Sample records for capture-s solid phase

  1. Capture-S, a nontreponemal solid-phase erythrocyte adherence assay for serological detection of syphilis.

    Stone, D L; Moheng, M C; Rolih, S; Sinor, L T


    A solid-phase erythrocyte adherence assay has been developed for the serological detection of reagin antibodies in syphilis. Capture-S (Immucor, Inc., Norcross, Ga.) is a nontreponemal, qualitative screening test for the detection of immunoglobulin G (IgG) and IgM antilipid antibodies in serum or plasma samples from blood donors. The Capture-S assay utilizes a modified Venereal Disease Research Laboratory antigen bound to microtitration wells and anti-IgG- plus anti-IgM-coated indicator eryth...

  2. Solid phase transformations II

    Čermák, J


    This topical volume includes ten invited papers that cover selected areas of the field of solid phase transformations. The first two contributions represent a burgeoning branch; that of the computer simulation of physical phenomena. The following three articles deal with the thermodynamics of phase transformations as a basic theory for describing the phenomenology of phase changes in matter. The next paper describes the interconnections between structural stability and the electronic structure of phases. Two further articles are devoted to displacive transformations; a field where there are ma

  3. Solid phase transformations

    Čermák, J


    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

  4. Solid-phase microextraction

    Nilsson, Torben

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

  5. Solid-Phase Random Glycosylation

    Agoston, K.; Kröger, Lars; Dekany, Gyula;


    Two different approaches were employed to study solid phase random glycosylations to obtain oligosaccharide libraries. In approach I, Wang resin esters were attached to the acceptors structures. Following their glycosylation and resin cleavage, the peracetylated components of the oligosaccharide...

  6. Solid-phase peptide synthesis

    Jensen, Knud Jørgen

    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....



    The solid-phase synthesis of isoxazolines on 2-polystyrylsulfonamidoethanol resin isreported. 2-Polystyrylsuifonamidoethanol resin 1 was reacted with acryloyl chloride to afford2-polystyrylsulfonylamidoethyl acrylate resin 2, which was further reacted with brominatedaldoximes by [3+2] cycioaddition to give isoxazoline resin 4. Resin 4 was treated with aqueous 6mol/L HCI solution to obtain isoxazolines in good yield and purity.


    SUNWeimin; LUOJuntao; 等


    The solid-phase synthesis of isoxazolines on 2-polystyrylsulfonamidoethanol resin is reported.2-Polystyrylsulfonamidoethanol resin 1 was reacted with acryloyl chloride to afford 2-polystyrylsulfonylamidoethyl acrylate resin 2,which was further reacted with brominated aldoximes by [3+2] cycloaddition to give isoxazoline resin 4.Resin 4 was treated with aqueous 6 mol/L HCl solution to obtain isoxazolines in good yield and purity.

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

    Cooke, Gary A.


    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.

  10. Solid-solid phase transformation kinetics

    Bauer, Rico


    Chapter 2 of this thesis presents the investigation of the microstructural evolution of Co precipitates formed upon isochronal annealing of an initially supersaturated Au 10.12 at. % Co solid solution. It was proven, that initially plate like bcc Co precipitates have formed, which deviates from the expected stable fcc Co crystal structure. Upon prolonged annealing, i. e. with ongoing precipitation reaction, the bcc Co was transformed into fcc Co accompanied with a morphological change of th...

  11. Molecular Modeling of Solid Fluid Phase Behavior

    Peter A. Monson


    This report gives a summary of the achievements under DOE contract No. DOE/ER/14150 during the period September 1, 1990 to December 31, 2007. This project was concerned with the molecular modeling of solid-fluid equilibrium. The focus was on understanding how solid-fluid and solid-solid phase behavior are related to molecular structure, and the research program made a seminal contribution in this area. The project led to 34 journal articles, including a comprehensive review article published in Advances in Chemical Physics. The DOE funding supported the work of 5 Ph.D. students, 2 M.S. students and 5 postdoctoral researchers.

  12. Binary Solid-Liquid Phase Equilibria

    Ellison, Herbert R.


    Indicates some of the information that may be obtained from a binary solid-liquid phase equilibria experiment and a method to write a computer program that will plot an ideal phase diagram to which the experimental results may be compared. (Author/CP)

  13. Phase equilibria in isotropic solids

    Šilhavý, Miroslav


    Roč. 25, č. 6 (2013), s. 795-802. ISSN 0935-1175 Institutional support: RVO:67985840 Keywords : phase transitions * equilibrium * interfaces Subject RIV: BA - General Mathematics Impact factor: 1.431, year: 2013

  14. Amorphous Phase Properties Of Oriented Polyethylene Solids

    Zahran, R. R; Kardos, J. L.


    Solid-state deformation of polyethylene results in a preferential orientation of both crystalline and amorphous regions. Usually, one major problem in the prediction of the mechanical and thermal expansion properties of anisotropic polyethylene lies in determining values for the amorphous phase properties and, particularly, at a given level of solid-state deformation. This paper outlines simple procedures for determining the two-dimensional amorphous orientation function and values for the...

  15. Multiplexed Colorimetric Solid-Phase Extraction

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


    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).

  16. Directed evolution and solid phase enzyme screening

    Bylina, Edward J.; Grek, Christina L.; Coleman, William J.; Youvan, Douglas C.


    A new digital imaging spectrophotometer and a series of colorimetric solid phase arrays have been developed to screen bacterial libraries expressing mutagenized enzymes undergoing directed evolution. This high-throughput solid- phase array system (known as `Kcat Technology') can detect less than a 20% difference in enzyme rates within microcolonies grown at a nearly confluent density of 500 colonies per cm2 on an assay disk. Each microcolony is analyzed simultaneously at single-pixel resolution (1.5 megapixels; 75 micron/pixel), requiring less than 100 nanoliters of substrate per measurement, a 1000-fold reduction over conventional liquid phase assays. Here we report the successful identification of variants of Agrobacterium (beta) -glucosidase--a glycosidase with broad substrate specificity that favors cleavage of glucosides over galactosides--by simultaneously assaying two different substrates tagged with spectrally distinct chromogenic reporters.

  17. DNA Extraction: Organic and Solid-Phase.

    Altayari, Wafa


    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. PMID:27259731

  18. Solid-phase fluoroimmunoassay for treponemal antibody.

    Stevens, R W; Schell, R F


    An objective, solid-phase fluoroimmunoassay for treponemal antibody was developed with a lysate of virulent Treponema pallidum (Nichols strain) adsorbed on cellulose acetate disks. A probe containing both the antigen and control disks is inserted successively into a serum specimen dilution, a buffer rinse, fluoroscein isothiocyanate-conjugated goat anti-human immunoglobulin G, and a second buffer rinse. Fluorescence signal units are measured with a fluorometer. To establish test calibration c...

  19. Elementary excitations and phase transformations in solids

    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)

  20. Solid drop based liquid-phase microextraction.

    Ganjali, Mohammad Reza; Sobhi, Hamid Reza; Farahani, Hadi; Norouzi, Parviz; Dinarvand, Rassoul; Kashtiaray, Amir


    Solid drop based liquid-phase microextraction (SDLPME) is a novel sample preparation technique possessing obvious advantages of simple operation with a high pre-concentration factor, low cost and low consumption of organic solvent. SDLPME coupled with gas chromatography (GC), high-performance liquid chromatography (HPLC), and atomic absorption spectrometry (AAS) has been widely applied to the analyses of a different variety of samples. The basic principles, parameters affecting the extraction efficiency, and the latest applications of SDLPME are reviewed in this article. PMID:19962710

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

    Xi, Peng; Cheng, Bowen [Tianjin Municipal Key Lab of Fiber Modification and Functional Fiber, Tianjin Polytechnic University, Tianjin 300160 (China); Gu, Xiaohua [Qiqihar University, 30 Wenhua Road, Qiqihar 161006 (China); CAS Key Laboratory of Engineering Plastics, Joint Laboratory of Polymer Science and Materials, Center for Molecular Science, Institute of Chemistry, The Chinese Academy of Sciences, Beijing 100080 (China); Wang, Yufei [Dalian University Technology, Dalian 116024 (China)


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

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

    Xi Peng [Tianjin Municipal Key Lab of Fiber Modification and Functional Fiber, Tianjin Polytechnic University, Tianjin 300160 (China); Gu Xiaohua [Qiqihar University, 30 Wenhua Road, Qiqihar 161006 (China); CAS Key Laboratory of Engineering Plastics, Joint Laboratory of Polymer Science and Materials, Center for Molecular Science, Institute of Chemistry, The Chinese Academy of Sciences, Beijing 100080 (China)], E-mail:; Cheng Bowen [Tianjin Municipal Key Lab of Fiber Modification and Functional Fiber, Tianjin Polytechnic University, Tianjin 300160 (China); Wang Yufei [Dalian University Technology, Dalian 116024 (China)


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

  3. Combinatorial Solid-Phase Synthesis of Balanol Analogues

    Nielsen, John; Lyngsø, Lars Ole


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

  4. Solid-solid phase transitions determined by differential scanning calorimetry.

    Murrill, E.; Whitehead, M. E.; Breed, L.


    Data are presented to show that tris(hydroxymethyl)acetic acid, monochloropentaerythritol, monofluoropentaerythritol, difluoropentaerythritol, monoaminopentaerythritol, and diaminopentaerythritol exhibit solid-state transitions to a plastic crystalline state. Transitional enthalpies in many of these substances are lower than might be expected by analogy with related structures, suggesting that some configurational contributions to their entropy increments have been inhibited.

  5. Analysis of solid-liquid phase change heat transfer enhancement

    ZHANG; Yinping(张寅平); WANG; Xin(王馨)


    Solid-liquid phase change processes have two important features: the process is an approximately isothermal process and the heat of fusion of phase change material tends to be much greater than its specific heat. Therefore, if any phase change material adjacent to a hot or cold surface undergoes phase change, the heat transfer rate on the surface will be noticeably enhanced. This paper presents a novel insight into the mechanisms of heat transfer enhancement induced by solid-liquid phase change based on the analogy analysis for heat conduction with an internal heat source and solid-liquid phase change heat transfer. Three degrees of surface heat transfer enhancement for different conditions are explored, and corresponding formulae are written to describe them. The factors influencing the degrees of heat transfer enhancement are clarified and their effects quantitatively analyzed. Both the novel insight and the analysis contribute to effective application of phase change heat transfer enhancement technique.

  6. Crystal-Phase Control by Solution-Solid-Solid Growth of II-VI Quantum Wires.

    Wang, Fudong; Buhro, William E


    A simple and potentially general means of eliminating the planar defects and phase alternations that typically accompany the growth of semiconductor nanowires by catalyzed methods is reported. Nearly phase-pure, defect-free wurtzite II-VI semiconductor quantum wires are grown from solid rather than liquid catalyst nanoparticles. The solid-catalyst nanoparticles are morphologically stable during growth, which minimizes the spontaneous fluctuations in nucleation barriers between zinc blende and wurtzite phases that are responsible for the defect formation and phase alternations. Growth of single-phase (in our cases the wurtzite phase) nanowires is thus favored. PMID:26731426

  7. Wax Precipitation Modeled with Many Mixed Solid Phases

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


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

  8. Automated solid-phase synthesis of oligosaccharides containing sialic acids

    Chian-Hui Lai


    Full Text Available A sialic acid glycosyl phosphate building block was designed and synthesized. This building block was used to prepare α-sialylated oligosaccharides by automated solid-phase synthesis selectively.

  9. The Structural Phase Transition in Solid DCN

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


    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. The Structural Phase Transition in Solid DCN

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


    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 energie...

  11. Low-temperature solid-phase chemical reactions

    Baluev, A.V.; Mityakhina, V.S.; Rogozev, B.I.; Silin, M.Yu.


    This paper is concerned with the possibility of solid-phase reactions carried out at 20-25 degrees C. A variety of solid complexes are ground and tested for their reaction capacity in the solid phase with acid phosphates, including complexes of iron, cesium, sodium, tin, and uranyl, using Moessbauer and infrared spectroscopy and thermal analysis. The reactions are considered viable not only because they avoid the expenditure of energy otherwise needed to heat the reactants but also because they provide a new method for the preparation of complex coordination compounds.

  12. Phase transition in solid molecular hydrogen at ultrahigh pressures

    Hemley, R. J.; Mao, H. K.


    Solid normal hydrogen was compressed in a diamond-anvil cell to pressures above 200 GPa. Spontaneous Raman spectra demonstrate that the solid undergoes a structural phase transformation beginning at 145 GPa at 77 K, as evidenced by an abrupt discontinuity in the intramolecular vibron frequency as a function of pressure. The magnitude of the vibron-frequency shift and the pressure-temperature conditions of the phase transformation are consistent with its identification as the theoretically predicted pressure-induced orientational ordering of the molecular solid.

  13. Magnetic Solid Phase Extraction Applied to Food Analysis

    Israel S. Ibarra


    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.

  14. A novel solid-solid phase change heat storage material with polyurethane block copolymer structure

    A novel polymeric solid-solid phase change heat storage material (PCM) with polyurethane block copolymer structure (PUPCM) composed of high molecule weight polyethylene glycol (PEG) as soft segment, 4,4'-diphenylmethane diissyanate (MDI) and 1,4-butanediol (BDO) as a chain extender were synthesized by a two step process. DSC, POM, SEM and WAXD tests were performed to investigate the phase transition behaviors and crystalline morphology. The results indicated that the PUPCM showed typical solid-solid phase transition properties, e.g. suitable transition temperature, high transition enthalpy and good thermal stability. It is a functional polyurethane with good energy storage effect, and the heat storage mechanism of PUPCM is the transfer between crystalline and amorphous states of the soft segment PEG of PUPCM, and the hard segment, serving as 'physical cross-links', restricted the molecular chain of the soft segment's free movement at high temperature. Thus, PUPCM can keep its solid state in the transition processing

  15. Integral dosimetric methods using solid phase

    Current methods are described used for personnel dosimetry based on solid state radiation effects. They mainly include thermoluminescence and radiophotoluminescence. The development is going on of a silicon diode for the dosimetry of fast neutrons and the use is studied of MOSFET transistors. Simple output signal processing is the advantage of another method, thermostimulated conductivity. The lyoluminescence method is also prospective since a number of compounds contained in biological tissue show lyoluminescence and biological material can thus be directly used as a dosemeter. (Ha)

  16. Solid state phase detector replaces bulky transformer circuit

    Moberly, C. L.


    Miniature solid state phase detector using MOSFETs is used in a phase lock loop with a sun-bit detector in an integrated data-link circuit. This replaces bulky transformer circuits. It uses an inverter amplifier, a modulator switch, and a buffer amplifier.

  17. N-Acyliminium Intermediates in Solid-Phase Synthesis

    Quement, Sebastian Thordal le; Petersen, Rico; Meldal, M.; Nielsen, Thomas Eiland


    N-Acyliminium ions are powerful intermediates in synthetic organic chemistry. Examples of their use are numerous in solution-phase synthesis, but there are unmerited few reports on these highly reactive electrophiles in solid-phase synthesis. The present review covers the literature to date and...

  18. Solid-Phase Products of Bacterial Oxidation of Arsenical Pyrite

    Carlson, Liisa; Lindström, E. Börje; Hallberg, Kevin B.; Tuovinen, Olli H.


    Bacterial leaching of an As-containing pyrite concentrate produced acidic (pH < 1) leachates. During the leaching, the bacteria solubilized both As and Fe, and these two elements were distributed in solution-phase and solid-phase products. Jarosite and scorodite were the exclusive crystalline products in precipitate samples from the bacterial leaching of the sulfide concentrate.

  19. Heterogeneous Ferroelectric Solid Solutions Phases and Domain States

    Topolov, Vitaly


    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. Electron-solid and electron-liquid phases in graphene

    Knoester, M. E.; Papić, Z.; Morais Smith, C.


    We investigate the competition between electron-solid and quantum-liquid phases in graphene, which arise in partially filled Landau levels. The differences in the wave function describing the electrons in the presence of a perpendicular magnetic field in graphene with respect to the conventional semiconductors, such as GaAs, can be captured in a form factor which carries the Landau-level index. This leads to a quantitative difference in the electron-solid and -liquid energies. For the lowest Landau level, there is no difference in the wave function of relativistic and nonrelativistic systems. We compute the cohesive energy of the solid phase analytically using a Hartree-Fock Hamiltonian. The liquid energies are computed analytically as well as numerically, using exact diagonalization. We find that the liquid phase dominates in the n =1 Landau level, whereas the Wigner crystal and electron-bubble phases become more prominent in the n =2 and 3 Landau level.

  1. Biogasification of solid wastes by two-phase anaerobic fermentation

    Municipal, industrial and agricultural solid wastes, and biomass deposits, cause large-scale pollution of land and water. Gaseous products of waste decomposition pollute the air and contribute to global warming. This paper describes the development of a two-phase fermentation system that alleviates methanogenic inhibition encountered with high-solids feed, accelerates methane fermentation of the solid bed, and captures methane (renewable energy) for captive use to reduce global warming. The innovative system consisted of a solid bed reactor packed with simulated solid waste at a density of 160 kg/m3 and operated with recirculation of the percolated culture (bioleachate) through the bed. A rapid onset of solids hydrolysis, acidification, denitrification and hydrogen gas formation was observed under these operating conditions. However, these fermentative reactions stopped at a total fatty acids concentration of 13,000 mg/l (as acetic) at pH 5, with a reactor head-gas composition of 75 percent carbon dioxide, 20 percent nitrogen, 2 percent hydrogen and 3 percent methane. Fermentation inhibition was alleviated by moving the bioleachate to a separate methane-phase fermenter, and recycling methanogenic effluents at pH 7 to the solid bed. Coupled operation of the two reactors promoted methanogenic conversion of the high-solids feed. (author)

  2. Solid state photomultiplier for astronomy, phase 2

    Besser, P. J.; Hays, K. M.; Laviolette, R. A.


    Epitaxial layers with varying donor concentration profiles were grown on silicon substrate wafers using chemical vapor deposition (CVD) techniques, and solid state photomultiplier (SSPM) devices were fabricated from the wafers. Representative detectors were tested in a low background photon flux, low temperature environment to determine the device characteristics for comparison to NASA goals for astronomical applications. The SSPM temperatures varied between 6 and 11 K with background fluxes in the range from less than 5 x 10 to the 6th power to 10 to the 13th power photons/square cm per second at wavelengths of 3.2 and 20 cm. Measured parameters included quantum efficiency, dark count rate and bias current. Temperature for optimal performance is 10 K, the highest ever obtained for SSPMs. The devices exhibit a combination of the lowest dark current and highest quantum efficiency yet achieved. Experimental data were reduced, analyzed and used to generate recommendations for future studies. The background and present status of the microscopic theory of SSPM operation were reviewed and summarized. Present emphasis is on modeling of the avalanche process which is the basis for SSPM operation. Approaches to the solution of the Boltzmann transport equation are described and the treatment of electron scattering mechanisms is presented. The microscopic single-electron transport theory is ready to be implemented for large-scale computations.

