the strain rate and the phase change rate, the latter being expressed as the time derivative of a vector which has components equal to the mass fractions of the constituent phases. A separate kinetic equation is required for evolution of this composition vector. Coefficients appearing in the constitutive equation depend only on properties that the mixture displays with a frozen composition which in turn depend directly on properties of the pure-phase components of the mixture. The constitutive equation is applied to solid-I--solid-II--liquid bismuth (N = 3). When wave propagation calculations on bismuth are compared with previous theory and experiments, a lower bound on the melting rate of 4 μsec -1 is found

  17. Alkali exchange equilibria between a silicate melt and coexisting magmatic volatile phase: an experimental study at 800°C and 100 MPa

    Science.gov (United States)

    Frank, Mark R.; Candela, Philip A.; Piccoli, Philip M.

    2003-04-01

    Many experimental studies have been performed to evaluate the composition of coexisting silicate melts and magmatic volatile phases (MVP). However, few studies have attempted to define the relationship between melt chemistry and the acidity of a chloride-bearing fluid. Here we report data on melt composition as a function of the HCl concentration of coexisting brines. We performed 35 experimental runs with a NaCl-KCl-HCl-H 2O brine (70 wt% NaCl [equivalent])-silicate melt (starting composition of Qtz 0.38Ab 0.33Or 0.29, anhydrous) assemblage at 800°C and 100 MPa. We determined an apparent equilibrium constant K 'meas (K, Na) =( C Nam× C KClb)/( C NaClb× C Km) for the equilibrium NaCl b+Σ K m=Σ Na m+ KCl b, (where CKClb, CNaClb, CKm, and CNam are total concentrations of potassium and sodium chloride in the brine, and potassium and sodium in the melt, respectively) as a function of the HCl concentration in the brine (C HClb). Although K' meas (K, Na) was not affected by variations in KCl/NaCl of the brine, it did vary inversely with C HClb. The relationship is given by K 'meas (K, Na) = K 'ex (K, Na) + a/C HClb [where C HClb is in wt% and a = 0.03; K' ex (K, Na) = 0.40 ± 0.03 (1σ) and represents the exchange of model sodium and potassium between chloride components in the brine and the aluminate components (NaAlO 2 and KAlO 2) in the melt. This empirical result will be discussed in light of a structural hypothesis; however, validation of the model awaits determinations based on spectroscopy or transport properties-thermodynamic relations alone cannot be used as evidence of structure. The form of this equation is consistent with a model wherein sodium is present in the melt as both sodium aluminate and sodium hydroxide components, and HCl reacts with the NaOH component in the melt to produce NaCl and H 2O. The correlation between fugacity of H 2O ( fH 2Osys), model NaOH m/ΣNa m, aluminum saturation index (ASI), and the ratio (HCl/NaCl) b of an exsolving MVP is

  18. Strong Isotope Effect in Phase II of Dense Solid Hydrogen and Deuterium

    Science.gov (United States)

    Geneste, Grégory; Torrent, Marc; Bottin, François; Loubeyre, Paul

    2012-10-01

    Quantum nuclear zero-point motions in solid H2 and D2 under pressure are investigated at 80 K up to 160 GPa by first-principles path-integral molecular dynamics calculations. Molecular orientations are well defined in phase II of D2, while solid H2 exhibits large and very asymmetric angular quantum fluctuations in this phase, with possible rotation in the (bc) plane, making it difficult to associate a well-identified single classical structure. The mechanism for the transition to phase III is also described. Existing structural data support this microscopic interpretation.

  19. 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

  20. Solid phase extraction of actinides using graphene oxide beads

    International Nuclear Information System (INIS)

    Gujar, R.B.; Mohapatra, P.K.

    2014-01-01

    Separation of actinide ions from dilute nitric acid feed solutions is important from radioactive waste remediation point of view. A large number of separation methods are available in the literature using methods such as precipitation, ion-exchange, solvent extraction, etc. Graphene oxide (GO) are reported to be a very good sorbent for actinide ions from weakly acidic feed solutions. However, it is difficult to handle GO fine particles and any chromatographic separation is bound to be difficult as the sorbent material may be finely dispersed in the aqueous phase. It was thus thought of interest to prepare GO-based resin materials in polyether sulphone (PES) by phase inversion technique. Preparation of resins by phase inversion technique has been found to be quite efficient for metal ion separation including actinide ions. In the present work, GO based PES resin beads were prepared by phase inversion technique and the uptake of actinide and lanthanide ions. In the present work, GO based beads were prepared by phase inversion technique and the uptake of actinide and lanthanide ions (such as Am(III), Eu(III), Th(IV), Pu(IV) and U(VI)) has been studied using radiotracers

  1. Improvements to solid phase phosphotriester synthesis of deoxyoligonucleotides.

    Science.gov (United States)

    Patel, T P; Millican, T A; Bose, C C; Titmas, R C; Mock, G A; Eaton, M A

    1982-09-25

    A solution of benzenesulphonic acid (3%, w/v) in a dimethylformamide and dichloromethane mixture (9:1, v/v) is shown to be a very effective reagent for the detritylation of deoxyoligonucleotides attached to a solid support. The levels of depurination with this reagent were lower than those observed with other reagents such as trichloroacetic acid. Coupling reactions are described using above ambient temperatures with no detectable increase in side products. Both procedures have been successfully incorporated into an automated system, which can compete with the rate of synthesis by the phosphite approach.

  2. Crystalline-to-plastic phase transitions in molecularly thin n-dotriacontane films adsorbed on solid surfaces

    DEFF Research Database (Denmark)

    Cisternas, Edgardo; Corrales, T. P.; del Campo, V.

    2009-01-01

    Crystalline-to-rotator phase transitions have been widely studied in bulk hydrocarbons, in particular in normal alkanes. But few studies of these transitions deal with molecularly thin films of pure n-alkanes on solid substrates. In this work, we were able to grow dotriacontane (n-C32H66) films...... identify with a solid-solid phase transition. At higher coverages, we observed additional steps in the ellipsometric signal that we identify with a solid-solid phase transition in multilayer islands (similar to 333 K) and with the transition to the rotator phase in bulk crystallites (similar to 337 K...

  3. A review on solid phase extraction of actinides and lanthanides with amide based extractants.

    Science.gov (United States)

    Ansari, Seraj A; Mohapatra, Prasanta K

    2017-05-26

    Solid phase extraction is gaining attention from separation scientists due to its high chromatographic utility. Though both grafted and impregnated forms of solid phase extraction resins are popular, the later is easy to make by impregnating a given organic extractant on to an inert solid support. Solid phase extraction on an impregnated support, also known as extraction chromatography, combines the advantages of liquid-liquid extraction and the ion exchange chromatography methods. On the flip side, the impregnated extraction chromatographic resins are less stable against leaching out of the organic extractant from the pores of the support material. Grafted resins, on the other hand, have a higher stability, which allows their prolong use. The goal of this article is a brief literature review on reported actinide and lanthanide separation methods based on solid phase extractants of both the types, i.e., (i) ligand impregnation on the solid support or (ii) ligand functionalized polymers (chemically bonded resins). Though the literature survey reveals an enormous volume of studies on the extraction chromatographic separation of actinides and lanthanides using several extractants, the focus of the present article is limited to the work carried out with amide based ligands, viz. monoamides, diamides and diglycolamides. The emphasis will be on reported applied experimental results rather than on data pertaining fundamental metal complexation. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    African Journals Online (AJOL)

    phase high performance liquid chromatography (RP-HPLC) to determine mitragynine (MG) in rat and human urine, and to investigate the influence of caffeine (CF) on urinary excretion of MG in rats. Methods: A two-dimensional wash-elute ...

  5. A molecular dynamics calculation of solid phase of malonic acid ...

    Indian Academy of Sciences (India)

    Recent studies suggest that hydrogen bonds, in particular, hydrogen bond chains play an important role in determining the properties of a substance.We report an investigation into the triclinic phase of crystalline malonic acid. One of two intermolecular interaction potentials proposed here is seen to predict the lattice ...

  6. Kinetics of solid state phase transformations: Measurement and ...

    Indian Academy of Sciences (India)

    Administrator

    This latter quan- tity that may be obtained from equilibrium phase diagram (lever rule) or may be set as an internal ref- erence value which is obtained under very slow heating or cooling conditions. A rough estimate of τ. (assumed to be β independent in the trial estimation) can be obtained from the experimental data using.

  7. Model Dust Envelopes Around Silicate Carbon Stars

    Directory of Open Access Journals (Sweden)

    Kyung-Won Suh

    2006-03-01

    Full Text Available We have modeled dust envelopes around silicate carbon stars using optical properties for a mixture of amorphous carbon and silicate dust grains paying close attention to the infrared observations of the stars. The 4 stars show various properties in chemistry and location of the dust shell. We expect that the objects that fit a simple detached silicate dust shell model could be in the transition phase of the stellar chemistry. For binary system objects, we find that a mixed dust chemistry model would be necessary.

  8. Synthesis of pure Portland cement phases

    DEFF Research Database (Denmark)

    Wesselsky, Andreas; Jensen, Ole Mejlhede

    2009-01-01

    Pure phases commonly found in Portland cement clinkers are often used to test cement hydration behaviour in simplified experimental conditions. The synthesis of these phases is covered in this paper, starting with a description of phase relations and possible polymorphs of the four main phases...... in Portland cement, i.e. tricalcium silicate, dicalcium silicate, tricalcium aluminate and tetracalcium alumino ferrite. Details of the The process of solid state synthesis are is described in general including practical advice on equipment and techniques. Finally In addition, some exemplary mix compositions...

  9. Viscosity of Heterogeneous Silicate Melts: A Non-Newtonian Model

    Science.gov (United States)

    Liu, Zhuangzhuang; Blanpain, Bart; Guo, Muxing

    2017-12-01

    The recently published viscosity data of heterogeneous silicate melts with well-documented structure and experimental conditions are critically re-analyzed and tabulated. By using these data, a non-Newtonian viscosity model incorporating solid fraction, solid shape, and shear rate is proposed on the basis of the power-law equation. This model allows calculating the viscosity of the heterogeneous silicate melts with solid fraction up to 34 vol pct. The error between the calculated and measured data is evaluated to be 32 pct, which is acceptable considering the large error in viscosity measurement of the completely liquid silicate melt.

  10. Enhanced denitrification of Pseudomonas stutzeri by a bioelectrochemical system assisted with solid-phase humin.

    Science.gov (United States)

    Xiao, Zhixing; Awata, Takanori; Zhang, Dongdong; Zhang, Chunfang; Li, Zhiling; Katayama, Arata

    2016-07-01

    The denitrification reactions performed by Pseudomonas stutzeri JCM20778 were enhanced electrochemically with the use of solid-phase humin, although P. stutzeri itself was incapable of receiving electrons directly from the graphite electrode. Electrochemically reduced humin enhanced the microbial, but not abiotic, denitrification reactions. Electric current and cyclic voltammetry analyses suggested that the solid-phase humin functioned as an electron donor for the denitrification reactions of P. stutzeri. Nitrogen balance study and the estimation of the first-order rate constants of the consecutive denitrification reactions suggested that the solid-phase humin enhanced all reducing reactions from nitrate to nitrogen gas. Considering the wide distribution of humin in the environment, the findings that solid-phase humin can assist in electron transfer, from the electrode to a denitrifying bacterium that has little ability to directly utilize external electrons, has important implications for the widespread application of bioelectrochemical systems assisted by solid-phase humin for enhancing microbial denitrification. Copyright © 2015 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

  11. 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

  12. Solid State KA-Band, Solid State W-Band and TWT Amplifiers, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Phase I of the proposal describes plans to develop a state of the art transmitter for the W-Band and KA -Band Cloud Radar system. Our focus will be concentrated in...

  13. The synthesis and properties of the phases obtained by solid-solid reactions

    Directory of Open Access Journals (Sweden)

    Blonska-Tabero A.

    2008-01-01

    Full Text Available The presented work encompasses the subject of the studies and the results obtained over the last years by the research workers of the Department of Inorganic Chemistry. They include mainly the studies on the reactivity of metal oxides, searching for new phases in binary and ternary systems of metal oxides as well as describing phase relations establishing in such systems. They also encompass works on the extensive characteristics of physico-chemical properties of the newly obtained compounds.

  14. Functional Ceramic Ferroelectromagnetic Materials in Single Phase Solid-Solutions

    Science.gov (United States)

    2007-12-05

    PbTiO3)1-x, where x= 0.10, 0.20, 0.30, 0.40, 0.67. ( work is still going on) Introduction: Recently BaTiO3 is doped with Ni and Co to get...xBaxMnO3 was expected to enhance the magnetic properties. LaMnO3 is an antiferromagnetic insulator and have cubic perovskite structure. The doping with...research in solid solutions like x (BiFeO3)-(1-x) (PbTiO3) ( BF-PT), BiFeO3- BaTiO3 , BiFeO3- Pb(FeNb)O3, BiFeO3-ReFeO3- BaTiO3 .Mainly the aim of the

  15. Solid-phase synthesis of polyamine toxin analogues

    DEFF Research Database (Denmark)

    Kromann, Hasse; Krikstolaityte, Sonata; Andersen, Anne J

    2002-01-01

    The wasp toxin philanthotoxin-433 (PhTX-433) is a nonselective and noncompetitive antagonist of ionotropic receptors, such as ionotropic glutamate receptors and nicotinic acetylcholine receptors. Polyamine toxins are extensively used for the characterization of subtypes of ionotropic glutamate...... receptors, in particular Ca(2+)-permeable AMPA and kainate receptors. We have previously shown that an analogue of PhTX-433 with one of the amino groups replaced by a methylene group, philanthotoxin-83 (PhTX-83) is a selective and potent antagonist of AMPA receptors. We now describe the solid...... of analogues, the acyl moiety of PhTX-83 was replaced by acids of different size and lipophilicity. Using electrophysiological techniques, PhTX-56 was shown to be a highly potent (K(i) = 3.3 +/- 0.78 nM) and voltage-dependent antagonist of homomeric GluR1 receptors and was more than 1000-fold less potent when...

  16. 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.

  17. Dielectric Property of Silicate-Doped CaBi4Ti4O15 Thin Films

    Science.gov (United States)

    Ogawa, Shota; Kondoh, Yohta; Kimura, Junichi; Funakubo, Hiroshi; Uchida, Hiroshi

    2012-09-01

    Thin films of silicate-doped CaBi4Ti4O15 were fabricated to enhance the insulating property of one-axis-oriented CaBi4Ti4O15 films under an applied electric field. The crystalline phase of CaBi4Ti4O15, a type of bismuth layer-structured dielectric (BLSD) compound, was successfully grown on (100)LaNiO3/(111)Pt/TiO2/(100)Si with the preferential orientation of the (001) plane by the addition of bismuth silicate with a nominal composition of Bi12SiO20 up to 1.00%. The crystallographic orientation of the (001)BLSD plane normal to the substrate surface was degraded by excessive bismuth silicate addition above 1.50%. The breakdown electric field was increased by bismuth silicate addition up to 2.00% without the degraded relative dielectric permittivity (ɛr) of approximately 230. The bismuth silicate could precipitate between the grain boundaries in the CaBi4Ti4O15 films without an interface reaction or a solid solution that enhances the insulating behavior of the BLSD films.

  18. 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

  19. 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.

  20. 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.

  1. 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

  2. Use of solid-phase inhomogeneities to increase the efficiency of ultrasonic therapy of oncological diseases

    Science.gov (United States)

    Nikolaev, A. L.; Gopin, A. V.; Bozhevol'Nov, V. E.; Treshchalina, E. M.; Andronova, N. V.; Melikhov, I. V.

    2009-10-01

    Authors’ concepts on the use of solid-phase sonosensitizer nanoinclusions in biological structures as ultrasonic energy concentrators in the therapy of oncological diseases are developed. The possibility of directed synthesis of nanoparticles and their aggregates in tumor tissue depending on its growth features is discussed. It was found that acoustic effects in polymer structures containing solid-phase inclusions depend on the nature of these inclusions and their bond with the polymer matrix. Using model gel systems, it was shown that solid-phase sonosensitizers enhance local thermal effects and amplitude-dependent scattering of ultrasound during its propagation in gel. Experimental studies on animals showed that the ultrasound exposure of malignant tumors containing nanoparticles of gold and some complex compounds results in a significant therapeutic effect.

  3. 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)

  4. Solid-Phase Synthesis of Amine/Carboxyl Substituted Prolines and Proline Homologues: Scope and Limitations.

    Science.gov (United States)

    Zhou, Ziniu; Scott, William L; O'Donnell, Martin J

    2016-03-15

    A solid-phase procedure is used to synthesize racemic peptidomimetics based on the fundamental peptide unit. The peptidomimetics are constructed around proline or proline homologues variably substituted at the amine and carbonyl sites. The procedure expands the diversity of substituted peptidomimetic molecules available to the Distributed Drug Discovery (D3) project. Using a BAL-based solid-phase synthetic sequence the proline or proline homologue subunit is both constructed and incorporated into the peptidomimetic by an α-alkylation, hydrolysis and intramolecular cyclization sequence. Further transformations on solid-phase provide access to a variety of piperazine derivatives representing a class of molecules known to exhibit central nervous system activity. The procedure works well with proline cores, but with larger six- and seven-membered ring homologues the nature of the carboxylic acid acylating the cyclic amine can lead to side reactions and result in poor overall yields.

  5. Solid-Phase Synthesis of Amine/Carboxyl Substituted Prolines and Proline Homologues: Scope and Limitations

    Directory of Open Access Journals (Sweden)

    Ziniu Zhou

    2016-03-01

    Full Text Available A solid-phase procedure is used to synthesize racemic peptidomimetics based on the fundamental peptide unit. The peptidomimetics are constructed around proline or proline homologues variably substituted at the amine and carbonyl sites. The procedure expands the diversity of substituted peptidomimetic molecules available to the Distributed Drug Discovery (D3 project. Using a BAL-based solid-phase synthetic sequence the proline or proline homologue subunit is both constructed and incorporated into the peptidomimetic by an α-alkylation, hydrolysis and intramolecular cyclization sequence. Further transformations on solid-phase provide access to a variety of piperazine derivatives representing a class of molecules known to exhibit central nervous system activity. The procedure works well with proline cores, but with larger six- and seven-membered ring homologues the nature of the carboxylic acid acylating the cyclic amine can lead to side reactions and result in poor overall yields.

  6. Silicate volcanism on Io

    Science.gov (United States)

    Carr, M. H.

    1986-03-01

    This paper is mainly concerned with the nature of volcanic eruptions on Io, taking into account questions regarding the presence of silicates or sulfur as principal component. Attention is given to the generation of silicate magma, the viscous dissipation in the melt zone, thermal anomalies at eruption sites, and Ionian volcanism. According to the information available about Io, it appears that its volcanism and hence its surface materials are dominantly silicic. Several percent of volatile materials such as sulfur, but also including sodium- and potassium-rich materials, may also be present. The volatile materials at the surface are continually vaporized and melted as a result of the high rates of silicate volcanism.

  7. [Solid phase reaction of hemoglobin with spillover hydrogen].

    Science.gov (United States)

    Zolotarev, Iu A; Dadaian, A K; Ziganshin, R Kh; Borisov, Iu A; Kozik, V S; Dorokhova, E M; Vas'kovskiĭ, B V; Miasoedov, N F

    2009-01-01

    The reaction of high-temperature solid-state catalytic isotope exchange (HSCIE) between bovine hemoglobin and spillover hydrogen (SH) was studied. It was shown that, in the field of subunit contact, there is a significant decrease in ability for hydrogen exchange by SH. A comparison of the distribution of the isotope label in the hemoglobin alpha-subunit was carried out for the HSCIE reaction with the hemoglobin complex and with the free alpha-subunit. To this end, enzymatic hydrolysis of protein under the action of trypsin was carried out. The separation of tritium-labeled tryptic peptides was achieved by HPLC. Changes in availability of polypeptide chain fragments caused by complex formation were calculated using a molecular model. The formation of the protein complex was shown to lead to a decrease in the ability of fragments of alpha-subunits MFLSFPTTK (A(32-40)) and VDPVNFK (A(93-99)) for hydrogen replacement by tritium by almost an order of magnitude; hence, their availability to water (1.4 A) twice decreased on the average. The decrease in ability to an exchange of hydrogen by spillover tritium on the formation of hemoglobin complex was shown to be connected with a reduction in availability of polypeptide chain fragments participating in spatial interactions of subunits with each other. Thus, the HSCIE reaction can be used not only for the preparative obtaining of tritium-labeled compounds, but also for determining the contact area in the formation of protein complexes.

  8. Soft x-ray induced femtosecond solid-to-solid phase transition

    Czech Academy of Sciences Publication Activity Database

    Tavella, F.; Höppner, H.; Tkachenko, V.; Medvedev, Nikita; Capotondi, F.; Golz, T.; Kai, Y.; Manfredda, M.; Pedersoli, E.; Prandolini, M.J.; Stojanovic, N.; Tanikawa, T.; Teubner, U.; Toleikis, S.; Ziaja, B.

    2017-01-01

    Roč. 24, Sep (2017), s. 22-27 ISSN 1574-1818 Institutional support: RVO:68378271 Keywords : soft x-ray * ultrashort x-ray pulses * grafitization of diamond * non-thermal phase transition Subject RIV: BL - Plasma and Gas Discharge Physics OBOR OECD: Fluids and plasma physics (including surface physics) Impact factor: 0.908, year: 2016

  9. Finite-deformation phase-field chemomechanics for multiphase, multicomponent solids

    Science.gov (United States)

    Svendsen, Bob; Shanthraj, Pratheek; Raabe, Dierk

    2018-03-01

    The purpose of this work is the development of a framework for the formulation of geometrically non-linear inelastic chemomechanical models for a mixture of multiple chemical components diffusing among multiple transforming solid phases. The focus here is on general model formulation. No specific model or application is pursued in this work. To this end, basic balance and constitutive relations from non-equilibrium thermodynamics and continuum mixture theory are combined with a phase-field-based description of multicomponent solid phases and their interfaces. Solid phase modeling is based in particular on a chemomechanical free energy and stress relaxation via the evolution of phase-specific concentration fields, order-parameter fields (e.g., related to chemical ordering, structural ordering, or defects), and local internal variables. At the mixture level, differences or contrasts in phase composition and phase local deformation in phase interface regions are treated as mixture internal variables. In this context, various phase interface models are considered. In the equilibrium limit, phase contrasts in composition and local deformation in the phase interface region are determined via bulk energy minimization. On the chemical side, the equilibrium limit of the current model formulation reduces to a multicomponent, multiphase, generalization of existing two-phase binary alloy interface equilibrium conditions (e.g., KKS). On the mechanical side, the equilibrium limit of one interface model considered represents a multiphase generalization of Reuss-Sachs conditions from mechanical homogenization theory. Analogously, other interface models considered represent generalizations of interface equilibrium conditions consistent with laminate and sharp-interface theory. In the last part of the work, selected existing models are formulated within the current framework as special cases and discussed in detail.

  10. Application of solid phase extraction procedures for rare earth elements determination in environmental samples.

    Science.gov (United States)

    Pyrzynska, Krystyna; Kubiak, Anna; Wysocka, Irena

    2016-07-01

    Determination of rare earth elements in environmental samples requires often pre-concentration and separation step due to a low metal content and high concentration of the interfering matrix components. A solid phase extraction technique with different kind of solid sorbents offers a high enrichment factor, rapid phase separation and the possibility of its combination with various detection techniques used either in on-line or off-line mode. The recent developments in this area published over the last five years are presented and discussed in this paper. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Synthesis of a Small Library of Imidazolidin-2-ones using Gold Catalysis on Solid Phase.

    Science.gov (United States)

    La-Venia, Agustina; Medran, Noelia S; Krchňák, Viktor; Testero, Sebastián A

    2016-08-08

    An efficient and high-yielding solid phase synthesis of a small library of imidazolidin-2-ones and imidazol-2-ones was carried out employing a high chemo- and regioselective gold-catalyzed cycloisomerization as a key step. Polymer-supported amino acids derivatized with several alkyne functionalities combined with tosyl- and phenylureas have been subjected to gold-catalysis exhibiting exclusively C-N bond formation. The present work proves the potential of solid phase synthesis and homogeneous gold catalysis as an efficient and powerful synthetic tool for the generation of drug-like heterocycles.

  12. Strong Isotopic Effect in Phase II of Dense Solid Hydrogen and Deuterium

    OpenAIRE

    Geneste, Grégory; Torrent, Marc; Bottin, François; Loubeyre, Paul

    2012-01-01

    Quantum nuclear zero-point motions in solid H$_2$ and D$_2$ under pressure are investigated at 80 K up to 160 GPa by first-principles path-integral molecular dynamics calculations. Molecular orientations are well-defined in phase II of D$_2$, while solid H$_2$ exhibits large and very asymmetric angular quantum fluctuations in this phase, with possible rotation in the (bc) plane, making it difficult to associate a well-identified single classical structure. The mechanism for the transition to ...

  13. Use of the 2-chlorotrityl chloride resin for microwave-assisted solid phase peptide synthesis.

    Science.gov (United States)

    Ieronymaki, Matthaia; Androutsou, Maria Eleni; Pantelia, Anna; Friligou, Irene; Crisp, Molly; High, Kirsty; Penkman, Kirsty; Gatos, Dimitrios; Tselios, Theodore

    2015-09-01

    A fast and efficient microwave (MW)-assisted solid-phase peptide synthesis protocol using the 2-chlorotrityl chloride resin and the Fmoc/tBu methodology, has been developed. The established protocol combines the advantages of MW irradiation and the acid labile 2-chlorotrityl chloride resin. The effect of temperature during the MW irradiation, the degree of resin substitution during the coupling of the first amino acids and the rate of racemization for each amino acid were evaluated. The suggested solid phase methodology is applicable for orthogonal peptide synthesis and for the synthesis of cyclic peptides. © 2015 Wiley Periodicals, Inc.

  14. Modeling of Thermal Phase Noise in a Solid Core Photonic Crystal Fiber-Optic Gyroscope.

    Science.gov (United States)

    Song, Ningfang; Ma, Kun; Jin, Jing; Teng, Fei; Cai, Wei

    2017-10-26

    A theoretical model of the thermal phase noise in a square-wave modulated solid core photonic crystal fiber-optic gyroscope has been established, and then verified by measurements. The results demonstrate a good agreement between theory and experiment. The contribution of the thermal phase noise to the random walk coefficient of the gyroscope is derived. A fiber coil with 2.8 km length is used in the experimental solid core photonic crystal fiber-optic gyroscope, showing a random walk coefficient of 9.25 × 10 -5 deg/√h.

  15. Novel functionalized polymeric fabric and fiber material as solid support for solid-phase synthesis and biomedical applications

    Science.gov (United States)

    Xiang, Bei

    The aim of the research is to develop novel polymer solid support by modifying or fabricating polymeric fibrous materials for peptide synthesis and biomedical applications. Originally chemical inert isotactic polypropylene (iPP) fabric was utilized and modified to serve as a functional flexible planar solid support for solid phase peptide synthesis. The modification was achieved through thermal initiated radical grafting polymerization using acrylic acid, poly (ethylene glycol) diacrylate as monomers, and benzoyl peroxide as radical initiator. The iPP fabric was successfully functionalized and possessing as high as 0.7mmol/g carboxylic acid groups. Peptide ligand LHPQF was successfully synthesized on the new functional planar support. Specific enzyme immobilization was fulfilled on the functional iPP fabric support. A commercially available ethylene-acrylic acid copolymer was made into ultrafine copolymer fiber bundles which are composed of nanofibers with diameters ranging from 200nm to 800nm. Various mixing ratios of copolymer/matrix materials were utilized to explore the effect on the final nanofiber physical properties including morphology and stability in solvents. The surface carboxylic acid groups were further converted to amino groups before the functional nanofibers can be applied in solid phase peptide synthesis. Two peptide ligands, LHPQF and HWRGWV, were also successfully synthesized on the nanofiber bundles. Streptavidin and human immunoglobulin G specific binding with the corresponding ligand which was anchored on the nanofibers was conducted successfully to illustrate the potential applications of the nanofiber materials in biomedical field. Further study on the dispersion of the ethylene-acrylic acid nanofiber bundles was pursued to take advantage of the super high active surface area of functional nanofibers. To manipulate the polymer nanofibers during synthesis and bio-assays, a technique was developed to controllably assemble and disperse the

  16. The Chemistry, Crystallization, Physicochemical Properties and Behavior of Sodium Aluminosilicate Solid Phases: Final Report

    International Nuclear Information System (INIS)

    Rosencrance, S.

    2003-01-01

    The synthesis of sodium aluminosilicate solids phases precipitated from NO 2 /NO 3 -free and NO 2 /NO 3 -rich liquors has been performed. Four sodium aluminosilicate precipitation products were formed. These are (1) X-ray/electron diffraction-indifferent amorphous phase; (2) crystalline zeolite A; (3)NO 2 /NO 3 -rich crystalline sodalite; and (4) NO 2 /NO 3 -rich crystalline cancrinite phase. Characterization of the physicochemical properties for these phases has been performed under conditions simulating Westinghouse Savannah River Company liquid waste processing

  17. Thermally stable coexistence of liquid and solid phases in gallium nanoparticles

    Science.gov (United States)

    Losurdo, Maria; Suvorova, Alexandra; Rubanov, Sergey; Hingerl, Kurt; Brown, April S.

    2016-09-01

    Gallium (Ga), a group III metal, is of fundamental interest due to its polymorphism and unusual phase transition behaviours. New solid phases have been observed when Ga is confined at the nanoscale. Herein, we demonstrate the stable coexistence, from 180 K to 800 K, of the unexpected solid γ-phase core and a liquid shell in substrate-supported Ga nanoparticles. We show that the support plays a fundamental role in determining Ga nanoparticle phases, with the driving forces for the nucleation of the γ-phase being the Laplace pressure in the nanoparticles and the epitaxial relationship of this phase to the substrate. We exploit the change in the amplitude of the evolving surface plasmon resonance of Ga nanoparticle ensembles during synthesis to reveal in real time the solid core formation in the liquid Ga nanoparticle. Finally, we provide a general framework for understanding how nanoscale confinement, interfacial and surface energies, and crystalline relationships to the substrate enable and stabilize the coexistence of unexpected phases.

  18. 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

  19. CO2 sequestration by magnesium silicate mineral carbonation in Finland

    International Nuclear Information System (INIS)

    Zevenhoven, R.; Kohlmann, J.

    2001-01-01

    Fixation Of CO 2 from fossil fuel combustion in the form of solid carbonates appears to be a realistic option for the capture and storage of this greenhouse gas. Vast amounts of magnesium silicate minerals exist worldwide that may be carbonated, with magnesium carbonate as stable and environmentally harmless product. Also in Finland magnesium silicate resources exist that could support Finnish commitments under the Kyoto Protocol. This paper describes the option Of CO 2 sequestration with magnesium silicates in Finland. Addressed are mineral resources, mineral quality and the mineral carbonation process, including some experimental results on magnesium silicate carbonation kinetics

  20. 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.

  1. 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.

  2. 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.

  3. Thermodynamics and Kinetics of Silicate Vaporization

    Science.gov (United States)

    Jacobson, Nathan S.; Costa, Gustavo C. C.

    2015-01-01

    Silicates are a common class of materials that are often exposed to high temperatures. The behavior of these materials needs to be understood for applications as high temperature coatings in material science as well as the constituents of lava for geological considerations. The vaporization behavior of these materials is an important aspect of their high temperature behavior and it also provides fundamental thermodynamic data. The application of Knudsen effusion mass spectrometry (KEMS) to silicates is discussed. There are several special considerations for silicates. The first is selection of an appropriate cell material, which is either nearly inert or has well-understood interactions with the silicate. The second consideration is proper measurement of the low vapor pressures. This can be circumvented by using a reducing agent to boost the vapor pressure without changing the solid composition or by working at very high temperatures. The third consideration deals with kinetic barriers to vaporization. The measurement of these barriers, as encompassed in a vaporization coefficient, is discussed. Current measured data of rare earth silicates for high temperature coating applications are discussed. In addition, data on magnesium-iron-silicates (olivine) are presented and discussed.

  4. Nanostructured silicate polymer concrete

    Directory of Open Access Journals (Sweden)

    Figovskiy Oleg L'vovich

    2014-03-01

    Full Text Available It has been known that acid-resistant concretes on the liquid glass basis have high porosity (up to 18~20 %, low strength and insufficient water resistance. Significant increasing of silicate matrix strength and density was carried out by incorporation of special liquid organic alkali-soluble silicate additives, which block superficial pores and reduce concrete shrinkage deformation. It was demonstrated that introduction of tetrafurfuryloxisilane additive sharply increases strength, durability and shock resistance of silicate polymer concrete in aggressive media. The experiments showed, that the strength and density of silicate polymer concrete increase in case of decreasing liquid glass content. The authors obtained optimal content of silicate polymer concrete, which possesses increased strength, durability, density and crack-resistance. Diffusive permeability of concrete and its chemical resistance has been investigated in various corroding media.

  5. Solid-Phase Organic Synthesis and Catalysis: Some Recent Strategies Using Alumina, Silica, and Polyionic Resins

    Directory of Open Access Journals (Sweden)

    Basudeb Basu

    2013-01-01

    Full Text Available Solid-phase organic synthesis (SPOS and catalysis have gained impetus after the seminal discovery of Merrifield’s solid-phase peptide synthesis and also because of wide applicability in combinatorial and high throughput chemistry. A large number of organic, inorganic, or organic-inorganic hybrid materials have been employed as polymeric solid supports to promote or catalyze various organic reactions. This review article provides a concise account on our approaches involving the use of (i alumina or silica, either having doped with metal salts or directly, and (ii polyionic resins to either promote various organic reactions or to immobilize reagents/metal catalysts for subsequent use in hydrogenation and cross-coupling reactions. The reaction parameters, scopes, and limitations, particularly in the context of green chemistry, have been highlighted with pertinent approaches by other groups.

  6. Regularities in Low-Temperature Phosphatization of Silicates

    Science.gov (United States)

    Savenko, A. V.

