Wax Precipitation Modeled with Many Mixed Solid Phases

DEFF Research Database (Denmark)

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

2005-01-01

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

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

Science.gov (United States)

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

2017-12-01

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

Multiple solid-phase microextraction

NARCIS (Netherlands)

Koster, EHM; de Jong, GJ

2000-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

1990-03-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2002-07-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

1997-06-24

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

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

NARCIS (Netherlands)

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

1979-01-01

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

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

Science.gov (United States)

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

2007-11-15

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

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

Directory of Open Access Journals (Sweden)

Xiaoyan Lu

2016-10-01

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

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

Science.gov (United States)

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

2018-04-01

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

Heterogeneous Ferroelectric Solid Solutions Phases and Domain States

CERN Document Server

Topolov, Vitaly

2012-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2017-09-10

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

Comparative solution and solid-phase glycosylations toward a disaccharide library

DEFF Research Database (Denmark)

Agoston, K.; Kröger, Lars; Agoston, Agnes

2009-01-01

A comparative study on solution-phase and solid-phase oligosaccharide synthesis was performed. A 16-member library containing all regioisomers of Glc-Glc, Glc-Gal, Gal-Glc, and Gal-Gal disaccharides was synthesized both in solution and on solid phase. The various reaction conditions for different...

Role of nanoparticles in analytical solid phase microextraction (SPME)

NARCIS (Netherlands)

Zielinska, K.; Leeuwen, van H.P.

2013-01-01

Solid phase microextraction (SPME) is commonly used to measure the free concentration of fairly hydrophobic substances in aqueous media on the basis of their partitioning between sample solution and a solid phase. Here we study the role of nanoparticles that may sorb the analyte in the sample

Analytical study of solids-gas two phase flow

International Nuclear Information System (INIS)

Hosaka, Minoru

1977-01-01

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

Materials research for passive solar systems: Solid-state phase-change materials

Science.gov (United States)

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

1985-03-01

A set of solid-state phase-change materials is being evaluated for possible use in passive solar thermal energy storage systems. The most promising materials are organic solid solutions of pentaerythritol (C5H12O4), pentaglycerinve (C5H12O3), and neopentyl glycol (C5H12O2). Solid solution mixtures of these compounds can be tailored so that they exhibit solid-to-solid phase transformations at any desired temperature between 25 C and 188 C, and have latent heats of transformation etween 20 and 70 cal/g. Transformation temperatures, specific heats, and latent heats of transformation have been measured for a number of these materials. Limited cyclic experiments suggest that the solid solutions are stable. These phase-change materials exhibit large amounts of undercooling; however, the addition of certain nucleating agents as particulate dispersions in the solid phase-change material greatly reduces this effect. Computer simulations suggest that the use of an optimized solid-state phase-change material in a Trombe wall could provide better performance than a concrete Trombe wall four times thicker and nine times heavier.

Solid-phase reductive amination for glycomic analysis.

Science.gov (United States)

Jiang, Kuan; Zhu, He; Xiao, Cong; Liu, Ding; Edmunds, Garrett; Wen, Liuqing; Ma, Cheng; Li, Jing; Wang, Peng George

2017-04-15

Reductive amination is an indispensable method for glycomic analysis, as it tremendously facilitates glycan characterization and quantification by coupling functional tags at the reducing ends of glycans. However, traditional in-solution derivatization based approach for the preparation of reductively aminated glycans is quite tedious and time-consuming. Here, a simpler and more efficient strategy termed solid-phase reductive amination was investigated. The general concept underlying this new approach is to streamline glycan extraction, derivatization, and purification on non-porous graphitized carbon sorbents. Neutral and sialylated standard glycans were utilized to test the feasibility of the solid-phase method. As results, almost complete labeling of those glycans with four common labels of aniline, 2-aminobenzamide (2-AB), 2-aminobenzoic acid (2-AA) and 2-amino-N-(2-aminoethyl)-benzamide (AEAB) was obtained, and negligible desialylation occurred during sample preparation. The labeled glycans derived from glycoproteins showed excellent reproducibility in high performance liquid chromatography (HPLC) and matrix assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) analysis. Direct comparisons based on fluorescent absorbance and relative quantification using isotopic labeling demonstrated that the solid-phase strategy enabled 20-30% increase in sample recovery. In short, the solid-phase strategy is simple, reproducible, efficient, and sensitive for glycan analysis. This method was also successfully applied for N-glycan profiling of HEK 293 cells with MALDI-TOF MS, showing its attractive application in the high-throughput analysis of mammalian glycome. Published by Elsevier B.V.

Study on confirmation of Solid-Meal Lag Phase of Gastric Emptying

International Nuclear Information System (INIS)

Lee, Ji Young; Lee, Kyoung Soo; Kim, Chang Guhn; Juhng, Seon Kwan; Won, Jong Jin; Nah, Yong Ho

1991-01-01

The purpose of this study was to examine the existence of a lag phase of gastric emptying of solid meals. We studied solid phase gastric emptying in 26 normal subject using continuous data acquisition for 30 minutes. Each ingested a 300 g meal containing 99m Tc-labeled scrambled egg (solid 150 g, milk 150 ml). Lag phase was determined by 1) inspection of the gastric emptying curve 2) time to a 2% decrease in stomach activity 3) the time of visual appearance of duodenal activity on computer image. We concluded that solid meal lag phase exist.

Study on confirmation of Solid-Meal Lag Phase of Gastric Emptying

Energy Technology Data Exchange (ETDEWEB)

Lee, Ji Young; Lee, Kyoung Soo; Kim, Chang Guhn; Juhng, Seon Kwan; Won, Jong Jin; Nah, Yong Ho [Wonkwang University School of Medicine, Iksan (Korea, Republic of)

1991-07-15

The purpose of this study was to examine the existence of a lag phase of gastric emptying of solid meals. We studied solid phase gastric emptying in 26 normal subject using continuous data acquisition for 30 minutes. Each ingested a 300 g meal containing {sup 99m}Tc-labeled scrambled egg (solid 150 g, milk 150 ml). Lag phase was determined by 1) inspection of the gastric emptying curve 2) time to a 2% decrease in stomach activity 3) the time of visual appearance of duodenal activity on computer image. We concluded that solid meal lag phase exist.

Novel solid – solid phase change material based on polyethylene glycol and cellulose used for temperature stabilisation

Directory of Open Access Journals (Sweden)

Wojda Marta

2014-01-01

Full Text Available Thermal management is one of crucial issues in the development of modern electronic devices. In the recent years interest in phase change materials (PCMs as alternative cooling possibility has increased significantly. Preliminary results concerning the research into possibility of the use of solid-solid phase change materials (S-S PCMs for stabilisation temperature of electronic devices has been presented in the paper. Novel solid-solid phase change material based on polyethylene glycol and cellulose has been synthesized. Attempt to improve its thermal conductivity has been taken. Material has been synthesized for the purpose of stabilisation of temperature of electronic devices.

Amino-modified diamond as a durable stationary phase for solid-phase extraction.

Science.gov (United States)

Saini, Gaurav; Yang, Li; Lee, Milton L; Dadson, Andrew; Vail, Michael A; Linford, Matthew R

2008-08-15

We report the formation of a highly stable amino stationary phase on diamond and demonstrate its use in solid-phase extraction (SPE). This process consists of spontaneous and self-limiting adsorption of polyallylamine (PAAm) from aqueous solution onto oxidized diamond. Thermal curing under reduced pressure or chemical cross-linking with a diepoxide was shown to fix the polymer to the particles. The resulting adsorbents are stable under even extreme pH conditions (from at least pH 0-14) and significantly more stable than a commercially available amino SPE adsorbent. Coated diamond particles were characterized by X-ray photoelectron spectroscopy (XPS) and diffuse reflectance Fourier transform-infrared spectroscopy (DRIFT). Model silicon surfaces were characterized by spectroscopic ellipsometry and wetting. Solid-phase extraction was demonstrated using cholesterol, hexadecanedioic acid, and palmitoyloleoylphosphatidylcholine as analytes, and these results were compared to those obtained with commercially available materials. Breakthrough curves indicate that, as expected, porous diamond particles have higher analyte capacity than nonporous solid particles.

N-Acyliminium Intermediates in Solid-Phase Synthesis

DEFF Research Database (Denmark)

Quement, Sebastian Thordal le; Petersen, Rico; Meldal, M.

2010-01-01

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

Solid-phase synthesis of molecularly imprinted nanoparticles.

Science.gov (United States)

Canfarotta, Francesco; Poma, Alessandro; Guerreiro, Antonio; Piletsky, Sergey

2016-03-01

Molecularly imprinted polymers (MIPs) are synthetic materials, generally based on acrylic or methacrylic monomers, that are polymerized in the presence of a specific target molecule called the 'template' and capable of rebinding selectively to this target molecule. They have the potential to be low-cost and robust alternatives to biomolecules such as antibodies and receptors. When prepared by traditional synthetic methods (i.e., with free template in solution), their usefulness has been limited by high binding site heterogeneity, the presence of residual template and the fact that the production methods are complex and difficult to standardize. To overcome some of these limitations, we developed a method for the synthesis of MIP nanoparticles (nanoMIPs) using an innovative solid-phase approach, which relies on the covalent immobilization of the template molecules onto the surface of a solid support (glass beads). The obtained nanoMIPs are virtually free of template and demonstrate high affinity for the target molecule (e.g., melamine and trypsin in our published work). Because of an affinity separation step performed on the solid phase after polymerization, poor binders and unproductive polymer are removed, so the final product has more uniform binding characteristics. The overall protocol, starting from the immobilization of the template onto the solid phase and including the purification and characterization of the nanoparticles, takes up to 1 week.

Solid phase extraction membrane

Science.gov (United States)

Carlson, Kurt C [Nashville, TN; Langer, Roger L [Hudson, WI

2002-11-05

A wet-laid, porous solid phase extraction sheet material that contains both active particles and binder and that possesses excellent wet strength is described. The binder is present in a relatively small amount while the particles are present in a relatively large amount. The sheet material is sufficiently strong and flexible so as to be pleatable so that, for example, it can be used in a cartridge device.

Solid phase syntheses of oligoureas

Energy Technology Data Exchange (ETDEWEB)

Burgess, K.; Linthicum, D.S.; Russell, D.H.; Shin, H.; Shitangkoon, A.; Totani, R.; Zhang, A.J.; Ibarzo, J. [Texas A& M Univ., College Station, TX (United States)

1997-02-19

Isocyanates 7 were formed from monoprotected diamines 3 or 6, which in turn can be easily prepared from commercially available N-BOC- or N-FMOC-protected amino acid derivatives. Isocyanates 7, formed in situ, could be coupled directly to a solid support functionalized with amine groups or to amino acids anchored on resins using CH{sub 2}Cl{sub 2} as solvent and an 11 h coupling time at 25 {degree}C. Such couplings afforded peptidomimetics with an N-phthaloyl group at the N-terminus. The optimal conditions identified for removal of the N-phthaloyl group were to use 60% hydrazine in DMF for 1-3 h. Several sequences of amino acids coupled to ureas (`peptidic ureas`) and of sequential urea units (`oligoureas`) were prepared via solid phase syntheses and isolated by HPLC. Partition coefficients were measured for two of these peptidomimetics, and their water solubilities were found to be similar to the corresponding peptides. A small library of 160 analogues of the YGGFL-amide sequence was prepared via Houghten`s tea bag methodology. This library was tested for binding to the anti-{beta}-endorphin monoclonal antibody. Overall, this paper describes methodology for solid phase syntheses of oligourea derivatives with side chains corresponding to some of the protein amino acids. The chemistry involved is ideal for high-throughput syntheses and screening operations. 51 refs., 3 figs., 2 tabs.

All solid-state SBS phase conjugate mirror

Science.gov (United States)

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

1999-03-09

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

Synthesis of beta alumina from aluminum hydroxide and oxyhydroxide precursors

CSIR Research Space (South Africa)

Van Zyl, A

1993-02-01

Full Text Available Two aluminium oxyhydroxides, boehmite and pseudoboehmite, and two aluminium hydroxides, bayerite and gibbsite, have been investigated as precursors for the synthesis of the solid electrolyte, beta alumina. Reaction pathways and products have been...

Solid-Phase S-Alkylation Promoted by Molecular Sieves.

Science.gov (United States)

Calce, Enrica; Leone, Marilisa; Mercurio, Flavia Anna; Monfregola, Luca; De Luca, Stefania

2015-11-20

A solid-phase S-alkylation procedure to introduce chemical modification on the cysteine sulfhydryl group of a peptidyl resin is reported. The reaction is promoted by activated molecular sieves and consists of a solid-solid process, since both the catalyst and the substrate are in a solid state. The procedure was revealed to be efficient and versatile, particularly when used in combination with the solution S-alkylation approach, allowing for the introduction of different molecular diversities on the same peptide molecule.

Linkage of biomolecules to solid phases for immunoassay

International Nuclear Information System (INIS)

Chapman, R.S.

1998-01-01

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

Phase diagram of a Lennard-Jones solid

International Nuclear Information System (INIS)

Choi, Y.; Ree, T.; Ree, F.H.

1993-01-01

A phase diagram of a Lennard-Jones solid at kT/ε≥0.8 is constructed by our recent perturbation theory. It shows the stability of the face-centered-cubic phase except within a small pressure and temperature domain, where the hexagonal-close packed phase may occur. The theory predicts anharmonic contributions to the Helmholtz free energy (important to the crystal stability) in good agreement with Monte Carlo data

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

International Nuclear Information System (INIS)

Cassidy, D.P.; Irvine, R.L.

1995-01-01

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

MOLECULARLY IMPRINTED SOLID PHASE EXTRACTION FOR TRACE ANALYSIS OF DIAZINON IN DRINKING WATER

Directory of Open Access Journals (Sweden)

M. Rahiminejad ، S. J. Shahtaheri ، M. R. Ganjali ، A. Rahimi Forushani ، F. Golbabaei

2009-04-01

Full Text Available Amongst organophosphate pesticides, the one most widely used and common environmental contaminant is diazinon; thus methods for its trace analysis in environmental samples must be developed. Use of diazinon imprinted polymers such as sorbents in solid phase extraction, is a prominent and novel application area of molecular imprinted polymers. For diazinon extraction, high performance liquid chromatography analysis was demonstrated in this study. During optimization of the molecular imprinted solid phase extraction procedure for efficient solid phase extraction of diazinon, Plackett-Burman design was conducted. Eight experimental factors with critical influence on molecular imprinted solid phase extraction performance were selected, and 12 different experimental runs based on Plackett-Burman design were carried out. The applicability of diazinon imprinted polymers as the sorbent in solid phase extraction, presented obtained good recoveries of diazinon from LC-grade water. An increase in pH caused an increase in the recovery on molecular imprinted solid phase extraction. From these results, the optimal molecular imprinted solid phase extraction procedure was as follows: solid phase extraction packing with 100 mg diazinon imprinted polymers; conditioning with 5 mL of methanol and 6 mL of LC-grade water; sample loading containing diazinon (pH=10; washing with 1 mL of LC-grade water, 1 mL LC- grade water containing 30% acetonitrile and 0.5 mL of acetonitrile, respectively; eluting with 1 mL of methanol containing 2% acetic acid. The percentage recoveries obtained by the optimized molecular imprinted solid phase extraction were more than 90% with drinking water spiked at different trace levels of diazinon. Generally speaking, the molecular imprinted solid phase extraction procedure and subsequent high performance liquid chromatography analysis can be a relatively fast and proper approach for qualitative and quantitative analysis of diazinon in

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

Science.gov (United States)

Wang, Nan; Upmanyu, Moneesh; Karma, Alain

2018-03-01

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

Solid phase microextraction.

Science.gov (United States)

Pawliszyn, J

2001-01-01

Solid Phase Microextraction (SPME) uses a small volume of sorbent dispersed typically on the surface of small fibres, to isolate and concentrate analytes from sample matrix. After contact with sample, analytes are absorbed or adsorbed by the fibre phase (depending on the nature of the coating) until an equilibrium is reached in the system. The amount of an analyte extracted by the coating at equilibrium is determined by the magnitude of the partition coefficient of the analyte between the sample matrix and the coating material. After the extraction step, the fibres are transferred, with the help of a syringe-like handling device, to analytical instrument, for separation and quantitation of target analytes. This technique integrates sampling, extraction and sample introduction and is a simple way of facilitating on-site monitoring. Applications of this technique include environmental monitoring, industrial hygiene, process monitoring, clinical, forensic, food, flavour, fragrance and drug analyses, in laboratory and on-site analysis.

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

Science.gov (United States)

Benson, D. K.; Christensen, C.

1983-11-01

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

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

Science.gov (United States)

Svendsen, Bob; Shanthraj, Pratheek; Raabe, Dierk

2018-03-01

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

Biogasification of solid wastes by two-phase anaerobic fermentation

International Nuclear Information System (INIS)

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

1997-01-01

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

solid phase extraction method for selective determination

African Journals Online (AJOL)

FATOKI

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

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

International Nuclear Information System (INIS)

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

1985-01-01

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

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

Science.gov (United States)

Cassidy, Daniel H.; Irvine, Robert L.

1995-10-01

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

The Pictet-Spengler reaction in solid-phase combinatorial chemistry

DEFF Research Database (Denmark)

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

2003-01-01

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

Phase 2, Solid waste retrieval strategy

International Nuclear Information System (INIS)

Johnson, D.M.

1994-01-01

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

Phase 2, Solid waste retrieval strategy

Energy Technology Data Exchange (ETDEWEB)

Johnson, D.M.

1994-09-29

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

The role of solid-solid phase transitions in mantle convection

Science.gov (United States)

Faccenda, Manuele; Dal Zilio, Luca

2017-01-01

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

Phase transitions in solids under high pressure

CERN Document Server

Blank, Vladimir Davydovich

2013-01-01

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

Solid Phase Extraction and Spectrophotometric Determination of ...

African Journals Online (AJOL)

NJD

2005-04-15

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

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

International Nuclear Information System (INIS)

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

2009-01-01

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

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

African Journals Online (AJOL)

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

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

International Nuclear Information System (INIS)

Robinson, C.M.

2004-01-01

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

Solid-phase equilibria on Pluto's surface

Science.gov (United States)

Tan, Sugata P.; Kargel, Jeffrey S.

2018-03-01

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

Mechanism and microstructures in Ga2O3 pseudomartensitic solid phase transition.

Science.gov (United States)

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

2016-07-21

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

Solid-phase synthesis of complex and pharmacologically interesting heterocycles

DEFF Research Database (Denmark)

Nielsen, Thomas Eiland

2009-01-01

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

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

Science.gov (United States)

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

2017-06-01

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

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

International Nuclear Information System (INIS)

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

2003-01-01

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

Solid phase radioimmunoassays for human C-reactive protein

International Nuclear Information System (INIS)

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

1981-01-01

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

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

African Journals Online (AJOL)

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

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

Science.gov (United States)

Lubach, Joseph W; Hau, Jonathan

2018-02-20

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

Bioinspired magnetite synthesis via solid precursor phases

NARCIS (Netherlands)

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

2016-01-01

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

Investigation of binary solid phases by calorimetry and kinetic modelling

OpenAIRE

Matovic, M.

2007-01-01

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

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

DEFF Research Database (Denmark)

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

2012-01-01

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

Unitized solid phase immunoassay kit and method

International Nuclear Information System (INIS)

1975-01-01

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

Solid-phase microextraction

DEFF Research Database (Denmark)

Nilsson, Torben

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

Phase segregation in cerium-lanthanum solid solutions

NARCIS (Netherlands)

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

2006-01-01

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

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

DEFF Research Database (Denmark)

Baatrup, G; Jonsson, H; Sjöholm, A

1988-01-01

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

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

Science.gov (United States)

Wang, Jianlong; Chu, Libing

2016-11-01

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

Solid-solid synthesis and structural phase transition process of SmF3

Science.gov (United States)

Yan, Qi-Cao; Guo, Xing-Min

2018-04-01

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

Thermodynamic phase behavior of API/polymer solid dispersions.

Science.gov (United States)

Prudic, Anke; Ji, Yuanhui; Sadowski, Gabriele

2014-07-07

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2012-12-15

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

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

International Nuclear Information System (INIS)

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

2008-01-01

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

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

Science.gov (United States)

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

2017-03-01

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

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

International Nuclear Information System (INIS)

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

1978-01-01

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

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

Science.gov (United States)

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

2009-04-17

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

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

International Nuclear Information System (INIS)

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

2007-01-01

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

Solid phase tube radioimmunoassay for digoxin detection

International Nuclear Information System (INIS)

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

1975-01-01

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

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

International Nuclear Information System (INIS)

Domanska, Urszula; Marciniak, Malgorzata

2007-01-01

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

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

Science.gov (United States)

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

2016-04-01

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

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

KAUST Repository

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

2016-01-01

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

Elementary excitations and phase transformations in solids

International Nuclear Information System (INIS)

Cowley, R.A.

1985-01-01

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

Semi-automated microwave assisted solid-phase peptide synthesis

DEFF Research Database (Denmark)

Pedersen, Søren Ljungberg

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

Investigation of solid-phase hydrogenation of amino acids and peptides

International Nuclear Information System (INIS)

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

1990-01-01

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

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

NARCIS (Netherlands)

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

1989-01-01

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

The growth and tensile deformation behavior of the silver solid solution phase with zinc

International Nuclear Information System (INIS)

Wu, Jiaqi; Lee, Chin C.

2016-01-01

The growth of homogeneous silver solid solution phase with zinc are conducted at two different compositions. X-ray diffraction (XRD) and Scanning electron microscope/Energy dispersive X-ray spectroscopy (SEM/EDX) are carried out for phase identification and chemical composition verification. The mechanical properties of silver solid solution phase with zinc are evaluated by tensile test. The engineering and true stress vs. strain curves are presented and analyzed, with those of pure silver in comparison. According to the experimental results, silver solid solution phase with zinc at both compositions show tempered yield strength, high tensile strength and large uniform strain compared to those of pure silver. Fractography further confirmed the superior ductility of silver solid solution phase with zinc at both compositions. Our preliminary but encouraging results may pave the way for the silver based alloys to be applied in industries such as electronic packaging and structure engineering.

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

Energy Technology Data Exchange (ETDEWEB)

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

2008-03-15

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

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

Science.gov (United States)

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

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

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

International Nuclear Information System (INIS)

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

1979-01-01

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

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

International Nuclear Information System (INIS)

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

1982-01-01

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

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

International Nuclear Information System (INIS)

Kuchta, B.; Etters, R.D.

1992-01-01

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

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

Science.gov (United States)

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

2017-09-01

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

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

Science.gov (United States)

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

2014-11-26

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

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

NARCIS (Netherlands)

de Jong, GJ; Koster, EHM

2000-01-01

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

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

African Journals Online (AJOL)

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

Solid phase separation technique for use in radioimmunoassays

International Nuclear Information System (INIS)

Tu, J.I.

1979-01-01

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

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

International Nuclear Information System (INIS)

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

2005-01-01

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

Studies in Solid Phase Peptide Synthesis: A Personal Perspective

Energy Technology Data Exchange (ETDEWEB)

Mitchell, A R

2007-06-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-02-07

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

Investigation of binary solid phases by calorimetry and kinetic modelling

NARCIS (Netherlands)

Matovic, M.

2007-01-01

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

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

African Journals Online (AJOL)

NICO

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

Ion-selective solid-phase electrode sensitive to ammonium ions

International Nuclear Information System (INIS)

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

1983-01-01

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

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

Science.gov (United States)

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

2014-10-01

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

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

DEFF Research Database (Denmark)

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

2004-01-01

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

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

International Nuclear Information System (INIS)

Na Liu; Yanfei Wang; Chuhua He

2016-01-01

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

Zirconium determination in rocks by solid-phase spectrophotometry

International Nuclear Information System (INIS)

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

1990-01-01

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

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

International Nuclear Information System (INIS)

El-Bayoumy, A.S.A.

2012-01-01

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

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

Science.gov (United States)

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

2018-01-01

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

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

International Nuclear Information System (INIS)

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

2011-01-01

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

The Effects of Solid Phase Additives on Sintering Properties of Alumina Bioceramic

Institute of Scientific and Technical Information of China (English)

WANG Xin-yu; LI Shi-pu; HE Jian-hua; JIANG Xin; LI Jian-hua

2003-01-01

In order to reduce the sintering temperature and improve the preparing conditions of alumina bioceramics,the Mg-Zr-Y composite solid phase additives were added into high purity Al2O3 micro-powder by chemical coprecipitation method.The powder was shaped under 200MPa cold isostatic pressure,and then the biscuits were sintered at 1600℃ under normal pressure.The sintered alumina materials were tested and the sintering mechanism was discussed.The results show that physical properties of the material were improved comparatively.The Mg-Zr-Y composite solid additives could promote the sintering of alumina bioceramics and the mechanism is solid phase sintering.

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

International Nuclear Information System (INIS)

Ren Jing; Gu Zhengfei; Cheng Gang; Zhou Huaiying

2005-01-01

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

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

International Nuclear Information System (INIS)

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

1985-01-01

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

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

DEFF Research Database (Denmark)

Nielsen, John

1998-01-01

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

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

African Journals Online (AJOL)

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

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

Science.gov (United States)

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

2018-01-01

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

Microwave-assisted solid-phase Ugi four-component condensations

DEFF Research Database (Denmark)

Nielsen, John

1999-01-01

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

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

International Nuclear Information System (INIS)

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

1980-01-01

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

Investigation into process of solid-phase synthesis of calcium vanadates

International Nuclear Information System (INIS)

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

1983-01-01

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

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

International Nuclear Information System (INIS)

Putnis, Andrew; Putnis, Christine V.