  3. Flow immunoassay using solid-phase entrapment.

    Locascio-Brown, L; Martynova, L; Christensen, R G; Horvai, G


    A flow injection immunoassay was performed using a column packed with reversed-phase sorbents to effect separation of the immunoreacted species by entrapping free analyte and allowing antibody-conjugated analyte to pass unretained. Fluorescein-labeled analyte was measured in a competitive assay for the anticonvulsant drug phenytoin. The simplicity of the assay was the greatest advantage of the technique, which allowed for measurement of phenytoin in a 2-min assay time. The reliable detection limit for the assay was 5 nmol L(-)(1) of phenytoin in serum. The columns were regenerated with periodic injections of ethanol solutions to remove the entrapped analyte and prepare the column for subsequent analyses. PMID:21619134

  4. Linkage of biomolecules to solid phases for immunoassay

    Topics covered by this lecture include a brief review of the principal methods of linkage of biomolecules to solid phase matrices. Copies of the key self explanatory slides are presented as figures together with reprints of two publications by the author dealing with a preferred chemistry for the covalent linkage of antibodies to hydroxyl and amino functional groups and the effects of changes in solid phase matrix and antibody coupling chemistry on the performance of a typical excess reagent immunoassay for thyroid stimulating hormone


    Yu-ying Li; Jia-song He


    Solid phase transition of the a form crystals to the β form crystals in syndiotactic polystyrene (sPS) samples has occurred in supercritical CO2. This transformation is different from those detected under other conditions. The effects of some factors (e.g. time, temperature, and pressure) on the solid phase transformation of sPS in supercritical CO2 were analyzed in detail. Experimental results show that longer time, higher temperature or higher pressure favors the transformation of the α form crystals to the β form crystals.

  6. Rigid polar composite supports for use in solid phase synthesis

    A number of particulate polyethylene and polypropylene based matrices have been γ-radiation grafted with poly(acryloylsarcosine methyl ester). The resulting composite materials have physicochemical properties attractive for use in continuous solid phase synthesis. Three macroporous polystyrene resins have also been impregnated with a secondary polyamide network using thermal initiation. All of these retain their rigid spherical structure and the composite properties again make them good candidates for use under pressure. One of these has been used in a preliminary solid phase experiment and two successive amino acid residues coupled with approx. 100% yield. 1 figure, 2 tables

  7. [Studies on the anaerobic phased solid digester system for municipal solid waste (MSW) treatment].

    Wang, Jun-qin; Shen, Dong-sheng


    Through analyzing and detecting the leaching pollutant (COD) in two bioreactors, anaerobic phased solid digester system and leachate direct-recirculating landfill, the changing rule of municipal solid waste and the characteristics of methanogenesis were studied. The results showed that anaerobic phased solid digester system accelerated the process of degrading municipal solid waste and stabilizing landfill site. The relationship between the leaching pollutant (COD) and refuse age was logarithmic linear correlation. More than 80% of biogas in volume occured in the methanogenisis bioreactor, the methane content in which was 55%-69%. The preferable volumetric COD loading rate of the methanogenisis bioreactor was 6.5-7.5 g/(L x d). PMID:15327275

  8. Preconcentration of strontium by micelle modified solid phase extraction

    The preconcentration of strontium using a solid phase separation technique with selective micelle forming complexant has been studied. Di-2-ethylhexylphosphoric acid and its thio- and dithio derivatives were used as modifiers. The goal of this work was to study the influence of physico-chemical parameters on recovery of strontium after its preconcentration on reverse phase (Si-C-18) using micelle modifiers. (author) 5 refs.; 7 figs

  9. Antibody coated tubes in T3 - solid phase radioimmunoassay

    The aim of this study was to develop a simple and inexpensive form of solid phase radioimmunoassay of T3 (3,5,3'-L- triiodothyronine); for the preparation of solid phase, the adsorption of anti-T3 antibodies to polystyrene tubes has been used. The polystyrene tubes were used without washing or other treatment; each tube was coated by addition of an uniform volume (175 μl) of diluted antiserum of moderately high titer. Antiserum dilution was 1:3000 and the optimal pH of buffer solution was 8.4 - 8.6. The best results were achieved with an exposure time to antiserum of 40 h at 4 deg C. The antibody - coated tubes prepared in this way were verified by using them to the radioimmunoassay of T3. The results obtained with the above mentioned solid phase in T3-RIA of three level control serums were found to be successful for setting up T3- solid phase radioimmunoassay of high precision. (authors)

  10. Solid phase separation technique for use in radioimmunoassays

    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

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

    Lyngsø, Lars O.; Nielsen, John


    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....

  12. Combinatorial solid-phase synthesis of hapalosin mimetics

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


    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...

  13. Solid-phase-supported synthesis of morpholinoglycine oligonucleotide mimics

    Tatyana V. Abramova


    Full Text Available An efficient solid-phase-supported peptide synthesis (SPPS of morpholinoglycine oligonucleotide (MorGly mimics has been developed. The proposed strategy includes a novel specially designed labile linker group containing the oxalyl residue and the 2-aminomethylmorpholino nucleoside analogues as first subunits.

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

    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.

  15. Binding of properdin to solid-phase immune complexes

    Junker, A; Baatrup, G; Svehag, S E; Wang, P; Holmström, E; Sturfelt, G; Sjöholm, A G


    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 w...

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

    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)


    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.

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

    Nielsen, Thomas Eiland


    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...

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

    Nielsen, John


    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-pyra...

  19. The solid phase of ginkgolide K: Structure and physicochemical properties

    Zhang, Yiwen; Zhang, Guoshun; Wang, Zhenzhong; Lv, Yang; Xiao, Wei


    Four solvates of ginkgolide K with dimethyl sulfoxide(I), water molecule(II), acetone-isopropyl alcohol(III), methanol-ethanol(IV) and one solvate-free (V) have been described in this work. And the solid-state techniques such as X-ray diffraction, thermal analysis and Fourier transform infrared spectroscopy were used for characterization of the solid phases. The single crystal structures of ginkgolide K solvates (I-IV) have been determined. Ginkgolide K shows strong inflexibility and solvents being incorporated in the crystal structure results in it forming polymorphs via the diverse hydrogen bond interactions.

  20. Qinshan phase Ⅱ expansion project to minimize solid waste transformation

    The nuclear power plant in the production and maintenance period usually have a certain amount of radioactive waste, according to the physical state of these wastes, it can be divided into radioactive waste gas, radioactive waste water and solid waste. Radioactive waste gas and water, treated by the waste treatment system, and the corresponding facilities for filtration, purification. compression, storage to meet discharging requirements, discharge to the environment finally. As for solid radioactive waste, common solution in nuclear power plants is to use specially formulated cement to cure and packaged into the barrel, stored in a particular building for naturally decaying. Qinshan NPP have optimized the solid waste treatment process m extension project. As the nuclear power industry prospering, radioactive solid waste generation would increased dramatically,. how to reduce solid waste production volume, how to control the volume of waste bins will become serious issues in future. Qinshan Phase Ⅱ expansion project as 'replica plus improvement' projects, 'solid waste minimization transformation' has received great attention from SEPA (State Environmental Protection Department). (authors)

  1. Modeling of liquid phase formation by solid-solid interaction of Zircaloy and AISI 316 Steel

    Two models were developed in order to describe the eutectic interaction between Zircaloy-4 and AISI 316 stainless steel, in the temperature range 1000 - 1300 C degree. The aim of the models is to simulate what could happen in the nucleus of a power reactor in an eventual transient high temperature accident. Entry data correspond to the instantaneous positions of the Zircaloy-4 / liquid and stainless steel / liquid inter phases, obtained from experimental data. The hypothesis corresponding to the first model are: that the liquid phase growths by diffusion of the main elements of each alloy in the liquid (Fe and Zr), that there is no interaction between these elements during diffusion, that the diffusion or convection in the solid state is not considered, and that volume changes are negligible during fusion and interdiffusion. Concentrations at the solid/liquid inter phases and the effective diffusion coefficients for Zr and Fe in the liquid can be obtained. The model allows to calculate the formation kinetics for the liquid phase as measured by Zr oxide layers of 0, 10, 20 and 50 microns initial width, formed on the Zircaloy in order to simulate the operating conditions of a reactor. Incubation times for the onset of the reaction, observed experimentally in pre-oxidized samples, were calculated taking into account the oxide dissolution. The second model considers diffusion of Fe in Zircaloy since Fe is a fast diffuser in Zr. As in the first model, concentrations at the solid/liquid inter phases as well as the effective diffusion coefficients for Fe and Zr in the liquid, are calculated. The results obtained in this case depend on the Fe concentration at the solid/liquid interphase at the solid Zircaloy side, and on the Fe diffusivity in Zircaloy-4, which was estimated by the Fe diffusivity in Zr. (author)

  2. Entransy dissipation minimization for liquid-solid phase change processes


    The liquid-solid phase change process of a simple one-dimensional slab is studied in this paper.By taking entransy dissipation minimization as optimization objective,the optimal external reservoir temperature profiles are derived by using optimal control theory under the condition of a fixed freezing or melting time.The entransy dissipation corresponding to the optimal heat exchange strategies of minimum entransy dissipation is 8/9 of that corresponding to constant reservoir temperature operations,which is independent of all system parameters.The obtained results for entransy dissipation minimization are also compared with those obtained for the optimal heat exchange strategies of minimum entropy generation and constant reservoir temperature operations by numerical examples.The obtained results can provide some theoretical guidelines for the choice of optimal cooling or heating strategy in practical liquid-solid phase change processes.

  3. Studies in Solid Phase Peptide Synthesis: A Personal Perspective

    Mitchell, A R


    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.

  4. On the nature of phase transition in solid electrolytes

    An attempt is made to precisely measure the solid electrolyte RbAg4I5 conductivity in the vicinity of the phase transition at 208 deg K. Polycrystalline samples obtained by common technique have been used as well as single RbAg4I5 crystals grown from the acetone solution of AgI and RbI. The dependence of conductivity on inverse temperature is given for different samples. The phase transition of the single crystals is accompanied by a jump (approximately 12%) of conductivity. This transfer is reversible, since no hysteresis is found in the +-0.3 deg K vicinity of the phase transition temperature. Polycrystalline samples display no pronounces jump of conductivity, but the conductivity curve has two bends, i.e. the phase transition is ''diffused''. The activation energy before the transition differs from that after the transition

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

    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.)

  6. Numerical studies of integrated concrete with a solid-solid phase change material

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


    The thermal storage performance of concrete cement integrated with a hypothetical solid-solid phase change material (PCM) was investigated. The thermal storage material was exposed to solar radiation on a sunny winter day in Toronto. The effects of weight ratio of PCM to cement and the thickness of cement were studied. The integrated PCM cement compound was treated as a homogenous mixture with uniform physical and thermal properties. Finite element modelling (FEM) was used to determine the effective heat capacity method. Governing equations for the heat transfer process in the solid-liquid PCMs included Navier-Stokes equations; mass conservation equations; and the energy conservation equation. The energy equation was the only governing equation for the binary solid state PCMs. The enthalpy method was used to apply governing equations of PCMs over the whole fixed domain of interest. The total energy required for the phase change was determined using the enthalpy function. The simulations showed that PCMs can reduce the fluctuation of temperature. Temperature fluctuations on the upper surface varied mainly in amplitude and in time phase due to thermal storage effects. The total amount of solar gain increased when the PCM ratio increased. However, the effect of the PCM ratio on the amount of released energy became less apparent when the thickness of the PCM was increased. It was concluded that a 30 per cent PCM ratio contributed the maximum overall released energy after the radiation gain vanished. 8 refs., 3 tabs., 11 figs.

  7. Phase field modeling and simulation of three-phase flow on solid surfaces

    Zhang, Qian; Wang, Xiao-Ping


    Phase field models are widely used to describe the two-phase system. The evolution of the phase field variables is usually driven by the gradient flow of a total free energy functional. The generalization of the approach to an N phase (N ≥ 3) system requires some extra consistency conditions on the free energy functional in order for the model to give physically relevant results. A projection approach is proposed for the derivation of a consistent free energy functional for the three-phase Cahn-Hilliard equations. The system is then coupled with the Navier-Stokes equations to describe the three-phase flow on solid surfaces with moving contact line. An energy stable scheme is developed for the three-phase flow system. The discrete energy law of the numerical scheme is proved which ensures the stability of the scheme. We also show some numerical results for the dynamics of triple junctions and four phase contact lines.

  8. Solid-Phase Preparation and Characterization of Chitosan

    GaoLe-ping; DuYu-min; ZhangDao-bin; ShiXiao-wen; ZhanHuai-yu; SongWen-hua


    Chitosan was prepared with stressing method by blending chitin and solid alkali in a single-screw extruder at given temperature and characterized by potentiometric titration, gel permeation chromatography (GPC), infrared spectrum (IR) and carborr13 magnetic resonance sperctroscopy (13C NMR). Chitosan with a deacetylation degree (DD) of 76. 1% was obtained at a mass ratio 0.2 : 1 : 1 for H20/chitin/NaOH at 160℃ for 12 mirL Compared to conventional solution method(usually 1 : 10 for chitin/NaOH), the alkali assumption greatly decreased. Molecular weight of chitosan obtained by solid-phase method(S3,M. 1.54 X 10s ) was lower than that obtained by suspension method(Y2,Mw3. 34×105). During deacetylation, molecular weight decreased with high reaction temperature and long reaction time but remained same at different initial ratios of NaOH/chitirL It might be concluded that degradation of chitosan was caused by breakout of the main chain of the oxidized chitosan catalyzed by alkali during the deactylation. IR and 13C NMR showed that structures of chitosans prepared by solid-phase method were not changed.

  9. Solid-phase catalytic reactions of tritium with carbohydrates. Communication 3. Mechanism of isomerization of epimeric pentoses in the course of solid-phase catalytic hydrogenation with tritium

    The mechanism of isomerization of ribose into arabinose in the solid phase under the action of spillover hydrogen in the course of solid-phase catalytic hydrogenation with tritium was studied. Isomerization of ribose was shown to occur by a complex mechanism similar to acid-catalyzed keto-enol tautomerization of epimeric sugars in solution; the active species in solid-phase catalytic hydrogenation of D-ribose with tritium is spillover hydrogen in the proton form

  10. Heat transfer in different phases of solid cyclohexene

    Konstantinov, V. A.; Krivchikov, A. I.; Korolyuk, O. A.; Revyakin, V. P.; Sagan, V. V.; Vdovichenko, G. A.; Zvonaryova, A. V.


    The thermal conductivity of solid cyclohexene C6H10 has been measured in two independent experiments in five different stable and metastable phase states: orientational glass (Ig), orientational glass (IIIg) with a partial order, dynamically orientationally disordered state (III) with a partial order, completely orientationally ordered phase (II) and “plastic” phase (I). The measurements were carried out at saturated vapor pressure in the temperature range 2-120 K and at isochoric conditions in “plastic” and orientationally ordered phases on samples of different densities. The isochoric thermal conductivity of “plastic” phase increases smoothly with temperature. It can be attributed to weakening of the translational orientational coupling which, in turn, leads to a decrease in phonon scattering on rotational excitations. The thermal conductivity of cyclohexene measured at saturated vapor pressure exhibits a similar behavior in phases Ig, IIIg, and II. At low temperatures (Tthermal conductivity tends to T2 dependence, passes through a maximum and decreases further with increasing temperature following the dependence, which is somewhat different from 1/T. It was found that the thermal conductivity can be represented as a sum of two contributions κ(T)=κ1(T)+κ2(T), where κ1(T) is due to propagating phonons whose mean-free path exceeds half the phonon wavelength, and κ2(T) is attributed to localized short-wavelength or “diffusive” vibrational modes.

  11. Solid phase extraction of petroleum carboxylic acids using a functionalized alumina as stationary phase.

    de Conto, Juliana Faccin; Nascimento, Juciara dos Santos; de Souza, Driele Maiara Borges; da Costa, Luiz Pereira; Egues, Silvia Maria da Silva; Freitas, Lisiane Dos Santos; Benvenutti, Edilson Valmir


    Petroleum essentially consists of a mixture of organic compounds, mainly containing carbon and hydrogen, and, in minor quantities, compounds with nitrogen, sulphur, and oxygen. Some of these compounds, such as naphthenic acids, can cause corrosion in pipes and equipment used in processing plants. Considering that the methods of separation or clean up the target compounds in low concentrations and in complex matrix use large amounts of solvents or stationary phases, is necessary to study new methodologies that consume smaller amounts of solvent and stationary phases to identify the acid components present in complex matrix, such as crude oil samples. The proposed study aimed to recover acid compounds using the solid phase extraction method, employing different types of commercial stationary ion exchange phases (SAX and NH(2)) and new phase alumina functionalized with 1,4-bis(n-propyl)diazoniabicyclo[2.2.2]octane chloride silsesquioxane (Dab-Al(2)O(3)), synthesized in this work. Carboxylic acids were used as standard mixture in the solid phase extraction for further calculation of recovery yield. Then, the real sample (petroleum) was fractionated into saturates, aromatics, resins, and asphaltenes, and the resin fraction of petroleum (B1) was eluted through stationary ion exchange phases. The stationary phase synthesized in this work showed an efficiency of ion exchange comparable to that of the commercial stationary phases. PMID:22589166

  12. Solid-phase fluorescence spectroscopy to characterize organic wastes.

    Muller, Mathieu; Milori, Débora Marcondes Bastos Pereira; Déléris, Stéphane; Steyer, Jean-Philippe; Dudal, Yves


    The production of solid organic waste (SOW) such as sewage sludge (SS) or municipal solid waste (MSW) has been continuously increasing in Europe since the beginning of the 1990'. Today, the European Union encourages the stabilization of these wastes using biologic processes such as anaerobic digestion and/or composting to produce bio-energy and organic fertilizers. However, the design and management of such biologic processes require knowledge about the quantity and quality of the organic matter (OM) contained in the SOW. The current methods to characterize SOW are tedious, time-consuming and often insufficiently informative. In this paper, we assess the potential of solid-phase fluorescence (SPF) spectroscopy to quickly provide a relevant characterization of SOW. First, we tested well known model compounds (tryptophan, bovine serum albumin, lignin and humic acid) and biologic matrix (Escherichia coli) in three dimensional solid-phase fluorescence (3D-SPF) spectroscopy. We recorded fluorescence spectra from proteinaceous samples but we could not record the fluorescence emitted by lignin and humic acid powders. For SOW samples, fluorescence spectra were successfully recorded for MSW and most of its sub-components (foods, cardboard) but impossible for SS, sludge compost (SC) and ligno-cellulosic wastes. Based on visual observations and additional assays, we concluded that the presence of highly light-absorptive chemical structures in such dark-colored samples was responsible for this limitation. For such samples, i.e. lignin, humic acid, SS, SC and ligno-cellulosic wastes, we show that laser induced fluorescence (LIF) spectroscopy enables the acquisition of 2D fluorescence spectra. PMID:21696938

  13. Novel solidsolid phase change material based on polyethylene glycol and cellulose used for temperature stabilisation

    Wojda Marta


    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.