    2018-01-01

    The regularities in low-temperature phosphatization of silicates are defined from long-term experiments on the interaction between different silicate minerals and phosphate-bearing solutions in a wide range of medium acidity. It is shown that the parameters of the reaction of phosphatization of hornblende, orthoclase, and labradorite have the same values as for clayey minerals (kaolinite and montmorillonite). This effect may appear, if phosphotization proceeds, not after silicate minerals with a different structure and composition, but after a secondary silicate phase formed upon interaction between silicates and water and stable in a certain pH range. Variation in the parameters of the reaction of phosphatization at pH ≈ 1.8 is due to the stability of the silicate phase different from that at higher pH values.

  7. Solid-phase synthesis of head and tail bis-acridinylated peptides

    Czech Academy of Sciences Publication Activity Database

    Šebestík, Jaroslav; Matějka, P.; Hlaváček, Jan; Stibor, I.

    2004-01-01

    Roč. 45, č. 6 (2004), s. 1203-1205 ISSN 0040-4039 R&D Projects: GA ČR GA203/02/1379 Institutional research plan: CEZ:AV0Z4055905 Keywords : 9-amino acridine * solid phase synthesis * head and tail peptide conjugates Subject RIV: CC - Organic Chemistry Impact factor: 2.484, year: 2004

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

    CSIR Research Space (South Africa)

    Mtshali, TN

    2012-11-01

    Full Text Available 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...

  9. Solid-phase synthesis of an apoptosis-inducing tetrapeptide mimicking the Smac protein

    DEFF Research Database (Denmark)

    Le Quement, Sebastian Thordal; Ishøy, Mette; Petersen, Mette Terp

    2011-01-01

    An approach for the solid-phase synthesis of apoptosis-inducing Smac peptidomimetics is presented. Using a Rink linker strategy, tetrapeptides mimicking the N-4-terminal residue of the Smac protein [(N-Me)AVPF sequence] were synthesized on PEGA resin in excellent purities and yields. Following two...

  10. Solid-gaseous phase transformation of elemental contaminants during the gasification of biomass.

    Science.gov (United States)

    Jiang, Ying; Ameh, Abiba; Lei, Mei; Duan, Lunbo; Longhurst, Philip

    2016-09-01

    Disposal of plant biomass removed from heavy metal contaminated land via gasification achieves significant volume reduction and can recover energy. However, these biomass often contain high concentrations of heavy metals leading to hot-corrosion of gasification facilities and toxic gaseous emissions. Therefore, it is of significant interest to gain a further understanding of the solid-gas phase transition of metal(loid)s during gasification. Detailed elemental analyses (C, H, O, N and key metal/metalloid elements) were performed on five plant species collected from a contaminated site. Using multi-phase equilibria modelling software (MTDATA), the analytical data allows modelling of the solid/gas transformation of metal(loid)s during gasification. Thermodynamic modelling based on chemical equilibrium calculations was carried out in this study to predict the fate of metal(loid) elements during typical gasification conditions and to show how these are influenced by metal(loid) composition in the biomass and operational conditions. As, Cd, Zn and Pb tend to transform to their gaseous forms at relatively low temperatures (gasification temperature range of 1000-1200°C. Whereas Cr, Al, Fe and Mg remain in solid phase at higher temperatures (>1200°C). Simulation of pressurised gasification conditions shows that higher pressures increase the temperature at which solid-to-gaseous phase transformations takes place. Copyright © 2015 The Authors. Published by Elsevier B.V. All rights reserved.

  11. Solution and solid-phase halogen and C-H hydrogen bonding to perrhenate.

    Science.gov (United States)

    Massena, Casey J; Riel, Asia Marie S; Neuhaus, George F; Decato, Daniel A; Berryman, Orion B

    2015-01-28

    (1)H NMR spectroscopic and X-ray crystallographic investigations of a 1,3-bis(4-ethynyl-3-iodopyridinium)benzene scaffold with perrhenate reveal strong halogen bonding in solution, and bidentate association in the solid state. A nearly isostructural host molecule demonstrates significant C-H hydrogen bonding to perrhenate in the same phases.

  12. Speciation analysis of aqueous nanoparticulate diclofenac complexes by solid-phase microextraction

    NARCIS (Netherlands)

    Zielinska, K.; Leeuwen, van H.P.; Thibault, S.; Town, R.M.

    2012-01-01

    The dynamic sorption of an organic compound by nanoparticles (NPs) is analyzed by solid-phase microextraction (SPME) for the example case of the pharmaceutical diclofenac in dispersions of impermeable (silica, SiO(2)) and permeable (bovine serum albumin, BSA) NPs. It is shown that only the

  13. Solid phase extraction of trace amounts of zinc and cadmium ions ...

    African Journals Online (AJOL)

    ... and determination of the zinc and cadmium ions in the water and food samples and satisfactory results were obtained. KEY WORDS: Solid phase extraction, Zinc determination, Cadmium determination, Preconcentration, Perlite. Bull. Chem. Soc. Ethiop. 2016, 30(2), 175-184. DOI: http://dx.doi.org/10.4314/bcse.v30i2.2 ...

  14. A convenient procedure for the solid-phase synthesis of hydroxamic acids on PEGA resins

    DEFF Research Database (Denmark)

    Nandurkar, Nitin Subhash; Petersen, Rico; Qvortrup, Katrine

    2011-01-01

    An efficient method for the solid-phase synthesis of hydroxamic acids is described. The method comprises the nucleophilic displacement of esters immobilized on PEGA resins with hydroxylamine/sodium hydroxide in isopropanol. The hydroxyaminolysis protocol is compatible with a broad range of PEGA...

  15. 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...

  16. Linkers, resins, and general procedures for solid-phase peptide synthesis

    DEFF Research Database (Denmark)

    Shelton, Anne Pernille Tofteng; Jensen, Knud Jørgen

    2013-01-01

    and linkers for solid-phase synthesis is a key parameter for successful peptide synthesis. This chapter provides an overview of the most common and useful resins and linkers for the synthesis of peptides with C-terminal amides, carboxylic acids, and more. The chapter finishes with robust protocols for general...

  17. Solid-phase extraction of berries’ anthocyanins and evaluation of their antioxidative properties

    Czech Academy of Sciences Publication Activity Database

    Denev, P.; Číž, Milan; Ambrožová, Gabriela; Lojek, Antonín; Yanakieva, I.; Kratchanova, M.

    2010-01-01

    Roč. 123, č. 4 (2010), s. 1055-1061 ISSN 0308-8146 R&D Projects: GA MŠk(CZ) OC08058 Institutional research plan: CEZ:AV0Z50040507; CEZ:AV0Z50040702 Keywords : anthocyanins * solid-phase extraction * berry extracts Subject RIV: BO - Biophysics Impact factor: 3.458, year: 2010

  18. Crystalline CoFeB/graphite interfaces for carbon spintronics fabricated by solid phase epitaxy

    NARCIS (Netherlands)

    Wong, P.K.J.; van Geijn, Elmer; van Geijn, E.; Zhang, W.; Starikov, A.A.; Tran, T. Lan Ahn; Sanderink, Johannes G.M.; Siekman, Martin Herman; Brocks, Gerardus H.L.A.; Kelly, Paul J.; van der Wiel, Wilfred Gerard; de Jong, Machiel Pieter

    2013-01-01

    Structurally ordered interfaces between ferromagnetic electrodes and graphene or graphite are of great interest for carbon spintronics, since they allow spin-filtering due to k-vector conservation. By solid phase epitaxy of amorphous/nanocrystalline CoFeB at elevated temperatures, the feasibility of

  19. 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

  20. Investigating the Retention Mechanisms of Liquid Chromatography Using Solid-Phase Extraction Cartridges

    Science.gov (United States)

    O'Donnell, Mary E.; Musial, Beata A.; Bretz, Stacey Lowery; Danielson, Neil D.; Ca, Diep

    2009-01-01

    Liquid chromatography (LC) experiments for the undergraduate analytical laboratory course often illustrate the application of reversed-phase LC to solve a separation problem, but rarely compare LC retention mechanisms. In addition, a high-performance liquid chromatography instrument may be beyond what some small colleges can purchase. Solid-phase…

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

    NARCIS (Netherlands)

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

    2017-01-01

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

  2. Practical application of solid phase spectrophotometry in analysis of materials and goods of mining and metallurgy

    International Nuclear Information System (INIS)

    Duan Qunzhang

    1999-01-01

    The author reviewed recent development and practical application of solid phase spectrophotometry in analysis of materials and goods of mining-metallurgy. Separation and preconcentration and conditions of coloring determination, sensitivity and range of detection, as well as interference of corresponding method are discussed

  3. 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 devel...... 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.......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...

  4. Solid-phase synthesis and biological activity of a thioether analogue of conotoxin G1

    DEFF Research Database (Denmark)

    Bondebjerg, Jon; Grunnet, Morten; Jespersen, Thomas

    2003-01-01

    A bicyclic thioether analogue of alpha-conotoxin G1, a neurotoxin found in the venom of cone snails, was synthesized on solid phase. Two successive intramolecular on-bead cyclizations between a cysteine residue and a chloroacetylated reduced peptide bond are the key steps in the synthesis...

  5. A new solid-phase sandwich radioimmunoassay and its application to the detection of snake venom

    International Nuclear Information System (INIS)

    Coulter, A.R.; Cox, J.C.; Sutherland, S.K.; Waddel, C.J.

    1978-01-01

    A solid-phase sandwich radioimmunoassay is described which can be used for the detection and quantitative estimation of crude snake venom and a snake neurotoxin in clinical and experimental situations. Rabbit IgG antivenom or antineurotoxin, covalently coupled to a solid phase (CH-Sepharose 4B) is incubated with sample of unknown venom concentration. Venom bound by the solid-phase antibody is detected by reaction with 125 I-labelled rabbit IgG antivenom or antineurotoxin ([ 125 I]IgG). The resultant count, T, is the total (specific and non-specific) uptake of [ 125 I]IgG. Non-specific binding N, is similarly determined, but with normal rabbit IgG antivenom or antineurotoxin ([ 125 I]IgG). The resultant count, T, is the total (specific and non-specific) uptake of [ 125 I]IgG. Non-specific binding N, is similarly determined, but with normal rabbit IgG bound to the solid phase. A T:N value greater than 1.8 for human serum or urine indicates the presence of venom in a sample (P>0.95). Positive samples are assayed at several dilutions and the venom present estimated from the specific count (T-N). Levels of 0.4 ng/ml of crude tiger snake venom (TSV) and 0.1 ng/ml of neurotoxin can be reliably detected by this procedure. (Auth.)

  6. Critical micelle concentration values for different surfactants measured with solid-phase microextraction fibers

    NARCIS (Netherlands)

    Haftka, Joris J H; Scherpenisse, Peter; Oetter, G??nter; Hodges, Geoff; Eadsforth, Charles V.; Kotthoff, Matthias; Hermens, Joop L M

    The amphiphilic nature of surfactants drives the formation of micelles at the critical micelle concentration (CMC). Solid-phase microextraction (SPME) fibres were used in the present study to measure CMC values of twelve nonionic, anionic, cationic and zwitterionic surfactants. The SPME derived CMC

  7. 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.

  8. Micro versus macro solid phase extraction for monitoring water contaminants: a preliminary study using trihalomethanes.

    Science.gov (United States)

    Alexandrou, Lydon D; Spencer, Michelle J S; Morrison, Paul D; Meehan, Barry J; Jones, Oliver A H

    2015-04-15

    Solid phase extraction is one of the most commonly used pre-concentration and cleanup steps in environmental science. However, traditional methods need electrically powered pumps, can use large volumes of solvent (if multiple samples are run), and require several hours to filter a sample. Additionally, if the cartridge is open to the air volatile compounds may be lost and sample integrity compromised. In contrast, micro cartridge based solid phase extraction can be completed in less than 2 min by hand, uses only microlitres of solvent and provides comparable concentration factors to established methods. It is also an enclosed system so volatile components are not lost. The sample can also be eluted directly into a detector (e.g. a mass spectrometer) if required. However, the technology is new and has not been much used for environmental analysis. In this study we compare traditional (macro) and the new micro solid phase extraction for the analysis of four common volatile trihalomethanes (trichloromethane, bromodichloromethane, dibromochloromethane and tribromomethane). The results demonstrate that micro solid phase extraction is faster and cheaper than traditional methods with similar recovery rates for the target compounds. This method shows potential for further development in a range of applications. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Solid-phase synthesis and biological evaluation of a combinatorial library of philanthotoxin analogues

    DEFF Research Database (Denmark)

    Strømgaard, K; Brier, T J; Andersen, K

    2000-01-01

    The modular structure of philanthotoxins was exploited for construction of the first combinatorial library of these compounds using solid-phase parallel synthesis. (S)-Tyrosine and (S)-3-hydroxyphenylalanine were used as amino acid components, spermine, 1,12-dodecanediamine, and 4,9-dioxa-1,12-do...

  10. Development of a Solid Phase Extraction Method for Agricultural Pesticides in Large-Volume Water Samples

    Science.gov (United States)

    An analytical method using solid phase extraction (SPE) and analysis by gas chromatography/mass spectrometry (GC/MS) was developed for the trace determination of a variety of agricultural pesticides and selected transformation products in large-volume high-elevation lake water sa...

  11. Recent developments in automatic solid-phase extraction with renewable surfaces exploiting flow-based approaches

    DEFF Research Database (Denmark)

    Miró, Manuel; Hartwell, Supaporn Kradtap; Jakmunee, Jaroon

    2008-01-01

    Solid-phase extraction (SPE) is the most versatile sample-processing method for removal of interfering species and/or analyte enrichment. Although significant advances have been made over the past two decades in automating the entire analytical protocol involving SPE via flow-injection approaches...

  12. Determination of Plant Volatiles Using Solid Phase Microextraction GC-MS

    Science.gov (United States)

    Van Bramer, Scott; Goodrich, Katherine R.

    2015-01-01

    This experiment combines analytical techniques of solid phase microextraction and gas chromatography-mass spectrometry with easily relatable and accessible plant volatile chemistry (floral and vegetative scents of local/available plants). The biosynthesis and structure of these chemicals are of interest in the areas of organic chemistry,…

  13. Determination of lidocaine in plasma by direct solid-phase microextraction combined with gas chromatography

    NARCIS (Netherlands)

    Koster, EHM; Wemes, C; Morsink, JB; de Jong, GJ

    2000-01-01

    Direct-immersion solid-phase microextraction (SPME) has been used to extract the local anesthetic lidocaine from human plasma. A simplified model shows the relationship between the total amount of drug in plasma and the amount of drug extracted. The model takes into account that the drug

  14. Solid-phase synthesis and biological evaluation of Joro spider toxin-4 from Nephila clavata

    DEFF Research Database (Denmark)

    Barslund, Anne Fuglsang; Poulsen, Mette Homann; Bach, Tinna Brøbech

    2011-01-01

    to be exploited in biological studies. Here, we have used solid-phase synthetic methodology for the efficient synthesis of Joro spider toxin-4 (JSTX-4) (1) from Nephila clavata, providing sufficient amounts of the toxin for biological evaluation at iGlu receptor subtypes using electrophysiology. Biological...

  15. Indirect solid-phase immunosorbent assay for detection of arenavirus antigens and antibodies

    Energy Technology Data Exchange (ETDEWEB)

    Ivanov, A.P.; Rezapkin, G.V.; Dzagurova, T.K.; Tkachenko, E.A. (Institute of Poliomyelitis anU Viral Encephalities of the U.S.S.R. Academy of Medical Sciences, Moscow)

    1984-05-01

    Indirect enzyme-linked immunosorbent assay (ELISA) and solid phase radioimmunoassay (SPRIA) using either enti-human or anti-mouse IgG labelled with horseradish peroxidase and /sup 125/I, respectively, were developed for the detection of Junin, Machupo, Tacaribe, Amapari, Tamiami, Lassa and LCM arenaviruses. Both methods allow high sensitivity detection of arenavirus antigens and antibodies.

  16. modeling and analysis of a three-phase solid-state var compensator

    African Journals Online (AJOL)

    Abstract. The problems associated with the flow of reactive power in transmission and distribution lines are well known. Several methods of var compensation have been applied in solv- ing these problems. This paper examines the performance of a three-phase solid-state var compensator employed in the power system for ...

  17. stability analysis of a three-phase solid-state var compensator

    African Journals Online (AJOL)

    2012-11-03

    Nov 3, 2012 ... Abstract. The problems associated with the flow of reactive power in transmission and distribution lines are well known. Several methods of var compensation have been applied in solving these problems. One of the modern devices employed in reactive power compensation is the three-phase solid-state.

  18. Solid-phase oligosaccharide synthesis with tris(alkoxy)benzyl amine (BAL) safety-catch anchoring

    DEFF Research Database (Denmark)

    Tolborg, Jakob Fjord; Jensen, Knud Jørgen

    2000-01-01

    A tris(alkoxy)benzylamine (BAL) handle strategy was developed for safety-catch anchoring of D-glucosamine derivatives in solid-phase synthesis of oligosaccharides; the linkage between the BAL handle and the amine proved stable to conc. TFA and Lewis acids, but after N-acylation the amide could...

  19. Obviation of hydrogen fluoride in Boc chemistry solid phase peptide synthesis of peptide-αthioesters.

    Science.gov (United States)

    Gates, Zachary P; Dhayalan, Balamurugan; Kent, Stephen B H

    2016-11-29

    Under suitable conditions, trifluoromethanesulfonic acid performs comparably to hydrogen fluoride for the on-resin global deprotection of peptides prepared by Boc chemistry solid phase peptide synthesis (SPPS). Obviation of hydrogen fluoride in Boc chemistry SPPS enables the straightforward synthesis of peptide- α thioesters for use in native chemical ligation.

  20. Thermal battery. [solid metal halide electrolytes with enhanced electrical conductance after a phase transition

    Science.gov (United States)

    Carlsten, R.W.; Nissen, D.A.

    1973-03-06

    The patent describes an improved thermal battery whose novel design eliminates various disadvantages of previous such devices. Its major features include a halide cathode, a solid metal halide electrolyte which has a substantially greater electrical conductance after a phase transition at some temperature, and a means for heating its electrochemical cells to activation temperature.

  1. Understanding processing-induced phase transformations in erythromycin-PEG 6000 solid dispersions

    DEFF Research Database (Denmark)

    Mirza, Sabiruddin; Heinämäki, Jyrki; Miroshnyk, Inna

    2006-01-01

    Since the quality and performance of a pharmaceutical solid formulation depend on solid state of the drug and excipients, a thorough investigation of potential processing-induced transformations (PITs) of the ingredients is required. In this study, the physical phenomena taking place during...... intermolecular interactions between the drug and polymer in the solid state were further studied by Fourier transform infrared (FTIR) spectroscopy. While in the absence of PEG the dehydration was the only transformation observed, hot-melt processing with the polymer caused the drug to undergo multiple phase...... formulation of erythromycin (EM) dihydrate solid dispersions with polyethylene glycol (PEG) 6000 by melting were investigated. PITs were monitored in situ using variable temperature X-ray powder diffraction (VT-XRPD), differential scanning calorimetry (DSC), and hot-stage microscopy (HSM). Possible...

  2. 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.

  3. Thermal conductivity of solid cyclohexane in orientationally ordered and disordered phases

    International Nuclear Information System (INIS)

    Konstantinov, V. A.; Revyakin, V. P.; Sagan, V. V.; Pursky, O. I.; Sysoev, V. M.

    2011-01-01

    Thermal conductivity Λ P of solid cyclohexane is measured at a pressure P = 0.1 MPa in the temperature range from 80 K to the melting point, which covers the ranges of low-temperature orientationally ordered phase II and high-temperature orientationally disordered phase I. Thermal conductivity Λ V is measured at a constant volume in orientationally disordered phase I. The thermal conductivity measured at atmospheric pressure decreases with increasing temperature as Λ P ∝ T −1.15 in phase II, whereas Λ P ∝ T −0.3 in phase I. As temperature increases, isochoric thermal conductivity Λ V in phase I increases gradually. The experimental data are described in terms of a modified Debye model of thermal conductivity with allowance for heat transfer by both phonons and “diffuse” modes.

  4. 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

  5. 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

  6. 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

  7. 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

  8. The influence of microwave radiation on the process of solid-phase recovery of ilmenite concentrate

    Science.gov (United States)

    Melkomukova, O. G.; Lanovetskiy, S. V.

    2018-01-01

    A study on the effect of intensive microwave radiation on the process of solid-phase recovery of ilmenite concentrate is presented. Assessment of the degree of recovery, the change in the phase composition and elemental analysis of the reaction products were carried out by x-ray diffraction and energy-dispersive analysis. By means of electron microscopy, the dynamics of the appearance and the droplet size of the restored iron formed under the influence of microwave irradiation on the surface of solid-phase synthesis products are evaluated. High efficiency of microwave exposure on the recovery of ilmenite concentrate in the carbon medium at a temperature of 1000 °C is shown. The possibility of reducing temperature and duration of the reduction process of iron oxides in the ilmenite ore, compared with the traditional high-temperature process of enrichment of titanium ore, is established.

  9. 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.

  10. Formation routes of interstellar glycine involving carboxylic acids: possible favoritism between gas and solid phase.

    Science.gov (United States)

    Pilling, Sergio; Baptista, Leonardo; Boechat-Roberty, Heloisa M; Andrade, Diana P P

    2011-11-01

    Despite the extensive search for glycine (NH₂CH₂COOH) and other amino acids in molecular clouds associated with star-forming regions, only upper limits have been derived from radio observations. Nevertheless, two of glycine's precursors, formic acid and acetic acid, have been abundantly detected. Although both precursors may lead to glycine formation, the efficiency of reaction depends on their abundance and survival in the presence of a radiation field. These facts could promote some favoritism in the reaction pathways in the gas phase and solid phase (ice). Glycine and these two simplest carboxylic acids are found in many meteorites. Recently, glycine was also observed in cometary samples returned by the Stardust space probe. The goal of this work was to perform theoretical calculations for several interstellar reactions involving the simplest carboxylic acids as well as the carboxyl radical (COOH) in both gas and solid (ice) phase to understand which reactions could be the most favorable to produce glycine in interstellar regions fully illuminated by soft X-rays and UV, such as star-forming regions. The calculations were performed at four different levels for the gas phase (B3LYP/6-31G*, B3LYP/6-31++G**, MP2/6-31G*, and MP2/6-31++G**) and at MP2/6-31++G** level for the solid phase (ice). The current two-body reactions (thermochemical calculation) were combined with previous experimental data on the photodissociation of carboxylic acids to promote possible favoritism for glycine formation in the scenario involving formic and acetic acid in both gas and solid phase. Given that formic acid is destroyed more in the gas phase by soft X-rays than acetic acid is, we suggest that in the gas phase the most favorable reactions are acetic acid with NH or NH₂OH. Another possible reaction involves NH₂CH₂ and COOH, one of the most-produced radicals from the photodissociation of acetic acid. In the solid phase, we suggest that the reactions of formic acid with NH

  11. 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...

  12. A lab-on-a-chip device for rapid identification of avian influenza viral RNA by solid-phase PCR

    DEFF Research Database (Denmark)

    Yi, Sun; Dhumpa, Raghuram; Bang, Dang Duong

    2011-01-01

    This paper describes a lab-on-a-chip device for fast AIV screening by integrating DNA microarray-based solid-phase PCR on a microfluidic chip.......This paper describes a lab-on-a-chip device for fast AIV screening by integrating DNA microarray-based solid-phase PCR on a microfluidic chip....

  13. Phase Evolution and Mechanical Behavior of the Semi-Solid SIMA Processed 7075 Aluminum Alloy

    Directory of Open Access Journals (Sweden)

    Behzad Binesh

    2016-02-01

    Full Text Available Microstructural and mechanical behaviors of semi-solid 7075 aluminum alloy were investigated during semi-solid processing. The strain induced melt activation (SIMA process consisted of applying uniaxial compression strain at ambient temperature and subsequent semi-solid treatment at 600–620 °C for 5–35 min. Microstructures were characterized by scanning electron microscope (SEM, energy dispersive spectroscopy (EDS, and X-ray diffraction (XRD. During the isothermal heating, intermetallic precipitates were gradually dissolved through the phase transformations of α-Al + η (MgZn2 → liquid phase (L and then α-Al + Al2CuMg (S + Mg2Si → liquid phase (L. However, Fe-rich precipitates appeared mainly as square particles at the grain boundaries at low heating temperatures. Cu and Si were enriched at the grain boundaries during the isothermal treatment while a significant depletion of Mg was also observed at the grain boundaries. The mechanical behavior of different SIMA processed samples in the semi-solid state were investigated by means of hot compression tests. The results indicated that the SIMA processed sample with near equiaxed microstructure exhibits the highest flow resistance during thixoforming which significantly decreases in the case of samples with globular microstructures. This was justified based on the governing deformation mechanisms for different thixoformed microstructures.

  14. First order magneto-structural phase transition and associated multi-functional properties in magnetic solids

    International Nuclear Information System (INIS)

    Roy, Sindhunil Barman

    2013-01-01

    We show that the first order magneto-structural phase transitions observed in various classes of magnetic solids are often accompanied by useful multi-functional properties, namely giant magneto-resistance, magneto-caloric effect and magneto-striction. We highlight various characteristic features associated with a disorder influenced first order phase transition namely supercooling, superheating, phase-coexistence and metastability, in several magnetic materials and discuss how a proper understanding of the transition process can help in fine tuning of the accompanied functional properties. Magneto-elastic coupling is a key element in this first order phase transition, and methods need to be explored for maximizing the contributions from both the lattice and the magnetic degree of freedom while simultaneously minimizing the thermomagnetic hysteresis loss. An analogy is also drawn with the first order phase transition observed in dielectric materials and vortex matter of type-II superconductors. (topical review)

  15. First order magneto-structural phase transition and associated multi-functional properties in magnetic solids.

    Science.gov (United States)

    Roy, Sindhunil Barman

    2013-05-08

    We show that the first order magneto-structural phase transitions observed in various classes of magnetic solids are often accompanied by useful multi-functional properties, namely giant magneto-resistance, magneto-caloric effect and magneto-striction. We highlight various characteristic features associated with a disorder influenced first order phase transition namely supercooling, superheating, phase-coexistence and metastability, in several magnetic materials and discuss how a proper understanding of the transition process can help in fine tuning of the accompanied functional properties. Magneto-elastic coupling is a key element in this first order phase transition, and methods need to be explored for maximizing the contributions from both the lattice and the magnetic degree of freedom while simultaneously minimizing the thermomagnetic hysteresis loss. An analogy is also drawn with the first order phase transition observed in dielectric materials and vortex matter of type-II superconductors.

  16. Solid–solid transformations via nanoscale intermediate interfacial phase: Multiple structures, scale and mechanics effects

    International Nuclear Information System (INIS)

    Levitas, Valery I.; Momeni, Kasra

    2014-01-01

    Solid–solid (SS) phase transformations via nanometer-size intermediate melts (IMs) within the SS interface, hundreds of degrees below melting temperature, were predicted thermodynamically and are consistent with experiments for various materials. A necessary condition for the appearance of IMs, using a sharp interface approach, was that the ratio of the energies of SS and solid–melt (SM) interfaces, k E , were >2. Here, an advanced phase-field approach coupled with mechanics is developed that reveals various new scale and interaction effects and phenomena. Various types of IM are found: (i) continuous and reversible premelting and melting; (ii) jump-like barrierless transformation to IMs, which can be kept at much lower temperature even for k E E E E =1. The theory developed here can be tailored for diffusive phase transformations, formation of intergranular and interfacial phases, and surface-induced phase transformations

  17. 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)

  18. Evidence for a Magnetic Collapse in the Epsilon Phase of Solid Oxygen

    International Nuclear Information System (INIS)

    Goncharenko, Igor N.

    2005-01-01

    Solid oxygen is the only elementary molecular magnet. Under the very high pressure of 96 GPa oxygen transforms into a metal and a superconductor. Theory predicts a nonmagnetic state occurring before the transition into the superconducting ξ phase. Nevertheless, until now there was no direct evidence of a magnetic collapse in high-pressure oxygen. For the first time direct information is provided on magnetic properties of the ε phase, which is sandwiched between the antiferromagnetic δ phase and the superconducting ξ phase. We used magnetic neutron diffraction. The data show that the long-range magnetic order disappears at the δ-ε transition. The magnetic collapse occurs at P≅8 GPa, far below the pressure of the insulator-metal (superconductor) transition. The collapse is preceded by a decrease in temperature of transition towards the long-range magnetically ordered state (T LRO ) in the δ phase, at P=7.6 GPa

  19. Evidence for a magnetic collapse in the epsilon phase of solid oxygen.

    Science.gov (United States)

    Goncharenko, Igor N

    2005-05-27

    Solid oxygen is the only elementary molecular magnet. Under the very high pressure of 96 GPa oxygen transforms into a metal and a superconductor. Theory predicts a nonmagnetic state occurring before the transition into the superconducting xi phase. Nevertheless, until now there was no direct evidence of a magnetic collapse in high-pressure oxygen. For the first time direct information is provided on magnetic properties of the epsilon phase, which is sandwiched between the antiferromagnetic delta phase and the superconducting xi phase. We used magnetic neutron diffraction. The data show that the long-range magnetic order disappears at the delta-epsilon transition. The magnetic collapse occurs at P approximately equal to 8 GPa, far below the pressure of the insulator-metal (superconductor) transition. The collapse is preceded by a decrease in temperature of transition towards the long-range magnetically ordered state (T(LRO)) in the delta phase, at P = 7.6 GPa.

  20. Influence of SiO2/Al2O3 Molar Ratio on Phase Composition and Surfaces Quality of Aluminum Silicate Sanitary Glazes in the SiO2-Al2O3-CaO-Na2O System

    Directory of Open Access Journals (Sweden)

    Leśniak M.

    2016-12-01

    Full Text Available This paper presents the results of research on aluminum silicate sanitary glazes in the SiO2-Al2O3-CaO-Na2O system with different SiO2/Al2O3 molar ratio. XRD, SEM-EDS and FITR measurement indicated that SiO2/Al2O3 molar ratio has a significant impact on the phase composition of the obtained glazes. Glass-ceramic glazes were obtained that consisted of both the glass phase and pseudowollastonite (Ca3[SiO3]3 or anorthite (Ca[Al2Si2O8] crystals. Subsequently, the influence of phase composition on surface quality (roughness was examined for the obtained samples. On the basis of the conducted examination of glaze surface roughness was observed that glazes of extreme SiO2/Al2O3 molar ratio are characterized with greatest surface roughness when compared to other glazes.

  1. On-line solid phase selective separation and preconcentration of Cd(II) by solid-phase extraction using carbon active modified with methyl thymol blue

    Energy Technology Data Exchange (ETDEWEB)

    Ensafi, Ali A. [College of Chemistry, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of)], E-mail: Ensafi@cc.iut.ac.ir; Ghaderi, Ali R. [College of Chemistry, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of)

    2007-09-05

    An on-line flow system was used to develop a selective and efficient on-line sorbent extraction preconcentration system for cadmium. The method is based on adsorption of cadmium ions onto the activated carbon modified with methyl thymol blue. Then the adsorbed ions were washed using 0.5 M HNO{sub 3} and the eluent was used to determine the Cd(II) ions using flame atomic absorption spectrometry. The results obtained show that the modified activated carbon has the greatest adsorption capacity of 80 {mu}g of Cd(II) per 1.0 g of the solid phase. The optimal pH value for the quantitative preconcentration was 9.0 and full desorption is achieved by using 0.5 M HNO{sub 3} solution. It is established that the solid phase can be used repeatedly without a considerable adsorption capacity loss. The detection limit was less than 1 ng mL{sup -1} Cd(II), with an enrichment factor of 1000. The calibration graph was linear in the range of 1-2000 ng mL{sup -1} Cd(II). The developed method has been applied to the determination of trace cadmium (II) in water samples and in the following reference materials: sewage sludge (CRM144R), and sea water (CASS.4) with satisfactory results. The accuracy was assessed through recovery experiments.

  2. Determination of triazine herbicides in seaweeds: development of a sample preparation method based on Matrix Solid Phase Dispersion and Solid Phase Extraction Clean-up.

    Science.gov (United States)

    Rodríguez-González, N; González-Castro, M J; Beceiro-González, E; Muniategui-Lorenzo, S; Prada-Rodríguez, D

    2014-04-01

    A method using dual process columns of Matrix Solid Phase Dispersion (MSPD) and Solid Phase Extraction (SPE) has been developed for extracting and cleaning-up of nine triazine herbicides (ametryn, atrazine, cyanazine, prometryn, propazine, simazine, simetryn, terbuthylazine and terbutryn) in seaweed samples. Under optimized conditions, samples were blended with 2g of octasilyl-derivatized silica (C8) and transferred into an SPE cartridge containing ENVI-Carb II/PSA (0.5/0.5 g) as a clean up co-sorbent. Then the dispersed sample was washed with 10 mL of n-hexane and triazines were eluted with 20 mL ethyl acetate and 5 mL acetonitrile. Finally the extract was concentrated to dryness, re-constituted with 1 mL methanol:water (1:1) and injected into the HPLC-DAD system. The linearity of the calibration curves was excellent in matrix matched standards, and yielded the coefficients of determination>0.995 for all the target analytes. The recoveries ranged from 75% to 100% with relative standard deviations lower than 7%. The achieved LOQs (seaweeds were subjected to the procedure proving the suitability of MSPD method for the analysis of triazines in different seaweeds samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. 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)

  4. The binary (solid + liquid) phase diagrams of (caprylic or capric acid) + (1-octanol or 1-decanol)

    International Nuclear Information System (INIS)

    Carareto, Natália D.D.; Castagnaro, Thamires; Costa, Mariana C.; Meirelles, Antonio J.A.