2007-01-01

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

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

Directory of Open Access Journals (Sweden)

Yoshinobu Fukumori

2013-07-01

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

Solid phase radioimmunoassay for HBe Ag and anti-HBe

Energy Technology Data Exchange (ETDEWEB)

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

1978-04-01

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

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

International Nuclear Information System (INIS)

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

2015-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2012-02-05

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

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

Science.gov (United States)

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

2006-05-25

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

Solid-phase oligosaccharide and glycopeptide synthesis using glycosynthases

DEFF Research Database (Denmark)

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

2002-01-01

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

Solid-Phase Synthesis of Smac Peptidomimetics Incorporating Triazoloprolines and Biarylalanines

DEFF Research Database (Denmark)

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

2011-01-01

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

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

NARCIS (Netherlands)

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

2001-01-01

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

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

KAUST Repository

Shao, Sihong

2012-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2008-08-15

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

New Solid Phases for Estimation of Hormones by Radioimmunoassay Technique

International Nuclear Information System (INIS)

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

2013-01-01

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

A solid-phase-radioimmunoassay for total serum thyroxine

International Nuclear Information System (INIS)

Moedder, G.; Sokolowski, G.

1978-01-01

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

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

Science.gov (United States)

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

2016-11-01

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

Determination of organophosphorus pesticides using molecularly imprinted polymer solid phase extraction

International Nuclear Information System (INIS)

Mohd Marsin Sanagi; Syairah Salleh; Wan Aini Wan Ibrahim

2011-01-01

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

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

Science.gov (United States)

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

2012-07-01

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

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

Science.gov (United States)

Mashile, Geaneth Pertunia; Nomngongo, Philiswa N

2017-03-04

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

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

NARCIS (Netherlands)

Zielinska, K.

2014-01-01

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

Solid-phase microextraction for the analysis of biological samples

NARCIS (Netherlands)

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

2000-01-01

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

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

Directory of Open Access Journals (Sweden)

Ireneusz Sowa

2018-03-01

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

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

Science.gov (United States)

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

2010-05-15

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

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

African Journals Online (AJOL)

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

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

Science.gov (United States)

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

2013-12-31

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

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

Science.gov (United States)

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

2017-12-01

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

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

International Nuclear Information System (INIS)

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

1980-01-01

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

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

African Journals Online (AJOL)

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

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

Energy Technology Data Exchange (ETDEWEB)

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

1998-12-31

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

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

International Nuclear Information System (INIS)

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

1983-01-01

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

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

International Nuclear Information System (INIS)

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

2009-01-01

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

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

DEFF Research Database (Denmark)

Hansen, Martin; Poulsen, Rikke; Luong, Xuan

2014-01-01

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

Solid phase extraction and metabolic profiling of exudates from living copepods

DEFF Research Database (Denmark)

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

2016-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2011-10-15

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

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

DEFF Research Database (Denmark)

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

2014-01-01

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

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

Science.gov (United States)

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

2013-12-20

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

Solid phase crystallisation of HfO2 thin films

International Nuclear Information System (INIS)

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

2005-01-01

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

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

Science.gov (United States)

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

2013-08-01

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

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

International Nuclear Information System (INIS)

Niemiec, W.

1985-01-01

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

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

International Nuclear Information System (INIS)

Mingarro, E.

1995-01-01

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

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

Science.gov (United States)

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

2015-12-01

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

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

DEFF Research Database (Denmark)

Qvortrup, Katrine; Nielsen, Thomas Eiland

2011-01-01

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

Copper welding in solid phase; Svarka medi v tverdoj faze

Energy Technology Data Exchange (ETDEWEB)

Avagyan, V Sh

1993-12-31

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

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

International Nuclear Information System (INIS)

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

2008-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-06-15

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

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

Science.gov (United States)

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

2014-04-01

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

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

Science.gov (United States)

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

2016-04-21

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

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

International Nuclear Information System (INIS)

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

2011-01-01

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

Solid-phase synthesis of polyfunctional polylysine dendrons using aldehyde linkers

DEFF Research Database (Denmark)

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

2014-01-01

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

Graft-copolymerization of styrene on polypropylene in the solid phase

NARCIS (Netherlands)

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

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

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

DEFF Research Database (Denmark)

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

1990-01-01

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

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

Science.gov (United States)

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

2018-03-01

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

Solid phase 125I labelled radioimmunoassay for spermidine

International Nuclear Information System (INIS)

Zhao Shimin

1991-01-01

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

Solid gas reaction phase diagram under high gas pressure

International Nuclear Information System (INIS)

Ishizaki, K.

1992-01-01

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

Solid phase micro-extraction in environmental atmosphere

International Nuclear Information System (INIS)

Tao Ping; Wei Lifan; Tan Yun

2002-01-01

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

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

Science.gov (United States)

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

2013-01-01

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

Double antibody solid-phase radioimmunoassay for staphylococcal enterotoxin A

International Nuclear Information System (INIS)

Lindroth, S.; Niskanen, A.

1977-01-01

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

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

International Nuclear Information System (INIS)

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

2016-01-01

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

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

Science.gov (United States)

Lü, Weichao; Shen, Shuchang; Wang, Chao

2017-11-08

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

Gibbs Energy Modeling of Digenite and Adjacent Solid-State Phases

Science.gov (United States)

Waldner, Peter

2017-08-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Czerkinsky, C.; Rees, A.S.; Bergimeier, L.A.; Challacombe, S.J. (Guy' s Hospital Medical and Dental Schools, London (UK))

1983-07-01

A solid phase radioimmunoassay has been developed which can be used for the detection of isotype specific antibodies to whole bacteria and other particulate antigens, and is applicable to a variety of species. Bacteria are bound to the solid phase by the use either of antibodies, or of methyl glyoxal. Both methods result in a sensitive and reproducible assay, and bacteria do not appear to desorb from the solid phase. The specificity of antibodies to whole bacteria was examined by absorption of antisera with various species of bacteria and retesting, or by determining the binding of antisera to various bacteria bound to the solid phase. Both methods revealed specificity for the bacteria examined. Inhibition studies showed that antibodies to Streptococcus mutans whole cells could be inhibited by purified cell surface antigens glucosyltransferase and antigen I/II, but only minimally by lipoteichoic acid, c polysaccharide or dextran. In murine antisera antibodies of the IgG, IgM, and IgA classes could be detected at amounts of less than 1 ng/ml.

Controlled phase gate for solid-state charge-qubit architectures

International Nuclear Information System (INIS)

Schirmer, S.G.; Oi, D.K.L.; Greentree, Andrew D.

2005-01-01

We describe a mechanism for realizing a controlled phase gate for solid-state charge qubits. By augmenting the positionally defined qubit with an auxiliary state, and changing the charge distribution in the three-dot system, we are able to effectively switch the Coulombic interaction, effecting an entangling gate. We consider two architectures, and numerically investigate their robustness to gate noise

Solid-phase Synthesis of Combinatorial 2,4-Disubstituted-1,3,5-Triazine via Amine Nucleophilic Reaction

Energy Technology Data Exchange (ETDEWEB)

Moon, Sung Won [KIST Gangneung Institute, Gangneung (Korea, Republic of); Ham, Jungyeob [Gangneung-Wonju National University, Gangneung (Korea, Republic of); Chang, Young-Tae [National University of Singapore, Singapore (Singapore); Lee, Jae Wook [University of Science and Technology, Daejon (Korea, Republic of)

2015-01-15

In combinatorial chemistry, solid-phase synthesis is a popular approach formass production of small molecules. Compared to solution-phase synthesis, it is easy to prepare and purify a large number of heterocyclic small molecules via solid-phase chemistry; the overall reaction time is decreased as well. 1,3,5-Triazine is a nitrogen-containing heterocyclic aromatic scaffold that was shown to be a druggable scaffold in recent studies. These structures have been reported as anticancer, antimicrobial, and antiretroviral compounds, as CDKs and p38 MAP kinase inhibitors, as estrogen receptor modulators, and as inosine monophosphate dehydrogenase inhibitors. we designed and synthesized disubstituted triazine compounds as an analog of disubstituted pyrimidine compounds. These disubstituted triazine compounds possess a linear structure which may have biological activity similar to that of disubstituted pyrimidine. Here we report the solid-phase synthesis of disubstituted triazine compounds.

Solid-phase Synthesis of Combinatorial 2,4-Disubstituted-1,3,5-Triazine via Amine Nucleophilic Reaction

International Nuclear Information System (INIS)

Moon, Sung Won; Ham, Jungyeob; Chang, Young-Tae; Lee, Jae Wook

2015-01-01

In combinatorial chemistry, solid-phase synthesis is a popular approach formass production of small molecules. Compared to solution-phase synthesis, it is easy to prepare and purify a large number of heterocyclic small molecules via solid-phase chemistry; the overall reaction time is decreased as well. 1,3,5-Triazine is a nitrogen-containing heterocyclic aromatic scaffold that was shown to be a druggable scaffold in recent studies. These structures have been reported as anticancer, antimicrobial, and antiretroviral compounds, as CDKs and p38 MAP kinase inhibitors, as estrogen receptor modulators, and as inosine monophosphate dehydrogenase inhibitors. we designed and synthesized disubstituted triazine compounds as an analog of disubstituted pyrimidine compounds. These disubstituted triazine compounds possess a linear structure which may have biological activity similar to that of disubstituted pyrimidine. Here we report the solid-phase synthesis of disubstituted triazine compounds

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

DEFF Research Database (Denmark)

Shelton, Anne Pernille Tofteng; Jensen, Knud Jørgen

2013-01-01

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

Binding of properdin to solid-phase immune complexes

DEFF Research Database (Denmark)

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

1998-01-01

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

Influence of pressure on the solid state phase transformation of Cu–Al–Bi alloy

International Nuclear Information System (INIS)

Gong, Li; Jian-Hua, Liu; Wen-Kui, Wang; Ri-Ping, Liu

2010-01-01

The solid state phase transformation of Cu-Al-Bi alloy under high pressure was investigated by x-ray diffraction, energy dispersive spectroscopy and transmission electron microscopy. Experimental results show that the initial crystalline phase in the Cu-Al-Bi alloy annealed at 750 °C under the pressures in the range of 0–6 GPa is α-Cu solid solution (named as α-Cu phase below), and high pressure has a great influence on the crystallisation process of the Cu-Al-Bi alloy. The grain size of the α-Cu phase decreases with increasing pressure as the pressure is below about 3 GPa, and then increases (P > 3 GPa). The mechanism for the effects of high pressure on the crystallisation process of the alloy has been discussed. (condensed matter: structure, thermal and mechanical properties)

Solid-phase PCR for rapid multiplex detection of Salmonella spp. at the subspecies level, with amplification efficiency comparable to conventional PCR

DEFF Research Database (Denmark)

Chin, Wai Hoe; Sun, Yi; Høgberg, Jonas

2017-01-01

Solid-phase PCR (SP-PCR) has attracted considerable interest in different research fields since it allows parallel DNA amplification on the surface of a solid substrate. However, the applications of SP-PCR have been hampered by the low efficiency of the solid-phase amplification. In order to incr...... diagnosis, high-throughput DNA sequencing, and single-nucleotide polymorphism analysis. Graphical abstract Schematic representation of solid-phase PCR....

General approach to standardization of the solid-phase radioimmunoassay for quantitation of class-specific antibodies

Energy Technology Data Exchange (ETDEWEB)

Zollinger, W D; Boslego, J W [Walter Reed Army Inst. of Research, Washington, DC (USA)

1981-10-30

The feasibility of using an anti-human immunoglobulin/human immunoglobulin/(/sup 125/I)anti-human immunoglobulin 'sandwich' in a solid-phase radioimmunoassay to produce a standard curve which could be used to quantitate antigen-specific antibody of a particular immunoglobulin class was investigated. The amount of secondary antibody (SAb) bound was determined as a function of whether the primary antibody (PAb) was bound to its specific solid-phase antigen or by a solid-phase anti-human immunoglobulin. No significant difference between the two values was observed. Quantitation of anti-tetanus toxoid antibody by this method was in a good agreement with quantitative precipitin tests. Comparison of SAb binding as a function of the way the PAb is bound was extended to class-specific PAb by use of murine monoclonal antibodies to meningococcal antigens. In most cases somewhat greater binding of SAb occurred when PAb was bound to antigen, but in several cases where low avidity antibody and/or poor quality antigens were used, greater SAb binding occurred when PAb was bound by anti-mouse immunoglobulin. The results indicate that this approach may be useful as a general method for standardizing the SPRIA and other solid-phase immunoassays such as the ELISA to measure class-specific antibody.

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

Science.gov (United States)

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

2015-04-15

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

Solid-phase extraction and determination of trace elements in environmental samples using naphthalene adsorbent

International Nuclear Information System (INIS)

Pourreza, N.

2004-01-01

Naphthalene co-precipitated with quaternary ammonium salt such as tetraoctyl ammonium bromide and methyltrioctyl ammonium chloride have been used as adsorbent for solid phase extraction of metal ions such as Hg, Cd and Fe. The metal ions are retained on the adsorbent in a column as their complexes with suitable ligands and eluted by an eluent before instrumental measurements. The optimization of the procedures for solid phase extraction and consequent determination of trace elements and application to environmental samples especially water samples will be discussed. (author)

Quantum computational capability of a 2D valence bond solid phase

International Nuclear Information System (INIS)

Miyake, Akimasa

2011-01-01

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

Structural study of chlorine tri-fluoride and bromine penta-fluoride in liquid and solid phase

International Nuclear Information System (INIS)

Rousson, R.

1973-01-01

This research thesis reports the structural study of chlorine tri-fluoride and bromine penta-fluoride between 20 C and about -265 C. After some generalities on these compounds and a presentation of the experimental technique, the author reports and discusses results obtained with these both compounds: Raman spectrum for the liquid and for the solid phase, infrared spectrum for the solid phase, calorimetric measurements. In the case of chlorine tri-fluoride, the author studies the evolution of the liquid spectrum with temperature, shows the existence of an intermediate solid phase, and compares results obtained by Raman spectroscopy and nuclear magnetic resonance. He also applies to bromine penta-fluoride an analysis of normal coordinates of a XF 5 molecule: relationship between force constants and vibration frequencies, application of Wilson method, resolution of the molecular equation, determination of normal vibration modes [fr

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

Directory of Open Access Journals (Sweden)

Wei Li

2018-02-01

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

Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

International Nuclear Information System (INIS)

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

2012-01-01

Highlights: ► The use of CNTs as sorbent for metal species in solid phase extraction has been described. ► Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. ► Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes – due to their high adsorption and desorption capacities – have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

Energy Technology Data Exchange (ETDEWEB)

Herrero Latorre, C., E-mail: carlos.herrero@usc.es [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain); Alvarez Mendez, J.; Barciela Garcia, J.; Garcia Martin, S.; Pena Crecente, R.M. [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain)

2012-10-24

Highlights: Black-Right-Pointing-Pointer The use of CNTs as sorbent for metal species in solid phase extraction has been described. Black-Right-Pointing-Pointer Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. Black-Right-Pointing-Pointer Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes - due to their high adsorption and desorption capacities - have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

Thermal conductivity of solid cyclohexane in orientationally ordered and disordered phases

International Nuclear Information System (INIS)

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

2011-01-01

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

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

Science.gov (United States)

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

2017-10-26

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

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

Czech Academy of Sciences Publication Activity Database

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

2004-01-01

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

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

Directory of Open Access Journals (Sweden)

Behzad Binesh

2016-02-01

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

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

OpenAIRE

Lazar, Paul

2005-01-01

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 (...

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

Science.gov (United States)

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

2018-03-01

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

Computer-aided design model for anaerobic-phased-solids digester system

Energy Technology Data Exchange (ETDEWEB)

Zhang, Z.; Zhang, R. [University of California, Davis, CA (United States); Tiangco, V. [California Energy Commission, Sacramento, CA (United States)

1999-07-01

The anaerobic-phased-solids (APS) digester system is a newly developed anaerobic digestion system for converting solid wastes, such as crop residues and food wastes, into biogas for power and heat generation. A computer-aided engineering design model has been developed to design the APS-digester system and study the heat transfer from the reactors and energy production of the system. Simulation results of a case study are presented by using the model to predict the heating energy requirement and biogas energy production for anaerobic digestion of garlic waste. The important factors, such as environmental conditions, insulation properties, and characteristics of the wastes, on net energy production are also investigated. (author)

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

National Research Council Canada - National Science Library

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

2005-01-01

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

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

OpenAIRE

MacFarlane, John D.

1997-01-01

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.

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

Science.gov (United States)

Polsin, D. N.

2017-10-01

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

The effect of high antigen density on solid-phase radioimmunoassays for antibody regardless of immunoglobulin class

International Nuclear Information System (INIS)

Rubin, R.L.; Hardtke, M.A.; Carr, R.I.

1980-01-01

Human sera containing antibody to casein or to bovine serum albumin were used to assess the validity and utility of a solid-phase assay for quantitating antibody activity. Rabbit anti-human immunoglobulin radiolabeled with 125 I and capable of reacting with all human immunoglobulin classes was used to detect antibody bound to antigen immobilized to polystyrene tubes by a new covalent technique. This method results in very high antigen concentrations in highly stable association with polystyrene tubes. Kinetic and absorption studies demonstrated that low avidity antibodies are better detected when antigen is immobilized by the covalent method than when passively adsorbed. Conditions are described for minimizing artifactual interactions and for obtaining results similar to those obtained with conventional, liquid-phase assays. Failure to reach equilibrium in solid-phase assays and other problems are proposed to explain, in part, the inability to obtain a better correlation between solid- and liquid-phase immunoassays. (Auth.)

Development of solid phase radioimmunoassay using antibody coupled magnetizable particles for measurement of progesterone in human serum

International Nuclear Information System (INIS)

Mehany, N.L.

2007-01-01

The aim of the present study was to prepare solid phase radioimmunoassay (RIA) reagents. Development as well as optimization and validation of RIA system using solid phase magnetic particles for the measurement of progesterone in human serum are described. The production of polyclonal antibodies was carried out by immunizing five white New-Zealand rabbits subcutaneously. Low density magnetizable cellulose iron oxide particles have been used to couple covalently to the IgG fraction of polyclonal anti-progesterone using carbonyl diimidazole activation method and applied as a solid phase separating agent for RIA of serum progesterone. 125 I-progesterone tracer was prepared using chloramine-T and iodogen oxidation methods and purified using high performance liquid chromatography. The progesterone standards were prepared using highly purified progesterone powder with hormone free serum as standard matrix. Optimization and validation of the assay were carried out. The results obtained provide a low cost, simple, sensitive, specific and accurate RIA system of progesterone based on magnetizable solid phase separation. This may be extremely helpful in diagnosis and proper management of ovulation during childbearing years

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

International Nuclear Information System (INIS)

Czerkinsky, C.; Rees, A.S.; Bergimeier, L.A.; Challacombe, S.J.

1983-01-01

A solid phase radioimmunoassay has been developed which can be used for the detection of isotype specific antibodies to whole bacteria and other particulate antigens, and is applicable to a variety of species. Bacteria are bound to the solid phase by the use either of antibodies, or of methyl glyoxal. Both methods result in a sensitive and reproducible assay, and bacteria do not appear to desorb from the solid phase. The specificity of antibodies to whole bacteria was examined by absorption of antisera with various species of bacteria and retesting, or by determining the binding of antisera to various bacteria bound to the solid phase. Both methods revealed specificity for the bacteria examined. Inhibition studies showed that antibodies to Streptococcus mutans whole cells could be inhibited by purified cell surface antigens glucosyltransferase and antigen I/II, but only minimally by lipoteichoic acid, c polysaccharide or dextran. In murine antisera antibodies of the IgG, IgM, and IgA classes could be detected at amounts of less than 1 ng/ml. (author)

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

International Nuclear Information System (INIS)

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

1978-01-01

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

New solid phase radioimmunoassay (CLB-RIA) for the detection of hepatitis-B antigen and antibody

Energy Technology Data Exchange (ETDEWEB)

Duimel, W J [Centraal Laboratorium van de Bloedtransfusiedienst, Amsterdam; Brummelhuis, H G.J.

1975-07-01

A new competitive solid phase radioimmunoassay (CLB-RIA) has been developed for the detection of HBAg and HBAb in human serum and plasma. In the assay, sheep antibodies to HBAg, covalently linked to an insoluble carrier, highly purified /sup 125/I labelled HBAg and the serum or plasma sample are incubated for 20 h at room temperature. After incubation, the bound and the free fraction of the tracer are separated by centrifugation. The presence of both HBAg and HBAb results in a decrease of the amount of bound tracer, when compared with a negative control serum. Differentiation between HBAg and HBAb requires the use of another type of radioimmunoassay. For this purpose a sandwich solid phase radioimmunoassay, for the detection of HBAb only, has been developed (CLB-AURIA). In this, assay-purified HBAg is covalently linked to an insoluble carrier. Using a mixture of both immunosorbents (insolubilized HBAg and HBAb), it is possible to detect and to distinguish HBAg and HBAb in one single solid phase radioimmunoassay (CLB-MIRIA). The influence of three parameters on the CLB-RIA, the incubation time, the amount of tracer and the effect of Tween-20 has been studied. The sensitivity of the described solid phase CLB-RIA for the detection of HBAg is comparable to that of other radioimmunoassays reported in literature; its specificity is very high.

Solid-phase vibrational redox reactions in coordinated oxides

International Nuclear Information System (INIS)

Kostikova, G.P.; Korol'kov, D.V.; Kostikov, Yu.P.

1996-01-01

The properties of multicomponent oxides (YBa 2 Cu 3 O 7-x , etc.), incorporating different valency forms of each of two (or more) different elements have been compared with the properties of the known chemical systems, where vibrational (periodic) redox-reactions are realized a fortiori. The essence of the new theoretical concept suggested consists in the following: high-T c superconductivity of the complex oxides and similar compounds originates from vibrational redox reaction proceeding in solid phase and involving different valency atoms of every element

Solid-phase extraction of carotenoids.

Science.gov (United States)

Shen, Yao; Hu, Yumin; Huang, Ke; Yin, Shi'an; Chen, Bo; Yao, Shouzhuo

2009-07-24

In this work, solid-phase extraction (SPE) trapping performance of lutein and beta-carotene, which were used as the model molecules of carotenoids, was investigated. The absorption, elution, and enrichment of carotenoids on SPE cartridges with four different sorbents, i.e. C(30), C(18), diol, and silica, were compared respectively with the help of frontal analysis technique. The high retentions of both lutein and beta-carotene were achieved on the C(18) and C(30) cartridges. The diol and silica cartridges only had good retention for lutein. The optimized SPE method for sample pretreatment for the carotenoids analysis was obtained after the investigation of trapping performance. The method was applied successfully to the analysis of biological sample, i.e. serum and human breast milk. The recovery, accuracy, and precision of SPE method comparing with those of traditional liquid-liquid extraction (LLE) method for the sample pretreatment for the analysis of carotenoids owned a number of advantages such as rapid, no chloroform used, and accurate versus LLE.

Visualizing a dilute vortex liquid to solid phase transition in a Bi2Sr2CaCu2O8 single crystal

International Nuclear Information System (INIS)

Shaw, Gorky; Mandal, Pabitra; Banerjee, S S; Tamegai, T

2012-01-01

Using high-sensitivity magneto-optical imaging, we find evidence for a jump in local vortex density associated with a vortex liquid to vortex solid phase transition just above the lower critical field in a single crystal of Bi 2 Sr 2 CaCu 2 O 8 . We find that the regions of the sample where the jump in vortex density occurs are associated with low screening currents. In the field–temperature vortex phase diagram, we identify phase boundaries demarcating a dilute vortex liquid phase and the vortex solid phase. The phase diagram also identifies a coexistence regime of the dilute vortex liquid and solid phases and shows the effect of pinning on the vortex liquid to vortex solid phase transition line. We find that the phase boundary lines can be fitted to the theoretically predicted expression for the low-field portion of the phase boundary delineating a dilute vortex solid from a vortex liquid phase. We show that the same theoretical fit can be used to describe the pinning dependence of the low-field phase boundary lines provided that the dependence of the Lindemann number on pinning strength is considered. (paper)

Powder metallurgy: Solid and liquid phase sintering of copper

Science.gov (United States)

Sheldon, Rex; Weiser, Martin W.

1993-01-01

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

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

International Nuclear Information System (INIS)

Bashir, T.

1996-01-01

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

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

Science.gov (United States)

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

2015-09-01

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

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

International Nuclear Information System (INIS)

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

2000-01-01

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

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

NARCIS (Netherlands)

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

2012-01-01

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

New practical algorithm for modelling analyte recovery in bioanalytical reversed phase and mixed-mode solid phase extraction

NARCIS (Netherlands)

Hendriks, G.; Uges, D. R. A.; Franke, J. P.

2008-01-01

Solid phase extraction (SPE) is a widely used method for sample cleanup and sample concentration in bioanalytical sample preparation. A few methods to model the retention behaviour on SPE cartridges have been described previously but they are either not applicable to ionised species or are not

Anti-glomerular basement membrane autoantibodies in the Brown Norway rat: detection by a solid-phase radioimmunoassay

International Nuclear Information System (INIS)

Bowman, C.; Peters, D.K.; Lockwood, C.M.