  14. Kinetics of (beta)(right arrow)(delta) Solid-Solid Phase Transition of HMX

    In order to calculate the kinetic parameters from DSC data, we have used the generally accepted methods of Bershtein [13]. We have calculated the rate constants for 4 temperatures and the activation energy based on the shift in the transition temperature, β → (delta) for HMX. The values of Ea from this work is 402 kJ/mol compared to previous results by Brill [9] of 204 kJ/mol. Brill and associates measured the phase transition of HMX using FTIR, sodium chloride plates and silicon oil. Given the differences in technique between FTIR and DSC the results found in this work are reasonable. In this investigation a large sample set (16) proved to be statistically valid for the determinations of k. Linear regressions were performed, observed and good fits were obtained, for each temperature. The enthalpy determination of ΔHo, for the β → (delta) phase transition was reproducible with in 3 parts in 100 over the range of this experiment. Thus, the data derived from this experiment k, Ea, and ΔHo are valid parameters for the solid-solid phase transition. Obtaining pure β phase HMX was very important for this investigation. Related to the phase change is the particle size distribution and is presented in Figure 3. Compared to previous work on HMX, this study utilized very pure β phase material. In addition, the particle size was controlled more rigorously at about 160 (micro)m, giving a more consistent result for α. Thus, these kinetic results should have less scatter than results with less control of HMX purity and particle size. The kinetic basis of the polymorphic conversion is due to the cohesive forces in the HMX crystal lattice [21]. The energy required to bring about change from chair to chair-chair conformation has been reported by Brill [21] as ring torsion and is essentially a normal mode of the molecule that requires about 4 kJ mol-1. For the purpose of this investigation the energy of activation found in this work relates to the disruption of the

  15. Liquid/solid/dual phase xenon γ-ray detectors

    It is recognized by various groups in the world that liquid xenon (LXe) is an interesting medium for the detection of γ-rays. In spite of all the experimental and theoretical effort expended during recent years, the processes that take place in this medium are not yet fully understood. We have obtained some preliminary results using an ionization chamber with a Frisch grid. This chamber could be filled with LXe and with solid xenon (SXe). We also investigated dual phase (GXe/SXe) systems. Our study will be continued with a newly developed detection cell described in this article. ((orig.))

  16. Liquid/solid/dual phase xenon γ-ray detectors

    van Sonsbeek, R.; Bom, V. R.; van Eijk, C. W. E.; Hollander, R. W.; Meijvogel, K.; Okx, W. J. C.


    It is recognized by various groups in the world that liquid xenon (LXe) is an interesting medium for the detection of γ-rays. In spite of all the experimental and theoretical effort expended during recent years, the processes that take place in this medium are not yet fully understood. We have obtained some preliminary results using an ionization chamber with a Frisch grid. This chamber could be filled with LXe and with solid xenon (SXe). We also investigated dual phase (GXe/SXe) systems. Our study will be continued with a newly developed detection cell described in this article.

  17. Solid phase speciation of radiocaesium in bottom sediments

    A comprehensive laboratory study is presented on the solid-phase speciation of ionic radiocaesium in bottom sediments (riverine, lacustrine, estuarine) covering some 75 samples of widely differing textural properties and originating from various locations in Europe. Sediments are characterised in terms of cation exchange capacities, exchangeable potassium and ammonium and specific radiocaesium sorption properties. It is shown that radiocaesium is quantitatively retained in the specific sorption sites associated with the micaceous clay minerals in the sediments. The practical consequences of this finding are discussed in terms of a predictive equation allowing forecasting of radiocaesium levels in the watercolumn or in the interstitial fluid of the sediment

  18. Development of SBS-phase conjugation mirror in solid media

    Yoshida, Hidetsugu; Fujita, Hisanori; Nakatsuka, Masahiro [Osaka Univ., Suita (Japan). Inst. of Laser Engineering


    An optical fiber offers a low power SBS threshold and stable performance at input energies of a few mJ level. For long pulse duration using a longer focusing lens, fused-silica glass had high SBS reflectivity over 90% without any damage occurrence at the incident energy of 380 mJ in 15-ns pulse duration. These properties of the fused-silica are almost comparable with those of highly performed gases or liquids. Damage-free operation using a fused-silica as a better phase conjugation material would lead to construct more compact laser-diode pumped all-solid-state laser system. (author)

  19. Development of SBS-phase conjugation mirror in solid media

    An optical fiber offers a low power SBS threshold and stable performance at input energies of a few mJ level. For long pulse duration using a longer focusing lens, fused-silica glass had high SBS reflectivity over 90% without any damage occurrence at the incident energy of 380 mJ in 15-ns pulse duration. These properties of the fused-silica are almost comparable with those of highly performed gases or liquids. Damage-free operation using a fused-silica as a better phase conjugation material would lead to construct more compact laser-diode pumped all-solid-state laser system. (author)

  20. Solid-phase synthesis of polyamine toxin analogues

    Kromann, Hasse; Krikstolaityte, Sonata; Andersen, Anne J; Andersen, Kim; Krogsgaard-Larsen, Povl; Jaroszewski, Jerzy W; Egebjerg, Jan; Strømgaard, Kristian


    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-phase...... synthesis of analogues of PhTX-83 and the electrophysiological characterization of these analogues on cloned AMPA and kainate receptors. The polyamine portion of PhTX-83 was modified systematically by changing the position of the secondary amino group along the polyamine chain. In another series of...

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

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


    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...

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

    Thurman, E.M.; Snavely, K.


    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.

  3. A rapid solution-phase screening technique for hybridoma culture supernatants using radiolabeled antigen and a solid-phase immunoadsorbent

    The solid-phase immunoassay commonly used to screen hybridoma supernatants at times gave falsely positive results. A solution-phase screening technique, which uses radiolabeled antigen and a solid-phase immunoadsorbent, is described. This technique overcomes the problem of false positives and can be easily adopted for other soluble antigens. (Auth.)

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

    Sheldon, Rex; Weiser, Martin W.


    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.

  5. Studies of phase transitions in the aripiprazole solid dosage form.

    Łaszcz, Marta; Witkowska, Anna


    Studies of the phase transitions in an active substance contained in a solid dosage form are very complicated but essential, especially if an active substance is classified as a BCS Class IV drug. The purpose of this work was the development of sensitive methods for the detection of the phase transitions in the aripiprazole tablets containing initially its form III. Aripiprazole exhibits polymorphism and pseudopolymorphism. Powder diffraction, Raman spectroscopy and differential scanning calorimetry methods were developed for the detection of the polymorphic transition between forms III and I as well as the phase transition of form III into aripiprazole monohydrate in tablets. The study involved the initial 10 mg and 30 mg tablets, as well as those stored in Al/Al blisters, a triplex blister pack and HDPE bottles (with and without desiccant) under accelerated and long term conditions. The polymorphic transition was not observed in the initial and stored tablets but it was visible on the DSC curve of the Abilify(®) 10 mg reference tablets. The formation of the monohydrate was observed in the diffractograms and Raman spectra in the tablets stored under accelerated conditions. The monohydrate phase was not detected in the tablets stored in the Al/Al blisters under long term conditions. The results showed that the Al/Al blisters can be recommended as the packaging of the aripiprazole tablets containing form III. PMID:26397209

  6. Natural uranium in Forsmark, Sweden: The solid phase

    Highlights: • Dissolved U was found at depths where reducing conditions would be expected. • U-bearing solid phases have been characterized in order to understand the source and timing of U oxidation. • Altered primary uraninite and uranothorite were found in local pegmatites. • Secondary CaU(VI)-silicates are associated with calcite and >1 Ga fracture minerals. • Coffinitized uraninite is associated with (Ca)FeAl-silicates and sulfides/sulfates of Palaeozoic age. - Abstract: U-bearing solid phases from Forsmark, Sweden, a proposed host for radioactive waste repositories, have been identified and characterized. Elevated dissolved U was found in some groundwater samples during the site investigations, prompting a need to study the local U geochemistry. Previous hydrochemical and whole-rock geochemical studies indicated that U was derived from local pegmatites, and mobilized and re-deposited during several geological events. In this study, down-hole gamma logs guided sampling of local pegmatites, cataclasites, and fracture fillings. Back-scattered electron-imaging, petrographic microscopy, and electron microprobe analyses were used to find and analyze U phases in thin sections. The results show that the principal U sources at Forsmark include pegmatitic uraninite (PbO up to ∼22 wt%) and metamict uranothorite. These primary minerals show variable degrees of alteration such as enrichment in Ca and Al and/or replacement by secondary Ca–U(VI)-silicates, haiweeite and uranophane. The haiweeite contains up to ∼5 wt% Al2O3, a chemical signature reflecting early (Proterozoic) events of hydrothermal fluid migration. Coffinitized, secondary uraninite is found in association with FeAl-silicates or Palaeozoic sulfide/sulfate minerals, indicating remobilization-precipitation and/or a secondary, sedimentary source of U. It is inferred that U was oxidized during geologically early periods. Later, U(IV) phases formed in fractures open to fluid circulation during the

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

    Barsky, Eugene


    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...

  8. Ferrofluid-based dispersive solid phase extraction of palladium.

    Farahani, Malihe Davudabadi; Shemirani, Farzaneh; Gharehbaghi, Maysam


    A new mode of dispersive solid phase extraction based on ferrofluid has been developed. In this method, an appropriate amount of ferrofluid is injected rapidly into the aqueous sample by a syringe. Since the sorbent is highly dispersed in the aqueous phase, extraction can be achieved within a few seconds. The ferrofluid can be attracted by a magnet and no centrifugation step is needed for phase separation. Palladium was used as a model compound in the development and evaluation of the extraction procedure in combination with flame atomic absorption spectrometry. The experimental parameters (pH, DDTC concentration, type and concentration of eluent, the amount of adsorbent, extraction time, and the effect of interfering ions) were investigated in detail. Under the optimized conditions, the calibration graph was linear over the range of 1-100 μg L(-1) and relative standard deviation of 3.3% at 0.1 μg mL(-1) was obtained (n=7). The limit of detection and enrichment factor (EF) was obtained to be 0.35 μg L(-1) and 267, respectively. The maximum adsorption capacity of the adsorbent at optimum conditions was found to be 24.6 mg g(-1) for Pd(II). The method was validated using certified reference material, and has been applied for the determination of trace Pd(II) in actual samples with satisfactory results. PMID:23618148

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

    S Z Mohamed Shamshuddin; N Nagaraju


    The transesterification of methyl salicylate with phenol has been studied in vapour phase over solid acid catalysts such as ZrO2, MoO3 and SO$^{2-}_{4}$ or Mo(VI) ions modified zirconia. The catalytic materials were prepared and characterized for their total surface acidity, BET surface area and powder XRD patterns. The effect of mole-ratio of the reactants, catalyst bed temperature, catalyst weight, flowrate of reactants, WHSV and time-on-stream on the conversion (%) of phenol and selectivity (%) of salol has been investigated. A good yield (up to 70%) of salol with 90% selectivity was observed when the reactions were carried out at a catalyst bed temperature of 200°C and flow-rate of 10 mL/h in presence of Mo(VI)/ZrO2 as catalyst. The results have been interpreted based on the variation of acidic properties and powder XRD phases of zirconia on incorporation of SO$^{2-}_{4}$ or Mo(VI) ions. The effect of poisoning of acid sites of SO$^{2-}_{4}$ or Mo(VI) ions modified zirconia on total surface acidity, powder XRD phases and catalytic activity was also studied. Possible reaction mechanisms for the formation of salol and diphenyl ether over acid sites are proposed.

  10. Gamma ray tomography and solid phase hold-up measurements in a gas-solid circulating fluidized bed

    Chemical industry has numerous cases wherein reactions are carried between reactants that exist in different phases. Equipment designed for such a reaction is called multiphase reactor and intimate contact between the phases in any multiphase reactor is a must to achieve high efficiencies. When the reactants are in gas and solid phases or when the solid phase is a catalyst or a product to be dried in a gas stream, better contact efficiency can be achieved by suspending fine solids in the high velocity of fluid streams. A number of configurations are possible for carrying out such operations, such as rotary bed, fixed bed, moving bed, and fluidized bed and its several sub-configurations. Circulating fluidized bed (Cf) is a special mode of fluidization, and comprises of a tall riser column in which the solids are fluidized at high carrier phase velocity (gas and/or liquid). The entrained solids are captured in a cyclone or bag filters and returned back to the bottom of the riser continuously. CFB has found important applications in petroleum and power industry. Fluidized catalytic cracking of crude naphtha to petroleum products is carried out in a CFB system wherein the catalyst particles are suspended and entrained at high temperature in gasified naphtha in the riser column. Naphtha cracking is a multi-million dollar application of CFB and requires close study for efficiency and performance. Optimized operation of a CFB requires knowledge of solid phase holdup profiles and residence time distribution in the riser column. Attempts, direct and indirect, have been made to accurately measure these quantities. Use of radioisotopes offers a powerful and cost effective method for estimating both solid phase holdup profiles as well as residence time distribution in continuous multiphase flow. Efforts were therefore made through this investigation to determine solid phase axial and radial holdup profiles in the riser section of a 'cold' gas-solid circulating fluidized bed

  11. Development of a solid phase RIA for human plasma somatostatin

    Somatostatin is widely distributed in tissues of biological fluids. In the present study we tested the validity of a new radioimmunoassay by a solid phase immunoextraction. Sensitivity was 1.8 pg/mL and the within-assay precision with two different pools of human plasma was 12.2% (CV) at a concentration of 19.2 ± 2.34 pg/ml (mean ± SD) and 11.9% at 8.53 ± 1.02 pg/ml. The between assay precision was 14.2% (CV) at a concentration of 11.8 ± 1.68 pg/ml. The accuracy was good as tested by the dilution test and the recovery test. The method had good correlation with a current extraction method. Basal value of somatostatin in the plasma of 32 normal subjects was 11.5 ± 5.80 pg/ml. (author)

  12. Nanoscale doping of compound semiconductors by solid phase dopant diffusion

    Ahn, Jaehyun; Chou, Harry; Koh, Donghyi; Kim, Taegon; Roy, Anupam; Song, Jonghan; Banerjee, Sanjay K.


    Achieving damage-free, uniform, abrupt, ultra-shallow junctions while simultaneously controlling the doping concentration on the nanoscale is an ongoing challenge to the scaling down of electronic device dimensions. Here, we demonstrate a simple method of effectively doping ΙΙΙ-V compound semiconductors, specifically InGaAs, by a solid phase doping source. This method is based on the in-diffusion of oxygen and/or silicon from a deposited non-stoichiometric silicon dioxide (SiOx) film on InGaAs, which then acts as donors upon activation by annealing. The dopant profile and concentration can be controlled by the deposited film thickness and thermal annealing parameters, giving active carrier concentration of 1.4 × 1018 cm-3. Our results also indicate that conventional silicon based processes must be carefully reviewed for compound semiconductor device fabrication to prevent unintended doping.

  13. TEM characterization of Solid-Phase Epitaxy in amorphized polysilicon

    Solid Phase Epitaxy (SPE) of amorphous silicon thin films can be employed to build novel device structures for VLSI applications. One way of achieving SPE is to use a room temperature silicon implant to amorphize a polysilicon layer followed by a thermal treatment to promote epitaxial growth. Both vertical SPE, in which the epitaxial film is grown directly on silicon substrate, and lateral SPE, in which the epitaxial growth is extended over a thin layer of oxide using the vertical SPE region as a seed, have been realized using this approach. This paper presents results obtained by cross-sectional TEM analysis of the epitaxial films, with particular emphasis on the effects of implant schedule and annealing conditions on the epitaxial regrowth

  14. Solid phase epitaxial regrowth of (001) anatase titanium dioxide

    Barlaz, David Eitan; Seebauer, Edmund G., E-mail: [Department of Chemical and Biomolecular Engineering, University of Illinois, 600 S Mathews Ave., Urbana, Illinois 61801 (United States)


    The growing interest in metal oxide based semiconductor technologies has driven the need to produce high quality epitaxial films of one metal oxide upon another. Largely unrecognized in synthetic efforts is that some metal oxides offer strongly polar surfaces and interfaces that require electrostatic stabilization to avoid a physically implausible divergence in the potential. The present work examines these issues for epitaxial growth of anatase TiO{sub 2} on strontium titanate (001). Solid phase epitaxial regrowth yields only the (001) facet, while direct crystalline growth by atomic layer deposition yields both the (112) and (001). The presence of amorphous TiO{sub 2} during regrowth may provide preferential stabilization for formation of the (001) facet.

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

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


    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. PMID:26574580


    Alpha fetoprotein (AFP) is a marker for hepatocellular and germ cell carcinoma. There are many different techniques used for measuring AFP in blood where the most accurate one is the immunoassay technique. The aim of the present study was to evaluate, optimize and prepare anti-AFP solid phase coated beads and use it for the determination of AFP in serum. The anti-AFP polyclonal antibodies were prepared by immunization of five rats with a highly purified AFP antigen and the anti-sera obtained were used for coating polystyrene beads to obtain the solid phase coated beads. Also, the AFP antigen was labelled with 125 I using chloramin-T (Ch-T) as oxidizing agent and the tracer obtained was purified using sephadex G-25 (PD-10) chromatography. The assay was performed using a set of AFP standards prepared by diluting the cord blood. The suitable conditions for coating process were obtained which include pH 8, molarity of coating buffer 0.05 M, volume of coating buffer 100 ml and dilution of antibody 1:1000 for coating 1000 beads. Because the coated beads prepared using borate buffer is more suitable than prepared using carbonate or phosphate buffers, they were chosen to complete the optimization and validation study. The optimization and characterization of the assay were performed to evaluate the quality of the proposed system. The system prepared proved a low cost, simple, sensitive and accurate results. The prepared system can be used to evaluate AFP in the blood and this will be helpful in diagnosing some diseases such as hepatocellular carcinoma and neural tube defects

  17. Solid-Phase Thermophilic Aerobic Reactor (STAR) Processing of Fecal, Food, and Plant Residues


    A description of the Solid Waste Resource Recovery ALS-NSCORT projects: Solid Phase Thermophilic Aerobic Reactor (STAR), Nitrogen Cycling in Advanced Life Support Systems, and Plant-based Anaerobic-Aerobic Bioreactor Linked Operation (PAABLO). 26 pages.

  18. New methods and materials for solid phase extraction and high performance liquid chromatography

    Dumont, P.J.


