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Sample records for graphitic stationary phase

  1. Graphitic carbon nitride as high-resolution stationary phase for gas chromatographic separations.

    Science.gov (United States)

    Zheng, Yunzhong; Qi, Meiling; Fu, Ruonong

    2016-07-08

    This work presents the first example of utilization of graphitic carbon nitride (g-C3N4) as stationary phase for capillary gas chromatographic (GC) separations. The statically coated g-C3N4 column showed the column efficiencies of 3760 plates/m and weak polarity. Its resolving capability and retention behaviours were investigated by using the Grob test mixture, and mixtures of diverse types of analytes, and structural and positional isomers. The results showed superior separation performance of the g-C3N4 stationary phase for some critical analytes and preferential retention for aromatic analytes. Specifically, it exhibited high-resolution capability for aromatic and aliphatic isomers such as methylnaphthalenes and dimethylnaphthalenes, phenanthrene and anthracene and alkane isomers. In addition, g-C3N4 column showed excellent thermal stability up to 280°C and good repeatability with relative standard deviation (RSD) values less than 0.09% for intra-day, below 0.23% for inter-day and in the range of 1.9-8.4% for between-column, respectively. The advantageous separation performance shows the potential of g-C3N4 and related materials as stationary phase in GC and other separation technologies. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Carbon nanotube stationary phases for microchip electrochromatography

    DEFF Research Database (Denmark)

    Mogensen, Klaus Bo; Bøggild, Peter; Kutter, Jörg Peter

    The use of nanomaterials in separation science has increased rapidly in the last decade. The reason for this is to take advantage of the unique properties of these materials, such as a very high surface-to-volume ratio and favourable sorbent behaviour. Carbon nanostructures, such as carbon...... surface can furthermore be used directly as a stationary phase in reverse-phase separations, thereby avoiding subsequent functionalization of the nanostructures. This significantly reduces the fabrication time and possibly also increases the reproducibility of the column performance. In this presentation......, microfluidic devices with microfabricated carbon nanotube columns for electrochromatographic separations will be presented. The electrically conductive carbon nanotube layer has been patterned into hexoganol micropillars in order to support electroosmotic flow without forming gas bubbles from electrolysis...

  3. Stationary phases for superheated water chromatography

    CERN Document Server

    Saha, S

    2002-01-01

    This project focused on the comparison of conventional liquid chromatography and superheated water chromatography. It examined the differences in efficiency and retention of a range of different stationary phases. Alkyl aryl ketones and eight aromatic compounds were separated on PBD-zirconia, Xterra RP 18, Luna C sub 1 sub 8 (2) and Oasis HLB columns using conventional LC and superheated water chromatography system. The retention indices were determined in the different eluents. On changing the organic component of the eluent from methanol to acetonitrile to superheated water considerable improvements were found in the peak shapes and column efficiencies on the PBD-zirconia and Oasis HLB columns. PS-DVB, PBD-zirconia and Xterra RP 18 columns have been used in efficiency studies. It was found that simply elevating the column temperature did not increase the efficiency of a separation in superheated water chromatography. The efficiency depended on flow rate, injection volume and also mobile phase preheating sys...

  4. Liquid Crystals as Stationary Phases in Chromatography.

    Science.gov (United States)

    Grajek, H; Witkiewicz, Z; Purchała, M; Drzewiński, W

    2016-01-01

    The most correct analysis of the compositions of diverse analytes mixtures is significant for analytical studies in different fields; however, many prevalent analytes cannot be identified employing traditional partition gas chromatographic methods. Thus, the increasing requirements on analytes of isomeric compounds and the problems encountered in their separation demand a study of more diverse analytical systems which are characterised by higher selectivity. Therefore, the selectivity and polarities of various liquid crystals (rod-like, banana-shape, biforked, oxygen, sulphur, nitrogen, and metal containing molecules, Schiff-base, and polymeric dendrimers) employed as liquid crystalline stationary phases (LCSPs) have been discussed from both points of views, namely, their analytical applications and thermodynamic characteristics of infinitely diluted probes with different acceptor-donor properties. Extreme particular effort has been paid to the different interdependencies between the bound up chemical structures of liquid crystal molecules with their different acceptor-donor properties and the connected resolution capabilities in the interpretation of the probe-LCSP systems, on the basis of the [Formula: see text] and [Formula: see text] dependencies, with regard to the LCSP compositions, which have been controlled by the counterbalancing of the enthalpy and entropy factors. The properties of binary systems composed of liquid crystalline poly(propyleneimine) dendrimers-rod-like molecules of liquid crystals and effects of the dendrimer structure, the chemical nature, and molecular size of the non-mesogens on the ability to dissolve in the liquid crystalline phases, have been interpreted. Practical applications of metallomesogenes and chiral stationary phases for analytical separation of different organic substances have also been taken into consideration.

  5. Low temperature vapor phase digestion of graphite

    Energy Technology Data Exchange (ETDEWEB)

    Pierce, Robert A.

    2017-04-18

    A method for digestion and gasification of graphite for removal from an underlying surface is described. The method can be utilized to remove graphite remnants of a formation process from the formed metal piece in a cleaning process. The method can be particularly beneficial in cleaning castings formed with graphite molding materials. The method can utilize vaporous nitric acid (HNO.sub.3) or vaporous HNO.sub.3 with air/oxygen to digest the graphite at conditions that can avoid damage to the underlying surface.

  6. Recent development of ionic liquid stationary phases for liquid chromatography.

    Science.gov (United States)

    Shi, Xianzhe; Qiao, Lizhen; Xu, Guowang

    2015-11-13

    Based on their particular physicochemical characteristics, ionic liquids have been widely applied in many fields of analytical chemistry. Many types of ionic liquids were immobilized on a support like silica or monolith as stationary phases for liquid chromatography. Moreover, different approaches were developed to bond covalently ionic liquids onto the supporting materials. The obtained ionic liquid stationary phases show multi-mode mechanism including hydrophobic, hydrophilic, hydrogen bond, anion exchange, π-π, and dipole-dipole interactions. Therefore, they could be used in different chromatographic modes including ion-exchange, RPLC, NPLC and HILIC to separate various classes of compounds. This review mainly summarizes the immobilized patterns and types of ionic liquid stationary phases, their retention mechanisms and applications in the recent five years. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Immobilized strychnine as a new chiral stationary phase for HPLC.

    Science.gov (United States)

    Sýkora, David; Vozka, Jiří; Tesařová, Eva; Kalíková, Květa; Havlík, Martin; Matějka, Pavel; Král, Vladimír

    2017-08-01

    A new ion-exchanger type chiral stationary phase for high-performance liquid chromatography was prepared. The synthetic protocol is based on derivatization of silica with (3-iodopropyl)trimethoxysilane in the first step followed by immobilization of strychnine via quaternization of nitrogen atom of the alkaloid strychnine. The synthesized chiral stationary phase was chromatographically characterized. The main effort was headed towards the evaluation of the enantioselectivity of the novel sorbent. For that purpose a set of suitable chiral probes, specifically, binaphthyl derivatives, was employed. The influence of methanol content, concentration of aqueous ammonium acetate buffer, and its pH on retention factors, separation selectivity, and resolution of the atropoisomers of the mentioned chiral solutes was studied in detail. It was demonstrated that the new chiral stationary phase was capable to separate atropoisomers of four out of seven testing compounds. Despite the strong influence of the above mentioned variables on retention, their impact on selectivity and resolution was rather moderate. Concerning retention mechanism, it seems that electrostatic interaction between the positively charged quaternary nitrogen of the chiral stationary phase and anionic solute participates significantly in the retention process. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Accumulation of hns mutations specifically in stationary phase in an ...

    Indian Academy of Sciences (India)

    + mutation profile in another control strain. These results suggest a positive selection for hns muta- tions when rpoS function is compromised and occurs specif- ically in the stationary phase. The strains used were iso- genic and differed only at the rpoS and tnaA loci that carried the transposon Tn10. No interaction between ...

  9. Accumulation of hns mutations specifically in stationary phase in an ...

    Indian Academy of Sciences (India)

    Accumulation of hns mutations specifically in stationary phase in an. E. coli strain carrying an impaired rpoS locus. STUTI K. DESAI and S. MAHADEVAN∗. Department of Molecular Reproduction, Development and Genetics, Indian Institute of Science,. Bangalore 560 012, India. Introduction. Interplay between regulators in ...

  10. Magnetic and Structural Phases of Monolayer 02 on Graphite

    DEFF Research Database (Denmark)

    McTague, J. P.; Nielsen, Mourits

    1976-01-01

    Neutron diffraction studies of O2 thin films physisorbed on the basal plane of graphite show three distinct two-dimensional crystalline phases, all incommensurate with the substrate lattice. The low-temperature monolayer phase has a distorted triangular structure analogous to the closest...

  11. Separation of flavonoids on different phenyl-bonded stationary phases-the influence of polar groups in stationary phase structure.

    Science.gov (United States)

    Janas, Petr; Bocian, Szymon; Jandera, Pavel; Kowalkowski, Tomasz; Buszewski, Bogusław

    2016-01-15

    Four phenyl-bonded stationary phases, differing in polar embedded group between spacer and phenyl ring, were used for the separation of flavonoids in reversed-phase conditions. In addition, the work was focused on the comparison of these stationary phases in terms of retention and nature of interactions between flavonoid solutes and both, mobile and stationary phases. The differences and similarities between the columns and between individual flavonoids were evaluated by a statistical analysis. The retention over the wider range of mobile phase composition was described using well known model suggested for partition chromatographic systems. Due to differences in polarity of flavonoids, gradient elution had to be applied to achieve appropriate conditions for the successful separation. A chromatographic optimization software was employed for establish the appropriate profiles of gradient separations using UV detection at 275 nm. The most appropriate conditions for the separation of flavonoids were apparent on the phenyl and phenoxy columns. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Graphite

    Science.gov (United States)

    Robinson, Gilpin R.; Hammarstrom, Jane M.; Olson, Donald W.; Schulz, Klaus J.; DeYoung,, John H.; Seal, Robert R.; Bradley, Dwight C.

    2017-12-19

    Graphite is a form of pure carbon that normally occurs as black crystal flakes and masses. It has important properties, such as chemical inertness, thermal stability, high electrical conductivity, and lubricity (slipperiness) that make it suitable for many industrial applications, including electronics, lubricants, metallurgy, and steelmaking. For some of these uses, no suitable substitutes are available. Steelmaking and refractory applications in metallurgy use the largest amount of produced graphite; however, emerging technology uses in large-scale fuel cell, battery, and lightweight high-strength composite applications could substantially increase world demand for graphite.Graphite ores are classified as “amorphous” (microcrystalline), and “crystalline” (“flake” or “lump or chip”) based on the ore’s crystallinity, grain-size, and morphology. All graphite deposits mined today formed from metamorphism of carbonaceous sedimentary rocks, and the ore type is determined by the geologic setting. Thermally metamorphosed coal is the usual source of amorphous graphite. Disseminated crystalline flake graphite is mined from carbonaceous metamorphic rocks, and lump or chip graphite is mined from veins in high-grade metamorphic regions. Because graphite is chemically inert and nontoxic, the main environmental concerns associated with graphite mining are inhalation of fine-grained dusts, including silicate and sulfide mineral particles, and hydrocarbon vapors produced during the mining and processing of ore. Synthetic graphite is manufactured from hydrocarbon sources using high-temperature heat treatment, and it is more expensive to produce than natural graphite.Production of natural graphite is dominated by China, India, and Brazil, which export graphite worldwide. China provides approximately 67 percent of worldwide output of natural graphite, and, as the dominant exporter, has the ability to set world prices. China has significant graphite reserves, and

  13. Kinetic performance of stationary phases for gas chromatography based on poly(oligoethyleneglycoldiacrylate).

    Science.gov (United States)

    Korolev, A; Shyrayeva, V; Popova, T; Kanateva, A; Kurganov, A

    2016-08-19

    Open capillary columns with polymeric stationary phases based on poly(oligoethyleneglycoldiacrylate) were prepared and tested on their kinetic performance. Stationary phases prepared with low molar mass monomers were inferior to stationary phases based on high molar mass monomers. Structure of these stationary phases appeared to be favorable for solute diffusion in the stationary phase. These columns were also characterized by improved kinetic performance limit. Stationary phase based on poly(ethylenglycol) and prepared according to the traditional procedure, demonstrated average kinetic performance. Optimal kinetic performance limit curves characterizing the prepared stationary phases were evaluated in this work using new simple procedure based on extraction of optimal values from the corresponding matrix. This technique makes it possible to evaluate optimal kinetic performance limit curves without any additional simplifications and cumbersome calculations. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. The novel reentrant fluid phase of HD physisorbed on graphite

    Energy Technology Data Exchange (ETDEWEB)

    Leinboeck, B.; Wiechert, H. [Mainz Univ., Mainz (Germany); Bienfait, M. [Centre Universitaire de Luminy, Aix-Marseille-2 Univ., 13 - Marseille (France); Johnson, M. [Institut Max von Laue - Paul Langevin (ILL), 38 - Grenoble (France)

    1999-11-01

    Quasielastic neutron-scattering measurements have been carried out on the backscattering spectrometer IN10 to gain new insight into the nature of the novel reentrant fluid phase occurring at the commensurate-incommensurate transition of deuterium hybrid (HD) monolayers physisorbed on the basal planes of graphite. Our high energy-resolution measurements show, for the first time, that translational particle mobility occurs in the reentrant fluid phase. This observation is consistent with the theory of the commensurate-incommensurate transition which predicts that the phase is a viscous fluid which can be characterised by thermally fluctuating striped domain walls separating commensurate micro-domains. (authors) 7 refs., 3 figs.

  15. Thermophysical properties estimation of paraffin/graphite composite phase change material using an inverse method

    International Nuclear Information System (INIS)

    Lachheb, Mohamed; Karkri, Mustapha; Albouchi, Fethi; Mzali, Foued; Nasrallah, Sassi Ben

    2014-01-01

    Highlights: • Preparation of paraffin/graphite composites by uni-axial compression technique. • Measurement of thermophysical properties of paraffin/graphite using the periodic method. • Measurement of the experimental densities of paraffin/graphite composites. • Prediction of the effective thermal conductivity using analytical models. - Abstract: In this paper, two types of graphite were combined with paraffin in an attempt to improve thermal conductivity of paraffin phase change material (PCM): Synthetic graphite (Timrex SFG75) and graphite waste obtained from damaged Tubular graphite Heat Exchangers. These paraffin/graphite phase change material (PCM) composites are prepared by the cold uniaxial compression technique and the thermophysical properties were estimated using a periodic temperature method and an inverse technique. Results showed that the thermal conductivity and thermal diffusivity are greatly influenced by the graphite addition

  16. Product Evaluation Task Force Phase Two report for CAGR graphite

    International Nuclear Information System (INIS)

    Francis, A.J.; Davies, A.

    1991-01-01

    It has been proposed that all Intermediate Level Wastes arising at Sellafield should be encapsulated prior to ultimate disposal. The Product Evaluation Task Force (PETF) was set up to investigate possible encapsulants and to produce an adequate data base to justify the preferred matrices. This report details the work carried out under Phase 2 of the Product Evaluation Task Force programme, on CAGR graphite. Three possible types of encapsulants for CAGR graphites:-Inorganic cements, Polymer cements and Polymers are evaluated using the Kepner Tregoe decision analysis technique. This technique provides a methodology for scoring and ranking alternative options and evaluating any risks associated with an option. The analysis shows that for all four stages of waste management operations ie Storage, Transport, handling and emplacement, Disposal and Process, cement matrices are considerably superior to other potential matrices. A matrix, consisting of three parts Blast Furnace Slag (BFS) to one part Ordinary Portland Cement (OPC) is recommended as the preferred matrix for Phase 3 studies on CAGR graphite. (author)

  17. Study of Stationary Phase Metabolism Via Isotopomer Analysis of Amino Acids from an Isolated Protein

    Energy Technology Data Exchange (ETDEWEB)

    Shaikh, AfshanS.; Tang, YinjieJ.; Mukhopadhyay, Aindrila; Martin, Hector Garcia; Gin, Jennifer; Benke, Peter; Keasling, Jay D.

    2009-09-14

    Microbial production of many commercially important secondary metabolites occurs during stationary phase, and methods to measure metabolic flux during this growth phase would be valuable. Metabolic flux analysis is often based on isotopomer information from proteinogenic amino acids. As such, flux analysis primarily reflects the metabolism pertinent to the growth phase during which most proteins are synthesized. To investigate central metabolism and amino acids synthesis activity during stationary phase, addition of fully 13C-labeled glucose followed by induction of green fluorescent protein (GFP) expression during stationary phase was used. Our results indicate that Escherichia coli was able to produce new proteins (i.e., GFP) in the stationary phase, and the amino acids in GFP were mostly from degraded proteins synthesized during the exponential growth phase. Among amino acid biosynthetic pathways, only those for serine, alanine, glutamate/glutamine, and aspartate/asparagine had significant activity during the stationary phase.

  18. Population Dynamics of the Stationary Phase Utilizing the ARGOS Method

    Science.gov (United States)

    Algarni, S.; Charest, A. J.; Iannacchione, G. S.

    2015-03-01

    The Area Recorded Generalized Optical Scattering (ARGOS) approach to light scattering employs large image capture array allowing for a well-defined geometry in which images may be manipulated to extract structure with intensity at a specific scattering wave vector (I(q)) and dynamics with intensity at a specific scattering wave vector over time (I (q,t)). The ARGOS method provides morphological dynamics noninvasively over a long time period and allows for a variety of aqueous conditions. This is important because traditional growth models do not provide for conditions similar to the natural environment. The present study found that the population dynamics of bacteria do not follow a traditional growth model and that the ARGOS method allowed for the observation of bacterial changes in terms of individual particles and population dynamics in real time. The observations of relative total intensity suggest that there is no stationary phase and that the bacterial population demonstrates sinusoidal type patterns consistently subsequent to the log phase growth. These observation were compared to shape changes by modeling fractal dimension and size changes by modeling effective radius.

  19. A new methodology to determine the isoeluotropic conditions on ultra-performance flash purification stationary phases from analytical reversed liquid chromatography stationary phase.

    Science.gov (United States)

    Héron, Sylvie; Charbonneau, Didier; Albisson, Pauline; Estievenart, Guillaume; Groni, Sihem; Tchapla, Alain

    2015-06-05

    Nowadays, the determination of the experimental chromatographic conditions to be used in Reversed Phase Liquid Ultra-Performance Flash Purification is still challenging. This is due to four different items. In most cases, flash purification stationary phases are not available with geometry of column used in analytical chromatography. The flash purification columns are single-use only. From the point of view of selectivity and retention, few RPLC phases exist with properties of separation identical for analytical and flash purification supports. Characterization methods and databases used for comparing analytical RPLC columns do not include stationary phases for RP flash purification columns. The goal of this work is to develop a new method development strategy which permits the determination of the experimental chromatographic conditions on RP ultra-performance flash purification columns. It relies on the knowledge of any isocratic conditions obtained on any given initial reversed stationary phase. The final conditions to implement on the RP ultra-performance flash purification phase enable either to keep the retention range of a selected solute constant, or to set it around a previously chosen value. The rules of transfer in linear gradient mode are also described. The methodology was valid, whatever the initial RP stationary and mobile phases, for different chemical classes, whatever the bonding, particle diameter, porous or core shell particle, towards different RP alkyl and analogues stationary and mobile phases. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. An integrated fritless column for on-chip capillary electrochromatography with conventional stationary phases

    NARCIS (Netherlands)

    Ceriotti, Laura; De Rooij, Nico F.; Verpoorte, Elisabeth

    2002-01-01

    A new polymer device for use with conventional particulate stationary phases for on-chip, fritless, capillary electrochromatography (CEC) has been realized. The structure includes an injector and a tapered column in which the particles of the stationary phase are retained and stabilized. The chips

  1. The method of stationary phase and the method of Fresnel zones

    NARCIS (Netherlands)

    Kampen, N.G. van

    1958-01-01

    The method of stationary phase is discussed and reasons are given why it is often preferable to the method of steepest descent, in spite of the mathematicians' partiality to the latter. The method of Fresnel zones is compared with the method of stationary phase and is shown to be a primitive version

  2. Phase diagram of the CF₄ monolayer and bilayer on graphite.

    Science.gov (United States)

    Thomas, Petros; Hess, George B

    2014-05-21

    We report an experimental study of physisorbed monolayers and bilayers of CF4 on graphite using infrared reflection absorption spectroscopy supplemented by ellipsometry. The symmetric C-F stretch mode ν3 near 1283 cm(-1) in the gas is strongly blue shifted in the film by dynamic dipole coupling. This blue shift provides a very sensitive measure of the inter-molecular spacing in the monolayer and, less directly, in the bilayer. We find that important corrections are necessary to the volumetric coverage scales used in previous heat capacity and x-ray diffraction studies of this system. This requires quantitative and some qualitative changes to the previously proposed phase diagram. We find evidence for a new phase transition in the middle of the hexagonal incommensurate region and construct new phase diagrams in both the variables coverage-temperature and chemical potential-temperature. We determine the compressibility and thermal expansion in the low-pressure hexagonal incommensurate phase and values for the entropy change in several phase transitions. Below about 55 K there is evidence of solution of up to 7% of an impurity, most likely CO, in our monolayer but not the bilayer film.