    2014-01-01

    Highlights: • SLE of mixtures of caprylic acid, (capric acid + 1-octanol), 1-decanol were studied. • Experimental data were obtained through DSC and Stepscan DSC. • Systems presented eutectic and peritectic points. • Liquidus line was modeled using Margules and NRTL models. • Solid phase was modeled using the Slaughter and Doherty approach. - Abstract: In the present study the phase diagrams of four (fatty acid + fatty alcohol) binary mixtures composed of caprylic (C8O2) or capric acid (C10O2) + 1-octanol (C8OH) or 1-decanol (C10OH) were obtained by differential scanning calorimetry (DSC). Eutectic and peritectic reactions occurred in the systems. In standard DSC analyses of the (C8O2 + C10OH) and (C10O2 + C8OH) systems, an exothermic transition occurs in association with the melting of a metastable phase. A Stepscan DSC method was used in order to avoid the formation of this metastable phase during the heating of the mixtures. The approach suggested by Slaughter and Doherty (1995) [24] was used for modeling the solid phase, and the Margules 2-suffix, Margules 3-suffix and NRTL models were applied for calculating the activity coefficients of the liquid phase. The best modeling results were obtained using the Margules-3-suffix with an average deviation between experimental and calculated values ranging from T = (0.3 to 0.9) K

  5. Determination of multi-class herbicides in soil by liquid-solid extraction coupled with headspace solid phase microextraction method

    Directory of Open Access Journals (Sweden)

    Đurović-Pejčev Rada

    2016-01-01

    Full Text Available A method is described for simultaneous determination of five herbicides (metribuzin, acetochlor, clomazone, oxyfluorfen and dimethenamid belonging to different pesticides groups in soil samples. Developed headspace solid phase microextraction method (HS-SPME in combination with liquid-solid sample preparation (LS was optimized and applied in the analysis of some agricultural samples. Optimization of microextraction conditions, such as temperature, extraction time and sodium chloride (NaCl content was perfor-med using 100 μm polydimethyl-siloxane (PDMS fiber. The extraction effi-ciencies of methanol, methanol:acetone=1:1 and methanol:acetone:hexane= =2:2:1 and the optimum number of extraction steps during the sample prepa-ration, were tested, as well. Gas chromatography-mass spectrometry (GC-MS was used for detection and quantification, obtaining relative standard deviation (RSD below 13%, and recovery values higher than 83% for multiple analyses of soil samples fortified at 30 μg kg-1 of each herbicide. Limits of detection (LOD were less than 1.2 μg kg-1 for all the studied herbicides. [Projekat Ministarstva nauke Republike Srbije, br. TR31043 i br. III43005

  6. LABORATORY INVESTIGATIONS OF SILICATE MUD CONTAMINATION WITH CALCIUM

    Directory of Open Access Journals (Sweden)

    Nediljka Gaurina-Međimurec

    2004-12-01

    Full Text Available The silicate-based drilling fluid is a low solids KCl/polymer system with the addition of soluble sodium or potassium silicate to enhance inhibition and wellbore stability. Silicate-based drilling fluids exhibit remarkable shale and chalk stabilizing properties, resulting in gauge hole and the formation of firm cuttings when drilling reactive shales and soft chalks. Silicates protect shales by in-situ gellation when exposed to the neutral pore fluid and precipitation, which occurs on contact with divalent ions present at the surface of the shale. Also, silicates prevent the dispersion and washouts when drilling soft chalk by reacting with the Ca2+ ions present on chalk surfaces of cutting and wellbore to form a protective film. The silicate-based drilling fluid can be used during drilling hole section through shale interbeded anhydrite formations because of its superior shale stabilizing characteristics. However, drilling through the anhydrite can decrease the silicate concentration and change rheological and filtration fluid properties. So, the critical concentration of calcium ions should be investigated by lab tests. This paper details the mechanism of shale inhibition using silicate-based drilling fluid, and presents results of lab tests conducted to ascertain the effect of Ca2+ ions on silicate level in the fluid and the fluid properties.

  7. Effect of transition dipole phase on high-order-harmonic generation in solid materials

    Science.gov (United States)

    Jiang, Shicheng; Wei, Hui; Chen, Jigen; Yu, Chao; Lu, Ruifeng; Lin, C. D.

    2017-11-01

    High-order harmonic spectra from solid materials driven by single-color multicycle laser fields sometimes contain even harmonics. In this work we attribute the appearance of even harmonics to the nonzero transition dipole phase (TDP) when the solid system has broken symmetry. By calculating the harmonic efficiency from graphene and gapped graphene by using the semiconductor Bloch equations under the tight-binding approximation, we demonstrate the role of the TDP, which has been ignored for a long time. When the crystal has inversion symmetry, or reflection symmetry with the symmetry plane perpendicular to the laser polarization direction, the TDP can be neglected. Without such symmetry, however, the TDP will lead to the appearance of even harmonics. We further show that the TDP is sensitive to the crystal geometry. To extract the structure information from the harmonic spectra of a solid the TDP cannot be ignored.

  8. Radioimmunoassay of diagoxin with the aid of the solid phase - microtitre plating technique

    International Nuclear Information System (INIS)

    Scheidt, C.

    1982-01-01

    Preliminary results are reported here on the development of a digoxin-radioimmunoassay with an anti-digoxin antibody (goat) in a solid phase technique (mictrotitre plate). The advantages compared to conventional RIAs are: Cross reactions towards digoxin is minimal, both in vitro and in vivo. The calibraton range extends from 0.25 to 8 ng/ml. The radioactive load could be reduced significantly by use of smaller amounts of tracer (0.004 μCi/single determination) and by reduction of waste volume (solid), waste weight (solid) and liquid waste. The DIGOXIN RIA BIOTEST MTP is, in addition, the only digoxin radioimmunoassay where radioactive waste is produced in a sealed form. The test is a simple one and can be carried out without the need for complicated apparatus and techniques. (orig./MG) [de

  9. Magnetic Phase Transition In CocMg1-CO Solid Solutions

    International Nuclear Information System (INIS)

    Mironova-Ulmane, N.; Ulmanis, U.; Kuzmin, A.; Sildos, I.; Pars, M.

    2007-01-01

    Full text: Co c Mg 1-C O system is a nice example of diluted antiferromagnet. It forms a continuous series of solid solutions, whose magnetic properties vary with the composition from antiferromagnetic-like behaviour with the Neel temperature T N =300 K for pure CoO to diamagnetic-like behaviour for pure MgO. For intermediate compositions with c>0.5, the paramagnetic-to-antiferromagnetic phase transition occurs upon cooling. In order to examine the influence of the dilution by diamagnetic ions on the magnetic ordering of single-crystal Co c Mg 1-c O solid solutions, we have performed Raman spectroscopy and domain structure studies. The temperature dependence of the intensity of Raman scattering from Co c Mg 1-c O solid solutions has been measured in a wide range of compositions (0.5< c<1) and temperatures (6 K< T<200 K). The obtained results will be discussed. (Authors)

  10. Solid-phase radioimmunoassay of immunoglobulins G, A and M: applicability in analysis of sucrose gradients

    International Nuclear Information System (INIS)

    Eriksen, E.F.; Danielsen, H.; Johansen, A.S.; Larsson, L.I.

    1984-01-01

    A simple and sensitive solid-phase radioimmunoassay for the detection of immunoglobulins G, A and M in sucrose gradients is described. The solid-phase consisted of immunoglobulins adsorbed to polystyrene tubes. Using buffers without detergent and 125 I-labeled sheep anti-rabbit IgA as radioligand, the assay was able to detect 0.8 ng per tube in the IgG assay and 1.6 ng per tube in the IgA and IgM assays. Standard curves with antigen dissolved in 10% and 32% sucrose were superimposable and did not deviate from standard curves with antigen dissolved in buffer without sucrose. Using these techniques on ultracentrifugation samples from patients with systemic lupus erythematosus, Schoenlein-Henoch nephritis and IgA glorulonephritis is was possible to detect both immunoglobulin fragments and immunoglobulin aggregates at the same time without prior dialysis of the samples. (Auth.)

  11. A competitive solid-phase radioimmunoassay for quantitation of the major allergen of Parietaria pollen

    International Nuclear Information System (INIS)

    Corbi, A.L.; Ayuso, R.; Lombardero, M.; Duffort, O.; Carreira, J.

    1985-01-01

    A competitive solid-phase radioimmunoassay has been developed for quantitation of the major allergen of Parietaria judaica pollen. The assay is based on: (1) the ability of AC/1.1 monoclonal antibody to bind specifically to the P. judaica major allergen, and (2) the ability of crude pollen extracts or purified allergen to inhibit the binding of 125 I-labelled allergen to solid-phase-bound AC/1.1 monoclonal antibody. The assay is sensitive enough to detect as little as 10 ng of allergen. A good correlation is found when the results obtained are compared with those produced by RAST inhibition (r = 0.95; P < 0.001). Thus, this method can also be used for the estimation of the allergenic activity of P. judaica pollen extracts. The assay is easily completed in 2 h, allowing simultaneous analysis of a number of extracts. (Auth.)

  12. 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.

  13. Development of a solid phase technic for radioimmunoassay of triiodothyronine (T3) in serum

    International Nuclear Information System (INIS)

    Hamada, M.M.; Mesquita, C.H.; Silva, C.P.G. da.

    1988-10-01

    We have developed a solid phase radioimmunoassay (RIA) system for triiodothyronine (T 3 ), by immobilizing triiodothyronine antibodies on the inner wall of reaction tubes. The antibody-coated tubes were made via reaction of antibody with glutaraldeyde residue pre coated on the inner wall of the tubes by alkaline self-polimerization. The quality of the coated tubes was tested through its performance in the RIA methodology, by analysing the following RIA parameters: minimum detectable dose (MDD), nonspecific binding (NSB), ''X 50% '', slope of the standard curve, intra and inter-assay precision, accuracy of the method and figure of merit. The serum levels of T 3 in hypothyroid and hyperthyroid patients and the normal values range were determined for the solid phase RIA system. The results are in agreement with found in the literature. (author) [pt

  14. Steam distillation-solid-phase microextraction for the detection of Ephedra sinica in herbal preparations.

    Science.gov (United States)

    Tellez, Mari R; Khan, Ikhlas A; Schaneberg, Brian T; Crockett, Sara L; Rimando, Agnes M; Kobaisy, Mozaina

    2004-01-30

    A new method involving concurrent solid-phase microextraction combined with continuous hydrodistillation of essential oil was developed. This new methodology allowed for the detection by GC-MS of very small amounts of a diagnostic peak for the authentication of Ephedra sinica, in a short period of time and using only small sample sizes. This diagnostic peak was identified as 4-vinylanisole, and elucidated from the chromatographic profile allowed for the identification of a sample as E. sinica among other species investigated in this study. To the best of our knowledge this is the first report on using continuous solid-phase microextraction coupled to hydrodistillation for the investigation of essential oil components, and the first report of 4-vinylanisole as a marker compound for E. sinica. A total of 46 collections representing 21 species of Ephedra were studied.

  15. Solid-phase extraction NMR studies of chromatographic fractions of saponins from Quillaja saponaria.

    Science.gov (United States)

    Nyberg, Nils T; Baumann, Herbert; Kenne, Lennart

    2003-01-15

    The saponin mixture QH-B from the tree Quillaja saponaria var. Molina was fractionated by RP-HPLC in several steps. The fractions were analyzed by solid-phase extraction NMR (SPE-NMR), a technique combining the workup by solid-phase extraction with on-line coupling to an NMR flow probe. Together with MALDI-TOF mass spectrometry and comparison with chemical shifts of similar saponins, the structures of both major and minor components in QH-B could be obtained. The procedure described is a simple method to determine the structure of components in a complex mixture. The two major fractions of the mixture were found to contain at least 28 saponins, differing in the carbohydrate substructures. Eight of these have not previously been determined. The 28 saponins formed 14 equilibrium pairs by the migration of an O-acyl group between two adjacent positions on a fucosyl residue.

  16. Numerical simulation of polishing U-tube based on solid-liquid two-phase

    Science.gov (United States)

    Li, Jun-ye; Meng, Wen-qing; Wu, Gui-ling; Hu, Jing-lei; Wang, Bao-zuo

    2018-03-01

    As the advanced technology to solve the ultra-precision machining of small hole structure parts and complex cavity parts, the abrasive grain flow processing technology has the characteristics of high efficiency, high quality and low cost. So this technology in many areas of precision machining has an important role. Based on the theory of solid-liquid two-phase flow coupling, a solid-liquid two-phase MIXTURE model is used to simulate the abrasive flow polishing process on the inner surface of U-tube, and the temperature, turbulent viscosity and turbulent dissipation rate in the process of abrasive flow machining of U-tube were compared and analyzed under different inlet pressure. In this paper, the influence of different inlet pressure on the surface quality of the workpiece during abrasive flow machining is studied and discussed, which provides a theoretical basis for the research of abrasive flow machining process.

  17. Solid phase graft copolymerization of acrylic monomers onto thermoplastics and their use as blend compatibilizers

    Science.gov (United States)

    Subramanian, Srinivas

    This research work is an extension of some of the earlier work done on the development of solid phase grafting technique to graft various monomers onto polymers as well as postulation of the usefulness of the graft copolymers thus synthesized. Polystyrene grafted with acrylic acid, previously developed in bench scale, was synthesized in pilot-plant scale batches. Process parameter studies on the grafting of acrylic acid onto polypropylene and developmental studies on the grafting of maleic anhydride onto polystyrene were also done. Polymers grafted with polar molecules such as maleic anhydride and acrylic acid have been used to compatibilize immiscible blends of polar and non-polar polymers. On the same note, the applicability of the solid phase graft copolymers as blend compatibilizers were investigated and their performance was compared to commercially available compatibilizers. Solid phase graft copolymerization process is a technique to synthesize graft copolymers. Some of its salient features are use of minimal solvent to conduct the reaction and easy equipment modification. It is a low pressure and low temperature process. This technique provides a viable alternative to the environmentally hazardous, and time consuming conventional process currently in use. Hence, development of this technique could be beneficial not only to the plastics industry, but also to mankind. Also, this technique provides a low-cost and extremely easy method to develop graft copolymers such as acrylic acid functionalized polymers that are rapidly gaining popularity as blend compatibilizers and polymer reinforcing agents. A study that proves the potential of these solid phase graft copolymers as good blend compatibilizers for industrially important immiscible polymers will develop interest in the industries about this grafting process. The free radical solid phase graft copolymerization process was carried in a modified Brabender-type mixer fitted with specially designed blades to

  18. Solid-phase radioimmunoassay of immunoglobulins G, A and M: applicability in analysis of sucrose gradients

    Energy Technology Data Exchange (ETDEWEB)

    Eriksen, E.F.; Danielsen, H. (Aarhus Kommunehospital (Denmark). Medical Department C); Johansen, A.S. (Aarhus Univ. (Denmark). Institute of Medical Biochemistry); Larsson, L.I. (Unit of Histochemistry, University Institute of Pathology, Copenhagen, Denmark)

    1984-01-01

    A simple and sensitive solid-phase radioimmunoassay for the detection of immunoglobulins G, A and M in sucrose gradients is described. The solid-phase consisted of immunoglobulins adsorbed to polystyrene tubes. Using buffers without detergent and /sup 125/I-labeled sheep anti-rabbit IgA as radioligand, the assay was able to detect 0.8 ng per tube in the IgG assay and 1.6 ng per tube in the IgA and IgM assays. Standard curves with antigen dissolved in 10% and 32% sucrose were superimposable and did not deviate from standard curves with antigen dissolved in buffer without sucrose. Using these techniques on ultracentrifugation samples from patients with systemic lupus erythematosus, Schoenlein-Henoch nephritis and IgA glorulonephritis is was possible to detect both immunoglobulin fragments and immunoglobulin aggregates at the same time without prior dialysis of the samples.

  19. 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.

  20. Molecular simulation of homogeneous crystal nucleation of AB2 solid phase from a binary hard sphere mixture

    Science.gov (United States)

    Bommineni, Praveen Kumar; Punnathanam, Sudeep N.

    2017-08-01

    Co-crystal formation from fluid-mixtures is quite common in a large number of systems. The simplest systems that show co-crystal (also called substitutionally ordered solids) formation are binary hard sphere mixtures. In this work, we study the nucleation of AB2 type solid compounds using Monte Carlo molecular simulations in binary hard sphere mixtures with the size ratio of 0.55. The conditions chosen for the study lie in the region where nucleation of an AB2 type solid competes with that of a pure A solid with a face-centered-cubic structure. The fluid phase composition is kept equal to that of the AB2 type solid. The nucleation free-energy barriers are computed using the seeding technique of Sanz et al. [J. Am. Chem. Soc. 135, 15008 (2013)]. Our simulation results show that the nucleation of the AB2 type solid is favored even under conditions where the pure A solid is more stable. This is primarily due to the similarity in the composition of the fluid phase and the AB2 type solid which in turn leads to much lower interfacial tension between the crystal nucleus and the fluid phase. This system is an example of how the fluid phase composition affects the structure of the nucleating solid phase during crystallization and has relevance to crystal polymorphism during crystallization processes.

  1. Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

    Directory of Open Access Journals (Sweden)

    Helena Prosen

    2014-05-01

    Full Text Available Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc. published in the last decade. Several innovative liquid-phase microextraction (LPME techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME, hollow fiber-liquid phase microextraction (HF-LPME, dispersive liquid-liquid microextraction (DLLME. Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

  2. Applications of liquid-phase microextraction in the sample preparation of environmental solid samples.

    Science.gov (United States)

    Prosen, Helena

    2014-05-23

    Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc.) published in the last decade. Several innovative liquid-phase microextraction (LPME) techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME), hollow fiber-liquid phase microextraction (HF-LPME), dispersive liquid-liquid microextraction (DLLME). Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

  3. Anisotropic solid-liquid interface kinetics in silicon: an atomistically informed phase-field model

    Science.gov (United States)

    Bergmann, S.; Albe, K.; Flegel, E.; Barragan-Yani, D. A.; Wagner, B.

    2017-09-01

    We present an atomistically informed parametrization of a phase-field model for describing the anisotropic mobility of liquid-solid interfaces in silicon. The model is derived from a consistent set of atomistic data and thus allows to directly link molecular dynamics and phase field simulations. Expressions for the free energy density, the interfacial energy and the temperature and orientation dependent interface mobility are systematically fitted to data from molecular dynamics simulations based on the Stillinger-Weber interatomic potential. The temperature-dependent interface velocity follows a Vogel-Fulcher type behavior and allows to properly account for the dynamics in the undercooled melt.

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

    International Nuclear Information System (INIS)

    Adekoya, O.A.

    1987-06-01

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

  5. Optimization of the solid-phase microextraction method in the determination of Ixodes ricinus (L.) volatiles

    Czech Academy of Sciences Publication Activity Database

    Zahradníčková, Helena; Bouman, Edwin Arien Poul

    2006-01-01

    Roč. 29, č. 2 (2006), s. 236-241 ISSN 1615-9306 R&D Projects: GA ČR(CZ) GA206/04/0751 Institutional research plan: CEZ:AV0Z50070508; CEZ:AV0Z60220518 Keywords : GC/MS * Ixodes ricinus * solid-phase microextraction Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.535, year: 2006

  6. R. Bruce Merrifield and Solid-Phase Peptide Synthesis: A Historical Assessment

    Energy Technology Data Exchange (ETDEWEB)

    Mitchell, A R

    2007-12-04

    Bruce Merrifield, trained as a biochemist, had to address three major challenges related to the development and acceptance of solid-phase peptide synthesis (SPPS). The challenges were (1) to reduce the concept of peptide synthesis on a insoluble support to practice, (2) overcome the resistance of synthetic chemists to this novel approach, and (3) establish that a biochemist had the scientific credentials to effect the proposed revolutionary change in chemical synthesis. How these challenges were met is discussed in this article.

  7. Visual monitoring of solid-phase extraction using chromogenic fluorous synthesis supports.

    Science.gov (United States)

    Blackburn, Christopher

    2012-03-12

    Reductive aminations and further transformations of an azo dye and fluorous tagged aldehyde are described. The intensely colored 2,4-dialkoxybenzyl protected amines undergo Fmoc-based peptide coupling, Suzuki reactions, and sulfonamide formation with product isolation facilitated by visual monitoring of fluorous solid phase extraction. Target compounds are released from the supports in high yields and purities by treatment with trifluoroacetic acid (TFA).

  8. Preparation of high-quality poly-Si films by a solid phase crystallizing method

    CERN Document Server

    Yao Ruo He

    2002-01-01

    A solid phase crystallizing method has been developed to grow a Si crystal at temperatures as low as 550 degree C. Using this method, a high-quality thin-film polycrystalline silicon (Poly-Si) was obtained. The largest grain size, examined with X-ray diffraction spectroscopy and scanning electron microscopy images of recrystallized samples, is approximately 1 mu m for substrate temperature at 300 degree C and annealed at 550 degree C for 3 hours

  9. Effect of Microwave Radiation on Enzymatic and Chemical Peptide Bond Synthesis on Solid Phase

    Directory of Open Access Journals (Sweden)

    Alessandra Basso

    2009-01-01

    Full Text Available Peptide bond synthesis was performed on PEGA beads under microwave radiations. Classical chemical coupling as well as thermolysin catalyzed synthesis was studied, and the effect of microwave radiations on reaction kinetics, beads' integrity, and enzyme activity was assessed. Results demonstrate that microwave radiations can be profitably exploited to improve reaction kinetics in solid phase peptide synthesis when both chemical and biocatalytic strategies are used.

  10. Solid phase carrier for radioimmuno analyses, as well as its manufacture and use

    International Nuclear Information System (INIS)

    Meriadec, B.; Roubertie, P.

    1979-01-01

    The solid phase carrier is in the form of a tablet containing freeze-dried protein-bonded gel, dicalcium phosphate and magnesium stearate. It is able to absorb 0.400 microlitre of an a solution containing antigen-antibody. When contacted with the solution, the tablet swells up and adapts to the shape of the column. The carrier is suitable for the TSH RIA test. (DG) [de

  11. Design of indirect solid-phase immunosorbent methods for detecting arenavirus antigens and antibodies

    Energy Technology Data Exchange (ETDEWEB)

    Ivanov, A.P.; Rezapkin, G.V.; Dzagurova, T.K.; Tkachenko, E.A.

    1984-05-01

    Specifications have been elaborated for formulating indirect solid-phase enzyme-linked immunosorbent assay (ELISA) and radioimmunoassay (SPRIA) methods that employ anti-human and anti-mice G class immunoglobulin (IgG), conjugated with horseradish peroxidase and /sup 125/I for detecting the arenaviruses Junin, Machupo, Tacaribe, Amalpari, Tamiami, Lassa, and LCM (lymphocytic choriomeningitis). These methods make it possible to identify with a high degree of sensitivity arenavirus antigens and antibodies in various kinds of material.

  12. Extraction of bioactive polyphenols from grape marc by a matrix solid-phase dispersion method

    OpenAIRE

    Lores, Marta; Iglesias Estévez, María; Álvarez Casas, Marta; Llompart Vizoso, María; García Jares, Carmen

    2012-01-01

    A matrix solid-phase dispersion process to extract polyphenols from grape marc, a winemaking byproduct, has been optimized by Response Surface Methodology. The dependent variables evaluated were the total polyphenols content, flavanols, hydrocynnamates, and flavonoids. The performance of the extraction method in terms of linearity and precision has also been assessed. The optimized MSPD method provides good results to extract polyphenols from white winemaking byproducts, much less studied tha...

  13. Formation mechanism and luminescence appearance of Mn-doped zinc silicate particles synthesized in supercritical water

    International Nuclear Information System (INIS)

    Takesue, Masafumi; Suino, Atsuko; Hakuta, Yukiya; Hayashi, Hiromichi; Smith, Richard Lee

    2008-01-01

    Luminescence appearance of Mn-doped zinc silicate (Zn 2 SiO 4 :Mn 2+ , ZSM) formed in supercritical water at 400 deg. C and 29 MPa at reaction times from 1 to 4320 min was studied in the relation to its phase formation mechanism. Appearance of luminescent ZSM from green emission by α-ZSM and yellow emission by β-ZSM occurred over the same time period during the onset of phase formation at a reaction time of 2 min. Luminescence appeared at a much lower temperature and at shorter reaction times than the conventional solid-state reaction. Needle-like-shaped α-ZSM was the most stable particle shape and phase in the supercritical water reaction environment and particles formed via two routes: a homogenous nucleation route and a heterogenous route that involves solid-state diffusion and recrystallization. - Graphical abstract: Luminescence appearance of Mn-doped zinc silicate (Zn 2 SiO 4 :Mn 2+ , ZSM) formed in supercritical water at 400 deg. C and 29 MPa were studied in the relation to its phase formation mechanism. Green emission by α-ZSM and yellow emission by β-ZSM occurred over the same time period during the onset of phase formation

  14. Solid, Semisolid, and Liquid Phase States of Individual Submicrometer Particles Directly Probed Using Atomic Force Microscopy.

    Science.gov (United States)

    Lee, Hansol D; Ray, Kamal K; Tivanski, Alexei V

    2017-12-05

    Currently, the impact of various phase states of aerosols on the climate is not well understood, especially for submicrometer sized aerosol particles that typically have extended lifetime in the atmosphere. This is largely due to the inherent size limitations present in current experimental techniques that aim to directly assess the phase states of fine aerosol particles. Herein we present a technique that uses atomic force microscopy to probe directly for the phase states of individual, submicrometer particles by using nanoindentation and nano-Wilhelmy methodologies as a function of relative humidity (RH) and ambient temperature conditions. When using these methodologies for substrate deposited individual sucrose particles, Young's modulus and surface tension can be quantified as a function of RH. We show that the force profiles collected to measure Young's modulus and surface tension can also provide both qualitative and quantitative assessments of phase states that accompany solid, semisolid, and liquid particle phases. Specifically, we introduce direct measurements of relative indentation depth and viscoelastic response distance on a single particle basis at a given applied force to quantitatively probe for the phase state as a function of RH and corresponding viscosity. Thus, we show that the three phase states and phase state transitions of sucrose can be identified and ultimately propose that this technique may also be used to study other atmospherically relevant systems.

  15. Calcium and magnesium silicate hydrates

    International Nuclear Information System (INIS)

    Lothenbach, B.; L'Hopital, E.; Nied, D.; Achiedo, G.; Dauzeres, A.

    2015-01-01

    Deep geological disposals are planed to discard long-lived intermediate-level and high-level radioactive wastes. Clay-based geological barriers are expected to limit the ingress of groundwater and to reduce the mobility of radioelements. In the interaction zone between the cement and the clay based material alteration can occur. Magnesium silicate hydrates (M-S-H) have been observed due to the reaction of magnesium sulfate containing groundwater with cements or in the interaction zone between low-pH type cement and clays. M-S-H samples synthesized in the laboratory showed that M-S-H has a variable composition within 0.7 ≤ Mg/Si ≤ 1.5. TEM/EDS analyses show an homogeneous gel with no defined structure. IR and 29 Si NMR data reveal a higher polymerization degree of the silica network in M-S-H compared to calcium silicate hydrates (C-S-H). The presence of mainly Q 3 silicate tetrahedrons in M-S-H indicates a sheet like or a triple-chain silica structure while C-S-H is characterised by single chain-structure. The clear difference in the silica structure and the larger ionic radius of Ca 2+ (1.1 Angstrom) compared to Mg 2+ (0.8 Angstrom) make the formation of an extended solid solution between M-S-H and C-S-H gel improbable. In fact, the analyses of synthetic samples containing both magnesium and calcium in various ratios indicate the formation of separate M-S-H and C-S-H gels with no or very little uptake of magnesium in CS-H or calcium in M-S-H

  16. A new method for the screening of solid-phase combinatorial libraries for affinity chromatography.

    Science.gov (United States)

    Roque, A Cecília A; Taipa, M Angela; Lowe, Christopher R

    2004-01-01

    A new methodology for the rapid assessment of affinity ligands synthesized by combinatorial solid-phase chemistry is reported. This screening strategy utilizes the target protein conjugated to FITC, and represents an almost universal technique for the preliminary screening of solid-phase combinatorial libraries. The assessment of a triazine-scaffolded solid-phase combinatorial library of ligands, designed to bind to human IgG, was performed with FITC-human IgG, and the results compared with those obtained by conventional affinity chromatographic screening assays. The effect of different molar conjugation ratios of FITC-IgG (F/P) was evaluated. Independently of the F/P ratio, no false negative results were observed, although lower F/P ratios diminished non-specific interactions and the number of false positives. The nature of the substituents on the triazine scaffold was not related to the number of false positive IgG-binding ligands. The reproducibility of the FITC technique, using FITC-human IgG conjugates with low F/P ratio (F/P=2), was also evaluated. The FITC-based technique proved to be efficient and accurate in the identification of strongly binding ligands (binding >50% of loaded protein, by standard affinity chromatographic assays), and is envisaged as a versatile and cost-effective method to screen other systems, and evaluate several binding/elution conditions at small-scale, prior to scale-up to standard affinity chromatography. Copyright 2004 John Wiley & Sons, Ltd.

  17. Nanocapsule-based probe for evaluating the orientation of antibodies immobilized on a solid phase.

    Science.gov (United States)

    Iijima, Masumi; Yoshimoto, Nobuo; Niimi, Tomoaki; Maturana, Andrés Daniel; Kuroda, Shun'ichi

    2013-06-21

    The orientation of sensing molecules on solid phase biosensors has to be optimized to facilitate efficient binding of analytes. Since conventional observation methods (e.g., electron microscopy, atomic force microscopy, time-of-flight secondary ion mass spectrometry) require exaggerated machines and possess insufficient resolution for single molecule analyses, functional assays based on the reactivity to analytes have thus far been used for this optimization. However, it is not clear whether these assays can judge whether sensing molecules are fixed in an oriented-immobilization manner or not. Here, we describe that bio-nanocapsules of about 30 nm diameter, displaying approximately 120 molecules of a tandem form of the immunoglobulin (Ig) G Fc-binding Z domain (ZZ-BNCs), can discriminate between the Fc regions of IgGs fixed in an oriented-immobilization manner and those fixed randomly, thus facilitating the evaluation of the orientation of IgGs in immunosensors. Furthermore, in sandwich immunoassays, ZZ-BNCs can bind specifically to detection-IgGs fixed in an oriented-immobilization manner by antigen-capture IgG complexes, rather than to capture-IgGs fixed randomly onto a solid phase, allowing the simultaneous use of the same IgG as capture- and detection-IgGs. Thus, we demonstrate that ZZ-BNCs are a unique probe for evaluating the orientation of IgGs on a solid phase.

  18. 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)

  19. Increased alloimmunisation and transfusion reaction reporting in patients with solid-phase panreactivity.

    Science.gov (United States)

    Olofson, Andrea M; Chandler, Rachael M; Marx-Wood, Cynthia R; Babcock, Craig A; Dunbar, Nancy M

    2017-11-01

    Automated solid-phase antibody screening uses red blood cell (RBC) membranes immobilised on polystyrene test wells to detect RBC specific antibodies. Despite its time-saving and labour-saving benefits, this method produces a higher rate of nonspecific reactivity compared with manual screening. Solid-phase panreactivity (SPP) is characterised by panreactivity (ie, all test cells reacting) in solid-phase testing accompanied by a negative autocontrol and a lack of reactivity when the same screening cells are tested in tube. The mechanisms underlying SPP and its clinical significance remain unclear. The goals of this study were to describe the prevalence of SPP at our institution and determine the alloimmunisation and transfusion reaction rates within this population. Data were collected on all patients undergoing type and screen testing over a 6-year period. Study patients undergoing subsequent transfusion were evaluated for reported transfusion reactions and development of new alloantibodies. Of the 76 051 patients studied, 0.7% demonstrated SPP of which 11% developed new alloantibodies. The transfusion reaction reporting rate among patients with SPP was 2%. Our data suggest that patients with SPP have higher rates of reported transfusion reactions and alloantibody development compared with those without SPP. Published by the BMJ Publishing Group Limited. For permission to use (where not already granted under a licence) please go to http://www.bmj.com/company/products-services/rights-and-licensing/.

  20. Studies on solid phase synthesis,characterization and fluorescent property of the new rare earth complexes

    Directory of Open Access Journals (Sweden)

    Jianwei SHI

    2015-04-01

    Full Text Available Rare earth-β-diketone ligand complex luminescent material has stable chemical properties and excellent luminous property. Using europium oxide and (γ-NTA as raw materials, novel rare earth-β-dione complexes are synthesized by solid state coordination chemistry. The synthesis temperature and milling time are discussed for optimization. Experimental results show that the suitable reaction situation is at 50 ℃ and 20 h for solid-phase synthesis. The compositions and structures of the complexes are characterized by means of elemental analysis, UV-Vis and FTIR methods, and the phase stability of the complex is determined by using TG-DTA technique. It is proved that preparation of waterless binary rare earth complexes by the solid phase reaction method results in a higher product yield. The fluorescence spectra show that between Eu (Ⅲ and γ-NTA, there exists efficient energy transfer, and the rare earth complexes synthesis is an excellent red bright light-emitting material with excellent UV excited luminescence properties.

  1. Preparation of fluorescent DNA probe by solid-phase organic synthesis

    Directory of Open Access Journals (Sweden)

    2009-08-01

    Full Text Available Fluorescent DNA probe based on fluorescence resonance energy transfer (FRET was prepared by solid-phase organic synthesis when CdTe quantum dots (QDs were as energy donors and Au nanoparticles (AuNPs were as energy accepters. The poly(divinylbenzene core/poly(4-vinylpyridine shell microspheres, as solid-phase carriers, were prepared by seeds distillation-precipitation polymerization with 2,2′-azobisisobutyronitrile (AIBN as initiator in neat acetonitrile. The CdTe QDs and AuNPs were self-assembled on the surface of core/shell microspheres, and then the linkage of CdTe QDs with oligonucleotides (CdTe-DNA and AuNPs with complementary single-stranded DNA (Au-DNA was on the solid-phase carriers instead of in aqueous solution. The hybridization of complementary double stranded DNA (dsDNA bonded to the QDs and AuNPs (CdTe-dsDNA-Au determined the FRET distance of CdTe QDs and AuNPs. Compared with the fluorescence of CdTe-DNA, the fluorescence of CdTe-dsDNA-Au conjugates (DNA probes decreased extremely, which indicated that the FRET occurred between CdTe QDs and AuNPs. The probe system would have a certain degree recovery of fluorescence when the complementary single stranded DNA was introduced into this system, which showed that the distance between CdTe QDs and AuNPs was increased.

  2. Solid phase extraction for the speciation and preconcentration of inorganic selenium in water samples: a review.

    Science.gov (United States)

    Herrero Latorre, C; Barciela García, J; García Martín, S; Peña Crecente, R M

    2013-12-04

    Selenium is an essential element for the normal cellular function of living organisms. However, selenium is toxic at concentrations of only three to five times higher than the essential concentration. The inorganic forms (mainly selenite and selenate) present in environmental water generally exhibit higher toxicity (up to 40 times) than organic forms. Therefore, the determination of low levels of different inorganic selenium species in water is an analytical challenge. Solid-phase extraction has been used as a separation and/or preconcentration technique prior to the determination of selenium species due to the need for accurate measurements for Se species in water at extremely low levels. The present paper provides a critical review of the published methods for inorganic selenium speciation in water samples using solid phase extraction as a preconcentration procedure. On the basis of more than 75 references, the different speciation strategies used for this task have been highlighted and classified. The solid-phase extraction sorbents and the performance and analytical characteristics of the developed methods for Se speciation are also discussed. Copyright © 2013 Elsevier B.V. All rights reserved.