    This paper describes methods for solid phase extraction and high performance liquid chromatography (HPLC). The following are described: Effects of Resin Sulfonation on the Retention of Polar Organic Compounds in Solid Phase Extraction; Ion-Chromatographic Separation of Alkali Metals In Non-Aqueous Solvents; Cation-Exchange Chromatography in Non-Aqueous Solvents; and Silicalite As a Stationary Phase For HPLC.

  19. Development of novel solid-phase protein formulations

    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

  20. Solid Phase Formylation of N-Terminus Peptides

    Anna Lucia Tornesello


    Full Text Available Formylation of amino groups is a critical reaction involved in several biological processes including post-translational modification of histones. The addition of a formyl group (CHO to the N-terminal end of a peptide chain generates biologically active molecules. N-formyl-peptides can be produced by different methods. We performed the N-formylation of two chemotactic hexapetides, Met1-Leu2-Lys3-Leu4-Ile5-Val6 and Met1-Met2-Tyr3-Ala4-Leu5-Phe6, carrying out the reaction directly on peptidyl-resin following pre-activation of formic acid with N,N-dicyclohexylcarbodiimmide (DCC in liquid phase. The overnight incubation at 4 °C resulted in a significant increase in production yields of formylated peptides compared to the reaction performed at room temperature. The method is consistently effective, rapid, and inexpensive. Moreover, the synthetic strategy can be applied for the formylation of all primary amines at N-terminus of peptide chains or amino groups of lysine side-chains in solid phase.

  1. Automated Solid-Phase Radiofluorination Using Polymer-Supported Phosphazenes

    Bente Mathiessen


    Full Text Available The polymer supported phosphazene bases PS-P2tBu and the novel PS-P2PEG allowed for efficient extraction of [18F]F− from proton irradiated [18O]H2O and subsequent radiofluorination of a broad range of substrates directly on the resin. The highest radiochemical yields were obtained with aliphatic sulfonates (69% and bromides (42%; the total radiosynthesis time was 35–45 min. The multivariate analysis showed that the radiochemical yields and purities were controlled by the resin load, reaction temperature, and column packing effects. The resins could be reused several times with the same or different substrates. The fully automated on-column radiofluorination methodology was applied to the radiosynthesis of the important PET radiotracers [18F]FLT and [18F]FDG. The latter was produced with 40% yield on a 120 GBq scale and passed GMP-regulated quality control required for commercial production of [18F]FDG. The combination of compact form factor, simplicity of [18F]F− recovery and processing, and column reusability can make solid phase radiofluorination an attractive radiochemistry platform for the emerging dose-on-demand instruments for bedside production of PET radiotracers.

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

    Veronika Mäde


    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.

  3. Quasi in situ observation of Si lateral solid phase epitaxy

    Ueno, T.; Kawai, K.; Morisawa, T.; Hatano, T.; Imai, S.; Kaneko, S.; Ohdomari, I.

    A quasi in situ observation of Si lateral solid phase epitaxy (L-SPE) has been carried out by an anneal-and-observe technique using a transmission electron microscope (TEM). For this observation, 3 mm Ø Si discs, which were thinned physically and chemically, were cut from a non-heated sample which had been prepared by depositing an amorphous Si (a-Si) film on the patterned amorphous insulator substrate. For the L-SPE growth, the thin specimens were heated in a furnace. The same areas of the same sample were repeatedly observed after an additional heating process at each interval. The direct origin of the (111) facet formation during the L-SPE growth has been precisely revealed by this method. Polygrains due to the random nucleation from the a-Si/a-insulator interface have been found to obstruct further L-SPE growth, while the L-SPE growth continued in the adjacent polygrain-free regions. As a result of this non-uniform growth rate, the (111) facets which nucleated at the polygrains grew into V-shaped valleys and finally caused a zig-zag growth front.

  4. Solid Phase Microextraction for the Analysis of Nuclear Weapons

    Chambers, D M


    This document is a compendium of answers to commonly asked questions about solid phase microextraction as it relates to the analysis of nuclear weapons. We have also included a glossary of terms associated with this analytical method as well as pertinent weapons engineering terminology. Microextraction is a new collection technique being developed to nonintrusively sample chemicals from weapon headspace gases for subsequent analysis. The chemicals that are being targeted outgas from the high explosives and other organic materials used in the weapon assembly. This technique is therefore a valuable tool to: (1) remotely detect and assess the aging of Lawrence Livermore National Laboratory (LLNL) and, in some cases, Sandia National Laboratory (SNL) organic materials; and (2) identify potential compatibility issues (i.e., materials interactions) that should be more carefully monitored during surveillance tear-downs. Microextraction is particularly attractive because of the practical constraints inherent to the weapon surveillance procedure. To remain transparent to other core surveillance activities and fall within nuclear safety guidelines, headspace analysis of the weapons requires a procedure that: (1) maintains ambient temperature conditions; (2) allows practical collection times of less than 20 min; (3) maintains the integrity of the weapon gas volume; (4) provides reproducible and quantitative results; and (5) can identify all possible targets.

  5. Phase I studies of porfiromycin (NSC--56410) in solid tumors.

    Grage, T B; Weiss, A J; Wilson, W; Reynolds, V


    Porfiromycin was given to a group of patients with a variety of solid tumors. Of 114 patients admitted to the study, 103 yielded evaluable data. The following dosage schedules were used to determine the toxicity of porfiromycin when given in multiple doses by intravenous injection: 0.2 mg/kg x 5 days, 0.3 mg/kg x 5 days, 0.35 mg/kg x 5 days, 0.4 mg/kg x 5 days, 0.24 mg/kg x 10 days and 0.6 mg/kg weekly. Toxic effects noted were mainly leukopenia, thrombocytopenia, and, when injected paravenously, local tissue necrosis. Biological effects were noted at all dosage levels and were more severe at the higher dosages. The data suggest that profiromycin administered intravenously at a dose of 0.35 mg/kg daily for 5 days results in moderate hermatological toxicity and clinical evaluation in a Phase II study at this dosage level is indicated. PMID:1177472

  6. Solid phase group specific absorbants in assays for glycoproteins

    The focus of this paper is on several technical advances in the assays for glycoprotein hormones and enzymes that have been achieved by use of the solid phase carbohydrate specific adsorbant concanavalin-A. Puriffication of glycoprotein radioligand after labelling by the chloramine-T method is readily accomplished using a small column of agarose bound concanavalin-A which separates glycoprotein radioligand from radioiodide and radiolabelled unadsorbed contaminants. After concanavalin-A column chromatography, radiolabelled glycoprotein hormone preparations exhibited improved binding to antibodies and tissue receptors. To increase the effective sensitivity of radioimmunoassays for glycoproteins, agarose bound concanavalin-A is used to extract and concentrate the glycoproteins from various biologic samples. For example, the effective sensitivity for the detection of human thyrotropin in serum was improved approximately 5 fold by using concanavalin-A concentrates of 1.5 ml of serum. Partial purification of the glycoprotein dopamine-β-hydroxylase from serum using agarose bound concanavalin-A resulted in separation of the serum factors that interfere with the measurement of enzyme activity. We conclude that in assays for glycoproteins, concanavalin-A is useful for purification of radioligand, for preparation of concentrates of glycoproteins from biologic samples, and for separation of glycoproteins from various interfering factors contained in biologic samples prior to radioligand or radioenzyme assay. (orig.)

  7. Solid phase epitaxy of amorphous silicon carbide: Ion fluence dependence

    We have investigated the effect of radiation damage and impurity concentration on solid phase epitaxial growth of amorphous silicon carbide (SiC) as well as microstructures of recrystallized layer using transmission electron microscopy. Single crystals of 6H-SiC with (0001) orientation were irradiated with 150 keV Xe ions to fluences of 1015 and 1016/cm2, followed by annealing at 890 deg. C. Full epitaxial recrystallization took place in a specimen implanted with 1015 Xe ions, while retardation of recrystallization was observed in a specimen implanted with 1016/cm2 Xe ions. Atomic pair-distribution function analyses and energy dispersive x-ray spectroscopy results suggested that the retardation of recrystallization of the 1016 Xe/cm2 implanted sample is attributed to the difference in amorphous structures between the 1015 and 1016 Xe/cm2 implanted samples, i.e., more chemically disordered atomistic structure and higher Xe impurity concentration in the 1016 Xe/cm2 implanted sample

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

    Emma Dixon

    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. A study on nuclear propulsion using gas-solid two-phase flow

    Miyato, Naoaki; Kataoka, Isao; Serizawa, Akimi [Kyoto Univ. (Japan). Faculty of Engineering


    A solid core nuclear rocket has been considered a candidate for the first manned mission to Mars. The reason is that the solid core nuclear rocket has higher specific impulse than a chemical rocket. But its engine thrust is as much as that of the chemical rocket. We have thought of use of gas-solid two-phase flow for higher engine thrust on nuclear thermal propulsion and examined the effect of gas-solid two-phase flow on the engine thrust and the specific impulse of the solid core nuclear rocket. (author)

  10. Equilibrium phases surrounding the αZr solid solution in the Zr-Sn-O system

    Phases in equilibrium with the αZr solid solution from 1010-1314oC (1287-1587 K) in zirconium-tin-oxygen alloys were characterized and their compositions were determined. The experimental results provide information on the equilibria of the αZr solid solution in order to propose tentative boundaries at isothermal sections of the phase diagram. (Author)

  11. Solid-state retrodirective phased array concepts for microwave power transmission from Solar Power Satellite

    Schroeder, K. G.; Petroff, I. K.


    Two prototype solid-state phased array systems concepts for potential use in the Solar Power Satellite are described. In both concepts, the beam is centered on the rectenna by means of phase conjugation of a pilot signal emanating from the ground. Also discussed is on-going solid-state amplifier development.

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

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


    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...

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

    Ambrose, D.


    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. Porous, High Capacity Coatings for Solid Phase Microextraction by Sputtering.

    Diwan, Anubhav; Singh, Bhupinder; Roychowdhury, Tuhin; Yan, DanDan; Tedone, Laura; Nesterenko, Pavel N; Paull, Brett; Sevy, Eric T; Shellie, Robert A; Kaykhaii, Massoud; Linford, Matthew R


    We describe a new process for preparing porous solid phase microextraction (SPME) coatings by the sputtering of silicon onto silica fibers. The microstructure of these coatings is a function of the substrate geometry and mean free path of the silicon atoms, and the coating thickness is controlled by the sputtering time. Sputtered silicon structures on silica fibers were treated with piranha solution (a mixture of concd H2SO4 and 30% H2O2) to increase the concentration of silanol groups on their surfaces, and the nanostructures were silanized with octadecyldimethylmethoxysilane in the gas phase. The attachment of this hydrophobic ligand was confirmed by X-ray photoelectron spectroscopy and contact angle goniometry on model, planar silicon substrates. Sputtered silicon coatings adhered strongly to their surfaces, as they were able to pass the Scotch tape adhesion test. The extraction time and temperature for headspace extraction of mixtures of alkanes and alcohols on the sputtered fibers were optimized (5 min and 40 °C), and the extraction performances of SPME fibers with 1.0 or 2.0 μm of sputtered silicon were compared to those from a commercial 7 μm poly(dimethylsiloxane) (PDMS) fiber. For mixtures of alcohols, aldehydes, amines, and esters, the 2.0 μm sputtered silicon fiber yielded signals that were 3-9, 3-5, 2.5-4.5, and 1.5-2 times higher, respectively, than those of the commercial fiber. For the heavier alkanes (undecane-hexadecane), the 2.0 μm sputtered fiber yielded signals that were approximately 1.0-1.5 times higher than the commercial fiber. The sputtered fibers extracted low molecular weight analytes that were not detectable with the commercial fiber. The selectivity of the sputtered fibers appears to favor analytes that have both a hydrophobic component and hydrogen-bonding capabilities. No detectable carryover between runs was noted for the sputtered fibers. The repeatability (RSD%) for a fiber (n = 3) was less than 10% for all analytes tested

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

    Both slurry-phase and solid-phase bioremediation are effective ex situ soil decontamination methods. Slurry is energy intensive relative to solid-phase treatment, but provides homogenization and uniform nutrient distribution. Limited contaminant bioavailability at concentrations above the required cleanup level reduces biodegradation rates and renders solid phase bioremediation more cost effective than complete treatment in a bioslurry reactor. Slurrying followed by solid-phase bioremediation combines the advantages and minimizes the weaknesses of each treatment method when used alone. A biological treatment system consisting of slurrying followed by aeration in solid phase bioreactors was developed and tested in the laboratory using a silty clay load contaminated with diesel fuel. The first set of experiments was designed to determine the impact of the water content and mixing time during slurrying on the ate and extent of contaminant removal in continuously aerated solid phase bioreactors. The second set of experiments compared the volatile and total diesel fuel removal in solid phase bioreactors using periodic and continuous aeration strategies

  16. Liquid-solid phase extraction of rare earth chlorides by oil sulfoxides

    Liquid - solid phase extraction of rare earth chlorides by oil sulfoxides is studied. It is determined that during extraction of anhydrous rare earth chlorides organic phase is enriched by heavy lanthanides. During extraction of crystal hydrates (H2O:M>5) it enriched by light lanthanides and separation factor increases with temperature growth. It is pointed out that solvent nature does not offer essential effect on isolation of chlorides of d- and f-elements during liquid - solid phase extraction

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

    Benson, D.K.; Webb, J.D.; Burrows, R.W.; McFadden, J.D.O.; Christensen, C.


    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.

  18. Crystallization and phase changes in paracetamol from the amorphous solid to the liquid phase.

    Sibik, Juraj; Sargent, Michael J; Franklin, Miriam; Zeitler, J Axel


    For the case of paracetamol, we show how terahertz time-domain spectroscopy can be used to characterize the solid and liquid phase dynamics. Heating of supercooled amorphous paracetamol from 295 K in a covered sample under vacuum leads to its crystallization at 330 K. First, form III is formed followed by the transformation of form III to form II at 375 K, to form I at 405 K, and finally melting is observed around 455 K. We discuss the difference between the featureless spectra of the supercooled liquid and its liquid melt. Lastly, we studied the onset of crystallization from the supercooled liquid in detail and quantified its kinetics based on the Avrami-Erofeev model. We determined an effective rate constant of k = 0.056 min(-1) with a corresponding onset of crystallization at T = 329.5 K for a heating rate of 0.4 K min(-1). PMID:24579729

  19. Quantitative characterization of solid state phases by secondary neutral mass spectrometry

    Oechsner, H.; Getto, R.; Kopnarski, M.


    The quantitative determination of chemical solid phases by secondary neutral mass spectrometry (SNMS) based on the quantitative character of this technique is described and demonstrated for several thin film structures. The intermetallic phases in a Ni-Zn coating on Fe are shown to be achieved directly from the concentration ratios determined by SNMS. When correlating the local elemental concentration tupels with the corresponding phase fractions by a matrix equation, the determination of chemical solid phase depth profiles becomes possible. This is exemplified by the detection of temperature induced chemical phases in Ni and Ti/Si films on SiC substrates.

  20. Design and Synthesis of a Dual Linker for Solid Phase Synthesis of Oleanolic Acid Derivatives

    Shaorong Wang


    Full Text Available A hydrophilic amino-terminated poly(ethylene glycol-type dual linker for solid phase synthesis of oleanolic acid derivatives using trityl chloride resin was designed and synthesized for the first time. Model reactions in both liquid and solid phase were performed to show the feasibility of its selective cleavage at two different sites. The biological assay results indicated that the long and flexible alkyl ether functionality in the linker is less likely to be critical for the binding event. Following the successful solid-phase synthesis of model compounds, the potential of this dual linker in reaction monitoring and target identification is deemed worthy of further study.

  1. Temperature and phase dependence of positron lifetimes in solid cyclohexane

    Eldrup, Morten Mostgaard


    The temperature dependence of position lifetimes in both the brittle and plastic phases of cyclohaxane has been examined. Long-lived components in both phases are associated with the formation of positronium (Ps). Two long lifetimes attributable to ortho-Ps are resolvable in the plastic phase. The...

  2. Quantum control of two-photon photochromism in a solid-state phase

    The possibility of the phase and polarization control of the photochromism event in the solid-state phase is experimentally demonstrated. The quantum control of the photochromic processes initiated by the two-photon absorption of the femtosecond laser pulses in the spiropyran voluminous polymer sample is accomplished through the change in the polarization state and phase modulation parameter of the laser pulses

  3. Liquid phase sintering, II: Computer study of skeletal settling and solid phase extrication in a microgravity environment

    Nikolić Z.S.


    Full Text Available A two-dimensional numerical method based on the Brownian motion model and on the Densification model for simulation of liquid phase sintering in microgravity environment will be developed. Both models will be based on domain topology (two-dimensional particle representation and control volume methodology and on three submodels for domain translation, solid skeleton formation and domain extrication. This method will be tested in order to conduct a study of diffusion phenomena and microgravitational effects on microstructural evolution influenced by skeletal settling combined with solid-phase extrication during liquid phase sintering of porous W-Ni system.

  4. On-chip solid phase extraction coupled with electrophoresis using modified magnetic microspheres as stationary phase


    A poly(dimethylsiloxane)(PDMS)/glass hybrid microchip for on-line solid phase extraction (SPE) and electrophoresis separation has been developed and evaluated. The SPE microchannel was crossed to the electrophoresis microchannel. All the microfluidic channels were etched on the glass substrate. The magnetic microspheres were coated with hydroxyl-terminated poly-dimethylsiloxane (PDMS-OH) serving as extraction phase,which could be conveniently immobilized into the sample pretreatment channel by magnetic field. The PDMS-OH microspheres were mobilized into and out of the pretreatment channel by injection flow. The 0.1 μmol/L solution of fluorescence isothiocyanate (FITC)-labeled phenylalanine (Phe) was electrically injected into the SPE channel and extracted onto the PDMS-OH microspheres bed. The enriched FITC-labeled Phe was electrically eluted by 9 mmol/L sodium acetate containing 10% acetonitrile and electrically driven into the electrophoresis channel and then separated. The preconcentration factor could reach 87.5 after sufficient extraction. A linear preconcentration curve was obtained with the initial FITC-labeled Phe concentration ranging from 6 nmol/L to 300 nmol/L (R2=0.9922) with 200 s loading time. The detection limit (S/N=3) for the FITC-labeled Phe was 3 nmol/L.

  5. Preparation and application of magnetic particle solid-phase second antibody for RIA

    A separation reagent of magnetic particle solid-phase second antibody for RIA has been studied. Amine silane modulated magnetic particles were activated using glutaraldehyde and coupled with purified second antibody at different pH values. And the experiment on adsorption of purified second antibody by non-activated magnetic particles at pH 8 was carried out simultaneously. The RIA test demonstrated that the binding percentage of non-activated magnetic particle solid-phase was lower and its stability was less than that of the activated magnetic particle solid-phase. The sensitivity was increased and the correlation coefficient of standard cure was 0.9950 for the activated magnetic particle solid-phase second antibody for CEA RIA. The correlation coefficient of the testing concentration in RIA between separations with liquid-phase and solid-phase was 0.9895. Therefore, it is possible for the magnetic particle solid-phase to be used as a general separation reagent for RIA. (authors)

  6. Solid-phase distribution in an airlift reactor with an enlarged degassing zone

    Freitas, Carla Maria Duarte de; Teixeira, J.A.