1983-01-01

A solid-phase radioimmunoassay (RIA) is described for the detection of IgG autoantibodies to glomerular basement membrane (GBM) induced in the Brown Norway rat by mercuric chloride. The assay involves the adsorption of a collagenase digest of GBM to plastic microtitre plates and detection of bound antibody with affinity purified radiolabelled rabbit anti-rat IgG. Comparison with existing immunofluorescence methods for detection of anti-GBM antibody showed that the solid-phase RIA is highly sensitive, allowing detection of antibody in solutions with as low as 0.5 ng protein/ml. The assay is suitable for detection of anti-GBM antibody both in serum and in eluates from nephritic kidneys. The assay proved to be specific in competitive studies of inhibition brought about by GBM, keyhole limpet antigen and ovalbumin. This solid-phase RIA is reproducible, robust and easy to perform. (Auth.)

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

Science.gov (United States)

Ensafi, Ali A; Ghaderi, Ali R

2007-09-05

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

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

KAUST Repository

Shao, Sihong; Qian, Tiezheng

2012-01-01

We develop a continuum hydrodynamic model for two-phase immiscible flows that involve electroosmotic effect in an electrolyte and moving contact line at solid surfaces. The model is derived through a variational approach based on the Onsager

Isostructural solid-solid transition of (colloidal) simple fluids

International Nuclear Information System (INIS)

Tejero, C.F.; Daanoun, A.; Lakkerkerker, H.N.W.; Baus, M.

1995-01-01

A variational approach based on the Gibbs-Bogoliubov inequality is used in order to evaluate the free energy of simple fluids described by a double-Yukawa pair potential. A hard-sphere reference fluid is used to describe the fluid phases, and an Einstein reference crystal to describe the solid phases. Apart from the usual type of phase diagram, typical of atomic simple fluids with long-ranged attractions, we find two types of phase diagrams, specific to colloidal systems with intermediate and short-ranged attractions. One of the latter phase diagrams exhibits an isostructural solid-solid transition, which has not yet been observed experimentally

Solid-phase peptide quantitation assay using labeled monoclonal antibody and glutaraldehyde fixation

International Nuclear Information System (INIS)

Kasprzyk, P.G.; Cuttitta, F.; Avis, I.; Nakanishi, Y.; Treston, A.; Wong, H.; Walsh, J.H.; Mulshine, J.L.

1988-01-01

A solid-phase radioimmunoassay utilizing iodinated peptide-specific monoclonal antibody as a detection system instead of labeled peptide has been developed. Regional specific monoclonal antibodies to either gastrin-releasing peptide or gastrin were used as models to validate the general application of our modified assay. Conditions for radioactive labeling of the monoclonal antibody were determined to minimize oxidant damage, which compromises the sensitivity of other reported peptide quantitation assays. Pretreatment of 96-well polyvinyl chloride test plates with a 5% glutaraldehyde solution resulted in consistent retention of sufficient target peptide on the solid-phase matrix to allow precise quantitation. This quantitative method is completed within 1 h of peptide solid phasing. Pretreatment of assay plates with glutaraldehyde increased binding of target peptide and maximized antibody binding by optimizing antigen presentation. The hypothesis that glutaraldehyde affects both peptide binding to the plate and orientation of the peptide was confirmed by analysis of several peptide analogs. These studies indicate that peptide binding was mediated through a free amino group leaving the carboxy-terminal portion of the target peptide accessible for antibody binding. It was observed that the length of the peptide also affects the amount of monoclonal antibody that will bind. Under the optimal conditions, results from quantitation of gastrin-releasing peptide in relevant samples agree well with those from previously reported techniques. Thus, we report here a modified microplate assay which may be generally applied for the rapid and sensitive quantitation of peptide hormones

Development Of Solid Phase Radioimmunoassay Using Antibody Coupled Cellulose Particles For Measurement Of Prolactin In Human Serum

International Nuclear Information System (INIS)

Abdel-Ghany, I.Y.

2013-01-01

The objective of the present study was to prepare solid phase radioimmunoassay (RIA) reagents. Development as well as optimization and validation of RIA system using solid phase cellulose particles for the measurement of prolactin (PRL) in human serum were described. The production of polyclonal antibodies was carried out by immunizing three Balb/C mice intraperitoneal through primary injection and two booster doses. The activation of cellulose particles using 1,1-carbonyl diimidazole (CDI) and coupling of these solid phase particles with IgG fraction of mouse anti-PRL were carried out. Preparation of 125 I-PRL tracer was prepared using lactoperoxidase method then purified by gel filtration using sephadex G-100. The PRL standards were prepared using a highly purified PRL antigen with assay buffer as standard matrix. Optimization and validation of the assay were carried out. The results obtained provide a low cost, simple, sensitive, specific and accurate RIA system of prolactin based on solid phase separation. These cellulose particles retain their characteristics during storage for 6 months at 4 degree C. In conclusion, this assay could be used as a useful diagnostic tool for pituitary dysfunctions and possible reproductive disability

Quantification of VX Nerve Agent in Various Food Matrices by Solid-Phase Extraction Ultra-Performance Liquid ChromatographyTime-of-Flight Mass Spectrometry

Science.gov (United States)

2016-04-01

QUANTIFICATION OF VX NERVE AGENT IN VARIOUS FOOD MATRICES BY SOLID - PHASE EXTRACTION ULTRA-PERFORMANCE...TITLE AND SUBTITLE Quantification of VX Nerve Agent in Various Food Matrices by Solid - Phase Extraction Ultra-Performance Liquid Chromatography...QUANTIFICATION OF VX NERVE AGENT IN VARIOUS FOOD MATRICES BY SOLID - PHASE EXTRACTION ULTRA-PERFORMANCE LIQUID CHROMATOGRAPHY–TIME-OF-FLIGHT MASS

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

International Nuclear Information System (INIS)

Strohm, W.D.; Legler, K.; Gerlich, W.; Stamm, B.; Zimmer, S.; Biotest-Serum-Institut G.m.b.H., Frankfurt am Main; Goettingen Univ.

1978-01-01

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.) [de

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

Energy Technology Data Exchange (ETDEWEB)

Strohm, W D; Legler, K; Gerlich, W; Stamm, B; Zimmer, S [Frankfurt Univ. (Germany, F.R.). Abt. fuer Gastroenterologie; Biotest-Serum-Institut G.m.b.H., Frankfurt am Main (Germany, F.R.); Goettingen Univ. (Germany, F.R.). Hygiene-Institut)

1978-09-01

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.

Uncovering the Connection Between Low-Frequency Dynamics and Phase Transformation Phenomena in Molecular Solids

Science.gov (United States)

Ruggiero, Michael T.; Zhang, Wei; Bond, Andrew D.; Mittleman, Daniel M.; Zeitler, J. Axel

2018-05-01

The low-frequency motions of molecules in the condensed phase have been shown to be vital to a large number of physical properties and processes. However, in the case of disordered systems, it is often difficult to elucidate the atomic-level details surrounding these phenomena. In this work, we have performed an extensive experimental and computational study on the molecular solid camphor, which exhibits a rich and complex structure-dynamics relationship, and undergoes an order-disorder transition near ambient conditions. The combination of x-ray diffraction, variable temperature and pressure terahertz time-domain spectroscopy, ab initio molecular dynamics, and periodic density functional theory calculations enables a complete picture of the phase transition to be obtained, inclusive of mechanistic, structural, and thermodynamic phenomena. Additionally, the low-frequency vibrations of a disordered solid are characterized for the first time with atomic-level precision, uncovering a clear link between such motions and the phase transformation. Overall, this combination of methods allows for significant details to be obtained for disordered solids and the associated transformations, providing a framework that can be directly applied for a wide range of similar systems.

Chromatography, solid-phase extraction, and capillary electrochromatography with MIPs.

Science.gov (United States)

Tóth, Blanka; Horvai, George

2012-01-01

Most analytical applications of molecularly imprinted polymers are based on their selective adsorption properties towards the template or its analogs. In chromatography, solid phase extraction and electrochromatography this adsorption is a dynamic process. The dynamic process combined with the nonlinear adsorption isotherm of the polymers and other factors results in complications which have limited the success of imprinted polymers. This chapter explains these problems and shows many examples of successful applications overcoming or avoiding the problems.

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

Directory of Open Access Journals (Sweden)

Helena Prosen

2014-05-01

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

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

Science.gov (United States)

Prosen, Helena

2014-05-23

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

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

International Nuclear Information System (INIS)

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

2014-01-01

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

On the formation of molecules and solid-state compounds from the AGB to the PN phases

Science.gov (United States)

García-Hernández, D. A.; Manchado, A.

2016-07-01

During the asymptoyic giant branch (AGB) phase, different elements are dredge- up to the stellar surface depending on progenitor mass and metallicity. When the mass loss increases at the end of the AGB, a circumstellar dust shell is formed, where different (C-rich or O-rich) molecules and solid-state compounds are formed. These are further processed in the transition phase between AGB stars and planetary nebulae (PNe) to create more complex organic molecules and inorganic solid-state compounds (e.g., polycyclic aromatic hydrocarbons, fullerenes, and graphene precursors in C-rich environments and oxides and crystalline silicates in O-rich ones). We present an observational review of the different molecules and solid-state materials that are formed from the AGB to the PN phases. We focus on the formation routes of complex fullerene (and fullerene-based) molecules as well as on the level of dust processing depending on metallicity.

Development of andrographolide molecularly imprinted polymer for solid-phase extraction

Science.gov (United States)

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

2011-06-01

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

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

Science.gov (United States)

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

2015-04-01

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

Safety profile of avelumab in patients with advanced solid tumors: A pooled analysis of data from the phase 1 JAVELIN solid tumor and phase 2 JAVELIN Merkel 200 clinical trials

OpenAIRE

Kelly, K; Infante, JR; Taylor, MH; Patel, MR; Wong, DJ; Iannotti, N; Mehnert, JM; Loos, AH; Koch, H; Speit, I; Gulley, JL

2018-01-01

© 2018 The Authors. Cancer published by Wiley Periodicals, Inc. on behalf of American Cancer Society. BACKGROUND: Antibodies targeting the programmed death-ligand 1 (PD-L1)/programmed cell death protein 1 (PD-1) checkpoint may cause adverse events (AEs) that are linked to the mechanism of action of this therapeutic class and unique from those observed with conventional chemotherapy. METHODS: Patients with advanced solid tumors who were enrolled in the phase 1 JAVELIN Solid Tumor (1650 patient...

Electronic structure of elements and compounds and electronic phases of solids

International Nuclear Information System (INIS)

Nadykto, B.A.

2000-01-01

The paper reviews technique and computed energies for various electronic states of many-electron multiply charged ions, molecular ions, and electronic phases of solids. The model used allows computation of the state energy for free many-electron multiply charged ions with relative accuracy ∼10 -4 suitable for analysis of spectroscopy data

Hypercrosslinked particles for the extraction of sweeteners using dispersive solid-phase extraction from environmental samples.

Science.gov (United States)

Lakade, Sameer S; Zhou, Qing; Li, Aimin; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa M

2018-04-01

This work presents a new extraction material, namely, Q-100, based on hypercrosslinked magnetic particles, which was tested in dispersive solid-phase extraction for a group of sweeteners from environmental samples. The hypercrosslinked Q-100 magnetic particles had the advantage of suitable pore size distribution and high surface area, and showed good retention behavior toward sweeteners. Different dispersive solid-phase extraction parameters such as amount of magnetic particles or extraction time were optimized. Under optimum conditions, Q-100 showed suitable apparent recovery, ranging in the case of river water sample from 21 to 88% for all the sweeteners, except for alitame (12%). The validated method based on dispersive solid-phase extraction using Q-100 followed by liquid chromatography with tandem mass spectrometry provided good linearity and limits of quantification between 0.01 and 0.1 μg/L. The method was applied to analyze samples from river water and effluent wastewater, and four sweeteners (acesulfame, saccharin, cyclamate, and sucralose) were found in both types of sample. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Homogeneous nucleation in phase separation of solid 3He-4He mixtures

International Nuclear Information System (INIS)

Poole, M.; Smith, A.; Maidanov, V.A.; Rudavskii, E.Ya.; Grigor'ev, V.N.; Slezov, V.V.; Saunders, J.; Cowan, B.

2003-01-01

NMR and pressure have been measured during phase separation in solid 3 He- 4 He mixtures. Spin echoes were used to observe bounded diffusion and to estimate the diffusion coefficient, size and nuclei concentration in the 3 He-enriched phase. The characteristic phase separation time constant of the mixture was found from pressure measurements. The results argue convincingly for homogeneous nucleation. The surface tension of the nuclei is found independently from NMR and from pressure measurements; the two determinations agree well and yield a surface tension coefficient of 4.9x10 -6 J m -2

Dispersive solid-phase imprinting of proteins for the production of plastic antibodies

DEFF Research Database (Denmark)

Ashley, Jon; Feng, Xiaotong; Halder, Arnab

2018-01-01

We describe a novel dispersive solid-phase imprinting technique for the production of nano-sized molecularly imprinted polymers (nanoMIPs) as plastic antibodies. The template was immobilized on in-house synthesized magnetic microspheres instead of conventional glass beads. As a result, high...

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

DEFF Research Database (Denmark)

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

2014-01-01

A facile and expedient route to the synthesis of arylopeptoid oligomers (N-alkylated aminomethyl benz-amides) using semi-automated microwave-assisted solid-phase synthesis is presented. The synthesis was optimized for the incorporation of side chains derived from sterically hindered or unreactive...

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

CSIR Research Space (South Africa)

Mtshali, TN

2012-11-01

Full Text Available Iron is a limiting nutrient in many parts of the oceans, including the unproductive regions of the Southern Ocean. Although the dominant fraction of the marine iron pool occurs in the form of solid-phase particles, its chemical speciation...

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

Science.gov (United States)

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

2018-04-01

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

An in-line clean system for the solid-phase extraction of emerging contaminants in natural waters

OpenAIRE

Sodré, Fernando F.; Locatelli, Marco Antonio F.; Jardim, Wilson F.

2010-01-01

A solid-phase in-line extraction system for water samples containing low levels of emerging contaminants is described. The system was specially developed for large volume samples (up to 4 L) using commercial solid-phase extraction (SPE) cartridges. Four sets containing PTFE-made connectors, brass adapters and ball valves were used to fit SPE cartridges and sample bottles to a 4-port manifold attached to a 20 L carboy. A lab-made vacuum device was connected to the manifold cap. The apparatus i...

Automated Solid-Phase Radiofluorination Using Polymer-Supported Phosphazenes

DEFF Research Database (Denmark)

Mathiessen, Bente; Zhuravlev, Fedor

2013-01-01

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.......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...

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

International Nuclear Information System (INIS)

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

2004-01-01

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

Solid-phase extraction (SPE) of Iron using Lanthanum Silicate ion exchange

International Nuclear Information System (INIS)

Kiarostami, V.; Husain, W.

2002-01-01

Solid-phase extraction (SPE) is gaining wide use as an effective and speedy technique which reduces solvent usage, disposal costs and extraction time. The analyte is adsorbed from solution onto a solid adsorbent, which is followed by elution of the analyte with a solvent appropriate for instrumental analysis. However, there is an increasing need for new selective adsorbents to expand the area of this technique. Lanthanum silicate ion exchanger, which shows unusual selectivity elements and in this study, it was employed to develop a SPE method for iron ion. Special experiments such as determination of distribution coefficient for iron ion in different solvent systems have been determined

Separation of phenolic acids from sugarcane rind by online solid-phase extraction with high-speed counter-current chromatography.

Science.gov (United States)

Geng, Ping; Fang, Yingtong; Xie, Ronglong; Hu, Weilun; Xi, Xingjun; Chu, Qiao; Dong, Genlai; Shaheen, Nusrat; Wei, Yun

2017-02-01

Sugarcane rind contains some functional phenolic acids. The separation of these compounds from sugarcane rind is able to realize the integrated utilization of the crop and reduce environment pollution. In this paper, a novel protocol based on interfacing online solid-phase extraction with high-speed counter-current chromatography (HSCCC) was established, aiming at improving and simplifying the process of phenolic acids separation from sugarcane rind. The conditions of online solid-phase extraction with HSCCC involving solvent system, flow rate of mobile phase as well as saturated extent of absorption of solid-phase extraction were optimized to improve extraction efficiency and reduce separation time. The separation of phenolic acids was performed with a two-phase solvent system composed of butanol/acetic acid/water at a volume ratio of 4:1:5, and the developed online solid-phase extraction with HSCCC method was validated and successfully applied for sugarcane rind, and three phenolic acids including 6.73 mg of gallic acid, 10.85 mg of p-coumaric acid, and 2.78 mg of ferulic acid with purities of 60.2, 95.4, and 84%, respectively, were obtained from 150 mg sugarcane rind crude extracts. In addition, the three different elution methods of phenolic acids purification including HSCCC, elution-extrusion counter-current chromatography and back-extrusion counter-current chromatography were compared. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

Science.gov (United States)

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

2018-03-01

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

Basal plane shift as an order parameter of transitions between antiferromagnetic phases of solid oxygen

International Nuclear Information System (INIS)

Gomonay, E.V.; Loktev, V.M.

2005-01-01

A phenomenological model in the spirit of the Landau theory of phase transitions is derived, and the conditions for existence and phase transitions between different magnetocrystal structures of solid oxygen are analyzed for wide ranges of pressure, temperature and external magnetic field

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

Energy Technology Data Exchange (ETDEWEB)

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

2007-09-05

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

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

International Nuclear Information System (INIS)

Ensafi, Ali A.; Ghaderi, Ali R.

2007-01-01

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

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

KAUST Repository

Song, Zhibo

2018-04-04

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

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

Science.gov (United States)

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

2018-04-01

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

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

Science.gov (United States)

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

1995-01-01

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

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

KAUST Repository

Zia, Asif I.

2016-03-30

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

Determination of solid- and liquid-phase gastric emptying half times in cats by use of nuclear scintigraphy.

Science.gov (United States)

Costello, M; Papasouliotis, K; Barr, F J; Gruffydd-Jones, T J; Caney, S M

1999-10-01

To use nuclear scintigraphy to establish a range of gastric emptying half times (t1/2) following a liquid or solid meal in nonsedated cats. 12 clinically normal 3-year-old domestic shorthair cats. A test meal of 75 g of scrambled eggs labeled with technetium Tc 99m tin colloid was fed to 10 of the cats, and solid-phase gastric emptying t1/2 were determined by use of nuclear scintigraphy. In a separate experiment, 8 of these cats plus an additional 2 cats were fed 18 ml (n = 5) or 36 ml (n = 5) of a nutrient liquid meal labeled with technetium Tc 99m pentetate. Liquid-phase gastric emptying t1/2 then were determined by use of scintigraphy. Solid-phase gastric emptying t1/2 were between 210 and 769 minutes (median, 330 minutes). Median liquid-phase gastric emptying t1/2 after ingestion of 18 or 36 ml of the test meal were 67 minutes (range, 60 to 96 minutes) and 117 minutes (range, 101 to 170 minutes), respectively. The median t1/2 determined for cats receiving 18 ml of the radiolabeled liquid was significantly less than that determined for cats receiving 36 ml of the test meal. The protocol was tolerated by nonsedated cats. Solid-phase gastric emptying t1/2 were prolonged, compared with liquid-phase t1/2, and a major factor governing the emptying rate of liquids was the volume consumed. Nuclear scintigraphy may prove useful in assessing gastric motility disorders in cats.

Application of a sepharose bead immunofluorescence assay and a solid-phase radioimmunoassay to the bovine leukemia virus system

International Nuclear Information System (INIS)

Fiebach, H.; Uckert, W.; Micheel, B.

1982-01-01

Several fluorescence assays with bovine leukemia virus (BLV) conjugated to activated Sepharose 4B were used for the detection of BLV and anti-BLV antibodies. These tests were compared with a solid-phase radioimmunoassay and found to be in the same sensitivity range. Sepharose bead immunofluorescence assay and solid-phase radioimmunoassay can be applied to the diagnosis of BLV infection in cattle. (author)

Application of a sepharose bead immunofluorescence assay and a solid-phase radioimmunoassay to the bovine leukemia virus system

Energy Technology Data Exchange (ETDEWEB)

Fiebach, H.; Uckert, W.; Micheel, B. (Akademie der Wissenschaften der DDR, Berlin. Zentralinstitut fuer Krebsforschung)

Several fluorescence assays with bovine leukemia virus (BLV) conjugated to activated Sepharose 4B were used for the detection of BLV and anti-BLV antibodies. These tests were compared with a solid-phase radioimmunoassay and found to be in the same sensitivity range. Sepharose bead immunofluorescence assay and solid-phase radioimmunoassay can be applied to the diagnosis of BLV infection in cattle.

DNA microarray-based solid-phase RT-PCR for rapid detection and identification of influenza virus type A and subtypes H5 and H7

DEFF Research Database (Denmark)

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

2011-01-01

of RNA extract in the liquid phase with sequence-specific nested PCR on the solid phase. A simple ultraviolet cross-linking method was used to immobilize the DNA probes over an unmodified glass surface, which makes solid-phase PCR a convenient possibility for AIV screening. The testing of 33 avian fecal....... In this article, a DNA microarray-based solid-phase polymerase chain reaction (PCR) approach has been developed for rapid detection of influenza virus type A and for simultaneous identification of pathogenic virus subtypes H5 and H7. This solid-phase RT-PCR method combined reverse-transcription amplification...

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

International Nuclear Information System (INIS)

Rosencrance, S.

2003-01-01

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

Fluorine incorporation during Si solid phase epitaxy

International Nuclear Information System (INIS)

Impellizzeri, G.; Mirabella, S.; Romano, L.; Napolitani, E.; Carnera, A.; Grimaldi, M.G.; Priolo, F.

2006-01-01

We have investigated the F incorporation and segregation in preamorphized Si during solid phase epitaxy (SPE) at different temperatures and for several implanted-F energies and fluences. The Si samples were amorphized to a depth of 550 nm by implanting Si at liquid nitrogen temperature and then enriched with F at different energies (65-150 keV) and fluences (0.07-5 x 10 14 F/cm 2 ). Subsequently, the samples were regrown by SPE at different temperatures: 580, 700 and 800 deg. C. We have found that the amount of F incorporated after SPE strongly depends on the SPE temperature and on the energy and fluence of the implanted-F, opening the possibility to tailor the F profile during SPE

A combination of solid-phase extraction and dispersive solid-phase extraction effectively reduces the matrix interference in liquid chromatography-ultraviolet detection during pyraclostrobin analysis in perilla leaves.

Science.gov (United States)

Farha, Waziha; Rahman, Md Musfiqur; Abd El-Aty, A M; Jung, Da-I; Kabir, Md Humayun; Choi, Jeong-Heui; Kim, Sung-Woo; Im, So Jeong; Lee, Young-Jun; Shin, Ho-Chul; Kwon, Chan-Hyeok; Son, Young-Wook; Lee, Kang-Bong; Shim, Jae-Han

2015-12-01

Perilla leaves contain many interfering substances; thus, it is difficult to protect the analytes during identification and integration. Furthermore, increasing the amount of sample to lower the detection limit worsens the situation. To overcome this problem, we established a new method using a combination of solid-phase extraction and dispersive solid-phase extraction to analyze pyraclostrobin in perilla leaves by liquid chromatography with ultraviolet absorbance detection. The target compound was quantitated by external calibration with a good determination coefficient (R(2) = 0.997). The method was validated (in triplicate) with three fortification levels, and 79.06- 89.10% of the target compound was recovered with a relative standard deviation <4. The limits of detection and quantification were 0.0033 and 0.01 mg/kg, respectively. The method was successfully applied to field samples collected from two different areas at Gwangju and Muan. The decline in the resiudue concentrations was best ascribed to a first-order kinetic model with half-lives of 5.7 and 4.6 days. The variation between the patterns was attributed to humidity. Copyright © 2015 John Wiley & Sons, Ltd.

Behaviour of solid phase ethyl cyanide in simulated conditions of Titan

Science.gov (United States)

Couturier-Tamburelli, I.; Toumi, A.; Piétri, N.; Chiavassa, T.

2018-01-01

In order to simulate different altitudes in the atmosphere of Titan, we investigated using infrared spectrometry and mass spectrometry the photochemistry of ethyl cyanide (CH3CH2CN) ices at different temperatures. Heating experiments of the solid phase until complete desorption showed up three phase transitions with a first one appearing to be approximately at the temperature of Titan's surface (94 K), measured by the Huygens probe. Ethyl cyanide, whose presence has been suggested in solid phase in Titan, can be considered as another nitrile for photochemical models of the Titan atmosphere after our first study (Toumi et al., 2016) concerning vinyl cyanide (CH2CHCN). The desorption energy of ethyl cyanide has been calculated to be 36.75 ( ± 0.55) kJ mol-1 using IRTF and mass spectroscopical techniques. High energetic photolysis (λ > 120 nm) have been performed and we identified ethyl isocyanide, vinyl cyanide, cyanoacetylene, ethylene, acetylene, cyanhydric acid and a methylketenimine form as photoproducts from ethyl cyanide. The branching ratios of the primary products were determined at characteristic temperatures of Titan thanks to the value of the νCN stretching band strength of ethyl cyanide that has been calculated to be 4.12 × 10-18 cm molecule-1. We also report here for the first time the values of the photodissociation cross sections of C2H5CN for different temperatures.

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

DEFF Research Database (Denmark)

Poreddy, Raju; Shunmugavel, Saravanamurugan; Riisager, Anders

2015-01-01

Zeolites were evaluated as solid acid catalysts for the liquid-phase benzylation of anisole with benzyl alcohol, benzyl bromide, and benzyl chloride at 80 °C. Among the examined zeolites, H-mordenite-10 (H-MOR-10) demonstrated particular high activity (>99 %) and excellent selectivity (>96...