  3. Luminescence properties of cerium-doped di-strontium magnesium di-silicate phosphor by the solid-state reaction method

    Science.gov (United States)

    Prasad Sahu, Ishwar

    2016-05-01

    A series of Sr2MgSi2O7:xCe3+ (x = 1.0%, 2.0%, 3.0%, 4.0% and 5.0%) phosphors were synthesized by the solid-state reaction method. The phosphor with optimum thermoluminescence, photoluminescence and mechanoluminescence (ML) intensity was characterized by X-ray diffraction, field emission scanning electron microscopy, energy-dispersive X-ray spectroscopy and Fourier transform infrared techniques. The trapping parameters (i.e. activation energy, frequency factor and order of the kinetics) of each synthesized phosphor have been calculated using the peak shape method and the results have been discussed. Under ultraviolet excitation (325 nm), Sr2MgSi2O7:xCe3+ phosphors were composed of a broad band peaking at 385 nm, belonging to the broad emission band which emits violet-blue color. Commission International de I'Eclairage coordinates have been calculated for each sample and their overall emission is near violet-blue light. In order to investigate the suitability of the samples for industrial uses, color purity and color rendering index were calculated. An ML intensity of optimum [Sr2MgSi2O7:Ce3+ (3.0%)] phosphor increases linearly with increasing impact velocity of the moving piston which suggests that these phosphors can be used as fracto-ML-based devices. The time of the peak ML intensity and the decay rate did not change significantly with respect to increasing impact velocity of the moving piston.

  4. Geochemistry, mineralogy, solid-phase fractionation and oral bioaccessibility of lead in urban soils of Lisbon.

    Science.gov (United States)

    Reis, A P; Patinha, C; Wragg, J; Dias, A C; Cave, M; Sousa, A J; Costa, C; Cachada, A; Ferreira da Silva, E; Rocha, F; Duarte, A

    2014-10-01

    An urban survey of Lisbon, the largest city in Portugal, was carried out to investigate its environmental burden, emphasizing metallic elements and their public health impacts. This paper examines the geochemistry of lead (Pb) and its influence on human health data. A total of 51 soil samples were collected from urban recreational areas used by children to play outdoors. The semi-quantitative analysis of Pb was carried out by inductively coupled plasma mass spectrometry after an acid digestion. X-ray diffraction was used to characterize the soil mineralogy. The solid-phase distribution of Pb in the urban soils was investigated on a subset of 7 soils, out of a total of 51 samples, using a non-specific sequential extraction method coupled with chemometric analysis. Oral bioaccessibility measurements were obtained using the Unified BARGE Method developed by the Bioaccessibility Research Group of Europe. The objectives of the study are as follows: (1) investigation of Pb solid-phase distribution; (2) interpretation of Pb oral bioaccessibility measurements; (3) integration of metal geochemistry with human health data; and (4) understanding the influence of geochemistry and mineralogy on oral bioaccessibility. The results show that the bioaccessible fraction of Pb is lower when major metal fractions are associated with less soluble soil phases such as Fe oxyhydroxides, and more increased when the metal is in the highly soluble carbonate phase. However, there is some evidence that the proportion of carbonates in the soil environment is also a key control over the oral bioaccessibility of Pb, irrespective of its solid-phase fractionation.

  5. 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.

  6. Lattice model theory of the equation of state covering the gas, liquid, and solid phases

    Science.gov (United States)

    Bonavito, N. L.; Tanaka, T.; Chan, E. M.; Horiguchi, T.; Foreman, J. C.

    1975-01-01

    The three stable states of matter and the corresponding phase transitions were obtained with a single model. Patterned after Lennard-Jones and Devonshires's theory, a simple cubic lattice model containing two fcc sublattices (alpha and beta) is adopted. The interatomic potential is taken to be the Lennard-Jones (6-12) potential. Employing the cluster variation method, the Weiss and the pair approximations on the lattice gas failed to give the correct phase diagrams. Hybrid approximations were devised to describe the lattice term in the free energy. A lattice vibration term corresponding to a free volume correction is included semi-phenomenologically. The combinations of the lattice part and the free volume part yield the three states and the proper phase diagrams. To determine the coexistence regions, the equalities of the pressure and Gibbs free energy per molecule of the coexisting phases were utilized. The ordered branch of the free energy gives rise to the solid phase while the disordered branch yields the gas and liquid phases. It is observed that the triple point and the critical point quantities, the phase diagrams and the coexistence regions plotted are in good agreement with the experimental values and graphs for argon.

  7. 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…

  8. Observation of a New High-Pressure Solid Phase in Dynamically Compressed Aluminum

    Science.gov (United States)

    Polsin, D. N.

    2017-10-01

    Aluminum is ideal for testing theoretical first-principles calculations because of the relative simplicity of its atomic structure. Density functional theory (DFT) calculations predict that Al transforms from an ambient-pressure, face-centered-cubic (fcc) crystal to the hexagonal close-packed (hcp) and body-centered-cubic (bcc) structures as it is compressed. Laser-driven experiments performed at the University of Rochester's Laboratory for Laser Energetics and the National Ignition Facility (NIF) ramp compressed Al samples to pressures up to 540 GPa without melting. Nanosecond in-situ x-ray diffraction was used to directly measure the crystal structure at pressures where the solid-solid phase transformations of Al are predicted to occur. Laser velocimetry provided the pressure in the Al. Our results show clear evidence of the fcc-hcp and hpc-bcc transformations at 216 +/- 9 GPa and 321 +/- 12 GPa, respectively. This is the first experimental in-situ observation of the bcc phase in compressed Al and a confirmation of the fcc-hcp transition previously observed under static compression at 217 GPa. The observations indicate these solid-solid phase transitions occur on the order of tens of nanoseconds time scales. In the fcc-hcp transition we find the original texture of the sample is preserved; however, the hcp-bcc transition diminishes that texture producing a structure that is more polycrystalline. The importance of this dynamic is discussed. The NIF results are the first demonstration of x-ray diffraction measurements at two different pressures in a single laser shot. This material is based upon work supported by the Department of Energy National Nuclear Security Administration under Award Number DE-NA0001944.

  9. Solid phase extraction and spectrophotometric determination of palladium with 2-(2-quinolylazo-5-diethylaminobenzoic acid

    Directory of Open Access Journals (Sweden)

    WEIZU YANG

    2006-07-01

    Full Text Available Asensitive, selective and rapid method for the determination of palladium based on the rapid reaction of palladium(II with 2-(2-quinolylazo-5-diethylaminobenzoic acid (QADEAB and the solid phase extraction of the Pd(II –QADEAB chelate with a reversed phase polymer-based C18 cartridge was developed. In the presence of 0.05 – 0. 5 mol/L of hydrochloric acid solution and cetyl trimethylammonium bromide (CTAB medium, QADEAB reacts with palladium(II to form a violet complex with a mole ratio 1:2 (palladium to QADEAB. The chelate was enriched by solid phase extraction with a reversed phase polymer-based C18 cartridge. An enrichment factor of 200 was obtained by elution of the chelate form the cartridge with the minimal amount of isopentyl alcohol. The molar absorptivity of the chelate in the isopentyl alcohol medium was 1.43 × 105 L mol-1 cm-1 at 628 nm. Beer’s law was obeyed in the range of 0.01 – 1.2 mg/mL. The relative standard deviation for eleven replicate samples at the 0.2 mg/L level was 2.18 %. The attained detection limit amounted to 0.02 mg/L in the original samples. This method was applied to the determination of palladium in environmental samples with good results.

  10. Quantum computational capability of a 2D valence bond solid phase

    International Nuclear Information System (INIS)

    Miyake, Akimasa

    2011-01-01

    Highlights: → Our model is the 2D valence bond solid phase of a quantum antiferromagnet. → Universal quantum computation is processed by measurements of quantum correlations. → An intrinsic complexity of strongly-correlated quantum systems could be a resource. - Abstract: Quantum phases of naturally-occurring systems exhibit distinctive collective phenomena as manifestation of their many-body correlations, in contrast to our persistent technological challenge to engineer at will such strong correlations artificially. Here we show theoretically that quantum correlations exhibited in the 2D valence bond solid phase of a quantum antiferromagnet, modeled by Affleck, Kennedy, Lieb, and Tasaki (AKLT) as a precursor of spin liquids and topological orders, are sufficiently complex yet structured enough to simulate universal quantum computation when every single spin can be measured individually. This unveils that an intrinsic complexity of naturally-occurring 2D quantum systems-which has been a long-standing challenge for traditional computers-could be tamed as a computationally valuable resource, even if we are limited not to create newly entanglement during computation. Our constructive protocol leverages a novel way to herald the correlations suitable for deterministic quantum computation through a random sampling, and may be extensible to other ground states of various 2D valence bond phases beyond the AKLT state.

  11. Long-wave equivalent viscoelastic solids for porous rocks saturated by two-phase fluids

    Science.gov (United States)

    Santos, J. E.; Savioli, G. B.

    2018-04-01

    Seismic waves traveling across fluid-saturated poroelastic materials with mesoscopic-scale heterogeneities induce fluid flow and Biot's slow waves generating energy loss and velocity dispersion. Using Biot's equations of motion to model these type of heterogeneities would require extremely fine meshes. We propose a numerical upscaling procedure to determine the complex and frequency dependent P-wave and shear moduli of an effective viscoelastic medium long-wave equivalent to a poroelastic solid saturated by a two-phase fluid. The two-phase fluid is defined in terms of capillary pressure and relative permeability flow functions. The P-wave and shear effective moduli are determined using harmonic compressibility and shear experiments applied on representative samples of the bulk material. Each experiment is associated with a boundary value problem that is solved using the finite element method. Since a poroelastic solid saturated by a two-phase fluid supports the existence of two slow waves, this upscaling procedure allows to analyze their effect on the mesoscopic-loss mechanism in hydrocarbon reservoir formations. Numerical results show that a two-phase Biot medium model predicts higher attenuation than classic Biot models.

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

    Science.gov (United States)

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

    2015-09-21

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

  13. Nanostructure of Calcium Silicate Hydrates in Cements

    KAUST Repository

    Skinner, L. B.

    2010-05-11

    Calcium silicate hydrate (CSH) is the major volume phase in the matrix of Portland cement concrete. Total x-ray scattering measurements with synchrotron x rays on synthetic CSH(I) shows nanocrystalline ordering with a particle diameter of 3.5(5) nm, similar to a size-broadened 1.1 nm tobermorite crystal structure. The CSH component in hydrated tricalcium silicate is found to be similar to CSH(I). Only a slight bend and additional disorder within the CaO sheets is required to explain its nanocrystalline structure. © 2010 The American Physical Society.

  14. 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

  15. Use of solid phase microextraction (SPME) for profiling the volatile metabolites produced by Glomerella cingulata.

    Science.gov (United States)

    Miyazawa, Mitsuo; Kimura, Minako; Yabe, Yoshito; Tsukamoto, Daisuke; Sakamoto, Masaya; Horibe, Isao; Okuno, Yoshiharu

    2008-01-01

    The profile of volatile organic compounds (VOCs) released from Glomerella cingulata using solid phase microextraction (SPME) with different fibers, Polydimethylsiloxane (PDMS), Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), Carboxen/Polydimethylsiloxane (CAR/PDMS) and Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), was investigated. C4-C6 aliphatic alcohols were the predominant fraction of VOCs isolated by CAR/PDMS fiber. Sesquiterpene hydrocarbons represented 20.3% of VOCs isolated by PDMS fiber. During the growth phase, Ochracin was produced in the large majority of VOCs. 3-Methylbutanol and phenylethyl alcohol were found in the log phase of it. Alcohols were found in cultures of higher age, while sesquiterpenes were found to be characteristic of initial growth stage of G. cingulata.

  16. Relationship between Structure and Fluctuations of Lipid Nonlamellar Phases Deposited at the Solid-Liquid Interface.

    Science.gov (United States)

    Nylander, Tommy; Soltwedel, Olaf; Ganeva, Marina; Hirst, Christopher; Holdaway, James; Arteta, Marianna Yanez; Wadsäter, Maria; Barauskas, Justas; Frielinghaus, Henrich; Holderer, Olaf

    2017-04-06

    The structure and dynamics of nanostructure films formed by mixtures of soy phosphatidylcholine and glycerol dioleate at the silicon-aqueous interface were studied by grazing incidence neutron spin echo spectroscopy (GINSES), specular and off-specular neutron reflectometry, and small-angle X-ray diffraction. Reverse hexagonal (H II ) and micellar cubic phase (Fd3m) layers at the solid-liquid interface have been identified with neutron reflectometry measurements. A preferred orientation of the liquid crystalline (LC) domains was observed only for the anisotropic H II phase. The size of the LC domains was found to be about 1 micrometer as estimated from the width of the diffraction peaks. GINSES revealed that the cubic phase forms rather rigid films. In comparison, the H II film was more flexible, appearing as a modified undulation spectrum of the cylinders due to the interaction with the substrate.

  17. Dimeric Building Blocks for Solid-Phase Synthesis of α-Peptide-β-Peptoid Chimeras

    DEFF Research Database (Denmark)

    Seigan, Gitte Bonke; Vedel, Line; Matthias, Witt,

    2008-01-01

    Recently, a novel type of antimicrobial and proteolytically stable peptidomimetic oligomers having an α-peptide-β-peptoid chimeric backbone was reported. The present paper describes efficient protocols for the preparation of a wide range of dimeric building blocks, displaying different types...... of side-chains, for use in solid-phase synthesis (SPS) of libraries of this type of oligomers. The β-peptoid monomers were obtained by microwave-assisted aza-Michael additions to acrylic esters. Subsequent solution-phase peptide coupling with suitably protected α-amino acids afforded dimeric intermediates....... Even sluggish peptide couplings, involving sterically hindered N-alkyl-β-alanines or amino acids with bulky side-chains, gave high yields on multigram-scale when using microwave (MW) irradiation. Protecting group and side-chain manipulations were performed as one-pot solution-phase procedures to afford...

  18. Solid-Phase and Oscillating Solution Crystallization Behavior of (+)- and (-)-N-Methylephedrine.

    Science.gov (United States)

    Tulashie, Samuel Kofi; Polenske, Daniel; Seidel-Morgenstern, Andreas; Lorenz, Heike

    2016-11-01

    This work involves the study of the solid-phase and solution crystallization behavior of the N-methylephedrine enantiomers. A systematic investigation of the melt phase diagram of the enantiomeric N-methylephedrine system was performed considering polymorphism. Two monotropically related modifications of the enantiomer were found. Solubilities and the ternary solubility phase diagrams of N-methylephedrine enantiomers in 2 solvents [isopropanol:water, 1:3 (Vol) and (2R, 3R)-diethyl tartrate] were determined in the temperature ranges between 15°C and 25°C, and 25°C and 40°C, respectively. Preferential nucleation and crystallization experiments at higher supersaturation leading to an unusual oscillatory crystallization behavior as well as a successful preferential crystallization experiment at lower supersaturation are presented and discussed. Copyright © 2016. Published by Elsevier Inc.

  19. Solid-phase extraction and HPLC assay of nicotine and cotinine in plasma and brain.

    Science.gov (United States)

    Dawson, Ralph; Messina, S M; Stokes, C; Salyani, S; Alcalay, N; De Fiebre, N C; De Fiebre, C M

    2002-01-01

    The aim of this study was to develop a simple and reliable assay for nicotine (NIC) and its major metabolite, cotinine (COT), in plasma and brain. A method was developed that uses an extraction method compatible with reverse-phase high-performance liquid chromatography (HPLC) separation and ultraviolet (UV) detection. Sequential solid-phase extraction on silica columns followed by extraction using octadecyl (C18) columns resulted in mean percent recovery (n = 5) of 51 +/- 5, 64 +/- 10, and 52 +/- 10% for NIC, COT, and phenylimidazole (PI), respectively, in spiked 1-mL serum samples. Recovery (mean +/- SEM) of the internal standard (PI) from spiked samples of nicotine-injected rats averaged 64.1 +/- 1.5% (n = 138) from plasma, and 20.7+/-0.8% (n = 128) from brain. The limits of detection of NIC in plasma samples were approximately 8 ng per mL, and of COT, 13.6 ng per mL. Further optimization of our extraction method, using slower flow rates and solid-phase extraction on silica columns, followed by C18 column extraction, yielded somewhat better recoveries (38 +/-3%) for 1-mL brain homogenates. Interassay precision (coefficient of variation) was determined on the basis of daily calibrations for 2 months and was found to be 7%, 9%, and 9% for NIC, COT, and PI, respectively, whereas intra-assay variability was 3.9% for both NIC and COT. Limited studies were performed on analytical columns for comparison of retention, resolution, asymmetry, and column capacity. We concluded that a simple two-step solid-phase extraction method, coupled with HPLC separation and UV detection, can be used routinely to measure NIC and COT in biological fluids and tissues.

  20. Surface-initiated phase transition in solid hydrogen under the high-pressure compression

    Science.gov (United States)

    Lei, Haile; Lin, Wei; Wang, Kai; Li, Xibo

    2018-03-01

    The large-scale molecular dynamics simulations have been performed to understand the microscopic mechanism governing the phase transition of solid hydrogen under the high-pressure compression. These results demonstrate that the face-centered-cubic-to-hexagonal close-packed phase transition is initiated first at the surfaces at a much lower pressure than in the volume and then extends gradually from the surface to volume in the solid hydrogen. The infrared spectra from the surface are revealed to exhibit a different pressure-dependent feature from those of the volume during the high-pressure compression. It is thus deduced that the weakening intramolecular H-H bonds are always accompanied by hardening surface phonons through strengthening the intermolecular H2-H2 coupling at the surfaces with respect to the counterparts in the volume at high pressures. This is just opposite to the conventional atomic crystals, in which the surface phonons are softening. The high-pressure compression has further been predicted to force the atoms or molecules to spray out of surface to degrade the pressure. These results provide a glimpse of structural properties of solid hydrogen at the early stage during the high-pressure compression.

  1. Solid-phase extractants based on ionic liquids for radionuclide preconcentration and separation

    International Nuclear Information System (INIS)

    Suchanek, P.; Galambos, M.; Rosskopfova, O.; Rajec, P.; Meciarova, M.

    2014-01-01

    Ionic liquids are organic salts composed by ions with melting temperature lower than 100 grad C. According to their unique properties such as immeasurable vapour pressure, non-flammablity, stability at higher temperatures, ability to solvate organic, inorganic or polymeric materials and high ionic conductivity are proposed to be used in various industry applications such as catalysts or environmental friendly solvents. One of the main objectives of ionic liquids research is their ability to replace conventional organic solvents, which are volatile, flammable, have carcinogenic effects on living organisms and have high impact on environment in industrial processes. They can be also used in biological reactions, as catalysts, in inorganic or organic synthesis, purification processes and for gas separation. Radionuclide extraction properties of ionic liquids are studied due to their high selectivity and kinetic properties of these compounds. The possibility of solid matrix impregnation with ionic liquids shows high potential for development of new solid phase extractants for radionuclide removal or concentration. The result of this work indicate that phosphonium ionic liquid Cyphos 101 impregnated on Teflon or Amberchrom CG-300s solid matrix is suitable for TcO 4 - extraction from aquaeous phase. (authors)

  2. Soxhlet-assisted matrix solid phase dispersion to extract flavonoids from rape (Brassica campestris) bee pollen.

    Science.gov (United States)

    Ma, Shuangqin; Tu, Xijuan; Dong, Jiangtao; Long, Peng; Yang, Wenchao; Miao, Xiaoqing; Chen, Wenbin; Wu, Zhenhong

    2015-11-15

    Soxhlet-assisted matrix solid phase dispersion (SA-MSPD) method was developed to extract flavonoids from rape (Brassica campestris) bee pollen. Extraction parameters including the extraction solvent, the extraction time, and the solid support conditions were investigated and optimized. The best extraction yields were obtained using ethanol as the extraction solvent, silica gel as the solid support with 1:2 samples to solid support ratio, and the extraction time of one hour. Comparing with the conventional solvent extraction and Soxhlet method, our results show that SA-MSPD method is a more effective technique with clean-up ability. In the test of six different samples of rape bee pollen, the extracted content of flavonoids was close to 10mg/g. The present work provided a simple and effective method for extracting flavonoids from rape bee pollen, and it could be applied in the studies of other kinds of bee pollen. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Application of solid-phase extraction to agar-supported fermentation.

    Science.gov (United States)

    Le Goff, Géraldine; Adelin, Emilie; Cortial, Sylvie; Servy, Claudine; Ouazzani, Jamal

    2013-09-01

    Agar-supported fermentation (Ag-SF), a variant of solid-state fermentation, has recently been improved by the development of a dedicated 2 m(2) scale pilot facility, Platotex. We investigated the application of solid-phase extraction (SPE) to Ag-SF in order to increase yields and minimize the contamination of the extracts with agar constituents. The selection of the appropriate resin was conducted on liquid-state fermentation and Diaion HP-20 exhibited the highest recovery yield and selectivity for the metabolites of the model fungal strains Phomopsis sp. and Fusarium sp. SPE applied to Ag-SF resulted in a particular compartmentalization of the culture. The mycelium that requires oxygen to grow migrates to the top layer and formed a thick biofilm. The resin beads intercalate between the agar surface and the mycelium layer, and trap directly the compounds secreted by the mycelium through a "solid-solid extraction" (SSE) process. The resin/mycelium layer is easily recovered by scraping the surface and the target metabolites extracted by methanol. Ag-SF associated to SSE represents an ideal compromise for the production of bioactive secondary metabolites with limited economic and environmental impact.

  4. Solid State Large Area Pulsed Solar Simulator for 3-, 4- and 6-Junction Solar Cell Arrays, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — The Phase I was successful in delivering a complete prototype of the proposed innovation, an LED-based, solid state, large area, pulsed, solar simulator (ssLAPSS)....

  5. Analysis of ecologically relevant pharmaceuticals in wastewater and surface water using selective solid phase extraction and UPLC/MS/MS

    Science.gov (United States)

    A rapid and sensitive method has been developed for the analysis of 48 human prescription active pharmaceutical ingredients (APIs) and 6 metabolites of interest, utilizing selective solid-phase extraction (SPE) and ultra performance liquid chromatography in combination with tripl...

  6. The Potential of Amorphous Solid Secondary Organic Aerosol to Form Mixed-Phase and Cirrus Clouds

    Science.gov (United States)

    Knopf, D. A.; Wang, B.; Lambe, A. T.; Massoli, P.; Onasch, T. B.; Davidovits, P.; Worsnop, D. R.

    2012-12-01

    Atmospheric ice formation by heterogeneous nucleation, which results in cirrus and mixed-phase cloud formation, is one of the least understood processes affecting the global radiation budget, the hydrological cycle, and water vapor distribution. It is commonly assumed that inorganic particles such as mineral dust and solid ammonium sulfate represent important atmospheric ice nuclei (IN). However, a growing body of evidence suggests that secondary organic aerosols (SOA), which are ubiquitous in the atmosphere, exist in a solid (glassy) state. This implies that SOA may also play a role in ice cloud formation by acting as IN, but has not previously been experimentally verified. Here, we report observations of water uptake and ice nucleation via condensation, immersion, and deposition modes initiated by amorphous SOA particles at temperatures from T = 200 - 250 K and relative humidity (RH) from subsaturation conditions up to water saturation. SOA particles with oxygen-to-carbon (O/C) ratios ranging from 0.3 to 1.0 are generated from gas-phase OH oxidation of naphthalene in a flow reactor. At T > 230 K, water uptake at subsaturation conditions is correlated with SOA oxidation level (O/C ratio). This initial water uptake is followed by a moisture-induced phase transition and subsequent immersion freezing. At T measurements of particle density, hygroscopicity, and bounced fraction, the latter indicating particle phase state. Above Tg, water uptake and immersion freezing is observed when the particles are liquid or semi-solid. Below Tg, deposition ice nucleation is observed when the particles are solid. The data show that particle phase and viscosity govern the particles' response to temperature and RH and provide a straightforward interpretation for the observed different heterogeneous ice nucleation pathways and water uptake by the laboratory-generated SOA and previously investigated fulvic acid surrogate particles and organic dominated field-collected particles. These

  7. Computer aided testing of steel samples deformation at coexistence liquid and solid phase

    International Nuclear Information System (INIS)

    Hojny, M.; Glowacki, M.

    2007-01-01

    The paper reports the results of experimental and theoretical work leading to construction of a CAE system dedicated to the numerical simulation of plastic deformation of steel at coexistence liquid and solid phase. A coupled thermal-mechanical model including inverse analysis technique was adopted for the solver. The advantage of the solution was the analytical form of both incompressibility and mass conservation conditions. This can prevent usual FEM variational solution problems concerning unintentional specimen volume loss caused by the numerical errors. The only well known machine allowing tests in the discussed temperature range is the GLEEBLE thermo-mechanical simulator. Experiments of deformation of steel in semi-solid state by using this machine are very expensive. Therefore, application of dedicated computer simulation system with inverse method makes tests possible and results in lowering testing cost

  8. Random phase approximation correlation energy using a compact representation for linear response functions: application to solids

    Science.gov (United States)

    Kaoui, Fawzi; Rocca, Dario

    2016-01-01

    A new approach was recently presented to compute correlation energies within the random phase approximation using Lanczos chains and an optimal basis set (Rocca 2014 J. Chem. Phys. 140 18A501). This novel method avoids the explicit calculation of conduction states and represents linear response functions on a compact auxiliary basis set obtained from the diagonalization of an approximate dielectric matrix that contains only the kinetic energy contribution. Here, we extend this formalism, originally implemented for molecular systems, to treat periodic solids. In particular, the approximate dielectric matrix used to build the auxiliary basis set is generalized to avoid unphysical negative gaps, that make the model inefficient. The numerical convergence of the method is discussed and the accuracy is demonstrated considering a set including three covalently bonded (C, Si, and SiC) and three weakly bonded (Ne, Ar, and Kr) solids.

  9. Liquid-solid surface phase transformation of fluorinated fullerene on monolayer tungsten diselenide

    KAUST Repository

    Song, Zhibo

    2018-04-04

    Hybrid van der Waals heterostructures constructed by the integration of organic molecules and two-dimensional (2D) transition metal dichalcogenide (TMD) materials have useful tunable properties for flexible electronic devices. Due to the chemically inert and atomically smooth nature of the TMD surface, well-defined crystalline organic films form atomically sharp interfaces facilitating optimal device performance. Here, the surface phase transformation of the supramolecular packing structure of fluorinated fullerene (C60F48) on single-layer tungsten diselenide (WSe2) is revealed by low-temperature scanning tunneling microscopy, from thermally stable liquid to solid phases as the coverage increases. Statistical analysis of the intermolecular interaction potential reveals that the repulsive dipole-dipole interaction induced by interfacial charge transfer and substrate-mediated interactions play important roles in stabilizing the liquid C60F48 phases. Theoretical calculations further suggest that the dipole moment per C60F48 molecule varies with the surface molecule density, and the liquid-solid transformation could be understood from the perspective of the thermodynamic free energy for open systems. This study offers insights into the growth behavior at 2D organic/TMD hybrid heterointerfaces.

  10. Liquid-solid surface phase transformation of fluorinated fullerene on monolayer tungsten diselenide

    Science.gov (United States)

    Song, Zhibo; Wang, Qixing; Li, Ming-Yang; Li, Lain-Jong; Zheng, Yu Jie; Wang, Zhuo; Lin, Tingting; Chi, Dongzhi; Ding, Zijing; Huang, Yu Li; Thye Shen Wee, Andrew

    2018-04-01

    Hybrid van der Waals heterostructures constructed by the integration of organic molecules and two-dimensional (2D) transition metal dichalcogenide (TMD) materials have useful tunable properties for flexible electronic devices. Due to the chemically inert and atomically smooth nature of the TMD surface, well-defined crystalline organic films form atomically sharp interfaces facilitating optimal device performance. Here, the surface phase transformation of the supramolecular packing structure of fluorinated fullerene (C60F48 ) on single-layer tungsten diselenide (WSe2) is revealed by low-temperature scanning tunneling microscopy, from thermally stable liquid to solid phases as the coverage increases. Statistical analysis of the intermolecular interaction potential reveals that the repulsive dipole-dipole interaction induced by interfacial charge transfer and substrate-mediated interactions play important roles in stabilizing the liquid C60F48 phases. Theoretical calculations further suggest that the dipole moment per C60F48 molecule varies with the surface molecule density, and the liquid-solid transformation could be understood from the perspective of the thermodynamic free energy for open systems. This study offers insights into the growth behavior at 2D organic/TMD hybrid heterointerfaces.

  11. On-cartridge derivatisation using matrix solid phase dispersion for the determination of cyclamate in foods

    International Nuclear Information System (INIS)

    Li, Jianjun; Liu, Yun; Liu, Qianping; Hui, Junfeng; Liu, Yangzi

    2017-01-01

    A novel method for determination of sodium cyclamate in foods was developed. In this method, a syringe was loaded with the homogeneous mixture of the sample, KMnO 4 powder and silica dispersant and used as a matrix solid phase dispersion (MSPD) reactor. As the reactor was infiltrated with small amounts of concentrated HCl, cyclamate was converted to 2-chlorocyclohexanone quickly and effectively within 5 min and determined by HPLC on a reversed-phase column using UV detection at a wavelength of 310 nm. Comparing with the traditional derivatisation in solution, the better clean-up was provided using on-cartridge derivatisation of MSPD, and much time, labor, and expense were saved. The results showed good linearity (r 2  = 0.9998) over the concentration range of 1–500 mg/L. The limit of detection (LOD) and limits of quantification (LOQ) of the cyclamate were 0.3 mg/L and 1 mg/L respectively. The recoveries ranged from 91.6% to 101.3% with the relative standard deviations (RSDs) in the range of 2.5%–4.3%. - Highlights: • A novel method was developed for the determination of cyclamate in foods. • On cartridge derivatisation, using matrix solid phase dispersion, was developed. • A new derivatisation reaction for cyclamate conversion to 2-chlorocyclohexanone was developed. • The method was rapid, simple, inexpensive, effective.

  12. On-cartridge derivatisation using matrix solid phase dispersion for the determination of cyclamate in foods

    Energy Technology Data Exchange (ETDEWEB)

    Li, Jianjun, E-mail: bootan12@126.com [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, Northwest University, Xi' an 710069 (China); National Engineering Research Center for Miniaturized Detection Systems, Xi' an 710069 (China); Liu, Yun [College of Food Engineering and Nutritional Science, Shaanxi Normal University, Xi' an 710062 (China); Liu, Qianping [National Engineering Research Center for Miniaturized Detection Systems, Xi' an 710069 (China); Hui, Junfeng [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, Northwest University, Xi' an 710069 (China); Liu, Yangzi [National Engineering Research Center for Miniaturized Detection Systems, Xi' an 710069 (China)

    2017-06-15

    A novel method for determination of sodium cyclamate in foods was developed. In this method, a syringe was loaded with the homogeneous mixture of the sample, KMnO{sub 4} powder and silica dispersant and used as a matrix solid phase dispersion (MSPD) reactor. As the reactor was infiltrated with small amounts of concentrated HCl, cyclamate was converted to 2-chlorocyclohexanone quickly and effectively within 5 min and determined by HPLC on a reversed-phase column using UV detection at a wavelength of 310 nm. Comparing with the traditional derivatisation in solution, the better clean-up was provided using on-cartridge derivatisation of MSPD, and much time, labor, and expense were saved. The results showed good linearity (r{sup 2} = 0.9998) over the concentration range of 1–500 mg/L. The limit of detection (LOD) and limits of quantification (LOQ) of the cyclamate were 0.3 mg/L and 1 mg/L respectively. The recoveries ranged from 91.6% to 101.3% with the relative standard deviations (RSDs) in the range of 2.5%–4.3%. - Highlights: • A novel method was developed for the determination of cyclamate in foods. • On cartridge derivatisation, using matrix solid phase dispersion, was developed. • A new derivatisation reaction for cyclamate conversion to 2-chlorocyclohexanone was developed. • The method was rapid, simple, inexpensive, effective.

  13. Process for forming a homogeneous oxide solid phase of catalytically active material

    Science.gov (United States)

    Perry, Dale L.; Russo, Richard E.; Mao, Xianglei

    1995-01-01

    A process is disclosed for forming a homogeneous oxide solid phase reaction product of catalytically active material comprising one or more alkali metals, one or more alkaline earth metals, and one or more Group VIII transition metals. The process comprises reacting together one or more alkali metal oxides and/or salts, one or more alkaline earth metal oxides and/or salts, one or more Group VIII transition metal oxides and/or salts, capable of forming a catalytically active reaction product, in the optional presence of an additional source of oxygen, using a laser beam to ablate from a target such metal compound reactants in the form of a vapor in a deposition chamber, resulting in the deposition, on a heated substrate in the chamber, of the desired oxide phase reaction product. The resulting product may be formed in variable, but reproducible, stoichiometric ratios. The homogeneous oxide solid phase product is useful as a catalyst, and can be produced in many physical forms, including thin films, particulate forms, coatings on catalyst support structures, and coatings on structures used in reaction apparatus in which the reaction product of the invention will serve as a catalyst.

  14. Light yield and energy resolution studies for SoLid phase 1

    Science.gov (United States)

    Boursette, Delphine; SoLid Collaboration

    2017-09-01

    The SoLid experiment is searching for sterile neutrinos at a nuclear research reactor. It looks for inverse beta decays (producing a positron and a neutron in delayed coincidence) with a very segmented detector made of thousands of scintillating cubes. SoLid has a very innovative hybrid technology with two different scintillators which have different light emissions: polyvynil-toluene cubes (PVT) to detect the positrons and 6LiF:ZnS sheets on two faces of each PVT cube to detect the neutrons. It allows us to do an efficient pulse shape analysis to identify the signals from neutrons and positrons. The 288 kg detector prototype (SM1) took data in 2015. It demonstrated the detection principle and background rejection efficiency. The construction of SoLid phase I (˜ 1.5 t) has now started. To improve the energy resolution of SoLid phase I, we have tried to increase the light yield studying separately the two scintillators: PVT and ZnS. A test bench has been built to fully characterize and improve the neutron detection with the ZnS using an AmBe source. To study the positron light yield on the PVT, we have built another test bench with a 207Bi source. We have improved the design of the cubes, their wrapping or the type and the configuration of the fibers. We managed to increase the PVT light yield by about 66 % and improve the resolution of the positron energy on the test bench from 21 % to 16 % at 1 MeV.