    The distribution of the solid-phase in an airlift reactor of the concentric draught tube type, with an enlarged degassing zone, has been determined. Samples were taken at eight points of the reactor for various airflow rates, solids loading and density. Hold-up of solids varied considerably within the reactor. The highest value, for all tested experimental conditions, was obtained immediately above the top of the riser and the lowest value near the wall of the degassing zone.

  7. Study on New Sensitive Method of Determination of Phosphorus by Solid Phase Spectrophotometry


    The use of solid phase spectrophotometry for the determination of trace phosphorus in the system of phosphomolybdate-fructose is described. The adsorption of the system on anion-exchange resin is reported.

  8. Fast, copper-free click chemistry: a convenient solid-phase approach to oligonucleotide conjugation

    Singh, Ishwar; Vyle, Joseph S.; Heaney, Frances


    Solid-phase oligonucleotide conjugation by nitrile oxide–alkyne click cycloaddition chemistry has been successfully demonstrated; the reaction, compatible with all nucleobases, requires no metal catalyst and proceeds under physiological conditions.

  9. Use of track detectors in solid phase in solving of radon problems

    In this thesis track detectors in solid phase in solving of radon problems were used. Risk of lung carcinomas formation is estimated. Results of radon monitoring in houses and caves in the Slovak Republic are presented

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

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


    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 ...


    Gavrilenko, N. A.; Saranchina, N. V.; Gavrilenko, M. A.


    This paper presents a solid-phase spectrophotometric method for the determination selenium(IV). The proposed method is based on the reaction between the selenium(IV) and dithizone immobilized into transparent polymethacrylate matrix in strongly acidic solution. It was shown that the interaction of selenium(IV) with dithizone in solid phase was accompanied by the formation of the complex with an absorption maximum 420 nm. The change of absorption at wavelength 610 nm corresponding to absorptio...

  12. Molecularly Imprinted Solid-Phase Extraction and Liquid Chromatography for Biological Samples

    Möller, Kristina


    This thesis focuses on the use of molecularly imprinted polymers as selective sorbents for solid-phase extraction (MISPE). The MISPE methods developed were mainly intended for use with biological samples, such as human urine and blood plasma. These body fluids are complex samples, which often need an effective clean-up step before analysis to reduce the levels of possible interfering substances from the matrix, especially if the analytes are present in trace amounts. Solid-phase extraction (S...

  13. Design of molecularly imprinted polymers for sensors and solid phase extraction

    Subrahmanyam, Sreenath


    This thesis presents broadly the applications of molecularly imprinted polymers in sensors and solid phase extraction. Sensors for creatine and creatinine have been reported using a novel method of rational design of molecularly imprinted polymers (MIPs), and solid phase extraction of aflatoxin-B 1 has also been described in the thesis. A method for the selective detection of creataine and creatinine is reported in this thesis, which is based on the reaction between polymeri...

  14. Temperature and phase dependence of positron lifetimes in solid cyclohexane

    Eldrup, Morten Mostgaard


    longer of these (≈ 2.5 ns), which is temperature dependent, is ascribed to ortho-Ps trapped at vacancies. The shorter lifetime (≈ 0.9 ns), shows little temperature dependence. In contrast to most other plastic crystals, no sigmoidal behaviour of the average ortho-Ps lifetime is observed. A possibility......The temperature dependence of position lifetimes in both the brittle and plastic phases of cyclohaxane has been examined. Long-lived components in both phases are associated with the formation of positronium (Ps). Two long lifetimes attributable to ortho-Ps are resolvable in the plastic phase. The...

  15. New insights in Microbial Fuel Cells: novel solid phase anolyte

    Tonia Tommasi; Gian Paolo Salvador; Marzia Quaglio


    For the development of long lasting portable microbial fuel cells (MFCs) new strategies are necessary to overcome critical issues such as hydraulic pump system and the biochemical substrate retrieval overtime to sustain bacteria metabolism. The present work proposes the use of a synthetic solid anolyte (SSA), constituted by agar, carbonaceous and nitrogen sources dissolved into diluted seawater. Results of a month-test showed the potential of the new SSA-MFC as a long lasting low energy consu...

  16. New insights in Microbial Fuel Cells: novel solid phase anolyte

    Tommasi, Tonia; Salvador, Gian Paolo; Quaglio, Marzia


    For the development of long lasting portable microbial fuel cells (MFCs) new strategies are necessary to overcome critical issues such as hydraulic pump system and the biochemical substrate retrieval overtime to sustain bacteria metabolism. The present work proposes the use of a synthetic solid anolyte (SSA), constituted by agar, carbonaceous and nitrogen sources dissolved into diluted seawater. Results of a month-test showed the potential of the new SSA-MFC as a long lasting low energy consuming system.

  17. Direct MD simulation of liquid-solid phase equilibria for two-component plasmas

    Schneider, A. S.; Hughto, J.; Horowitz, C. J.; Berry, D. K.


    We determine the liquid-solid phase diagram for carbon-oxygen and oxygen-selenium plasma mixtures using two-phase MD simulations. We identified liquid, solid, and interface regions using a bond angle metric. To study finite size effects, we perform 27648 and 55296 ion simulations. To help monitor non-equilibrium effects, we calculate diffusion constants $D_i$. For the carbon-oxygen system we find that $D_O$ for oxygen ions in the solid is much smaller than $D_C$ for carbon ions and that both ...

  18. Positronium in solid phases of n-alkane binary mixtures

    Highlights: • Rotator phase in even alkanes CnH2n+2 with n ⩽ 20 appears in mixed samples only. • Interlamellar gap width is the same for shorter chain alkane concentration x and 1 − x. • Excess electron trapping diminishes with broadening of alkane chain distribution Δn. - Abstract: Binary mixtures of even-numbered normal alkanes CnH2n+2 and Cn+2H2n+6 with n ⩽ 18 were investigated by positron annihilation spectroscopy. Formation of the rotator phase was observed in mixed structures, while no such a phase in neat alkanes in this range of n was found. Phase diagrams for n = 18 and n = 16 are very similar to the diagrams for binary mixtures of odd-numbered alkanes. The effect of positronium formation with trapped excess electrons weakens with decreasing n, at low n values the time constant of Ps rise contains the component much shorter than 1 h

  19. Research on the pattern of solid-liquid two-phase distribution in chemical process pump

    In order to explore the pattern of solid-liquid two-phase flow distribution in first stage of double-suction impeller and the double volute channel of the HD type petrol-chemical process pump, the flow field in double-suction impeller and double volute is simulated with the CFD software, by taking the Reynolds Averaged Navier Stokes equations as its governing equations, and the standard k-ε model for turbulence, derives the pattern of solid particle concentration distribution in the impeller and double volute channel under different initial particle concentrations and different particle diameters. The results show that in the double-suction impeller, solid phase distribution changes a lot along with the increase of initial particle concentration; the concentration near the back side is higher than the face side. Solid particles have the motion trend to the back side of blade in double-suction impeller along with the increase of particle diameters. In double volute channel, solid phase concentration distribution is uneven and solid particle concentration is relatively higher from section 1 to section 8. In the diffusion section, concentration is high in lateral side and low in medial side, the solid particles have the motion trend to the lateral side and the solid particle concentration is relatively higher.

  20. Application of nuclear techniques in two-phase liquid-solid particles hydrotransport investigations

    Zych Marcin


    Full Text Available The paper presents gamma radiation application to two-phase flow investigation in a vertical pipeline, where the flow of solid particles transported by water was examined by use of both: radiotracers and gamma-absorption method. The simultaneous use of two methods allows analyzing of important parameters of solid particles hydrotransport. In the described experiments as solid phase the ceramic models representing natural polymetallic ocean nodules were used. Radiotracers allow to track the movements of selected models, representing specified grain size and the designation of its velocity. However gamma-absorption method enables measurement of average solid-phase velocity. For analysis of electrical signals obtained from scintillation detectors the cross-correlation method has been applied.

  1. Application of nuclear techniques in two-phase liquid-solid particles hydrotransport investigations

    Zych, Marcin; Hanus, Robert; Vlasak, Pavel; Petryka, Leszek; Jaszczur, Marek


    The paper presents gamma radiation application to two-phase flow investigation in a vertical pipeline, where the flow of solid particles transported by water was examined by use of both: radiotracers and gamma-absorption method. The simultaneous use of two methods allows analyzing of important parameters of solid particles hydrotransport. In the described experiments as solid phase the ceramic models representing natural polymetallic ocean nodules were used. Radiotracers allow to track the movements of selected models, representing specified grain size and the designation of its velocity. However gamma-absorption method enables measurement of average solid-phase velocity. For analysis of electrical signals obtained from scintillation detectors the cross-correlation method has been applied.


    TANG Xuelin; QIAN Zhongdong; WU Yulin


    The dense solid-phase governing equations for two-phase flows are obtained by using the kinetic theory of gas molecules. Assuming that the solid-phase velocity distributions obey the Maxwell equations, the collision term for particles under dense two-phase flow conditions is also derived.In comparison with the governing equations of a dilute two-phase flow, the solid-particle's governing equations are developed for a dense turbulent solid-liquid flow by adopting some relevant terms from the dilute two-phase governing equations. Based on Cauchy-Helmholtz theorem and Smagorinsky model,a second-order dynamic sub-grid-scale (SGS) model, in which the sub-grid-scale stress is a function of both the strain-rate tensor and the rotation-rate tensor, is proposed to model the two-phase governing equations by applying dimension analyses. Applying the SIMPLEC algorithm and staggering grid system to the two-phase discretized governing equations and employing the slip boundary conditions on the walls, the velocity and pressure fields, and the volumetric concentration are calculated. The simulation results are in a fairly good agreement with experimental data in two operating cases in a conduit with a rectangular cross-section and these comparisons imply that these models are practical.

  3. Study of solid solution strengthening of alloying element with phase structure factors


    Using the empirical electron theory of solids and molecules (EET), the phase structure factors, nA and nB, of the carbon-containing structural units with mass fraction of carbon (wC) below 0.8% and the mono-alloy structural units with wC at 0.2% in austenite and martensite are calculated. The solid solution strengthening brought by C-containing interstitial solid solution and alloy-substitutional solid solution in γ-Fe and α-Fe is discussed at electron structural level. The coefficient (s) of solid solution strengthening is advanced according to the bonding force between atoms. The study shows that when the criterion is applied to the carbonaceous or alloying element-containing solid solution the results of calculation will coincide with the experimental result very well.

  4. Detecting Lesch-Nyhan syndrome by solid phase primer extension

    Shumaker, J.M.; Caskey, C.T. [Baylor College of Medicine, Houston, TX (United States); Metspalu, A.


    A mutation detection method based upon the wild type human HPRT sequence is presented for identification of Lesch Nyhan syndrome. The technique consists of performing a biotinlyated PCR amplification of the region of interest, followed by isolation and purification of single stranded template using magnetic separation. Allele-specific primers are annealed adjacent to the potential mutation site on the template. A terminal fluorescent deoxynucleotide addition is performed with a DNA template-dependent polymerase to distinguish between the mutant and wild-type sequence. The products are purified from unincorporated ddNTPs, eluted and finally analyzed on an ABI 373 to identify the mutation. The length of an extension primer is used as a position signature for mutations. The fidelity of nucleotide incorporation provides an excellent signal-to-noise ratio for the detection of nine HPRT mutations within eight cell lines. This method should detect all types of mutations except for repeated sequences that are longer than the primers. Moreover, the method is being extended to a solid support assay, whereby the extension primers are attached to a two-dimensional glass surface. Following extension, the solid support is analyzed for radioactive incorporation. We have shown the sequence determination of a five base region of a wild-type sequence and two different HPRT mutations. As more dense oligonucleotide arrays are produced, this method could be extended to sequence the complete coding region of HPRT.

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

    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

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

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


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

  7. Influences of solid particles on the formation of the third phase crud during solvent extraction

    ZHENG Qi; RUAN Renman; WEN Jiankang; SONG Yongsheng; DONG Qinghai; WU Minglin; YAO Guocheng


    The influences of solid particles in leach solution on the formation of the third phase crud during solvent extraction of copper were studied.Analyzed from the point of view of pH value and surface tension,the study results showed that the solid particle is one of the most important contributors for the formation of the third phase crud. During solvent extraction,if the pH value was greater than 2.30,the number of solid particles in the mother solution increased,in which case the possibility of forming the third phase crud could also increase,and the interface tension value might grow in pace with the quantity of the third phase crud.

  8. Stability of phases in (Ba, Gd)MnO3 solid solution system

    Migaku Kobayashi; Hidenori Tamura; Hiromi Nakano; Hirohisa Satoh; Naoki Kamegashira


    The existing phases in BaxGd1-xMnO3 solid solution system (0≦x≦1) were studied by analyzing the detailed crystal structure of each composition from the results of the Rietveld method using powder X-ray diffraction data. For a small substitution of Ba for Gd (0≦x<0.1), the orthorhombic phase with a perovskite type structure (Pnma space group) was stably formed and this fact was supported by the electron diffraction data. There existed an intermediate phase of Ba0.33Gd0.67MnO3, which was characterized as the tetragonal phase with perovskite structure. The composition range of this phase was narrow and almost line compound. Between the regions of these phases, there existed two-phase region. There was also a two-phase region between the intermediate tetragonal phase and BaMnO3. Measurement of electrical conductivities of these orthorhombic solid solutions and tetragonal phases showed semiconducting behaviors for both phases and the existence of the phase transition at high temperature for the orthorhombic phase. The transition temperature decreased as the Ba content increased.

  9. Positronium in solid phases of n-alkane binary mixtures

    Zgardzińska, B.; Goworek, T.


    Highlights: • Rotator phase in even alkanes C{sub n}H{sub 2n+2} with n ⩽ 20 appears in mixed samples only. • Interlamellar gap width is the same for shorter chain alkane concentration x and 1 − x. • Excess electron trapping diminishes with broadening of alkane chain distribution Δn. - Abstract: Binary mixtures of even-numbered normal alkanes C{sub n}H{sub 2n+2} and C{sub n+2}H{sub 2n+6} with n ⩽ 18 were investigated by positron annihilation spectroscopy. Formation of the rotator phase was observed in mixed structures, while no such a phase in neat alkanes in this range of n was found. Phase diagrams for n = 18 and n = 16 are very similar to the diagrams for binary mixtures of odd-numbered alkanes. The effect of positronium formation with trapped excess electrons weakens with decreasing n, at low n values the time constant of Ps rise contains the component much shorter than 1 h.

  10. Liquid-solid phase transitions in a deformable container

    Krejčí, Pavel; Rocca, E.; Sprekels, J.

    1. Berlin: Springer, 2010 - (Albers, B.), s. 285-300 ISBN 978-3-642-11444-1 Institutional research plan: CEZ:AV0Z10190503 Keywords : phase transition * energy balance * equilibrium state Subject RIV: BA - General Mathematics

  11. Flow characteristics of gas-liquid-solid three-phase bubbly flow in vertical pipes

    The volumetric fractions of each phase in air-water-particle three-phase bubbly flows were measured in vertical pipes of about 10 m in height, and of 20.9, 30.8 and 50.4 mm inside diameter, respectively. The solid particles used in this experiment were three kinds of spherical particles of 1.15, 2.56 and 4.16 mm mean diameter, made of aluminum ceramics with 2270-2400 kg/m3 density. Characteristics of the volumetric fractions of each phase were discussed in this experimental range, especially on the effects of the volumetric flux of each phase, pipe diameter and mean particle diameter. Then, empirical correlations of the volumetric fractions of each phase were proposed. The present empirical correlations would be useful as constitutive equations required to analyze the gas-liquid-solid three-phase bubbly flow in vertical pipes based on the slip flow model. (author)

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

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

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

    Phase coexistence in ferroelectric solid solutions near the tricritical point has been theoretically analyzed by using the Landau-Devonshire theory. Results revealed that different phases having similar potential wells could coexist in a narrow composition range near the tricritical point in the classical Pb(Zr1−xTix)O3 system. The potential barrier between potential wells increases with the decrease of temperature. Coexisting phases or different domains of the same phase can produce adaptive strains to maintain atomic coherency at the interfaces or domain walls. Such compatibility strains have influence on the energy potential as well as the stability of relative phases, leading to the appearance of energetically unfavorable monoclinic phases. Those competing and coexisting phases also construct an easy phase transition path with small energy barrier in between, so that very small stimuli can produce large response in compositions near the morphotropic phase boundary, especially near the tricritical point

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

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


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

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

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


    We have studied the complete two-dimensional phase diagram of a core-shell microgel-laden fluid interface by synchronizing its compression with the deposition of the interfacial monolayer. Applying a new protocol, different positions on the substrate correspond to different values of the monolayer surface pressure and specific area. Analyzing the microstructure of the deposited monolayers, we discovered an isostructural solid-solid phase transition between two crystalline phases with the same hexagonal symmetry, but with two different lattice constants. The two phases corresponded to shell-shell and core-core inter-particle contacts, respectively; with increasing surface pressure the former mechanically failed enabling the particle cores to come into contact. In the phase-transition region, clusters of particles in core-core contacts nucleate, melting the surrounding shell-shell crystal, until the whole monolayer moves into the second phase. We furthermore measured the interfacial rheology of the monolayers as a function of the surface pressure using an interfacial microdisk rheometer. The interfaces always showed a strong elastic response, with a dip in the shear elastic modulus in correspondence with the melting of the shell-shell phase, followed by a steep increase upon the formation of a percolating network of the core-core contacts. These results demonstrate that the core-shell nature of the particles leads to a rich mechanical and structural behavior that can be externally tuned by compressing the interface, indicating new routes for applications, e.g. in surface patterning or emulsion stabilization. PMID:26948023

  16. Predicting phase transition pressure in solids:a semiclasical possibility

    Celebonovic, V.


    This is a short review of the physical ideas,algorithm for the calculation of the phase transition pressure and some results of a semi-classical theory of the behaviour of materials under high pressure proposed by P.Savic and R.Kasanin.It is base on the Coulomb interaction,supplemented by a microscopic selection rule and a set of experimentally founded postulates,and it has found applications from DAC experiments to planetary structure modelling.

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

    Blonska-Tabero A.


    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.