  3. Ceramic stationary gas turbine development. Final report, Phase 1

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1994-09-01

    This report summarizes work performed by Solar Turbines Inc. and its subcontractors during the period September 25, 1992 through April 30, 1993. The objective of the work is to improve the performance of stationary gas turbines in cogeneration through implementation of selected ceramic components.

  4. The proteomics of quiescent and nonquiescent cell differentiation in yeast stationary-phase cultures.

    Science.gov (United States)

    Davidson, George S; Joe, Ray M; Roy, Sushmita; Meirelles, Osorio; Allen, Chris P; Wilson, Melissa R; Tapia, Phillip H; Manzanilla, Elaine E; Dodson, Anne E; Chakraborty, Swagata; Carter, Mark; Young, Susan; Edwards, Bruce; Sklar, Larry; Werner-Washburne, Margaret

    2011-04-01

    As yeast cultures enter stationary phase in rich, glucose-based medium, differentiation of two major subpopulations of cells, termed quiescent and nonquiescent, is observed. Differences in mRNA abundance between exponentially growing and stationary-phase cultures and quiescent and nonquiescent cells are known, but little was known about protein abundance in these cells. To measure protein abundance in exponential and stationary-phase cultures, the yeast GFP-fusion library (4159 strains) was examined during exponential and stationary phases, using high-throughput flow cytometry (HyperCyt). Approximately 5% of proteins in the library showed twofold or greater changes in median fluorescence intensity (abundance) between the two conditions. We examined 38 strains exhibiting two distinct fluorescence-intensity peaks in stationary phase and determined that the two fluorescence peaks distinguished quiescent and nonquiescent cells, the two major subpopulations of cells in stationary-phase cultures. GFP-fusion proteins in this group were more abundant in quiescent cells, and half were involved in mitochondrial function, consistent with the sixfold increase in respiration observed in quiescent cells and the relative absence of Cit1p:GFP in nonquiescent cells. Finally, examination of quiescent cell-specific GFP-fusion proteins revealed symmetry in protein accumulation in dividing quiescent and nonquiescent cells after glucose exhaustion, leading to a new model for the differentiation of these cells.

  5. Novel open tubular CEC with tentacle-type polymer stationary phase functionalized by phenylalanine.

    Science.gov (United States)

    Xu, Liang; Sun, Yan

    2008-02-01

    A novel stationary phase with tentacle-type polymer chains with epoxy groups was fabricated for open tubular CEC. The fabrication procedure of the stationary phase included pretreatment of capillary inner wall, silanization, and glycidyl methacrylate (GMA)-grafted polymerization. The influence of initiator concentration and polymerization time on the resulting polymer stationary phase was studied by measuring EOF mobility and hydrophobicity of the prepared capillary column. SEM showed that the capillary inner wall was evenly coated with a polymer film showing a wrinkly surface. The prepared GMA-grafted stationary phase could be easily modified with different chromatographic ligands by the ring-opening reaction of the epoxy groups. In this study, phenylalanine (Phe) was selected as the ligand. Benzene derivatives and three amino acids were then separated, respectively, using the Phe modified tentacle-type capillary column. As a control, separations were also performed on a monolayer Phe-modified capillary. The tentacle-type polymer stationary phase was found affording stronger retention and better resolution in the separation of benzene derivatives and tryptophan, tyrosine, and Phe mixtures compared with the monolayer stationary phase.

  6. Graphite electrode arc melter demonstration Phase 2 test results

    Energy Technology Data Exchange (ETDEWEB)

    Soelberg, N.R.; Chambers, A.G.; Anderson, G.L.; O`Connor, W.K.; Oden, L.L.; Turner, P.C.

    1996-06-01

    Several U.S. Department of Energy organizations and the U.S. Bureau of Mines have been collaboratively conducting mixed waste treatment process demonstration testing on the near full-scale graphite electrode submerged arc melter system at the Bureau`s Albany (Oregon) Research Center. An initial test series successfully demonstrated arc melter capability for treating surrogate incinerator ash of buried mixed wastes with soil. The conceptual treatment process for that test series assumed that buried waste would be retrieved and incinerated, and that the incinerator ash would be vitrified in an arc melter. This report presents results from a recently completed second series of tests, undertaken to determine the ability of the arc melter system to stably process a wide range of {open_quotes}as-received{close_quotes} heterogeneous solid mixed wastes containing high levels of organics, representative of the wastes buried and stored at the Idaho National Engineering Laboratory (INEL). The Phase 2 demonstration test results indicate that an arc melter system is capable of directly processing these wastes and could enable elimination of an up-front incineration step in the conceptual treatment process.

  7. Graphite electrode arc melter demonstration Phase 2 test results

    International Nuclear Information System (INIS)

    Soelberg, N.R.; Chambers, A.G.; Anderson, G.L.; O'Connor, W.K.; Oden, L.L.; Turner, P.C.

    1996-06-01

    Several U.S. Department of Energy organizations and the U.S. Bureau of Mines have been collaboratively conducting mixed waste treatment process demonstration testing on the near full-scale graphite electrode submerged arc melter system at the Bureau's Albany (Oregon) Research Center. An initial test series successfully demonstrated arc melter capability for treating surrogate incinerator ash of buried mixed wastes with soil. The conceptual treatment process for that test series assumed that buried waste would be retrieved and incinerated, and that the incinerator ash would be vitrified in an arc melter. This report presents results from a recently completed second series of tests, undertaken to determine the ability of the arc melter system to stably process a wide range of open-quotes as-receivedclose quotes heterogeneous solid mixed wastes containing high levels of organics, representative of the wastes buried and stored at the Idaho National Engineering Laboratory (INEL). The Phase 2 demonstration test results indicate that an arc melter system is capable of directly processing these wastes and could enable elimination of an up-front incineration step in the conceptual treatment process

  8. Evaluating the robustness of the enantioselective stationary phases on the Rosetta mission against space vacuum vaporization

    Science.gov (United States)

    Meierhenrich, Uwe J.; Cason, Julie R. L.; Szopa, Cyril; Sternberg, Robert; Raulin, François; Thiemann, Wolfram H.-P.; Goesmann, Fred

    2013-12-01

    The European Space Agency's Rosetta mission was launched in March 2004 in order to reach comet 67P/Churyumov-Gerasimenko by August 2014. The Cometary Sampling and Composition experiment (COSAC) onboard the Rosetta mission's lander "Philae" has been designed for the cometary in situ detection and quantification of organic molecules using gas chromatography coupled to mass spectrometry (GC-MS). The GC unit of COSAC is equipped with eight capillary columns that will each provide a specific stationary phase for molecular separation. Three of these stationary phases will be used to chromatographically resolve enantiomers, as they are composed of liquid polymers of polydimethylsiloxane (PDMS) to which chiral valine or cyclodextrin units are attached. Throughout the ten years of Rosetta's journey through space to reach comet 67P, these liquid stationary phases have been exposed to space vacuum, as the capillary columns within the COSAC unit were not sealed or filled with carrier gas. Long term exposures to space vacuum can cause damage to such liquid stationary phases as key monomers, volatiles, and chiral selectors can be vaporized and lost in transit. We have therefore exposed identical spare units of COSAC's chiral stationary phases over eight years to vacuum conditions mimicking those experienced in space and we have now investigated their resolution capabilities towards different enantiomers both before and after exposure to space vacuum environments. We have observed that enantiomeric resolution capabilities of these chiral liquid enantioselective stationary phases has not been affected by exposure to space vacuum conditions. Thus we conclude that the three chiral stationary phases of the COSAC experiment onboard the Rosetta mission lander "Philae" can be considered to have maintained their resolution capacities throughout their journey prior to cometary landing in November 2014.

  9. A new 14-membered tetraazamacrocycle-bonded silica stationary phase for reversed-phase high-performance liquid chromatography.

    Science.gov (United States)

    He, Lijun; Zhang, Mingliang; Zhao, Wenjie; Liu, Jie; Jiang, Xiuming; Zhang, Shusheng; Qu, Lingbo

    2012-01-30

    A new high-performance liquid chromatography stationary phase has been prepared by covalently bonding 14-membered tetraazamacrocycle to silica gel using γ-chloropropyltrimethoxylsilane as coupling agent. The structure of the new material was characterized by infrared spectroscopy and elemental analysis. With 32 solutes including aromatic and aliphatic compounds, the linear solvation energy relationship method was successfully used to chromatographically evaluate the new phase in reversed phase mode. The retention property of the new phase shows evident similarity with that of ODS stationary phase, as well as distinctive, unique retention characteristics. The separations of n-alkylbenzene, carbamate and organophosphorus pesticides with diversified functional groups as well as phenolic compounds demonstrate that in addition to hydrophobic interaction, dipole-dipole interaction and hydrogen bonding interaction plus acid-base equilibrium could also be simultaneously offered by this new stationary phase, as a result excellent chromatographic performances are guaranteed. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. A Nanotube Surface Reinforced Graphite Fiber Exhibiting Significantly Enhanced Properties, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — The completed Phase I work was directed at the application of nanotechnology to graphite/epoxy composites. A novel approach to the application of the nanotubes onto...

  11. Surface Modification of Exfoliated Graphite Nano-Reinforcements, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Nano forms of graphite and carbon, such as flakes, worms, and tubes, can significantly modify the properties of polymers when used as reinforcements. Challenges...

  12. Evaluation of gamma radiation effects on stationary phases using gas chromatografy

    International Nuclear Information System (INIS)

    Basso, M.A.; Collins, K.E.; Collins, C.H.

    1988-01-01

    The overall objetive of this project is a thorough study of the effect of gamma radiation on supported stationary phases used in packed-column gas chromatography. The phases studied were SP-2100 on Supelcoport and SE-30 on Chromsorb W. The fases were irradiated with cobalt-60 gamma rays to various doses and subsequently subjected to tests of extractability, termal stability and efficiency as a chromatographic column packing. Extraction tests indicate that low doses of radiation are sufficient to produce significant immobilization of these polymethylsilicones; that is, to produce chemical bonds between different polymer chains or between the stationary phase and the support. Thermal stability is also increased. The values calculated for the number of theoretical plates (n) and resolution (Rsub (s)) after analysis of four synthetic mixtures of organic compounds also increase, in most cases, indicating that the gamma irradiation has positively altered the behavior of these stationary phases. (author) [pt

  13. Comparison of GC stationary phases for the separation of fatty acid methyl esters in biodiesel fuels.

    Science.gov (United States)

    Goding, Julian C; Ragon, Dorisanne Y; O'Connor, Jack B; Boehm, Sarah J; Hupp, Amber M

    2013-07-01

    The fatty acid methyl ester (FAME) content of biodiesel fuels has traditionally been determined using gas chromatography with a polar stationary phase. In this study, a direct comparison of the separation of FAMEs present in various biodiesel samples on three polar stationary phases and one moderately polar stationary phase (with comparable column dimensions) was performed. Retention on each column was based on solubility in and polarity of the phase. Quantitative metrics describing the resolution of important FAME pairs indicate high resolution on all polar columns, yet the best resolution, particularly of geometric isomers, is achieved on the cyanopropyl column. In addition, the separation of four C18 monounsaturated isomers was optimized and the elution order determined on each column. FAME composition of various biodiesel fuel types was determined on each column to illustrate (1) chemical differences in biodiesels produced from different feedstocks and (2) chemical similarities in biodiesels of the same feedstock type produced in different locations and harvest seasons.

  14. Evaluation of hydrophilic interaction liquid chromatography stationary phases for analysis of opium alkaloids.

    Science.gov (United States)

    Bagheri, Mohsen; Taheri, Mohammadreza; Farhadpour, Mohsen; Rezadoost, Hassan; Ghassempour, Alireza; Aboul-Enein, Hassan Y

    2017-08-18

    The separation of a mixture containing five major opium alkaloids, namely morphine, codeine, thebaine, noscapine and papaverine has been investigated in hydrophilic interaction liquid chromatography (HILIC) mode using five different stationary phases: bare silica, zwitterion, aminopropyl, diol and cyanopropyl. In order to propose the appropriate column for separation and purification, retention behaviors of the five natural opioids have been studied on mentioned HILIC stationary phases. The mechanism of separation in diverse HILIC media, based on the formation of water-rich layer on surface of the HILIC stationary phases and the physicochemical properties of opium alkaloids, such as pKa (acidic pK) and the octanol-water distribution coefficient (log Do/w) are discussed. Chromatographic responses including modified limit of detection LOD m , signal to noise ratio (S/N) m , and defined modified R Sm have considered for suggestion of the suitable column for quantitative/qualitative and preparative purposes. According to the obtained results, diol stationary phase is best suited for analytical chromatography, whereas bare silica and zwitterionic stationary phases are appropriate for preparative applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Enantiomeric Resolution of Drugs and Metabolites in Polysaccharide- and Protein-Based Chiral Stationary Phases

    Directory of Open Access Journals (Sweden)

    Bonato Pierina S.

    2002-01-01

    Full Text Available Several chiral stationary phases based on polysaccharide derivatives and proteins were evaluated for the resolution of some chiral drugs and their metabolites. The polysaccharide-based stationary phases CHIRALCEL OD-H, CHIRALCEL OB-H, CHIRALCEL OJ, CHIRALPAK AD and CHIRALPAK AS were evaluated under normal phase conditions, using hexane:2-propanol or hexane:ethanol as mobile phase. Diethylamine and trifluoracetic acid were also added to improve peak shape. The CHIRALCEL OJ-R, CHIRALCEL OD-R and CHIRALCEL OD-H columns were evaluated under reversed-phase conditions, using acetonitrile:H2O or acetonitrile:NaClO4 solution. The protein- based stationary phases, CHIRAL AGP and ULTRON ES-OVM columns were used with mobile phases consisting of a buffer solution supplemented with an organic modifier. Among the polysaccharide-based stationary phases, CHIRALPAK AD provided better resolution for almost all drugs and metabolites studied. The ULTRON ES-OVM column was particularly suitable for the resolution of the four enantiomers of thioridazine-2-sulfoxide.

  16. Metal-Organic Framework Thin Films as Stationary Phases in Microfabricated Gas-Chromatography Columns.

    Energy Technology Data Exchange (ETDEWEB)

    Read, Douglas [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Sillerud, Colin Halliday [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2016-01-01

    The overarching goal of this project is to integrate Sandia's microfabricated gas-chromatography ( GC) columns with a stationary phase material that is capable of retaining high-volatility chemicals and permanent gases. The successful integration of such a material with GCs would dramatically expand the repertoire of detectable compounds for Sandia's various microanalysis systems. One such promising class of candidate materials is metal-organic frameworks (MOFs). In this report we detail our methods for controlled deposition of HKUST-1 MOF stationary phases within GC columns. We demonstrate: the chromatographic separation of natural gas; a method for determining MOF film thickness from chromatography alone; and the first-reported GC x GC separation of natural gas -- in general -- let alone for two disparate MOF stationary phases. In addition we determine the fundamental thermodynamic constant for mass sorption, the partition coefficient, for HKUST-1 and several light hydrocarbons and select toxic industrial chemicals.

  17. NHEJ enzymes LigD and Ku participate in stationary-phase mutagenesis in Pseudomonas putida.

    Science.gov (United States)

    Paris, Ülvi; Mikkel, Katren; Tavita, Kairi; Saumaa, Signe; Teras, Riho; Kivisaar, Maia

    2015-07-01

    Under growth-restricting conditions bacterial populations can rapidly evolve by a process known as stationary-phase mutagenesis. Bacterial nonhomologous end-joining (NHEJ) system which consists of the DNA-end-binding enzyme Ku and the multifunctional DNA ligase LigD has been shown to be important for survival of bacteria especially during quiescent states, such as late stationary-phase populations or sporulation. In this study we provide genetic evidence that NHEJ enzymes participate in stationary-phase mutagenesis in a population of carbon-starved Pseudomonas putida. Both the absence of LigD or Ku resulted in characteristic spectra of stationary-phase mutations that differed from each other and also from the wild-type spectrum. This indicates that LigD and Ku may participate also in mutagenic pathways that are independent from each other. Our results also imply that both phosphoesterase (PE) and polymerase (POL) domains of the LigD protein are involved in the occurrence of mutations in starving P. putida. The participation of both Ku and LigD in the occurrence of stationary-phase mutations was further supported by the results of the analysis of mutation spectra in stationary-phase sigma factor RpoS-minus background. The spectra of mutations identified in the RpoS-minus background were also distinct if LigD or Ku was absent. Interestingly, the effects of the presence of these enzymes on the frequency of occurrence of certain types of mutations were different or even opposite in the RpoS-proficient and deficient backgrounds. These results imply that RpoS affects performance of mutagenic pathways in starving P. putida that utilize LigD and/or Ku. Copyright © 2015. Published by Elsevier B.V.

  18. Photochemically Immobilized 4-Methylbenzoyl Cellulose as a Powerful Chiral Stationary Phase for Enantioselective Chromatography

    Directory of Open Access Journals (Sweden)

    Eric Francotte

    2016-12-01

    Full Text Available A process to immobilize para-methylbenzoyl cellulose (PMBC on silica gel has been developed and applied to prepare chiral stationary phases (CSPs for enantioselective chromatography. The immobilization was achieved by simple irradiation of the polysaccharide derivative with ultraviolet light after coating on a silica gel support. The influence of parameters such as irradiation time and solvent on immobilization effectiveness were investigated. The performance of the prepared immobilized phases were evaluated by injection of a series of racemic compounds onto the packed columns and determination of their chiral recognition ability. By contrast to the classical coated phase, the immobilized CSP can be used under various chromatographic conditions without limitation of organic solvent types as the mobile phase. This extended applicability permits to improve selectivity and to resolve chiral compounds which are not or only poorly soluble in the mobile phases which are compatible with the non-immobilized PMBC stationary phase.

  19. Profiling of Campylobacter jejuni Proteome in Exponential and Stationary Phase of Growth

    Directory of Open Access Journals (Sweden)

    Hana Turonova

    2017-05-01

    Full Text Available Campylobacter jejuni has been reported as a major cause of bacterial food-borne enteritides in developed countries during the last decade. Despite its fastidious growth requirements, including low level of oxygen and high level of CO2, this pathogen is able to persist in the environment without permanent loss of its viability and virulence. As C. jejuni is not able to multiply outside a host, the cells spend significant amount of time in stationary phase of growth. The entry into the stationary phase is often correlated to resistance to various stresses in bacteria. The switching between exponential and stationary phases is frequently mediated by the regulator sigma S (RpoS. However, this factor is absent in C. jejuni and molecular mechanisms responsible for transition of cells to the stationary phase remain elusive. In this work, proteomic profiles of cells from exponential and stationary phases were compared using 2-D electrophoresis (2DE fingerprinting combined with mass spectrometry analysis and qRT-PCR. The identified proteins, whose expression differed between the two phases, are mostly involved in protein biosynthesis, carbon metabolism, stress response and motility. Altered expression was observed also in the pleiotropic regulator CosR that was over-expressed during stationary phase. A shift between transcript and protein level evolution of CosR throughout the growth of C. jejuni was observed using qRT-PCR and (2DE. From these data, we hypothesized that CosR could undergo a negative autoregulation in stationary phase. A consensus sequence resulting from promoter sequence alignment of genes potentially regulated by CosR, including its own upstream region, among C. jejuni strains is proposed. To verify experimentally the potential autoregulation of CosR at the DNA level, electrophoretic mobility shift assay was performed with DNA fragments of CosR promoter region and rCosR. Different migration pattern of the promoter fragments indicates

  20. [Using barium fluoride fine particles as stationary phase for TLC/FTIR analysis].