  15. 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.

  16. Perovskite solid solutions with multiferroic morphotropic phase boundaries and property enhancement

    Directory of Open Access Journals (Sweden)

    M. Algueró

    2016-06-01

    Full Text Available Recently, large phase-change magnetoelectric response has been anticipated by a first-principles investigation of phases in the BiFeO3–BiCoO3 perovskite binary system, associated with the existence of a discontinuous morphotropic phase boundary (MPB between multiferroic polymorphs of rhombohedral and tetragonal symmetries. This might be a general property of multiferroic phase instabilities, and a novel promising approach for room temperature magnetoelectricity. We review here our current investigations on the identification and study of additional material systems, alternative to BiFeO3–BiCoO3 that has only been obtained by high pressure synthesis. Three systems, whose phase diagrams were, in principle, liable to show multiferroic MPBs have been addressed: the BiMnO3–PbTiO3 and BiFeO3–PbTiO3 binary systems, and the BiFeO3–BiMnO3–PbTiO3 ternary one. A comprehensive study of multiferroism across different solid solutions was carried out based on electrical and magnetic characterizations, complemented with mechanical and electromechanical measurements. An in-depth structural analysis was also accomplished when necessary.

  17. A Convergent Solid-Phase Synthesis of Actinomycin Analogues - Towards Implementation of Double-Combinatorial Chemistry

    DEFF Research Database (Denmark)

    Tong, Glenn; Nielsen, John

    1996-01-01

    The actinomycin antibiotics bind to nucleic acids via both intercalation and hydrogen bonding. We found this 'double-action attack' mechanism very attractive in our search for a novel class of nucleic acid binders. A highly convergent, solid-phase synthetic strategy has been developed for a class...... with the requirements for combinatorial synthesis and furthermore, the final segment condensation allows, for the first time, double-combinatorial chemistry to be performed where two combinatorial libraries can be reacted with each other. Copyright (C) 1996 Elsevier Science Ltd....

  18. Highly Selective Liquid-Phase Benzylation of Anisole with Solid-Acid Zeolite Catalysts

    DEFF Research Database (Denmark)

    Poreddy, Raju; Shunmugavel, Saravanamurugan; Riisager, Anders

    2015-01-01

    Zeolites were evaluated as solid acid catalysts for the liquid-phase benzylation of anisole with benzyl alcohol, benzyl bromide, and benzyl chloride at 80 °C. Among the examined zeolites, H-mordenite-10 (H-MOR-10) demonstrated particular high activity (>99 %) and excellent selectivity (>96...... %) to the monobenzylated products, ortho/para benzyl anisole, using benzyl alcohol as reagent (anisole/alcohol molar ratio = 28). Analogous reactions with benzyl halides resulted in lower yields of the desired monobenzylated products. The conversion of benzyl alcohol was confirmed to be proportional to the amount of added...

  19. A rapid solid-phase radioimmunoassay for human plasma follicle-stimulating hormone

    International Nuclear Information System (INIS)

    Lovesey, A.C.

    1980-01-01

    The measurement of plasma levels of human follicle-stimulating hormone (FSH) has proved to be of value for the study of the hypothalamic-hypophyseal-gonadal axis, greatly facilitating the diagnosis and management of problems relating to the menopause and infertility. A solid-phase radioimmunoassay for human FSH has been developed. This system is characterised by high precision, is economical, and is considerably faster to operate than conventional double antibody systems used in the hospital assay service. Reference values for plasma FSH in various endocrine states are recorded and discussed. (author)

  20. A microplate adaptation of the solid-phase C1q immune complex assay

    International Nuclear Information System (INIS)

    Hunt, J.S.; Kennedy, M.P.; Barber, K.E.; McGiven, A.R.

    1980-01-01

    A method has been developed for the detection of C1q binding immune complexes in serum in which microculture plates are used as the solid-phase matrix for adsorption of C1q. This micromethod used only one-tenth of the amount of both C1q and [ 125 I]antihuman immunoglobulin per test and enabled 7 times as many samples to be tested in triplicate in comparison with the number performed in duplicate by the standard tube assay. (Auth.)

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

    OpenAIRE

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

    2010-01-01

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

  2. 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......Apoptotic induction mechanisms are of crucial importance for the general homeostasis of multicellular organisms. In cancer the apoptotic pathways are downregulated, which, at least partly, is due to an abundance of inhibitors of apoptosis proteins (IAPs) that block the apoptotic cascade...

  3. Determination of phenols in landfill leachate-contaminated groundwaters by solid-phase extraction

    DEFF Research Database (Denmark)

    Ask Reitzel, Lotte; Ledin, Anna

    2002-01-01

    A solid-phase extraction method for phenols in landfill leachates was developed and optimized in order to solve the expected and observed problems associated with an anaerobic matrix containing high concentrations of salts and organic matter. Isolute ENV1 cartridges exhibited the best retention...... be identified in leachates from three Danish landfills, ranging in concentration from 0.01 to 29 mg/ L, which is at the lower end of the concentration range usually found for phenols in landfill leachates (sub-mg/L to mg/L).  2002 Elsevier Science B.V. All rights reserved....

  4. Solid-Phase Immunoassay of Polystyrene-Encapsulated Semiconductor Coreshells for Cardiac Marker Detection

    Directory of Open Access Journals (Sweden)

    Sanghee Kim

    2012-01-01

    Full Text Available A solid-phase immunoassay of polystyrene-encapsulated semiconductor nanoparticles was demonstrated for cardiac troponin I (cTnI detection. CdSe/ZnS coreshells were encapsulated with a carboxyl-functionalized polystyrene nanoparticle to capture the target antibody through a covalent bonding and to eliminate the photoblinking and toxicity of semiconductor luminescent immunosensor. The polystyrene-encapsulated CdSe/ZnS fluorophores on surface-modified glass chip identified cTnI antigens at the level of ~ng/mL. It was an initial demonstration of diagnostic chip for monitoring a cardiovascular disease.

  5. Rapid and convenient semi-automated microwave-assisted solid-phase synthesis of arylopeptoids

    DEFF Research Database (Denmark)

    Rasmussen, Jakob Ewald; Boccia, Marcello Massimo; Nielsen, John

    2014-01-01

    A facile and expedient route to the synthesis of arylopeptoid oligomers (N-alkylated aminomethyl benz-amides) using semi-automated microwave-assisted solid-phase synthesis is presented. The synthesis was optimized for the incorporation of side chains derived from sterically hindered or unreactive...... amines and both ortho- and para-substituted arylo-backbones. By utilizing this optimized protocol a complex nonameric arylopeptoid was synthesized in less than 11 h, featuring a novel alternating ortho-, meta-, and para-substituted backbone pattern and a variety of chemically diverse and challenging side...

  6. Solid phase electron donors control denitrification in groundwater at agricultural sites

    Science.gov (United States)

    Green, C. T.; Liao, L.; Bekins, B. A.; Bohlke, J. K.

    2011-12-01

    Increased concentrations of nitrate in groundwater caused by agricultural use of chemical and organic fertilizers are a concern because of possible risks to environmental and human health. At many sites, these problems are mitigated by natural attenuation of nitrate as a result of microbially mediated denitrification of nitrate to nitrogen gas. Recent studies have clarified the factors affecting the rates and extents of denitrification in groundwater in agricultural areas. Intensive studies were conducted by the US Geological Survey to study agricultural chemicals in California, Nebraska, Washington, and Maryland using laboratory analyses, field measurements, and flow and transport modeling for monitoring well transects (0.5 to 2.5 km in length) and vertical profiles (0 to 50 m in depth). Groundwater analyses included major ion chemistry, dissolved gases, nitrogen and oxygen stable isotopes, and atmospheric age-tracers. Sediments were analyzed for concentrations of potential electron donors for denitrification, including reduced iron and sulfur, and organic carbon. Geochemical data and mass balance calculations indicated that solid-phase electron donors were an important factor controlling denitrification at these sites. To examine the generality of this result, a mathematical model of vertical flux of water, oxygen, and nitrate was developed and applied at these study sites along with 2 new study sites in Iowa and Mississippi and 8 additional sites from previous studies in Nebraska, Texas, Minnesota, Wisconsin, North Carolina, Maryland (2 sites), and New York. Model results confirmed the importance of solid phase electron donors. The normalized reaction rates on an electron flux basis tended to increase with depth from the shallow oxygen reduction zone to the underlying nitrate reduction zone. The pattern of higher rates at depth is consistent with a reaction rate controlled by solid phase donors that are depleted under oxidizing conditions near the surface and in

  7. Preparation of bioconjugates by solid-phase conjugation to ion exchange matrix-adsorbed carrier proteins

    DEFF Research Database (Denmark)

    Houen, G.; Olsen, D.T.; Hansen, P.R.

    2003-01-01

    of ovalbumin and various peptides were prepared in a similar manner and used for production of peptide antisera by direct immunization with the conjugates bound to the ion exchanger. Advantages of the method are its solid-phase nature, allowing fast and efficient reactions and intermediate washings......, and immunization experiments with the eluted conjugates showed that the more substituted conjugates gave rise to the highest titers of glutathione antibodies. Direct immunization with the conjugates adsorbed to the ion exchange matrix was possible and gave rise to high titers of glutathione antibodies. Conjugates...

  8. Sequential, solid-phase assay for biotin in physiologic fluids that correlates with expected biotin status

    International Nuclear Information System (INIS)

    Mock, D.M.; DuBois, D.B.

    1986-01-01

    Interest in accurate measurement of biotin concentrations in plasma and urine has been stimulated by recent advances in the understanding of biotin-responsive inborn errors of metabolism and by several reports describing acquired biotin deficiency during parenteral alimentation. This paper presents a biotin assay utilizing radiolabeled avidin in a sequential, solid-phase method; the assay has increased sensitivity compared to previous methods (greater than or equal to 10 fmol/tube), correlates with expected trends in biotin concentrations in blood and urine in a rat model of biotin deficiency, and can utilize commercially available radiolabeled avidin

  9. Interfacial Behavior of Fatty-Acylated Sericin Prepared by Lipase-Catalyzed Solid-Phase Synthesis

    OpenAIRE

    Ogino, Masato; Tanaka, Rie; 服部, 誠; Yoshida, Tadashi; 横手, よし子; 高橋, 幸資

    2006-01-01

    Fatty-acylated sericin {1:0.7 molar ratio of sericin (Mr 18,700) to oleic acid} was prepared by lipase-catalyzed solid-phase synthesis in n-hexane containing oleic acid to endow sericin with interfacial properties. Acylation with oleic acid was confirmed by 1H-NMR. The fatty-acylated sericin exhibited superior emulsifying activity index and emulsion stability in the presence of 0?0.5 M NaCl, in a temperature range of 30?80 °C and pH range of 2?7, as compared with the control sericin. The fatt...

  10. Solid Phase Characterization of Tank 241-AY-102 Annulus Space Particulate

    Energy Technology Data Exchange (ETDEWEB)

    Cooke, G. A.

    2013-01-30

    The Special Analytical Studies Group at the 222-S Laboratory (222-S) examined the particulate recovered from a series of samples from the annular space of tank 241-AY-102 (AY-102) using solid phase characterization (SPC) methods. These include scanning electron microscopy (SEM) using the ASPEX®1 scanning electron microscope, X-ray diffraction (XRD) using the Rigaku®2 MiniFlex X-ray diffractometer, and polarized light microscopy (PLM) using the Nikon®3 Eclipse Pol optical microscope. The SEM is equipped with an energy dispersive X-ray spectrometer (EDS) to provide chemical information.

  11. Solid Phase Characterization of Tank 241-AY-102 Annulus Space Particulate

    International Nuclear Information System (INIS)

    Cooke, G. A.

    2013-01-01

    The Special Analytical Studies Group at the 222-S Laboratory (222-S) examined the particulate recovered from a series of samples from the annular space of tank 241-AY-102 (AY-102) using solid phase characterization (SPC) methods. These include scanning electron microscopy (SEM) using the ASPEX(R)1 scanning electron microscope, X-ray diffraction (XRD) using the Rigaku(R)2 MiniFlex X-ray diffractometer, and polarized light microscopy (PLM) using the Nikon(R)3 Eclipse Pol optical microscope. The SEM is equipped with an energy dispersive X-ray spectrometer (EDS) to provide chemical information

  12. Evaluation of a Solid Phase DNA Binding Matrix for Downstream PCR Analysis

    Science.gov (United States)

    2005-12-01

    caus6s par les UV et pour inactiver rapidement des organismes emp~chant ainsi la croissance des bactdries et autres organismes dont les pathog~nes A...Defence Research and Recherche et d6veloppement Development Canada pour la defense Canada DEFENCE DEFENSE Evaluation of a Solid Phase DNA Binding...Document Revie,... 4 el © Her Majesty the Queen as represented by the Minister of National Defence, 2005 © Sa majestW la reine, repr~sent~e par le

  13. ZnO nanorod array solid phase micro-extraction fiber coating: fabrication and extraction capability

    International Nuclear Information System (INIS)

    Wang Dan; Zhang Zhuomin; Li Tiemei; Zhang Lan; Chen Guonan; Luo Lin

    2009-01-01

    In this paper, a ZnO nanorod array has been introduced as a coating to the headspace solid phase micro-extraction (HSSPME) field. The coating shows good extraction capability for volatile organic compounds (VOCs) by use of BTEX as a standard and can be considered suitable for sampling trace and small molecular VOC targets. In comparison with the randomly oriented ZnO nanorod HSSPME coating, ZnO nanorod array HSSPME fiber coating shows better extraction capability, which is attributed to the nanorod array structure of the coating. Also, this novel nanorod array coating shows good extraction selectivity to 1-propanethiol.

  14. Radiation effects in silicate glasses

    International Nuclear Information System (INIS)

    Bibler, N.E.; Howitt, D.G.

    1988-01-01

    The study of radiation effects in complex silicate glasses has received renewed attention because of their use in special applications such as high level nuclear waste immobilization and fiber optics. Radiation changes the properties of these glasses by altering their electronic and atomic configurations. These alterations or defects may cause dilatations or microscopic phase changes along with absorption centers that limit the optical application of the glasses. Atomic displacements induced in the already disordered structure of the glasses may affect their use where heavy irradiating particles such as alpha particles, alpha recoils, fission fragments, or accelerated ions are present. Large changes (up to 1%) in density may result. In some cases the radiation damage may be severe enough to affect the durability of the glass in aqueous solutions. In the paper, the authors review the literature concerning radiation effects on density, durability, stored energy, microstructure and optical properties of silicate glasses. Both simple glasses and complex glasses used for immobilization of nuclear waste are considered

  15. Extension of Toth function from gas-solid to liquid-solid equilibria and application to reversed-phase liquid chromatography systems

    Energy Technology Data Exchange (ETDEWEB)

    Gritti, Fabrice [University of Tennessee, Knoxville (UTK); Guiochon, Georges A [ORNL

    2006-03-01

    The extension of the {Psi} function developed by Toth from equilibria taking place at gas-solid interfaces to those taking place at liquid-solid interfaces was investigated. The results were applied to conventional liquid-solid systems used in reversed-phase liquid chromatography (RPLC). The adsorbents in these systems are made of porous silica having a hydrophobic solid surface obtained by chemically bonding C{sub 18} alkyl chains to a porous silica gel then endcapping the surface with trimethylsilyl groups. The liquid is an aqueous solution of an organic solvent, most often methanol or acetonitrile. The probe compound used here is phenol. Adsorption data of phenol were measured using the dynamic frontal analysis (FA) method. The excess adsorption of the organic solvent was measured using the minor disturbance (MD) method. Activity coefficients in the bulk were estimated through the UNIFAC group contributions. The results show that the {Psi} function predicts 90% of the total free energy of immersion, {Delta}F, of the solid when the concentration of phenol is moderate (typically less than 10 g/L). At higher concentrations, the nonideal behavior of the bulk liquid phase becomes significant and it may contribute up to about 30% of {Delta}F. The high concentration of adsorbed molecules of phenol at the interface decreases the interfacial tension, {sigma}, by about 18 mN/m, independently of the structure of the adsorbed phase and of the nature of the organic solvent.

  16. Extension of Tóth Psi function from gas-solid to liquid-solid equilibria and application to reversed-phase liquid chromatography systems.

    Science.gov (United States)

    Gritti, Fabrice; Guiochon, Georges

    2006-07-01

    The extension of the Psi function developed by Tóth from equilibria taking place at gas-solid interfaces to those taking place at liquid-solid interfaces was investigated. The results were applied to conventional liquid-solid systems used in reversed-phase liquid chromatography (RPLC). The adsorbents in these systems are made of porous silica having a hydrophobic solid surface obtained by chemically bonding C(18) alkyl chains to a porous silica gel then endcapping the surface with trimethylsilyl groups. The liquid is an aqueous solution of an organic solvent, most often methanol or acetonitrile. The probe compound used here is phenol. Adsorption data of phenol were measured using the dynamic frontal analysis (FA) method. The excess adsorption of the organic solvent was measured using the minor disturbance (MD) method. Activity coefficients in the bulk were estimated through the UNIFAC group contributions. The results show that the Psi function predicts 90% of the total free energy of immersion, DeltaF, of the solid when the concentration of phenol is moderate (typically less than 10 g/L). At higher concentrations, the nonideal behavior of the bulk liquid phase becomes significant and it may contribute up to about 30% of DeltaF. The high concentration of adsorbed molecules of phenol at the interface decreases the interfacial tension, sigma, by about 18 mN/m, independently of the structure of the adsorbed phase and of the nature of the organic solvent.

  17. PHYSICOCHEMICAL PROPERTIES OF THE SOLID COMPONENT OF WELDING AEROSOL. I. PHASE COMPOSITION

    Directory of Open Access Journals (Sweden)

    T. L. Rakitskaya

    2015-02-01

    Full Text Available The phase composition of the solid component of welding aerosol (SCWA obtained as a result of metal welding with electrodes of ANO-4 and TsL-11 types manufactured according to ISO 2560 E432R 21 and ISO E19.9NbB20 standards, respectively, and differing in com-position of their wires and coatings was determined with the help of a Siemens D500 diffrac- a Siemens D500 diffrac-tometer supplied with the manufacturer’s software. Four and thirteen phases were identified in SCWA-ANO-4 and SCWA-TsL-11, respectively. Evaluation of crystallite sizes by the use of the Scherer equation showed that the crystallites formed in the course of welding with a TsL-11 type electrode are larger than those in the case of an ANO-4 type one: 65-89 nm and 30-49 nm, respectively.

  18. "Reagentless" flow injection determination of ammonia and urea using membrane separation and solid phase basification

    Science.gov (United States)

    Akse, J. R.; Thompson, J. O.; Sauer, R. L.; Atwater, J. E.

    1998-01-01

    Flow injection analysis instrumentation and methodology for the determination of ammonia and ammonium ions in an aqueous solution are described. Using in-line solid phase basification beds containing crystalline media. the speciation of ammoniacal nitrogen is shifted toward the un-ionized form. which diffuses in the gas phase across a hydrophobic microporous hollow fiber membrane into a pure-water-containing analytical stream. The two streams flow in a countercurrent configuration on opposite sides of the membrane. The neutral pH of the analytical stream promotes the formation of ammonium cations, which are detected using specific conductance. The methodology provides a lower limit of detection of 10 microgram/L and a dynamic concentration range spanning three orders of magnitude using a 315-microliters sample injection volume. Using immobilized urease to enzymatically promote the hydrolysis of urea to produce ammonia and carbon dioxide, the technique has been extended to the determination of urea.

  19. Fabrication of tungsten composite parts by direct HIP of powders in solid phase

    International Nuclear Information System (INIS)

    Mandet, F.; Palacio, M.; Boncoeur, M.

    1985-01-01

    Tungsten composites of the type W = 95%, Ni = 3.5% Fe = 1.5%, which are usually produced by cold isostatic pressing (CIP) followed by liquid phase natural sintering, are obtained here by direct hot isostatic pressing (HIP) of powders in solid phase. This method which is more reliable than the traditional process allows the production of large-sized parts while considerably reducing the required quantity of powder. The product fabrication by HIP is described as well as the results of the final material's character. Although the density of the product is similar to that of the commercial product, the mechanical properties in traction, and especially elongation, are weaker. Several hypotheses are suggested to explain this fall in ductility

  20. Evaluation of a solid phase R.I.A. technique and solid phase E.L.I.S.A. technique for the demonstration of hepatitis B surface antigen

    International Nuclear Information System (INIS)

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

    1977-01-01

    We compared the sensitivity of a solidphase radio-immunoassay (R.I.A.), a solid-phase enzyme-immunoassay (E.L.I.S.A.) and a hemagglutination test (R.P.H.A.) for the detection of the HBs Ag in two ways: 1) by screening a panel of 300 sera (97 positives and 203 negatives) 2) by titrating serial dilutions of 10 positive sera. Ninety seven sera were positive by R.I.A., 95% were detected by E.L.I.S.A. and 81% were detected by R.P.H.A. In the serial dilutions the average end points of the titration were for R.I.A. 0.005 ng/ml, for E.L.I.S.A. 0,01 ng/ml and for R.P.H.A. 0.04 ng/ml. It can be concluded that the sensitivity of the E.L.I.S.A. test is intermediate between the sensitivity of the R.I.A. and the sensitivity of the R.P.H.A. The E.L.I.S.A. and the R.P.H.A. tests seam to be a little more sensitive for the detection of subtype ay than the detection of subtype ad. (orig.) [de

  1. Effect of Magnetic Hysteresis of the Solid Phase on the Rheological Properties of Mr Fluids

    Science.gov (United States)

    de Vicente, J.; Durán, J. D. G.; Delgado, A. V.; González-Caballero, F.; Bossis, G.

    An experimental investigation is described concerning the effect of the existence of a remanent magnetization of the dispersed particles on the rheological properties of magnetorheological fluids (MRF). Two MRF's were used: (1) solid phase: cobalt ferrite particles + silica gel (1.5% w/w) liquid phase: silicone oil (viscosity 20 mPa.s) and (2) solid phase: carbonyl iron + silica gel; liquid phase; silicone oil. The cobalt ferrite particles were synthetized as monodisperse colloidal spheres with an average diameter of 850 nm. The dependence of the dimensionless shear stress (τ*/φ) vs. Mason number (Mn) fails to scale when a ``magnetorheological hysteresis procedure'' is followed, specially for the higher volume fractions used (~ 7.5%). The yield stress (τy) is first estimated from successive rheograms obtained decreasing the external field (H0) values for different φ. A more precise determination can be done by applying a stress ramp in the oscillatory regime. The critical stress amplitude (τc) needed to exceed the viscoelastic linear region (VLR) is obtained. It is found that both τy and τc strongly depend on the magnetic history of the sample. As expected, the previous results were not obtained in a classical MRF of carbonyl iron particles since they do not present magnetic hysteresis. We conclude that cobalt ferrite suspensions are an other kind of MRF which works at low fields (0 - 17.8 kA/m) with the opposite effect: decrease of the yield stress with the field. This property can be improved using particles with stronger remanent magnetization.

  2. The hydrolytic stage in high solids temperature phased anaerobic digestion improves the downstream methane production rate.

    Science.gov (United States)

    Buffière, P; Dooms, M; Hattou, S; Benbelkacem, H

    2018-07-01

    The role of the hydrolytic stage in high solids temperature phased anaerobic digestion was investigated with a mixture of cattle slurry and maize silage with variable ratios (100, 70 and 30% volatile solids coming from cattle slurry). It was incubated for 48 h at 37, 55, 65 and 72 °C. Soluble chemical oxygen demand and biochemical methane potential were measured at 0, 24 and 48 h. Higher temperatures improved the amount of solubilized COD, which confirmed previously reported results. Nevertheless, solubilization mostly took place during the first 24 h. The rate of methane production in post-hydrolysis BMPs increased after 48 h hydrolysis time, but not after 24 h. The first order kinetic constant rose by 40% on average. No correlation was observed between soluble COD and downstream methane production rate, indicating a possible modification of the physical structure of the particulate solids during the hydrolytic stage. Copyright © 2018 Elsevier Ltd. All rights reserved.

  3. Hydrodynamic and thermal modeling of solid particles in a multi-phase, multi-component flow

    International Nuclear Information System (INIS)

    Tentner, A.M.; Wider, H.U.

    1983-01-01

    This paper presents the new thermal hydraulic models describing the hydrodynamics of the solid fuel/steel chunks during an LMFBR hypothetical core-disruptive accident. These models, which account for two-way coupling between the solid and fluid phases, describe the mass, momentum, and energy exchanges which occur when the chunks are present at any axial location. They have been incorporated in LEVITATE, a code for the analysis of fuel and cladding dynamics under Loss-of-Flow (LOF) conditions. Their influence on fuel motion is presented in the context of the L6 TREAT experiment analysis. It is shown that the overall hydrodynamic behavior of the molten fuel and solid-fuel chunks is dependent on both the size of the chunks and the power level. At low and intermediate power levels the fuel motion is more dispersive when small chunks, rather than large ones, are present. At high power levels the situation is reversed. These effects are explained in detail

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

    Science.gov (United States)

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

    2005-03-01

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

  5. Interfacial phase formation of Al-Cu bimetal by solid-liquid casting method

    Directory of Open Access Journals (Sweden)

    Ying Fu

    2017-05-01

    Full Text Available The solid-liquid method was used to prepare the continuous casting of copper cladding aluminium by liquid aluminum alloy and solid copper, and the interfacial phase formation of Al-Cu bimetal at different pouring temperatures (700, 750, 800 oC was investigated by means of metallograph, scanning electron microscopy (SEM and energy dispersive spectrometry (EDS methods. The results showed that the pouring temperature of aluminum melt had an important influence on the element diffusion of Cu from the solid Cu to Al alloy melt and the reactions between Al and Cu, as well as the morphology of the Al-Cu interface. When the pouring temperature was 800 oC, there were abundant Al-Cu intermetallic compounds (IMCs near the interface. However, a lower pouring temperature (700 oC resulted in the formation of cavities which was detrimental to the bonding and mechanical properties. Under the conditions in this study, the good metallurgical bonding of Al-Cu was achieved at a pouring temperature of 750 oC.

  6. Applications of monolithic solid-phase extraction in chromatography-based clinical chemistry assays.

    Science.gov (United States)

    Bunch, Dustin R; Wang, Sihe

    2013-04-01

    Complex matrices, for example urine, serum, plasma, and whole blood, which are common in clinical chemistry testing, contain many non-analyte compounds that can interfere with either detection or in-source ionization in chromatography-based assays. To overcome this problem, analytes are extracted by protein precipitation, solid-phase extraction (SPE), and liquid-liquid extraction. With correct chemistry and well controlled material SPE may furnish clean specimens with consistent performance. Traditionally, SPE has been performed with particle-based adsorbents, but monolithic SPE is attracting increasing interest of clinical laboratories. Monoliths, solid pieces of stationary phase, have bimodal structures consisting of macropores, which enable passage of solvent, and mesopores, in which analytes are separated. This structure results in low back-pressure with separation capabilities similar to those of particle-based adsorbents. Monoliths also enable increased sample throughput, reduced solvent use, varied support formats, and/or automation. However, many of these monoliths are not commercially available. In this review, application of monoliths to purification of samples from humans before chromatography-based assays will be critically reviewed.

  7. Solid-Phase Synthesis of Molecularly Imprinted Polymer Nanoparticles with a Reusable Template - "Plastic Antibodies".

    Science.gov (United States)

    Poma, Alessandro; Guerreiro, Antonio; Whitcombe, Michael J; Piletska, Elena V; Turner, Anthony P F; Piletsky, Sergey A

    2013-06-13

    Molecularly Imprinted Polymers (MIPs) are generic alternatives to antibodies in sensors, diagnostics and separations. To displace biomolecules without radical changes in infrastructure in device manufacture, MIPs should share their characteristics (solubility, size, specificity and affinity, localized binding domain) whilst maintaining the advantages of MIPs (low-cost, short development time and high stability) hence the interest in MIP nanoparticles. Herein we report a reusable solid-phase template approach (fully compatible with automation) for the synthesis of MIP nanoparticles and their precise manufacture using a prototype automated UV photochemical reactor. Batches of nanoparticles (30-400 nm) with narrow size distributions imprinted with: melamine (d = 60 nm, K d = 6.3 × 10 -8 m), vancomycin (d = 250 nm, K d = 3.4 × 10 -9 m), a peptide (d = 350 nm, K d = 4.8 × 10 -8 m) and proteins have been produced. Our instrument uses a column packed with glass beads, bearing the template. Process parameters are under computer control, requiring minimal manual intervention. For the first time we demonstrate the reliable re-use of molecular templates in the synthesis of MIPs (≥ 30 batches of nanoMIPs without loss of performance). NanoMIPs are produced template-free and the solid-phase acts both as template and affinity separation medium.

  8. Development of andrographolide molecularly imprinted polymer for solid-phase extraction

    Science.gov (United States)

    Yin, Xiaoying; Liu, Qingshan; Jiang, Yifan; Luo, Yongming

    2011-06-01

    A method employing molecularly imprinted polymer (MIP) as selective sorbent for solid-phase extraction (SPE) to pretreat samples was developed. The polymers were prepared by precipitation polymerization with andrographolide as template molecule. The structure of MIP was characterized and its static adsorption capacity was measured by the Scatchard equation. In comparison with C 18-SPE and non-imprinted polymer (NIP) SPE column, MIP-SPE column displays high selectivity and good affinity for andrographolide and dehydroandrographolide for extract of herb Andrographis paniculata ( Burm.f.) Nees (APN). MIP-SPE column capacity was 11.9 ± 0.6 μmol/g and 12.1 ± 0.5 μmol/g for andrographolide and dehydroandrographolide, respectively and was 2-3 times higher than that of other two columns. The precision and accuracy of the method developed were satisfactory with recoveries between 96.4% and 103.8% (RSD 3.1-4.3%, n = 5) and 96.0% and 104.2% (RSD 2.9-3.7%, n = 5) for andrographolide and dehydroandrographolide, respectively. Various real samples were employed to confirm the feasibility of method. This developed method demonstrates the potential of molecularly imprinted solid phase extraction for rapid, selective, and effective sample pretreatment.

  9. Zinc oxide crystal whiskers as a novel sorbent for solid-phase extraction of flavonoids.

    Science.gov (United States)

    Wang, Licheng; Shangguan, Yangnan; Hou, Xiudan; Jia, Yong; Liu, Shujuan; Sun, Yingxin; Guo, Yong

    2017-08-15

    As a novel solid-phase extraction material, zinc oxide crystal whiskers were used to extract flavonoid compounds and showed good extraction abilities. X-ray diffraction, scanning electron microscopy with energy dispersive X-ray spectroscopy and surface area/pore volume characterized the sorbent. The zinc oxide was packed into a solid-phase extraction micro-column and its extraction ability was evaluated by four model flavonoid compounds. The sample loading and elution parameters were optimized and the zinc oxide based analytical method for flavonoids was established. It showed that the method has wide linearities from 1 to 150μg/L and low limits of detection at 0.25μg/L. The relative standard deviations of a single column repeatability and column to column reproducibility were less than 6.8% and 10.6%. Several real samples were analyzed by the established method and satisfactory results were obtained. The interactions between flavonoids and zinc oxide were calculated and proved to be from the Van der Waals' forces between the 4p and 5d orbitals from zinc atom and the neighboring π orbitals from flavonoid phenyl groups. Moreover, the zinc oxide crystal whiskers showed good stability and could be reused more than 50 times under the operation conditions. This work proves that the zinc oxide crystal whiskers are a good candidate for flavonoids enrichment. Copyright © 2017. Published by Elsevier B.V.

  10. Solid-phase extraction microfluidic devices for matrix removal in trace element assay of actinide materials.

    Science.gov (United States)

    Gao, Jun; Manard, Benjamin T; Castro, Alonso; Montoya, Dennis P; Xu, Ning; Chamberlin, Rebecca M

    2017-05-15

    Advances in sample nebulization and injection technology have significantly reduced the volume of solution required for trace impurity analysis in plutonium and uranium materials. Correspondingly, we have designed and tested a novel chip-based microfluidic platform, containing a 100-µL or 20-µL solid-phase microextraction column, packed by centrifugation, which supports nuclear material mass and solution volume reductions of 90% or more compared to standard methods. Quantitative recovery of 28 trace elements in uranium was demonstrated using a UTEVA chromatographic resin column, and trace element recovery from thorium (a surrogate for plutonium) was similarly demonstrated using anion exchange resin AG MP-1. Of nine materials tested, compatibility of polyvinyl chloride (PVC), polypropylene (PP), and polytetrafluoroethylene (PTFE) chips with the strong nitric acid media was highest. The microcolumns can be incorporated into a variety of devices and systems, and can be loaded with other solid-phase resins for trace element assay in high-purity metals. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Magnetic nanoparticle based solid-phase extraction of heavy metal ions: A review on recent advances.

    Science.gov (United States)

    Hemmati, Maryam; Rajabi, Maryam; Asghari, Alireza

    2018-02-06

    This review (with 151 refs) focuses on recent progress that has been made in magnetic nanoparticle-based solid phase extraction (SPE), pre-concentration and speciation of heavy metal ions. In addition, it discusses applications to complex real samples such as environmental, food, and biological matrices. The introduction addresses current obstacles and limitations associated with established SPE approaches and discusses the present state of the art in different formats of off-line and on-line SPE. The next section covers magnetized inorganic nanomaterials for use in SPE, with subsections on magnetic silica, magnetic alumina and titania, and on magnetic layered double oxides. A further section treats magnetized carbonaceous nanomaterials for use in SPE, with subsections on magnetic graphene and/or graphene oxides, magnetic carbon nanotubes and magnetic carbon nitrides. We then discuss the progress made in SPE based on the use of magnetized organic polymers (mainly non-imprinted and ion-imprinted polymer). This is followed by shorter sections on the use of magnetized metal organic frameworks, magnetized ionic liquids and magnetized biosorbents. All sections include discussions of the nanomaterials in terms of selectivity, sorption capacity, mechanisms of sorption and common routes for material synthesis. A concluding section addresses actual challenges and discusses perspective routes towards further improvements. Graphical abstract An overview on booster nanomaterials (ionic liquids, inorganic, organic and biological materials, and metal-organic frameworks) for use in magnetic nanoparticle-based solid-phase extraction of heavy metal ions.