  18. Solid phosphorus phase in aluminum- and iron-treated biosolids.

    Huang, Xiao-Lan; Chen, Yona; Shenker, Moshe


    Stabilization of phosphorus (P) in sewage sludge (biosolids) to reduce water-soluble P concentrations is essential for minimizing P loss from amended soils and maximizing the capacity of the soil to safely serve as an outlet for this waste material. The chemical form at which P is retained in biosolids stabilized by Al(2)(SO(4))(3) x 18H(2)O (alum) or FeSO(4) x 7H(2)O (FeSul) was investigated by scanning electron microscopy (SEM) equipped with energy-dispersive X-ray elemental spectrometry (EDXS) and by X-ray diffraction (XRD). Both treatments resulted in the formation of a Ca-P phase, probably brushite. Phosphorus was further retained in the alum-treated biosolids by precipitation of an Al-P phase with an Al/P molar ratio of about 1:1, while in the FeSul-treated biosolids, P was retained by both precipitation with Fe/P molar ratios of 1:1 or 1.5:1, and by adsorption onto newly formed Fe hydroxides exhibiting an Fe/P molar ratio of up to 11:1. All of these mechanisms efficiently reduced P solubility and are crucial in biosolids environmentally safe agronomic beneficial use for this waste product; however, each P phase formed may react differently in the amended soil, depending on soil properties. Thus, the proper P stabilization method would depend on the target soil. PMID:17332259

  19. Effect of temperature on the solubility and solid phase stability of zirconium hydroxide

    The solubility and solid phase stability of zirconium hydroxide was investigated in the acidic pH range after heating the aqueous samples at 50, 70 and 90 C. The solubility measured at room temperature after exposing the batch samples to elevated temperatures for a given period of time significantly decreased with increasing heating periods. The Zr concentrations at given pH after heating at 90 C for 3 weeks are about 5 orders of magnitude lower than the solubility of amorphous zirconium hydroxide (Zr(OH)4(am)) kept at room temperature. Size distributions of the Zr colloidal species after heating were investigated by sequential filtration using different pore-sized membranes, and the contribution of the colloidal species to the solubility was assessed. The TEM images and XRD spectra of the solid phases after heating indicated the agglomeration and crystallization of the initial amorphous hydroxide solid phase. The solid phase was identified as crystalline oxide after heating at 90 C. The solubility product determined from the solubility data excluding contributions of colloidal species is correlated to the particle size of the solid phase. (orig.)

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

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


    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. PMID:26905325

  1. Biogas production from municipal solid wastes using an integrated rotary drum and anaerobic-phased solids digester system.

    Zhu, Baoning; Zhang, Ruihong; Gikas, Petros; Rapport, Joshua; Jenkins, Bryan; Li, Xiujin


    This research was conducted to develop an integrated rotary drum reactor (RDR)-anaerobic-phased solids (APS) digester system for the treatment of municipal solid waste (MSW) to produce biogas energy and achieve waste reduction. A commercial RDR facility was used to provide a 3-d pretreatment and sufficient separation of the organics from MSW and then the organics were digested in a laboratory APS-digester system for biogas production. The organics generated from the RDR contained 50% total solids (TS) and 36% volatile solids (VS) on wet basis. The APS-digester was started at an organic loading rate (OLR) of 3.1 gVS L(-1) d(-1) and operated at three higher OLRs of 4.6, 7.7 and 9.2 gVS L(-1) d(-1). At the OLR of 9.2 gVS L(-1) d(-1) the system biogas production rate was 3.5 L L(-1) d(-1) and the biogas and methane yields were 0.38 and 0.19 L gVS(-1), respectively. Anaerobic digestion resulted in 38% TS reduction and 53% VS reduction in the organic solids. It was found that the total VFA concentration reached a peak value of 15,000 mg L(-1) as acetic acid in the first 3d of batch digestion and later decreased to about 500 mg L(-1). The APS-digester system remained stable at each OLRs for over 100d with the pH in the hydrolysis reactors in the range of 7.3-7.8 and the pH in the biogasification reactor in 7.9-8.1. The residual solids after the digestion had a high heating value of 14.7 kJ gTS(-1). PMID:20409703

  2. Numerical simulation of gas–liquid–solid three-phase flow using particle methods

    We want to simulate, based on particle methods, the dynamic behavior of multi-phase flows in a gas–solid–liquid mixture system. With the governing equations discretized within the finite volume particle method, the effects of contact and collision between solid particles were modeled by the distinct element method. Applicability of the viscosity model and an empirical drag force model were confirmed for the hydrodynamic interactions between solid particles and fluid. Simulations were performed of a single bubble rising in a tank of stagnant solid particle–liquid. The results for the dynamic behavior indicate that the present computational framework of particle-based simulation method may be useful for numerical simulations of multi-phase flow behavior in a solid particle–fluid mixture system. (author)

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

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


    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......), respectively. After considering three alternative explanations, we propose that the step upward in the ellipsometric signal observed at similar to 331 K on heating the submonolayer film is the signature of a transition from a perpendicular monolayer phase to a denser phase in which the alkane chains contain on...

  4. Etching and forward transfer of fused silica in solid-phase by femtosecond laser-induced solid etching (LISE)

    We present a femtosecond laser-based technique for etching and forward transfer of bulk transparent materials in solid-phase. Femtosecond laser pulses with λ=800 nm were focused through a fused silica block onto an absorbing thin film of Cr. A constraining Si wafer was pressed into tight contact with the Cr film to prevent lift-off of the film. A combination of the high temperature and pressure of the Cr, and compressive stress from the Si, resulted in etching of smooth features from the fused silica by cracking. Unlike in conventional ablative or chemical etching, the silica was removed from the bulk as single solid-phase pieces which could be collected on the Si. Using this so-called laser-induced solid etching (LISE) technique, 1-2 μm deep pits and channels have been produced in the silica surface, and corresponding dots and lines deposited on the Si. The threshold fluence for etching was found to be ∼0.4J/cm2 with ∼130 fs duration pulses. The morphology of the etched features are investigated as functions of fluence and exposure to multiple pulses.

  5. The study of solid phase removal from water using magnetite particles

    Радовенчик, В. М.; Радовенчик, Я. В.


    The results of research of the water treatment method effectiveness using high-dispersion magnetite particles were given. It was found that the treatment of wastewater after wastepaper recycling process, which contains a wide range of solid pollutants, using only the magnetite particles was ineffective. The pH adjustment can decrease residual content of solid phase in the treated water but it prevents reuse of such water. Best results can be obtained using additional reagents. Top coagulant e...

  6. Determination of Atrazine, Acetochlor, Clomazone, Pendimethalin and Oxyfluorfen in Soil by a Solid Phase Microextraction Method

    Rada Đurović; Jelena Gajić-Umiljendić; Tijana Đorđević


    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, extractio...

  7. Solid-Phase Synthesis of Modified Peptides as Putative Inhibitors of Histone Modifying Enzymes

    Cohrt, Anders Emil O'Hanlon

    for the solid-phase synthesis of thiourea- and guanidinemodified peptides are presented. By activating N,N ’-di-Boc-thiourea with Mukaiyama’s reagent or HgCl2, the N -terminal of solid-supported peptides could be cleanly converted into the corresponding thiourea or guanidine derivative. The reactions...... strategy was employed in the identification of individual library members. Changes in the acetylation pattern could also be detecting using a quantitative ninhydrin assay....

  8. Mixed Model for Silt-Laden Solid-Liquid Two-Phase Flows

    唐学林; 徐宇; 吴玉林


    The kinetic theory of molecular gases was used to derive the governing equations for dense solid-liquid two-phase flows from a microscopic flow characteristics viewpoint by multiplying the Boltzmann equation for each phase by property parameters and integrating over the velocity space. The particle collision term was derived from microscopic terms by comparison with dilute two-phase flow but with consideration of the collisions between particles for dense two-phase flow conditions and by assuming that the particle-phase velocity distribution obeys the Maxwell equations. Appropriate terms from the dilute two-phase governing equations were combined with the dense particle collision term to develop the governing equations for dense solid-liquid turbulent flows. The SIMPLEC algorithm and a staggered grid system were used to solve the discretized two-phase governing equations with a Reynolds averaged turbulence model. Dense solid-liquid turbulent two-phase flows were simulated for flow in a duct. The simulation results agree well with experimental data.

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

    Wang, Jianlong; Chu, Libing


    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. PMID:27396522

  10. Phosphorus Sorption and Redistribution on Soil Solid Phase in a Brazilian Haplorthox Amended with Bio solids

    Land application of bio solids (SS) can cause a buildup of phosphorus (P) in the top soil. The changes in the soil P characteristics may be assessed by the sorption isotherm and the sequential fractionation techniques. Samples of Haplorthox were collected from a field experiment where maize was cultivated for two years, after two applications of SS originated from two cities of San Paulo State, Brazil. SS applications added a total of 125, 250, 500, 1000 and 2000 kg ha-1 of P in the area. To perform the sorption isotherms and obtain P maximum sorption capacity (Omax) and the binding energy, soil samples were submitted to increasing P concentration solutions until equilibrium was reached. Sequential fractionation was done by a sequential extraction with CaCl2, NaHCO3, NaOH, HCl, and HNO3 + HClO4 (residual). Addition of bio solids from both cities to the soil decreased Qmax and the binding energy obtained by the Langmuir equation. SS additions changed the P fractions distribution in the soil by increasing the labile fractions (P-CaCl2 and P-NaHCO3) and the moderately labile fraction (P-NaOH) by 11.2% and 20.3%, respectively, in detriment of the most resistant P fraction

  11. The use of coal in a solid phase reduction of iron oxide

    Nokhrina, O. I.; Rozhihina, I. D.; Hodosov, I. E.


    The results of the research process of producing metalized products by solid-phase reduction of iron using solid carbonaceous reducing agents. Thermodynamic modeling was carried out on the model of the unit the Fe-C-O and system with iron ore and coal. As a result of modeling the thermodynamic boundary reducing, oxidizing, and transition areas and the value of the ratio of carbon and oxygen in the system. Simulation of real systems carried out with the gas phase obtained in the pyrolys of coal. The simulation results allow to determine the optimal cost of coal required for complete reduction of iron ore from a given composition. The kinetics of the processes of solid-phase reduction of iron using coal of various technological brands.

  12. Development and Optimization of Sepharose Solid Phase Radioimmunoassay for Estimation of Thyroid Stimulating Hormone

    The aim of the present study was oriented to develop, optimize and validate solid phase radioimmunoassay, through many studies on Sepharose, for estimation of thyroid stimulating hormone in humane serum. Preparation of polyclonal antibodies was carried out in host rabbit animals against TSH antigen followed by partial purification of 1gG. Linkage of antibody 1gG to activated Sepharose CL-4B was carried out after activation of Sepharose with 1,1- carbonyldiimidazole. Labeling of TSH was carried out using chloramine-T as an oxidizing agent and the labeled tracer was purified through PD-10 column. Extensive studies were carried out to obtain the optimum conditions of using solid phase Sepharose to reach higher separation efficiency. The results of validation tests reveal that the local solid phase system is precise and accurate for evaluation of thyroid disorders

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

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


    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 a...... 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....

  14. NASA satellite communications application research. Phase 2: Efficient high power, solid state amplifier for EFH communications

    Benet, James


    The final report describes the work performed from 9 Jun. 1992 to 31 Jul. 1993 on the NASA Satellite Communications Application Research (SCAR) Phase 2 program, Efficient High Power, Solid State Amplifier for EHF Communications. The purpose of the program was to demonstrate the feasibility of high-efficiency, high-power, EHF solid state amplifiers that are smaller, lighter, more efficient, and less costly than existing traveling wave tube (TWT) amplifiers by combining the output power from up to several hundred solid state amplifiers using a unique orthomode spatial power combiner (OSPC).

  15. Extraction of Pb2+ using Silica from Rice Husks Ash (RHA – Chitosan as Solid Phase

    Hanandayu Widwiastuti


    Full Text Available The existence of lead (Pb compounds in waters can be caused of waste pollution from industrial activities such as dye and battery industries. Lead has toxic characteristic and is able to causing deseases. The levels of Cr(VI can be decreased by methods such as electroplating, oxidation, reduction, and membrane separation. But this methods require high cost and produce a lot of waste. Furthermore, those methods cannot determine the small concentration of Pb2+. Therefore, solid phase extraction is used because it’s a simple method and can be used to preconcentrate Pb2+ ion. The aim of this study is to create solid phase from nature material as an alternative method to determine Pb2+ in water samples. The solid phase is silica from rice husks ash (RHA that was modified using chitosan. To achieve that aim, the optimization of silica : chitosan composition was done. The influence of Pb2+ concentration and citric acid concentration was studied to obtain optimum recovery of Pb2+. Interaction between Pb2+ ion and solid phase silica – chitosan could be estimated based on the result. The result showed the optimum composition of silica : chitosan is 65% silica : 35% chitosan with Cation Exchange Capacity (CEC 0.00455 mek/g. Mass Adsorbed Pb2+for 1 g silica : chitosan 65% is 9.715 mg/g. Optimum recovery of Pb2+ on solid phase extraction is reached at concentration of Pb2+ 10 ppm and citric acid concentration 0.05 M (88.25 % and 81.18 %. This result showed that solid phase extraction using silica – chitosan can be used as an alternative method to determine Pb2+ in water.

  16. Binary Solid-Liquid Phase Diagram of Phenol and t-Butanol: An Undergraduate Physical Chemistry Experiment

    Xu, Xinhua; Wang, Xiaogang; Wu, Meifen


    The determination of the solid-liquid phase diagram of a binary system is always used as an experiment in the undergraduate physical chemistry laboratory courses. However, most phase diagrams investigated in the lab are simple eutectic ones, despite the fact that complex binary solid-liquid phase diagrams are more common. In this article, the…

  17. Oxygen mass transfer in a high solids loading three-phase internal-loop airlift reactor

    Freitas, Carla Maria Duarte de; Teixeira, J.A.


    Determinations of volumetric mass transfer coefficient were conducted in a three-phase internal-loop airlift reactor with an enlarged degassing zone. The effect of parameters such as the airflow rate (riser superficial gas velocities between 0.01 and 0.5 m/s), solids loading (up to 30%, v/v), solids density (1023 and 1048 kg/m3) and the liquid-phase properties on kLa was studied. It was observed that the increase of the airflow rate and the introduction of ethanol enhanced the volume...

  18. Solid-Phase Synthetic Route to Multiple Derivatives of a Fundamental Peptide Unit

    Martin J. O’Donnell


    Full Text Available Amino acids are Nature’s combinatorial building blocks. When substituted on both the amino and carboxyl sides they become the basic scaffold present in all peptides and proteins. We report a solid-phase synthetic route to large combinatorial variations of this fundamental scaffold, extending the variety of substituted biomimetic molecules available to successfully implement the Distributed Drug Discovery (D3 project. In a single solid-phase sequence, compatible with basic amine substituents, three-point variation is performed at the amino acid a-carbon and the amino and carboxyl functionalities.

  19. Characteristics of temporal- spatial parameters in quasi- solid-fluid phase transition of granular materials


    The quasi-solid-fluid phase transition of granular materials is closely related to the shear rate and solid concentration in addition to their intrinsic properties. The contact duration and the coordination number are two important temporal-spatial parameters to describe the granular interaction in phase transition. In this study, characteristics of the contact duration and the coordination number associated with the transition processes are determined using a 3D discrete element model under different shear rates and concentrations. The resulting macroscopic stress and strain-rate relations are discussed. The temporal and spatial parameters provide a linkage between the macroscopic constitutive law and inter- particle micromechanics.

  20. Differing results of direct and indirect solid phase radioimmunoassay for HBsAg in acute hepatitis

    In 54 patients suffering from active viral hepatitis the indirect solid phase radioimmunoassay (ind-SPRIA) for HBsAg was positive in 9 cases the direct solid phase radioimmunoassay (d-SPRIA) being negative. In 2 further cases ind-SPRIA was positive during several weeks but d-SPRIA only once. AntiHBc could be detected in 9 of these patients. In 7 patients the usual decrease of the transaminase activity was followed by a second elavation with prolongation of the disease. The unknown factor detected by ind-SPRIA suggests a special of acute hepatitis. (orig.)

  1. Solid-Phase Spectrophotometric Analysis of 1-Naphthol Using Silica Functionalized with m-Diazophenylarsonic Acid.

    Zaitseva, Nataliya; Alekseev, Sergei; Zaitsev, Vladimir; Raks, Viktoria


    The m-aminophenylarsonic acid (m-APAA) was immobilized onto the silica gel surface with covalently grafted quaternary ammonium groups via ion exchange. The diazotization of ion-bonded m-APAA resulted in a new solid-phase spectrophotometric reagent for detection of 1-naphtol in environmental water samples. The procedure of solid-phase spectrophotometric analysis is characterized by 20 μg L(-1) limit of detection (LOD) of 1-naphtol, up to 2000 concentration factor, and insensitivity to the presence of natural water components as well as to 30-fold excess of phenol, resorcinol, and catechol. PMID:26979727

  2. Solid-Phase Spectrophotometric Analysis of 1-Naphthol Using Silica Functionalized with m-Diazophenylarsonic Acid

    Zaitseva, Nataliya; Alekseev, Sergei; Zaitsev, Vladimir; Raks, Viktoria


    The m-aminophenylarsonic acid (m-APAA) was immobilized onto the silica gel surface with covalently grafted quaternary ammonium groups via ion exchange. The diazotization of ion-bonded m-APAA resulted in a new solid-phase spectrophotometric reagent for detection of 1-naphtol in environmental water samples. The procedure of solid-phase spectrophotometric analysis is characterized by 20 μg L-1 limit of detection (LOD) of 1-naphtol, up to 2000 concentration factor, and insensitivity to the presence of natural water components as well as to 30-fold excess of phenol, resorcinol, and catechol.

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

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


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

  4. Holmium redistribution during solid phase epitaxial crystallization in amorphized silicon layers

    The concentration profiles of holmium were studied after annealing of silicon layers at 620 deg C. Silicon was implanted with Ho+ ions at 1 MeV energy and (1-3) · 1014 cm-2 doses. Recrystallization of amorphized silicon layer occurs by the mechanism of the solid phase epitaxy. The regularities of segregation redistribution of Ho impurity are similar to the Er redistribution regularities studied earlier. A decrease of Ho concentration at the initial stage of solid phase epitaxial recrystallization is due to a low velocity of mass transport through the crystal-amorphous interface

  5. Detection of ibuprofen and ciprofloxacin by solid-phase extraction and UV/Vis spectroscopy

    Zhou, Zhengwei; Jiang, Jia Qian


    A simple and economic solid-phase extraction coupled with UV/Vis spectrophotometric method is described for the analysis of ibuprofen and ciprofloxacin. Following solid-phase extraction from model wastewater samples containing standard ibuprofen or ciprofloxacin, elutes were analyzed by a UV/Vis spectrophotometer at 225 nm for ibuprofen and 280 nm for ciprofloxacin. The assay was linear for both compounds with good coefficients of correlation. This method shows good recoveries for both compounds with 101.0 ± 9.8% for ibuprofen and 99.4 ± 11.8% ciprofloxacin.