    Science.gov (United States)

    Liu, Xi; Pan, Qing-hua; Ding, Jie; Zhu, Qing; He, An-qi; Yue, Shi-juan; Li, Xiao-pei; Hu, Li-ping; Xia, Jin-ming; Liu, Cui-ge; Wei, Yong-ju; Yu, Jiang; Yang, Zhan-lan; Zhu, Xi; Xu, Yi-zhuang; Wu, Jin-guang

    2011-07-01

    In situ TLC/FTIR technique has tremendous potential in the analysis of complex mixtures. However, the progress in this technique was quite slow. The reason is that conventional stationary phase such as silica gel etc. has strong absorption in FTIR spectrum and thus brings about severe interference in the detection of samples. To solve the problem, the authors propose to use barium fluoride fine particles as stationary phase of TLC plate. The reasons are as follows: Barium fluoride wafer has been extensively used as infrared window in FTIR experiments and it has no absorbance in an IR region between 4 000 and 800 cm'. As a matter of fact, the atomic mass of barium and fluoride is quite large, thus the normal vibration of BaF2 lattice is limited in far-IR region and low frequency part of mid-IR region. Therefore, the interference caused by IR absorption of stationary phase can be resolved if BaF2 is used as stationary phase of TLC plate. Moreover, BaF2 is quite stable and insolvable in water and most organic solvents and it will not be dissolved by mobile phase or react with samples in TLC separation. Additionally, decreasing the particle size of BaF2 is very important in TLC/FTIR analysis technique. The reason is two-fold: First, decreasing the particle size of stationary phase is helpful to improving the efficiency of separation by TLC plate; second, decreasing the size of BaFz particle can improve the quality of FTIR spectra by alleviating the problem of light scattering. By optimizing the synthetic conditions, fine particles of barium fluoride were obtained. SEM results indicate that the size of the BaF2 particles is around 500 nm. FTIR spectrum of the BaF2 particles shows that no absorption of impurity was observed. Moreover, the elevation of baseline caused by light scattering is insignificant. The authors have developed a new technique named "settlement volatilization method" to prepare TLC plate without polymeric adhesive that may bring about significant

  1. Convergence to stationary solutions for a parabolic-hyperbolic phase-field system

    Czech Academy of Sciences Publication Activity Database

    Grasselli, M.; Petzeltová, Hana; Schimperna, G.

    2006-01-01

    Roč. 5, č. 4 (2006), s. 827-838 ISSN 1534-0392 R&D Projects: GA AV ČR(CZ) IAA1019302 Institutional research plan: CEZ:AV0Z10190503 Keywords : phase-field models * convergence to stationary solutions * Łojasiewicz-Simon inequality Subject RIV: BA - General Mathematics Impact factor: 0.857, year: 2006

  2. Carbon nanotube based stationary phases for microchip chromatography

    DEFF Research Database (Denmark)

    Mogensen, Klaus Bo; Kutter, Jörg Peter

    2012-01-01

    already been demonstrated in more classical formats, for improved separation performance in gas and liquid chromatography, and for unique applications in solid phase extraction. Carbon nanotubes are now also entering the field of microfluidics, where there is a large potential to be able to provide......The objective of this article is to provide an overview and critical evaluation of the use of carbon nanotubes and related carbon-based nanomaterials for microchip chromatography. The unique properties of carbon nanotubes, such as a very high surface area and intriguing adsorptive behaviour, have...... integrated, tailor-made nanotube columns by means of catalytic growth of the nanotubes inside the fluidic channels. An evaluation of the different implementations of carbon nanotubes and related carbon-based nanomaterials for microfluidic chromatography devices is given in terms of separation performance...

  3. Nanomaterials as stationary phases and supports in liquid chromatography.

    Science.gov (United States)

    Beeram, Sandya R; Rodriguez, Elliott; Doddavenkatanna, Suresh; Li, Zhao; Pekarek, Allegra; Peev, Darin; Goerl, Kathryn; Trovato, Gianfranco; Hofmann, Tino; Hage, David S

    2017-10-01

    The development of various nanomaterials over the last few decades has led to many applications for these materials in liquid chromatography (LC). This review will look at the types of nanomaterials that have been incorporated into LC systems and the applications that have been explored for such systems. A number of carbon-based nanomaterials and inorganic nanomaterials have been considered for use in LC, ranging from carbon nanotubes, fullerenes and nanodiamonds to metal nanoparticles and nanostructures based on silica, alumina, zirconia and titanium dioxide. Many ways have been described for incorporating these nanomaterials into LC systems. These methods have included covalent immobilization, adsorption, entrapment, and the synthesis or direct development of nanomaterials as part of a chromatographic support. Nanomaterials have been used in many types of LC. These applications have included the reversed-phase, normal-phase, ion-exchange, and affinity modes of LC, as well as related methods such as chiral separations, ion-pair chromatography and hydrophilic interaction liquid chromatography. Both small and large analytes (e.g., dyes, drugs, amino acids, peptides and proteins) have been used to evaluate possible applications for these nanomaterial-based methods. The use of nanomaterials in columns, capillaries and planar chromatography has been considered as part of these efforts. Potential advantages of nanomaterials in these applications have included their good chemical and physical stabilities, the variety of interactions many nanomaterials can have with analytes, and their unique retention properties in some separation formats. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Exploitation of a microporous organic polymer as a stationary phase for capillary gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Lu, Cuiming; Liu, Shuqin; Xu, Jianqiao; Ding, Yajuan; Ouyang, Gangfeng, E-mail: cesoygf@mail.sysu.edu.cn

    2016-01-01

    Microporous organic polymers (MOPs) have emerged as a new class of functional porous materials with unique characteristics and potential uses in diverse areas. However, the field of MOPs for gas chromatographic (GC) separations has not been well explored. Herein, a MOP namely KAPs-1 was dynamic coated onto a capillary column for the first time. The fabricated column exhibited a nonpolar nature and the column efficiency for n-dodecane was up to 7769 plates m{sup −1}. The KAPs-1 coated column showed high GC separation performance for a series of volatile organic compounds (VOCs) including the challenging ethylbenzene and xylene isomers, which could not be resolved at baseline on the commercial 5% phenyl polysiloxane stationary phase. Moreover, the relative standard deviations for five replicate determinations of the studied analytes were 0.0–0.6%, 0.9–3.2%, 1.1–5.9%, 0.8–3.7% for retention time, peak area, peak height and peak width, respectively. To investigate the interaction between some analytes and the stationary phase, thermodynamic and kinetic parameters were also evaluated. The results of this study show it is very promising to utilize MOPs as stationary phases for capillary GC. - Highlights: • A microporous organic polymer was explored as a novel stationary phase for capillary GC. • The column showed high separation performance for VOCs including the challenging ethylbenzene and xylene isomers. • Thermodynamic and kinetic parameters for BTEXs were determined to study the analyte-stationary phase interaction.

  5. Exploitation of a microporous organic polymer as a stationary phase for capillary gas chromatography

    International Nuclear Information System (INIS)

    Lu, Cuiming; Liu, Shuqin; Xu, Jianqiao; Ding, Yajuan; Ouyang, Gangfeng

    2016-01-01

    Microporous organic polymers (MOPs) have emerged as a new class of functional porous materials with unique characteristics and potential uses in diverse areas. However, the field of MOPs for gas chromatographic (GC) separations has not been well explored. Herein, a MOP namely KAPs-1 was dynamic coated onto a capillary column for the first time. The fabricated column exhibited a nonpolar nature and the column efficiency for n-dodecane was up to 7769 plates m −1 . The KAPs-1 coated column showed high GC separation performance for a series of volatile organic compounds (VOCs) including the challenging ethylbenzene and xylene isomers, which could not be resolved at baseline on the commercial 5% phenyl polysiloxane stationary phase. Moreover, the relative standard deviations for five replicate determinations of the studied analytes were 0.0–0.6%, 0.9–3.2%, 1.1–5.9%, 0.8–3.7% for retention time, peak area, peak height and peak width, respectively. To investigate the interaction between some analytes and the stationary phase, thermodynamic and kinetic parameters were also evaluated. The results of this study show it is very promising to utilize MOPs as stationary phases for capillary GC. - Highlights: • A microporous organic polymer was explored as a novel stationary phase for capillary GC. • The column showed high separation performance for VOCs including the challenging ethylbenzene and xylene isomers. • Thermodynamic and kinetic parameters for BTEXs were determined to study the analyte-stationary phase interaction.

  6. Advances in enantiomeric resolution on monolithic chiral stationary phases in liquid chromatography and electrochromatography.

    Science.gov (United States)

    Al-Othman, Zeid A; Al-Warthan, Abdulrahman; Ali, Imran

    2014-05-01

    During the last decade, chiral monolithic stationary phases have been prepared and used for rapid enantioseparations in CEC and HPLC. Various chiral selectors are used to prepare these CSPs. The preparation, properties, and applications of these CSPs are discussed in this paper. Attempts have been made to describe optimization strategies and the chiral recognition mechanisms. A comparison of chiral separations in CEC and HPLC is described. Efforts have also been made to predict the future perspectives and challenges of chiral monolithic stationary phases. The most effective chiral selectors include polysaccharides, cyclodextrins, and macrocyclic glycopeptide antibiotics. These chiral phases produced acceptable analytical enantiomeric separation of a variety of racemates. However, the development of these CSPs for preparative-scale separations is needed. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. HPLC Enantioseparation of Phenylcarbamic Acid Derivatives by Using Macrocyclic Chiral Stationary Phases

    Directory of Open Access Journals (Sweden)

    Hroboňová Katarína

    2016-06-01

    Full Text Available The HPLC by using chiral stationary phases based on macrocyclic antibiotics, dimethylphenyl carbamate cyklofructan 7 and β-cyclodextrin in terms of polar-organic separation mode (mobile phase methanol/acetonitrile/acetic acid/triethylamine were used for enantioseparation of alkoxy derivatives of phenylcarbamic acid. The effect of the analyte structures on the efficiency of enantioseparation was investigated. The most suitable stationary phase was teicoplanin aglycone, where the separations of the enantiomers were obtained (the resolution value from 0.65 to 2.90, depending on the structure of the analyte. Significant effect on the resolution of the enantiomers has position of alkoxy substituent in the hydrophobic part of the molecule. The enantiorecognition was achieved for 3-alkoxysubstituted derivatives.

  8. From superconductivity near a quantum phase transition to superconducting graphite

    Directory of Open Access Journals (Sweden)

    S. S. Saxena

    2006-09-01

    Full Text Available   The collapse of antiferromagnetic order as a function of some quantum tuning parameter such as carrier density or hydrostatic pressure is often accompanied by a region of superconductivity. The corresponding phenomenon in the potentially simpler case of itinerant-electron ferromagnetism, however, remains more illusive. In this paper we consider the reasons why this may be so and summaries evidence suggesting that the obstacles to observing the phenomenon are apparently overcome in a few metallic ferromagnets. A new twist to the problem presented by the recent discoveries in ferroelectric symmetric systems and new graphite intercalate superconductors will also be discussed.

  9. A comparison of the radiosensitivity of stationary, exponential and G1 phase wild type and repair deficient yeast cultures: supporting evidence for stationary phase yeast cells being in G0

    International Nuclear Information System (INIS)

    Tippins, R.S.; Parry, J.M.

    1982-01-01

    The main points to emerge from this comparison of the radiosensitivity of stationary, exponential and G 1 phase yeast cultures were: (1) In wild type yeast cultures, G 1 cells were the most sensitive to the lethal effects of X-rays, exponential phase cells were the most resistant and stationary phase cells were intermediate in sensitivity. (2) With the excision-repair-defective strain D61-3 (rad 3) stationary phase cells were more resistant than exponential cells with G 1 cells again being most sensitive. (3) The rad 50 gene present in JD50 had a marked effect on the X-ray inactivation response of this strain. In the presence of the defective rad 50 allele, exponential phase cells were as sensitive as G 1 phase cells, with stationary phase cells being more resistant than either. (4) There were marked differences in sensitivity between stationary phase and G 1 phase cells. These differences, along with other physiological differences reported by other workers, lead the authors to suggest that stationary phase cells can be better described as being in G 0 phase, i.e. a stage which is outside the normal mitotic cell cycle of an exponential culture. (author)

  10. The extracellular proteome of Rhizobium etli CE3 in exponential and stationary growth phase

    Directory of Open Access Journals (Sweden)

    Mendoza-Hernández Guillermo

    2010-10-01

    Full Text Available Abstract Background The extracellular proteome or secretome of symbiotic bacteria like Rhizobium etli is presumed to be a key element of their infection strategy and survival. Rhizobia infect the roots of leguminous plants and establish a mutually beneficial symbiosis. To find out the possible role of secreted proteins we analyzed the extracellular proteome of R. etli CE3 in the exponential and stationary growth phases in minimal medium, supplemented with succinate-ammonium. Results The extracellular proteins were obtained by phenol extraction and identified by LC-ESI MS/MS. We identified 192 and 191 proteins for the exponential and stationary phases respectively. Using the software Signal P, we predicted signal peptides for 12.95% and 35.60% of the proteins identified in the exponential and stationary phases, respectively, which could therefore be secreted by the Sec pathway. For the exponential growth phase, we found in abundance proteins like the ribosomal proteins, toxins and proteins belonging to the group "defence mechanisms". For the stationary growth phase, we found that the most abundant proteins were those with unknown function, and in many of these we identified characteristic domains of proteases and peptidases. Conclusions Our study provided the first dataset of the secretome of R. etli and its modifications, which may lead to novel insights into the adaptive response of different stages of growth. In addition, we found a high number of proteins with unknown function; these proteins could be analyzed in future research to elucidate their role in the extracellular proteome of R. etli.

  11. Nucleation mechanism for the direct graphite-to-diamond phase transition

    Science.gov (United States)

    Khaliullin, Rustam Z.; Eshet, Hagai; Kühne, Thomas D.; Behler, Jörg; Parrinello, Michele

    2011-09-01

    Graphite and diamond have comparable free energies, yet forming diamond from graphite in the absence of a catalyst requires pressures that are significantly higher than those at equilibrium coexistence. At lower temperatures, the formation of the metastable hexagonal polymorph of diamond is favoured instead of the more stable cubic diamond. These phenomena cannot be explained by the concerted mechanism suggested in previous theoretical studies. Using an ab initio quality neural-network potential, we carried out a large-scale study of the graphite-to-diamond transition assuming that it occurs through nucleation. The nucleation mechanism accounts for the observed phenomenology and reveals its microscopic origins. We demonstrate that the large lattice distortions that accompany the formation of diamond nuclei inhibit the phase transition at low pressure, and direct it towards the hexagonal diamond phase at higher pressure. The proposed nucleation mechanism should improve our understanding of structural transformations in a wide range of carbon-based materials.

  12. Tetrafluoromethane monolayer physisorbed on graphite : its orientational walls and its complex phase diagram

    OpenAIRE

    Croset , B.; Marti , C.; Thorel , P.; Lauter , H.

    1982-01-01

    Neutron diffraction results for a monolayer of CF4 physisorbed on different graphites show the complexity of the system, mainly due to the non spherical shape of the admolecule. From our neutron data and LEED results [6] we recognize at least 6 different phases. These are, with decreasing temperature, liquid, plastic, commensurate solid, incommensurate solid, incommensurate tilted and a surprising triple-peaked incommensurate phase. This low temperature phase is especially studied and compare...

  13. Separation of piracetam derivatives on polysaccharide-based chiral stationary phases.

    Science.gov (United States)

    Kažoka, H; Koliškina, O; Veinberg, G; Vorona, M

    2013-03-15

    High-performance liquid chromatography was used for the enantiomeric separation of two chiral piracetam derivatives. The suitability of six commercially available polysaccharide-based chiral stationary phases (CSPs) under normal phase mode for direct enantioseparation has been investigated. The influence of the CSPs as well the nature and content of an alcoholic modifier in the mobile phase on separation and elution order was studied. It was established that CSP Lux Amylose-2 shows high chiral recognition ability towards 4-phenylsubstituted piracetam derivatives. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. Selectivity differences of water-soluble vitamins separated on hydrophilic interaction stationary phases.

    Science.gov (United States)

    Yang, Yuanzhong; Boysen, Reinhard I; Hearn, Milton T W

    2013-06-01

    In this study, the retention behavior and selectivity differences of water-soluble vitamins were evaluated with three types of polar stationary phases (i.e. an underivatized silica phase, an amide phase, and an amino phase) operated in the hydrophilic interaction chromatographic mode with ESI mass spectrometric detection. The effects of mobile phase composition, including buffer pH and concentration, on the retention and selectivity of the vitamins were investigated. In all stationary phases, the neutral or weakly charged vitamins exhibited very weak retention under each of the pH conditions, while the acidic and more basic vitamins showed diverse retention behaviors. With the underivatized silica phase, increasing the salt concentration of the mobile phase resulted in enhanced retention of the acidic vitamins, but decreased retention of the basic vitamins. These observations thus signify the involvement of secondary mechanisms, such as electrostatic interaction in the retention of these analytes. Under optimized conditions, a baseline separation of all vitamins was achieved with excellent peak efficiency. In addition, the effects of water content in the sample on retention and peak efficiency were examined, with sample stacking effects observed when the injected sample contained a high amount of water. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Nickel-graphite composites of variable architecture by graphitization-accompanied spark plasma sintering and hot pressing and their response to phase separation

    Directory of Open Access Journals (Sweden)

    Dudina D.V.

    2015-01-01

    Full Text Available We report the formation and phase separation response of nickel-graphite composites with variable-architecture phases by graphitization-accompanied consolidation via Spark Plasma Sintering and hot pressing. It was shown that the application of pressure during consolidation is crucial for the occurrence of graphitization and formation of 3D graphite structures. We evaluated the suitability of the synthesized composites as precursors for making porous structures. Nickel behaved as a space holder with the particle size and spatial distribution changing during consolidation with the temperature and determining the structure of porous graphite formed by phase separation by dissolution in HCl. The response of the consolidated Ni-Cgr to separation of carbon by its burnout in air was studied. The result of the carbon removal was either the formation of a dense and continuous NiO film on the surface of the compacts or oxidation through the compact thickness. The choice between these two options depended on the density of the compacts and on the presence of carbon dissolved in nickel. It was found that during the burnout of graphite from Ni-Cgr composites, sintering, rather than formation of pores, dominated.

  16. Strengthening of the DNA-protein complex during stationary phase aging of cell cultures

    International Nuclear Information System (INIS)

    Khokhlov, A.N.; Chirkova, E.Yu.; Gorin, A.I.

    1986-01-01

    The possibility of accumulation of cross-linkages in the DNA-protein complex was studied during stationary phase aging of cells in culture. Chinese hamster cells were used in the experiments, along with human fibroblasts. 3 H-thymidine, 14 C-valine, and 14 C-leucine were added to the medium. The quantity of protein firmly bound with DNA was judged from the value of the coefficient 14 C/ 3 H determined with allowance for penetration of counting from the 14 C-channel into the 3 H-channel. The authors maintain that the results presented in this paper provide further evidence of the value of stationary phase cell cultures for the study of the mechanisms of aging and also of some of the general principles underlying hereditary pathology

  17. Experimental comparison of chiral metal-organic framework used as stationary phase in chromatography.

    Science.gov (United States)

    Xie, Sheng-Ming; Zhang, Mei; Fei, Zhi-Xin; Yuan, Li-Ming

    2014-10-10

    Chiral metal-organic frameworks (MOFs) are a new class of multifunctional material, which possess diverse structures and unusual properties such as high surface area, uniform and permanent cavities, as well as good chemical and thermal stability. Their chiral functionality makes them attractive as novel enantioselective adsorbents and stationary phases in separation science. In this paper, the experimental comparison of a chiral MOF [In₃O(obb)₃(HCO₂)(H₂O)] solvent used as a stationary phase was investigated in gas chromatography (GC), high-performance liquid chromatography (HPLC) and capillary electrochromatography (CEC). The potential relationship between the structure and components of chiral MOFs with their chiral recognition ability and selectivity are presented. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Temporal transcriptomic analysis of Desulfovibrio vulgaris Hildenborough transition into stationary phase growth during electrondonor depletion

    Energy Technology Data Exchange (ETDEWEB)

    Clark, M.E.; He, Q.; He, Z.; Huang, K.H.; Alm, E.J.; Wan, X.-F.; Hazen, T.C.; Arkin, A.P.; Wall, J.D.; Zhou, J.-Z.; Fields, M.W.