  12. Comparison of fluorescence microscopy and solid-phase cytometry methods for counting bacteria in water

    Science.gov (United States)

    Lisle, John T.; Hamilton, Martin A.; Willse, Alan R.; McFeters, Gordon A.

    2004-01-01

    Total direct counts of bacterial abundance are central in assessing the biomass and bacteriological quality of water in ecological and industrial applications. Several factors have been identified that contribute to the variability in bacterial abundance counts when using fluorescent microscopy, the most significant of which is retaining an adequate number of cells per filter to ensure an acceptable level of statistical confidence in the resulting data. Previous studies that have assessed the components of total-direct-count methods that contribute to this variance have attempted to maintain a bacterial cell abundance value per filter of approximately 106 cells filter-1. In this study we have established the lower limit for the number of bacterial cells per filter at which the statistical reliability of the abundance estimate is no longer acceptable. Our results indicate that when the numbers of bacterial cells per filter were progressively reduced below 105, the microscopic methods increasingly overestimated the true bacterial abundance (range, 15.0 to 99.3%). The solid-phase cytometer only slightly overestimated the true bacterial abundances and was more consistent over the same range of bacterial abundances per filter (range, 8.9 to 12.5%). The solid-phase cytometer method for conducting total direct counts of bacteria was less biased and performed significantly better than any of the microscope methods. It was also found that microscopic count data from counting 5 fields on three separate filters were statistically equivalent to data from counting 20 fields on a single filter.

  13. A star-shaped polythiophene dendrimer coating for solid-phase microextraction of triazole agrochemicals.

    Science.gov (United States)

    Abolghasemi, Mir Mahdi; Habibiyan, Rahim; Jaymand, Mehdi; Piryaei, Marzieh

    2018-02-14

    A nanostructured star-shaped polythiophene dendrimer was prepared and used as a fiber coating for headspace solid phase microextraction of selected triazolic pesticides (tebuconazole, hexaconazole, penconazole, diniconazole, difenoconazole, triticonazole) from water samples. The dendrimer with its large surface area was characterized by thermogravimetric analysis, UV-Vis spectroscopy and field emission scanning electron microscopy. It was placed on a stainless steel wire for use in SPME. The experimental conditions for fiber coating, extraction, stirring rate, ionic strength, pH value, desorption temperature and time were optimized. Following thermal desorption, the pesticides were quantified by GC-MS. Under optimum conditions, the repeatability (RSD) for one fiber (for n = 3) ranges from 4.3 to 5.6%. The detection limits are between 8 and 12 pg mL -1 . The method is fast, inexpensive (in terms of equipment), and the fiber has high thermal stability. Graphical abstract Schematic presentation of a nanostructured star-shaped polythiophene dendrimer for use in headspace solid phase microextraction of the triazolic pesticides (tebuconazole, hexaconazole, penconazole, diniconazole, difenoconazole, triticonazole). They were then quantified by gas chromatography-mass spectrometry.

  14. Isolation of genomic DNA using magnetic nanoparticles as a solid-phase support

    Energy Technology Data Exchange (ETDEWEB)

    Saiyed, Z M; Ramchand, C N [Kemin Nutritional Technologies (India) Pvt Ltd, Trapezium, Nelson Manickam Road, Chennai 600 029 (India); Telang, S D [Department of Biochemistry, Faculty of Science, M S University of Baroda, Sayajigunj, Vadodara 390 002 (India)], E-mail: cnramchand@yahoo.com, E-mail: ramchand.cn@kemin.com

    2008-05-21

    In recent years, techniques employing magnetizable solid-phase supports (MSPS) have found application in numerous biological fields. This magnetic separation procedure offers several advantages in terms of subjecting the analyte to very little mechanical stress compared to other methods. Secondly, these methods are non-laborious, cheap, and often highly scalable. The current paper details a genomic DNA isolation method optimized in our laboratory using magnetic nanoparticles as a solid-phase support. The quality and yields of the isolated DNA from all the samples using magnetic nanoparticles were higher or equivalent to the traditional DNA extraction procedures. Additionally, the magnetic method takes less than 15 min to extract polymerase chain reaction (PCR) ready genomic DNA as against several hours taken by traditional phenol-chloroform extraction protocols. Moreover, the isolated DNA was found to be compatible in PCR amplification and restriction endonuclease digestion. The developed procedure is quick, inexpensive, robust, and it does not require the use of organic solvents or sophisticated instruments, which makes it more amenable to automation and miniaturization.

  15. Isolation of genomic DNA using magnetic nanoparticles as a solid-phase support

    Science.gov (United States)

    Saiyed, Z. M.; Ramchand, C. N.; Telang, S. D.

    2008-05-01

    In recent years, techniques employing magnetizable solid-phase supports (MSPS) have found application in numerous biological fields. This magnetic separation procedure offers several advantages in terms of subjecting the analyte to very little mechanical stress compared to other methods. Secondly, these methods are non-laborious, cheap, and often highly scalable. The current paper details a genomic DNA isolation method optimized in our laboratory using magnetic nanoparticles as a solid-phase support. The quality and yields of the isolated DNA from all the samples using magnetic nanoparticles were higher or equivalent to the traditional DNA extraction procedures. Additionally, the magnetic method takes less than 15 min to extract polymerase chain reaction (PCR) ready genomic DNA as against several hours taken by traditional phenol-chloroform extraction protocols. Moreover, the isolated DNA was found to be compatible in PCR amplification and restriction endonuclease digestion. The developed procedure is quick, inexpensive, robust, and it does not require the use of organic solvents or sophisticated instruments, which makes it more amenable to automation and miniaturization.

  16. Isolation and analysis of sugar nucleotides using solid phase extraction and fluorophore assisted carbohydrate electrophoresis.

    Science.gov (United States)

    Barnes, Jarrod; Tian, Liping; Loftis, Jacqueline; Hiznay, James; Comhair, Suzy; Lauer, Mark; Dweik, Raed

    2016-01-01

    The building blocks of simple and complex oligosaccharides, termed sugar nucleotides, are often overlooked for their role in metabolic diseases and may hold the key to the underlying disease pathogenesis. Multiple reasons may account for the lack of analysis and quantitation of these sugar nucleotides, including the difficulty in isolation and purification as well as the required expensive instrumentation such as a high performance liquid chromatography (HPLC), mass spectrometer, or capillary electrophoresis. We have established a simple yet effective way to purify and quantitate sugar nucleotides using solid phase extraction (SPE) chromatography combined with fluorophore assisted carbohydrate electrophoresis (FACE). The simplicity of use, combined with the ability to run multiple samples at one time, give this technique a distinct advantage over the established methods for isolation and analysis of sugar nucleotides from cell culture models. •Sugar nucleotides can be easily purified with solid phase extraction chromatography.•FACE can be used to analyze multiple nucleotide sugar extracts with a single run.•The proposed method is simple, affordable, and uses common everyday research labware.

  17. Silicon carbide nanomaterial as a coating for solid-phase microextraction.

    Science.gov (United States)

    Tian, Yu; Feng, Juanjuan; Wang, Xiuqin; Sun, Min; Luo, Chuannan

    2018-01-26

    Silicon carbide has excellent properties, such as corrosion resistance, high strength, oxidation resistance, high temperature, and so on. Based on these properties, silicon carbide was coated on stainless-steel wire and used as a solid-phase microextraction coating, and polycyclic aromatic hydrocarbons were employed as model analytes. Using gas chromatography, some important factors that affect the extraction efficiency were optimized one by one, and an analytical method was established. The analytical method showed wide linear ranges (0.1-30, 0.03-30, and 0.01-30 μg/L) with satisfactory correlation coefficients (0.9922-0.9966) and low detection limits (0.003-0.03 μg/L). To investigate the practical application of the method, rainwater and cigarette ash aqueous solution were collected as real samples for extraction and detection. The results indicate that silicon carbide has excellent application in the field of solid-phase microextraction. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. The effect of residual chlorides on resultant properties of solid and liquid phases after carbonization process

    Energy Technology Data Exchange (ETDEWEB)

    Plevova Eva; Sugarkova Vera; Kaloc Miroslav [Institute of Geonics ASCR, Ostrava (Czech Republic). Laboratory of Petrology

    2004-07-01

    The low-concentration condition was employed to model the carbonisation mode for local (Czech Republic) coals with higher concentrations of some metals. After completing the carbonisation, mass balance calculations were performed. Results show that the presence of zinc dichloride, copper dichloride and sodium chloride caused the most pronounced impediment to the formation of tar in contrast to lead dichloride and aluminium chloride that increased tar. The results demonstrated that adding of chloride agents effect both the course of the coking process and the properties of solid and liquid products of coking. Evaluation of the solid phase showed that chloride addition caused a decrease of the caking and swelling value, which corresponds with measurements of plasticity values that are of significant influence on mechanical properties closely related to coking plant processes. Evaluation of the liquid phase pointed towards an increase of aromatic hydrocarbons and their derivatives (especially phenanthrene, fluoranthene, acenaphthylene, pyrene) but a decrease of naphthalene and methylnaphthalene. Chloride addition increased aromaticity and caused a difference in substitution rate at aromatic nucleus. Mesophase estimation indicated extensive mosaic, domain and laminated anisotropic texture occurrence after chloride addition, mainly NaCl and CuCl{sub 2} addition. A more detailed evaluation including detailed screening, TGA, IR and RTG analysis will be subject of further investigation. 4 refs., 2 figs., 5 tabs.

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

    KAUST Repository

    Zia, Asif I.

    2016-03-30

    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-phase extraction (MISPE) polymer. The polymers were functionalized on an interdigital capacitive sensor for selective binding of phthalate molecules from a complex mixture of chemicals. Both polymers owned predetermined selectivity by formation of valuable molecular recognition sites for Bis (2-ethylhexyl) phthalate (DEHP). Polymers were immobilized on planar electrochemical sensor fabricated on a single crystal silicon substrate with 500 nm sputtered gold electrodes fabricated using MEMS fabrication techniques. Impedance spectra were obtained using electrochemical impedance spectroscopy (EIS) to determine sample conductance for evaluation of phthalate concentration in the spiked sample solutions with various phthalate concentrations. Experimental results revealed that the ability of SPME polymer to adsorb target molecules on the sensing surface is better than that of MISPE polymer for phthalates in the sensing system. Testing the extracted samples using high performance liquid chromatography with photodiode array detectors validated the results.

  20. Solid phase extraction of uranium from phosphoric acid. Kinetic and thermodynamic study

    Energy Technology Data Exchange (ETDEWEB)

    Abdel-Magied, Ahmed Fawzy [Nuclear Materials Authority, Cairo (Egypt); Stockholm Univ. (Sweden). Dept. of Organic Chemistry

    2017-07-01

    There is a high interest to develop suitable solid phase extractants for uranium separation from aqueous solutions in order to reduce cost and enhance the efficiency. This paper describes solid phase extraction of uranium(VI) from aqueous phosphoric acid solution using MCM-41 based D2HEPA-TOPO organophosphorous extractants. The mixture of D2HEPA (di-2-ethyl-hexylphosphoric acid) and TOPO (tri-n-octylphosphine oxide) was impregnated into the pores of MCM-41 and the synthesized sorbent was fully characterized. The influences of different factors such as synergistic mixture ratio, phosphoric acid concentration, mixing time and temperature were investigated. The results showed that 90% of uranium(VI) extraction can be achieved within 5 min, using D2HEPA-TOPO rate at MCM-41 (mass ratio 2:1 w/w) from 1 M phosphoric acid containing 64 ppm of uranium at room temperature. High adsorption capacity of uranium(VI) have been achieved at the mentioned conditions. The rate constant for the chemical adsorption of uranium(VI) was 0.988 g mg{sup -1} min{sup -1} calculated by the pseudo-second order rate equation. The obtained thermodynamics parameters showed that uranium(VI) adsorption from H{sub 3}PO{sub 4} is an exothermic and spontaneous process.

  1. Chemically bonded carbon nanotubes on modified gold substrate as novel unbreakable solid phase microextraction fiber

    International Nuclear Information System (INIS)

    Bagheri, H.; Ayazi, Z.; Sistani, H.

    2011-01-01

    A new technique is introduced for preparation of an unbreakable fiber using gold wire as a substrate for solid phase microextraction (SPME). A gold wire is used as a solid support, onto which a first film is deposited that consists of a two-dimensional polymer obtained by hydrolysis of a self-assembled monolayer of 3-(trimethoxysilyl)-1-propanthiol. This first film is covered with a layer of 3-(triethoxysilyl)-propylamine. Next, a stationary phase of oxidized multi-walled carbon nanotubes was chemically bound to the surface. The synthetic strategy was verified by Fourier transform infrared spectroscopy and scanning electron microscopy. Thermal stability of new fiber was examined by thermogravimetric analysis. The applicability of the novel coating was verified by its employment as a SPME fiber for isolation of diazinon and fenthion, as model compounds. Parameters influencing the extraction process were optimized to result in limits of detection as low as 0.2 ng mL -1 for diazinon, and 0.3 ng mL -1 for fenthion using the time-scheduled selected ion monitoring mode. The method was successfully applied to real water, and the recoveries for spiked samples were 104% for diazinon and 97% for fenthion. (author)

  2. Effect of elevated carrier-gas pressure on hydraulic characteristics of gas-solid particle two-phase flow

    International Nuclear Information System (INIS)

    Timoshenko, V.I.; Knyshenko, Y.V.; Kopysov, V.F.; Gromov, E.N.

    1992-01-01

    The effect of elevated gas pressure on the hydraulic resistance and critical velocity of a two-phase flow is studied on a pneumatic-transport bench. It is established that for each working-pressure level there exists a limiting solid-phase concentration, the exceeding of which causes an abrupt rise in hydraulic resistance. 16 refs., 3 figs

  3. Environmental mobility of cobalt-Influence of solid phase characteristics and groundwater chemistry

    International Nuclear Information System (INIS)

    Payne, T.E.; Itakura, T.; Comarmond, M.J.; Harrison, J.J.

    2009-01-01

    The adsorption of cobalt on samples from a potential waste repository site in an arid region was investigated in batch experiments, as a function of various solution phase parameters including the pH and ionic strength. The samples were characterized using a range of techniques, including BET surface area measurements, total clay content and quantitative X-ray diffraction. The statistical relationships between the measured cobalt distribution coefficients (K d values) and the solid and liquid phase characteristics were assessed. The sorption of cobalt increased with the pH of the aqueous phase. In experiments with a fixed pH value, the measured K d values were strongly correlated to the BET surface area, but not to the amount of individual clay minerals (illite, kaolinite or smectite). A further set of sorption experiments was undertaken with two samples of distinctive mineralogy and surface area, and consequently different sorption properties. A simple surface complexation model (SCM) that conceptualized the surface sites as having equivalent sorption properties to amorphous Fe-oxide was moderately successful in explaining the pH dependence of the sorption data on these samples. Two different methods of quantifying the input parameters for the SCM were assessed. While a full SCM for cobalt sorption on these complex environmental substrates is not yet possible, the basic applicability and predictive capability of this type of modeling is demonstrated. A principal requirement to further develop the modeling approach is adequate models for cobalt sorption on component mineral phases of complex environmental sorbents.

  4. Multiple headspace-solid-phase microextraction: An application to quantification of mushroom volatiles

    International Nuclear Information System (INIS)

    Costa, Rosaria; Tedone, Laura; De Grazia, Selenia; Dugo, Paola; Mondello, Luigi

    2013-01-01

    Highlights: ► Multiple headspace extraction-solid phase microextraction (MHS-SPME) has been applied to the analysis of Agaricus bisporus. ► Mushroom flavor is characterized by the presence of compounds with a 8-carbon atoms skeleton. ► Formation of 8-carbon compounds involves a unique fungal biochemical pathway. ► The MHS-SPME allowed to determine quantitatively 5 target analytes of A. bisporus for the first time. -- Abstract: Multiple headspace-solid phase microextraction (MHS-SPME) followed by gas chromatography/mass spectrometry (GC–MS) and flame ionization detection (GC–FID) was applied to the identification and quantification of volatiles released by the mushroom Agaricus bisporus, also known as champignon. MHS-SPME allows to perform quantitative analysis of volatiles from solid matrices, free of matrix interferences. Samples analyzed were fresh mushrooms (chopped and homogenized) and mushroom-containing food dressings. 1-Octen-3-ol, 3-octanol, 3-octanone, 1-octen-3-one and benzaldehyde were common constituents of the samples analyzed. Method performance has been tested through the evaluation of limit of detection (LoD, range 0.033–0.078 ng), limit of quantification (LoQ, range 0.111–0.259 ng) and analyte recovery (92.3–108.5%). The results obtained showed quantitative differences among the samples, which can be attributed to critical factors, such as the degree of cell damage upon sample preparation, that are here discussed. Considerations on the mushrooms biochemistry and on the basic principles of MHS analysis are also presented

  5. Multiple headspace-solid-phase microextraction: An application to quantification of mushroom volatiles

    Energy Technology Data Exchange (ETDEWEB)

    Costa, Rosaria; Tedone, Laura; De Grazia, Selenia [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Dugo, Paola [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Centro Integrato di Ricerca (C.I.R.), Università Campus-Biomedico, Via Álvaro del Portillo, 21, 00128 Roma (Italy); Mondello, Luigi, E-mail: lmondello@unime.it [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Centro Integrato di Ricerca (C.I.R.), Università Campus-Biomedico, Via Álvaro del Portillo, 21, 00128 Roma (Italy)

    2013-04-03

    Highlights: ► Multiple headspace extraction-solid phase microextraction (MHS-SPME) has been applied to the analysis of Agaricus bisporus. ► Mushroom flavor is characterized by the presence of compounds with a 8-carbon atoms skeleton. ► Formation of 8-carbon compounds involves a unique fungal biochemical pathway. ► The MHS-SPME allowed to determine quantitatively 5 target analytes of A. bisporus for the first time. -- Abstract: Multiple headspace-solid phase microextraction (MHS-SPME) followed by gas chromatography/mass spectrometry (GC–MS) and flame ionization detection (GC–FID) was applied to the identification and quantification of volatiles released by the mushroom Agaricus bisporus, also known as champignon. MHS-SPME allows to perform quantitative analysis of volatiles from solid matrices, free of matrix interferences. Samples analyzed were fresh mushrooms (chopped and homogenized) and mushroom-containing food dressings. 1-Octen-3-ol, 3-octanol, 3-octanone, 1-octen-3-one and benzaldehyde were common constituents of the samples analyzed. Method performance has been tested through the evaluation of limit of detection (LoD, range 0.033–0.078 ng), limit of quantification (LoQ, range 0.111–0.259 ng) and analyte recovery (92.3–108.5%). The results obtained showed quantitative differences among the samples, which can be attributed to critical factors, such as the degree of cell damage upon sample preparation, that are here discussed. Considerations on the mushrooms biochemistry and on the basic principles of MHS analysis are also presented.

  6. Tungsten-Based Mesoporous Silicates W-MMM-E as Heterogeneous Catalysts for Liquid-Phase Oxidations with Aqueous H2O2

    Directory of Open Access Journals (Sweden)

    Nataliya Maksimchuk

    2018-02-01

    Full Text Available Mesoporous tungsten-silicates, W-MMM-E, have been prepared following evaporation-induced self-assembly methodology and characterized by elemental analysis, XRD, N2 adsorption, STEM-HAADF (high angle annular dark field in scanning-TEM mode, DRS UV-vis, and Raman techniques. DRS UV-vis showed the presence of two types of tungsten oxo-species in W-MMM-E samples: isolated tetrahedrally and oligomeric octahedrally coordinated ones, with the ratio depending on the content of tungsten in the catalyst. Materials with lower W loading have a higher contribution from isolated species, regardless of the preparation method. W-MMM-E catalyzes selectively oxidize of a range of alkenes and organic sulfides, including bulky terpene or thianthrene molecules, using green aqueous H2O2. The selectivity of corresponding epoxides reached 85–99% in up to 80% alkene conversions, while sulfoxides formed with 84–90% selectivity in almost complete sulfide conversions and a 90–100% H2O2 utilization efficiency. The true heterogeneity of catalysis over W-MMM-E was proved by hot filtration tests. Leaching of inactive W species depended on the reaction conditions and initial W loading in the catalyst. After optimization of the catalyst system, it did not exceed 20 ppm and 3 ppm for epoxidation and sulfoxidation reactions, respectively. Elaborated catalysts could be easily retrieved by filtration and reused several times with maintenance of the catalytic behavior.

  7. Sphene and zircon in the Highland Range volcanic sequence (Miocene, southern Nevada, USA): Elemental partitioning, phase relations, and influence on evolution of silicic magma

    Science.gov (United States)

    Colombini, L.L.; Miller, C.F.; Gualda, G.A.R.; Wooden, J.L.; Miller, J.S.

    2011-01-01

    Sphene is prominent in Miocene plutonic rocks ranging from diorite to granite in southern Nevada, USA, but it is restricted to rhyolites in coeval volcanic sequences. In the Highland Range volcanic sequence, sphene appears as a phenocryst only in the most evolved rocks (72-77 mass% SiO2; matrix glass 77-78 mass% SiO2). Zr-in-sphene temperatures of crystallization are mostly restricted to 715 and 755??C, in contrast to zircon (710-920??C, Ti-in-zircon thermometry). Sphene rim/glass Kds for rare earth elements are extremely high (La 120, Sm 1200, Gd 1300, Lu 240). Rare earth elements, especially the middle REE (MREE), decrease from centers to rims of sphene phenocrysts along with Zr, demonstrating the effect of progressive sphene fractionation. Whole rocks and glasses have MREE-depleted, U-shaped REE patterns as a consequence of sphene fractionation. Within the co-genetic, sphene-rich Searchlight pluton, only evolved leucogranites show comparable MREE depletion. These results indicate that sphene saturation in intruded and extruded magmas occurred only in highly evolved melts: abundant sphene in less silicic plutonic rocks represents a late-stage 'bloom' in fractionated interstitial melt. ?? 2011 Springer-Verlag.

  8. Binding of monoclonal antibody to protein antigen in fluid phase or bound to solid supports

    Energy Technology Data Exchange (ETDEWEB)

    Kennel, S.J.

    1982-01-01

    Rat monoclonal antibody (MoAb) to fragment D (FgD) of human fibrinogen was used to characterize the direct binding of antibody to protein in solution or bound to solid supports. Purified IgG, F(ab')/sub 2/ and Fab' were prepared from ascites fluid of hybridoma 104-14B which is a fusion product of spleen cells from a rat immunized with FgD and the mouse myeloma cell line, P3-X63-Ag8. Two-dimensional electrophoresis of radioiodinated antibody preparations demonstrated the presence of hybrid immunoglobulin molecules, but only structures having rat heavy and rat light chains had active antibody combinig sites. The affinity constant for IgG as well as F(ab')/sub 2/ and Fab', 6x10/sup 9/ M/sup -1/, was identical when tested using fluid phase antigen (/sup 125/I-labeled FgD). Affinity constants determined for direct binding of iodinated IgG using FgD immobilized on solid supports showed a slight dependence on the antigen concentration used in the measurement. These values ranged from 0.5x10/sup 9/ M/sup -1/ at high antigen concentrations (1.3x10/sup -7/ M) to 9x10/sup 9/ M/sup -1/ at low antigen concentration (1.3x10/sup -10/ M). Binding constants for F(ab')/sub 2/ and Fab' gave similar results indicating that binding was homogeneous and univalent. The capacity of solid state antigen to bind antibody varied with the method used to bind FgD to the solid support. FgD bound directly to polystyrene plates was least efficient at binding labeled antibody; FgD bound to plates through intermediate carriers poly(L-lysine) was only slightly more efficient, while antigen bound to Sepharose beads by cyanogen bromide activation was the most active.

  9. Polymer-Layer Silicate Nanocomposites

    DEFF Research Database (Denmark)

    Potarniche, Catalina-Gabriela

    Nowadays, some of the material challenges arise from a performance point of view as well as from recycling and biodegradability. Concerning these aspects, the development of polymer layered silicate nanocomposites can provide possible solutions. This study investigates how to obtain polymer layered...... silicate nanocomposites and their structure-properties relationship. In the first part of the thesis, thermoplastic layered silicates were obtained by extrusion. Different modification methods were tested to observe the intercalation treatment effect on the silicate-modifier interactions. The silicate...... modification was studied at different silicate/modifier ratios and properties were investigated for obtained nanocomposites with different amounts of modified layered silicate loadings. The obtained nanocomposites presented improved mechanical properties such as toughness, stiffness or a good balance between...

  10. The research on particle trajectory of solid-liquid two-phase flow and erosion predicting in screw centrifugal pump

    Science.gov (United States)

    Shen, Z. J.; Li, R. N.; Han, W.; Zhao, W. G.; Wang, X. H.

    2016-05-01

    Use the Discrete Phase Model (DPM) based on Euler-Lagrange method, the internal flow field of screw centrifugal pump was simulated by computational fluid dynamics(CFD) code when transmission medium is solid-liquid two phase flow with large-size particles. The research of liquid phase is under the Euler coordinate system while the solid phase is under the Lagrange coordinate system. The energy change, trajectory characteristic of solid phase particle and its erosion damage rule of solid-phase particle in whole computational domain is analyzed with different density, partical size(d=0.05mm, d=0.2mm, d=2mm) and solid volume fraction(Cv=3%, Cv=5%, Cv=7%).The result shows that within a given diameter range, the low density fine particles trajectory are longer, more collision times with flow passage components, more energy loss and the erosion parts are relatively uniform, but particles which are large-size diameter and high density has a big collision angle with the surface of impeller and volute, even the area of impact and abrasion are quite focus, and easy to be transported. particles will impact with the head of impeller when it enter into impeller domain, the erosion mainly occurs on the work side of impeller.

  11. The study of thermal interaction and microstructure of sodium silicate/bentonite composite under microwave radiation

    Energy Technology Data Exchange (ETDEWEB)

    Subannajui, Kittitat, E-mail: kittitat.sub@mahidol.ac.th [Faculty of Science, Mahidol University, 272 Rama VI Road, Ratchathewi District, Bangkok 10400 (Thailand); Center of Nanoscience and Nanotechnology Research Unit, Mahidol University, 272 Rama VI Road, Ratchathewi District, Bangkok 10400 (Thailand)

    2016-12-01

    The commercial heating oven usually consumes the power around 2500–3000 Watt and the temperature inside the oven is still below 350 °C. If we need to increase a temperature above 500 °C, a special heating setup with a higher power furnace is required. However, in this work, we propose a composite material that interacts with 2.45 GHz 500 Watt microwave and rapidly redeems the thermal energy with the temperature around 600–900 °C. The composite amorphous material easily forms liquid ceramics phase with a high temperature output and responds to the microwave radiation better than that of the solid phase. During the heating process, phase transformation occurs. This method is very effective and can be used to drastically reduce the power consumption of any heating process. - Highlights: • Amorphous phase transforms to liquid phase by microwave radiation. • Pure sodium silicate and pure bentonite cannot show temperature overshoot. • Silicate-bentonite composite shows a high temperature overshoot above 700 °C. • A rapid heating crucible for the annealing application is fabricated.

  12. The effect of high antigen density on solid-phase radioimmunoassays for antibody regardless of immunoglobulin class

    International Nuclear Information System (INIS)

    Rubin, R.L.; Hardtke, M.A.; Carr, R.I.

    1980-01-01

    Human sera containing antibody to casein or to bovine serum albumin were used to assess the validity and utility of a solid-phase assay for quantitating antibody activity. Rabbit anti-human immunoglobulin radiolabeled with 125 I and capable of reacting with all human immunoglobulin classes was used to detect antibody bound to antigen immobilized to polystyrene tubes by a new covalent technique. This method results in very high antigen concentrations in highly stable association with polystyrene tubes. Kinetic and absorption studies demonstrated that low avidity antibodies are better detected when antigen is immobilized by the covalent method than when passively adsorbed. Conditions are described for minimizing artifactual interactions and for obtaining results similar to those obtained with conventional, liquid-phase assays. Failure to reach equilibrium in solid-phase assays and other problems are proposed to explain, in part, the inability to obtain a better correlation between solid- and liquid-phase immunoassays. (Auth.)

  13. Solid-phase Synthesis of Combinatorial 2,4-Disubstituted-1,3,5-Triazine via Amine Nucleophilic Reaction

    International Nuclear Information System (INIS)

    Moon, Sung Won; Ham, Jungyeob; Chang, Young-Tae; Lee, Jae Wook

    2015-01-01

    In combinatorial chemistry, solid-phase synthesis is a popular approach formass production of small molecules. Compared to solution-phase synthesis, it is easy to prepare and purify a large number of heterocyclic small molecules via solid-phase chemistry; the overall reaction time is decreased as well. 1,3,5-Triazine is a nitrogen-containing heterocyclic aromatic scaffold that was shown to be a druggable scaffold in recent studies. These structures have been reported as anticancer, antimicrobial, and antiretroviral compounds, as CDKs and p38 MAP kinase inhibitors, as estrogen receptor modulators, and as inosine monophosphate dehydrogenase inhibitors. we designed and synthesized disubstituted triazine compounds as an analog of disubstituted pyrimidine compounds. These disubstituted triazine compounds possess a linear structure which may have biological activity similar to that of disubstituted pyrimidine. Here we report the solid-phase synthesis of disubstituted triazine compounds

  14. Solid-phase Synthesis of Combinatorial 2,4-Disubstituted-1,3,5-Triazine via Amine Nucleophilic Reaction

    Energy Technology Data Exchange (ETDEWEB)

    Moon, Sung Won [KIST Gangneung Institute, Gangneung (Korea, Republic of); Ham, Jungyeob [Gangneung-Wonju National University, Gangneung (Korea, Republic of); Chang, Young-Tae [National University of Singapore, Singapore (Singapore); Lee, Jae Wook [University of Science and Technology, Daejon (Korea, Republic of)

    2015-01-15

    In combinatorial chemistry, solid-phase synthesis is a popular approach formass production of small molecules. Compared to solution-phase synthesis, it is easy to prepare and purify a large number of heterocyclic small molecules via solid-phase chemistry; the overall reaction time is decreased as well. 1,3,5-Triazine is a nitrogen-containing heterocyclic aromatic scaffold that was shown to be a druggable scaffold in recent studies. These structures have been reported as anticancer, antimicrobial, and antiretroviral compounds, as CDKs and p38 MAP kinase inhibitors, as estrogen receptor modulators, and as inosine monophosphate dehydrogenase inhibitors. we designed and synthesized disubstituted triazine compounds as an analog of disubstituted pyrimidine compounds. These disubstituted triazine compounds possess a linear structure which may have biological activity similar to that of disubstituted pyrimidine. Here we report the solid-phase synthesis of disubstituted triazine compounds.

  15. Silicates in Alien Asteroids

    Science.gov (United States)

    2009-01-01

    This plot of data from NASA's Spitzer Space Telescopes shows that asteroid dust around a dead 'white dwarf' star contains silicates a common mineral on Earth. The data were taken primarily by Spitzer's infrared spectrograph, an instrument that breaks light apart into its basic constituents. The yellow dots show averaged data from the spectrograph, while the orange triangles show older data from Spitzer's infrared array camera. The white dwarf is called GD 40.

  16. A New Thermodynamic Parameter to Predict Formation of Solid Solution or Intermetallic Phases in High Entropy Alloys (Postprint)

    Science.gov (United States)

    2015-11-02

    AFRL-RX-WP-JA-2016-0345 A NEW THERMODYNAMIC PARAMETER TO PREDICT FORMATION OF SOLID SOLUTION OR INTERMETALLIC PHASES IN HIGH ENTROPY ...INTERMETALLIC PHASES IN HIGH ENTROPY ALLOYS (POSTPRINT) 5a. CONTRACT NUMBER FA8650-10-D-5226-0005 5b. GRANT NUMBER 5c. PROGRAM ELEMENT NUMBER...simple thermodynamic criterion is proposed to predict the presence or absence of equilibrium intermetallic phases in a high entropy alloy at a given

  17. Local Cloudiness Development Forecast Based on Simulation of Solid Phase Formation Processes in the Atmosphere

    Science.gov (United States)

    Barodka, Siarhei; Kliutko, Yauhenia; Krasouski, Alexander; Papko, Iryna; Svetashev, Alexander; Turishev, Leonid

    2013-04-01

    Nowadays numerical simulation of thundercloud formation processes is of great interest as an actual problem from the practical point of view. Thunderclouds significantly affect airplane flights, and mesoscale weather forecast has much to contribute to facilitate the aviation forecast procedures. An accurate forecast can certainly help to avoid aviation accidents due to weather conditions. The present study focuses on modelling of the convective clouds development and thunder clouds detection on the basis of mesoscale atmospheric processes simulation, aiming at significantly improving the aeronautical forecast. In the analysis, the primary weather radar information has been used to be further adapted for mesoscale forecast systems. Two types of domains have been selected for modelling: an internal one (with radius of 8 km), and an external one (with radius of 300 km). The internal domain has been directly applied to study the local clouds development, and the external domain data has been treated as initial and final conditions for cloud cover formation. The domain height has been chosen according to the civil aviation forecast data (i.e. not exceeding 14 km). Simulations of weather conditions and local clouds development have been made within selected domains with the WRF modelling system. In several cases, thunderclouds are detected within the convective clouds. To specify the given category of clouds, we employ a simulation technique of solid phase formation processes in the atmosphere. Based on modelling results, we construct vertical profiles indicating the amount of solid phase in the atmosphere. Furthermore, we obtain profiles demonstrating the amount of ice particles and large particles (hailstones). While simulating the processes of solid phase formation, we investigate vertical and horizontal air flows. Consequently, we attempt to separate the total amount of solid phase into categories of small ice particles, large ice particles and hailstones. Also, we

  18. Tailored Nanocomposites of Polypropylene with Layered Silicates

    Energy Technology Data Exchange (ETDEWEB)

    Xu, L.; Nakajima, H; Manias, E; Krishnamoorti, R

    2009-01-01

    The melt rheological properties of layered silicate nanocomposites with maleic anhydride (MA) functionalized polypropylene are contrasted to those based on ammonium-terminated polypropylene. While the MA functionalized PP based nanocomposites exhibit solid-like linear viscoelastic behavior, consistent with the formation of a long-lived percolated nanoparticle network, the single-end ammonium functionalized PP based nanocomposites demonstrated liquid-like behavior at comparable montmorillonite concentrations. The differences in the linear viscoelasticity are attributed to the presence of bridging interactions in MA functionalized nanocomposites. Further, the transient shear stress of the MA functionalized nanocomposites in start-up of steady shear is a function of the shear strain alone, and the steady shear response is consistent with that of non-Brownian systems. The weak dependence of the steady first normal stress difference on the steady shear stress suggests that the polymer chain mediated silicate network contributes to such unique flow behavior.