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

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


    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. PMID:27337593

  7. 2,6-Diketopiperazines from amino acids, from solution-phase to solid-phase organic synthesis.

    Perrotta, E; Altamura, M; Barani, T; Bindi, S; Giannotti, D; Harmat, N J; Nannicini, R; Maggi, C A


    A method to prepare 1,3-disubstituted 2,6-diketopiperazines (2,6-DKP) as useful heterocyclic library scaffolds in the search of new leads for drug discovery is described. The method can be used in solution-phase and solid-phase conditions. In the key step of the synthesis, the imido portion of the new molecule is formed in solution through intramolecular cyclization, under basic conditions, of a secondary amide nitrogen on a benzyl ester. A Wang resin carboxylic ester is used as the acylating agent under solid-phase conditions, allowing the cyclization to take place with simultaneous cleavage of the product from the resin ("cyclocleavage"). The synthetic method worked well with several couples of amino acids, independently from their configuration, and was used for the parallel synthesis of a series of fully characterized compounds. The use of iterative conditions in the solid phase (repeated addition of fresh solvent and potassium carbonate to the resin after filtering out the product-containing solution) allowed us to keep diastereoisomer content below the detection limit by HPLC and (1)H NMR (200 MHz). PMID:11549363

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

    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

  9. Mechanism and microstructures in Ga2O3 pseudomartensitic solid phase transition.

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


    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

  10. Phase wettability and microstructural evolution in solid oxide fuel cell anode materials

    Recent experimental and theoretical findings suggest that high-temperature solid oxide fuel cells (SOFCs) often suffer from performance degradation due to coarsening of the metallic-phase particles within the anode. In this study, we explore the feasibility of improving the microstructural stability of SOFC anode materials by tuning the contact angle between the metallic phase and electrolyte particles. To this end, a continuum diffuse-interface model is employed to capture the coarsening behavior of the metallic phase and simulate a range of equilibrium contact angles. The evolution of performance-critical, microstructural features is presented for varying degrees of phase wettability. It is found that both the density of electrochemically active triple- phase regions and contiguity of the electron-conducting phase display undesirable minima near the contact angle of conventional SOFC materials. Our results suggest that tailoring the interfacial properties of the constituent phases could lead to a significant increase in the performance and lifetime of SOFCs

  11. Optical manipulation of Berry phase in a solid-state spin qubit

    Yale, Christopher G; Zhou, Brian B; Auer, Adrian; Burkard, Guido; Awschalom, David D


    The phase relation between quantum states represents an essential resource for the storage and processing of quantum information. While quantum phases are commonly controlled dynamically by tuning energetic interactions, utilizing geometric phases that accumulate during cyclic evolution may offer superior robustness to noise. To date, demonstrations of geometric phase control in solid-state systems rely on microwave fields that have limited spatial resolution. Here, we demonstrate an all-optical method based on stimulated Raman adiabatic passage to accumulate a geometric phase, the Berry phase, in an individual nitrogen-vacancy (NV) center in diamond. Using diffraction-limited laser light, we guide the NV center's spin along loops on the Bloch sphere to enclose arbitrary Berry phase and characterize these trajectories through time-resolved state tomography. We investigate the limits of this control due to loss of adiabiaticity and decoherence, as well as its robustness to noise intentionally introduced into t...


    S. Manna


    Full Text Available High performance liquid chromatographic determination of organophosphorous compound has been done by reverse phase chromatography in goats. The goats were dying showing the symptoms of organophosphorous poisoning. The viscera and stomach contents sample were received from Project Co-Ordinator, Animal Disease Research Institute, Phulnakhara, Cuttack, Orissa. The analysis of samples by HPLC with UV detector after cleaning up in Solid Phase Extraction (SPE revealed presence of malathion that was later quantified.

  13. Dipolar recoupling in solid state NMR by phase alternating pulse sequences

    J. Lin; Bayro, M.; Griffin, R G; Khaneja, N.


    We describe some new developments in the methodology of making heteronuclear and homonuclear recoupling experiments in solid state NMR insensitive to rf-inhomogeneity by phase alternating the irradiation on the spin system every rotor period. By incorporating delays of half rotor periods in the pulse sequences, these phase alternating experiments can be made γ encoded. The proposed methodology is conceptually different from the standard methods of making recoupling experiments robust by the u...

  14. Application of SMES coordinated with solid-state phase shifter toload frequency control

    Ngamroo, I.; Mitani, Yasunori; K. Tsuji


    This paper proposes a sophisticated application of SMES to load frequency control (LFC) in an interconnected power system. The SMES is coordinated with a solid-state phase shifter to enhance the LFC. The frequency control concept and control design of a SMES coordinated with a phase shifter are presented. Numerical results demonstrate the significant effects of LFC by the proposed control and the economical advantage of MJ capacity of SMES

  15. Treatment technologies of liquid and solid wastes from two-phase olive oil mills

    Rincón, Bárbara; Raposo, Francisco; Borja, Rafael


    Over the last 10 years the manufacture of olive oil has undergone important evolutionary changes in the equipment used for the separation of olive oil from the remaining components. The latest development has been the introduction of a two-phase centrifugation process in which a horizontally-mounted centrifuge is used for a primary separation of the olive oil fraction from the vegetable solid material and vegetation water. Therefore, the new two-phase olive oil mills produce three identifiabl...

  16. Treatment technologies of liquid and solid wastes from two-phase olive oil mills

    Borja Padilla, Rafael; Raposo Bejines, Francisco; Rincón, Bárbara


    Over the last 10 years the manufacture of olive oil has undergone important evolutionary changes in the equipment used for the separation of olive oil from the remaining components. The latest development has been the introduction of a two-phase centrifugation process in which a horizontally-mounted centrifuge is used for a primary separation of the olive oil fraction from the vegetable solid material and vegetation water. Therefore, the new two-phase olive oil mills produce three ident...

  17. Application of the method of solid-phase spectrometry for test-determination of antioxidants

    Бельтюкова, C. D.; Лівенцова, О. О.; СТЕПАНОВА А.А.


    The work reveals advantages of a method of solid-phase spectrometry, with registration of a luminescent signal of anolyte in a sorbent phase in paticular, compared with usual spectroscopic methods. The possibility of use of a sensitized luminescence of lanthanides (ions of Terbium(III) ) as a luminescent marker when determining antioxidants of polyphenolic type is established. Advantages of this method, allowing to carry out quality control, safety or falsifications of foodstuff are noted. Th...

  18. Phase I study of afatinib combined with nintedanib in patients with advanced solid tumours

    Bahleda, Rastislav; Hollebecque, Antoine; Varga, Andrea; Gazzah, Anas; Massard, Christophe; Deutsch, Eric; Amellal, Nadia; Farace, Françoise; Ould-Kaci, Mahmoud; Roux, Flavien; Marzin, Kristell; Soria, Jean-Charles


    Background: This Phase I study evaluated continuous- and intermittent-dosing (every other week) of afatinib plus nintedanib in patients with advanced solid tumours. Methods: In the dose-escalation phase (n=45), maximum tolerated doses (MTDs) were determined for continuous/intermittent afatinib 10, 20, 30 or 40 mg once daily plus continuous nintedanib 150 or 200 mg twice daily. Secondary objectives included safety and efficacy. Clinical activity of continuous afatinib plus nintedanib at the MT...

  19. Volatile profile of yellow passion fruit juice by static headspace and solid phase microextraction techniques

    Gilberto Costa Braga; Adna Prado; Jair Sebastião da Silva Pinto; Severino Matias de Alencar


    The profile of volatile compounds of yellow passion fruit juice was analyzed by solid phase microextraction headspace (HS-SPME) and optimized static headspace (S-HS) extraction techniques. Time, temperature, NaCl concentration and sample volume headspace equilibrium parameters was adjusted to the S-HS technique. The gaseous phase in the headspace of samples was collected and injected into a gas chromatograph coupled to a mass spectrometer. In the HS-SPME technique was identified 44 volatile c...

  20. Influence of copolymer composition on the phase behavior of solid dispersions.

    Prudic, Anke; Kleetz, Tobias; Korf, Marcel; Ji, Yuanhui; Sadowski, Gabriele


    The incorporation of poorly soluble active pharmaceutical ingredients (APIs) into excipients (e.g., polymers) to formulate an amorphous solid dispersion is a promising strategy to improve the oral bioavailability of the API. The application of copolymer excipients allows access to combinations of different monomers and thus to the design of excipients to improve solid-dispersion properties. In this work, the thermodynamic phase behavior of solid dispersions was investigated as a function of the API, type of monomer, and copolymer composition. The glass-transition temperatures and API solubilities in the solid dispersions of naproxen and indomethacin in polyvinylpyrrolidone, polyvinyl acetate, and copolymers with different weight fractions of vinylpyrrolidone and vinyl actetate were investigated. It is shown that the thermodynamic phase behavior of API/copolymer solid dispersions is a function of monomer type and copolymer composition. This effect was also predicted by using the perturbed-chain statistical associating fluid theory (PC-SAFT). The glass-transition temperature of the solid dispersions was calculated with the Gordon-Taylor equation. PMID:25295846

  1. Optically driven atomic coherences: from the gas phase to the solid state

    Full text: Coherent interactions between strong radiation and quantum systems provide well-established tools to control optical properties and processes. Among others, applications aim at efficient data storage and processing of optically stored data, e.g. as required in quantum information processing. Thus, a large number of experimental studies in quantum information science have been conducted in atomic media in the gas phase. Only few experiments on coherent, adiabatic interactions were conducted in solid state media. Appropriate solid materials for such investigations are quantum dots, color centers, or rare-earth doped solids. The latter combine the advantages of atoms in the gas phase, i.e. spectrally narrow transitions and long dephasing times, with the advantages of solids, i.e. large density and scalability. In the talk we present implementations of coherent interactions in a rare-earth doped solid, i.e. a Pr:YSO crystal. In particular we report on the experimental implementation of stimulated Raman adiabatic passage (STIRAP) in Pr:YSO. Our data provide clear and striking proof for complete population inversion between hyperfine levels in the praseodymium dopants. Time-resolved absorption measurements serve to monitor the adiabatic population dynamics during the STIRAP process. We will discuss the possibilities of STIRAP and related techniques to drive atomic coherences in the solid state environment, e.g. for applications in optical and quantum information processing. (author)

  2. Dynamically slow solid-to-solid phase transition induced by thermal treatment of DimimFeCl4 magnetic ionic liquid.

    de Pedro, Imanol; Fabelo, Oscar; García-Saiz, Abel; Vallcorba, Oriol; Junquera, Javier; Blanco, Jesús Angel; Waerenborgh, João Carlos; Andreica, D; Wildes, Andrew; Fernández-Díaz, María Teresa; Fernández, Jesús Rodríguez


    The results reported here represent the first direct experimental observations supporting the existence of a solid-to-solid phase transition induced by thermal treatment in magnetic ionic liquids (MILs). The phase transitions of the solid phases of 1,3-dimethylimidazolium tetrachloroferrate, DimimFeCl4, are closely related to its thermal history. Two series of solid-to-solid phase transitions can be described in this MIL: (i) from room temperature (RT) phase II [space group (s.g.) = P21] to phase I-a [s.g. = P212121] via thermal quenching or via fast cooling at T > 2 K min(-1); (ii) from phase I-a to phase I-b [s.g. = P21/c] when the temperature was kept above 180 K for several minutes. The latter involves a slow translational and reorientational dynamical process of both the imidazolium cation and the tetrachloroferrate anion and has been characterized using synchrotron and neutron powder diffraction and DFT (density functional theory) studies. The transition is also related to the modification of the super-exchange pathways of low-temperature phases which show a overall antiferromagnetic behavior. A combination of several experimental methods such as magnetometry, Mössbauer and muon spectroscopy together with polarized and non-polarized neutron powder diffraction has been used in order to characterize the different features observed in these phases. PMID:27439896

  3. Ni coarsening in the three-phase solid oxide fuel cell anode - a phase-field simulation study

    Chen, Hsun-Yi; Cronin, J Scott; Wilson, James R; Barnett, Scott A; Thornton, Katsuyo


    Ni coarsening in Ni-yttria stabilized zirconia (YSZ) solid oxide fuel cell anodes is considered a major reason for anode degradation. We present a predictive, quantative modeling framework based on the phase-field approach to systematically examine coarsening kinetics in such anodes. The initial structures for simulations are experimentally acquired functional layers of anodes. Sample size effects and error analysis of contact angles are examined. Three phase boundary (TPB) lengths and Ni surface areas are quantatively identified on the basis of the active, dead-end, and isolated phase clusters throughout coarsening. Tortuosity evolution of the pores is also investigated. We find that phase clusters with larger characteristic length evolve slower than those with smaller length scales. As a result, coarsening has small positive effects on transport, and impacts less on the active Ni surface area than the total counter part. TPBs, however, are found to be sensitive to local morphological features and are only i...

  4. Phosphopeptide Characterization by Mass Spectrometry using Reversed-Phase Supports for Solid-Phase β-Elimination/Michael Addition

    Nika, Heinz; Lee, Jaehoon; Willis, Ian M.; Angeletti, Ruth Hogue; Hawke, David H.


    We have adapted the Ba2+ ion-catalyzed concurrent Michael addition reaction to solid-phase derivatization on ZipTipC18 pipette tips using 2-aminoethanethiol as a nucleophile. This approach provides several advantages over the classical in-solution-based techniques, including ease of operation, completeness of reaction, improved throughput, efficient use of dilute samples, and amenability to automation. Phosphoseryl and phosphothreonyl peptides, as well as phosphoserine peptides with adjoining...

  5. Two-phase flow meter for determining water and solids volumetric flow rate in vertical and inclined solids-in-water flows

    Muhamedsalih, Yousif


    Multiphase flow can be defined as the simultaneous flow of a stream of two or more phases. Solids-in-water flow is a multiphase flows where solids and liquid are both present. Due to the density differences of the two phases, the results for such flow is often to have non-uniform profiles of the local volume fraction and local axial velocity for both phases in the flow cross-section. These non-uniform profiles are clearly noticeable in solids-in-water stratified flow with moving bed for incli...

  6. A Solid Phase Synthesis of Chalcones by Claisen-Schmidt Condensations


    In order to accelerate the development of relatively inexpensive antimalarials that are effective against chloroquine-resistant strains of Plasmodium falclparum, a methodology for the solid phase synthesis of chalcone (l, 3-diphenyl-2-propen-l-one) analogues in reasonably high yields has been developed.

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

    Tolborg, Jakob Fjord; Jensen, Knud Jørgen


    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 be...

  8. Effects of Inoculum Size on Solid-Phase Fermentation of Fodder Beets for Fuel Ethanol Production

    Gibbons, William R.; Westby, Carl A.


    This fuel ethanol study examined the effects of Saccharomyces cerevisiae inoculum size on solid-phase fermentation of fodder beet pulp. A 5% inoculum (wt/wt) resulted in rapid yeast and ethanol (9.1% [vol/vol]) production. Higher inocula showed no advantages. Lower inocula resulted in lowered final yeast populations and increased fermentation times.

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

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


    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.

  10. Matrix solid-phase dispersion for the liquid chromatographic determination of phenolic acids in Melissa officinalis.

    Ziaková, Alica; Brandsteterová, Eva; Blahová, Eva


    Matrix solid-phase dispersion (MSPD) was used for sample preparation of plant material (Melissa officinalis, Lemon Balm) prior to liquid chromatography of rosmarinic, caffeic and protocatechuic acids, phenolic compounds present in this herb. Different MSPD sorbents and various elution agents were tested and the optimal extraction conditions determined with the aim to obtain extraction recoveries greater than 90% for all analytes. PMID:12568390

  11. An amine-derivatized, DOTA-loaded polymeric support for Fmoc Solid Phase Peptide Synthesis

    Yoo, Byunghee; Sheth, Vipul R.; Pagel, Mark D.


    An amine-derivatized DOTA has been used to modify the surface of a polymeric support for conventional Solid Phase Peptide Synthesis (SPPS) following standard Fmoc chemistry methods. This methodology was used to synthesize a peptide-DOTA conjugate that was demonstrated to be a PARACEST MRI contrast agent. Therefore, this synthesis methodology can facilitate Fmoc SPPS of molecular imaging contrast agents.

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

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


    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...

  13. Solid-phase microextraction of hydrocarbons from water in a centrifuge

    Ryabov, A. Yu.; Chuikin, A. V.; Velikov, A. A.


    The results of our study of solid-phase microextraction of substances using a centrifuge for determining the microquantities of hydrocarbon impurities in water are presented. The cartridge diameter, sorbent mass, and solvent volume were shown to affect the percent extraction of substances and the analytical signal intensity. The relationship between the cartridge geometry, the sorbent mass, and the solvent volume was considered.

  14. Kinetic study of solid phase crystallisation of expanding thermal plasma deposited a-Si:H

    Law, F.; Hoex, B.; Wang, J.; Luther, J.; Sharma, K.; Creatore, M.; M. C. M. van de Sanden,


    In-situ X-ray diffraction was used to study the dynamics of the solid phase crystallisation (SPC) of hydrogenated amorphous silicon (a-Si:H) films deposited by expanding thermal plasma technique. The Johnson-Mehl-Avrami-Kolmogorov model was used for the analysis of the dynamic data and the activatio

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

    Van Bramer, Scott; Goodrich, Katherine R.


    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,…

  16. Final Report for Nucleation and growth of semiconductor nanocrystals by solid-phase reaction

    P. D. Persans; T. M. Hayes


    This final report describes the technical output of a scientific program aimed at understanding the formation and structure of II-VI nanocrystals formed by solid phase precipitation within a glass environment. The principle probes were optical absorption spectroscopy to determine crystallite sizes, Raman scattering to determine composition, and x-ray absorption spectroscopy to study the evolution of local reactant environments.

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

    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)


    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.

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

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


    [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...


    Data is presented on the development of a new automated system combining solid phase extraction (SPE) with GC/MS spectrometry for the single-run analysis of water samples containing a broad range of organic compounds. The system uses commercially available automated in-line sampl...

  20. Technical note: New applications for on-line automated solid phase extraction

    MacFarlane, John D.


    This technical note explains the disadvantages of manual solid phase extraction (SPE) techniques and the benefits to be gained with automatic systems. The note reports on a number of general and highly specific applications using the Sample Preparation Unit OSP-2A.

  1. Automatic reactor for solid-phase synthesis of molecularly imprinted polymeric nanoparticles (MIP NPs) in water

    Poma, Alessandro; Guerreiro, Antonio; Caygill, Sarah; Moczko, Ewa; Piletsky, Sergey


    We report the development of an automated chemical reactor for solid-phase synthesis of MIP NPs in water. Operational parameters are under computer control, requiring minimal operator intervention. In this study, “ready for use” MIP NPs with sub-nanomolar affinity are prepared against pepsin A, trypsin and α-amylase in only 4 hours.