    2006-08-01

    Desulfovibrio vulgaris was cultivated in a defined medium, and biomass was sampled for approximately 70 h to characterize the shifts in gene expression as cells transitioned from the exponential to the stationary phase during electron donor depletion. In addition to temporal transcriptomics, total protein, carbohydrate, lactate, acetate, and sulfate levels were measured. The microarray data were examined for statistically significant expression changes, hierarchical cluster analysis, and promoter element prediction and were validated by quantitative PCR. As the cells transitioned from the exponential phase to the stationary phase, a majority of the down-expressed genes were involved in translation and transcription, and this trend continued at the remaining times. There were general increases in relative expression for intracellular trafficking and secretion, ion transport, and coenzyme metabolism as the cells entered the stationary phase. As expected, the DNA replication machinery was down-expressed, and the expression of genes involved in DNA repair increased during the stationary phase. Genes involved in amino acid acquisition, carbohydrate metabolism, energy production, and cell envelope biogenesis did not exhibit uniform transcriptional responses. Interestingly, most phage-related genes were up-expressed at the onset of the stationary phase. This result suggested that nutrient depletion may affect community dynamics and DNA transfer mechanisms of sulfate-reducing bacteria via the phage cycle. The putative feoAB system (in addition to other presumptive iron metabolism genes) was significantly up-expressed, and this suggested the possible importance of Fe{sup 2+} acquisition under metal-reducing conditions. The expression of a large subset of carbohydrate-related genes was altered, and the total cellular carbohydrate levels declined during the growth phase transition. Interestingly, the D. vulgaris genome does not contain a putative rpoS gene, a common attribute

  19. Escherichia coli adhesive coating as a chiral stationary phase for open tubular capillary electrochromatography enantioseparation

    International Nuclear Information System (INIS)

    Fu, Qifeng; Zhang, Kailian; Gao, Die; Wang, Lujun; Yang, Fengqing; Liu, Yao; Xia, Zhining

    2017-01-01

    Bacteria, the microorganism with intrinsic chirality, have numerous fascinating chiral phenomena such as various chirality-triggered biological processes and behaviors. Herein, bacteria were firstly explored as novel chiral stationary phases in open-tubular capillary electrochromatography (OT-CEC) for enantioseparation of fluoroquinolone enantiomers and simultaneous separation of six fluoroquinolone antibiotics. The model strain, i.e. non-pathogenic Escherichia coli (E. coli) DH5α, was adhered onto the inner surface of positively charged polyethyleneimine (PEI) modified capillaries based on the bacterial adhesion characteristics and strong electrostatic interaction. The morphology and thickness of the bacteria adhesive coatings in the capillary were characterized by field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM). Baseline separation of ofloxacin and partial separation of lomefloxacin enantiomers could be achieved by the E. coli coated columns. The preparation parameters including the coating time and concentration of bacteria that affecting the chiral resolution were intensively investigated. The electrophoretic parameters, including pH, buffer concentration and applied voltage, were also optimized. The developed method was validated (linearity, LOD, LOQ, intra-day, inter-day and column-to-column repeatability and recovery) and successfully utilized for the quantitative analysis of ofloxacin enantiomers in the ofloxacin tablets. Moreover, only a slight decrease in the separation efficiency was observed after 90 consecutive runs on the E. coli@capillary. These results demonstrated that bacteria are promising stationary phases for chiral separation in CEC. - Highlights: • Bacteria were firstly introduced in OT-CEC as a chiral stationary phase for chiral separation. • Enantioseparation of ofloxacin enantiomers was achieved on E. coli coated open tubular capillary column. • Bacterial stationary phases may be used to

  20. Escherichia coli adhesive coating as a chiral stationary phase for open tubular capillary electrochromatography enantioseparation

    Energy Technology Data Exchange (ETDEWEB)

    Fu, Qifeng, E-mail: fuqifeng1990@163.com [Department of Medicinal Chemistry, Southwest Medical University, Luzhou 646000 (China); Zhang, Kailian; Gao, Die; Wang, Lujun [Department of Medicinal Chemistry, Southwest Medical University, Luzhou 646000 (China); Yang, Fengqing; Liu, Yao [School of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400030 (China); Xia, Zhining, E-mail: tcm_anal_cqu@163.com [Innovative Drug Research Centre and School of Pharmaceutical Sciences, Chongqing University, Chongqing 400030 (China); School of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400030 (China)

    2017-05-29

    Bacteria, the microorganism with intrinsic chirality, have numerous fascinating chiral phenomena such as various chirality-triggered biological processes and behaviors. Herein, bacteria were firstly explored as novel chiral stationary phases in open-tubular capillary electrochromatography (OT-CEC) for enantioseparation of fluoroquinolone enantiomers and simultaneous separation of six fluoroquinolone antibiotics. The model strain, i.e. non-pathogenic Escherichia coli (E. coli) DH5α, was adhered onto the inner surface of positively charged polyethyleneimine (PEI) modified capillaries based on the bacterial adhesion characteristics and strong electrostatic interaction. The morphology and thickness of the bacteria adhesive coatings in the capillary were characterized by field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM). Baseline separation of ofloxacin and partial separation of lomefloxacin enantiomers could be achieved by the E. coli coated columns. The preparation parameters including the coating time and concentration of bacteria that affecting the chiral resolution were intensively investigated. The electrophoretic parameters, including pH, buffer concentration and applied voltage, were also optimized. The developed method was validated (linearity, LOD, LOQ, intra-day, inter-day and column-to-column repeatability and recovery) and successfully utilized for the quantitative analysis of ofloxacin enantiomers in the ofloxacin tablets. Moreover, only a slight decrease in the separation efficiency was observed after 90 consecutive runs on the E. coli@capillary. These results demonstrated that bacteria are promising stationary phases for chiral separation in CEC. - Highlights: • Bacteria were firstly introduced in OT-CEC as a chiral stationary phase for chiral separation. • Enantioseparation of ofloxacin enantiomers was achieved on E. coli coated open tubular capillary column. • Bacterial stationary phases may be used to

  1. Stationary phase selection and comprehensive two-dimensional gas chromatographic analysis of trace biodiesel in petroleum-based fuel.

    Science.gov (United States)

    Seeley, John V; Bates, Carly T; McCurry, James D; Seeley, Stacy K

    2012-02-24

    The GC×GC solvation parameter model has been used to identify effective stationary phases for the separation of fatty acid methyl esters (FAMEs) from petroleum hydrocarbons. This simple mathematical model was used to screen the 1225 different combinations of 50 stationary phases. The most promising pairs combined a poly(methyltrifluoropropylsiloxane) stationary phase with a poly(dimethyldiphenylsiloxane) stationary phase. The theoretical results were experimentally tested by equipping a GC×GC instrument with a DB-210 primary stationary phase and an HP-50+ secondary stationary phase. This instrument was used to analyze trace levels of FAMEs in kerosene. The FAMEs were fully separated from the petroleum hydrocarbons on the secondary dimension of the 2-D chromatogram. The resulting GC×GC method was shown to be capable of accurately quantifying FAME levels as low as 2 ppm (w/w). These results demonstrate the utility of the solvation parameter model for identifying optimal stationary phases for high resolution GC×GC separations. Furthermore, this work presents an effective method for determining the level of biodiesel contamination in aviation fuel and other petroleum-based fuels. Copyright © 2011 Elsevier B.V. All rights reserved.

  2. Exploitation of a microporous organic polymer as a stationary phase for capillary gas chromatography.

    Science.gov (United States)

    Lu, Cuiming; Liu, Shuqin; Xu, Jianqiao; Ding, Yajuan; Ouyang, Gangfeng

    2016-01-01

    Microporous organic polymers (MOPs) have emerged as a new class of functional porous materials with unique characteristics and potential uses in diverse areas. However, the field of MOPs for gas chromatographic (GC) separations has not been well explored. Herein, a MOP namely KAPs-1 was dynamic coated onto a capillary column for the first time. The fabricated column exhibited a nonpolar nature and the column efficiency for n-dodecane was up to 7769 plates m(-1). The KAPs-1 coated column showed high GC separation performance for a series of volatile organic compounds (VOCs) including the challenging ethylbenzene and xylene isomers, which could not be resolved at baseline on the commercial 5% phenyl polysiloxane stationary phase. Moreover, the relative standard deviations for five replicate determinations of the studied analytes were 0.0-0.6%, 0.9-3.2%, 1.1-5.9%, 0.8-3.7% for retention time, peak area, peak height and peak width, respectively. To investigate the interaction between some analytes and the stationary phase, thermodynamic and kinetic parameters were also evaluated. The results of this study show it is very promising to utilize MOPs as stationary phases for capillary GC. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Enhanced dipicolinic acid production during the stationary phase in Bacillus subtilis by blocking acetoin synthesis.

    Science.gov (United States)

    Toya, Yoshihiro; Hirasawa, Takashi; Ishikawa, Shu; Chumsakul, Onuma; Morimoto, Takuya; Liu, Shenghao; Masuda, Kenta; Kageyama, Yasushi; Ozaki, Katsuya; Ogasawara, Naotake; Shimizu, Hiroshi

    2015-01-01

    Bacterial bio-production during the stationary phase is expected to lead to a high target yield because the cells do not consume the substrate for growth. Bacillus subtilis is widely used for bio-production, but little is known about the metabolism during the stationary phase. In this study, we focused on the dipicolinic acid (DPA) production by B. subtilis and investigated the metabolism. We found that DPA production competes with acetoin synthesis and that acetoin synthesis genes (alsSD) deletion increases DPA productivity by 1.4-fold. The mutant showed interesting features where the glucose uptake was inhibited, whereas the cell density increased by approximately 50%, resulting in similar volumetric glucose consumption to that of the parental strain. The metabolic profiles revealed accumulation of pyruvate, acetyl-CoA, and the TCA cycle intermediates in the alsSD mutant. Our results indicate that alsSD-deleted B. subtilis has potential as an effective host for stationary-phase production of compounds synthesized from these intermediates.

  4. Eukaryotic initiation factor 5A dephosphorylation is required for translational arrest in stationary phase cells.

    Science.gov (United States)

    Chung, Janete; Rocha, Antonio A; Tonelli, Renata R; Castilho, Beatriz A; Schenkman, Sergio

    2013-04-15

    The protein known as eIF5A (eukaryotic initiation factor 5A) has an elusive role in translation. It has a unique and essential hypusine modification at a conserved lysine residue in most eukaryotes. In addition, this protein is modified by phosphorylation with unknown functions. In the present study we show that a phosphorylated state of eIF5A predominates in exponentially growing Trypanosoma cruzi cells, and extensive dephosphorylation occurs in cells in stationary phase. Phosphorylation occurs mainly at Ser(2), as shown in yeast eIF5A. In addition, a novel phosphorylation site was identified at Tyr(21). In exponential cells, T. cruzi eIF5A is partially associated with polysomes, compatible with a proposed function as an elongation factor, and becomes relatively enriched in polysomal fractions in stationary phase. Overexpression of the wild-type eIF5A, or eIF5A with Ser(2) replaced by an aspartate residue, but not by alanine, increases the rate of cell proliferation and protein synthesis. However, the presence of an aspartate residue instead of Ser(2) is toxic for cells reaching the stationary phase, which show a less-pronounced protein synthesis arrest and a decreased amount of eIF5A in dense fractions of sucrose gradients. We conclude that eIF5A phosphorylation and dephosphorylation cycles regulate translation according to the growth conditions.

  5. Hierarchical CaCO3 chromatography: a stationary phase based on biominerals.

    Science.gov (United States)

    Sato, Kosuke; Oaki, Yuya; Takahashi, Daisuke; Toshima, Kazunobu; Imai, Hiroaki

    2015-03-23

    In biomineralization, acidic macromolecules play important roles for the growth control of crystals through a specific interaction. Inspired by this interaction, we report on an application of the hierarchical structures in CaCO3 biominerals to a stationary phase of chromatography. The separation and purification of acidic small organic molecules are achieved by thin-layer chromatography and flash chromatography using the powder of biominerals as the stationary phase. The unit nanocrystals and their oriented assembly, the hierarchical structure, are suitable for the adsorption site of the target organic molecules and the flow path of the elution solvents, respectively. The separation mode is ascribed to the specific adsorption of the acidic molecules on the crystal face and the coordination of the functional groups to the calcium ions. The results imply that a new family of stationary phase of chromatography can be developed by the fine tuning of hierarchical structures in CaCO3 materials. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    NARCIS (Netherlands)

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

    2013-01-01

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

  7. Silanol suppressing potency of alkyl-imidazolium ionic liquids on C18 stationary phases.

    Science.gov (United States)

    Fernández-Navarro, J J; Torres-Lapasió, J R; Ruiz-Ángel, M J; García-Álvarez-Coque, M C

    2012-04-06

    Residual silanols on C18 columns yield undesirable slow-kinetics ion-exchange interactions with positively charged basic compounds that result in asymmetrical peaks, low efficiencies and long retention times. The purity of the silica employed as supporting material, and the technique used to form the bonded phase, which varies with the brand and manufacturer, give rise to different amounts of residual silanols in the packings, and consequently, different chromatographic performance. One of the most efficient and widespread strategies to reduce or even eliminate the different performance among columns is the addition of a reagent to the mobile phase to block the silanol sites. However, the intrinsic nature of both stationary phase and additive leads to particular results. In this work, a group of basic compounds were analysed using six C18 stationary phases (Zorbax SB-C18, X-Terra MS C18, Kromasil, Lichrospher, Nucleosil, and Spherisorb) and acetonitrile-water mixtures. Two ionic liquids (ILs), 1-butyl- and 1-hexyl-3-methyl-imidazolium tetrafluoroborates, were added to the mobile phases to evaluate their silanol suppressing potency, based on the decreased retention of the basic compounds when the silanols are blocked (described by the Horváth equation), and the improvement in peak profile (described by the plots of the peak half-widths at diverse retention times). The suppressing potency based on the retention can be misleading when the adsorption of the IL anion is not negligible, since the anion attracts the cationic basic compounds increasing the retention. However, the accessibility of basic compounds to the silanols is prevented by both IL cation and anion, improving the peak profiles for all stationary phases. This was especially remarkable for Spherisorb, which in the absence of additive yielded by far the worst performance. 1-Hexyl-3-methyl-imidazolium tetrafluoroborate was the best additive in terms of retention and peak profile (width and asymmetry

  8. Enantioseparation of Six Antihistamines with Immobilized Cellulose Chiral Stationary Phase by HPLC.

    Science.gov (United States)

    Zhou, Jie; Luo, Pei; Chen, Shanshan; Meng, Lingchang; Sun, Chong; Du, Qiuzheng; Sun, Fang

    2016-04-01

    A stereoselective high performance liquid chromatography method has been developed for the chiral separation of the enantiomers of six antihistamines, doxylamine, carbinoxamine, dioxopromethazine, oxomemazine, cetirizine and hydroxyzine. The effects of mobile phase additive, column temperature and flow rate on the retention time and resolution were studied. Enantiomeric separation of cetirizine, doxylamine and hydroxyzine were achieved on cellulose tris-(3,5-dichlorophenylcarbamate) immobilized on silica gel chiral stationary phase known as Chiralpak IC (RS = 3.74, RS = 1.85 and RS = 1.74, respectively). © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  9. Radiation stimulation during the early stationary growth phase in Synechococcus lividus and its correlation with photooxidative stress occurring before the stationary phase

    International Nuclear Information System (INIS)

    Conter, A.; Dupouy, D.; Vincent, C.; Planel, H.

    1987-01-01

    The effects of chronic gamma radiation at dose rates ranging from 0.058 mGy d-1 on growth rate calculated during the early stationary phase were studied. A stimulatory effect occurred for all doses and for all phases of the cells selected for use in the inoculation of the medium. During the same period, the rate of nucleic acid synthesis was increased in irradiated cultures compared to control cultures. The stimulating effect always occurred in cultures irradiated from the inoculation to the eighteenth day only. This result led us to conclude that the stimulation mechanism depended upon the events occurring at the end of the exponential phase in the deceleration period. Studies on cell metabolism showed that cells presented features of photooxidative stress in this period. Increases in superoxide dismutase, glutathione reductase and glucose-6-phosphate dehydrogenase were observed in irradiated cultures. It was assumed that irradiation at very low doses could help cells to better defend against photooxidative stress by increasing oxidants that activate the glucose metabolism and C5-sugars production and nucleic acid synthesis

  10. Search for improved fluorinated stationary phases for separation of fluorine-containing pharmaceuticals from their desfluoro analogs.

    Science.gov (United States)

    Regalado, Erik L; Makarov, Alexey A; McClain, Ray; Przybyciel, Matthew; Welch, Christopher J

    2015-02-06

    Evaluation of a several fluorine-containing stationary phases for the chromatographic separation of fluorine-containing pharmaceuticals from their corresponding desfluoro analogs revealed a number of perfluoroaryl and perfluoroalky stationary phases that afford good separations. These fluorous stationary phases exhibit greater retention for the fluorine-containing compounds relative to the H-containing analogs, consistent with a fluorophilic retention mechanism. While both perfluoroalkyl and perfluoroaryl stationary phases afford adequate resolution, the perfluoroaryl columns generally exhibit superior separation factor (α) and peak efficiency (N), resulting in faster baseline separations, with the Hypersil Gold PFP and Poroshell 120 PFP columns providing the best overall performance for the test group studied. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Argentation gas chromatography revisited: Separation of light olefin/paraffin mixtures using silver-based ionic liquid stationary phases.

    Science.gov (United States)

    Nan, He; Zhang, Cheng; Venkatesh, Amrit; Rossini, Aaron J; Anderson, Jared L

    2017-11-10

    Silver ion or argentation chromatography utilizes stationary phases containing silver ions for the separation of unsaturated compounds. In this study, a mixed-ligand silver-based ionic liquid (IL) was evaluated for the first time as a gas chromatographic (GC) stationary phase for the separation of light olefin/paraffin mixtures. The selectivity of the stationary phase toward olefins can be tuned by adjusting the ratio of silver ion and the mixed ligands. The maximum allowable operating temperature of these stationary phases was determined to be between 125°C and 150°C. Nuclear magnetic resonance (NMR) spectroscopy was used to characterize the coordination behavior of the silver-based IL as well as provide an understanding into the retention mechanism of light olefins. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Mechanically Induced Graphite-Nanodiamonds-Phase Transformations During High-Energy Ball Milling

    Science.gov (United States)

    El-Eskandarany, M. Sherif

    2017-05-01

    Due to their unusual mechanical, chemical, physical, optical, and biological properties, nearly spherical-like nanodiamonds have received much attention as desirable advanced nanomaterials for use in a wide spectrum of applications. Although, nanodiamonds can be successfully synthesized by several approaches, applications of high temperature and/or high pressure may restrict the real applications of such strategic nanomaterials. Distinct from the current preparation approaches used for nanodiamonds preparation, here we show a new process for preparing ultrafine nanodiamonds (3-5 nm) embedded in a homogeneous amorphous-carbon matrix. Our process started from high-energy ball milling of commercial graphite powders at ambient temperature under normal atmospheric helium gas pressure. The results have demonstrated graphite-single wall carbon nanotubes-amorphous-carbon-nanodiamonds phase transformations carried out through three subsequent stages of ball milling. Based on XRD and RAMAN analyses, the percentage of nanodiamond phase + C60 (crystalline phase) produced by ball milling was approximately 81%, while the amorphous phase amount was 19%. The pressure generated on the powder together the with temperature increase upon the ball-powder-ball collision is responsible for the phase transformations occurring in graphite powders.

  13. Surface Modification of Exfoliated Graphite Nano-Reinforcements, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — Phase I results showed that two surface treatments, oxidative plasma and reactive finishes, are effective means of modifying the surface chemistry of exfoliated...

  14. Theory for Transitions Between Exponential and Stationary Phases: Universal Laws for Lag Time

    Science.gov (United States)

    Himeoka, Yusuke; Kaneko, Kunihiko

    2017-04-01

    The quantitative characterization of bacterial growth has attracted substantial attention since Monod's pioneering study. Theoretical and experimental works have uncovered several laws for describing the exponential growth phase, in which the number of cells grows exponentially. However, microorganism growth also exhibits lag, stationary, and death phases under starvation conditions, in which cell growth is highly suppressed, for which quantitative laws or theories are markedly underdeveloped. In fact, the models commonly adopted for the exponential phase that consist of autocatalytic chemical components, including ribosomes, can only show exponential growth or decay in a population; thus, phases that halt growth are not realized. Here, we propose a simple, coarse-grained cell model that includes an extra class of macromolecular components in addition to the autocatalytic active components that facilitate cellular growth. These extra components form a complex with the active components to inhibit the catalytic process. Depending on the nutrient condition, the model exhibits typical transitions among the lag, exponential, stationary, and death phases. Furthermore, the lag time needed for growth recovery after starvation follows the square root of the starvation time and is inversely related to the maximal growth rate. This is in agreement with experimental observations, in which the length of time of cell starvation is memorized in the slow accumulation of molecules. Moreover, the lag time distributed among cells is skewed with a long time tail. If the starvation time is longer, an exponential tail appears, which is also consistent with experimental data. Our theory further predicts a strong dependence of lag time on the speed of substrate depletion, which can be tested experimentally. The present model and theoretical analysis provide universal growth laws beyond the exponential phase, offering insight into how cells halt growth without entering the death phase.

  15. Proteomic Analysis of Stationary Phase in the Marine Bacterium "Candidatus Pelagibacter ubique"

    Energy Technology Data Exchange (ETDEWEB)

    Sowell, S. M.; Norbeck, A. D.; Lipton, M. S.; Nicora, C. D.; Callister, S. J.; Smith, R. D.; Barofsky, D. F.; Giovannoni, S. J.