  19. 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

  20. Petrophysical Analysis of Siliceous Ooze Sediments, Ormen Lange Field, Norway

    DEFF Research Database (Denmark)

    Awedalkarim, Ahmed; Fabricius, Ida Lykke

    Skeletal remains of siliceous algae form biogenic fine grained highly porous pelagic siliceous ooze sediments that were found above the reservoir of the Ormen Lange gas field which is located in the southern part of the Norwegian Sea (Figure 1a). The Palaeocene sandstone of the “Egga” Formation...... structure is complex and the solids are mechanically fragile and hydrous. Normal petrophysical methods used in formation evaluation might not be suitable for interpreting siliceous ooze. For example, density and neutron logging tools are calibrated to give correct porosity readings in a limestone formation......, but apparent porosity indications in any other lithology, such as siliceous ooze, are wrong and they should be corrected. The apparent bulk density log should be influenced by the hydrogen in opal as also the neutron porosity tools because they are sensitive to the amount of hydrogen in a formation...

  1. Anaerobic digestion of onion residuals using a mesophilic Anaerobic Phased Solids Digester

    International Nuclear Information System (INIS)

    Romano, Rowena T.; Zhang, Ruihong

    2011-01-01

    The anaerobic digestion of onion residual from an onion processing plant was studied under batch-fed and continuously-fed mesophilic (35 ± 2 o C) conditions in an Anaerobic Phased Solids (APS) Digester. The batch digestion tests were performed at an initial loading of 2.8 gVS L -1 and retention time of 14 days. The biogas and methane yields, and volatile solids reduction from the onion residual were determined to be 0.69 ± 0.06 L gVS -1 , 0.38 ± 0.05 L CH 4 gVS -1 , and 64 ± 17%, respectively. Continuous digestion tests were carried out at organic loading rates (OLRs) of 0.5-2.0 gVS L -1 d -1 . Hydrated lime (Ca(OH) 2 ) was added to the APS-Digester along with the onion residual at 16 mg Ca(OH) 2 gVS -1 to control the pH of the biogasification reactor above 7.0. At steady state the average biogas yields were 0.51, 0.56, and 0.62 L gVS -1 for the OLRs of 0.5, 1.0, and 2.0 gVS L -1 d -1 respectively. The methane yields at steady state were 0.29, 0.32, and 0.31 L CH 4 gVS -1 for the OLRs of 0.5, 1.0, and 2.0 gVS L -1 d -1 respectively. The study shows that the digestion of onion residual required proper alkalinity and pH control, which was possible through the use of caustic chemicals. However, such chemicals will begin to have an inhibitory effect on the microbial population at high loading rates, and therefore alternative operational parameters are needed. -- Highlights: → An APS-Digester was used to study biogas production from onion solid residues. → Biogas and methane yields from onion solids were determined. → Study showed substantial findings for treating onion solid residues.

  2. Direct visualisation of mesh phases at solid/solution interfaces by AFM

    International Nuclear Information System (INIS)

    Blom, A.; Warr, G.G.

    2003-01-01

    Full text: Using soft-contact AFM imaging, the adsorbed layer structure of single chained dodecyltrimethylammonium bromide (DTAB) and double chained didodecyldimethylammonium bromide (DDAB) mixed solutions at varying compositions has been studied. DTAB forms rods on mica and globules on quartz whereas DDAB exists as bilayer on both substrates. On mica, the observed morphologies as composition was changed from DDAB-rich mixtures to DTAB-rich mixtures changed from bilayer to rods but also exhibited an isotropic, periodically textured structure in a narrow intermediate composition range. On quartz, the transition sequence followed bilayer > periodic isotropic texture >rods >globules with increasing DTAB content. Again, the periodic isotropic texture was observed only over a very narrow composition range. We interpret the observed transitions by the formation of a mesh phase on the surface. This phase is consistent with the average curvature progression from bilayer to rods, and consists of branched rods. Studies performed on solution structures of fluorinated surfactants 1 and long-chained polyoxyethylene surfactants 2 have elucidated the balance between headgroup curvature forces and alkyl chain flexibility as responsible for formation of intermediate structures in bulk. It is believed that the resulting balance of forces between structures of high curvature preferred by DTAB and the reduced alkyl chain flexibility of DDAB is being satisfied by the formation of a mesh phase at the solid/solution interface

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  4. Symmetry-adapted order parameters and free energies for solids undergoing order-disorder phase transitions

    Science.gov (United States)

    Natarajan, Anirudh Raju; Thomas, John C.; Puchala, Brian; Van der Ven, Anton

    2017-10-01

    Accurate thermodynamic descriptions are a key ingredient to kinetic theories that describe the mesoscale evolution of a solid undergoing ordering or decomposition reactions. We introduce a general approach to identify order parameters for order-disorder reactions and to calculate first-principles free-energy surfaces as a function of these order parameters. The symmetry of the disordered phase is used to formulate order parameters as linear combinations of sublattice compositions of a reference supercell. The order parameters can distinguish the disordered phase from the symmetrically equivalent variants of a particular ordered phase. A thermodynamic formalism is then developed to rigorously define a coarse-grained free energy as a function of order parameters. Bias potentials are added to the potential energy to enable sampling of the unstable regions within the order-parameter domain. Monte Carlo sampling in the biased ensemble is combined with free-energy integration to calculate high-temperature free energies. We illustrate the approach by analyzing the free energies of order-disorder transitions on a two-dimensional triangular lattice and in the technologically important Ni-Al alloy.

  5. Determination of Iron Species by Combination of Solvent Assisted-Dispersive Solid Phase Extraction and Spectrophotometry

    Directory of Open Access Journals (Sweden)

    Zahra Dehghani

    2015-06-01

    Full Text Available A simple, rapid and sensitive solvent assisted-dispersive solid phase extraction method was developed for the extraction of iron(II prior to its spectrophotometric determination. The Fe(II reacted with 2,4,6-tris(2-pyridyl-1,3,5-triazine, neutralized with sodium dodecyl sulfate and extracted onto the fine particles of benzophenone which were formed upon rapid injection of a mixture of benzophenone as the sorbent and ethanol as the disperser solvent into the aqueous solution. After phase separation, the sedimented phase containing the complex was dissolved in ethanol and the analyte concentration was determined by measuring its absorption at 594 nm. Total iron was determined after the reduction of Fe(III to Fe(II with hydroxylamine hydrochloride. Under the optimized conditions, an enhancement factor of 32, the detection limit of 0.16 µg l-1, and the relative standard deviation of 1.9% (n = 6 at 20 µg l-1 concentration level of Fe(II were achieved. The method was successfully applied to the determination of iron species in water samples and total iron in infant dry formula milk, apple, rice, spinach and parsley samples.

  6. 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)

  7. Energetics analysis of interstitial loops in single-phase concentrated solid-solution alloys

    Science.gov (United States)

    Wang, Xin-Xin; Niu, Liang-Liang; Wang, Shaoqing

    2018-04-01

    Systematic energetics analysis on the shape preference, relative stability and radiation-induced segregation of interstitial loops in nickel-containing single-phase concentrated solid-solution alloys have been conducted using atomistic simulations. It is shown that the perfect loops prefer rhombus shape for its low potential energy, while the Frank faulted loops favor ellipse for its low potential energy and the possible large configurational entropy. The decrease of stacking fault energy with increasing compositional complexity provides the energetic driving force for the formation of faulted loops, which, in conjunction with the kinetic factors, explains the experimental observation that the fraction of faulted loops rises with increasing compositional complexity. Notably, the kinetics is primarily responsible for the absence of faulted loops in nickel-cobalt with a very low stacking fault energy. We further demonstrate that the simultaneous nickel enrichment and iron/chromium depletion on interstitial loops can be fully accounted for by their energetics.

  8. Human Thrombin Detection Through a Sandwich Aptamer Microarray: Interaction Analysis in Solution and in Solid Phase

    Science.gov (United States)

    Sosic, Alice; Meneghello, Anna; Cretaio, Erica; Gatto, Barbara

    2011-01-01

    We have developed an aptamer-based microarray for human thrombin detection exploiting two non-overlapping DNA thrombin aptamers recognizing different exosites of the target protein. The 15-mer aptamer (TBA1) binds the fibrinogen-binding site, whereas the 29-mer aptamer (TBA2) binds the heparin binding domain. Extensive analysis on the complex formation between human thrombin and modified aptamers was performed by Electrophoresis Mobility Shift Assay (EMSA), in order to verify in solution whether the chemical modifications introduced would affect aptamers/protein recognition. The validated system was then applied to the aptamer microarray, using the solid phase system devised by the solution studies. Finally, the best procedure for Sandwich Aptamer Microarray (SAM) and the specificity of the sandwich formation for the developed aptasensor for human thrombin were optimized. PMID:22163703

  9. 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

  10. Development Of Radioimmunoassay For Prolactin HORMONE Using Solid Phase Magnetic Particles

    International Nuclear Information System (INIS)

    SHAFIK, H.M.; MEHANY, N.L.

    2009-01-01

    The preparation and development of primary reagents of prolactin (PRL) radioimmunoassay (RIA) technique using solid phase magnetic particles with low cost is considered to be the main objective of the present study. The production of polyclonal antibodies was undertaken by immunizing four female New-Zealand rabbits through primary injection and four booster doses subcutaneously. The preparation of 125 I-prolactin radiotracer was carried out using chloramine-T. The preparation of standard prolactin was undertaken by preparing stock standard solution of prolactin and diluted with assay buffer. Activation and coupling of low magnetizable particles with the purified anti-PRL was carried out. Optimization and validation of the assay were carried out. The results obtained provide a highly sensitive, specific and accurate RIA system of PRL. In conclusion, this assay could be used in diagnosis of galactorrhea, prolactinoma, visual impairment and diagnosis of infertility in males and females.

  11. Automated solid-phase subcloning based on beads brought into proximity by magnetic force.

    Science.gov (United States)

    Hudson, Elton P; Nikoshkov, Andrej; Uhlen, Mathias; Rockberg, Johan

    2012-01-01

    In the fields of proteomics, metabolic engineering and synthetic biology there is a need for high-throughput and reliable cloning methods to facilitate construction of expression vectors and genetic pathways. Here, we describe a new approach for solid-phase cloning in which both the vector and the gene are immobilized to separate paramagnetic beads and brought into proximity by magnetic force. Ligation events were directly evaluated using fluorescent-based microscopy and flow cytometry. The highest ligation efficiencies were obtained when gene- and vector-coated beads were brought into close contact by application of a magnet during the ligation step. An automated procedure was developed using a laboratory workstation to transfer genes into various expression vectors and more than 95% correct clones were obtained in a number of various applications. The method presented here is suitable for efficient subcloning in an automated manner to rapidly generate a large number of gene constructs in various vectors intended for high throughput applications.

  12. Modeling of sorption processes on solid-phase ion-exchangers

    Science.gov (United States)

    Dorofeeva, Ludmila; Kuan, Nguyen Anh

    2018-03-01

    Research of alkaline elements separation on solid-phase ion-exchangers is carried out to define the selectivity coefficients and height of an equivalent theoretical stage for both continuous and stepwise filling of column by ionite. On inorganic selective sorbents the increase in isotope enrichment factor up to 0.0127 is received. Also, parametrical models that are adequately describing dependence of the pressure difference and the magnitude expansion in the ion-exchange layer from the flow rate and temperature have been obtained. The concentration rate value under the optimum realization conditions of process and depending on type of a selective material changes in a range 1.021÷1.092. Calculated results show agreement with experimental data.

  13. Facile synthesis of stereoregular carbon fiber precursor polymers by template assisted solid phase polymerization

    Directory of Open Access Journals (Sweden)

    G. Santhana Krishnan

    2012-09-01

    Full Text Available Predominantly isotactic stereoregular polyacrylonitrile copolymers (PAC were prepared by solid phase polymerization techniques using hexagonal crystalline metal salts as template compounds. Stereoregular distributions of the prepared polymer were studied using high resolution 13C nuclear magnetic resonance spectroscopy (13C NMR spectra. The extent of isotacticity was directly determined from the peak intensity of the methine carbon (CH. The triad tacticity from the intensities of methine carbon peaks were examined by statistical methods. It was found that the PAC was predominantly isotactic in stereoregularity, and its sequence distribution obeys Bernoulli statistics. The optimum polymerization conditions ensuring isotactic content over 50% were disclosed experimentally. The chemical composition of PAC was confirmed with 1H NMR data. The obtained polyacrylonitrile copolymers were also characterized for molecular parameters such as viscosity average molecular weight (Mv, number average molecular weight (Mn, weight average molecular weight (Mw and polydispersity index.

  14. Reducing the sulfur-dioxide binding power of sweet white wines by solid-phase extraction.

    Science.gov (United States)

    Saidane, Dorra; Barbe, Jean-Christophe; Birot, Marc; Deleuze, Hervé

    2013-11-01

    The high sulfur-dioxide binding power of sweet white wines may be reduced by extracting the naturally present carbonyl compounds from wine that are responsible for carbonyl bisulphites formation. The carbonyl compounds mainly responsible for trapping SO2 are acetaldehyde, pyruvic acid, and 2-oxoglutaric acid. The method employed was selective solid phase extraction, using phenylsulfonylhydrazine as a scavenging agent. The scavenging function was grafted onto a support prepared from raw materials derived from lignin. This approach is more acceptable to winemakers than the polymer media previously reported, as it reduces the possible contamination of wine to molecules already present in the wine making process. Copyright © 2013 Elsevier Ltd. All rights reserved.

  15. Rapid determination of volatile organic compounds in environmentally hazardous wastewaters using solid phase microextraction

    Energy Technology Data Exchange (ETDEWEB)

    James, K.J.; Stack, M.A. [Ecotoxicology Research Unit, Chemistry Department, Cork RTC, Bishopstown, Cork (Ireland)

    1997-08-01

    Solid phase micro-extraction (SPME) was applied to the determination of volatile organic compounds (VOC) in wastewater discharges. Environmentally significant samples, typical of those subject to regulatory control, were examined and included discharges from pharmaceutical, petrochemical and municipal sewerage treatment plants. Analysis was performed using gas chromatography - mass spectrometry (GC-MS) following sampling using headspace or immersion SPME. Fused silica fibres, coated with either poly(dimethylsiloxane) or poly(acrylate), were examined to determine VOC which included chloroform, saturated carboxylic acids, alkylbenzenes, phenol, benzonitrile and benzofuran. Detection limits varied from 10 to 170 ng/ml and satisfactory relative standard deviations (%RSD < 10) were obtained. For most samples, headspace sampling was preferred to immersion. SPME was found to be a useful technique for the rapid screening of wastewaters for VOC. (orig.) With 2 figs., 3 tabs.

  16. Direct solid-phase radioimmunoassay for the detection of Aujeszky's disease antibodies

    Energy Technology Data Exchange (ETDEWEB)

    Doeller, G.; Jakubik, J.

    1980-06-01

    A direct solid-phase radioimmunoassy (dRIA) was developed in order to demonstrate antibodies against Aujeszky's disease virus (ADV) in sera obtained from pigs and rabbits. In the presence of guinea-pig complement the above test is 160-fold to 1500-fold more sensitive than the neutralization test (NT) and 320-fold to 150 000-fold more sensitive than sera obtained from an ADV-infected farm, which were found to be negative in the complement assisted NT. It is possible to test a single dilution of unknown serum by dRIA by comparing same with a standard curve and to make a statement regarding its ADV-specific binding capacity to /sup 125/I-labelled ADV antigen. The advantages of dRIA in comparison to the indirect RIA and the advantages and disadvantages with regard to ELISA were discussed.

  17. Recent Developments in Solid-Phase Extraction for Near and Attenuated Total Reflection Infrared Spectroscopic Analysis

    Directory of Open Access Journals (Sweden)

    Christian W. Huck

    2016-05-01

    Full Text Available A review with more than 100 references on the principles and recent developments in the solid-phase extraction (SPE prior and for in situ near and attenuated total reflection (ATR infrared spectroscopic analysis is presented. New materials, chromatographic modalities, experimental setups and configurations are described. Their advantages for fast sample preparation for distinct classes of compounds containing different functional groups in order to enhance selectivity and sensitivity are discussed and compared. This is the first review highlighting both the fundamentals of SPE, near and ATR spectroscopy with a view to real sample applicability and routine analysis. Most of real sample analyses examples are found in environmental research, followed by food- and bioanalysis. In this contribution a comprehensive overview of the most potent SPE-NIR and SPE-ATR approaches is summarized and provided.

  18. Analysis of a solid-phase radioimmunoassay for antibodies to cytoplasmic antigen fractions of Candida albicans

    International Nuclear Information System (INIS)

    Mauch, H.; Bromback, J.

    1981-01-01

    An indirect solid-phase radioimmunoassay (SPRIA) in individual polystyrene microtiter cups has been adapted for measurement of antibody to various cytoplasmic and carbohydrate antigen fractions of Candida albicans. The assay was optimized for sensitivity, precision and linearization of serum dilution curves. The optimized procedure allows computerized measurement of anti-Candida antibodies and can be used for measurement of antibody over a wide concentration range. The procedure obviates variation due to changes in day-to-day counts as a result of isotope decay and end-point antibody dilutions. The assay has been used to demonstrate a Poisson-like distribution of antibody levels in the sera of persons showing no symptoms of candidiasis. The minimum antibody level detectable by the assay is about two orders of magnitude lower than the lowest level found in human serum and 4 orders of magnitude lower than the most sensitive test used hitherto, the hemagglutination test. (Auth.)

  19. 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.

  20. A carbon nanotube confinement strategy to implement homogeneous asymmetric catalysis in the solid phase.

    Science.gov (United States)

    Hashimoto, Kazuki; Kumagai, Naoya; Shibasaki, Masakatsu

    2015-03-09

    A readily recyclable asymmetric catalyst has been developed based on the self-assembly of a homogeneous catalyst in a fibrous network of multiwalled carbon nanotubes (MWNTs). Dimerization of an amide-based chiral ligand with a suitable spacer allows for the efficient formation of a heterogeneous catalyst by self-assembly on addition of Er(OiPr)3. The self-assembly proceeds in the MWNT fibrous network and small clusters of assembled catalyst are confined in the MWNTs, producing an easily handled solid-phase catalyst. The resulting MWNT-confined catalyst exhibits a good catalytic performance in a catalytic asymmetric Mannich-type reaction, which can be conducted in a repeated batch system and in a continuous-flow platform. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Solid-Phase Iminium Cyclization Reactions for the Synthesis of Natural Product-Like Diketopiperazines

    DEFF Research Database (Denmark)

    Petersen, Rico

    The development of methodology for the solid-phase synthesis of fused 2,5-diketopiperazines with an emphasis on structural and stereochemical control, has been accomplished through two different approaches. The first approach was based on a highly trans-stereoselective (82% d.e.) intramolecular N......-suited for the synthesis of diastereoisomeric mixtures of 2,5-diketopiperazino[6,1-a]tetrahydroisoquinolines in high purities (74 to 90%), allowing for the separation of the cis-diastereoisomers. The route based on glyoxylic acid was found to be cis-stereoselective (1:2) generating the 2,5-diketopiperazino[6,1-a...... inhibitors based on the 2,5-diketopiperazino[6,1-a]tetrahydroisoquinoline scaffold was prepared and subsequently evaluated for biologically activity. The compounds showed inhibitory activity against a nuclear extract of HeLa cells, on average 200-fold lower than the activity of SAHA. When screened towards...

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

    International Nuclear Information System (INIS)

    McCallum, J.C.

    1998-01-01

    The kinetics of dopant-enhanced solid phase epitaxy (SPE) have been measured in buried a-Si layers doped with arsenic. SPE rates were measured over the temperature range 480 - 660 deg C for buried a-Si layers containing ten different As concentrations. In the absence of H-retardation effects, the dopant-enhanced SPE rate is observed to depend linearly on the As concentration over the entire range of concentrations, 1-16 x 10 19 cm -3 covered in the study. The Fermi level energy was calculated as a function of doping and find an equation that can provide good fits to the data. The implications of these results for models of the SPE process is discussed

  3. Determination of trace amounts of beryllium in water by solid-phase spectrophotometry

    International Nuclear Information System (INIS)

    Valencia, M.C.; Boudra, S.; Bosque-Sendra, J.M.

    1993-01-01

    A method for the determination of trace amounts of beryllium has been developed, based on solid-phase spectrophotometry. Beryllium reacts with Eriochrome Cyanine R in the presence of ethylenediaminetetraacetic acid to give a highly absorbent complex, which is fixed on a dextran-type anion-exchange gel. The absorbances of the gel, at 580 and 750 nm, packed in a 1 mm cell, is measured directly. The calibration graph is linear over the concentration range 0.1-1.2 μg 1 -1 and the relative standard deviation is 2.3%. The detection limit of the 1000 ml sample method is 6 ng 1 -1 for 0.030 g of anion-exchange gel. The sensitivity can be enhanced by increasing the sample volume. It has been applied to the determination of beryllium in tap water, spring water and well water contaminated with water from the leaching of industrial wastes from a uranium treatment plant. (author)

  4. 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 constitute a specific chemical pattern either qualitatively or quantitatively indicating copepod presence. The majority of the compounds were present in both female and male exudates, but nine compounds were mainly or exclusively present in female exudates and hence potential pheromone candidates......Copepods are ubiquitous in aquatic habitats. They exude bioactive compounds that mediate mate finding or induce defensive traits in prey organisms. However, little is known about the chemical nature of the copepod exometabolome that contributes to the chemical landscape in pelagic habitats. Here we...

  5. Separation and Purification of Sulforaphane from Broccoli by Solid Phase Extraction

    Science.gov (United States)

    Han, Dandan; Row, Kyung Ho

    2011-01-01

    A simple solid-phase extraction (SPE) method for the determination of sulforaphane in broccoli has been developed. The optimal conditions were found to be use of a silica SPE cartridge, and ethyl acetate and dichloromethane as washing and eluting solvents, respectively, which could eliminate interferences originating from the broccoli matrix. The extracts were sufficiently clean to be directly injected into high-performance liquid chromatography (HPLC) for further chromatographic analysis. Good linearity was obtained from 0.05 to 200 μg/mL (r = 0.998) for sulforaphane with the relative standard deviations less than 3.6%. The mean recoveries of sulforaphane from broccoli were more than 90.8% and the detection limit (S/N = 3:1) was 0.02 μg/mL. The SPE method provides a higher yield of sulforaphane from crude extracts compared to conventional liquid-liquid extraction. PMID:21673926

  6. Influence of sediment composition on apparent toxicity in a solid-phase test using bioluminescent bacteria

    Energy Technology Data Exchange (ETDEWEB)

    Benton, M.J. [East Tennessee State Univ., Johnson City, TN (United States). Dept. of Environmental Health; Malott, M.L. [Univ. of Mississippi, University, MS (United States)]|[Dept. of Agriculture, Oxford, MS (United States); Knight, S.S.; Cooper, C.M. [Dept. of Agriculture, Oxford, MS (United States); Benson, W.H. [Univ. of Mississippi, University, MS (United States)

    1995-03-01

    Clean and spiked sediment formulations of various silt:sand and clay:sand ratios were tested for toxicity using a bioassay that utilizes bioluminescent bacteria. Measured toxicities of clean and copper sulfate-spiked sediments were negatively but nonlinearly related with percent silt and percent clay, but no significant relationship existed between measured toxicity and sediment composition for methyl parathion-spiked formulations. Results suggest that solid-phase sediment bioassays using bioluminescence bacteria may be useful for testing the toxicities of single contaminants in formulated artificial sediments of known particle-size composition, and for repeated samples collected from the same site. However, extreme caution must be taken when testing sediments of varying composition or which may be differentially contaminated or contain a suite of contaminants.

  7. Effect of structural defects on anomalous ultrasound propagation in solids during second-order phase transitions

    International Nuclear Information System (INIS)

    Prudnikov, P. V.; Prudnikov, V. V.; Nosikhin, E. A.

    2008-01-01

    The effect of structural defects on the critical ultrasound absorption and ultrasound velocity dispersion in Ising-like three-dimensional systems is studied. A field-theoretical description of the dynamic effects of acoustic-wave propagation in solids during phase transitions is performed with allowance for both fluctuation and relaxation absorption mechanisms. The temperature and frequency dependences of the scaling functions of the absorption coefficient and the ultrasound velocity dispersion are calculated in a two-loop approximation for homogeneous and structurally disordered systems, and their asymptotic behavior in hydrodynamic and critical regions is separated. As compared to a homogeneous system, the presence of structural defects in it is shown to cause a stronger increase in the sound absorption coefficient and the sound velocity dispersion even in the hydrodynamic region as the critical temperature is reached. As compared to homogeneous analogs, structurally disordered systems should exhibit stronger temperature and frequency dependences of the acoustic characteristics in the critical region

  8. Separation and Purification of Sulforaphane from Broccoli by Solid Phase Extraction

    Directory of Open Access Journals (Sweden)

    Kyung Ho Row

    2011-03-01

    Full Text Available A simple solid-phase extraction (SPE method for the determination of sulforaphane in broccoli has been developed. The optimal conditions were found to be use of a silica SPE cartridge, and ethyl acetate and dichloromethane as washing and eluting solvents, respectively, which could eliminate interferences originating from the broccoli matrix. The extracts were sufficiently clean to be directly injected into high-performance liquid chromatography (HPLC for further chromatographic analysis. Good linearity was obtained from 0.05 to 200 μg/mL (r = 0.998 for sulforaphane with the relative standard deviations less than 3.6%. The mean recoveries of sulforaphane from broccoli were more than 90.8% and the detection limit (S/N = 3:1 was 0.02 μg/mL. The SPE method provides a higher yield of sulforaphane from crude extracts compared to conventional liquid-liquid extraction.

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

    Science.gov (United States)

    Mills, G A; Walker, V

    2000-12-01

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

  10. Automated Chemical Solid-Phase Synthesis and Deprotection of 5-Hydroxymethylcytosine-Containing RNA.

    Science.gov (United States)

    Riml, Christian; Micura, Ronald

    2017-01-01

    5-Hydroxymethylcytosine is an epigenetic base modification that is part of the demethylation pathway of 5-methylcytosine in DNA. 5-Methylcytosine is iteratively oxidized to 5-hydroxymethylcytosine, 5-formylcytosine, and 5-carboxycytosine by enzymes of the TET protein family. Since the discovery of 5-hydroxymethylcytosine also in RNA its role in regulatory processes and metabolism remains elusive. To gain more insight into the function of RNA containing 5-hydroxymethylcytidine, innovative and interdisciplinary approaches are required. In this context, synthetic oligoribonucleotides containing 5-hyroxymethylcytidine are an inevitable tool. Therefore, in this chapter, we present the efficient synthesis of RNA oligonucleotides containing 5-hydroxymethylcytosine by solid-phase synthesis. The incorporation of the modified cytosine derivative into RNA is compatible with standard phosphoramidite-based synthesis procedures of oligoribonucleotides.

  11. Use of a PKZh-902 instrument for monitoring solid phases in an organic coolant

    International Nuclear Information System (INIS)

    Gavrillin, A.I.; Gagarin, S.I.; Sokolov, V.E.; Zabelin, A.I.

    1986-01-01

    Preliminary tests have been performed with a PKZh-902 in checking feed and circulating coolant, and also in evaluating the performance of the cleaning devices. The test program involved determining the stability of the esnsor materials in ditolymethane, examining the effects of radioactive products and those of the optical characteristics of impurities in the first-loop coolant on the readings and errors of measurement, and checking the scope for using the instrument for continuous monitoring of particle concentrations. Results confirm that the PKZh-902 enables one to monitor the composition and concentration of the solid dispersed phase reliably and with adequate accuracy in the feed coolant. The use for monitoring the loop coolant requires additonal research

  12. Process for preparation of a solid-phase radioimmunoassay support and use thereof

    International Nuclear Information System (INIS)

    Meriadec, B.; Roubertie, P.

    1979-01-01

    A process is described for the preparation of a support useful in radioimmunoassay chromatographic columns. The process involves the preparation of a chromatographic gel capable of selectively retaining one or more components contained in an antigen-antibody-containing solution. The gel is bound to the appropriate antiserum, then freeze-dried, pulverized and compressed into a tablet. The tablet support swells upon contact with an antigen-antibody-containing solution to conform to the shape of the columns. An example of the application of this support in the radioimmunoassay of thyroid-stimulating hormone is described. This type of support is also particularly useful in second antibody solid phase radioimmunoassays since there is no limit to the size of the antigen to which this technology may be applied. (U.K.)

  13. Headspace Solid-Phase Microextraction Analysis of Volatile Components in Phalaenopsis Nobby’s Pacific Sunset

    Directory of Open Access Journals (Sweden)

    Chih-Hsin Yeh

    2014-09-01

    Full Text Available Phalaenopsis is the most important economic crop in the Orchidaceae family. There are currently numerous beautiful and colorful Phalaenopsis flowers, but only a few species of Phalaenopsis have an aroma. This study reports the analysis volatile components present in P. Nobby’s Pacific Sunset by solid-phase microextraction (SPME coupled with gas chromatography (GC and gas chromatography/mass spectrometry (GC-MS. The results show that the optimal extraction conditions were obtained by using a DVB/CAR/PDMS fiber. A total of 31 compounds were identified, with the major compounds being geraniol, linalool and α-farnesene. P. Nobby’s Pacific Sunset had the highest odor concentration from 09:00 to 13:00 on the eighth day of storage. It was also found that in P. Nobby’s Pacific Sunset orchids the dorsal sepals and petals had the highest odor concentrations, whereas the column had the lowest.

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

    Directory of Open Access Journals (Sweden)

    Ashraf Yehia El-Naggar

    2013-01-01

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

  15. Lanthanide-Mediated Dephosphorylation Used for Peptide Cleavage during Solid Phase Peptide Synthesis

    Directory of Open Access Journals (Sweden)

    Byunghee Yoo

    2013-04-01

    Full Text Available Lanthanide(III ions can accelerate the hydrolysis of phosphomonoesters and phosphodiesters in neutral aqueous solution. In this paper, lanthanide-mediated dephosphorylation has been applied in aqueous media as an orthogonal cleavage condition that can be employed in conventional solid phase peptide synthesis (SPPS. A phosphorylated polymeric support for SPPS was developed using Boc chemistry. The cleavage of resin-bound phosphates was investigated with the addition of Eu(III, Yb(III, acid or base, a mixture of solvents or different temperatures. To demonstrate the utility of this approach for SPPS, a peptide sequence was synthesized on a phosphorylated polymeric support and quantitatively cleaved with lanthanide ions in neutral aqueous media. The protecting groups for side chains were retained during peptide cleavage using lanthanide ions. This new methodology provides a mild orthogonal cleavage condition of phosphoester as a linker during SPPS.

  16. Thermodynamic and kinetic analysis of solid-phase interaction of alkali metal carbonates with arsenic pentoxide

    International Nuclear Information System (INIS)

    Pashinkin, A.S.; Buketov, E.A.; Isabaeva, S.M.; Kasenov, B.K.