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

DEFF Research Database (Denmark)

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

2011-01-01

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

Mechanism of Formation of Li ₇ P ₃ S ₁₁ Solid Electrolytes through Liquid Phase Synthesis

Energy Technology Data Exchange (ETDEWEB)

Wang, Yuxing [Energy; Lu, Dongping [Energy; Bowden, Mark [Environmental; El Khoury, Patrick Z. [Environmental; Han, Kee Sung [Environmental; Deng, Zhiqun Daniel [Energy; Xiao, Jie [Energy; Zhang, Ji-Guang [Energy; Liu, Jun [Energy

2018-01-22

Crystalline Li7P3S11 is a promising solid electrolyte for all solid state lithium/lithium ion batteries. A controllable liquid phase synthesis of Li7P3S11 is more desirable compared to conventional mechanochemical synthesis, but recent attempts suffer from reduced ionic conductivities. Here we elucidate the formation mechanism of crystalline Li7P3S11 synthesized in the liquid phase (acetonitrile, or ACN). We conclude that the crystalline Li7P3S11 forms through a two-step reaction: 1) formation of solid Li3PS4∙ACN and amorphous Li2S∙P2S5 phases in the liquid phase; 2) solid-state conversion of the two phases. The implication of this two-step reaction mechanism to the morphology control and the transport properties of liquid phase synthesized Li7P3S11 is identified and discussed.

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

International Nuclear Information System (INIS)

Nakao, Ryuji; Halldin, Christer

2013-01-01

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

Application of solid-phase microextraction in analytical toxicology.

Science.gov (United States)

Pragst, Fritz

2007-08-01

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

Phase-field-crystal model for magnetocrystalline interactions in isotropic ferromagnetic solids

Science.gov (United States)

Faghihi, Niloufar; Provatas, Nikolas; Elder, K. R.; Grant, Martin; Karttunen, Mikko

2013-09-01

An isotropic magnetoelastic phase-field-crystal model to study the relation between morphological structure and magnetic properties of pure ferromagnetic solids is introduced. Analytic calculations in two dimensions were used to determine the phase diagram and obtain the relationship between elastic strains and magnetization. Time-dependent numerical simulations in two dimensions were used to demonstrate the effect of grain boundaries on the formation of magnetic domains. It was shown that the grain boundaries act as nucleating sites for domains of reverse magnetization. Finally, we derive a relation for coercivity versus grain misorientation in the isotropic limit.

Phase transitions in solid Kr-CH4 solutions and rotational excitations in phase II

International Nuclear Information System (INIS)

Bagatskii, M.I.; Mashchenko, D.A.; Dudkin, V.V.

2007-01-01

The heat capacity C p of solid Kr-n CH 4 solutions with the CH 4 concentrations n=0.82, 0.86, 0.90 as well as solutions with n=0.90, 0.95 doped with 0.002 O 2 impurity has been investigated under equilibrium vapor pressure over the internal 1-24 K. The (T,n)-phase diagram was refined and the region of two-phase states was determined for Kr-n CH 4 solid solutions. The contribution of the rotational subsystem, C r ot, to the heat capacity of the solutions has been separated. Analysis of C r ot(T) at T 1 and E 2 between the tunnel levels of the A-, T- and A-, E--nuclear-spin species of CH 4 molecules in the orientationally ordered subsystem, and to determine the effective energy gaps E 1 between lowest levels of the A- and T- species. The relations τ(n) and E 1 (n) stem from changes of the effective potential field caused as the replacement of CH 4 molecules by Kr atoms at sites of the ordered sublattices. The effective gaps E L between a group of tunnel levels of the ground-state liberation state and the nearest group of excited levels of the liberation state of the ordered CH 4 molecules in the solutions with n=0.90 (E L =52 K) and 0.95 (E L =55 K) has been estimated

Microwave-assisted solid phase conversion study of Meldrum's acid to ethylenetetracarboxylic dianhydride (C 6O 6)

Science.gov (United States)

Taherpour, Avat (Arman)

2010-01-01

Utilization of microwave irradiation provides an effective method for fast synthesizing of some important compounds. Microwave-assisted solid phase is an especial class in chemical synthesis. By the use of MW-irradiation on chemicals, sometimes interesting results can be seen. The synthesis of the interesting molecule ethylenetetracarboxylic dianhydride (C 6O 6) was attempted with a few different methods. In this study, the microwave-assisted solid phase conversion of Meldrum's acid to ethylenetetracarboxylic dianhydride was reported. This conversion was characterized by FT-IR, GC/MS and NMR spectroscopy results.

Room-temperature solid phase ionic liquid (RTSPIL) coated Ω-transaminases: Development and application in organic solvents

DEFF Research Database (Denmark)

Grabner, B.; Nazario, M. A.; Gundersen, M. T.

2018-01-01

ω-Transaminases ATA-40, ATA-47 and ATA-82P were coated with room-temperature solid phase ionic liquids (RTSPILs) by means of three methods, melt coating, precipitation coating, and co‐lyophilization, and showed increased stability in all of the five tested organic solvents. Co‐lyophilization and ......ω-Transaminases ATA-40, ATA-47 and ATA-82P were coated with room-temperature solid phase ionic liquids (RTSPILs) by means of three methods, melt coating, precipitation coating, and co‐lyophilization, and showed increased stability in all of the five tested organic solvents. Co...

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

Science.gov (United States)

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

2009-01-01

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

Solid-phase synthesis of yttrium ferrites with structures of perovskite and garnet

Energy Technology Data Exchange (ETDEWEB)

Tkachenko, E V; Shapovalov, A G; Aksel' rod, N L; Pazdnikov, I P [Ural' skij Gosudarstvennyj Univ., Sverdlovsk (USSR)

1980-09-01

The solid phase synthesis of yttrium ferrites having a perovskite- and garnet-like structure has been investigated in the temperature range from 800 to 1500 deg C and temper times of up to 80 hours by reaction zone simulation and magnetic phase analysis. It is shown that for conversion degrees d<0.15 the reactions are diffusion-controlled. The rate constants and effective diffusion in the formation of YFeO/sub 3/ and Y/sub 3/Fe/sub 5/O/sub 12/ have been determined.

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

Science.gov (United States)

Blackburn, Christopher

2012-03-12

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

A Facile, Choline Chloride/Urea Catalyzed Solid Phase Synthesis of Coumarins via Knoevenagel Condensation

Directory of Open Access Journals (Sweden)

Hosanagara N. Harishkumar

2011-01-01

Full Text Available The influence of choline chloride/urea ionic liquid in solid phase on the Knoevenagel condensation is demonstrated. The active methylene compounds such as meldrum’s acid, diethylmalonate, ethyl cyanoacetate, dimethylmalonate, were efficiently condensed with various salicylaldehydes in presence of choline chloride/urea ionic liquid without using any solvents or additional catalyst. The reaction is remarkably facile because of the air and water stability of the catalyst, and needs no special precautions. The reactions were completed within 1hr with excellent yields (95%. The products formed were sufficiently pure, and can be easily recovered. The use of ionic liquid choline chloride/urea in solid phase offered several significant advantages such as low cost, greater selectivity and easy isolation of products.

A Two-Phase Solid/Fluid Model for Dense Granular Flows Including Dilatancy Effects

Science.gov (United States)

Mangeney, Anne; Bouchut, Francois; Fernandez-Nieto, Enrique; Narbona-Reina, Gladys

2015-04-01

We propose a thin layer depth-averaged two-phase model to describe solid-fluid mixtures such as debris flows. It describes the velocity of the two phases, the compression/dilatation of the granular media and its interaction with the pore fluid pressure, that itself modifies the friction within the granular phase (Iverson et al., 2010). The model is derived from a 3D two-phase model proposed by Jackson (2000) based on the 4 equations of mass and momentum conservation within the two phases. This system has 5 unknowns: the solid and fluid velocities, the solid and fluid pressures and the solid volume fraction. As a result, an additional equation inside the mixture is necessary to close the system. Surprisingly, this issue is inadequately accounted for in the models that have been developed on the basis of Jackson's work (Bouchut et al., 2014). In particular, Pitman and Le replaced this closure simply by imposing an extra boundary condition at the surface of the flow. When making a shallow expansion, this condition can be considered as a closure condition. However, the corresponding model cannot account for a dissipative energy balance. We propose here an approach to correctly deal with the thermodynamics of Jackson's equations. We close the mixture equations by a weak compressibility relation involving a critical density, or equivalently a critical pressure. Moreover, we relax one boundary condition, making it possible for the fluid to escape the granular media when compression of the granular mass occurs. Furthermore, we introduce second order terms in the equations making it possible to describe the evolution of the pore fluid pressure in response to the compression/dilatation of the granular mass without prescribing an extra ad-hoc equation for the pore pressure. We prove that the energy balance associated with this Jackson closure is dissipative, as well as its thin layer associated model. We present several numerical tests for the 1D case that are compared to the

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

Science.gov (United States)

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

2015-11-17

This Phase I study evaluated continuous- and intermittent-dosing (every other week) of afatinib plus nintedanib in patients with advanced solid tumours. 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 MTD was further evaluated in an expansion phase (n=25). The most frequent dose-limiting toxicities were diarrhoea (11%) and transaminase elevations (7%). Maximum tolerated doses were afatinib 30 mg continuously plus nintedanib 150 mg, and afatinib 40 mg intermittently plus nintedanib 150 mg. Treatment-related adverse events (mostly Grade⩽3) included diarrhoea (98%), asthenia (64%), nausea (62%) and vomiting (60%). In the dose-escalation phase, two patients had partial responses (PRs) and 27 (60%) had stable disease (SD). In the expansion phase, one complete response and three PRs were observed (all non-small cell lung cancer), with SD in 13 (52%) patients. No pharmacokinetic interactions were observed. MTDs of continuous or intermittent afatinib plus nintedanib demonstrated a manageable safety profile with proactive management of diarrhoea. Antitumour activity was observed in patients with solid tumours.

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

Science.gov (United States)

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

2013-12-04

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

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

Science.gov (United States)

Tovbin, Yu. K.

2017-08-01

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

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

Czech Academy of Sciences Publication Activity Database

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

2010-01-01

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

Solid-phase immunoradiometric assay for C-reactive protein using magnetisable cellulose particles

International Nuclear Information System (INIS)

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

1982-01-01

An immunoradiometric assay (IRMA) for C-reactive protein (CRP) was developed using magnetisable cellulose particles as the solid-phase support for anti-CRP antibodies. 125 I-labelled immunopurified anti-CRP antibody was used to quantitate the amount of CRP taken up by the solid phase. Unbound label was easily and rapidly removed by decantation after sedimenting the particles on a magnet. The assay could detect 1 μg CRP/l and had a range of up to 10 mg/l with the portion of the standard curve between 10 μg/l and 2-3 mg/l being linear. Fifty samples per hour could be processed manually from serum to CRP result with an intra-assay CV of 5.2% and an inter-assay CV of 10.0%, based on 5 replicates of 5 samples with CRP levels between 2 mg/l and 180 mg/l run in 5 separate assays. Fifty clinical samples were assayed in parallel with a standard electroimmunoassay and yielded a linear correlation coefficient (r) of 0.975 and a slope of 0.98. With its single, brief incubation step including all reagents and its simple phase separation procedure the present method may be the assay of choice when precise measurement of CRP concentrations is required rapidly. (Auth.)

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

Science.gov (United States)

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

2016-11-01

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

A multilevel simulation approach to derive the slip boundary condition of the solid phase in two-fluid models

Science.gov (United States)

Feng, Zhi-Gang; Michaelides, Efstathios; Mao, Shaolin

2011-11-01

The simulation of particulate flows for industrial applications often requires the use of a two-fluid model (TFM), where the solid particles are considered as a separate continuous phase. One of the underlining uncertainties in the use of aTFM in multiphase computations comes from the boundary condition of the solid phase. The no-slip condition at a solid boundary is not a valid assumption for the solid phase. Instead, several researchers advocate a slip condition as a more appropriate boundary condition. However, the question on the selection of an exact slip length or a slip velocity coefficient is still unanswered. In the present work we propose a multilevel simulation approach to compute the slip length that is applicable to a TFM. We investigate the motion of a number of particles near a vertical solid wall, while the particles are in fluidization using a direct numerical simulation (DNS); the positions and velocities of the particles are being tracked and analyzed at each time step. It is found that the time- and vertical-space averaged values of the particle velocities converge, yielding velocity profiles that can be used to deduce the particle slip length close to a solid wall. This work was supported by a grant from the DOE-NETL (DE-NT0008064) and by a grant from NSF (HRD-0932339).

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

Science.gov (United States)

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

2006-01-06

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-04-07

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

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

International Nuclear Information System (INIS)

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

2015-01-01

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

Diffusionless phase transition with two order parameters in spin-crossover solids

Energy Technology Data Exchange (ETDEWEB)

Gudyma, Iurii, E-mail: yugudyma@gmail.com; Ivashko, Victor [Department of General Physics, Chernivtsi National University, 58012 Chernivtsi (Ukraine); Linares, Jorge [Groupe d' Etude de la Matière Condensée (GEMAC), UMR 8635, CNRS, Université de Versailles Saint Quentin, 45 avenue des Etats-Unis, 78035 Versailles (France)

2014-11-07

The quantitative analysis of the interface boundary motion between high-spin and low-spin phases is presented. The nonlinear effect of the switching front rate on the temperature is shown. A compressible model of spin-crossover solid is studied in the framework of the Ising-like model with two-order parameters under statistical approach, where the effect of elastic strain on interaction integral is considered. These considerations led to examination of the relation between the order parameters during temperature changes. Starting from the phenomenological Hamiltonian, entropy has been derived using the mean field approach. Finally, the phase diagram, which characterizes the system, is numerically analyzed.

Solid-phase immunoradiometric assay for serum amyloid A protein using magnetisable cellulose particles

International Nuclear Information System (INIS)

De Beer, F.C.; Dyck, R.F.; Pepys, M.B.

1982-01-01

An immunoradiometric assay for human serum amyloid A protein (SAA) was developed using magnetisable cellulose particles as the solid phase. Rabbit antiserum to SAA was raised by immunization with SAA isolated from acute-phase serum by gel filtration in formic acid. The antiserum was rendered monospecific for SAA by solid-phase immunoabsorption with normal human serum, which contains only traces of SAA, and some was coupled covalently to the cellulose particles. Immunopurified anti-SAA antibodies were isolated from the monospecific anti-SAA serum by binding to, and elution from insolubilized acute-phase serum and were radiolabelled with 125 I. The assay was calibrated with an acute phase serum which contained 6000 times more SAA than normal sera with the lowest detectable level of SAA, and an arbitrary value of 6000 U/l was assigned to this standard. Sera were tested in the native, undenatured state and there was no increase in SAA immunoreactivity following alkali treatment or heating. The assay range was from 1-2000 U/l so that all SAA levels above 6 U/l could be measured on a single (1:6) dilution of serum. The intra- and interassay coefficients of variation were 11.7 and 15.0% respectively. Among 100 healthy normal subjects (50 male, 50 female) the median SAA level was 9 U/l, range <1-100, with 93% below 20 U/l and only 2% below the lower limit of sensitivity of the assay (1 U/l). (Auth.)

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

NARCIS (Netherlands)

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

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

Solid-phase cloning for high-throughput assembly of single and multiple DNA parts

DEFF Research Database (Denmark)

Lundqvist, Magnus; Edfors, Fredrik; Sivertsson, Åsa

2015-01-01

We describe solid-phase cloning (SPC) for high-throughput assembly of expression plasmids. Our method allows PCR products to be put directly into a liquid handler for capture and purification using paramagnetic streptavidin beads and conversion into constructs by subsequent cloning reactions. We ...

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

Science.gov (United States)

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

2015-01-28

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

Optimized Solid Phase-Assisted Synthesis of Dendrons Applicable as Scaffolds for Radiolabeled Bioactive Multivalent Compounds Intended for Molecular Imaging

Directory of Open Access Journals (Sweden)

Gabriel Fischer

2014-05-01

Full Text Available Dendritic structures, being highly homogeneous and symmetric, represent ideal scaffolds for the multimerization of bioactive molecules and thus enable the synthesis of compounds of high valency which are e.g., applicable in radiolabeled form as multivalent radiotracers for in vivo imaging. As the commonly applied solution phase synthesis of dendritic scaffolds is cumbersome and time-consuming, a synthesis strategy was developed that allows for the efficient assembly of acid amide bond-based highly modular dendrons on solid support via standard Fmoc solid phase peptide synthesis protocols. The obtained dendritic structures comprised up to 16 maleimide functionalities and were derivatized on solid support with the chelating agent DOTA. The functionalized dendrons furthermore could be efficiently reacted with structurally variable model thiol-bearing bioactive molecules via click chemistry and finally radiolabeled with 68Ga. Thus, this solid phase-assisted dendron synthesis approach enables the fast and straightforward assembly of bioactive multivalent constructs for example applicable as radiotracers for in vivo imaging with Positron Emission Tomography (PET.

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

Science.gov (United States)

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

2003-01-15

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

Separation of lanthanum (3) and samarium (3) extraction with tributylphosphate in the solvent presence of solid phase

International Nuclear Information System (INIS)

Korotkevich, I.B.; Kolesnikov, A.A.; Bomshtejn, V.E.

1990-01-01

Lanthanum (3) and samarium (3) extraction from nitric acid solutions by tributylphosphate in the presence of solid phase has been investigated. An increase in samarium α-nitrate distribution factor in the presence of solid phase with a decrease in its concentration in the initial solution and with lanthanum nitrate concentration increase is detected. The greatest effect of separation is observed in samarium nitrate microregion. The method of quantitative extraction of samarium from lanthanum nitrate solutions with samarium-lanthanum separation factor exceeding 50 has been suggested

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

OpenAIRE

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

2006-01-01

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...

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

OpenAIRE

Rincón, Bárbara; Raposo, Francisco; Borja, Rafael

2006-01-01

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...

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

International Nuclear Information System (INIS)

Fortier, Andre; Chen, Che Pen

1976-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

1977-09-01

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

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

DEFF Research Database (Denmark)

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

2003-01-01

A solid-phase conjugation method utilizing carrier protein bound to an ion exchange matrix was developed. Ovalbumin was adsorbed to an anion exchange matrix using a batch procedure, and the immobilized protein was then derivatized with iodoacetic acid N-hydroxysuccinimid ester. The activated......, and immunization experiments with the eluted conjugates showed that the more substituted conjugates gave rise to the highest titers of glutathione antibodies. Direct immunization with the conjugates adsorbed to the ion exchange matrix was possible and gave rise to high titers of glutathione antibodies. Conjugates...... of ovalbumin and various peptides were prepared in a similar manner and used for production of peptide antisera by direct immunization with the conjugates bound to the ion exchanger. Advantages of the method are its solid-phase nature, allowing fast and efficient reactions and intermediate washings...

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

International Nuclear Information System (INIS)

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

1988-10-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

1984-05-01

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

Municipal solid waste development phases: Evidence from EU27.

Science.gov (United States)

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

2015-12-01

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

The EPOS Implementation Phase: building thematic and integrated services for solid Earth sciences

Science.gov (United States)

Cocco, Massimo; Epos Consortium, the

2015-04-01

The European Plate Observing System (EPOS) has a scientific vision and approach aimed at creating a pan-European infrastructure for Earth sciences to support a safe and sustainable society. To follow this vision, the EPOS mission is integrating a suite of diverse and advanced Research Infrastructures (RIs) in Europe relying on new e-science opportunities to monitor and understand the dynamic and complex Earth system. To this goal, the EPOS Preparatory Phase has designed a long-term plan to facilitate integrated use of data and products as well as access to facilities from mainly distributed existing and new research infrastructures for solid Earth Science. EPOS will enable innovative multidisciplinary research for a better understanding of the Earth's physical processes that control earthquakes, volcanic eruptions, ground instability and tsunami as well as the processes driving tectonics and Earth surface dynamics. Through integration of data, models and facilities EPOS will allow the Earth Science community to make a step change in developing new concepts and tools for key answers to scientific and socio-economic questions concerning geo-hazards and geo-resources as well as Earth sciences applications to the environment and to human welfare. Since its conception EPOS has been built as "a single, Pan-European, sustainable and distributed infrastructure". EPOS is, indeed, the sole infrastructure for solid Earth Science in ESFRI and its pan-European dimension is demonstrated by the participation of 23 countries in its preparatory phase. EPOS is presently moving into its implementation phase further extending its pan-European dimension. The EPOS Implementation Phase project (EPOS IP) builds on the achievements of the successful EPOS preparatory phase project. The EPOS IP objectives are synergetic and coherent with the establishment of the new legal subject (the EPOS-ERIC in Italy). EPOS coordinates the existing and new solid Earth RIs within Europe and builds the

Separation of lanthanum (3) and neodymium (3) by tributyl phosphate extraction in the presence of solid phase

International Nuclear Information System (INIS)

Korotkevich, I.B.; Kolesnikov, A.A.; Bomshtejn, V.E.; Shikhaleeva, N.N.

1987-01-01

Lanthanum (3) and neodymium (3) extraction from nitric acid solutions by tributyl phosphate in the presence of solid phase of the element nitrates is investigated. An increase in distribution of neodymium nitrate in the presence of solid phase with the decrease in its concentration in the initial solution and with the increase in lanthanum nitrate concentration is detected. The highest effect of extractive-crystallizational separation is observed in the range of neodymium nitrate microconcentrations. A method of neodymium quantitative extraction from lanthanum nitrate solutions with neodymium - lanthanum separation coefficient exceeding 25 is suggested

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

Science.gov (United States)

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

2002-01-01

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

Solid-state phase transitions in CuCl under hydrostatic pressures to 12.8 GPa

International Nuclear Information System (INIS)

Liebenberg, D.H.; Mills, R.L.; Huang, C.Y.; Olsen, C.; Schmidt, L.C.

1981-01-01

The phase transitions in solid CuCl under hydrostatic conditions at pressures to 12.8 GPa are examined. The transition at 4.4 GPa from zinc-blende to tetragonal is observed. Our negative observations for the upper transition at 8.2 GPa and for the formation of an opaque phase due to the disproportionation reaction support the contention that pressure gradients are important in affecting the behavior of pure CuCl

Automated Solid-Phase Subcloning Based on Beads Brought into Proximity by Magnetic Force

DEFF Research Database (Denmark)

Hudson, Elton P.; Nikoshkov, Andrej; Uhlén, Mathias

2012-01-01

In the fields of proteomics, metabolic engineering and synthetic biology there is a need for high-throughput and reliable cloning methods to facilitate construction of expression vectors and genetic pathways. Here, we describe a new approach for solid-phase cloning in which both the vector and th...

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

International Nuclear Information System (INIS)

Scheidt, C.

1982-01-01

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

Fifty years of solid-phase extraction in water analysis--historical development and overview.

Science.gov (United States)

Liska, I

2000-07-14

The use of an appropriate sample handling technique is a must in an analysis of organic micropollutants in water. The efforts to use a solid phase for the recovery of analytes from a water matrix prior to their detection have a long history. Since the first experimental trials using activated carbon filters that were performed 50 years ago, solid-phase extraction (SPE) has become an established sample preparation technique. The initial experimental applications of SPE resulted in widespread use of this technique in current water analysis and also to adoption of SPE into standardized analytical methods. During the decades of its evolution, chromatographers became aware of the advantages of SPE and, despite many innovations that appeared in the last decade, new SPE developments are still expected in the future. A brief overview of 50 years of the history of the use of SPE in organic trace analysis of water is given in presented paper.

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

Energy Technology Data Exchange (ETDEWEB)

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

2017-07-15

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

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

International Nuclear Information System (INIS)

Berlin, Katja; Trampert, Achim

2017-01-01

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

Mycoestrogen determination in cow milk: Magnetic solid-phase extraction followed by liquid chromatography and tandem mass spectrometry analysis.

Science.gov (United States)

Capriotti, Anna Laura; Cavaliere, Chiara; Foglia, Patrizia; La Barbera, Giorgia; Samperi, Roberto; Ventura, Salvatore; Laganà, Aldo

2016-12-01

Recently, magnetic solid-phase extraction has gained interest because it presents various operational advantages over classical solid-phase extraction. Furthermore, magnetic nanoparticles are easy to prepare, and various materials can be used in their synthesis. In the literature, there are only few studies on the determination of mycoestrogens in milk, although their carryover in milk has occurred. In this work, we wanted to develop the first (to the best of our knowledge) magnetic solid-phase extraction protocol for six mycoestrogens from milk, followed by liquid chromatography and tandem mass spectrometry analysis. Magnetic graphitized carbon black was chosen as the adsorbent, as this carbonaceous material, which is very different from the most diffuse graphene and carbon nanotubes, had already shown selectivity towards estrogenic compounds in milk. The graphitized carbon black was decorated with Fe 3 O 4 , which was confirmed by the characterization analyses. A milk deproteinization step was avoided, using only a suitable dilution in phosphate buffer as sample pretreatment. The overall process efficiency ranged between 52 and 102%, whereas the matrix effect considered as signal suppression was below 33% for all the analytes even at the lowest spiking level. The obtained method limits of quantification were below those of other published methods that employ classical solid-phase extraction protocols. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

NMR relaxation and phase transitions in solid methane and deuterated derivatives

International Nuclear Information System (INIS)

Putten, D. van der.