    2008-05-09

    The α-proteobacterium ‘Candidatus Pelagibacter ubique’ str. HTCC1062, and most other members of the SAR11 clade, lack genes for assimilatory sulfate reduction, making them dependent on organosulfur compounds that occur naturally in seawater. To investigate how these cells adapt to sulfur limitation, batch cultures were grown in defined media containing either limiting or non-limiting amounts of dimethylsulfoniopropionate (DMSP) as the sole sulfur source. Protein and mRNA expression were measured during exponential growth, immediately prior to stationary phase, and in late stationary phase. Two distinct responses were observed: one as DMSP became exhausted, and another as cells acclimated to a sulfur-limited environment. The first response was characterized by increased transcription and translation of all Ca. P. ubique genes downstream of previously confirmed S-adenosyl methionine (SAM) riboswitches: bhmT, mmuM, and metY. Proteins encoded by these genes were up to 33 times more abundant as DMSP became limiting. Their predicted function is to shunt all available sulfur to methionine. The secondary response, observed during sulfur-depleted stationary phase, was a 6-10 fold increase in transcription of the heme c shuttle ccmC and two small genes of unknown function (SAR11_1163 and SAR11_1164). This bacterium's strategy for coping with sulfur stress appears to be intracellular redistribution to support methionine biosynthesis, rather than increasing organosulfur import. Many of the genes and SAM riboswitches involved in this response are located in a hypervariable genome region (HVR). One of these HVR genes, ordL, is located downstream of a conserved motif that evidence suggests is a novel riboswitch.

  16. Stationary phase expression of the arginine biosynthetic operon argCBH in Escherichia coli

    Directory of Open Access Journals (Sweden)

    Sun Yuan

    2006-02-01

    Full Text Available Abstract Background Arginine biosynthesis in Escherichia coli is elevated in response to nutrient limitation, stress or arginine restriction. Though control of the pathway in response to arginine limitation is largely modulated by the ArgR repressor, other factors may be involved in increased stationary phase and stress expression. Results In this study, we report that expression of the argCBH operon is induced in stationary phase cultures and is reduced in strains possessing a mutation in rpoS, which encodes an alternative sigma factor. Using strains carrying defined argR, and rpoS mutations, we evaluated the relative contributions of these two regulators to the expression of argH using operon-lacZ fusions. While ArgR was the main factor responsible for modulating expression of argCBH, RpoS was also required for full expression of this biosynthetic operon at low arginine concentrations (below 60 μM L-arginine, a level at which growth of an arginine auxotroph was limited by arginine. When the argCBH operon was fully de-repressed (arginine limited, levels of expression were only one third of those observed in ΔargR mutants, indicating that the argCBH operon is partially repressed by ArgR even in the absence of arginine. In addition, argCBH expression was 30-fold higher in ΔargR mutants relative to levels found in wild type, fully-repressed strains, and this expression was independent of RpoS. Conclusion The results of this study indicate that both derepression and positive control by RpoS are required for full control of arginine biosynthesis in stationary phase cultures of E. coli.

  17. Graphite-supported platinum catalysts: Effects of gas and aqueous phase treatments

    Energy Technology Data Exchange (ETDEWEB)

    Vleeming, J.H.; Kuster, B.F.M.; Marin, G.B. [Eindhoven Univ. of Technology (Netherlands)] [and others

    1997-03-01

    The effects on the platinum particle diameter and the available platinum surface area of a graphite-supported platinum catalyst resulting from pretreatments and from performing a selective oxidation reaction are investigated. In the gas phase considerable catalyst sintering occurs only in the presence of oxygen at 773 K due to extensive carbon burn-off, whereas in an aqueous phase platinum particle growth is limited upon oxidative treatment. A hydrogen treatment in aqueous phase at 363 K causes platinum particle growth, aggregate formation, and covering of metal sites. These phenomena become more important with increasing pH. Platinum particle growth and aggregate formation are attributed to platinum particle rather than platinum adatom mobility and is caused by the destruction of the oxygen-containing surface groups on the graphite support, which serve as anchorage sites for the platinum particles. Site covering is caused by products originating from the graphite support, which are formed as a result of the reductive treatments. When performing the aqueous phase oxidation of methyl {alpha}-D-glucopyranoside at 323 K and a pH of 9, catalyst modifications are small under oxidative conditions. Exposure of the catalyst for several hours to methyl {alpha}-D-glucopyranoside under the same conditions but in the absence of oxygen causes site covering. 50 refs., 9 figs., 1 tab.

  18. Bacteriophage T4 Infection of Stationary Phase E. coli: Life after Log from a Phage Perspective.

    Science.gov (United States)

    Bryan, Daniel; El-Shibiny, Ayman; Hobbs, Zack; Porter, Jillian; Kutter, Elizabeth M

    2016-01-01

    Virtually all studies of phage infections investigate bacteria growing exponentially in rich media. In nature, however, phages largely encounter non-growing cells. Bacteria entering stationary phase often activate well-studied stress defense mechanisms that drastically alter the cell, facilitating its long-term survival. An understanding of phage-host interactions in such conditions is of major importance from both an ecological and therapeutic standpoint. Here, we show that bacteriophage T4 can efficiently bind to, infect and kill E. coli in stationary phase, both in the presence and absence of a functional stationary-phase sigma factor, and explore the response of T4-infected stationary phase cells to the addition of fresh nutrients 5 or 24 h after that infection. An unexpected new mode of response has been identified. "Hibernation" mode is a persistent but reversible dormant state in which the infected cells make at least some phage enzymes, but halt phage development until appropriate nutrients become available before producing phage particles. Our evidence indicates that the block in hibernation mode occurs after the middle-mode stage of phage development; host DNA breakdown and the incorporation of the released nucleotides into phage DNA indicate that the enzymes of the nucleotide synthesizing complex, under middle-mode control, have been made and assembled into a functional state. Once fresh glucose and amino acids become available, the standard lytic infection process rapidly resumes and concentrations of up to 10(11) progeny phage (an average of about 40 phage per initially present cell) are produced. All evidence is consistent with the hibernation-mode control point lying between middle mode and late mode T4 gene expression. We have also observed a "scavenger" response, where the infecting phage takes advantage of whatever few nutrients are available to produce small quantities of progeny within 2 to 5 h after infection. The scavenger response seems able

  19. Bacteriophage T4 Infection of Stationary Phase E. coli: Life after Log from a Phage Perspective

    Directory of Open Access Journals (Sweden)

    Elizabeth Martin Kutter

    2016-09-01

    Full Text Available Virtually all studies of phage infections investigate bacteria growing exponentially in rich media. In nature, however, phages largely encounter non-growing cells. Bacteria entering stationary phase often activate well-studied stress defense mechanisms that drastically alter the cell, facilitating its long-term survival. An understanding of phage-host interactions in such conditions is of major importance from both an ecological and therapeutic standpoint. Here, we show that bacteriophage T4 can efficiently bind to, infect and kill E. coli in stationary phase, both in the presence and absence of a functional stationary-phase sigma factor, and explore the response of T4-infected stationary phase cells to the addition of fresh nutrients 5 or 24 hours after that infection. An unexpected new mode of response has been identified. Hibernation mode is a persistent but reversible dormant state in which the infected cells make at least some phage enzymes, but halt phage development until appropriate nutrients become available before producing phage particles. Our evidence indicates that the block in hibernation mode occurs after the middle-mode stage of phage development; host DNA breakdown and the incorporation of the released nucleotides into phage DNA indicate that the enzymes of the nucleotide synthesizing complex, under middle-mode control, have been made and assembled into a functional state. Once fresh glucose and amino acids become available, the standard lytic infection process rapidly resumes and concentrations of up to 1011 progeny phage (an average of about 40 phage per initially-present cell are produced. All evidence is consistent with the hibernation-mode control point lying between middle mode and late mode T4 gene expression. We have also observed a scavenger response, where the infecting phage takes advantage of whatever few nutrients are available to produce small quantities of progeny within 2 to 5 hours after infection. The scavenger

  20. Homochiral metal-organic framework used as a stationary phase for high-performance liquid chromatography.

    Science.gov (United States)

    Kong, Jiao; Zhang, Mei; Duan, Ai-Hong; Zhang, Jun-Hui; Yang, Rui; Yuan, Li-Ming

    2015-02-01

    Metal-organic frameworks are promising porous materials. Chiral metal-organic frameworks have attracted considerable attention in controlling enantioselectivity. In this study, a homochiral metal-organic framework [Co(2) (D-cam)(2) (TMDPy)] (D-cam = D-camphorates, TMDPy = 4,4'-trimethylenedipyridine) with a non-interpenetrating primitive cubic net has been used as a chiral stationary phase in high-performance liquid chromatography. It has allowed the successful separation of six positional isomers and six chiral compounds. The good selectivity and baseline separation, or at least 60% valley separation, confirmed its excellent molecular recognition characteristics. The relative standard deviations for the retention time of run-to-run and column-to-column were less than 1.8 and 3.1%, respectively. These results demonstrate that [Co(2) (D-cam)(2) (TMDPy)] may represent a promising chiral stationary phase for use in high-performance liquid chromatography. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Accelerating the quality control of pharmaceuticals using monolithic stationary phases: a review of recent HPLC applications.

    Science.gov (United States)

    Zacharis, Constantinos K

    2009-07-01

    High-performance liquid chromatography (HPLC) is the predominant technique in the quality control of pharmaceutical formulations. HPLC offers highly sensitive and selective analytical methods with increased robustness and separation efficiency. The majority of HPLC-based methodologies are based on the usage of particulate-based columns and cannot be applied at elevated flow rates (> 2 mL/min) due to excessive back-pressure. Therefore, the typical duration of separation cycles is in the range of 5-30 min, making most assays time-consuming, especially when a lot of samples have to be analyzed in a minimum amount of time. Monolithic stationary phases for HPLC offer a very interesting alternative to conventional particulate-based columns. The size of the skeleton and the distribution of the pores of monolithic materials offer the possibility of developing efficient separation protocols at higher flow-rates due to the low pressure-drop across the column. The present review intends to cover the applications of monolithic based HPLC stationary phases in the quality control of pharmaceutical formulations, including identification of active pharmaceutical ingredient, assay, purity, dissolution, blending, and dosage uniformity, etc.

  2. Battle of the Bacteria: Characterizing the Evolutionary Advantage of Stationary Phase Growth

    Directory of Open Access Journals (Sweden)

    Karin E. Kram

    2016-05-01

    Full Text Available Providing students with authentic research opportunities has been shown to enhance learning and increase retention in STEM majors. Accordingly, we have developed a novel microbiology lab module, which focuses on the molecular mechanisms of evolution in E. coli, by examining the growth advantage in stationary phase (GASP phenotype. The GASP phenotype is demonstrated by growing cells into long-term stationary phase (LTSP and then competing them against un-aged cells in a fresh culture. This module includes learning goals related to strengthening practical laboratory skills and improving student understanding of evolution. In addition, the students generate novel data regarding the effects of different environmental stresses on GASP and the relationship between evolution, genotypic change, mutation frequency, and cell stress. Pairs of students are provided with the experimental background, select a specific aspect of the growth medium to modify, and generate a hypothesis regarding how this alteration will impact the GASP phenotype. From this module, we have demonstrated that students are able to achieve the established learning goals and have produced data that has furthered our understanding of the GASP phenotype.

  3. The Trypanosoma cruzi nucleolus: a morphometrical analysis of cultured epimastigotes in the exponential and stationary phases.

    Science.gov (United States)

    Nepomuceno-Mejía, Tomás; Lara-Martínez, Reyna; Cevallos, Ana María; López-Villaseñor, Imelda; Jiménez-García, Luis Felipe; Hernández, Roberto

    2010-12-01

    Our group is interested in rRNA and ribosome biogenesis in the parasitic protozoan Trypanosoma cruzi. Epimastigotes represent an extracellular replicative stage of T. cruzi and can be cultured in axenic media. The growth curve of epimastigotes allows assessment of potential differences in the nucleoli of cells undergoing growth-rate transitions. To establish cellular parameters for studying ribosome biogenesis in T. cruzi, a morphometric analysis of the nucleoli of cultured cells in the exponential and stationary phases was conducted. Electron micrograph-based measurements of nuclear sections from independent cells demonstrated that the nucleolar area is over twofold higher in exponentially growing cells, as compared with epimastigotes in the stationary phase. The granular component of the nucleoli of actively growing cells was the main structural element. Cycloheximide moderately reduced the apparent size of the nucleoli without an apparent disruption of their architecture. Our results provide a firm basis for the establishment of an experimental model to study the organization of the nucleolus during the growth and development of T. cruzi. © 2010 Federation of European Microbiological Societies Published by Blackwell Publishing Ltd. All rights reserved.

  4. Retention behavior of resorcinarene-based cavitands on C8 and C18 stationary phases.

    Science.gov (United States)

    Bartó, Endre; Prauda, Ibolya; Kilár, Ferenc; Kiss, Ibolya; Felinger, Attila

    2015-09-01

    The understanding of the retention behavior of large molecules is an area of interest in liquid chromatography. Resorcinarene-based cavitands are cavity-shaped cyclic oligomers that can create host-guest interactions. We have investigated the chromatographic behavior of two types of cyclic tetramers as analytes in high-performance liquid chromatography. The experiments were performed at four different temperatures (15, 25, 35, 45°C) on two types of reversed stationary phases (C8 and C18 ) from two different manufacturers. We have found a huge difference between the retention of resorcinarenes and cavitands. In some cases, the retention factor of cavitands was even a hundred times larger than the retention factor of resorcinarenes. The retention of methylated derivates was two to four times larger compared to that of demethylated compounds on every column. The opposite retention behavior of the resorcinarenes and cavitands on the two types of stationary phases showed well the difference of the selectivity of the XTerra and BDS Hypersil columns. The retention mechanism was studied by the thermodynamic parameters calculated from the van't Hoff equation. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Genomewide Dam Methylation in Escherichia coli during Long-Term Stationary Phase.

    Science.gov (United States)

    Westphal, Lacey L; Sauvey, Peter; Champion, Matthew M; Ehrenreich, Ian M; Finkel, Steven E

    2016-01-01

    DNA methylation in prokaryotes is widespread. The most common modification of the genome is the methylation of adenine at the N-6 position. In Escherichia coli K-12 and many gammaproteobacteria, this modification is catalyzed by DNA adenine methyltransferase (Dam) at the GATC consensus sequence and is known to modulate cellular processes including transcriptional regulation of gene expression, initiation of chromosomal replication, and DNA mismatch repair. While studies thus far have focused on the motifs associated with methylated adenine (meA), the frequency of meA across the genome, and temporal dynamics during early periods of incubation, here we conduct the first study on the temporal dynamics of adenine methylation in E. coli by Dam throughout all five phases of the bacterial life cycle in the laboratory. Using single-molecule real-time sequencing, we show that virtually all GATC sites are significantly methylated over time; nearly complete methylation of the chromosome was confirmed by mass spectroscopy analysis. However, we also detect 66 sites whose methylation patterns change significantly over time within a population, including three sites associated with sialic acid transport and catabolism, suggesting a potential role for Dam regulation of these genes; differential expression of this subset of genes was confirmed by quantitative real-time PCR. Further, we show significant growth defects of the dam mutant during long-term stationary phase (LTSP). Together these data suggest that the cell places a high premium on fully methylating the chromosome and that alterations in methylation patterns may have significant impact on patterns of transcription, maintenance of genetic fidelity, and cell survival. IMPORTANCE While it has been shown that methylation remains relatively constant into early stationary phase of E. coli , this study goes further through death phase and long-term stationary phase, a unique time in the bacterial life cycle due to nutrient

  6. Integrated Time and Phase Synchronization Strategy for a Multichannel Spaceborne-Stationary Bistatic SAR System

    Directory of Open Access Journals (Sweden)

    Feng Hong

    2016-07-01

    Full Text Available The spatial separation of the transmitter and receiver in Bistatic Synthetic Aperture Radar (BiSAR makes it a promising and useful supplement to a classical Monostatic SAR system (MonoSAR. This paper proposes a novel integrated time and phase synchronization strategy for a multichannel spaceborne-stationary BiSAR system. Firstly, the time synchronization strategy is proposed, which includes Pulse Repetition Frequency (PRF generation under noisy conditions, multichannel calibration and the alignment of the recorded data with the orbital data. Furthermore, the phase synchronization strategy, which fully considers the deteriorative factors in the BiSAR configuration, is well studied. The contribution of the phase synchronization strategy includes two aspects: it not only compensates the phase error, but also improves the Signal to Noise Ratio (SNR of the obtained signals. Specifically, all direct signals on different PRF time can be reconstructed with the shift and phase compensation operation using a reference signal. Besides, since the parameters of the reference signal can be estimated only once using the selected practical direct signal and a priori information, the processing complexity is well reduced. Final imaging results with and without compensation for real data are presented to validate the proposed synchronization strategy.

  7. New graphite/salt materials for high temperature energy storage. Phase change properties study

    International Nuclear Information System (INIS)

    Lopez, J.

    2007-07-01

    This work is a contribution to the study of new graphite/salt composites dedicated to high temperature energy storage (≥200 C). The aim is to analyse and to understand the influence of both graphite and composite microstructure on the phase change properties of salts. This PhD is carried out within the framework of two projects: DISTOR (European) and HTPSTOCK (French). The major contributions of this work are threefold: 1) An important database (solid-liquid phase change properties) is provided from the DSC analysis of six salts and the corresponding composites. 2) Rigorous modeling of salts melting in confined media in several geometries are proposed to understand why, during the first melting of the compression elaborated composites, problems of salt leakage are observed. These models show that the materials morphology is responsible for these phenomena: the graphite matrix restrains the volume expansion due to salt melting: salt melts under pressure, which leads to a melting on a large temperature range and to a loss of energy density. Sensitivity analysis of parameters (geometric and physic) shows that matrix rigidity modulus is the parameter on which it is necessary to act during the composites elaboration to blur this phenomenon. 3) Finally, this work proposes a thermodynamic formulation of both surface/interface phenomena and the presence of dissolved impurities being able to explain a melting point lowering. It seems that the melting point lowering observed (∼ 5 C) are mainly due to the presence of dissolved impurities (brought by graphite) in the liquid, along with an additional Gibbs-Thomson effect (∼ 1 C, related to the size of the clusters crystals). (author)

  8. Novel RpoS-Dependent Mechanisms Strengthen the Envelope Permeability Barrier during Stationary Phase.

    Science.gov (United States)

    Mitchell, Angela M; Wang, Wei; Silhavy, Thomas J

    2017-01-15

    Gram-negative bacteria have effective methods of excluding toxic compounds, including a largely impermeable outer membrane (OM) and a range of efflux pumps. Furthermore, when cells become nutrient limited, RpoS enacts a global expression change providing cross-protection against many stresses. Here, we utilized sensitivity to an anionic detergent (sodium dodecyl sulfate [SDS]) to probe changes occurring to the cell's permeability barrier during nutrient limitation. Escherichia coli is resistant to SDS whether cells are actively growing, carbon limited, or nitrogen limited. In actively growing cells, this resistance depends on the AcrAB-TolC efflux pump; however, this pump is not necessary for protection under either carbon-limiting or nitrogen-limiting conditions, suggesting an alternative mechanism(s) of SDS resistance. In carbon-limited cells, RpoS-dependent pathways lessen the permeability of the OM, preventing the necessity for efflux. In nitrogen-limited but not carbon-limited cells, the loss of rpoS can be completely compensated for by the AcrAB-TolC efflux pump. We suggest that this difference simply reflects the fact that nitrogen-limited cells have access to a metabolizable energy (carbon) source that can efficiently power the efflux pump. Using a transposon mutant pool sequencing (Tn-Seq) approach, we identified three genes, sanA, dacA, and yhdP, that are necessary for RpoS-dependent SDS resistance in carbon-limited stationary phase. Using genetic analysis, we determined that these genes are involved in two different envelope-strengthening pathways. These genes have not previously been implicated in stationary-phase stress responses. A third novel RpoS-dependent pathway appears to strengthen the cell's permeability barrier in nitrogen-limited cells. Thus, though cells remain phenotypically SDS resistant, SDS resistance mechanisms differ significantly between growth states. Gram-negative bacteria are intrinsically resistant to detergents and many

  9. New poly(styrene/divinylbenzene) based stationary phases for the solid phase extraction of pesticides and the chromatography of carbohydrates

    International Nuclear Information System (INIS)

    Wartusch, I.