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

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

  3. 40 CFR 227.32 - Liquid, suspended particulate, and solid phases of a material.


    ... the case may be, may require that the separation of liquid, suspended particulate, and solid phases of the material be performed upon a mixture of the waste with ocean water rather than on the material... alkaline waste) based on guidance provided by EPA on particular cases, or in accordance with approved...

  4. Use of Solid Phase Extraction in the Biochemistry Laboratory to Separate Different Lipids

    Flurkey, William H.


    Solid-phase extraction (SPE) was used to demonstrate how various lipids and lipid classes could be separated in a biochemistry laboratory setting. Three different SPE methods were chosen on their ability to separate a lipid mixture, consisting of a combination of a either a fatty acid, a triacylglycerol, a mono- or diacylglycerol, phospholipid,…

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

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


    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

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

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


    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…

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

    Shelton, Anne Pernille Tofteng; Jensen, Knud Jørgen

    This chapter describes the basic protocols for solid-phase peptide synthesis using the Fmoc group as the N-alpha-protecting group (Fmoc-SPPS). The chapter introduces resins and their handling, choice of linkers, and the most common methods for peptide chain assembly. The proper choice of resins a...

  8. Solid-phase synthesis of polyfunctional polylysine dendrons using aldehyde linkers

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


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

  9. Microwave-assisted solid-phase Ugi four-component condensations

    Nielsen, John


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

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

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


    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. PMID:26454344

  11. Hydrodynamic and thermal fields analysis in gas-solid two-phase flow

    The present work aims to investigate numerically the flowfield and heat transfer process in gas-solid suspension in a vertical pneumatic conveying pipe. The Eulerian-Lagrangian model is used to simulate the flow of the two-phases. The gas phase is simulated based on Reynolds Average Navier-Stokes equations (RANS) with low Reynolds number k-ε model, while particle tracking procedure is used for the solid phase. An anisotropic model is used to calculate the Reynolds stresses and the turbulent Prandtl number is calculated as a function of the turbulent viscosity. The model takes into account the lift and drag forces and the effect of particle rotation as well as the particles dispersion by turbulence effect. The effects of inter-particles collisions and turbulence modulation by the solid particles, i.e. four-way coupling, are also included in the model. Comparisons between different models for turbulence modulation with experimental data are carried out to select the best model. The model is validated against published experimental data for velocities of the two phases, turbulence intensity, solids concentration, pressure drop, heat transfer rates and Nusselt number distribution. The comparisons indicate that the present model is able to predict the complex interaction between the two phases in non-isothermal gas-solid flow in the tested range. The results indicate that the particle-particle collision, turbulence dispersion and lift force play a key role in the concentration distribution. In addition, the heat transfer rate increases as the mass loading ratio increases and Nusselt number increases as the pipe diameter increases.

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

    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 125I-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. 125I-Labeled serum albumen, fibrinogen, and rat pulmonary basement membrane were also susceptible to hydrolysis by trypsin in the solid phase. When [14C]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

  13. Solid-state dual-frequency laser free from anti-phase noise

    El Amili, Abdelkrim; Loas, Goulc'Hen; De, Syamsundar; Schwartz, Sylvain; Feugnet, Gilles; Pocholle, Jean-Paul; Bretenaker, Fabien; Alouini, Mehdi


    Dual-frequency solid-state lasers are attractive for a large number of applications such as microwave photonics, spectroscopy, and metrology. As far as dual-frequency lasers are considered, the intensity noise spectrum of each eigenmode exhibits two peaks lying at the well-known in-phase and anti-phase eigen-frequencies of two coupled oscillators. The in-phase noise, which corresponds to the standard relaxation oscillations of the laser, can be reduced either electronically or optically using...

  14. Free energy model for solid high-pressure phases of carbon.

    Schöttler, Manuel; French, Martin; Cebulla, Daniel; Redmer, Ronald


    Analytic free energy models for three solid high-pressure phases--diamond, body centered cubic phase with eight atoms in the unit cell (BC8), and simple cubic (SC)--are developed using density functional theory. We explicitly include anharmonic effects by performing molecular dynamics simulations and investigate their density and temperature dependence in detail. Anharmonicity in the nuclear motion shifts the phase transitions significantly compared to the harmonic approximation. Furthermore, we apply a thermodynamically constrained correction that brings the equation of state in accordance with diamond anvil cell experiments. The performance of our thermodynamic functions is validated against Hugoniot experiments. PMID:26974530

  15. New methodological improvements in the Microtox® solid phase assay.

    Burga Pérez, Karen F; Charlatchka, Rayna; Sahli, Leila; Férard, Jean-François


    The classic Microtox® solid phase assay (MSPA) based on the inhibition of light production of the marine bacteria recently renamed Aliivibrio fischeri suffers from various bias and interferences, mainly due to physico-chemical characteristics of the tested solid phase. To precisely assess ecotoxicity of sediments, we have developed an alternative method, named Microtox® leachate phase assay (MLPA), in order to measure the action of dissolved pollutants in the aqueous phase. Two hypotheses were formulated to explain the observed difference between MSPA and MLPA results: a real ecotoxicity of the solid phase or the fixation of bacteria to fine particles and/or organic matter. To estimate the latter, flow cytometry analyses were performed with two fluorochromes (known for their ability to stain bacterial DNA), allowing correction of MSPA measurements and generation of new (corrected) IC50. Comparison of results of MLPA with the new IC50 MSPA allows differentiating real ecotoxic and fixation effect in classic MSPA especially for samples with high amount of fines and/or organic matter. PMID:21962521

  16. Optical manipulation of the Berry phase in a solid-state spin qubit

    Yale, Christopher G.; Heremans, F. Joseph; Zhou, Brian B.; Auer, Adrian; Burkard, Guido; Awschalom, David D.


    Phase relations between quantum states represent a resource for storing and processing quantum information. Although quantum phases are commonly controlled dynamically by tuning energetic interactions, the use of geometric phases that accumulate during cyclic evolution may offer superior robustness to noise. To date, demonstrations of geometric phase in solid-state systems employ microwave fields that have limited spatial resolution. Here, we demonstrate an all-optical method to accumulate a geometric phase, the Berry phase, in an individual nitrogen-vacancy centre in diamond. Using stimulated Raman adiabatic passage controlled by diffraction-limited laser light, we loop the nitrogen-vacancy centre's spin around the Bloch sphere to enclose an arbitrary Berry phase. We investigate the limits of this control due to the loss of adiabaticity and decoherence, as well as its robustness to noise introduced into the experimental control parameters. These techniques set the foundation for optical geometric manipulation in photonic networks of solid-state qubits linked and controlled by light.

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

    Shao, Sihong


    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.

  18. Transport mechanisms and wetting dynamics in molecularly thin films of long-chain alkanes at solid/vapour interface : relation to the solid-liquid phase transition

    Lazar, Paul


    Wetting and phase transitions play a very important role our daily life. Molecularly thin films of long-chain alkanes at solid/vapour interfaces (e.g. C30H62 on silicon wafers) are very good model systems for studying the relation between wetting behaviour and (bulk) phase transitions. Immediately above the bulk melting temperature the alkanes wet partially the surface (drops). In this temperature range the substrate surface is covered with a molecularly thin ordered, solid-like alkane film (...

  19. Temperature-composition-order parameter phase diagram for compositionally ordering solid solutions of lead scandium niobate - lead scandium tantalate

    It is established that the temperature of ferroelectric phase transition in crystals of lead scandium niobate - lead scandium tantalate ordering solid solutions both with low - and high order parameters has a linear dependence on the composition x. On the basis of the data obtained for the first time the phase diagram T-x-S is calculated for these solid solutions

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

    Qvortrup, Katrine; Nielsen, Thomas Eiland


    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-subs......-substituted NH-triazoles in high purity and yield....

  1. Development of solid-phase extraction and solid-phase microextraction methods for the determination of chlorophenols in cork macerate and wine samples.

    Insa, S; Salvadó, V; Anticó, E


    Tri-, tetra- and pentachlorophenol (TCP, TeCP and PCP) can be considered the precursors in the formation of corresponding chloroanisoles, known to be powerful odorants in corks and wine. Determining the presence of these chlorophenolic compounds in cork soaking solutions (ethanol/water mixtures, 12% (v/v) ethanol used for cork quality control testing), or in wine can be achieved by acetylation/gas chromatography electron-capture detection. In order to reach the required sensitivity, a previous preconcentration step is necessary. Solid-phase extraction (SPE) and headspace solid-phase microextraction (HS-SPME) have given good results for the preconcentration of TCP, TeCP and PCP in such matrices. The use of Oasis HLB cartridges gives acceptable recoveries for the three compounds when different volumes (50-250 mL) of cork macerate with concentrations ranging from 20 to 150 ng/L are processed. Preconcentration based on HS-SPME has also been optimised with a 100 microm polydimethylsiloxane fibre and in situ derivatization. The HS-SPME method allows chlorophenols in a cork soaking solution and in wine to be determined with a limit of detection of 1 ng/L for each compound (in cork macerate) and a repeatability of around 0.5%-5% (n=8) for a concentration level of 30 ng/L. PMID:15481456

  2. Ethanol/Water extraction combined with solid-phase extraction and solid-phase microextraction concentration for the determination of chlorophenols in cork stoppers.

    Insa, Sara; Besalú, Emili; Iglesias, Cristina; Salvadó, Victoria; Anticó, Enriqueta


    The appearance of 2,4,6-trichloroanisole (TCA) in cork stoppers is of great concern because it can cause off-flavors in bottled wine. To prevent this sensorial defect, there should not be any traces of 2,4,6-trichlorophenol (TCP), 2,3,4,6-tetrachlorophenol (TeCP), or pentachlorophenol (PCP) in the finished corks, because they are the direct precursors of TCA. In the course of this study two methodologies based upon an extraction with ethanol/water mixtures to determine the chlorophenolic content in cork matrices were developed. The cork extract is preconcentrated using both solid-phase extraction and solid-phase microextraction methodologies. The latter was optimized by applying a full two-level factorial design. Finally, spiked ground corks at nanogram per gram levels of each chlorophenol were analyzed under optimal conditions and by applying both procedures. The obtained results demonstrate that chlorophenols can be detected in corks contaminated at the nanogram per gram level and, thus, these approaches can be successfully applied as quality control measures in the cork industry. PMID:16448159

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

    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, kE, 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 kEEEE=1. The theory developed here can be tailored for diffusive phase transformations, formation of intergranular and interfacial phases, and surface-induced phase transformations

  4. Synthesis of silicon carbide nanowires by solid phase source chemical vapor deposition

    NI Jie; LI Zhengcao; ZHANG Zhengjun


    In this paper,we report a simple approach to synthesize silicon carbide(SiC)nanowires by solid phase source chemical vapor deposition(CVD) at relatively low temperatures.3C-SiC nanowires covered by an amorphous shell were obtained on a thin film which was first deposited on silicon substrates,and the nanowires are 20-80 am in diameter and several μm in length,with a growth direction of[200].The growth of the nanowires agrees well on vapor-liquid-solid (VLS)process and the film deposited on the substrates plays an important role in the formation of nanowires.

  5. Effects of potassium nitrate on the solid phase transitions of ammonium nitrate particles

    Wu, Hong Bo; Chan, Chak K.

    Ammonium nitrate (NH 4NO 3) is a common constituent of atmospheric particulate pollutants. It exists in five stable polymorphic forms, designated as phases V, IV, III, II and I, below its melting point of 170 °C. In atmospheric research, very little attention has been paid to the solid phase transitions of NH 4NO 3 because phase IV NH 4NO 3 particles are stable over a wide range of tropospheric temperatures. Potassium nitrate (KNO 3) is often found to co-exist with NH 4NO 3 in atmospheric aerosols, and it can change the phase transition behaviors of solid NH 4NO 3 particles. In this study, we investigated the effects of KNO 3 on the solid phase transitions of NH 4NO 3 particles using in situ microscopic Raman spectroscopy. Both the transition path and transition temperature of NH 4NO 3 single particles (40-700 μm) depend on the KNO 3 mass percentage and the particle size. With the addition of KNO 3, the IV→II transition, which appears at 52 °C for pure NH 4NO 3 particles, is replaced by the IV→III transition. The KNO 3 mass percentage required for this change in transition path increases with decreasing particle size and the transition temperature decreases with increasing KNO 3 mass percentage. At a relatively high mass percentage of KNO 3 (⩾7.4 wt%), the KNO 3/NH 4NO 3 mixed particles undergo the IV→III transition under ambient temperatures, or even crystallize directly in phase III from droplets with a further increase in the mass percentage of KNO 3. Submicron KNO 3/NH 4NO 3 particles crystallize to phase IV at low KNO 3 mass percentages (⩽5.7 wt%) but to phase III at higher KNO 3 mass percentages (⩾7.4 wt%). These results suggest that atmospheric solid NH 4NO 3 particles may exist in phase III and the phase transitions should not be ignored in atmospheric chemical models.

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

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


    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)

  7. Electron Shuttling Capacity of Solid-Phase Organic Matter in Forest Soils

    Patel, A.; Zhao, Q.; Yang, Y.


    Soil organic matter, as an electron shuttle, plays an important role in regulating the biogeochemical cycles of metals, especially the redox reactions for iron. Microorganisms can reduce soil organic matter under anaerobic conditions, and biotically-reduced soil organic matter can abiotically donate electrons to ferric oxides. Such soil organic matter-mediated electron transport can facilitate the interactions between microorganisms and insoluble terminal electron acceptors, i.e. iron minerals. Most previous studies have been focused on the electron shuttling processes through dissolved soil organic matter, and scant information is available for solid-phase soil organic matter. In this study, we aim to quantify the electron accepting capacity for solid-phase organic matter in soils collected from four different forests in the United States, including Truckee (CA), Little Valley (NV), Howland (ME) and Hart (MI). We used Shewanella oneidensisMR-1 to biotically reduce soil slurries, and then quantified the electrons transferred to solid-phase and solution-phase organic matter by reacting them with Fe(III)-nitrilotriacetic acid (Fe(III)-NTA). The generation of Fe(II) was measured by a ferrozine assay to calculate the electron accepting capacity of soil organic matter. Our preliminary results showed that the Truckee soil organic matter can accept 0.51±0.07 mM e-/mol carbon. We will measure the electron accepting capacity for four different soils and correlate them to the physicochemical properties of soils. Potential results will provide information about the electron accepting capacity of solid-phase soil organic matter and its governing factors, with broad implication on the coupled biogeochemical cycles of carbon and iron.

  8. Mesomorphism in columnar phases studied by solid-state nuclear magnetic resonance.

    Dvinskikh, Sergey V; Thaning, Johan; Stevensson, Baltzar; Jansson, Kjell; Kumar, Sandeep; Zimmermann, Herbert; Maliniak, Arnold


    In this paper, we present 13C and 1H NMR investigations of 2, 3, 6, 7, 10, 11-hexahexyl-thiotriphenylene (HHTT). The measurements were carried out under both static and magic-angle spinning conditions. The phase diagram of HHTT is KHD(hd)I , where H is a helical phase and D(hd) is a columnar liquid crystal. The motivation was to characterize the molecular order and dynamics and to investigate differences at the molecular level between the two mesophases: H and D(hd). It is shown that D(hd) is a conventional columnar liquid crystal, where the molecular core undergoes fast rotation about the symmetry axis. The orientational order in this mesophase is lower and the temperature dependence of the order parameter is steeper than in other triphenylene-based compounds. On the other hand, in the helical phase the core, similarly to the solid phase, is essentially rigid. The difference between the solid and helical phases is mainly manifested in an increased mobility of the aliphatic chains observed in the latter phase. In addition, the sample exhibits thermal history effects, which are observed in the different behavior upon cooling and heating. PMID:17025448

  9. Solid Phase Characterization Of Heel Samples From Tank 241-C-110

    During sluicing operations of tank 241-C-110, a significant amount of solids were unable to be retrieved. These solids (often referred to as the tank 'heel') were sampled in 2010 and chemically and mineralogically analyzed in the 222-S Laboratory. Additionally, dissolution tests were performed to identify the amount of undissolvable material after using multiple water contacts. This report covers the solid phase characterization of six samples from these tests using scanning electron microscopy, polarized light microscopy, and X-ray diffraction. The chemical analyses, particle size distribution analysis, and dissolution test results are reported separately. Two of the samples were from composites created from as-received material - Composite A and Composite B. The main phase in these samples was sodium-fluoride-phosphate hydrate (natrophosphate) - in the X-ray diffraction spectra, this phase was the only phase identifiable. Polarized light microscopy showed the presence of minor amounts of gibbsite and other phases. These phases were identified by scanning electron microscopy - energy dispersive X-ray spectroscopy as sodium aluminosilicates, sodium diuranate, and sodium strontium phosphate hydrate (nastrophite) crystals. The natrophosphate crystals in the scanning electron microscopy analysis showed a variety of erosive and dissolution features from perfectly shaped octahedral to well-rounded appearance. Two samples were from water-washed Composites A and B, with no change in mineralogy compared to the as-received samples. This is not surprising, since the water wash had only a short period of water contact with the material as opposed to the water dissolution tests. The last two samples were residual solids from the water dissolution tests. These tests included multiple additions of water at 15 C and 45 C. The samples were sieved to separate a coarser fraction of > 710 μm and a finer fraction of < 710 μm. These two fractions were analyzed separately. The coarser




    During sluicing operations of tank 241-C-110, a significant amount of solids were unable to be retrieved. These solids (often referred to as the tank 'heel') were sampled in 2010 and chemically and mineralogically analyzed in the 222-S Laboratory. Additionally, dissolution tests were performed to identify the amount of undissolvable material after using multiple water contacts. This report covers the solid phase characterization of six samples from these tests using scanning electron microscopy, polarized light microscopy, and X-ray diffraction. The chemical analyses, particle size distribution analysis, and dissolution test results are reported separately. Two of the samples were from composites created from as-received material - Composite A and Composite B. The main phase in these samples was sodium-fluoride-phosphate hydrate (natrophosphate) - in the X-ray diffraction spectra, this phase was the only phase identifiable. Polarized light microscopy showed the presence of minor amounts of gibbsite and other phases. These phases were identified by scanning electron microscopy - energy dispersive X-ray spectroscopy as sodium aluminosilicates, sodium diuranate, and sodium strontium phosphate hydrate (nastrophite) crystals. The natrophosphate crystals in the scanning electron microscopy analysis showed a variety of erosive and dissolution features from perfectly shaped octahedral to well-rounded appearance. Two samples were from water-washed Composites A and B, with no change in mineralogy compared to the as-received samples. This is not surprising, since the water wash had only a short period of water contact with the material as opposed to the water dissolution tests. The last two samples were residual solids from the water dissolution tests. These tests included multiple additions of water at 15 C and 45 C. The samples were sieved to separate a coarser fraction of > 710 {mu}m and a finer fraction of < 710 {mu}m. These two fractions were analyzed