1984-01-01

This thesis describes an investigation of properties of solid methane at high pressure (till 10 kbar) with temperatures ranging from 2 until 100 K. The high inverse moment of inertia of the molecule combined with low ordering potentials gives rise to properties for which quantum effects play an important role: e.g. the transition temperature to a partially ordered phase shows an isotope effect of 35% when CH 4 protons are substituted by deuterons. Interpretation of NMR properties of solid methane also show quantum effects. First, a helium cryostat is developed and described and NMR results for CH 4 , CH 2 D 2 and CD 4 are given. The influence of discrete tunnel states on the spin-lattice relaxation is studied theoretically. Application of group theory has simplified the calculations considerably. (G.J.P.)

Multiple headspace-solid-phase microextraction: An application to quantification of mushroom volatiles

Energy Technology Data Exchange (ETDEWEB)

Costa, Rosaria; Tedone, Laura; De Grazia, Selenia [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Dugo, Paola [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Centro Integrato di Ricerca (C.I.R.), Università Campus-Biomedico, Via Álvaro del Portillo, 21, 00128 Roma (Italy); Mondello, Luigi, E-mail: lmondello@unime.it [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Centro Integrato di Ricerca (C.I.R.), Università Campus-Biomedico, Via Álvaro del Portillo, 21, 00128 Roma (Italy)

2013-04-03

Highlights: ► Multiple headspace extraction-solid phase microextraction (MHS-SPME) has been applied to the analysis of Agaricus bisporus. ► Mushroom flavor is characterized by the presence of compounds with a 8-carbon atoms skeleton. ► Formation of 8-carbon compounds involves a unique fungal biochemical pathway. ► The MHS-SPME allowed to determine quantitatively 5 target analytes of A. bisporus for the first time. -- Abstract: Multiple headspace-solid phase microextraction (MHS-SPME) followed by gas chromatography/mass spectrometry (GC–MS) and flame ionization detection (GC–FID) was applied to the identification and quantification of volatiles released by the mushroom Agaricus bisporus, also known as champignon. MHS-SPME allows to perform quantitative analysis of volatiles from solid matrices, free of matrix interferences. Samples analyzed were fresh mushrooms (chopped and homogenized) and mushroom-containing food dressings. 1-Octen-3-ol, 3-octanol, 3-octanone, 1-octen-3-one and benzaldehyde were common constituents of the samples analyzed. Method performance has been tested through the evaluation of limit of detection (LoD, range 0.033–0.078 ng), limit of quantification (LoQ, range 0.111–0.259 ng) and analyte recovery (92.3–108.5%). The results obtained showed quantitative differences among the samples, which can be attributed to critical factors, such as the degree of cell damage upon sample preparation, that are here discussed. Considerations on the mushrooms biochemistry and on the basic principles of MHS analysis are also presented.

Multiple headspace-solid-phase microextraction: An application to quantification of mushroom volatiles

International Nuclear Information System (INIS)

Costa, Rosaria; Tedone, Laura; De Grazia, Selenia; Dugo, Paola; Mondello, Luigi

2013-01-01

Highlights: ► Multiple headspace extraction-solid phase microextraction (MHS-SPME) has been applied to the analysis of Agaricus bisporus. ► Mushroom flavor is characterized by the presence of compounds with a 8-carbon atoms skeleton. ► Formation of 8-carbon compounds involves a unique fungal biochemical pathway. ► The MHS-SPME allowed to determine quantitatively 5 target analytes of A. bisporus for the first time. -- Abstract: Multiple headspace-solid phase microextraction (MHS-SPME) followed by gas chromatography/mass spectrometry (GC–MS) and flame ionization detection (GC–FID) was applied to the identification and quantification of volatiles released by the mushroom Agaricus bisporus, also known as champignon. MHS-SPME allows to perform quantitative analysis of volatiles from solid matrices, free of matrix interferences. Samples analyzed were fresh mushrooms (chopped and homogenized) and mushroom-containing food dressings. 1-Octen-3-ol, 3-octanol, 3-octanone, 1-octen-3-one and benzaldehyde were common constituents of the samples analyzed. Method performance has been tested through the evaluation of limit of detection (LoD, range 0.033–0.078 ng), limit of quantification (LoQ, range 0.111–0.259 ng) and analyte recovery (92.3–108.5%). The results obtained showed quantitative differences among the samples, which can be attributed to critical factors, such as the degree of cell damage upon sample preparation, that are here discussed. Considerations on the mushrooms biochemistry and on the basic principles of MHS analysis are also presented

How fast are the ultra-fast nano-scale solid-liquid phase transitions induced by energetic particles in solids?

International Nuclear Information System (INIS)

Lopasso, E.M.; Caro, A.; Caro, M.

2003-01-01

We study the thermodynamic forces acting on the evolution of the nanoscale regions excited by collisions of energetic particles into solid targets. We analyze the role of diffusion, thermo-migration, and the liquidus-solidus two-phase field crossing, as the system cools down from the collision-induced melt under different conditions of energy deposition. To determine the relevance of these thermodynamic forces, solute redistribution is evaluated using molecular dynamics simulations of equilibrium Au-Ni solid solutions. At low collision energies, our results show that the quenching of spherical cascades is too fast to allow for solute redistribution according to equilibrium solidification as determined from the equilibrium phase diagram (zone refining effect), and only thermo-migration is observed. At higher energies instead, in the cylindrical symmetry of ion tracks, quenching rate is in a range that shows the combined effects of thermo-migration and solute redistribution that, depending on the material, can reinforce or cancel each other. These results are relevant for the interpretation of the early stage of radiation damage in alloys, and show that the combination of ultra-fast but nano-scale characteristics of these processes can still be described in terms of linear response of the perturbed system

Homogeneous synthesis of cellulose acrylate-g-poly (n-alkyl acrylate) solid-solid phase change materials via free radical polymerization.

Science.gov (United States)

Qian, Yong-Qiang; Han, Na; Bo, Yi-Wen; Tan, Lin-Li; Zhang, Long-Fei; Zhang, Xing-Xiang

2018-08-01

A novel solid-solid phase change materials, namely, cellulose acrylate-g-poly (n-alkyl acrylate) (CA-g-PAn) (n = 14, 16 and 18) were successfully synthesized by free radical polymerization in N, N-dimethylacetamide (DMAc). The successful grafting was confirmed by fourier transform infrared spectra (FT-IR) and nuclear magnetic resonance (NMR). The properties of the CA-g-PAn copolymers were investigated by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA). The phase change temperatures and the melting enthalpies of CA-g-PAn copolymers are in the range of 10.1-53.2 °C and 15-95 J/g, respectively. It can be adjusted by the contents of poly (n-alkyl acrylate) and the length of alkyl side-chain. The thermal resistant temperatures of CA-g-PA14, 16 and 18 copolymers are 308 °C, 292 °C and 273 °C, respectively. It show that all of grafting materials exhibit good thermal stability and shape stability. Therefore, it is expected to be applied in the cellulose-based thermos-regulating field. Copyright © 2018 Elsevier Ltd. All rights reserved.

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

International Nuclear Information System (INIS)

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

1985-01-01

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

Conditioning of radioactive ash residue in a wave of solid-phase exothermal reactions

International Nuclear Information System (INIS)

Karlina, O.K.; Varlakova, G.A.; Ozhovan, M.I.; Tivanskij, V.M.; Dmitriev, S.A.

2001-01-01

The abilities for utilization of exothermic reaction heat in solid phase for conditioning the ash residue produced as a result of solid radioactive waste burning are analyzed. It is shown that the process of ash residue making monolithic with obtaining the glass-like finish product containing 50-60 mass % of ash residue which meets the requirements for solidified radioactive wastes may be realized without energy supplying from external heat sources. The conditioning is realized in a special crucible furnace-container designed not only for the process conducting but also for subsequent storage or disposal of the finish product [ru

Safety test No. S-6, launch pad abort sequential test Phase II: solid propellant fire

International Nuclear Information System (INIS)

Snow, E.C.

1975-08-01

In preparation for the Lincoln Laboratory's LES 8/9 space mission, a series of tests was performed to evaluate the nuclear safety capability of the Multi-Hundred Watt (MHW) Radioisotope Thermoelectric Generator (RTG) to be used to supply power for the satellite. One such safety test is Test No. S-6, Launch Pad Abort Sequential Test. The objective of this test was to subject the RTG and its components to the sequential environments characteristic of a catastrophic launch pad accident to evaluate their capability to contain the 238 PuO 2 fuel. This sequence of environments was to have consisted of the blast overpressure and fragments, followed by the fireball, low velocity impact on the launch pad, and solid propellant fire. The blast overpressure and fragments were subsequently eliminated from this sequence. The procedures and results of Phase II of Test S-6, Solid Propellant Fire are presented. In this phase of the test, a simulant Fuel Sphere Assembly (FSA) and a mockup of a damaged Heat Source Assembly (HSA) were subjected to single proximity solid propellant fires of approximately 10-min duration. Steel was introduced into both tests to simulate the effects of launch pad debris and the solid rocket motor (SRM) casing that might be present in the fire zone. (TFD)

Specific features of concentrated phase under decomposition of weak solid /sup 3/He-/sup 4/He solution

Energy Technology Data Exchange (ETDEWEB)

Mikheev, V A; Majdamov, V A; Kal' noj, S E; Omelaenko, N I

1988-06-01

The decomposition of solid /sup 3/He-/sup 4/He solutuions is studied on the samples 0.54% /sup 3/He(V=20.55 cm/sup 3//mole) and 0.60% /sup 4/He (V=24.04-24.93 cm/sup 3//mole) using pulse NMR method. At T=100 mK the decomposition of a weak solution proceeds more than for 30 h, the decomposition rate and temperature being dependent on the sample prehistory. In the concentrated phase of the decomposed weak solution the spin diffraction of /sup 3/He is of the quasi-one-dimensional character with the diffusion coefficient D /similar to/ 10/sup -5/ cm/sup 2//sec typical of liquid /sup 3/He and exceeding that bulk solid /sup 3/He by two orders of magnitude. The longitudinal relaxation time in the quasi-one-dimensional phase (/similar to/ 1 sec) is characteristic of the solid state and coinsides with data for bulk /sup 3/He. The temperature behaviour of magnetization in the quasi-one-dimensional phase is well described by the Curie law.

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

Science.gov (United States)

Chen, Xin; Shu, Jiapei; Chen, Qing

2017-04-24

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

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

Science.gov (United States)

Yang, Yanqin; Chu, Guohai; Zhou, Guojun; Jiang, Jian; Yuan, Kailong; Pan, Yuanjiang; Song, Zhiyu; Li, Zuguang; Xia, Qian; Lu, Xinbo; Xiao, Weiqiang

2016-03-01

An ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction was first employed to determine the volatile components in tobacco samples. The method combined the advantages of ultrasound, microwave, and headspace solid-phase microextraction. The extraction, separation, and enrichment were performed in a single step, which could greatly simplify the operation and reduce the whole pretreatment time. In the developed method, several experimental parameters, such as fiber type, ultrasound power, and irradiation time, were optimized to improve sampling efficiency. Under the optimal conditions, there were 37, 36, 34, and 36 components identified in tobacco from Guizhou, Hunan, Yunnan, and Zimbabwe, respectively, including esters, heterocycles, alkanes, ketones, terpenoids, acids, phenols, and alcohols. The compound types were roughly the same while the contents were varied from different origins due to the disparity of their growing conditions, such as soil, water, and climate. In addition, the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method was compared with the microwave-assisted extraction coupled to headspace solid-phase microextraction and headspace solid-phase microextraction methods. More types of volatile components were obtained by using the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method, moreover, the contents were high. The results indicated that the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction technique was a simple, time-saving and highly efficient approach, which was especially suitable for analysis of the volatile components in tobacco. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Probing the liquid and solid phases in closely spaced two-dimensional systems

Energy Technology Data Exchange (ETDEWEB)

Zhang, Ding

2014-03-06

Gas, liquid and solid phases are the most common states of matter in our daily encountered 3-dimensional space. The school example is the H{sub 2}O molecule with its phases vapor, water and ice. Interestingly, electrons - with their point-like nature and negative charges - can also organize themselves under certain conditions to bear properties of these three common phases. At relatively high temperature, where Boltzmann statistics prevails, the ensemble of electrons without interactions can be treated as a gas of free particles. Cooling down the system, this electron gas condenses into a Fermi liquid. Finally, as a result of the repulsive Coulomb forces, electrons try to avoid each other by maximizing their distances. When the Coulomb interaction becomes sufficiently strong, a regular lattice emerges - an electron solid. The story however does not end here. Nature has much more in store for us. Electronic systems in fact exhibit a large variety of phases induced by spatial confinement, an external magnetic field, Coulomb interactions, or interactions involving degrees of freedom other than charge such as spin and valley. Here in this thesis, we restrict ourselves to the study of electrons in a 2-dimenisonal (2D) plane. Already in such a 2D electron system (2DES), several distinct states of matter appear: integer and fractional quantum Hall liquids, the 2D Wigner solid, stripe and bubble phases etc. In 2DES it is sufficient to sweep the perpendicular magnetic field to pass from one of these phases into another. Experimentally, many of these phases can be revealed by simply measuring the resistance. For a quantum Hall state, the longitudinal resistance vanishes, while the Hall resistance exhibits a plateau. The quantum Hall plateau is a manifestation of localization induced by the inevitable sample disorder. Coulomb interaction can also play an important role to localize charges. Even in the disorder-free case, electrons - more precisely quasi-particles in the

Probing the liquid and solid phases in closely spaced two-dimensional systems

International Nuclear Information System (INIS)

Zhang, Ding

2014-01-01

Gas, liquid and solid phases are the most common states of matter in our daily encountered 3-dimensional space. The school example is the H 2 O molecule with its phases vapor, water and ice. Interestingly, electrons - with their point-like nature and negative charges - can also organize themselves under certain conditions to bear properties of these three common phases. At relatively high temperature, where Boltzmann statistics prevails, the ensemble of electrons without interactions can be treated as a gas of free particles. Cooling down the system, this electron gas condenses into a Fermi liquid. Finally, as a result of the repulsive Coulomb forces, electrons try to avoid each other by maximizing their distances. When the Coulomb interaction becomes sufficiently strong, a regular lattice emerges - an electron solid. The story however does not end here. Nature has much more in store for us. Electronic systems in fact exhibit a large variety of phases induced by spatial confinement, an external magnetic field, Coulomb interactions, or interactions involving degrees of freedom other than charge such as spin and valley. Here in this thesis, we restrict ourselves to the study of electrons in a 2-dimenisonal (2D) plane. Already in such a 2D electron system (2DES), several distinct states of matter appear: integer and fractional quantum Hall liquids, the 2D Wigner solid, stripe and bubble phases etc. In 2DES it is sufficient to sweep the perpendicular magnetic field to pass from one of these phases into another. Experimentally, many of these phases can be revealed by simply measuring the resistance. For a quantum Hall state, the longitudinal resistance vanishes, while the Hall resistance exhibits a plateau. The quantum Hall plateau is a manifestation of localization induced by the inevitable sample disorder. Coulomb interaction can also play an important role to localize charges. Even in the disorder-free case, electrons - more precisely quasi-particles in the partially

HPLC WITH SOLID PHASE EXTRACTION FOR IDENTIFICATION AND DIAGNOSIS OF ORGANOPHOSPHOROUS POISONING IN GOATS

Directory of Open Access Journals (Sweden)

S. Manna

2014-12-01

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.

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

Science.gov (United States)

Benet, James

1993-01-01

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).

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

Directory of Open Access Journals (Sweden)

Andreas Beyer

2015-10-01

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

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

OpenAIRE

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

2015-01-01

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

Use of solid-phase salt catalysts in furfural preparation

Energy Technology Data Exchange (ETDEWEB)

Morozov, E.F.; Shkut, V.M.; Kebich, M.S.; Kuznetsova, T.A.

1981-01-01

The manufacture of furfural (I) from tanning waste, birch sawdust, or corncobs at 220-230 degrees in the presence of 2.0-3.0% double superphosphate, ammophos, (NH/sub 4/)/sub 2/SO/sub 4/, NH/sub 4/NO/sub 3/, or NH/sub 4/Cl was evaluated. Most of I is formed within 40 minutes in the presence of NH4NO3 or NH4Cl, and within 55 minutes in the presence of double superphosphate. The highest yield of I was obtained in the presence of NH4NO3 and/or NH4Cl. The solid-phase catalyst caused a little degradation of lignocellulose.

Novel nanoporous sorbent for solid-phase extraction in petroleum fingerprinting

Science.gov (United States)

Alayande, S. Oluwagbemiga; Hlengilizwe, Nyoni; Dare, E. Olugbenga; Msagati, Titus A. M.; Akinlabi, A. Kehinde; Aiyedun, P. O.

2016-04-01

Sample preparation is crucial in the analysis of petroleum and its derivatives. In this study, developing affordable sorbent for petroleum fingerprinting analysis using polymer waste such expanded polystyrene was explored. The potential of electrospun expanded polystyrene (EPS) as a sorbent for the solid-phase extraction (SPE) technique was investigated, and its efficiency was compared with commercial cartridges such as alumina, silica and alumina/silica hybrid commercial for petroleum fingerprinting analysis. The chromatograms showed that the packed electrospun EPS fibre demonstrated excellent properties for SPE applications relative to the hybrid cartridges.

Sensitive and fast mutation detection by solid phase chemical cleavage

DEFF Research Database (Denmark)

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

1996-01-01

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

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

DEFF Research Database (Denmark)

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

2011-01-01

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

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

NARCIS (Netherlands)

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

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

Direct determination of enthalpies of solid phase reactions by immersion method; Determination directe des enthalpies de reaction en phase solide par une methode de plongee

Energy Technology Data Exchange (ETDEWEB)

Roux, A; Richard, M; Eyraud, L; Stevanovic, M; Elston, J [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

1967-07-01

It is not generally possible to measure the enthalpy change corresponding to solid phase reactions using the dynamic differential thermal analysis method because these reactions are usually too slow at the temperature of operation of present equipment. A ballistic differential thermal analysis apparatus has been developed which is based on an immersion-compensation method; it overcomes the difficulties previously encountered. This apparatus has been used after calibration for determining the enthalpies of formation of calcium and cadmium titanates. and also the Wigner energies of BeO, MgO and Al{sub 2}O{sub 3} samples irradiated at variable dose at a temperature of under 100 deg. C. (authors) [French] Il n'est generalement pas possible de mesurer la variation d'enthalpie correspondant aux reactions en phase solide par la methode d'analyse thermique differentielle dynamique. En effet, ces reactions sont le plus souvent trop lentes aux temperatures d'utilisation des dispositifs actuels. Un appareil d'analyse thermique differentielle balistique, base sur une methode de plongee avec compensation, a ete mis au point et permet de surmonter les difficultes precedentes. Apres etalonnages, cet appareil a ete utilise pour la determination des enthalpies de formation du titanate de calcium et du titanate de cadmium ainsi que pour celle des energies Wigner emmagasinees dans des echantillons de BeO, MgO et Al{sub 2}O{sub 3} irradies a une temperature inferieure a 100 deg. C et a differentes doses. (auteurs)

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

International Nuclear Information System (INIS)

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

2011-01-01

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

Ultrasensitive microfluidic solid-phase ELISA using an actuatable microwell-patterned PDMS chip.

Science.gov (United States)

Wang, Tanyu; Zhang, Mohan; Dreher, Dakota D; Zeng, Yong

2013-11-07

Quantitative detection of low abundance proteins is of significant interest for biological and clinical applications. Here we report an integrated microfluidic solid-phase ELISA platform for rapid and ultrasensitive detection of proteins with a wide dynamic range. Compared to the existing microfluidic devices that perform affinity capture and enzyme-based optical detection in a constant channel volume, the key novelty of our design is two-fold. First, our system integrates a microwell-patterned assay chamber that can be pneumatically actuated to significantly reduce the volume of chemifluorescent reaction, markedly improving the sensitivity and speed of ELISA. Second, monolithic integration of on-chip pumps and the actuatable assay chamber allow programmable fluid delivery and effective mixing for rapid and sensitive immunoassays. Ultrasensitive microfluidic ELISA was demonstrated for insulin-like growth factor 1 receptor (IGF-1R) across at least five orders of magnitude with an extremely low detection limit of 21.8 aM. The microwell-based solid-phase ELISA strategy provides an expandable platform for developing the next-generation microfluidic immunoassay systems that integrate and automate digital and analog measurements to further improve the sensitivity, dynamic ranges, and reproducibility of proteomic analysis.

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

Science.gov (United States)

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

2015-09-21

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

Analysis of Solid and Aqueous Phase Products from Hydrothermal Carbonization of Whole and Lipid-Extracted Algae

Directory of Open Access Journals (Sweden)

Amber Broch

2013-12-01

Full Text Available Microalgae have tremendous potential as a feedstock for production of liquid biofuels, particularly biodiesel fuel via transesterification of algal lipids. However, biodiesel production results in significant amounts of algal residues, or “lipid extracted algae” (LEA. Suitable utilization of the LEA residue will improve the economics of algal biodiesel. In the present study, we evaluate the hydrothermal carbonization (HTC of whole and lipid extracted algal (Spirulina maxima feedstocks in order to produce a solid biofuel (hydrochar and value-added co-products in the aqueous phase. HTC experiments were performed using a 2-L Parr reactor (batch type at 175–215 °C with a 30-min holding time. Solid, aqueous and gaseous products were analyzed using various laboratory methods to evaluate the mass and carbon balances, and investigate the existence of high value chemicals in the aqueous phase. The HTC method is effective in creating an energy dense, solid hydrochar from both whole algae and LEA at lower temperatures as compared to lignocellulosic feedstocks, and is effective at reducing the ash content in the resulting hydrochar. However, under the treatment temperatures investigated, less than 1% of the starting dry algae mass was recovered as an identified high-value chemical in the aqueous phase.

Simultaneous solid phase extraction of cobalt, strontium and cesium from liquid radioactive waste using microcrystalline naphthalene

International Nuclear Information System (INIS)

Hamed, Mostafa Mohamed; Attallah, Mohamed Fathy; Metwally, Sayed Sayed

2014-01-01

Most of the procedures developed for the extraction of cobalt, strontium and cesium by solid phase extraction do not employ simultaneous extraction of them. In this study, rapid simultaneous removal of Co 2+ , Sr 2+ and Cs + on microcrystalline naphthalene as solid-phase extractant was investigated. These ions were allowed to form chelates with oxine and then adsorbed on freshly microcrystalline naphthalene from aqueous solutions. The solid phase extraction procedure (SPE) was optimized by using model solution containing Co 2+ , Sr 2+ and Cs + in batch system. The effects of different parameters such as variation in pH, reagent concentration, standing time, naphthalene solution concentration and contact time on the simultaneous removal of these ions was studied. The obtained results indicated that, sorption was found to be rapid, and the percentage removal of Co 2+ , Sr 2+ and Cs + was found to be 98, 79 and 68% within 10 min, respectively. The kinetics of the sorption process was investigated to understand the kinetic characteristics of sorption of metal chelates onto microcrystalline naphthalene. The developed procedure has been successfully applied to the removal and recovery of 60 Co and 134 Cs from liquid radioactive waste. The parameters can be used for designing a plant for treatment of wastewater economically.

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

Directory of Open Access Journals (Sweden)

Wilma Regina Barrionuevo

2001-04-01

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

Surface morphology and structure of Ge layer on Si(111) after solid phase epitaxy

Science.gov (United States)

Yoshida, Ryoma; Tosaka, Aki; Shigeta, Yukichi

2018-05-01

The surface morphology change of a Ge layer on a Si(111) surface formed by solid phase epitaxy has been investigated with a scanning tunneling microscope (STM). The Ge film was deposited at room temperature and annealed at 400 °C or 600 °C. The STM images of the sample surface after annealing at 400 °C show a flat wetting layer (WL) with small three-dimensional islands on the WL. After annealing at 600 °C, the STM images show a surface roughening with large islands. From the relation between the average height of the roughness and the deposited layer thickness, it is confirmed that the diffusion of Ge atoms becomes very active at 600 °C. The Si crystal at the interface is reconstructed and the intermixing occurs over 600 °C. However, the intermixing is fairly restricted in the solid phase epitaxy growth at 400 °C. The surface morphology changes with the crystallization at 400 °C are discussed by the shape of the islands formed on the WL surface. It is shown that the diffusion of the Ge atoms in the amorphous phase is active even at 400 °C.

Solid-liquid phase equilibria of Fe-Cr-Al alloys and spinels

Science.gov (United States)

McMurray, J. W.; Hu, R.; Ushakov, S. V.; Shin, D.; Pint, B. A.; Terrani, K. A.; Navrotsky, A.

2017-08-01

Ferritic FeCrAl alloys are candidate accident tolerant cladding materials. There is a paucity of data concerning the melting behavior for FeCrAl and its oxides. Analysis tools have therefore had to utilize assumptions for simulations using FeCrAl cladding. The focus of this study is to examine in some detail the solid-liquid phase equilibria of FeCrAl alloys and spinels with the aim of improving the accuracy of severe accident scenario computational studies.

Monitoring of chloropesticide methoxychlor preconcentration from waste water using hplc - solid phase extraction (abstract)

International Nuclear Information System (INIS)

Butt, S.B.; Saqlin, M.; Riaz, M.