    2002-02-01

    The introduced sorbents based on poly(styrene/divinylbenzene) are studied regarding their extraction behavior of pesticides out of water. The sorbents are prepared with different porogens like n-octanol, n-decanol, n-dodecanol and acetone. The comparison of the extraction properties of these substances shows that the use of n-octanol as a porogen leads to the best recoveries. Furthermore this sorbent is compared to a stationary phase prepared via ring opening metathesis polymerization (ROMP) and to commercially available silica-C18. It is shown that the poly(styrene/divinylbenzene) based material on average yields higher recoveries as the other materials. Only the extraction of relatively polar pesticides works better with the ROMP based sorbent. For the chromatography of carbohydrates nonporous particles with diameters of about 3 μm were synthesized via poly(styrene/divinylbenzene) using the activated swelling method. Quaternary ammonia functional groups were introduced into the poly(styrene/divinylbenzene) particles via their nitration, reduction and quaternization. The applicability of these stationary phases for anion exchange chromatography is shown by separation of different kinds of sugars using a pulsed amperometric detection system. Monosaccharides are isocratically separated using an eluent containing sodium hydroxide, separations of disaccharides and oligosaccharides are performed using sodium acetate gradients. Linearity, detection limits and reproducibility of the system are investigated by the analysis of glucose, sucrose and fructose out of the real samples Coca Cola and apple juice. (author)

  10. Second-Phase Sampling Designs for Non-Stationary Spatial Variables.

    Science.gov (United States)

    Delmelle, Eric M; Goovaerts, Pierre

    2009-10-15

    In spatial sampling, once initial samples of the primary variable have been collected, it is possible to take additional measurements, an approach known as second-phase sampling. Additional samples are usually collected away from observation locations, or where the kriging variance is maximum. However, the kriging variance (also known as prediction error variance) is independent of data values and computed under the assumption of stationary spatial process, which is often violated in practice. In this paper, we weight the kriging variance with another criterion, giving greater sampling importance to locations exhibiting significant spatial roughness that is computed by a spatial moving average window. Additional samples are allocated using a simulated annealing procedure since the weighted objective function is non-linear. A case study using an exhaustive remote sensing image illustrates the procedure. Combinations of first-phase systematic and nested sampling designs (or patterns) of varying densities are generated, while the location of additional observations is guided in a way which optimizes the proposed objective function. The true pixel value at the new points is extracted, the semivariogram model updated, and the image reconstructed. Second-phase sampling patterns optimizing the proposed criterion lead to predictions closer to the true image than when using the kriging variance as the main criterion. This improvement is stronger when there is a low density of first-phase samples, and decreases however as the initial density increases.

  11. Application of the zeta potential for stationary phase characterization in ion chromatography.

    Science.gov (United States)

    Buszewski, Bogusław; Jaćkowska, Magdalena; Bocian, Szymon; Dziubakiewicz, Ewelina

    2013-01-01

    Two series of homemade stationary bonded phases for ion chromatography were investigated according to their zeta potential. One set of dendrimer anion exchanger was synthesized on the polymer support whereas the second material was prepared on the silica gel. The zeta potential data in water environment as well as buffered water solution were obtained. The influence of the length of anion-exchanger chains, the type of the support of the modified surface, and charge distribution on these data was investigated. Additionally, the zeta potential was correlated with retention factor of inorganic ions to describe their influence on the retention mechanism in ion chromatography. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Formation of aromatics in thermally induced reactions of chemically bonded RP-C18 stationary phase.

    Science.gov (United States)

    Prus, Wojciech

    2014-10-01

    In continuation of the research on the thermally induced chemical transformation of the silica-based chemically bonded stationary phases (C18), the oxidative cleavage of the silicon-carbon bonds with hydrogen peroxide and potassium fluoride was utilized, followed by the gas chromatography coupled with mass spectrometry (GC-MS) study of the resulting products. These investigations allowed determination of the probable structures of certain thermal modification products as the various different alkyl derivatives of the phenylsilane ligands. Apart from aromatic compounds, the products with unsaturated bonds and carbonyl functionalities were found in the analyzed extracts. The analysis of the GC-MS chromatograms reveals that under the applied working conditions, the investigated process runs with relatively low yields. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

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

    Directory of Open Access Journals (Sweden)

    Ashraf Yehia El-Naggar

    2013-01-01

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

  14. Braze Development of Graphite Fiber for Use in Phase Change Material Heat Sinks

    Science.gov (United States)

    Quinn, Gregory; Beringer, Woody; Gleason, Brian; Stephan, Ryan

    2011-01-01

    Hamilton Sundstrand (HS), together with NASA Johnson Space Center, developed methods to metallurgically join graphite fiber to aluminum. The goal of the effort was to demonstrate improved thermal conductance, tensile strength and manufacturability compared to existing epoxy bonded techniques. These improvements have the potential to increase the performance and robustness of phase change material heat sinks that use graphite fibers as an interstitial material. Initial work focused on evaluating joining techniques from four suppliers, each consisting of a metallization step followed by brazing or soldering of one inch square blocks of Fibercore graphite fiber material to aluminum end sheets. Results matched the strength and thermal conductance of the epoxy bonded control samples, so two suppliers were down-selected for a second round of braze development. The second round of braze samples had up to a 300% increase in strength and up to a 132% increase in thermal conductance over the bonded samples. However, scalability and repeatability proved to be significant hurdles with the metallization approach. An alternative approach was pursued which used a nickel braze allow to prepare the carbon fibers for joining with aluminum. Initial results on sample blocks indicate that this approach should be repeatable and scalable with good strength and thermal conductance when compared with epoxy bonding.

  15. Conventional and fast gas chromatography analysis of biodiesel blends using an ionic liquid stationary phase.

    Science.gov (United States)

    Ragonese, Carla; Tranchida, Peter Quinto; Sciarrone, Danilo; Mondello, Luigi

    2009-12-18

    The present research is focused on the GC-FID determination of fatty acid methyl esters (FAMEs) in diesel blends, by means of an ionic liquid stationary phase, characterized by a dicationic 1,9-di(3-vinyl-imidazolium)nonane bis(trifluoromethyl)sulfonylimidate structure (SLB-IL100). The high polarity of the ionic liquid stationary phase allowed the separation of the FAMEs, from the less-retained hydrocarbons, thus avoiding the requirement of a hydrocarbon LC pre-separation. The results derived from the analyses of a soybean FAMEs B20 sample, carried out on an SLB-IL100 conventional column (30 m x 0.25 mm i.d. x 0.20 mm d(f)), were compared with those attained on a polyethylene glycol column, of equivalent dimensions. Conventional and fast GC methods, for the analysis of FAMEs in diesel blends, were developed on an SLB-IL100 30 m x 0.25 mm i.d. x 0.20 microm d(f) and on an SLB-IL100 12 m x 0.10 mm i.d. x 0.08 microm d(f) column, respectively. The optimized IL methods were subjected to validation: retention time and peak area intra-day precision (n=5) were good, with CV % values lower than 0.08% and 4.9%, respectively. With regards to the quantitation of FAMEs in biodiesel blends, a five points calibration curve was constructed, using C(17:0) as internal standard.

  16. Graphite targets at LAMPF

    International Nuclear Information System (INIS)

    Brown, R.D.; Grisham, D.L.

    1983-01-01

    Rotating polycrystalline and stationary pyrolytic graphite target designs for the LAMPF experimental area are described. Examples of finite element calculations of temperatures and stresses are presented. Some results of a metallographic investigation of irradiated pyrolytic graphite target plates are included, together with a brief description of high temperature bearings for the rotating targets

  17. Procedure 5 Quality Assurance Requirements For Vapor Phase Mercury Continuous Emissions Monitoring Systems And Sorbent Trap Monitoring Systems Used For Compliance Determination At Stationary Sources

    Science.gov (United States)

    Promulgated quality assurance Procedure 5 Quality Assurance Requirements For Vapor Phase Mercury Continuous Emissions Monitoring Systems And Sorbent Trap Monitoring Systems Used For Compliance Determination At Stationary Sources

  18. Enantioseparation and chiral recognition mechanism of new chiral derivatives of xanthones on macrocyclic antibiotic stationary phases.

    Science.gov (United States)

    Fernandes, Carla; Tiritan, Maria Elizabeth; Cass, Quezia; Kairys, Visvaldas; Fernandes, Miguel Xavier; Pinto, Madalena

    2012-06-08

    A chiral HPLC method using four macrocyclic antibiotic chiral stationary phases (CSPs) has been investigated for determination of the enantiomeric purity of fourteen new chiral derivatives of xanthones (CDXs). The separations were performed with the CSPs Chirobiotic T, Chirobiotic TAG, Chirobiotic V and Chirobiotic R under multimodal elution conditions (normal-phase, reversed-phase and polar ionic mode). The analyses were performed at room temperature in isocratic mode and UV and CD detection at a wavelength of 254 nm. The best enantioselectivity and resolution were achieved on Chirobiotic R and Chirobiotic T CSPs, under normal elution conditions, with R(S) ranging from 1.25 to 2.50 and from 0.78 to 2.06, respectively. The optimized chromatographic conditions allowed the determination of the enantiomeric ratio of eight CDXs, always higher than 99%. In order to better understand the chromatographic behavior at a molecular level, and the structural features associated with the chiral recognition mechanism, computational studies by molecular docking were carried out using VDock. These studies shed light on the mechanisms involved in the enantioseparation for this important class of chiral compounds. Copyright © 2012 Elsevier B.V. All rights reserved.

  19. Nanocellulose Derivative/Silica Hybrid Core-Shell Chiral Stationary Phase: Preparation and Enantioseparation Performance

    Directory of Open Access Journals (Sweden)

    Xiaoli Zhang

    2016-05-01

    Full Text Available Core-shell silica microspheres with a nanocellulose derivative in the hybrid shell were successfully prepared as a chiral stationary phase by a layer-by-layer self-assembly method. The hybrid shell assembled on the silica core was formed using a surfactant as template by the copolymerization reaction of tetraethyl orthosilicate and the nanocellulose derivative bearing triethoxysilyl and 3,5-dimethylphenyl groups. The resulting nanocellulose hybrid core-shell chiral packing materials (CPMs were characterized and packed into columns, and their enantioseparation performance was evaluated by high performance liquid chromatography. The results showed that CPMs exhibited uniform surface morphology and core-shell structures. Various types of chiral compounds were efficiently separated under normal and reversed phase mode. Moreover, chloroform and tetrahydrofuran as mobile phase additives could obviously improve the resolution during the chiral separation processes. CPMs still have good chiral separation property when eluted with solvent systems with a high content of tetrahydrofuran and chloroform, which proved the high solvent resistance of this new material.

  20. Peptidoglycan Recycling in Gram-Positive Bacteria Is Crucial for Survival in Stationary Phase

    Science.gov (United States)

    Borisova, Marina; Gaupp, Rosmarie; Duckworth, Amanda; Schneider, Alexander; Dalügge, Désirée; Mühleck, Maraike; Deubel, Denise; Unsleber, Sandra; Yu, Wenqi; Muth, Günther; Bischoff, Markus; Götz, Friedrich

    2016-01-01

    ABSTRACT Peptidoglycan recycling is a metabolic process by which Gram-negative bacteria reutilize up to half of their cell wall within one generation during vegetative growth. Whether peptidoglycan recycling also occurs in Gram-positive bacteria has so far remained unclear. We show here that three Gram-positive model organisms, Staphylococcus aureus, Bacillus subtilis, and Streptomyces coelicolor, all recycle the sugar N-acetylmuramic acid (MurNAc) of their peptidoglycan during growth in rich medium. They possess MurNAc-6-phosphate (MurNAc-6P) etherase (MurQ in E. coli) enzymes, which are responsible for the intracellular conversion of MurNAc-6P to N-acetylglucosamine-6-phosphate and d-lactate. By applying mass spectrometry, we observed accumulation of MurNAc-6P in MurNAc-6P etherase deletion mutants but not in either the isogenic parental strains or complemented strains, suggesting that MurQ orthologs are required for the recycling of cell wall-derived MurNAc in these bacteria. Quantification of MurNAc-6P in ΔmurQ cells of S. aureus and B. subtilis revealed small amounts during exponential growth phase (0.19 nmol and 0.03 nmol, respectively, per ml of cells at an optical density at 600 nm [OD600] of 1) but large amounts during transition (0.56 nmol and 0.52 nmol) and stationary (0.53 nmol and 1.36 nmol) phases. The addition of MurNAc to ΔmurQ cultures greatly increased the levels of intracellular MurNAc-6P in all growth phases. The ΔmurQ mutants of S. aureus and B. subtilis showed no growth deficiency in rich medium compared to the growth of the respective parental strains, but intriguingly, they had a severe survival disadvantage in late stationary phase. Thus, although peptidoglycan recycling is apparently not essential for the growth of Gram-positive bacteria, it provides a benefit for long-term survival. PMID:27729505

  1. Effect of expanded graphite on the phase change materials of high density polyethylene/wax blends

    Energy Technology Data Exchange (ETDEWEB)

    AlMaadeed, M.A., E-mail: m.alali@qu.edu.qa [Center for Advanced Materials, Qatar University, 2713 Doha (Qatar); Labidi, Sami [Center for Advanced Materials, Qatar University, 2713 Doha (Qatar); Krupa, Igor [QAPCO Polymer Chair, Center for Advanced Materials, Qatar University, P.O. Box 2713, Doha (Qatar); Karkri, Mustapha [Université Paris-Est CERTES, 61 avenue du Général de Gaulle, 94010 Créteil (France)

    2015-01-20

    Highlights: • Expanded graphite (EG) and low melting point (42.3 °C) wax were added to HDPE to form phase change material. • EG was well dispersed in the composites and did not affect the melting or crystallization of the HDPE matrix. • EG increased the thermal stability of the composites by reducing chain mobility and inhibiting degradation. • The addition of a relatively small quantity of EG enhances the heat conduction in the composite. • HDPE/40% RT42 that contained up to 15% EG demonstrated excellent mechanical and thermal properties and can be used as PCM. - Abstract: Phase change materials fabricated from high density polyethylene (HDPE) blended with 40 or 50 wt% commercial wax (melting point of 43.08 °C) and up to 15 wt% expanded graphite (EG) were studied. Techniques including scanning electron microscope (SEM), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and an experimental device to measure diffusivity and conductivity (DICO) were used to determine the microstructural, mechanical and thermal properties of the composites. The composites possessed good mechanical properties. Additionally, no leaching was observed during material processing or characterization. Although the Young’s modulus increased with the addition of EG, no significant changes in tensile strength were detected. The maximum Young’s modulus achieved was 650 MPa for the HDPE/40% wax composite with 15 wt% EG. The EG was well dispersed within the composites and did not affect the melting or crystallization of the HDPE matrix. The incorporation of EG increased the thermal stability of the composites by reducing chain mobility and inhibiting degradation. The intensification of thermal conductivity occurred with increasing fractions of EG, which was attributed to the high thermal conductivity of graphite. The maximum quantity of heat stored by latent heat was found for the HDPE/40% wax composite with EG. The addition of a relatively small quantity

  2. Effect of expanded graphite on the phase change materials of high density polyethylene/wax blends

    International Nuclear Information System (INIS)

    AlMaadeed, M.A.; Labidi, Sami; Krupa, Igor; Karkri, Mustapha

    2015-01-01

    Highlights: • Expanded graphite (EG) and low melting point (42.3 °C) wax were added to HDPE to form phase change material. • EG was well dispersed in the composites and did not affect the melting or crystallization of the HDPE matrix. • EG increased the thermal stability of the composites by reducing chain mobility and inhibiting degradation. • The addition of a relatively small quantity of EG enhances the heat conduction in the composite. • HDPE/40% RT42 that contained up to 15% EG demonstrated excellent mechanical and thermal properties and can be used as PCM. - Abstract: Phase change materials fabricated from high density polyethylene (HDPE) blended with 40 or 50 wt% commercial wax (melting point of 43.08 °C) and up to 15 wt% expanded graphite (EG) were studied. Techniques including scanning electron microscope (SEM), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and an experimental device to measure diffusivity and conductivity (DICO) were used to determine the microstructural, mechanical and thermal properties of the composites. The composites possessed good mechanical properties. Additionally, no leaching was observed during material processing or characterization. Although the Young’s modulus increased with the addition of EG, no significant changes in tensile strength were detected. The maximum Young’s modulus achieved was 650 MPa for the HDPE/40% wax composite with 15 wt% EG. The EG was well dispersed within the composites and did not affect the melting or crystallization of the HDPE matrix. The incorporation of EG increased the thermal stability of the composites by reducing chain mobility and inhibiting degradation. The intensification of thermal conductivity occurred with increasing fractions of EG, which was attributed to the high thermal conductivity of graphite. The maximum quantity of heat stored by latent heat was found for the HDPE/40% wax composite with EG. The addition of a relatively small quantity

  3. Effect of benzalkonium chloride on viability and energy metabolism in exponential- and stationary-growth-phase cells of Listeria monocytogenes

    NARCIS (Netherlands)

    Luppens, S.B.I.; Abee, T.; Oosterom, J.

    2001-01-01

    The difference in killing exponential- and stationary-phase cells of Listeria monocytogenes by benzalkonium chloride (BAC) was investigated by plate counting and linked to relevant bioenergetic parameters. At a low concentration of BAC (8 mg liter-1), a similar reduction in viable cell numbers was

  4. Synthesis and characterization of mesoporous silica modified with chiral auxiliaries for their potential application as chiral stationary phase.

    Science.gov (United States)

    Mayani, Vishal J; Abdi, S H R; Kureshy, R I; Khan, N H; Agrawal, Santosh; Jasra, R V

    2008-05-16

    Novel chiral stationary phase (CSP) based on chiral aminoalcohol immobilized on ordered mesoporous silica SBA-15 1a and standard silica 1b and their copper complexes 1a' and 1b', respectively, was synthesized as potential material for chiral ligand exchange chromatography (CLEC). Microanalysis, inductively coupled plasma spectroscopy (ICP), thermo-gravimetric analysis (TGA), cross polarized magic angle spinning (CP-MAS) (13)C NMR, Powder X-ray diffraction (PXRD), FTIR, N(2) adsorption isotherm, scanning electron microscopy (SEM), transmitted electron microscope (TEM) and solid reflectance UV-vis spectroscopy were used to characterize these materials. All the chiral stationary phases thus synthesized were used for the separation of different racemic compounds such as mandelic acid, 2,2'-dihydroxy-1,1'-binaphthalene BINOL) and diethyl tartrate by simple medium-pressure column chromatography. Successful enantio-separation of racemic mandelic acid was achieved with all the stationary phases but 1a and 1b gave slightly better resolution than their copper complexes 1a' and 1b'. Remarkably these materials are stable under the given experimental conditions and can be used repeatedly for several cycles of enantioresolution. It was observed that the porosity and surface area of the stationary phase play an important role in the chiral separation.

  5. Recombinant Staphylococcal protein A with cysteine residue for preparation of affinity chromatography stationary phase and immunosensor applications

    Directory of Open Access Journals (Sweden)

    Gorbatiuk O. B.

    2015-04-01

    Full Text Available Aim. Engineering of recombinant Staphylococcal protein A with cysteine residue (SPA-Cys for preparation of affinity chromatography stationary phase and formation of bioselective element of immunosensor. Methods. DNA sequences encoding IgG-binding region of SPA, His-tag and cysteine were genetically fused and expressed in E. coli. SPA-Cys was immobilized on maleimide-functionalized silica beads for affinity chromatography stationary phase preparation and on a gold sensor surface as a bioselective element of immunosensor. Results. SPA-Cys was expressed at a high-level in a soluble form. The target protein was purified and showed a high IgG-binding activity. The capacity of the obtained SPA-Cys-based affinity chromatography stationary phase was 10–12 mg of IgG /ml. The purity of eluted IgG was more than 95 % in one-step purification procedure. The developed SPA-Cys-based bioselective element of immunosensor selectively interacted with human IgG and did not interact with the control proteins. Conclusions. The recombinant Staphylococcal protein A with cysteine residue was successfully used for the preparation of affinity chromatography stationary phase and formation of the bioselective element of immunosensor.

  6. Applications of graphite-enabled phase change material composites to improve thermal performance of cementitious materials

    Science.gov (United States)

    Li, Mingli; Lin, Zhibin; Wu, Lili; Wang, Jinhui; Gong, Na

    2017-11-01

    Enhancing the thermal efficiency to decrease the energy consumption of structures has been the topic of much research. In this study, a graphite-enabled microencapsulated phase change material (GE-MEPCM) was used in the production of a novel thermal energy storage engineered cementitious composite feathering high heat storage capacity and enhanced thermal conductivity. The surface morphology and particle size of the microencapsulated phase change material (MEPCM) were investigated by scanning electron microscopy (SEM). Thermal properties of MEPCM was determined using differential scanning calorimetry (DSC). In addition, thermal and mechanical properties of the cementitious mortar with different admixtures were explored and compared with those of a cementitious composite. It was shown that the latent heat of MEPCM was 162 J/g, offering much better thermal energy storage capacity to the cementitious composite. However, MEPCM was found to decrease the thermal conductivity of the composite, which can be effectively solved by adding natural graphite (NG). Moreover, the incorporation of MEPCM has a certain decrease in the compressive strength, mainly due to the weak interfaces between MEPCM and cement matrix.