    1985-01-01

    The thermodynamic analysis of solid-phase reactions of alkali metal carbonates with arsenic pentoxide showing the possibility of formation of all arsenates at a higher than the room temperature is performed. Energetically most advantageous is formation of meta-arsenates. It is shown that temperature increase favours the reaction process. By Gibbs standard energy decrease the reactions form the Li>Na>K>Rb>Cs series. On the base of calculation data linear dependence of Gibbs standard energy in reactions on the atomic number of alkali metalis established. By the continuous weighing method the kinetics of interaction of alkali metal carbonates with arsenic pentoxide under isothermal conditions in the 450-500 deg C range is studied. Studies is the dependence of apparent energy of interaction of carbonates wih As 2 0 5 an atomic parameters of al

  17. Numerical Simulations of Liquid-Gas-Solid Three-Phase Flows in Microgravity

    Directory of Open Access Journals (Sweden)

    Xinyu Zhang

    2012-03-01

    Full Text Available Three-phase liquid-gas-solid flows under microgravity condition are studied. An Eulerian-Lagrangian computational model was developed and used in the simulations. In this approach, the liquid flow was modeled by a volume-averaged system of governing equations, whereas motions of particles and bubbles were evaluated using the Lagrangian trajectory analysis procedure. It was assumed that the bubbles remained spherical, and their shape variations were neglected. The bubble-liquid, particle-liquid and bubbl-particle two-way interactions were accounted for in the analysis. The discrete phase equations used included drag, lift, buoyancy, and virtual mass forces. Particle-particle interactions and bubble-bubble interactions were accounted for by the hard sphere model. Bubble coalescence was also included in the model. The transient flow characteristics of the three-phase flow were studied; and the effects of gravity, inlet bubble size and g-jitter acceleration on variation of flow characteristics were discussed. The low gravity simulations showed that most bubbles are aggregated in the inlet region. Also, under microgravity condition, bubble transient time is much longer than that in normal gravity. As a result, the Sauter mean bubble diameter, which is proportional to the transient time of the bubble, becomes rather large, reaching to more than 9 mm. The bubble plume in microgravity exhibits a plug type flow behavior. After the bubble plume reaches the free surface, particle volume fraction increases along the height of the column. The particles are mainly located outside the bubble plume, with very few particles being retained in the plume. In contrast to the normal gravity condition, the three phases in the column are poorly mixed under microgravity conditions. The velocities of the three phases were also found to be of the same order. Bubble size significantly affects the characteristics of the three-phase flows under microgravity conditions. For

  18. Identification of Solid Phases in Saltcake from Hanford Site Waste Tanks

    Energy Technology Data Exchange (ETDEWEB)

    HERTING, D L; COOKE, G A

    2002-09-26

    One of the primary tasks in the clean up of the Hanford Reservation is the retrieval of waste from single-shell and double-shell storage tanks. The waste will be used as feedstock for the vitrification plant under construction in the Hanford 200 East area. To accomplish this tank waste retrieval, the River Protection Project requires physical and chemical data on the nature of the wastes. For several years, laboratory tests have been conducted at the 222-S Laboratory on the dissolution characteristics of Hanford saltcake waste from single shell tanks (Herting 1998, 1999, 2000,2001). The bulk physical and chemical data determined during these studies has provided valuable input for evaluating the Environmental Simulation Program produced by OLI Systems, Inc. of Moms Plains, New Jersey. This computer program is used by the River Protection Project to predict chemical solubility during dilution and retrieval of tank wastes. The characterization of solid phases found in saltcake undergoing dissolution and evaporative concentration is an important adjunct to the bulk physical and chemical properties of the saltcake waste. The phase analysis of Tank BY-109' saltcake, described in this report, was conducted using polarized light microscopy (PLM), X-Ray diffraction (XRD) and scanning electron microscopy (SEM). The phases Na{sub 7}F(PO{sub 4}){sub 2} {center_dot} 19H{sub 2}O, Na{sub 3}FSO{sub 4}, Na{sub 2}C{sub 2}O{sub 4} and NaF were identified in BY-IO9 saltcake by all three instruments, while Na{sub 3}AlF{sub 6} was observed in XRD and SEM analyses. In addition, the SEM found significant amounts of a fine-grained aluminum-rich phase, frequently associated with lesser amounts of chromium and sodium. PLM noted the presence of a fine-grained agglomerated phase that was probably this aluminum-rich phase, and XRD confirmed the presence of an aluminum hydroxide, bayerite, in one sample. Finally, the SEM located a number of discrete particles of an aluminosilicate phase

  19. Solid Phase Extraction for Monitoring of Occupational Exposure to Cr (III

    Directory of Open Access Journals (Sweden)

    S.J. Shahtaheri

    2007-01-01

    Full Text Available Chromium is an important constituent widely used in different industrial processes for production of various synthetic materials. For evaluation of workers’ exposure to trace toxic metal of Cr (III, environmental and biological monitoring are essential processes, in which, preparation of samples is one of the most time-consuming and error-prone aspects prior to analysis. The use of solid-phase extraction (SPE has grown and is a fertile technique of sample preparation as it provides better results than those produced by liquid-liquid extraction (LLE. SPE using mini columns filled with XAD-4 resin was optimized regarding to sample pH, ligand concentration, loading flow rate, elution solvent, sample volume, elution volume, amount of resins, and sample matrix interferences. Chromium was retained on solid sorbent and was eluted with 2 M HNO3 followed by simple determination of analytes by using flame atomic absorption spectrometery. Obtained recoveries of metal ion were more than 92%. The optimized procedure was also validated with three different pools of spiked urine samples and showed a good reproducibility over six consecutive days as well as six within-day experiments. Through this study, suitable results were obtained for relative standard deviation, therefore, it is concluded that, this optimized method can be considered to be successful in simplifying sample preparation for trace residue analysis of Cr in different matrices for evaluation of occupational and environmental exposures. To evaluate occupational exposure to chromium, 16 urine samples were taken, prepared, and analyzed based on optimized procedure.

  20. Study of the Hall effect in gallium and indium arsenides in solid and liquid phases

    International Nuclear Information System (INIS)

    Glazov, V.M.; Kol'tsov, V.B.; Sulejmanov, I.R.

    1985-01-01

    Hall effect in gallium and indium arsenides in solid and liquid state is investigated within the framework of a united experiment for the first time. As a result the Hall constant change in the course of these compounds melting is determined experimentally, and on the basis of data obtained and using well-known hopping electric conductivity values, changes of charge carrier density and mobility are estimated. The observed differences in the jumps of pointed characteristics in the course of melting of GaAs compounds on the one hand and InAs - on the other are explained by behaviour peculiarities of the latter in a solid phase dose to the melting temperature. Data on Hall effect in GaAs and InAs melts is abtaned for the first time. Thermal width values of forbidden zone of A 3 As compound calculated on the basis of Hall measurements, conform well with assessment results on the basis of data on electric conductivity

  1. Multiple headspace-solid-phase microextraction: an application to quantification of mushroom volatiles.

    Science.gov (United States)

    Costa, Rosaria; Tedone, Laura; De Grazia, Selenia; Dugo, Paola; Mondello, Luigi

    2013-04-03

    Multiple headspace-solid phase microextraction (MHS-SPME) followed by gas chromatography/mass spectrometry (GC-MS) and flame ionization detection (GC-FID) was applied to the identification and quantification of volatiles released by the mushroom Agaricus bisporus, also known as champignon. MHS-SPME allows to perform quantitative analysis of volatiles from solid matrices, free of matrix interferences. Samples analyzed were fresh mushrooms (chopped and homogenized) and mushroom-containing food dressings. 1-Octen-3-ol, 3-octanol, 3-octanone, 1-octen-3-one and benzaldehyde were common constituents of the samples analyzed. Method performance has been tested through the evaluation of limit of detection (LoD, range 0.033-0.078 ng), limit of quantification (LoQ, range 0.111-0.259 ng) and analyte recovery (92.3-108.5%). The results obtained showed quantitative differences among the samples, which can be attributed to critical factors, such as the degree of cell damage upon sample preparation, that are here discussed. Considerations on the mushrooms biochemistry and on the basic principles of MHS analysis are also presented. Copyright © 2013 Elsevier B.V. All rights reserved.

  2. Flame Retardancy of Sorbitol Based Bioepoxy via Combined Solid and Gas Phase Action

    Directory of Open Access Journals (Sweden)

    Beáta Szolnoki

    2016-08-01

    Full Text Available Flame-retarded bioepoxy resins were prepared with the application of commercially available sorbitol polyglycidyl ether (SPE. The additive-type flame retardancy of the cycloaliphatic amine-cured SPE was investigated. Three-percent phosphorus (P-containing samples were prepared with the application of the liquid resorcinol bis(diphenyl phosphate (RDP, the solid ammonium polyphosphate (APP, and by combining them. Synergistic effect was found between the inorganic APP and the organophosphorus RDP, when applied in combination: formulations applying RDP or APP alone showed increased limiting oxygen index (LOI values, however, their UL-94 standard ratings remained HB. When the same amount of P originated from the two additives, V-0, self-extinguishing rating and LOI value of 34% (v/v was reached. By the combined approach the heat release rate of SPE could be lowered by approximately 60%. The assumed balanced solid and gas phase mechanism was confirmed by thermogravimetric analysis, Fourier transform infrared spectrometry (FTIR analysis (of the gases formed during laser pyrolysis, attenuated total reflection-infrared spectrometry (ATR-IR analysis (of the charred residues, as well as by mechanical testing (of the char obtained after combustion.

  3. Multiscreening determination of organic pollutants in molluscs using matrix solid phase dispersion.

    Science.gov (United States)

    Ziarrusta, H; Olivares, M; Delgado, A; Posada-Ureta, O; Zuloaga, O; Etxebarria, N

    2015-04-24

    This work describes the optimisation, validation and application of matrix solid-phase dispersion (MSPD) coupled to gas chromatography mass spectrometry, both single quadrupole (GC-MS) and tandem (GC-MS/MS), for the quantification in molluscs of up to 40 different analytes belonging to several families of priority and emerging organic contaminants, including polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), polybrominated diphenyl ethers (PBDEs), organochlorine pesticides (OCPs), organophosphorus pesticides (OPPs) and musk fragrances. The MSPD procedure was fully optimised with a special focus on the clean-up strategy. The best recoveries were obtained using glass syringes, 0.30 g of freeze-dried sample, 0.30 g of Florisil as solid support, 4.00 g of activated silica and 25 mL of dichloromethane as elution solvent. Using GC-MS/MS the method afforded good linearities (r(2), between 0.980 and 0.9996), adequate repeatability and reproducibility (RSDmollusc species collected in Colombia and Nicaragua, where PAHs, PCBs, musks and pesticides were detected at low ng g(-1) levels. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. Combinatorial Libraries on Rigid Scaffolds: Solid Phase Synthesis of Variably Substituted Pyrazoles and Isoxazoles

    Directory of Open Access Journals (Sweden)

    Eduard R. Felder

    1997-01-01

    Full Text Available The synthesis of combinatorial compound libraries has become a powerful lead finding tool in modern drug discovery. The ability to synthesize rapidly, in high yield, new chemical entities with low molecular weight on a solid support has a recognized strategic relevance (“small molecule libraries”. We designed and validated a novel solid phase synthesis scheme, suitable to generate diversity on small heterocycles of the pyrazole and isoxazole type. Appropriate conditions were worked out for each reaction, and a variety of more or less reactive agents (building blocks was utilized for discrete conversions, in order to exploit the system’s breadth of applicability. Four sequential reaction steps were validated, including the loading of the support with an acetyl bearing moiety, a Claisen condensation, an a-alkylation and a cyclization of a b-diketone with monosubstituted hydrazines. In a second stage, the reaction sequence was applied in a split and mix approach, in order to prepare a combinatorial library built-up from 4 acetyl carboxylic acids (R1, 35 carboxylic esters (R2 and 41 hydrazines (R4 (and 1 hydroxylamine to yield a total of 11,760 compounds divided into 41 pyrazole sublibraries with 140 pairs of regioisomers and 1 isoxazole sublibrary of equal size.

  5. Determination of Atrazine, Acetochlor, Clomazone, Pendimethalin and Oxyfluorfen in Soil by a Solid Phase Microextraction Method

    Directory of Open Access Journals (Sweden)

    Rada Đurović

    2008-01-01

    Full Text Available A solid phase microextraction (SPME method for simultaneous determination of atrazine, acetochlor, clomazone, pendimethalin and oxyfluorfen in soil samples was developed. The method is based on a combination of conventional liquid-solid procedure and a following SPME determination of the selected pesticides. Initially, various microextraction conditions, such as the fibre type, desorption temperature and time, extraction time and NaCl content, were investigated and optimized. Then, extraction efficiencies of severalsolvents (water, hexane, acetonitrile, acetone and methanol and the optimum number of extraction steps within the sample preparation step were optimized. According to the results obtained in these two sets of experiments, two successive extractions with methanol as the extraction solvent were the optimal sample preparation procedure, while the following conditions were found to be most efficient for SPME measurements: 100 μm PDMS fibre, desorption for 7 min at 2700C, 30 min extraction time and 5% NaCl content (w/v. Detection and quantification were done by gas chromatography-mass spectrometry(GC/MS. Relative standard deviation (RSD values for multiple analysis of soil samples fortified at 30 μg/kg of each pesticide were below 19%. Limits of detection (LOD for all the compounds studied were less than 2 μg/kg.

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

    Science.gov (United States)

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

    2007-01-01

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

  7. Probing the liquid and solid phases in closely spaced two-dimensional systems

    International Nuclear Information System (INIS)

    Zhang, Ding

    2014-01-01

    Gas, liquid and solid phases are the most common states of matter in our daily encountered 3-dimensional space. The school example is the H 2 O molecule with its phases vapor, water and ice. Interestingly, electrons - with their point-like nature and negative charges - can also organize themselves under certain conditions to bear properties of these three common phases. At relatively high temperature, where Boltzmann statistics prevails, the ensemble of electrons without interactions can be treated as a gas of free particles. Cooling down the system, this electron gas condenses into a Fermi liquid. Finally, as a result of the repulsive Coulomb forces, electrons try to avoid each other by maximizing their distances. When the Coulomb interaction becomes sufficiently strong, a regular lattice emerges - an electron solid. The story however does not end here. Nature has much more in store for us. Electronic systems in fact exhibit a large variety of phases induced by spatial confinement, an external magnetic field, Coulomb interactions, or interactions involving degrees of freedom other than charge such as spin and valley. Here in this thesis, we restrict ourselves to the study of electrons in a 2-dimenisonal (2D) plane. Already in such a 2D electron system (2DES), several distinct states of matter appear: integer and fractional quantum Hall liquids, the 2D Wigner solid, stripe and bubble phases etc. In 2DES it is sufficient to sweep the perpendicular magnetic field to pass from one of these phases into another. Experimentally, many of these phases can be revealed by simply measuring the resistance. For a quantum Hall state, the longitudinal resistance vanishes, while the Hall resistance exhibits a plateau. The quantum Hall plateau is a manifestation of localization induced by the inevitable sample disorder. Coulomb interaction can also play an important role to localize charges. Even in the disorder-free case, electrons - more precisely quasi-particles in the partially

  8. Phase I study of the Hedgehog pathway inhibitor IPI-926 in adult patients with solid tumors.

    Science.gov (United States)

    Jimeno, Antonio; Weiss, Glen J; Miller, Wilson H; Gettinger, Scott; Eigl, Bernard J C; Chang, Anne Lynne S; Dunbar, Joi; Devens, Shannon; Faia, Kerrie; Skliris, Georgios; Kutok, Jeff; Lewis, Karl D; Tibes, Raoul; Sharfman, William H; Ross, Robert W; Rudin, Charles M

    2013-05-15

    To conduct a first-in-human phase I study to determine the dose-limiting toxicities (DLT), characterize the pharmacokinetic profile, and document the antitumor activity of IPI-926, a new chemical entity that inhibits the Hedgehog pathway (HhP). Patients with solid tumors refractory to standard therapy were given IPI-926 once daily (QD) by mouth in 28-day cycles. The starting dose was 20 mg, and an accelerated titration schedule was used until standard 3 + 3 dose-escalation cohorts were implemented. Pharmacokinetics were evaluated on day -7 and day 22 of cycle 1. Ninety-four patients (32F, 62M; ages, 39-87) received doses ranging from 20 to 210 mg QD. Dose levels up to and including 160 mg administered QD were well tolerated. Toxicities consisted of reversible elevations in aspartate aminotransferase (AST), alanine aminotransferase (ALT) and bilirubin, fatigue, nausea, alopecia, and muscle spasms. IPI-926 was not associated with hematologic toxicity. IPI-926 pharmacokinetics were characterized by a slow absorption (T(max) = 2-8 hours) and a terminal half-life (t(1/2)) between 20 and 40 hours, supporting QD dosing. Of those HhP inhibitor-naïve patients with basal cell carcinoma (BCC) who received more than one dose of IPI-926 and had a follow-up clinical or Response Evaluation Criteria in Solid Tumors (RECIST) assessment, nearly a third (8 of 28 patients) showed a response to IPI-926 at doses ≥130 mg. IPI-926 was well tolerated up to 160 mg QD within 28-day cycles, which was established as the recommended phase II dose and schedule for this agent. Single-agent activity of IPI-926 was observed in HhP inhibitor-naïve patients with BCC. ©2013 AACR

  9. A phase 1 study of oral ridaforolimus in pediatric patients with advanced solid tumors.

    Science.gov (United States)

    Pearson, Andrew D J; Federico, Sara M; Aerts, Isabelle; Hargrave, Darren R; DuBois, Steven G; Iannone, Robert; Geschwindt, Ryan D; Wang, Ruixue; Haluska, Frank G; Trippett, Tanya M; Geoerger, Birgit

    2016-12-20

    Ridaforolimus is an investigational, potent, selective mTOR inhibitor. This study was conducted to determine the recommended phase 2 dose (RP2D), maximum tolerated dose, safety, pharmacokinetics, and antitumor activity of oral ridaforolimus in children with advanced solid tumors. In this phase 1, multicenter, open-label study in children aged 6 to orally for 5 consecutive days/week in 28-day cycles until progression, unacceptable toxicity, or consent withdrawal. Dose started at 22 mg/m2 and increased to 28 mg/m2 and 33 mg/m2, followed by expansion at the RP2D. Twenty patients were treated; 18 were evaluable for dose-limiting toxicities. One dose-limiting toxicity (grade 3 increased alanine aminotransferase) occurred in 1 patient at 33 mg/m2. Dose escalation concluded at 33 mg/m2; the maximum tolerated dose was not determined. The most common treatment-related adverse events (frequency ≥40%) were manageable grade 1-2 stomatitis, thrombocytopenia, hypertriglyceridemia, increased alanine aminotransferase, fatigue, hypercholesterolemia, anemia, and increased aspartate aminotransferase. Ridaforolimus exposure at 28 mg/m2 and 33 mg/m2 exceeded adult target levels. The RP2D for oral ridaforolimus in children was defined as 33 mg/m2. Four patients received at least 4 cycles; 2 with pineoblastoma and diffuse intrinsic pontine glioma had stable disease for 12 and 46 cycles, respectively. Ridaforolimus is orally bioavailable and well tolerated in children with advanced solid tumors. The RP2D (33 mg/m2, 5 days/week) exceeds the adult RP2D. The favorable toxicity and pharmacokinetic profiles may allow for combination therapy, a promising therapeutic option in pediatric malignancies.

  10. Sample preparation with solid phase microextraction and exhaustive extraction approaches: Comparison for challenging cases.

    Science.gov (United States)

    Boyacı, Ezel; Rodríguez-Lafuente, Ángel; Gorynski, Krzysztof; Mirnaghi, Fatemeh; Souza-Silva, Érica A; Hein, Dietmar; Pawliszyn, Janusz

    2015-05-11

    In chemical analysis, sample preparation is frequently considered the bottleneck of the entire analytical method. The success of the final method strongly depends on understanding the entire process of analysis of a particular type of analyte in a sample, namely: the physicochemical properties of the analytes (solubility, volatility, polarity etc.), the environmental conditions, and the matrix components of the sample. Various sample preparation strategies have been developed based on exhaustive or non-exhaustive extraction of analytes from matrices. Undoubtedly, amongst all sample preparation approaches, liquid extraction, including liquid-liquid (LLE) and solid phase extraction (SPE), are the most well-known, widely used, and commonly accepted methods by many international organizations and accredited laboratories. Both methods are well documented and there are many well defined procedures, which make them, at first sight, the methods of choice. However, many challenging tasks, such as complex matrix applications, on-site and in vivo applications, and determination of matrix-bound and free concentrations of analytes, are not easily attainable with these classical approaches for sample preparation. In the last two decades, the introduction of solid phase microextraction (SPME) has brought significant progress in the sample preparation area by facilitating on-site and in vivo applications, time weighted average (TWA) and instantaneous concentration determinations. Recently introduced matrix compatible coatings for SPME facilitate direct extraction from complex matrices and fill the gap in direct sampling from challenging matrices. Following introduction of SPME, numerous other microextraction approaches evolved to address limitations of the above mentioned techniques. There is not a single method that can be considered as a universal solution for sample preparation. This review aims to show the main advantages and limitations of the above mentioned sample

  11. Combined liquid and solid-phase extraction improves quantification of brain estrogen content

    Directory of Open Access Journals (Sweden)

    Andrew eChao

    2011-09-01

    Full Text Available Accuracy in quantifying brain-derived steroid hormones (‘neurosteroids’ has become increasingly important for understanding the modulation of neuronal activity, development, and physiology. Relative to other neuroactive compounds and classical neurotransmitters, steroids pose particular challenges with regard to isolation and analysis, owing to their lipid solubility. Consequently, anatomical studies of the distribution of neurosteroids have relied primarily on the expression of neurosteroid synthesis enzymes. To evaluate the distribution of synthesis enzymes vis-à-vis the actual steroids themselves, traditional steroid quantification assays, including radioimmunoassays (RIA, have successfully employed liquid extraction methods (e.g., ether, dichloromethane or methanol to isolate steroids from microdissected brain tissue. Due to their sensitivity, safety and reliability, the use of commercial enzyme immunoassays (EIA for laboratory quantification of steroids in plasma and brain has become increasingly widespread. However, EIAs rely on enzymatic reactions in vitro, making them sensitive to interfering substances in brain tissue and thus producing unreliable results. Here, we evaluate the effectiveness of a protocol for combined, two-stage liquid/solid phase extraction as compared to conventional liquid extraction alone for the isolation of estradiol (E2 from brain tissue. We employ the songbird model system, in which brain steroid production is pronounced and linked to neural mechanisms of learning and plasticity. This study outlines a combined liquid-solid phase extraction protocol that improves the performance of a commercial EIA for the quantification of brain E2 content. We demonstrate the effectiveness of our optimized method for evaluating the region specificity of brain E2 content, compare these results to established anatomy of the estrogen synthesis enzyme and estrogen receptor, and discuss the nature of potential EIA interfering

  12. Isolation/separation of plasmid DNA using hemoglobin modified magnetic nanocomposites as solid-phase adsorbent.

    Science.gov (United States)

    Chen, Xu-Wei; Mao, Quan-Xing; Liu, Jia-Wei; Wang, Jian-Hua

    2012-10-15

    Hemoglobin (Hb) modified magnetic nanocomposites are prepared by immobilization of Hb onto the surface of amino-functionalized Fe(3)O(4)@SiO(2) magnetic nanoparticles via covalent bonding with glutaraldehyde as cross-linker. The obtained nanocomposites are characterized with FT-IR, SEM, XRD and surface charge analysis. A direct solid-phase extraction procedure for the isolation/separation of plasmid DNA using this nanocomposite as a novel adsorbent is thus developed. Some important experimental parameters governing the sorption efficiency, i.e., the pH of sample solution and the ionic strength, are investigated. The Hb modified magnetic nanocomposites provide a sorption capacity of 27.86 mg g(-1) for DNA. By using 2.0mg of the nanocomposites as sorption medium and a suitable acidity of pH 6.1, a sorption efficiency of 93% is achieved for 25 μg mL(-1) of DNA in 1.0 mL of sample solution. Afterwards, the absorbed DNA could be readily recovered by using 1.0 mL of Tris-HCl buffer (pH 8.9, 0.01 mol L(-1)), giving rise to a recovery of ca. 68.3%. The present solid-phased extraction protocol is applied for the isolation of plasmid DNA from Escherichia coli culture, resulting in comparable yield and purity of plasmid DNA with respect to those obtained by using commercial kits. Copyright © 2012 Elsevier B.V. All rights reserved.

  13. Poly(Dimethylsiloxane)-Poly(Vinyl Alcohol) Coated Solid Phase Micro extraction Fiber for Chloropyrifos Analysis

    International Nuclear Information System (INIS)

    Wan Aini Wan Ibrahim; Nor Fairul Zukry Ahmad Rasdy; Norfazilah Muhamad

    2016-01-01

    Traditional liquid - liquid extraction of pesticides consumes large volumes of organic solvent which are hazardous to the operator and is not environment friendly. Solid phase micro extraction (SPME) is a solvent less extraction method which is safer to the operator and is environmental friendly. A sol-gel hybrid fibre coating material, poly(dimethylsiloxane)-poly(vinyl alcohol) (PDMS-PVA) was synthesized and used in head space solid phase micro extraction (HS-SPME) of chloropyrifos. The thickness of the synthesised PDMS-PVA fiber coating was 13.5 μm and it is thermally stable up to 400 degree Celsius. The PDMS-PVA sol-gel hybrid fiber was also stable to two organic solvents tested; acetonitrile and dichloromethane (1 hour dipping) and showed no significant changes in extraction performance for chloropyrifos. Extracted chloropyrifos was analysed using gas chromatography electron capture detector (GC-ECD). Optimum SPME parameters affecting the PDMS-PVA HS-SPME performance namely extraction time (15 min), extraction temperature (50 degree Celsius), desorption time (5 min), desorption temperature (260 degree Celsius) and stirring rate (120 rpm) were used for extraction. It was found that HSSPME using PDMS-PVA sol-gel fiber gave significantly better extraction performance of chloropyrifos compared to commercial 100 μm PDMS fiber. The PDMS-PVA fiber showed excellent operational performances such as temperature stability (up to 380 degree Celsius), coating lifetime (up to 170 times use) and organic solvent stability. The PDMS-PVA-HS-SPME method showed excellent recovery for chloropyrifos from tomatoes (98.0 %, 5.9 % RSD) at 0.01 μg/ g spiked level (5 times lower than maximum residue limit set by European Union). (author)

  14. Cold fiber solid-phase microextraction device based on thermoelectric cooling of metal fiber.

    Science.gov (United States)

    Haddadi, Shokouh Hosseinzadeh; Pawliszyn, Janusz

    2009-04-03

    A new cold fiber solid-phase microextraction device was designed and constructed based on thermoelectric cooling. A three-stage thermoelectric cooler (TEC) was used for cooling a copper rod coated with a poly(dimethylsiloxane) (PDMS) hollow fiber, which served as the solid-phase microextraction (SPME) fiber. The copper rod was mounted on a commercial SPME plunger and exposed to the cold surface of the TEC, which was enclosed in a small aluminum box. A heat sink and a fan were used to dissipate the generated heat at the hot side of the TEC. By applying an appropriate dc voltage to the TEC, the upper part of the copper rod, which was in contact to the cold side of the TEC, was cooled and the hollow fiber reached a lower temperature through heat transfer. A thermocouple was embedded in the cold side of the TEC for indirect measurement of the fiber temperature. The device was applied in quantitative analysis of off-flavors in a rice sample. Hexanal, nonanal, and undecanal were chosen as three off-flavors in rice. They were identified according to their retention times and analyzed by GC-flame ionization detection instrument. Headspace extraction conditions (i.e., temperature and time) were optimized. Standard addition calibration graphs were obtained at the optimized conditions and the concentrations of the three analytes were calculated. The concentration of hexanal was also measured using a conventional solvent extraction method (697+/-143ng/g) which was comparable to that obtained from the cold fiber SPME method (644+/-8). Moreover, the cold fiber SPME resulted in better reproducibility and shorter analysis time. Cold fiber SPME with TEC device can also be used as a portable device for field sampling.

  15. Environmentally Friendly Method: Development and Application to Carbon Aerogel as Sorbent for Solid-Phase Extraction.

    Science.gov (United States)

    Dong, Sheying; Huang, Guiqi; Su, Meiling; Huang, Tinglin

    2015-10-14

    We developed two simple, fast, and environmentally friendly methods using carbon aerogel (CA) and magnetic CA (mCA) materials as sorbents for micro-solid-phase extraction (μ-SPE) and magnetic solid-phase extraction (MSPE) techniques. The material performances such as adsorption isotherm, adsorption kinetics, and specific surface area were discussed by N2 adsorption-desorption isotherm measurements, ultraviolet and visible (UV-vis) spectrophotometry, scanning electron microscopy (SEM), and high resolution transmission electron microscopy (HR-TEM). The experimental results proved that the heterogeneities of CA and mCA were well modeled with the Freundlich isotherm model, and the sorption process well followed the pseudo-second-order rate equation. Moreover, plant growth regulators (PGRs) such as kinetin (6-KT), 6-benzylaminopurine (6-BA), 2,4-dichlorophenoxyacetic acid (2,4-D), and uniconazole (UN) in a reservoir raw water sample were selected as the evaluation of applicability for the proposed μ-SPE and MSPE techniques using high performance liquid chromatography (HPLC). The experimental conditions of two methods such as the amount of sorbent, extraction time, pH, salt concentration, and desorption conditions were studied. Under the optimized conditions, two extraction methods provided high recoveries (89-103%), low the limits of detection (LODs) (0.01-0.2 μg L(-1)), and satisfactory analytical features in terms of precision (relative standard deviation, RSD, 1.7-5.1%, n=3). This work demonstrates the feasibility and the potential of CA and mCA materials as sorbents for μ-SPE and MSPE techniques. Besides, it also could serve as a basis for future development of other functional CAs in pretreatment technology and make them valuable for analysis of pollutants in environmental applications.

  16. Principles and applications of colorimetric solid-phase extraction with negligible depletion

    International Nuclear Information System (INIS)

    Dias, Neil C.; Porter, Marc D.; Fritz, James S.

    2006-01-01

    Colorimetric solid-phase extraction (C-SPE) is an integrated technique in which an analyte is selectively concentrated onto a disk and then quantitated by diffuse reflectance spectroscopy. This paper describes the results of an investigation that applies the concept of negligible depletion (ND) to C-SPE, representing the first application of ND concepts to solid-phase extractions. The approach relies on passing the minimal volume of sample through the disk required to reach an equilibrium in which the concentration of analyte in the sample entering and exiting the disk are equal. At this point, the amount of analyte extracted by the disk is proportional to the sample concentration but is independent of the sample volume passed through the disk. With this new method, called C-SPE/ND, the precise measurement of sample volume is no longer necessary. The work herein details the general principles of this new methodology, and validates its basic tenets in an investigation of the extraction of the organic dye methyl violet. The analytical capabilities of C-SPE/ND are then demonstrated by its application to measurements of iodine. Iodine is a biocide increasingly used as a simple and effective disinfectant for water in locations where municipal water treatment systems are potentially compromised. Thus, the ability to operate C-SPE in an ND mode notably enhances the broad-based utility of this methodology as a reliable and an easy-to-use analysis tool for water quality assessments. Since iodine is also the biocide used on NASAs Space Shuttle, C-SPE/ND has the potential to overcome problems associated with the removal of air bubbles entrapped in a water sample in the microgravity environment encountered in space exploration. Extensions of C-SPE/ND to facile determinations of other water quality parameters with respect to both earth- and space-based needs are briefly discussed

  17. Synthesis of Orthogonally Protected Muramic Acid Building Blocks for Solid Phase Peptide Synthesis

    Directory of Open Access Journals (Sweden)

    Kristina Vlahoviček-Kahlina

    2015-07-01

    Full Text Available Muramic acid is found in many peptide natural products containing oligo(polysaccharide moieties. Taking into consideration that the Fmoc methodology is routinely used for solid-phase peptide synthesis, preparation of orthogonally protected muramic acid building blocks for total solid-phase synthesis of these natural products is of particular practical importance. Herein a simple and efficient synthesis of benzyl 2-amino-4,6-O-benzylidene-3-O-[(R-1-carboxyethyl]-2-deoxy-N-9-fluorenylmethyloxycarbonyl-α-D-glucopyranoside (6 from N-acetylglucosamine (1 is described. Important improvements over previous synthetic approaches to glucopyranosides 2 (benzyl 2-acetamido-2-deoxy-α-D-glucopyranoside and 3 (benzyl 2-acetamido-4,6-O-benzylidene-2-deoxy-α-D-glucopyranoside, key building blocks in preparation of 6, include synthesis simplification and efficient isolation and purification. Optically pure (S-2-chloropropionic acid 7 was prepared and introduced to the positon 3-O of sugar moiety to give compound 4 (benzyl 2-acetamido-4,6-O-benzylidene-3-O-[(R-1-carboxyethyl]-2-deoxy-α-D-glucopyranoside with the (R-configuration of the lactyl side-chain in excellent overall yield and optical purity. Deacetylation of amino group gave compound 5 (benzyl 2-amino-4,6-O-benzylidene-3-O-[(R-1-carboxyethyl]-2-deoxy-α-D-glucopyranoside suitable for incorporation of the Fmoc protecting group to give protected muramic acid derivative 6, a useful building block in peptide synthesis.

  18. Improved resins and novel materials and methods for solid phase extraction and high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Freeze, Ronald [Iowa State Univ., Ames, IA (United States)

    1997-10-08

    Solid-phase extraction (SPE) has grown to be one of the most widely used methods for isolation and preconcentration of a vast range of compounds from aqueous solutions. By modifying polymeric SPE resins with chelating functional groups, the selective uptake of metals was accomplished. The resin, along with adsorbed metals, was vaporized in the ICP and detection of the metals was then possible using either mass or emission spectroscopy. Drug analyses in biological fluids have received heightened attention as drug testing is on the increase both in sports and in the work environment. By using a direct-injection technique, biological fluids can be injected directly into the liquid chromatographic system with no pretreatment. A new surfactant, a sulfonated form of Brij-30 (Brij-S) is shown to prevent the uptake of serum proteins on commercial HPLC columns by forming a thin coating on the silica C18 surface. Excellent separations of eight or more drugs with a wide range of retention times were obtained. The separations had sharper peaks and lower retention times than similar separations performed with the surfactant sodium dodecylsulfate (SDS). Quantitative recovery of a number of drugs with limits of detection near 1 ppm with a 5 μl injection volume were obtained. Finally, a method for solid-phase extraction in a syringe is introduced. The system greatly reduced the volume of solvent required to elute adsorbed analytes from the SPE bed while providing a semi-automated setup. SPE in a syringe consists of a very small bed of resin-loaded membrane packed into a GC or HPLC syringe. After extraction, elution was performed with just a few μl of solvent. This small elution volume allowed injection of the eluent directly from the syringe into the chromatographic system, eliminating the handling problems associated with such small volumes.

  19. Structural study of chlorine tri-fluoride and bromine penta-fluoride in liquid and solid phase

    International Nuclear Information System (INIS)

    Rousson, R.

    1973-01-01

    This research thesis reports the structural study of chlorine tri-fluoride and bromine penta-fluoride between 20 C and about -265 C. After some generalities on these compounds and a presentation of the experimental technique, the author reports and discusses results obtained with these both compounds: Raman spectrum for the liquid and for the solid phase, infrared spectrum for the solid phase, calorimetric measurements. In the case of chlorine tri-fluoride, the author studies the evolution of the liquid spectrum with temperature, shows the existence of an intermediate solid phase, and compares results obtained by Raman spectroscopy and nuclear magnetic resonance. He also applies to bromine penta-fluoride an analysis of normal coordinates of a XF 5 molecule: relationship between force constants and vibration frequencies, application of Wilson method, resolution of the molecular equation, determination of normal vibration modes [fr

  20. Solid solution or amorphous phase formation in TiZr-based ternary to quinternary multi-principal-element films

    Directory of Open Access Journals (Sweden)

    Mariana Braic

    2014-08-01

    The deposited films exhibited only solid solution (fcc, bcc or hcp or amorphous phases, no intermetallic components being detected. It was found that the hcp structure was stabilized by the presence of Hf or Y, bcc by Nb or Al and fcc by Cu. For the investigated films, the atomic size difference, mixing enthalpy, mixing entropy, Gibbs free energy of mixing and the electronegativity difference for solid solution and amorphous phases were calculated based on Miedema׳s approach of the regular solution model. It was shown that the atomic size difference and the ratio between the Gibbs free energies of mixing of the solid solution and amorphous phases were the most significant parameters controlling the film crystallinity.