2011-01-01

The method involves preconcentration of methoxychlor by solid phase extraction (SPE) with 1 mL silica based C-18 and 3 mL polymer based C-18 cartridge and then quantification by high performance liquid chromatography with UV detector (HPLC-UV). Optimization of HPLC parameters was done by determining max of methoxychlor on a double beam UV/Visible spectrophotometer, flow rate of mobile phase on reversed phase columns. Lowest detection limit for methoxychlor dissolved in water and methanol was 0.2ppm and 0.1ppm respectively. For solid phase extraction recovery studies and effect of different parameters such as initial concentration of analyte 0.01 to 0.05 ppm, loading rate 1 and 2mL/min, nature of desorbing solvent (methanol, ethyl acetate and acetonitrile) were investigated. Periodic self degradation of methoxychlor, and reusing potential of both SPE materials was also explored. Lower initial concentrations and slower loading rate of methoxychlor solutions gave improved recoveries. Recoveries were in the range of 80 to 90% for new SPE cartridge and reduced to 35 to 57% for once used silica based C-18 tubes. It was around 73 % for HLB C18 on their second use, and decreased on their repeated reuse. Lastly recoveries for stimulant and real waste water samples were determined to be 77 and 60% respectively. (author)

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

DEFF Research Database (Denmark)

Mysling, Simon; Palmisano, Giuseppe; Højrup, Peter

2010-01-01

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

Domain patterns and hysteresis in phase-transforming solids: analysis and numerical simulations of a sharp interface dissipative model via phase-field approximation

Czech Academy of Sciences Publication Activity Database

DeSimone, A.; Kružík, Martin

2013-01-01

Roč. 8, č. 2 (2013), s. 481-499 ISSN 1556-1801 R&D Projects: GA ČR(CZ) GAP201/12/0671 Institutional support: RVO:67985556 Keywords : hysteresis * shape memory Subject RIV: BA - General Mathematics Impact factor: 0.952, year: 2013 http://library.utia.cas.cz/separaty/2013/MTR/kruzik-domain patterns and hysteresis in phase-transforming solids analysis and numerical simulations of a sharp interface dissipative model via phase-field approximation.pdf

Density of phonon-fracton states of disordered solids in the vicinity of percolation phase transitions

International Nuclear Information System (INIS)

Korzhenevskii, A.L.; Luzhkov, A.A.

1991-01-01

The development of a theory of phase transitions in disordered materials is still one of the central problems in solid-state physics. The model of a percolation phase transition plays the same role among the models put forward to account for phase transitions in disordered media as does the Ising model for second-order phase transitions in ideal crystals. In addition to the clear picture of the processes occurring in the course of a percolation phase transition, a scaling theory has been developed and various techniques have been used to calculate the critical exponents describing the thermodynamics of a medium in the vicinity of the percolation threshold. The authors adopt a field-theoretic approach in a study of acoustic properties of disordered solids undergoing percolation phase transitions characterized by h ∼ 1. Among these transitions they concentrate on the case with the simplest type of striction interaction when the solution of a stochastic vector differential equation of motion describing the behavior of an elastic medium in the critical region can be reduced to a scalar equation. The results of their calculations by the field renormalization group method confirmed the existence of the scaling relationships between the critical exponents and also the conclusion on the nature of short- and long-wavelength vibrations near the percolation threshold, which follow from phenomenological considerations of the scaling theory. The values of the upper critical dimensionality and of the critical exponents of the problem are shown to differ from the values applicable to percolation phase transitions characterized by h much-lt 1

Application of solid-phase antibodies to radioimmunoassay

International Nuclear Information System (INIS)

McConway, M.G.; Chapman, R.S.

1986-01-01

Two types of polymeric microparticle, Dynospheres and reprecipitated acid-hydrolysed nylon 6/6, and two methods of activating these particles with either tresyl chloride or carbonyldiimidazole (CDI) prior to covalent linkage of antibodies were investigated with a view towards their respective adoption for the preparation of general solid-phase reagents for immunoassay applications. Activation of each particle and coupling of antibodies was rapid irrespective of the activator. CDI proved to be the activator of choice since it was cheap, less hazardous, more efficient and less pH dependent than tresyl chloride. Both types of microparticle remain buoyant during the RIA incubation periods and form stable pellets after centrifugation. In second antibody applications immobilisation of the first antibody occurs with a short incubation period of 30 min. Nylon microparticles have a higher antibody-coupling capacity and are the particles of choice in both first and second antibody applications. However, the nylon microparticles possess marginally higher non-specific binding characteristics. (Auth.)

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

Science.gov (United States)

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

2018-02-14

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

Platform construction and extraction mechanism study of magnetic mixed hemimicelles solid-phase extraction

Science.gov (United States)

Xiao, Deli; Zhang, Chan; He, Jia; Zeng, Rong; Chen, Rong; He, Hua

2016-12-01

Simple, accurate and high-throughput pretreatment method would facilitate large-scale studies of trace analysis in complex samples. Magnetic mixed hemimicelles solid-phase extraction has the power to become a key pretreatment method in biological, environmental and clinical research. However, lacking of experimental predictability and unsharpness of extraction mechanism limit the development of this promising method. Herein, this work tries to establish theoretical-based experimental designs for extraction of trace analytes from complex samples using magnetic mixed hemimicelles solid-phase extraction. We selected three categories and six sub-types of compounds for systematic comparative study of extraction mechanism, and comprehensively illustrated the roles of different force (hydrophobic interaction, π-π stacking interactions, hydrogen-bonding interaction, electrostatic interaction) for the first time. What’s more, the application guidelines for supporting materials, surfactants and sample matrix were also summarized. The extraction mechanism and platform established in the study render its future promising for foreseeable and efficient pretreatment under theoretical based experimental design for trace analytes from environmental, biological and clinical samples.

Solid phase synthesis and antiprotozoal evaluation of di- and trisubstituted 5'-carboxamidoadenosine analogues.

Science.gov (United States)

Rodenko, Boris; Detz, Remko J; Pinas, Victorine A; Lambertucci, Catia; Brun, Reto; Wanner, Martin J; Koomen, Gerrit-Jan

2006-03-01

The rapid increase of resistance to drugs commonly used in the treatment of tropical diseases such as malaria and African sleeping sickness calls for the prompt development of new safe and efficacious drugs. The pathogenic protozoan parasites lack the capability of synthesising purines de novo and they take up preformed purines from their host through various transmembrane transporters. Adenosine derivatives constitute a class of potential therapeutics due to their selective internalisation by these transporters. Automated solid-phase synthesis can speed up the process of lead finding and we pursued the solid-phase synthesis of di- and trisubstituted 5'-carboxamidoadenosine derivatives by using a safety-catch approach. While efforts with Kenner's sulfonamide linker remained fruitless, successful application of the hydrazide safety-catch linker allowed the construction of two representative combinatorial libraries. Their antiprotozoal evaluation identified two compounds with promising activity: N(6)-benzyl-5'-N-phenylcarboxamidoadenosine with an IC(50) value of 0.91 microM against Trypanosoma brucei rhodesiense and N(6)-diphenylethyl-5'-phenylcarboxamidoadenosine with an IC(50) value of 1.8 microM against chloroquine resistant Plasmodium falciparum.

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

Science.gov (United States)

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

2015-10-14

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

Liquid-liquid and liquid-solid phase separation and flocculation for a charged colloidal dispersion

International Nuclear Information System (INIS)

Lai, S.K.; Wu, K.L.

2002-01-01

We model the intercolloidal interaction by a hard-sphere Yukawa repulsion to which is added the long-range van der Waals attraction. In comparison with the Derjaguin-Landau-Verwey-Overbeek repulsion, the Yukawa repulsion explicitly incorporates the spatial correlations between colloids and small ions. As a result, the repulsive part can be expressed analytically and has a coupling strength depending on the colloidal volume fraction. By use of this two-body potential of mean force and in conjunction with a second-order thermodynamic perturbation theory, we construct the colloidal Helmholtz free energy and use it to calculate the thermodynamic quantities, pressure and chemical potential, needed in the determination of the liquid-liquid and liquid-solid phase diagrams. We examine, in an aqueous charged colloidal dispersion, the effects of the Hamaker constant and particle size on the conformation of a stable liquid-liquid phase transition calculated with respect to the liquid-solid coexistence phases. We find that there exists a threshold Hamaker constant or particle size whose value demarcates the stable liquid-liquid coexistence phases from their metastable counterparts. Applying the same technique and using the energetic criterion, we extend our calculations to study the flocculation phenomenon in aqueous charged colloids. Here, we pay due attention to determining the loci of a stability curve stipulated for a given temperature T 0 , and obtain the parametric phase diagram of the Hamaker constant vs the coupling strength or, at given surface potential, the particle size. By imposing T 0 to be the critical temperature T c , i.e., setting k B T 0 (=k B T c ) equal to a reasonable potential barrier, we arrive at the stability curve that marks the irreversible reversible phase transition. The interesting result is that there occurs a minimum size for the colloidal particles below (above) which the colloidal dispersion is driven to an irreversible (reversible) phase

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

International Nuclear Information System (INIS)

Niemiec, W.

1985-01-01

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

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

Science.gov (United States)

Yang, Bin; Lai, Wen-Sheng

2009-06-01

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

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

Directory of Open Access Journals (Sweden)

Ying Fu

2017-05-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Mitchell, A R

2007-12-04

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

Solid-phase glycan isolation for glycomics analysis.

Science.gov (United States)

Yang, Shuang; Zhang, Hui

2012-12-01

Glycosylation is one of the most significant protein PTMs. The biological activities of proteins are dramatically changed by the glycans associated with them. Thus, structural analysis of the glycans of glycoproteins in complex biological or clinical samples is critical in correlation with the functions of glycans with diseases. Profiling of glycans by HPLC-MS is a commonly used technique in analyzing glycan structures and quantifying their relative abundance in different biological systems. Methods relied on MS require isolation of glycans from negligible salts and other contaminant ions since salts and ions may interfere with the glycans, resulting in poor glycan ionization. To accomplish those objectives, glycan isolation and clean-up methods including SPE, liquid-phase extraction, chromatography, and electrophoresis have been developed. Traditionally, glycans are isolated from proteins or peptides using a combination of hydrophobic and hydrophilic columns: proteins and peptides remain on hydrophobic absorbent while glycans, salts, and other hydrophilic reagents are collected as flowthrough. The glycans in the flowthrough are then purified through graphite-activated carbon column by hydrophilic interaction LC. Yet, the drawback in these affinity-based approaches is nonspecific binding. As a result, chemical methods by hydrazide or oxime have been developed for solid-phase isolation of glycans with high specificity and yield. Combined with high-resolution MS, specific glycan isolation techniques provide tremendous potentials as useful tools for glycomics analysis. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Molecular imprinting solid phase extraction for selective detection of methidathion in olive oil.

Science.gov (United States)

Bakas, Idriss; Oujji, Najwa Ben; Moczko, Ewa; Istamboulie, Georges; Piletsky, Sergey; Piletska, Elena; Ait-Ichou, Ihya; Ait-Addi, Elhabib; Noguer, Thierry; Rouillon, Régis

2012-07-13

A specific adsorbent for extraction of methidathion from olive oil was developed. The design of the molecularly imprinted polymer (MIP) was based on the results of the computational screening of the library of polymerisable functional monomers. MIP was prepared by thermal polymerisation using N,N'-methylene bisacrylamide (MBAA) as a functional monomer and ethylene glycol dimethacrylate (EGDMA) as a cross-linker. The polymers based on the itaconic acid (IA), methacrylic acid (MAA) and 2-(trifluoromethyl)acryl acid (TFMAA) functional monomers and one control polymer which was made without functional monomers with cross-linker EGDMA were also synthesised and tested. The performance of each polymer was compared using corresponding imprinting factor. As it was predicted by molecular modelling the best results were obtained for the MIP prepared with MBAA. The obtained MIP was optimised in solid-phase extraction coupled with high performance liquid chromatography (MISPE-HPLC-UV) and tested for the rapid screening of methidathion in olive oil. The proposed method allowed the efficient extraction of methidathion for concentrations ranging from 0.1 to 9 mg L(-1) (r(2)=0.996). The limits of detection (LOD) and quantification (LOQ) in olive oil were 0.02 mg L(-1) and 0.1 mg L(-1), respectively. MIPs extraction was much more effective than traditional C18 reverse-phase solid phase extraction. Copyright © 2012 Elsevier B.V. All rights reserved.

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

Energy Technology Data Exchange (ETDEWEB)

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

1984-01-01

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

Modeling of sorption processes on solid-phase ion-exchangers

Science.gov (United States)

Dorofeeva, Ludmila; Kuan, Nguyen Anh

2018-03-01

Research of alkaline elements separation on solid-phase ion-exchangers is carried out to define the selectivity coefficients and height of an equivalent theoretical stage for both continuous and stepwise filling of column by ionite. On inorganic selective sorbents the increase in isotope enrichment factor up to 0.0127 is received. Also, parametrical models that are adequately describing dependence of the pressure difference and the magnitude expansion in the ion-exchange layer from the flow rate and temperature have been obtained. The concentration rate value under the optimum realization conditions of process and depending on type of a selective material changes in a range 1.021÷1.092. Calculated results show agreement with experimental data.

Effects of Ni(2+) on aluminum hydroxide scale formation and transformation on a simulated drinking water distribution system.

Science.gov (United States)

Wang, Wendong; Song, Shan; Zhang, Xiaoni; Mitchell Spear, J; Wang, Xiaochang; Wang, Wen; Ding, Zhenzhen; Qiao, Zixia

2014-07-01

Observations of aluminum containing sediments/scales formed within the distribution pipes have been reported for several decades. In this study, the effect of Ni(2+) on the formation and transformation processes of aluminum hydroxide sediment in a simulated drinking water distribution system were investigated using X-ray diffraction spectrum (XRD), Fourier transform infrared spectrum (FT-IR), scanning electron microscope (SEM), and thermodynamic calculation methods. It was determined that the existence of Ni(2+) had notable effects on the formation of bayerite. In the system without Ni(2+) addition, there was no X-ray diffraction signal observed after 400 d of aging. The presence of Ni(2+), however, even when present in small amounts (Ni/Al=1:100) the formation of bayerite would occur in as little as 3d at pH 8.5. As the molar ratio of Ni/Al increase from 1:100 to 1:10, the amount of bayerite formed on the pipeline increased further; meanwhile, the specific area of the pipe scale decreased from 160 to 122 m(2)g(-1). In the system with Ni/Al molar ratio at 1:3, the diffraction spectrum strength of bayerite became weaker, and disappeared when Ni/Al molar ratios increased above 1:1. At these highs Ni/Al molar ratios, Ni5Al4O11⋅18H2O was determined to be the major component of the pipe scale. Further study indicated that the presence of Ni(2+) promoted the formation of bayerite and Ni5Al4O11⋅18H2O under basic conditions. At lower pH (6.5) however, the existence of Ni(2+) had little effect on the formation of bayerite and Ni5Al4O11⋅18H2O, rather the adsorption of amorphous Al(OH)3 for Ni(2+) promoted the formation of crystal Ni(OH)2. Copyright © 2013 Elsevier Ltd. All rights reserved.

Effect of solid-meal caloric content on gastric emptying kinetics of solids and liquids.

Science.gov (United States)

Urbain, J L; Siegel, J A; Mortelmans, L; van Cutsem, E; van den Maegdenbergh, V; de Roo, M

1989-08-01

In this study, we have evaluated the effect of the caloric content of a physiological test meal on the gastric emptying kinetics of solids and liquids. 22 healthy male volunteers were studied in two groups matched for age. After an overnight fast, each volunteer underwent the same test procedure; in the first group (G I), 10 volunteers received a meal consisting of bread, 111In-DTPA water and 1 scrambled egg labeled with 99mTc-labelled sulphur colloid; in the second group (G II) 12 volunteers were given the same meal but with 2 labeled eggs in order to increase the caloric content of the solid phase meal. Simultaneous anterior and posterior images were recorded using a dual-headed gamma camera. Solid and liquid geometric mean data were analyzed to determine the lag phase, the emptying rate and the half-emptying time for both solids and liquids. Solid and liquid gastric half-emptying times were significantly prolonged in G II compared to G I volunteers. For the solid phased, the delay was accounted for by a longer lag phase and a decrease in the equilibrium emptying rate. The emptying rate of the liquid phase was significantly decreased in G II compared to G I. Within each group, no statistically significant difference was observed between solid and liquid emptying rates. We conclude that the caloric content of the solid portion of a meal not only alters the emptying of the solid phase but also affects the emptying of the liquid component of the meal.

Effect of solid-meal caloric content on gastric emptying kinetics of solids and liquids

International Nuclear Information System (INIS)

Urbain, J.L.; Mortelmans, L.; Cutsem, E. van; Maegdenbergh, V. van den; Roo, M. de

1989-01-01

In this study, we have evaluated the effect of the caloric content of a physiological test meal on the gastric emptying kinetics of solids and liquids. 22 healthy male volunteers were studied in two groups matched for age. After an overnight fast, each volunteer underwent the same test procedure; in the first group (G I), 10 volunteers received a meal consisting of bread, 111 In-DTPA water and 1 scrambled egg labeled with 99m Tc-labelled sulphur colloid; in the second group (G II) 12 volunteers were given the same meal but with 2 labeled eggs in order to increase the caloric content of the solid phase meal. Simultaneous anterior and posterior images were recorded using a dual-headed gamma camera. Solid and liquid geometric mean data were analyzed to determine the lag phase, the emptying rate and the half-emptying time for both solids and liquids. Solid and liquid gastric half-emptying times were significantly prolonged in G II compared to G I volunteers. For the solid phased, the delay was accounted for by a longer lag phase and a decrease in the equilibrium emptying rate. The emptying rate of the liquid phase was significantly decreased in G II compared to G I. Within each group, no statistically significant difference was observed between solid and liquid emptying rates. We conclude that the caloric content of the solid portion of a meal not only alters the emptying of the solid phase but also affects the emptying of the liquid component of the meal. (orig.) [de

Solid-state diffusion-controlled growth of the phases in the Au-Sn system

Science.gov (United States)

Baheti, Varun A.; Kashyap, Sanjay; Kumar, Praveen; Chattopadhyay, Kamanio; Paul, Aloke

2018-01-01

The solid state diffusion-controlled growth of the phases is studied for the Au-Sn system in the range of room temperature to 200 °C using bulk and electroplated diffusion couples. The number of product phases in the interdiffusion zone decreases with the decrease in annealing temperature. These phases grow with significantly high rates even at the room temperature. The growth rate of the AuSn4 phase is observed to be higher in the case of electroplated diffusion couple because of the relatively small grains and hence high contribution of the grain boundary diffusion when compared to the bulk diffusion couple. The diffraction pattern analysis indicates the same equilibrium crystal structure of the phases in these two types of diffusion couples. The analysis in the AuSn4 phase relating the estimated tracer diffusion coefficients with grain size, crystal structure, the homologous temperature of experiments and the concept of the sublattice diffusion mechanism in the intermetallic compounds indicate that Au diffuses mainly via the grain boundaries, whereas Sn diffuses via both the grain boundaries and the lattice.

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

Science.gov (United States)

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

2016-08-15

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

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

NARCIS (Netherlands)

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

2017-01-01

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

Microextração por fase sólida SPME, Solid Phase Micro-Extration

Directory of Open Access Journals (Sweden)

Antonio Luiz Pires Valente

2000-08-01

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

Preparation of peptide thioesters through fmoc-based solid-phase peptide synthesis by using amino thioesters

DEFF Research Database (Denmark)

Stuhr-Hansen, N.; Wilbek, T.S.; Strømgaard, K.

2013-01-01

protected peptide thioester, which was globally deprotected to afford the desired unprotected peptide thioester. The method is compatible with labile groups such as phosphoryl and glycosyl moieties. The synthesis of peptide alkyl thioesters by 9-fluorenylmethoxycarbonyl (Fmoc) solid-phase peptide synthesis...

Solid-State NMR Study of New Copolymers as Solid Polymer Electrolytes

Directory of Open Access Journals (Sweden)

Jean-Christophe Daigle

2018-01-01

Full Text Available We report the analysis of comb-like polymers by solid-state NMR. The polymers were previously evaluated as solid-polymer-electrolytes (SPE for lithium-polymer-metal batteries that have suitable ionic conductivity at 60 °C. We propose to develop a correlation between 13C solid-state NMR measurements and phase segregation. 13C solid-state NMR is a perfect tool for differentiating polymer phases with fast or slow motions. 7Li was used to monitor the motion of lithium ions in the polymer, and activation energies were calculated.

Solubility and hydrolysis of Np(V) in dilute to concentrated alkaline NaCl solutions. Formation of Na-Np(V)-OH solid phases at 22 C

Energy Technology Data Exchange (ETDEWEB)

Petrov, Vladimir G. [Lomonosov Moscow State Univ. (Russian Federation). Dept. of Chemistry; Fellhauer, David; Gaona, Xavier; Dardenne, Kathy; Rothe, Joerg; Altmaier, Marcus [Karlsruhe Institute of Technology (Germany). Inst. for Nuclear Waste Disposal; Kalmykov, Stepan N. [Lomonosov Moscow State Univ. (Russian Federation). Dept. of Chemistry; NRC Kurchatov Institute, Moscow (Russian Federation)

2017-03-01

The solubility of Np(V) was investigated at T=22±2 C in alkaline NaCl solutions of different ionic strength (0.1-5.0 M). The solid phases controlling the solubility at different -log{sub 10} m{sub H{sup +}}(pH{sub m}) and NaCl concentration were characterized by XRD, quantitative chemical analysis, SEM-EDS and XAFS (both XANES and EXAFS). Aqueous phases in equilibrium with Np(V) solids were investigated for selected samples within 8.9≤pH{sub m}≤10.3 by UV-vis/NIR absorption spectroscopy. In 0.1 M NaCl, the experimental solubility of the initial greenish NpO{sub 2}OH(am) solid phase is in good agreement with previous results obtained in NaClO{sub 4} solutions, and is consistent with model calculations for fresh NpO{sub 2}OH(am) using the thermodynamic data selection in NEA-TDB. Below pH{sub m}∝11.5 and for all NaCl concentrations studied, Np concentration in equilibrium with the solid phase remained constant during the timeframe of this study (∝2 years). This observation is in contrast to the aging of the initial NpO{sub 2}OH(am) into a more crystalline modification with the same stoichiometry, NpO{sub 2}OH(am, aged), as reported in previous studies for concentrated NaClO{sub 4} and NaCl. Instead, the greenish NpO{sub 2}OH(am) transforms into a white solid phase in those systems with [NaCl]≥1.0 M and pH{sub m}≥11.5, and into two different pinkish phases above pH{sub m}∝13.2. The solid phase transformation is accompanied by a drop in Np solubility of 0.5-2 log{sub 10}-units (depending upon NaCl concentration). XANES analyses of green, white and pink phases confirm the predominance of Np(V) in all cases. Quantitative chemical analysis shows the incorporation of Na{sup +} in the original NpO{sub 2}OH(am) material, with Na:Np ≤ 0.3 for the greenish solids and 0.8 ≤ Na:Np ≤ 1.6 for the white and pinkish phases. XRD data confirms the amorphous character of the greenish phase, whereas white and pink solids show well-defined but discrepant XRD patterns

Analytical methodologies based on LC-MS/MS for monitoring selected emerging compounds in liquid and solid phases of the sewage sludge.

Science.gov (United States)

Boix, C; Ibáñez, M; Fabregat-Safont, D; Morales, E; Pastor, L; Sancho, J V; Sánchez-Ramírez, J E; Hernández, F

2016-01-01

In this work, two analytical methodologies based on liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) were developed for quantification of emerging pollutants identified in sewage sludge after a previous wide-scope screening. The target list included 13 emerging contaminants (EC): thiabendazole, acesulfame, fenofibric acid, valsartan, irbesartan, salicylic acid, diclofenac, carbamazepine, 4-aminoantipyrine (4-AA), 4-acetyl aminoantipyrine (4-AAA), 4-formyl aminoantipyrine (4-FAA), venlafaxine and benzoylecgonine. The aqueous and solid phases of the sewage sludge were analyzed making use of Solid-Phase Extraction (SPE) and UltraSonic Extraction (USE) for sample treatment, respectively. The methods were validated at three concentration levels: 0.2, 2 and 20 μg L(-1) for the aqueous phase, and 50, 500 and 2000 μg kg(-1) for the solid phase of the sludge. In general, the method was satisfactorily validated, showing good recoveries (70-120%) and precision (RSD metabolites of dipyrone had not been studied before in sewage sludge.

Solid phase extraction of uranium from phosphoric acid. Kinetic and thermodynamic study

Energy Technology Data Exchange (ETDEWEB)

Abdel-Magied, Ahmed Fawzy [Nuclear Materials Authority, Cairo (Egypt); Stockholm Univ. (Sweden). Dept. of Organic Chemistry

2017-07-01

There is a high interest to develop suitable solid phase extractants for uranium separation from aqueous solutions in order to reduce cost and enhance the efficiency. This paper describes solid phase extraction of uranium(VI) from aqueous phosphoric acid solution using MCM-41 based D2HEPA-TOPO organophosphorous extractants. The mixture of D2HEPA (di-2-ethyl-hexylphosphoric acid) and TOPO (tri-n-octylphosphine oxide) was impregnated into the pores of MCM-41 and the synthesized sorbent was fully characterized. The influences of different factors such as synergistic mixture ratio, phosphoric acid concentration, mixing time and temperature were investigated. The results showed that 90% of uranium(VI) extraction can be achieved within 5 min, using D2HEPA-TOPO rate at MCM-41 (mass ratio 2:1 w/w) from 1 M phosphoric acid containing 64 ppm of uranium at room temperature. High adsorption capacity of uranium(VI) have been achieved at the mentioned conditions. The rate constant for the chemical adsorption of uranium(VI) was 0.988 g mg{sup -1} min{sup -1} calculated by the pseudo-second order rate equation. The obtained thermodynamics parameters showed that uranium(VI) adsorption from H{sub 3}PO{sub 4} is an exothermic and spontaneous process.