  7. A polyacrylamide-based silica stationary phase for the separation of carbohydrates using alcohols as the weak eluent in hydrophilic interaction liquid chromatography.

    Science.gov (United States)

    Cai, Jianfeng; Cheng, Lingping; Zhao, Jianchao; Fu, Qing; Jin, Yu; Ke, Yanxiong; Liang, Xinmiao

    2017-11-17

    A hydrophilic interaction liquid chromatography (HILIC) stationary phase was prepared by a two-step synthesis method, immobilizing polyacrylamide on silica sphere particles. The stationary phase (named PA, 5μm dia) was evaluated using a mixture of carbohydrates in HILIC mode and the column efficiency reached 121,000Nm -1 . The retention behavior of carbohydrates on PA stationary phase was investigated with three different organic solvents (acetonitrile, ethanol and methanol) employed as the weak eluent. The strongest hydrophilicity of PA stationary phase was observed in both acetonitrile and methanol as the weak eluent, when compared with another two amide stationary phases. Attributing to its high hydrophilicity, three oligosaccharides (xylooligosaccharide, fructooligosaccharide and chitooligosaccharides) presented good retention on PA stationary phase using alcohols/water as mobile phase. Finally, PA stationary phase was successfully applied for the purification of galactooligosaccharides and saponins of Paris polyphylla. It is feasible to use safer and cheaper alcohols to replace acetonitrile as the weak eluent for green analysis and purification of polar compounds on PA stationary phase. Copyright © 2017. Published by Elsevier B.V.

  8. Impact of column and stationary phase properties on the productivity in chiral preparative LC.

    Science.gov (United States)

    Forssén, Patrik; Fornstedt, Torgny

    2018-03-01

    By generating 1500 random chiral separation systems, assuming two-site Langmuir interactions, we investigated numerically how the maximal productivity (P R,max ) was affected by changes in stationary phase adsorption properties. The relative change in P R,max , when one adsorption property changed 10%, was determined for each system and for each studied parameter the corresponding productivity change distribution of the systems was analyzed. We could conclude that there is no reason to have columns with more than 500 theoretical plates and larger selectivity than 3. More specifically, we found that changes in selectivity have a major impact on P R,max if it is below ∼2 and, interestingly, increasing selectivity when it is above ∼3 decreases P R,max . Increase in relative saturation capacity will have a major impact on P R,max if it is below ∼40%, but only modest above this percent. Increasing total monolayer saturation capacity, or decreasing the first eluting enantiomer's retention factor, will have a modest effect on P R,max and increased efficiency will have almost no effect at all on P R,max unless it is below ∼500 theoretical plates. Finally, we showed that chiral columns with superior analytic performance might have inferior preparative performance, or vice versa. It is, therefore, not possible to assess columns based on their analytical performance alone. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Proteomic analysis of lactose-starved Lactobacillus casei during stationary growth phase.

    Science.gov (United States)

    Hussain, M A; Knight, M I; Britz, M L

    2009-03-01

    Starvation stress is a condition that nonstarter lactic acid bacteria (NSLAB) normally encounter. This study was aimed to investigate starvation-induced proteins in Lactobacillus casei during stationary growth phase. The impact of carbohydrate starvation on L. casei GCRL163 was investigated using two different media (a modified de Man, Rogosa and Sharpe broth and a semi-defined medium). Cells were grown in the presence of excess lactose (1%) or starvation (0%) and differences in the patterns of one-dimensional sodium dodecyl sulfate-polyacrylamide gel electrophoresis and two-dimensional electrophoresis of the cytosolic protein fractions were investigated. Differentially regulated proteins were identified by MALDI-TOF/TOF mass spectrometry. Many differentially regulated proteins were enzymes of various metabolic pathways involved in carbohydrate metabolism to yield energy. Differences in protein expression were also observed in the two culture conditions tested in this experiment. Numerous glycolytic enzymes were differentially regulated under lactose starvation. The differential expression of these glycolytic enzymes suggests a potential survival strategy under harsh growth conditions (i.e. lactose starvation). This paper reports improved understanding of stress responses and survival mechanism of NSLAB under lactose-depleted cheese-ripening condition. This knowledge of how NSLAB bacteria adapt to lactose starvation could be applied to predict the performances of bacteria in other industrial applications.

  10. Site-Specific Ser/Thr/Tyr Phosphoproteome of Sinorhizobium meliloti at Stationary Phase.

    Directory of Open Access Journals (Sweden)

    Tao Liu

    Full Text Available Sinorhizobium meliloti, a facultative microsymbiont of alfalfa, should fine-tune its cellular processes to live saprophytically in soils characterized with limited nutrients and diverse stresses. In this study, TiO2 enrichment and LC-MS/MS were used to uncover the site-specific Ser/Thr/Tyr phosphoproteome of S. meliloti in minimum medium at stationary phase. There are a total of 96 unique phosphorylated sites, with a Ser/Thr/Tyr distribution of 63:28:5, in 77 proteins. Phosphoproteins identified in S. meliloti showed a wide distribution pattern regarding to functional categories, such as replication, transcription, translation, posttranslational modification, transport and metabolism of amino acids, carbohydrate, inorganic ion, succinoglycan etc. Ser/Thr/Tyr phosphosites identified within the conserved motif in proteins of key cellular function indicate a crucial role of phosphorylation in modulating cellular physiology. Moreover, phosphorylation in proteins involved in processes related to rhizobial adaptation was also discussed, such as those identified in SMa0114 and PhaP2 (polyhydroxybutyrate synthesis, ActR (pH stress and microaerobic adaption, SupA (potassium stress, chaperonin GroEL2 (viability and potentially symbiosis, and ExoP (succinoglycan synthesis and secretion. These Ser/Thr/Tyr phosphosites identified herein would be helpful for our further investigation and understanding of the role of phosphorylation in rhizobial physiology.

  11. A comparison of protein A chromatographic stationary phases: performance characteristics for monoclonal antibody purification.

    Science.gov (United States)

    Liu, Zhuo; Mostafa, Sigma S; Shukla, Abhinav A

    2015-01-01

    Protein A chromatography remains the dominant capture step used during the downstream purification of monoclonal antibodies (mAbs). With the recent expiry of the Repligen patent on recombinant Protein A, a variety of new Protein A resins have been introduced in the market. Given productivity limitations during downstream processing that have come into sharper focus with the recent increase in cell culture titers for mAbs, the selection of an appropriate Protein A resin has direct implications on the overall process economics of mAb production. The performance of seven different Protein A chromatographic resins was compared with respect to static binding capacity and dynamic binding capacity as a function of flow rate. This data was translated into a comparison of productivity (g mAb purified per unit resin volume per unit time) for the seven stationary phases. In addition, elution pH and host cell protein impurity levels after product capture on each of these resins were determined. The current article provides an effective methodology and dataset for the selection of the optimal Protein A chromatographic resin. © 2014 International Union of Biochemistry and Molecular Biology, Inc.

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

    Directory of Open Access Journals (Sweden)

    S. Faramawy

    2016-09-01

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

  13. Alkali Metal Modification of Silica Gel-Based Stationary Phase in Gas Chromatography

    Directory of Open Access Journals (Sweden)

    Ashraf Yehia El-Naggar

    2013-01-01

    Full Text Available Modification of the precipitated silica gel was done by treatment with alkali metal (NaCl before and after calcination. The silica surfaces before and after modification were confirmed by infrared spectroscopy in order to observe the strength and abundance of the acidic surface OH group bands which play an important role in the adsorption properties of polar and nonpolar solutes. The surface-modified silica gels were tested as GC solid stationary phases in terms of the separation efficiency for various groups of non-polar and polar solutes. Also, thermodynamic parameters (ΔH, ΔG, and ΔS were determined using n-hexane as a probe in order to show the adsorbate-adsorbent interaction. It was observed that the non-polar solutes could be separated Independent on the reactivity and porosity of the silica surfaces. The efficiency of the surface-modified silica gels to separate the aromatic hydrocarbons seemed to be strongly influenced by the density of the surface hydroxyls.

  14. Graphene nanosheets preparation using magnetic nanoparticle assisted liquid phase exfoliation of graphite: The coupled effect of ultrasound and wedging nanoparticles.

    Science.gov (United States)

    Hadi, Alireza; Zahirifar, Jafar; Karimi-Sabet, Javad; Dastbaz, Abolfazl

    2018-06-01

    This study aims to investigate a novel technique to improve the yield of liquid phase exfoliation of graphite to graphene sheets. The method is based on the utilization of magnetic Fe 3 O 4 nanoparticles as "particle wedge" to facilitate delamination of graphitic layers. Strong shear forces resulted from the collision of Fe 3 O 4 particles with graphite particles, and intense ultrasonic waves lead to enhanced exfoliation of graphite. High quality of graphene sheets along with the ease of Fe 3 O 4 particle separation from graphene solution which arises from the magnetic nature of Fe 3 O 4 nanoparticles are the unique features of this approach. Initial graphite flakes and produced graphene sheets were characterized by various methods including field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Raman spectroscopy, atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and Zeta potential analysis. Moreover, the effect of process factors comprising initial graphite concentration, Fe 3 O 4 nanoparticles concentration, sonication time, and sonication power were investigated. Results revealed that graphene preparation yield and the number of layers could be manipulated by the presence of magnetic nanoparticles. Copyright © 2018 Elsevier B.V. All rights reserved.

  15. Chiral separation of helical chromenes with chloromethyl phenylcarbamate polysaccharide-based stationary phases.

    Science.gov (United States)

    Ianni, Federica; Scorzoni, Stefania; Gentili, Pier Luigi; Di Michele, Alessandro; Frigoli, Michel; Camaioni, Emidio; Ortica, Fausto; Sardella, Roccaldo

    2017-12-12

    Two chloromethyl phenylcarbamate-based chiral stationary phases, one containing an amylose-type chiral selector (Lux Amylose 2, from Phenomenex) and the other a cellulose-type one (Lux Cellulose-4, from Phenomenex), were successfully used for the chiral resolution of three helical chromenes featuring a helicene-like structure. The compound bearing a phenyl substituent on the helicene-like structure was enantioresolved at 25°C with Lux Cellulose-4 and a n-hexane/1-propanol 99:1 v/v eluent. With a n-hexane/2-propanol 99.8:0.2 v/v mobile phase, the same column (operated at 35°C) provided the separation of the four isomers of the compound having a hexyl residue on the helicene-like motif and an additional asymmetric carbon. Lux Amylose-2 was necessary for the enantioseparation of the compound having the sole hexyl residue on the helical scaffold. For the last compound a n-hexane/2-propanol 99.8:0.2 v/v eluent was used, and the column temperature was fixed at 5°C. The enantiomer elution order was appraised by using electronic circular dichroism and theoretical calculations. Notably, different thermodynamics of retention and enantioseparation were observed for molecules with pronounced structural similarity, that is, the enantiomer pairs of the compound containing the additional asymmetric carbon atom. Indeed, both entropically and enthalpically controlled adsorption and separation processes were observed. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Enantioselective determination of arotinolol in human plasma by HPLC using teicoplanin chiral stationary phase.

    Science.gov (United States)

    Aboul-Enein, Hassan Y; Hefnawy, Mohamed M

    2003-10-01

    A sensitive enantioselective high-performance liquid chromatography (HPLC) method was developed and validated to determine S-(+)- and R-(-)-arotinolol in human plasma. Baseline resolution was achieved by using teicoplanin macrocyclic antibiotic chiral stationary phase (CSP) known as Chirobiotic T with a polar organic mobile phase consisting of methanol:glacial acetic acid:triethylamine, 100:0.1:0.1, (v/v/v) at a fl ow rate of 0.8 mL/min and UV detection set at 317 nm. Human plasma was spiked with stock solution of arotinolol enantiomers and labetalol as the internal standard. The assay involved the use of liquid-liquid extraction procedure with ethyl ether under alkaline condition for human plasma sample prior to HPLC analysis. Recoveries for S-(+)- and R-(-)-arotinolol enantiomers were in the range 93-103% at 200-1400 ng/mL level. Intra-day and inter-day precision calculated as %RSD was in the ranges 1.3-3.4 and 1.9-4.5% for both enantiomers, respectively. Intra-day and inter-day accuracies calculated as percentage error were in the ranges 1.2-3.5 and 1.5-6.2% for both enantiomers, respectively. Linear calibration curves in the concentration range 100-1500 ng/mL for each enantiomer showed a correlation coefficient (r) of 0.9998. The limit of quantitation (LOQ) and limit of detection (LOD) for each enantiomer in human plasma were 100 and 50 ng/mL (S/N = 3), respectively. Copyright 2003 John Wiley & Sons, Ltd.

  17. Shock Compression of Highly Oriented Pyrolytic Graphite: Role of Microstructure on the Phase Transformation

    Science.gov (United States)

    Volz, Travis; Gupta, Y. M.

    2017-06-01

    Past experiments on shock-compressed highly oriented pyrolytic graphite (HOPG) have shown that HOPG samples with different orientational orders respond differently above and below the 20 GPa phase transition. The objectives of the present study are to examine and compare the high pressure response of the ZYH-grade HOPG and ZYB-grade HOPG above the phase change stress, to determine the structure of the high pressure phase for the two types of HOPG samples, and to understand the role of the orientational order on the phase change mechanisms in shocked HOPG. Three types of plane shock wave experiments, utilizing time-resolved measurements, are being conducted to address these objectives. Transmission experiments to measure the propagating wave profiles, front-surface impact experiments to accurately characterize the peak shocked state and to determine the longitudinal sound speeds in the peak state, and XRD measurements to determine the microstructure of shocked ZYB and ZYH-grade HOPG samples above the transition. All three types of experiments have provided good initial data and analysis of the experimental results is currently underway. Our initial findings suggest that the shock response of the two HOPG grades, above the phase change stress, is more similar than previously reported. Further experiments and detailed analyses are underway. Work supported by the DOE/NNSA.

  18. Synthesis of a mixed-model stationary phase derived from glutamine for HPLC separation of structurally different biologically active compounds: HILIC and reversed-phase applications.

    Science.gov (United States)

    Aral, Tarık; Aral, Hayriye; Ziyadanoğulları, Berrin; Ziyadanoğulları, Recep

    2015-01-01

    A novel mixed-mode stationary phase was synthesised starting from N-Boc-glutamine, aniline and spherical silica gel (4 µm, 60 Å). The prepared stationary phase was characterized by IR and elemental analysis. The new stationary phase bears an embedded amide group into phenyl ring, highly polar a terminal amide group and non-polar groups (phenyl and alkyl groups). At first, this new mixed-mode stationary phase was used for HILIC separation of four nucleotides and five nucleosides. The effects of different separation conditions, such as pH value, mobile phase and temperature, on the separation process were investigated. The optimum separation for nucleotides was achieved using HILIC isocratic elution with aqueous mobile phase and acetonitrile with 20°C column temperature. Under these conditions, the four nucleotides could be separated and detected at 265 nm within 14 min. Five nucleosides were separated under HILIC isocratic elution with aqueous mobile phase containing pH=3.25 phosphate buffer (10mM) and acetonitrile with 20°C column temperature and detected at 265 nm within 14 min. Chromatographic parameters as retention factor, selectivity, theoretical plate number and peak asymmetry factor were calculated for the effect of temperature and water content in mobile phase on the separation process. The new column was also tested for nucleotides and nucleosides mixture and six analytes were separated in 10min. The chromatographic behaviours of these polar analytes on the new mixed-model stationary phase were compared with those of HILIC columns under similar conditions. Further, phytohormones and phenolic compounds were separated in order to see influence of the new stationary phase in reverse phase conditions. Eleven plant phytohormones were separated within 13 min using RP-HPLC gradient elution with aqueous mobile phase containing pH=2.5 phosphate buffer (10mM) and acetonitrile with 20°C column temperature and detected at 230 or 278 nm. The best separation

  19. Microstructure-based analysis and simulation of flow and mass transfer in chromatographic stationary phases

    Science.gov (United States)

    Koku, Harun

    Limitations of mass transfer in chromatographic bioseparations employing traditional packed particles have fuelled the inception and development of alternative stationary phases with improved performance characteristics. This work investigates case studies in two categories of these alternative media, namely polymer-modified packed particles and continuous monolithic phases, for insight into their enhanced properties. Specifically, high-resolution microscopy techniques and image-based analysis algorithms were implemented to extract morphology information for these materials, in an attempt to elucidate the relation between microstructure and performance. For the monolith, mesoscopic simulation methods were also employed for a more rigorous analysis of the flow and dispersion behavior. Scanning and transmission electron microscopy images of the commercial polymer-modified, agarose-based particle Sepharose XL were compared to those for its unmodified counterpart, Sepharose FF. Local regions in the composite dextran-agarose Sepharose XL particles were noted to exhibit a denser network of fibers and smaller pore sizes overall, compared to those in the traditional Sepharose FF particles. Images of particles equilibrated with high concentrations of protein revealed a significant difference in protein localization patterns, with the stained protein in XL occupying a markedly higher area fraction of the images. This suggests a higher volume available for adsorption and provides visual clues into how the consistently higher static capacity of these polymer-modified particles is manifested. Treatment of the XL particles with dextranase, an enzyme that breaks down dextran, resulted in a reduction of protein coverage, providing evidence that it is indeed the dextran that is responsible for the improved static capacity in this polymer-modified stationary phase. Imaging and image analysis techniques were also used to analyze the commercial CIM(TM) disk monolith. Two- and three

  20. A nano-graphite/paraffin phase change material with high thermal conductivity

    International Nuclear Information System (INIS)

    Li, Min

    2013-01-01

    Highlights: ► Paraffin and NG formed a nanoscale compound. ► The thermal conductivity increased gradually with the content of NG. ► The thermal conductivity of the material containing 10% NG were 0.9362 W/m K. - Abstract: Nano-graphite (NG)/paraffin composites were prepared as composite phase change materials. NG has the function of improving the thermal conductivity of the composite. The microstructure and thermal properties of the materials were examined with environmental scanning electron microscopy and differential scanning calorimetry. The results indicated that the NG layers were randomly dispersed in the paraffin, and the thermal conductivity increased gradually with the content of NG. Thermal conductivity of the material containing 10% NG were 0.9362 W/m K

  1. Liquid-phase microextraction combined with graphite furnace atomic absorption spectrometry: A review.

    Science.gov (United States)

    de la Calle, Inmaculada; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

    2016-09-14

    An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Regenerated silica gel as stationary phase on vacuum column chromatography to purify temulawak's extracts

    Science.gov (United States)

    Cahyono, Bambang; Maduwu, Ratna Dewi; Widayat, Suzery, Meiny

    2015-12-01

    Commercial silica gel only used once by many researchers and affected high cost for purification process, also less support the green chemistry program. This research focused in regeneration silica gel that used purification of temulawak's extracts (Curcuma xanthorrhiza Roxb) by vacuum column chromatography. Sample extracts (contains 10.1195±0.5971% of curcuminoids) was purified by vacuum column chromatography (pressure: 45 kPa, column: 100mm on length and 16mm on diameter). Ethanol 96% and acetone were compared as eluent. The amount of solvent and yield of curcuminoids used as indicator purification. The silica gel was regenerated with heating in 600°C for 8 hours The silica gels were analyzed by IR spectroscopy and X-ray diffraction. Furthermore, regenerated silica gel was used as the stationary phase in vacuum column chromatography under the same conditions with the previous purification. All the purification experiments were performed in three repetitions. Based on regression equation, y=0.132x+0.0011 (r2=0.9997) the yield of curcuminoids on purified products using ethanol as the eluent was improved 4.26% (to 14.3724±0.5749%) and by acetone was improved 3,03% (to 13.1450 ±0.6318%). The IR spectrum of both silica gel showed the same vibration profile and also there were three crystallinity peaks missing on its X-ray diffraction. Regenerated silica gel has the same performance with new silica gel in purification of temulawak's extract: by ethanol has increased 4.08% (14.1947±0.7415%) and 2.93% (13.0447±0.4822) by acetone. In addition, all purification products showed similar TLC profiles. Purification using regenerated silica gel as the adsorbent on vacuum column chromatography has exactly same potential with the new silica gel.

  3. Enantiodifferentiation of whisky and cognac lactones using gas chromatography with different cyclodextrin chiral stationary phases.