Photodegradation of polycyclic aromatic hydrocarbon pyrene by iron oxide in solid phase

International Nuclear Information System (INIS)

Wang, Y.; Liu, C.S.; Li, F.B.; Liu, C.P.; Liang, J.B.

2009-01-01

To better understand the photodegradation of polycyclic aromatic hydrocarbons (PAH) in solid phase in natural environment, laboratory experiments were conducted to study the influencing factors, kinetics and intermediate compound of pyrene photodegradation by iron oxides. The results showed that the pyrene photodegradation rate followed the order of α-FeOOH > α-Fe 2 O 3 > γ-Fe 2 O 3 > γ-FeOOH at the same reaction conditions. Lower dosage of α-FeOOH and higher light intensity increased the photodegradation rate of pyrene. Iron oxides and oxalic acid can set up a photo-Fenton-like system without additional H 2 O 2 in solid phase to enhance the photodegradation of pyrene under UV irradiation. All reaction followed the first-order reaction kinetics. The half-life (t 1/2 ) of pyrene in the system showed the higher efficiencies of using iron oxide as photocatalyst to degrade pyrene. Intermediate compound pyreno was found during photodegradation reactions by gas chromatography-mass spectrometry (GC-MS). The photodegradation efficiency for PAHs in this photo-Fenton-like system was also confirmed by using the contaminated soil samples. This work provides some useful information to understand the remediation of PAHs contaminated soils by photochemical techniques under practical condition

Solid phase stability of a double-minimum interaction potential system

International Nuclear Information System (INIS)

Suematsu, Ayumi; Yoshimori, Akira; Saiki, Masafumi; Matsui, Jun; Odagaki, Takashi

2014-01-01

We study phase stability of a system with double-minimum interaction potential in a wide range of parameters by a thermodynamic perturbation theory. The present double-minimum potential is the Lennard-Jones-Gauss potential, which has a Gaussian pocket as well as a standard Lennard-Jones minimum. As a function of the depth and position of the Gaussian pocket in the potential, we determine the coexistence pressure of crystals (fcc and bcc). We show that the fcc crystallizes even at zero pressure when the position of the Gaussian pocket is coincident with the first or third nearest neighbor site of the fcc crystal. The bcc crystal is more stable than the fcc crystal when the position of the Gaussian pocket is coincident with the second nearest neighbor sites of the bcc crystal. The stable crystal structure is determined by the position of the Gaussian pocket. These results show that we can control the stability of the solid phase by tuning the potential function

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

Science.gov (United States)

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

2018-02-08

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

SODIUM ALUMINOSILICATE FOULING AND CLEANING OF DECONTAMINATED SALT SOLUTION COALESCERS

International Nuclear Information System (INIS)

Poirier, M.; Thomas Peters, T.; Fernando Fondeur, F.; Samuel Fink, S.

2008-01-01

During initial non-radioactive operations at the Modular Caustic Side Solvent Extraction Unit (MCU), the pressure drop across the decontaminated salt solution coalescer reached ∼10 psi while processing ∼1250 gallons of salt solution, indicating possible fouling or plugging of the coalescer. An analysis of the feed solution and the 'plugged coalescer' concluded that the plugging was due to sodium aluminosilicate solids. MCU personnel requested Savannah River National Laboratory (SRNL) to investigate the formation of the sodium aluminosilicate solids (NAS) and the impact of the solids on the decontaminated salt solution coalescer. Researchers performed developmental testing of the cleaning protocols with a bench-scale coalescer container 1-inch long segments of a new coalescer element fouled using simulant solution. In addition, the authors obtained a 'plugged' Decontaminated Salt Solution coalescer from non-radioactive testing in the MCU and cleaned it according to the proposed cleaning procedure. Conclusions from this testing include the following: (1) Testing with the bench-scale coalescer showed an increase in pressure drop from solid particles, but the increase was not as large as observed at MCU. (2) Cleaning the bench-scale coalescer with nitric acid reduced the pressure drop and removed a large amount of solid particles (11 g of bayerite if all aluminum is present in that form or 23 g of sodium aluminosilicate if all silicon is present in that form). (3) Based on analysis of the cleaning solutions from bench-scale test, the 'dirt capacity' of a 40 inch coalescer for the NAS solids tested is calculated as 450-950 grams. (4) Cleaning the full-scale coalescer with nitric acid reduced the pressure drop and removed a large amount of solid particles (60 g of aluminum and 5 g of silicon). (5) Piping holdup in the full-scale coalescer system caused the pH to differ from the target value. Comparable hold-up in the facility could lead to less effective cleaning and

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

International Nuclear Information System (INIS)

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

1988-09-01

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

Effect of Cold Stress on Fruiting Body Production by Medicinal Basidiomycetes in Submerged and Solid-phase Culture

Directory of Open Access Journals (Sweden)

E.P. Vetchinkina

2017-05-01

Full Text Available The ability of the medicinal xylotrophic basidiomycetes Lentinus edodes, Pleurotus ostreatus, Ganoderma lucidum and Grifola frondosa to produce typical and atypical fruiting bodies with viable basidiospores in submerged and solid-phase culture under stationary conditions in a beer wort-containing medium under cold stress was shown. The examined mushrooms, when not exposed to temperature stress, did not form fruiting bodies. In solid-phase culture in an agarized medium after cold treatment, the basidiome formation period was shortened by 1.5–2 times. Furthermore, the use of a mycelium subjected to temperature stress for inoculation induced and accelerated the formation of fruiting bodies on an industrial wood substrate, which is of great biotechnological importance.

Automated solid-phase extraction of phenolic acids using layered double hydroxide-alumina-polymer disks.

Science.gov (United States)

Ghani, Milad; Palomino Cabello, Carlos; Saraji, Mohammad; Manuel Estela, Jose; Cerdà, Víctor; Turnes Palomino, Gemma; Maya, Fernando

2018-01-26

The application of layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disks for solid-phase extraction is reported for the first time. Al 2 O 3 is embedded in a polymer matrix followed by an in situ metal-exchange process to obtain a layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disk with excellent flow-through properties. The extraction performance of the prepared disks is evaluated as a proof of concept for the automated extraction using sequential injection analysis of organic acids (p-hydroxybenzoic acid, 3,4-dihydroxybenzoic acid, gallic acid) following an anion-exchange mechanism. After the solid-phase extraction, phenolic acids were quantified by reversed-phase high-performance liquid chromatography with diode-array detection using a core-shell silica-C18 stationary phase and isocratic elution (acetonitrile/0.5% acetic acid in pure water, 5:95, v/v). High sensitivity and reproducibility were obtained with limits of detection in the range of 0.12-0.25 μg/L (sample volume, 4 mL), and relative standard deviations between 2.9 and 3.4% (10 μg/L, n = 6). Enrichment factors of 34-39 were obtained. Layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disks had an average lifetime of 50 extractions. Analyte recoveries ranged from 93 to 96% for grape juice and nonalcoholic beer samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

Science.gov (United States)

Sutter, Eli; Sutter, Peter

2008-02-01

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

Divergent solid-phase synthesis of natural product-inspired bipartite cyclodepsipeptides : total synthesis of seragamide A

NARCIS (Netherlands)

Arndt, H.-D.; Rizzo, S.; Nöcker, Chr.; Wackchaure, V.N.; Milroy, L.G.; Bieker, V.; Calderon, A.; Tran, T.T.N.; Brand, S.; Dehmelt, L.; Waldmann, H.

2015-01-01

Macrocyclic natural products (NPs) and analogues thereof often show high affinity, selectivity, and metabolic stability, and methods for the synthesis of NP-like macrocycle collections are of major current interest. We report an efficient solid-phase/cyclorelease method for the synthesis of a

Basic hydrolysis of 1, 3, 4, 6-tetra-O-acetyl-2-[18F] fluoro-D-glucose on solid phase extraction

International Nuclear Information System (INIS)

Zhang Jinming; Tian Jiahe; He Yijie; Huan Dingcai; Liu Boli

2003-01-01

A new base hydrolysis method are used for 1, 3, 4, 6-tetra-O-acetyl-2-[ 18 F] fluoro-D-glucose on solid phase extraction. The labeled intermediate is trapped on an active C-18 solid phase extraction cartridge, and hydrolyzed in cartridge with 1 mL 2 mol/L NaOH at room temperature. The results show that there are over 99% of the labeled intermediate being turned into 18 F-FDG within 2 min. It is easy to get 18 F-FDG after neutralized with phosphate buffer, purified by C-18 and Alumina cartridge. The basic hydrolysis on solid extraction is a simple method for preparation of 18 F-FDG

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

Science.gov (United States)

Reinhart, William

2011-06-01

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

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

International Nuclear Information System (INIS)

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

1995-09-01

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

Molecularly imprinted solid-phase extraction of glutathione from urine samples

International Nuclear Information System (INIS)

Song, Renyuan; Hu, Xiaoling; Guan, Ping; Li, Ji; Zhao, Na; Wang, Qiaoli

2014-01-01

Molecularly imprinted polymer (MIP) particles for glutathione were synthesized through iniferter-controlled living radical precipitation polymerization (IRPP) under ultraviolet radiation at ambient temperature. Static adsorption, solid-phase extraction, and high-performance liquid chromatography were carried out to evaluate the adsorption properties and selective recognition characteristics of the polymers for glutathione and its structural analogs. The obtained IRPP-MIP particles exhibited a regularly spherical shape, rapid binding kinetics, high imprinting factor, and high selectivity compared with the MIP particles prepared using traditional free-radical precipitation polymerization. The selective separation and enrichment of glutathione from the mixture of glycyl-glycine and glutathione disulfide could be achieved on the IRPP-MIP cartridge. The recoveries of glutathione, glycyl-glycine, and glutathione disulfide were 95.6% ± 3.65%, 29.5% ± 1.26%, and 49.9% ± 1.71%, respectively. The detection limit (S/N = 3) of glutathione was 0.5 mg·L −1 . The relative standard deviations (RSDs) for 10 replicate detections of 50 mg·L −1 of glutathione were 5.76%, and the linear range of the calibration curve was 0.5 mg·L −1 to 200 mg·L −1 under optimized conditions. The proposed approach was successfully applied to determine glutathione in spiked human urine samples with recoveries of 90.24% to 96.20% and RSDs of 0.48% to 5.67%. - Highlights: • Imprinted polymer particles were prepared by IRPP at ambient temperature. • High imprinting factor, high selectivity, and rapid binding kinetics were achieved. • Selective solid-phase extraction of glutathione from human urine samples

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

NARCIS (Netherlands)

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

1999-01-01

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

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

International Nuclear Information System (INIS)

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

2014-01-01

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

Detection of viral antigens by solid phase radioimmunoassay on polyethylene film

Energy Technology Data Exchange (ETDEWEB)

Prokudina, E N; Semenova, N P; Zhdanov, V M

1986-04-01

Polyethylene film, without any pretreatment, may serve as a solid phase (SP) for RIA. Viral antigens (HBsAg, and influenza virus) are detected by SP-RIA on the film with a sensitivity of about 2-3 ng/ml or 40-60 pg/assay. The use of polyethylene film allows one to record RIA autographically. The use of micro amounts of reagents and specimens tested is an added advantage. No special equipment is necessary, the method is inexpensive, easy to perform and may be used for mass screening. (Auth.). 7 refs.; 4 figs.

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

Energy Technology Data Exchange (ETDEWEB)

Cooke, G. A.

2013-01-30

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

Formation of metastable and equilibrium phases in the decomposition of the β solid solution in Zr alloys

International Nuclear Information System (INIS)

Zakharova, M.I.; Kirov, S.A.; Khundzhua, A.G.

1978-01-01

The decomposition of the β solid solution is studied in Zr-Nb alloys with adding Mo, Al, V, Fe by the methods of electron microscopy and X-ray diffraction on single crystals. The intermetallic compounds forming during crystallization of the alloys do not influence the precipitation of the ω- and α-phases during ageing. In the local regions of foils prepared by electropolishing after ageing the formation of the metastable f.c.c. phase and in some cases the inverse transformation of two phase state to the parent phase is observed. (author)

Solid solubility, phase transitions, thermal expansion, and compressibility in Sc{sub 1−x}Al{sub x}F{sub 3}

Energy Technology Data Exchange (ETDEWEB)

Morelock, Cody R.; Gallington, Leighanne C. [School of Chemistry and Biochemistry, Georgia Institute of Technology, Atlanta, GA 30332-0400 (United States); Wilkinson, Angus P., E-mail: angus.wilkinson@chemistry.gatech.edu [School of Chemistry and Biochemistry, Georgia Institute of Technology, Atlanta, GA 30332-0400 (United States); School of Materials Science and Engineering, Georgia Institute of Technology, Atlanta, GA 30332-0245 (United States)

2015-02-15

With the goal of thermal expansion control, the synthesis and properties of Sc{sub 1−x}Al{sub x}F{sub 3} were investigated. The solubility limit of AlF{sub 3} in ScF{sub 3} at ∼1340 K is ∼50%. Solid solutions (x≤0.50) were characterized by synchrotron powder diffraction at ambient pressure between 100 and 900 K and at pressures <0.414 GPa while heating from 298 to 523 K. A phase transition from cubic to rhombohedral is observed. The transition temperature increases smoothly with Al{sup 3+} content, approaching 500 K at the solid solubility limit, and also upon compression at fixed Al{sup 3+} content. The slope of the pressure–temperature phase boundary is ∼0.5 K MPa{sup −1}, which is steep relative to that for most symmetry-lowering phase transitions in perovskites. The volume coefficient of thermal expansion (CTE) for the rhombohedral phase is strongly positive, but the cubic-phase CTE varies from negative (x<0.15) to near-zero (x=0.15) to positive (x>0.20) between ∼600 and 800 K. The cubic solid solutions elastically stiffen on heating, while Al{sup 3+} substitution causes softening at a given temperature. - Graphical abstract: The cubic-phase coefficient of thermal expansion for Sc{sub 1−x}Al{sub x}F{sub 3}(solubility limit ∼50% at ∼1340 K) becomes more positive with increased Al{sup 3+} substitution, but the average isothermal bulk modulus decreases (elastic softening). - Highlights: • The solubility limit of AlF{sub 3} in ScF{sub 3} at ∼1340 K is ∼50%. • The phase transition temperature of Sc{sub 1−x}Al{sub x}F{sub 3} increases smoothly with x. • The cubic-phase volume CTE varies from negative to positive with increasing x. • The cubic solid solutions elastically stiffen on heating. • Al{sup 3+} substitution causes softening at a given temperature.

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

International Nuclear Information System (INIS)

Meriadec, B.; Roubertie, P.

1979-01-01

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

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

International Nuclear Information System (INIS)

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

2015-01-01

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

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

Science.gov (United States)

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

1973-03-06

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

Synthesis of 2,4-disubstituted thiazole combinatorial unit on solid-phase: microwave assisted conversion of alcohol to amine monitored by FT-IR

International Nuclear Information System (INIS)

Antonow, Dyeison; Eifler-Lima, Vera Lucia; Mahler, S. Graciela; Serra, Gloria L.; Manta, Eduardo

2005-01-01

Microwave-assisted solid-phase synthesis of the 2,4-disubstituted thiazole 3 on Merrifield Resin is described. The hydroxyl moiety was converted to amine in five steps - including coupling and cleavage - within a total reaction time of 2 hours and 26% overall yield. The entire solid-phase synthesis was efficiently monitored by FT-IR/KBr pellets and allows potential use in combinatorial chemistry. (author)

[Simultaneous determination of 15 industrial synthetic dyes in condiment by solid phase extraction-high performance liquid chromatography].

Science.gov (United States)

Liu, Min; Li, Xiaolin; Bie, Wei; Wang, Minglin; Feng, Qian

2011-02-01

A new method was established for the determination of 15 industrial synthetic dyes in condiment by solid phase extraction-high performance liquid chromatography (SPE-HPLC). The samples were extracted by methanol-water (1:1, v/v) and purified by a solid phase extraction column. Then, the chromatographic separation was achieved on a Luna C18 column by linear gradient elution. The mobile phase was 10 mmol/L ammonium acetate-acetonitrile (containing 1% acetic acid). The results showed that the 15 industrial synthetic dyes can be separated efficiently. The recoveries of the 15 industrial synthetic dyes spiked in condiment were between 84.6% and 114.2% with the relative standard deviations of 0.9% - 10.3%. The limits of detection of this method was 0.05 - 0.18 mg/kg for the 15 industrial synthetic dyes. The method is simple, sensitive, accurate, repeatable and can be used for simultaneous determination of the 15 illegally added industrial synthetic dyes.

Radiation Polymerization in the Solid Phase; Polymerisation radiochimique en phase solide; Radiatsionnaya polimerizatsiya v tverdoj faze; Radiopolimerizacion en fase solida

Energy Technology Data Exchange (ETDEWEB)

Barkalov, I. M.; Gol' danskij, V. I.; Enikolopov, N. S.; Terekhova, S. F.; Trofimova, G. M.

1963-11-15

The radiation polymerization of solid and frozen monomers has recently attracted a great deal of attention because of its theoretical and practical importance in chemical kinetics and radiation chemistry. The strict spacing of monomer units in a polymer brings about a sharp improvement in the physico-chemical properties without any change of chemicai composition. In the synthesis of stereo-regular polymers, the matrix principle is used, i.e. the monomer unit is strictly oriented spatially by the formation of a complex with a catalyst or some other compound. In the radiation polymerization of a number of monomers oriented in clathrate complexes of urea and thio-urea, for instance, crystal stereo-regular polymers were obtained. The simplest variation, however, is the orientation of a monomer in its own crystal lattice. Although many of the theoretical questions involved remain obscure, the technique is extremely promising. Thus, highly crystalline polyoxymethylene has already been obtained by the radiation polymerization of crystalline trioxane. Nevertheless, a more detailed theoretical investigation of the technique is required. For each separate monomer, the contribution to the general picture made by the different types of reaction taking place during irradiation and the subsequent fusion of the solid monomers (specific radiation reaction, post-polymerization and polymerization at phase transition points) needs clarification. Recent detailed research at the Institute of Chemical Physics, USSR, into the solid-phase radiation-polymerization kinetics of a number of monomers, using the calorimetric method and an EPR signal, has revealed the essential role of the specific radiation reaction during the irradiation. The polymerization process for acrylonitrile (from -196{sup o}C to -140{sup o}C) and vinyl acetate (-196{sup o}C to -100{sup o}C) ceases when irradiation is discontinued despite the retention of the shape and intensity of the EPR signal and despite the long

A simple solid-phase radioimmunoassay for the measurement of IgG secreted in vitro by human lymphocytes

International Nuclear Information System (INIS)

Romagnani, S.; Prete, G.F. del; Giudizi, G.M.; Almerigogna, F.; Ricci, M.

1979-01-01

A radioimmunoassay is described for measuring IgG, based on the ability of immunoglobulins of this class to inhibit the binding of radioiodinated staphylococcal protein A to IgG linked to a solid phase. The solid phase is represented by ox erythrocytes coated with anti-ox erthrocyte rabbit IgG, a reagent used for detecting cells equipped with receptors for the Fc fragment of IgG. By this assay the IgG secreted in vitro by human peripheral blood lymphocytes stimulated with PWM and those present in samples of very diluted human sera were measured. It was found that the assay is a very rapid, simple and and reproducible procedure for the detection of IgG immunoglobulin at the nanogram level. (Auth.)

Dynamic speciation analysis of atrazine in aqueous latex nanoparticle dispersions using solid phase microextraction (SPME)

NARCIS (Netherlands)

Benhabib, K.; Town, R.M.; Leeuwen, van H.P.

2009-01-01

Solid phase microextraction (SPME) is applied in the dynamic speciation analysis of the pesticide atrazine in an aqueous medium containing sorbing latex nanoparticles. It is found that the overall rate of extraction of the analyte is faster than in the absence of nanoparticles and governed by the

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

International Nuclear Information System (INIS)

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

2005-01-01

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

Determination of phenprocoumon in plasma and urine using at-line solid-phase extraction-capillary electrophoresis.

NARCIS (Netherlands)

Veraart, J.R.; Gooijer, C.; Lingeman, H.; Velthorst, N.H.; Brinkman, U.A.T.

1998-01-01

The use of capillary electrophoresis (CE) for the analysis of biological samples is rather problematic because of the large number of interferences present in the matrix. One of the possibilities to solve such problems is to couple solid-phase extraction (SPE) at-line with CE, a technique developed

Phase I study of single-agent ribociclib in Japanese patients with advanced solid tumors.

Science.gov (United States)

Doi, Toshihiko; Hewes, Becker; Kakizume, Tomoyuki; Tajima, Takeshi; Ishikawa, Norifumi; Yamada, Yasuhide

2018-01-01

The cyclin D-CDK4/6-INK4-Rb pathway is frequently dysregulated in cancers. Ribociclib, an orally available, selective CDK4/6 inhibitor, showed preliminary clinical activity in a phase I study in the USA and Europe for patients with solid tumors and lymphomas. The present study aimed to determine the single-agent maximum tolerated dose (MTD) and recommended dose for expansion (RDE) in Japanese patients with advanced solid tumors. Ribociclib safety, tolerability, pharmacokinetic profile, and preliminary antitumor activity were also assessed. Japanese patients with solid tumors that had progressed on prior therapies received escalating doses of single-agent ribociclib on a 3-weeks-on/1-week-off schedule. Treatment continued until the development of toxicity or disease progression. A dose escalation was planned for patients with esophageal cancer. In the dose-escalation phase, 4 patients received 400 mg ribociclib and 13 patients received 600 mg ribociclib. Four patients experienced dose-limiting toxicities, 3 of whom were in the 600 mg group. The RDE was declared to be 600 mg, and the MTD was not determined. The most frequent adverse events were hematologic and gastrointestinal. Four patients achieved stable disease at the 600 mg dose; no patients achieved complete or partial response. All patients discontinued the study, the majority due to disease progression. No patients discontinued due to adverse events. Dose escalation was not pursued due to lack of observed efficacy in esophageal cancer. At the RDE of 600 mg/d on a 3-weeks-on/1-week-off schedule, ribociclib showed acceptable safety and tolerability profiles in Japanese patients with advanced solid tumors. © 2017 The Authors. Cancer Science published by John Wiley & Sons Australia, Ltd on behalf of Japanese Cancer Association.

Sensing dissolved sediment porewater concentrations of persistent and bioaccumulative poolutants using disposable solid-phase microextraction fibers

NARCIS (Netherlands)

Mayer, P.; Vaes, W.H.J.; Wijnker, F.; Legierse, K.C.H.M.; Kraaij, R.H.; Tolls, J.; Hermens, J.L.M.

2000-01-01

Polymer coated glass fibers were applied as disposable samplers to measure dissolved concentrations of persistent and bioaccumulative pollutants (PBPs) in sediment porewater. The method is called matrix solid-phase microextraction (matrix-SPME), because it utilizes the entire sediment matrix as a

Solid-phase single molecule biosensing using dual-color colocalization of fluorescent quantum dot nanoprobes

Science.gov (United States)

Liu, Jianbo; Yang, Xiaohai; Wang, Kemin; Wang, Qing; Liu, Wei; Wang, Dong

2013-10-01

The development of solid-phase surface-based single molecule imaging technology has attracted significant interest during the past decades. Here we demonstrate a sandwich hybridization method for highly sensitive detection of a single thrombin protein at a solid-phase surface based on the use of dual-color colocalization of fluorescent quantum dot (QD) nanoprobes. Green QD560-modified thrombin binding aptamer I (QD560-TBA I) were deposited on a positive poly(l-lysine) assembled layer, followed by bovine serum albumin blocking. It allowed the thrombin protein to mediate the binding of the easily detectable red QD650-modified thrombin binding aptamer II (QD650-TBA II) to the QD560-TBA I substrate. Thus, the presence of the target thrombin can be determined based on fluorescent colocalization measurements of the nanoassemblies, without target amplification or probe separation. The detection limit of this assay reached 0.8 pM. This fluorescent colocalization assay has enabled single molecule recognition in a separation-free detection format, and can serve as a sensitive biosensing platform that greatly suppresses the nonspecific adsorption false-positive signal. This method can be extended to other areas such as multiplexed immunoassay, single cell analysis, and real time biomolecule interaction studies.The development of solid-phase surface-based single molecule imaging technology has attracted significant interest during the past decades. Here we demonstrate a sandwich hybridization method for highly sensitive detection of a single thrombin protein at a solid-phase surface based on the use of dual-color colocalization of fluorescent quantum dot (QD) nanoprobes. Green QD560-modified thrombin binding aptamer I (QD560-TBA I) were deposited on a positive poly(l-lysine) assembled layer, followed by bovine serum albumin blocking. It allowed the thrombin protein to mediate the binding of the easily detectable red QD650-modified thrombin binding aptamer II (QD650-TBA II) to

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

International Nuclear Information System (INIS)

Chakraborty, Tanmoy; Rogal, Jutta; Drautz, Ralf

2015-01-01

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

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

DEFF Research Database (Denmark)

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

1998-01-01

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

Characterization of van der Waals type bimodal,- lambda,- meta- and spinodal phase transitions in liquid mixtures, solid suspensions and thin films.

Science.gov (United States)

Rosenholm, Jarl B

2018-03-01

The perfect gas law is used as a reference when selecting state variables (P, V, T, n) needed to characterize ideal gases (vapors), liquids and solids. Van der Waals equation of state is used as a reference for models characterizing interactions in liquids, solids and their mixtures. Van der Waals loop introduces meta- and unstable states between the observed gas (vapor)-liquid P-V transitions at low T. These intermediate states are shown to appear also between liquid-liquid, liquid-solid and solid-solid phase transitions. First-order phase transitions are characterized by a sharp discontinuity of first-order partial derivatives (P, S, V) of Helmholtz and Gibbs free energies. Second-order partial derivatives (K T , B, C V , C P , E) consist of a static contribution relating to second-order phase transitions and a relaxation contribution representing the degree of first-order phase transitions. Bimodal (first-order) and spinodal (second-order) phase boundaries are used to separate stable phases from metastable and unstable phases. The boundaries are identified and quantified by partial derivatives of molar Gibbs free energy or chemical potentials with respect to P, S, V and composition (mole fractions). Molecules confined to spread Langmuir monolayers or adsorbed Gibbs monolayers are characterized by equation of state and adsorption isotherms relating to a two-dimensional van der Waals equation of state. The basic work of two-dimensional wetting (cohesion, adsorption, spreading, immersion), have to be adjusted by a horizontal surface pressure in the presence of adsorbed vapor layers. If the adsorption is extended to liquid films a vertical surface pressure (Π) may be added to account for the lateral interaction, thus restoring PV = ΠAh dependence of thin films. Van der Waals attraction, Coulomb repulsion and structural hydration forces contribute to the vertical surface pressure. A van der Waals type coexistence of ordered (dispersed) and disordered

Kinetics of the (solid + solid) transformations for the piracetam trimorphic system: Incidence on the construction of the p–T equilibrium phase diagram

International Nuclear Information System (INIS)

Corvis, Yohann; Spasojević-de Biré, Anne; Alzina, Camille

2016-01-01

Highlights: • Thermal analyses and X-ray diffraction experiments are performed. • Scan-rate dependence of the transition points is highlighted. • A new phase diagram of piracetam is proposed. • The new hierarchy of polymorphs stability is now coherent with all published data. - Abstract: The three common polymorphs of piracetam have been characterized by associating thermal analysis, X-ray diffraction and densimetry. DSC experiments showed that the (solid + solid) transition temperature between Forms II and I and between Forms III and I is scan-rate dependent. The transition temperatures decrease when the DSC scan rate decreases and the thermodynamic temperatures were confirmed by isothermal X-ray diffraction. These new results in terms of temperature and enthalpy of transition allow us to propose a new equilibrium phase diagram establishing the relative thermodynamic stability of the three common polymorphs of piracetam as a function of the temperature and the pressure. The diagram suggests that Form II presents a small stability domain located just above the stability domain of Form I. As a consequence, Form I should transform into Form II, which itself can turn into Form III when placed under pressure.

The fabrication of quantum wires in silicon utilising the characteristics of solid phase epitaxial regrowth of crystalline silicon

International Nuclear Information System (INIS)

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

1998-01-01

The process of solid phase epitaxy (SPE) in semiconductor materials is one which has been intensively researched due to possible applications in the semiconductor industry. SPE is a solid phase transformation, in which an amorphous layer can be recrystallized either through heating or a combination of heating and ion bombardment. The transformation is believed to occur exclusively at the interface between the amorphous and crystalline layers, with individual atoms from the amorphous phase being incorporated into the crystalline phase by some point defect mechanism. The process has been observed to follow an Arrhenius temperature dependence. A wafer silicon was subjected to a multi-energy silicon implant through a fine nickel grid to amorphise region to a depth of 5μm creating an array of amorphous wells. Metal impurity atoms were then implanted in this region at energy of 500 keV. Samples were examined using an optical microscope and the Alphastep profiler at RMIT. It was confirmed that burgeoning wells were about 2 μm wide and rose about 0.01 μm above the silicon substrate

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

International Nuclear Information System (INIS)

Hojny, M.; Glowacki, M.

2007-01-01

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

Quantitation of complement factor D in human serum by a solid-phase radioimmunoassay

Energy Technology Data Exchange (ETDEWEB)

Barnum, S R; Niemann, M A; Kearney, J F; Volanakis, J E [Alabama Univ., Birmingham (USA)

1984-03-16

A sensitive solid-phase radioimmunoassay is described which quantitates human D to 1-2 ng/ml. The assay was used to measure the concentration of D in normal and acute-phase sera and sera from individuals with systemic lupus erythematosus. All 3 groups of sera had comparable levels of D with mean values of 1.8, 2.3 and 2.5 ..mu..g/ml, respectively. Also tested were sera decomplemented in vitro by activators of the classical and alternative pathways. The results indicated that D is not depleted by alternative or classical pathway activation. However, heat inactivation (56/sup 0/C, 30 min) of serum resulted in almost complete loss of antigenic D.

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

International Nuclear Information System (INIS)

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

1984-01-01

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

Heavy metal levels and solid phase speciation in street dusts of Delhi, India

International Nuclear Information System (INIS)

Banerjee, Anju D.K.

2003-01-01

Although the street dusts of Delhi contain considerably high levels of Cr, Ni, Cu, Cd, Zn and Pb, solid phase speciation results indicate comparatively limited environmental mobility and bioavailability of Ni and Cr. - Street dust samples were collected from three different localities (industrial, heavy traffic and rural) situated in the greater Delhi area of India. The samples analyzed for Cd, Zn, Pb, Ni, Cu, and Cr indicated remarkably high levels of Cr, Ni, and Cu in the industrial area, whilst Pb and Cd did not show any discernible variations between the three localities. A multivariate statistical approach (Principal Component Analysis) was used to define the possible origin of metals in dusts. The street dusts were sequentially extracted so that the solid pools of Cd, Zn, Pb, Ni, Cu, Cr could be partitioned into five operationally defined fractions viz. exchangeable, bound to carbonates, bound to Fe-Mn oxides, bound to organic matter and residual. Metal recoveries in sequential extractions were ±10% of the independently measured total metal concentrations. Cd was the only metal present appreciably (27.16%) in the exchangeable fraction and Cu was the only metal predominantly associated (44.26%) with organic fraction. Zn (45.64%) and Pb (28.26%) were present mainly in the Fe-Mn oxide fraction and the residual fraction was the most dominant solid phase pool of Cr (88.12%) and Ni (70.94%). Assuming that the mobility and bioavailability are related to the solubility of geochemical forms of the metals and decrease in order of extraction, the apparent mobility and potential metal bioavailability for these highly contaminated street dust samples is: Cd>Zn congruent with Pb>Ni>Cu>Cr

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

Science.gov (United States)

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

2017-01-01

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

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

International Nuclear Information System (INIS)

Cooke, G. A.

2013-01-01

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

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

International Nuclear Information System (INIS)

Duan Qunzhang

1999-01-01

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

Modification of Soil Solid Aluminium Phases During an Extreme Experimental Acidification of A Horizons of Forest Soils from Southwest Europe

International Nuclear Information System (INIS)

Novoa-Munoz, J. C.; Garcia-Rodeja Gayoso, E.

2007-01-01

Four umbric A horizons from acid forest soils were acidified in a batch type experiment and its effect in the Al pools of the solid phase analysed by means of selective dissolution methods. The results showed that Al release accounted for the consumption of 85-99% of the added protons, and causes a decrease of 2-33% of the 'reactive' Al pool of the soil solid phase. In these A horizons, inorganic non-crystalline Al and high stability Al-humus complexes are the main sources of the dissolved Al. The contribution of the complexes with intermediate stability only was relevant in the more acid horizon developed from phyllites (P18-A). The increase of equilibration time from 96 to 720 h did not caused significant differences in the decrease of the 'reactive' Al pool suggesting the acid neutralising reactions occurred in less than 96 h. In most cases the quantity of released Al is in agreement with the decrease of the different reactive Al pools of the solid phase

Local Cloudiness Development Forecast Based on Simulation of Solid Phase Formation Processes in the Atmosphere

Science.gov (United States)

Barodka, Siarhei; Kliutko, Yauhenia; Krasouski, Alexander; Papko, Iryna; Svetashev, Alexander; Turishev, Leonid

2013-04-01

Nowadays numerical simulation of thundercloud formation processes is of great interest as an actual problem from the practical point of view. Thunderclouds significantly affect airplane flights, and mesoscale weather forecast has much to contribute to facilitate the aviation forecast procedures. An accurate forecast can certainly help to avoid aviation accidents due to weather conditions. The present study focuses on modelling of the convective clouds development and thunder clouds detection on the basis of mesoscale atmospheric processes simulation, aiming at significantly improving the aeronautical forecast. In the analysis, the primary weather radar information has been used to be further adapted for mesoscale forecast systems. Two types of domains have been selected for modelling: an internal one (with radius of 8 km), and an external one (with radius of 300 km). The internal domain has been directly applied to study the local clouds development, and the external domain data has been treated as initial and final conditions for cloud cover formation. The domain height has been chosen according to the civil aviation forecast data (i.e. not exceeding 14 km). Simulations of weather conditions and local clouds development have been made within selected domains with the WRF modelling system. In several cases, thunderclouds are detected within the convective clouds. To specify the given category of clouds, we employ a simulation technique of solid phase formation processes in the atmosphere. Based on modelling results, we construct vertical profiles indicating the amount of solid phase in the atmosphere. Furthermore, we obtain profiles demonstrating the amount of ice particles and large particles (hailstones). While simulating the processes of solid phase formation, we investigate vertical and horizontal air flows. Consequently, we attempt to separate the total amount of solid phase into categories of small ice particles, large ice particles and hailstones. Also, we

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

International Nuclear Information System (INIS)

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

2015-01-01

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

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

Science.gov (United States)

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

2008-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

1984-05-01

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

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

Science.gov (United States)

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.

Sulfonated poly(styrene-divinylbenzene) modified with amines and the application for pipette-tip solid-phase extraction of carbendazim in apples.

Science.gov (United States)

Ma, Yuxin; Liu, Lingling; Tang, Weiyang; Zhu, Tao

2017-10-01

Sulfonated poly(styrene-divinylbenzene) modified with five kinds of amine functional groups was applied to the determination of carbendazim in apple samples with a pipette-tip solid-phase extraction method. The structures of the polymers were characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, and thermogravimetric analysis. Five different modifications of the solid-phase extraction sorbent based on sulfonated poly(styrene-divinylbenzene) were tested under static and pipette-tip solid-phase extraction conditions. The polymer modified with p-methoxyaniline showed the best recognition capacity and adsorption amount for carbendazim. Under the optimum conditions, 3.00 mg of the adsorbent, 1.00 mL of ethyl acetate as washing solvent, and 1.00 mL of ammonia/acetonitrile (5:95, v/v) as elution solvent were used in the pretreatment procedure of apple samples. The calibration graphs of carbendazim in methanol were linear over 5.00-200.00 μg/mL, and the limits of detection and quantification were 0.01 and 0.03 μg/mL, respectively. The method recoveries of carbendazim were in the range of 91.31-98.13% with associated intraday relative standard deviations of 0.76-2.13% and interday relative standard deviations of 1.10-1.85%. Sulfonated poly(styrene-divinylbenzene) modified with p-methoxyaniline showed satisfactory results (recovery: 97.96%) and potential for the rapid purification of carbendazim in apple samples combined with the pipette-tip solid-phase extraction. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Serum protein profiling by miniaturized solid-phase extraction and matrix-assisted laser desorption/ionization mass spectrometry

DEFF Research Database (Denmark)

Callesen, Anne K; Mohammed, Shabaz; Bunkenborg, Jakob

2005-01-01

for translation of MALDI-MS based diagnostic methods to clinical applications. We have investigated a number of MALDI matrices and several miniaturized solid-phase extraction (SPE) methods for serum protein concentration and desalting with the aim of generating reproducible, high-quality protein profiles by MALDI...

An Experimental Design Approach for the Analysis of Liquid Phase Products in Water for Hydrogenolysis of Glycerol using Immersed Solid-Phase Micro extraction

International Nuclear Information System (INIS)

Noraini Hamzah; Rozita Osman; Noraini Hamzah; Mohd Ambar Yarmo

2013-01-01

In this study, a response surface methodology (RSM) was applied to optimize the immersed-solid-phase micro extraction (immersed-SPME) conditions for the first time using a polyacrylate (PA) coated fiber. This was to determine liquid phase compounds in water for hydrogenolysis reaction of glycerol. There are a three-factor response surface experimental design was used to evaluate the interactive effects of extraction temperature (30-70 degree Celsius), extraction time (10-30 minutes) and desorption time (2-18 minutes) on the analysis of liquid phase compounds in water for hydrogenolysis of glycerol using immersed-solid-phase micro extraction (immersed-SPME). The extraction conditions using immersed-SPME were optimized in order to achieve high enrichment of the analytes from aqueous samples. The isolated compounds from the SPME fiber were desorbed and separated on a capillary polar column of a gas chromatography-flame ionization detector (GC-FID). The extraction time and desorption time were found significant in increasing the amount of glycerol in aqueous hydrogenolysis of glycerol. Nevertheless, the effect of extraction temperature was not significant. In terms of interactions between the effects, the relation between extraction temperature and extraction time was the most significant. The optimised immersed-SPME conditions were at extraction temperature of 27 degree Celsius, extraction time of 30 minutes and 15 minutes of desorption time. Thus, the application of SPME was found to be a rapid and effective technique in the determination of glycerol and propylene glycol compounds in aqueous hydrogenolysis glycerol. (author)

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

Science.gov (United States)

Bechtel, Jonathon S.; Van der Ven, Anton

2018-04-01

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

Chemical evolution of leaked high-level liquid wastes in Hanford soils

Energy Technology Data Exchange (ETDEWEB)

NYMAN,MAY D.; KRUMHANSL,JAMES L.; ZHANG,PENGCHU; ANDERSON,HOWARD L.; NENOFF,TINA M.

2000-05-19

A number of Hanford tanks have leaked high level radioactive wastes (HLW) into the surrounding unconsolidated sediments. The disequilibrium between atmospheric C0{sub 2} or silica-rich soils and the highly caustic (pH > 13) fluids is a driving force for numerous reactions. Hazardous dissolved components such as {sup 133}Cs, {sup 79}Se, {sup 99}Tc may be adsorbed or sequestered by alteration phases, or released in the vadose zone for further transport by surface water. Additionally, it is likely that precipitation and alteration reactions will change the soil permeability and consequently the fluid flow path in the sediments. In order to ascertain the location and mobility/immobility of the radionuclides from leaked solutions within the vadose zone, the authors are currently studying the chemical reactions between: (1) tank simulant solutions and Hanford soil fill minerals; and (2) tank simulant solutions and C0{sub 2}. The authors are investigating soil-solution reactions at: (1) elevated temperatures (60--200 C) to simulate reactions which occur immediately adjacent a radiogenically heated tank; and (2) ambient temperature (25 C) to simulate reactions which take place further from the tanks. The authors studies show that reactions at elevated temperature result in dissolution of silicate minerals and precipitation of zeolitic phases. At 25 C, silicate dissolution is not significant except where smectite clays are involved. However, at this temperature CO{sub 2} uptake by the solution results in precipitation of Al(OH){sub 3} (bayerite). In these studies, radionuclide analogues (Cs, Se and Re--for Tc) were partially removed from the test solutions both during high-temperature fluid-soil interactions and during room temperature bayerite precipitation. Altered soils would permanently retain a fraction of the Cs but essentially all of the Se and Re would be released once the plume was past and normal groundwater came in contact with the contaminated soil. Bayerite

Chemical evolution of leaked high-level liquid wastes in Hanford soils

International Nuclear Information System (INIS)

NYMAN, MAY D.; KRUMHANSL, JAMES L.; ZHANG, PENGCHU; ANDERSON, HOWARD L.; NENOFF, TINA M.

2000-01-01

A number of Hanford tanks have leaked high level radioactive wastes (HLW) into the surrounding unconsolidated sediments. The disequilibrium between atmospheric C0 2 or silica-rich soils and the highly caustic (pH > 13) fluids is a driving force for numerous reactions. Hazardous dissolved components such as 133 Cs, 79 Se, 99 Tc may be adsorbed or sequestered by alteration phases, or released in the vadose zone for further transport by surface water. Additionally, it is likely that precipitation and alteration reactions will change the soil permeability and consequently the fluid flow path in the sediments. In order to ascertain the location and mobility/immobility of the radionuclides from leaked solutions within the vadose zone, the authors are currently studying the chemical reactions between: (1) tank simulant solutions and Hanford soil fill minerals; and (2) tank simulant solutions and C0 2 . The authors are investigating soil-solution reactions at: (1) elevated temperatures (60--200 C) to simulate reactions which occur immediately adjacent a radiogenically heated tank; and (2) ambient temperature (25 C) to simulate reactions which take place further from the tanks. The authors studies show that reactions at elevated temperature result in dissolution of silicate minerals and precipitation of zeolitic phases. At 25 C, silicate dissolution is not significant except where smectite clays are involved. However, at this temperature CO 2 uptake by the solution results in precipitation of Al(OH) 3 (bayerite). In these studies, radionuclide analogues (Cs, Se and Re--for Tc) were partially removed from the test solutions both during high-temperature fluid-soil interactions and during room temperature bayerite precipitation. Altered soils would permanently retain a fraction of the Cs but essentially all of the Se and Re would be released once the plume was past and normal groundwater came in contact with the contaminated soil. Bayerite, however, will retain significant

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

Energy Technology Data Exchange (ETDEWEB)

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

2011-04-21

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

Dipole-Oriented Molecular Solids Can Undergo a Phase Change and Still Maintain Electrical Polarization

Energy Technology Data Exchange (ETDEWEB)

Glavic, Artur G [ORNL; Cassidy, Andrew M [ORNL; Jorgensen, Mads Ry Ry [University of Aarhus, Denmark; Lauter, Valeria [ORNL; Rosu-Finsen, Alexander [Heriot-Watt University, Edinburgh, UK; Lasne, Jérôme [Heriot-Watt University, Edinburgh, UK; Jorgensen, Jakob [Aarhus University, Denmark; Iversen, Bo [ORNL; McCoustra, Martin [Heriot-Watt University, Edinburgh, UK; Field, David [University of Aarhus, Denmark

2016-10-02

It has recently been demonstrated that nanoscale molecular films can spontaneously assemble to self-generate intrinsic electric fields that can exceed 10⁸ V/m. These electric fields originate from polarization charges in the material that arise because the films self-assemble to orient molecular dipole moments. This has been called the spontelectric effect. Such growth of spontaneously polarized layers of molecular solids has implications for our understanding of how intermolecular interactions dictate the structure of molecular materials used in a range of applications, for example, molecular semiconductors, sensors, and catalysts. In this paper, we present the first in situ structural characterization of a representative spontelectric solid, nitrous oxide. Infrared spectroscopy, temperature-programmed desorption, and neutron reflectivity measurements demonstrate that polarized films of nitrous oxide undergo a structural phase transformation upon heating above 48 K. A mean-field model can be used to describe quantitatively the magnitude of the spontaneously generated field as a function of film-growth temperature, and this model also recreates the phase change. Finally, this reinforces the spontelectric model as a means of describing long-range dipole–dipole interactions and points to a new type of ordering in molecular thin films.

Energy Harvesting, Electrode Processes and the Partitioning and Speciation of Solid Phase Iron and Sulfur in Marine Sediments

National Research Council Canada - National Science Library

Reimers, Clare

2003-01-01

.... Sediment, pore water and electrode surface analyses indicated that electricity product ion is coupled to the oxidation of dissolved and solid-phase forms of reduced sulfur supplied from the sediments...

Physicochemical investigation of Bi2MoO6 solid-phase interaction with Sm2MoO6

International Nuclear Information System (INIS)

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

1986-01-01

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

Solid Phases Precipitating in Artificial Urine in the Absence and Presence of Bacteria Proteus mirabilis—A Contribution to the Understanding of Infectious Urinary Stone Formation

Directory of Open Access Journals (Sweden)

Jolanta Prywer

2018-04-01

Full Text Available Magnesium ammonium phosphate hexahydrate, called struvite, is the dominant component of infectious urinary stones. In addition to struvite, infectious urinary stones include solid phases with poor crystallinity as well as amorphous matter. This article is devoted to the analysis of these solid phases, because they have not been characterized well until now. The solid phases tested were obtained from artificial urine in the absence and presence of Proteus mirabilis. The solid phases were characterized by different techniques (X-ray Diffraction, Energy Dispersive X-ray, Scanning Electron Microscopy, as well as Raman and Infrared Spectroscopies. According to the results these phases are carbonate apatite (CA, hydroxylapatite (HAP, amorphous calcium carbonate (ACC, amorphous calcium phosphate (ACP and/or amorphous carbonated calcium phosphate (ACCP. Carbonate apatite and hydroxylapatite may occur in non-stoichiometric forms, i.e., various anions can be substituted for CO32−, OH−, and PO43− groups in them. The non-stoichiometry of carbonate apatite and hydroxylapatite also implies a deficiency of calcium ions, i.e., calcium ions may be partially replaced by other cations. Experimental techniques and chemical speciation analysis demonstrate that the presence of magnesium influences the formation of CA and HAP.

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

International Nuclear Information System (INIS)

Song, Shaojie; Liu, Feng

2016-01-01

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

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

OpenAIRE

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

2014-01-01

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.

Design and control of a three-phase four-leg inverter for solid-state transformer applications

NARCIS (Netherlands)

Shri, A.; Popovic, J.; Ferreira, J.A.; Gerber, M.B.

2013-01-01

This paper proposes the use of a three-phase four-leg (3P4L) converter in combination with an LCL filter for the inverter stage of a solid state transformer (SST). This configuration gives full control over the line-to-line, as well as the line-to-neutral voltage and currents, while providing

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-02-01

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

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

International Nuclear Information System (INIS)

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

2009-01-01

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

High-order-harmonic generation from solids: The contributions of the Bloch wave packets moving at the group and phase velocities

Science.gov (United States)

Du, Tao-Yuan; Huang, Xiao-Huan; Bian, Xue-Bin

2018-01-01

We study numerically the Bloch electron wave-packet dynamics in periodic potentials to simulate laser-solid interactions. We introduce an alternative perspective in the coordinate space combined with the motion of the Bloch electron wave packets moving at group and phase velocities under the laser fields. This model interprets the origins of the two contributions (intra- and interband transitions) in the high-order harmonic generation (HHG) processes by investigating the local and global behaviours of the wave packets. It also elucidates the underlying physical picture of the HHG intensity enhancement by means of carrier-envelope phase, chirp, and inhomogeneous fields. It provides a deep insight into the emission of high-order harmonics from solids. This model is instructive for experimental measurements and provides an alternative avenue to distinguish mechanisms of the HHG from solids in different laser fields.

Study on Solid Phase Extraction and Spectrophotometric Determination of Nickel in Waters and Biological Samples

International Nuclear Information System (INIS)

Hu, Qiufen; Yang, Guangyu; Huang, Zhangjie; Yin, Jiayuan

2004-01-01

A sensitive, selective and rapid method for the determination of nickel based on the rapid reaction of nickel(II) with QADMAA and the solid phase extraction of the Ni(II)-QADMAA chelate with C 18 membrane disks has been developed. In the presence of pH 6.0 buffer solution and sodium dodecyl sulfonate (SDS) medium, QADMAA reacts with nickel to form a violet complex of a molar ratio of 1 : 2 (nickel to QADMAA). This chelate was enriched by solid phase extraction with C 18 membrane disks. An enrichment factor of 50 was obtained by elution of the chelates form the disks with the minimal amount of isopentyl alcohol. The molar absorptivity of the chelate was 1.32 x 10 5 L mol -1 cm -1 at 590 nm in the measured solution. Beer's law was obeyed in the range of 0.01-0.6 μg/mL. This method was applied to the determination of nickel in water and biological samples with good results

Numerical Thermodynamic Analysis of Two-Phase Solid-Liquid Abrasive Flow Polishing in U-Type Tube

Directory of Open Access Journals (Sweden)

Junye Li

2014-08-01

Full Text Available U-type tubes are widely used in military and civilian fields and the quality of the internal surface of their channel often determines the merits and performance of a machine in which they are incorporated. Abrasive flow polishing is an effective method for improving the channel surface quality of a U-type tube. Using the results of a numerical analysis of the thermodynamic energy balance equation of a two-phase solid-liquid flow, we carried out numerical simulations of the heat transfer and surface processing characteristics of a two-phase solid-liquid abrasive flow polishing of a U-type tube. The distribution cloud of the changes in the inlet turbulent kinetic energy, turbulence intensity, turbulent viscosity, and dynamic pressure near the wall of the tube were obtained. The relationships between the temperature and the turbulent kinetic energy, between the turbulent kinetic energy and the velocity, and between the temperature and the processing velocity were also determined to develop a theoretical basis for controlling the quality of abrasive flow polishing.

Fabrication of a Schottky junction diode with direct growth graphene on silicon by a solid phase reaction

International Nuclear Information System (INIS)

Kalita, Golap; Hirano, Ryo; Ayhan, Muhammed E; Tanemura, Masaki

2013-01-01

We demonstrate fabrication of a Schottky junction diode with direct growth graphene on n-Si by the solid phase reaction approach. Metal-assisted crystallization of a-C thin film was performed to synthesize transfer-free graphene directly on a SiO 2 patterned n-Si substrate. Graphene formation at the substrate and catalyst layer interface is achieved in presence of a Co catalytic and CoO carbon diffusion barrier layer. The as-synthesized material shows a linear current–voltage characteristic confirming the metallic behaviour of the graphene structure. The direct grown graphene on n-Si substrate creates a Schottky junction with a potential barrier of 0.44 eV and rectification diode characteristic. Our finding shows that the directly synthesized graphene on Si substrate by a solid phase reaction process can be a promising technique to fabricate an efficient Schottky junction device. (paper)