    Science.gov (United States)

    Schmarr, Hans-Georg; Mathes, Maximilian; Wall, Kristina; Metzner, Frank; Fraefel, Marius

    2017-09-22

    The chiral lactone 5-butyl-4-methyloxolan-2-one or 5-butyl-4-methyldihydro-2(3H)-furanone, often named whisky lactone, is found in oak wood, then contributing to the appreciated flavor of beverages stored in such wooden barrels. Its next higher homologue is named cognac lactone (5-pentyl-4-methyloxolan-2-one or 5-pentyl-4-methyldihydro-2(3H)-furanone), however is much less known, probably due to its minor concentration level. In order to study the direct enantioseparation of both lactones by gas chromatography on chiral stationary phases, individual enantiomers, particularly for cognac lactone were made available. This was achieved by baker's yeast reduction of synthesized ethyl 3-methyl-4-oxononanoate or, after hydrolysis, of the corresponding 4-ketoacid, that gave access to individual enantiomers of cognac lactone. Good enantioseparation was achieved for both whisky and cognac lactone with high values for the chiral resolution with 6-O-tert. butyl dimethylsilyl-2,3-dialkylated or 6-O-tert. butyl dimethylsilyl-2,3-diacylated cyclodextrin derivatives as chiral selectors. The influence of the nature and position of derivatization of the cyclodextrin moiety revealed a strong impact on the chiral recognition mechanism, as the investigated alkylated derivatives heptakis-(2,6-di-O-iso-pentyl-3-O-allyl)-β-cyclodextrin and octakis-(2,3-di-O-pentyl-6-O-methyl)-γ-cyclodextrin did not provide any or only minor chiral selectivity for the two lactones. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Enantiomeric separation of iridium (III) complexes using HPLC chiral stationary phases based on amylose derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Hee Eun; Seo, Na Hyeon; Hyun, Myung Ho [Dept. of Chemistry and Chemistry Institute for Functional Materials, Pusan National University, Busan (Korea, Republic of)

    2016-12-15

    Cyclometalated iridium (III) complexes formed with three identical cyclometalating (C-N) ligands (homoleptic) or formed with two cyclometalating (C-N) ligands and one ancillary (LX) ligand (heteroleptic) have been known as highly phosphorescent materials and, thus, they have been utilized as efficient phosphorescent dopants in organic light emitting diodes (OLEDs) 1–3 or as effective phosphorescent chemosensors. 4–7 Cylometalated iridium (III) complexes are chiral compounds consisting of lambda (Λ, left-handed) and delta (Δ, right-handed) isomers. Racemic cyclometa- lated iridium (III) complexes emit light with no net polarization, but optically active cyclometalated iridium (III) complexes emit circularly polarized light. 8,9 Circularly polarized light can be used in various fields including highly efficient three dimensional electronic devices, photo nic devices for optical data storage, biological assays, and others. 8,9 In order to obtain optically active cylometalated iridium (III) complexes and to determine the enantiomeric composition of optically active cylometalated iridium (III) complexes, liquid chromatogr aphic enantiomer separation method on chiral stationary phases (CSPs) has been used. For example, Okamoto and coworkers first reported the high performance liquid chromatographic (HPLC) direct enantiomeric separation of two homoleptic cylometalated iridium (III) complexes on immobilized amylose tris(3,5- dimethylphenylcarbamate) (Chiralpak IA), coated cellulose tris(3,5-dimethylphenylcarbamate) (Chiralc el OD), and coated cellulose tris(4-methylbenzoate) (Chiralce l OJ). 10 Supercritical fluid chromatography (SFC) was also used by Bernhard and coworkers for the enantiomeric separation of cylometalated iridium (III) complexes on coated amylose tris(3,5-dimethylphenylcarbamate) (Chiralpak AD-H). 8 However, the general use of the HPLC method for the direct enantiomeric separation of homoleptic.

  5. Regenerated silica gel as stationary phase on vacuum column chromatography to purify temulawak’s extracts

    International Nuclear Information System (INIS)

    Cahyono, Bambang; Maduwu, Ratna Dewi; Widayat,; Suzery, Meiny

    2015-01-01

    Commercial silica gel only used once by many researchers and affected high cost for purification process, also less support the green chemistry program. This research focused in regeneration silica gel that used purification of temulawak’s extracts (Curcuma xanthorrhiza Roxb) by vacuum column chromatography. Sample extracts (contains 10.1195±0.5971% of curcuminoids) was purified by vacuum column chromatography (pressure: 45 kPa, column: 100mm on length and 16mm on diameter). Ethanol 96% and acetone were compared as eluent. The amount of solvent and yield of curcuminoids used as indicator purification. The silica gel was regenerated with heating in 600°C for 8 hours The silica gels were analyzed by IR spectroscopy and X-ray diffraction. Furthermore, regenerated silica gel was used as the stationary phase in vacuum column chromatography under the same conditions with the previous purification. All the purification experiments were performed in three repetitions. Based on regression equation, y=0.132x+0.0011 (r 2 =0.9997) the yield of curcuminoids on purified products using ethanol as the eluent was improved 4.26% (to 14.3724±0.5749%) and by acetone was improved 3,03% (to 13.1450 ±0.6318%). The IR spectrum of both silica gel showed the same vibration profile and also there were three crystallinity peaks missing on its X-ray diffraction. Regenerated silica gel has the same performance with new silica gel in purification of temulawak’s extract: by ethanol has increased 4.08% (14.1947±0.7415%) and 2.93% (13.0447±0.4822) by acetone. In addition, all purification products showed similar TLC profiles. Purification using regenerated silica gel as the adsorbent on vacuum column chromatography has exactly same potential with the new silica gel

  6. Regenerated silica gel as stationary phase on vacuum column chromatography to purify temulawak’s extracts

    Energy Technology Data Exchange (ETDEWEB)

    Cahyono, Bambang; Maduwu, Ratna Dewi; Widayat,; Suzery, Meiny [Organic Chemistry Laboratory, Departement of Chemistry, Diponegoro University Jln Prof. Soedharto SH, Tembalang, Semarang 50275, Indonesia Tel / Fax: (024) 7460058 (Indonesia)

    2015-12-29

    Commercial silica gel only used once by many researchers and affected high cost for purification process, also less support the green chemistry program. This research focused in regeneration silica gel that used purification of temulawak’s extracts (Curcuma xanthorrhiza Roxb) by vacuum column chromatography. Sample extracts (contains 10.1195±0.5971% of curcuminoids) was purified by vacuum column chromatography (pressure: 45 kPa, column: 100mm on length and 16mm on diameter). Ethanol 96% and acetone were compared as eluent. The amount of solvent and yield of curcuminoids used as indicator purification. The silica gel was regenerated with heating in 600°C for 8 hours The silica gels were analyzed by IR spectroscopy and X-ray diffraction. Furthermore, regenerated silica gel was used as the stationary phase in vacuum column chromatography under the same conditions with the previous purification. All the purification experiments were performed in three repetitions. Based on regression equation, y=0.132x+0.0011 (r{sup 2}=0.9997) the yield of curcuminoids on purified products using ethanol as the eluent was improved 4.26% (to 14.3724±0.5749%) and by acetone was improved 3,03% (to 13.1450 ±0.6318%). The IR spectrum of both silica gel showed the same vibration profile and also there were three crystallinity peaks missing on its X-ray diffraction. Regenerated silica gel has the same performance with new silica gel in purification of temulawak’s extract: by ethanol has increased 4.08% (14.1947±0.7415%) and 2.93% (13.0447±0.4822) by acetone. In addition, all purification products showed similar TLC profiles. Purification using regenerated silica gel as the adsorbent on vacuum column chromatography has exactly same potential with the new silica gel.

  7. Enantiomeric separation of iridium (III) complexes using HPLC chiral stationary phases based on amylose derivatives

    International Nuclear Information System (INIS)

    Kim, Hee Eun; Seo, Na Hyeon; Hyun, Myung Ho

    2016-01-01

    Cyclometalated iridium (III) complexes formed with three identical cyclometalating (C-N) ligands (homoleptic) or formed with two cyclometalating (C-N) ligands and one ancillary (LX) ligand (heteroleptic) have been known as highly phosphorescent materials and, thus, they have been utilized as efficient phosphorescent dopants in organic light emitting diodes (OLEDs) 1–3 or as effective phosphorescent chemosensors. 4–7 Cylometalated iridium (III) complexes are chiral compounds consisting of lambda (Λ, left-handed) and delta (Δ, right-handed) isomers. Racemic cyclometa- lated iridium (III) complexes emit light with no net polarization, but optically active cyclometalated iridium (III) complexes emit circularly polarized light. 8,9 Circularly polarized light can be used in various fields including highly efficient three dimensional electronic devices, photo nic devices for optical data storage, biological assays, and others. 8,9 In order to obtain optically active cylometalated iridium (III) complexes and to determine the enantiomeric composition of optically active cylometalated iridium (III) complexes, liquid chromatogr aphic enantiomer separation method on chiral stationary phases (CSPs) has been used. For example, Okamoto and coworkers first reported the high performance liquid chromatographic (HPLC) direct enantiomeric separation of two homoleptic cylometalated iridium (III) complexes on immobilized amylose tris(3,5- dimethylphenylcarbamate) (Chiralpak IA), coated cellulose tris(3,5-dimethylphenylcarbamate) (Chiralc el OD), and coated cellulose tris(4-methylbenzoate) (Chiralce l OJ). 10 Supercritical fluid chromatography (SFC) was also used by Bernhard and coworkers for the enantiomeric separation of cylometalated iridium (III) complexes on coated amylose tris(3,5-dimethylphenylcarbamate) (Chiralpak AD-H). 8 However, the general use of the HPLC method for the direct enantiomeric separation of homoleptic

  8. Capillary electrochromatography of inorganic cations in open tubular columns with a controllable capacity multilayered stationary phase architecture

    Czech Academy of Sciences Publication Activity Database

    Kubáň, Pavel; Kubáň, P.; Kubáň, V.; Hauser, P.C.; Boček, Petr

    2008-01-01

    Roč. 1190, 1-2 (2008), s. 377-382 ISSN 0021-9673 R&D Projects: GA ČR GA203/08/1536; GA AV ČR IAA400310703; GA AV ČR IAA400310609 Institutional research plan: CEZ:AV0Z40310501 Keywords : contactless conductivity detection * open- tubular columns * stationary phases Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.756, year: 2008

  9. Role of nutrient limitation and stationary-phase existence in Klebsiella pneumoniae biofilm resistance to ampicillin and ciprofloxacin.

    Science.gov (United States)

    Anderl, Jeff N; Zahller, Jeff; Roe, Frank; Stewart, Philip S

    2003-04-01

    Biofilms formed by Klebsiella pneumoniae resisted killing during prolonged exposure to ampicillin or ciprofloxacin even though these agents have been shown to penetrate bacterial aggregates. Bacteria dispersed from biofilms into medium quickly regained most of their susceptibility. Experiments with free-floating bacteria showed that stationary-phase bacteria were protected from killing by either antibiotic, especially when the test was performed in medium lacking carbon and nitrogen sources. These results suggested that the antibiotic tolerance of biofilm bacteria could be explained by nutrient limitation in the biofilm leading to stationary-phase existence of at least some of the cells in the biofilm. This mechanism was supported by experimental characterization of nutrient availability and growth status in biofilms. The average specific growth rate of bacteria in biofilms was only 0.032 h(-1) compared to the specific growth rate of planktonic bacteria of 0.59 h(-1) measured in the same medium. Glucose did not penetrate all the way through the biofilm, and oxygen was shown to penetrate only into the upper 100 micro m. The specific catalase activity was elevated in biofilm bacteria to a level similar to that of stationary-phase planktonic cells. Transmission electron microscopy revealed that bacteria were affected by ampicillin near the periphery of the biofilm but were not affected in the interior. Taken together, these results indicate that K. pneumoniae in this system experience nutrient limitation locally within the biofilm, leading to zones in which the bacteria enter stationary phase and are growing slowly or not at all. In these inactive regions, bacteria are less susceptible to killing by antibiotics.

  10. Research on the transformation mechanism of graphite phase and microstructure in the heated region of gray cast iron by laser cladding

    Science.gov (United States)

    Liu, Yancong; Zhan, Xianghua; Yi, Peng; Liu, Tuo; Liu, Benliang; Wu, Qiong

    2018-03-01

    A double-track lap cladding experiment involving gray cast iron was established to investigate the transformation mechanism of graphite phase and microstructure in a laser cladding heated region. The graphite phase and microstructure in different heated regions were observed under a microscope, and the distribution of elements in various heated regions was analyzed using an electron probe. Results show that no graphite existed in the cladding layer and in the middle and upper parts of the binding region. Only some of the undissolved small graphite were observed at the bottom of the binding region. Except the refined graphite size, the morphological characteristics of substrate graphite and graphite in the heat-affected zone were similar. Some eutectic clusters, which grew along the direction of heat flux, were observed in the heat-affected zone whose microstructure was transformed into a mixture of austenite, needle-like martensite, and flake graphite. Needle-like martensite around graphite was fine, but this martensite became sparse and coarse when it was away from graphite. Some martensite clusters appeared in the local area near the binding region, and the carbon atoms in the substrate did not diffuse into the cladding layer through laser cladding, which only affected the bonding area and the bottom of the cladding layer.

  11. Preparation of a ribonucleic acid-(polyamidoamine)-(zirconia-urea-formaldehyde resin) high-performance liquid affinity chromatographic stationary phase.

    Science.gov (United States)

    Lei, S; Yu, S; Zhao, C

    2001-07-01

    A preparative method for a high-performance liquid affinity chromatographic (HPLAC) stationary phase is described. The 3- to 5-microm nonporous composite spherical microparticles of zirconia and urea-formaldehyde (UF) resin are synthesized through the reaction of zirconyl chloride with hexamethylene tetra-amine and urea, and then it is used as the matrix of the HPLAC stationary phase of which the diameter and structure are determined by scanning electron microscopy. In a methanol medium, the polyamidoamine (PAMAM) starburst dentritic spacer arms are linked with the imido-groups on the surface of the matrix by the Michael addition reaction with methyl acrylate and the amination reaction with ethylene diamine. After repeating these steps in triplets, amine-terminated dentritic spacer arms with a generation of 3 are obtained. The topological structure of the spacer arms is examined by solid-state 13C NMR. The Br-substituted ribonucleic acid (RNA) ligand is obtained by the reaction of liquid bromine with RNA and bonded to the dendritic spacer arms of the matrix in a solution of NaOH (pH 9-11). The binding capacity of RNA is measured by UV spectrophotometry. A new type of stationary phase--RNA-(PAMAM)-(zirconia-UF resin--for HPLAC, which possesses starburst dendritic spacer arms, is synthesized and used for the separation of biological macromolecules.

  12. Micro-fabricated semi-packed column for gas chromatography by using functionalized parylene as a stationary phase

    International Nuclear Information System (INIS)

    Nakai, T; Nishiyama, S; Shuzo, M; Delaunay, J-J; Yamada, I

    2009-01-01

    The conformal coating of effective stationary phases onto micro-fabricated columns having complex geometries such as semi-packed columns poses a real challenge. Here, we report for the first time the conformal coating of a semi-packed column with amino-functionalized parylene diX-AM (poly-aminomethyl-[2,2]-paracyclophane), which was found to be an effective stationary-phase material for the chromatography of short-retention-time compounds. A semi-packed column (consisting of a zigzag array of 30 µm square micro-pillars in a 1.0 m long, 180 µm wide and 230 µm deep channel) and an open tubular column (1.0 m long, 160 µm wide and 230 µm deep channel) used for comparison purposes were micro-fabricated on silicon that was subsequently coated with diX-AM parylene and thermally bonded. The chromatograms recorded on a commercial gas chromatograph demonstrated the usefulness of the conformal diX-AM coating as a stationary phase for semi-packed columns. The separation efficiency of the semi-packed column was found to be more than ten times that of the open tubular column

  13. A stationary phase solution for mountain waves with application to mesospheric mountain waves generated by Auckland Island

    Science.gov (United States)

    Broutman, Dave; Eckermann, Stephen D.; Knight, Harold; Ma, Jun

    2017-01-01

    A relatively general stationary phase solution is derived for mountain waves from localized topography. It applies to hydrostatic, nonhydrostatic, or anelastic dispersion relations, to arbitrary localized topography, and to arbitrary smooth vertically varying background temperature and vector wind profiles. A simple method is introduced to compute the ray Jacobian that quantifies the effects of horizontal geometrical spreading in the stationary phase solution. The stationary phase solution is applied to mesospheric mountain waves generated by Auckland Island during the Deep Propagating Gravity Wave Experiment. The results are compared to a Fourier solution. The emphasis is on interpretations involving horizontal geometrical spreading. The results show larger horizontal geometrical spreading for nonhydrostatic waves than for hydrostatic waves in the region directly above the island; the dominant effect of horizontal geometrical spreading in the lower ˜30 km of the atmosphere, compared to the effects of refraction and background density variation; and the enhanced geometrical spreading due to directional wind in the approach to a critical layer in the mesosphere.

  14. Continuous Carbon Nanotube-Ultrathin Graphite Hybrid Foams for Increased Thermal Conductivity and Suppressed Subcooling in Composite Phase Change Materials.

    Science.gov (United States)

    Kholmanov, Iskandar; Kim, Jaehyun; Ou, Eric; Ruoff, Rodney S; Shi, Li

    2015-12-22

    Continuous ultrathin graphite foams (UGFs) have been actively researched recently to obtain composite materials with increased thermal conductivities. However, the large pore size of these graphitic foams has resulted in large thermal resistance values for heat conduction from inside the pore to the high thermal conductivity graphitic struts. Here, we demonstrate that the effective thermal conductivity of these UGF composites can be increased further by growing long CNT networks directly from the graphite struts of UGFs into the pore space. When erythritol, a phase change material for thermal energy storage, is used to fill the pores of UGF-CNT hybrids, the thermal conductivity of the UGF-CNT/erythritol composite was found to increase by as much as a factor of 1.8 compared to that of a UGF/erythritol composite, whereas breaking the UGF-CNT bonding in the hybrid composite resulted in a drop in the effective room-temperature thermal conductivity from about 4.1 ± 0.3 W m(-1) K(-1) to about 2.9 ± 0.2 W m(-1) K(-1) for the same UGF and CNT loadings of about 1.8 and 0.8 wt %, respectively. Moreover, we discovered that the hybrid structure strongly suppresses subcooling of erythritol due to the heterogeneous nucleation of erythritol at interfaces with the graphitic structures.

  15. Preparation, characterization and application of a reversed phase liquid chromatography/hydrophilic interaction chromatography mixed-mode C18-DTT stationary phase.

    Science.gov (United States)

    Wang, Qing; Long, Yao; Yao, Lin; Xu, Li; Shi, Zhi-Guo; Xu, Lanying

    2016-01-01

    A mixed-mode chromatographic stationary phase, C18-DTT (dithiothreitol) silica (SiO2) was prepared through "thiol-ene" click chemistry. The obtained material was characterized by fourier transform infrared spectroscope, nitrogen adsorption analysis and contact angle analysis. Chromatographic performance of the C18-DTT was systemically evaluated by studying the effect of acetonitrile content, pH, buffer concentration of the mobile phase and column temperature. It was demonstrated that the novel stationary phase possessed reversed phase liquid chromatography (RPLC)/hydrophilic interaction liquid chromatography (HILIC) mixed-mode property. The stop-flow test revealed that C18-DTT exhibited excellent compatibility with 100% aqueous mobile phase. Additionally, the stability and column-to-column reproducibility of the C18-DTT material were satisfactory, with relative standard deviations of retention factor of the tested analytes (verapamil, fenbufen, guanine, tetrandrine and nicotinic acid) in the range of 1.82-3.72% and 0.85-1.93%, respectively. Finally, the application of C18-DTT column was demonstrated in the separation of non-steroidal anti-inflammatory drugs, aromatic carboxylic acids, alkaloids, nucleo-analytes and polycyclic aromatic hydrocarbons. It had great resolving power in the analysis of various compounds in HILIC and RPLC chromatographic conditions and was a promising RPLC/HILIC mixed-mode stationary phase. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. [Detecting Thallium in Water Samples using Dispersive Liquid Phase Microextraction-Graphite Furnace Atomic Absorption Spectroscopy].

    Science.gov (United States)

    Zhu, Jing; Li, Yan; Zheng, Bo; Tang, Wei; Chen, Xiao; Zou, Xiao-li

    2015-11-01

    To develope a method of solvent demulsification dispersive liquid phase microextraction (SD-DLPME) based on ion association reaction coupled with graphite furnace atomic absorption spectroscopy (GFAAS) for detecting thallium in water samples. Methods Thallium ion in water samples was oxidized to Tl(III) with bromine water, which reacted with Cl- to form TlCl4-. The ionic associated compound with trioctylamine was obtained and extracted. DLPME was completed with ethanol as dispersive solvent. The separation of aqueous and organic phase was achieved by injecting into demulsification solvent without centrifugation. The extractant was collected and injected into GFAAS for analysis. With palladium colloid as matrix modifier, a two step drying and ashing temperature programming process was applied for high precision and sensitivity. The linear range was 0.05-2.0 microg/L, with a detection limit of 0.011 microg/L. The relative standard derivation (RSD) for detecting Tl in spiked water sample was 9.9%. The spiked recoveries of water samples ranged from 94.0% to 103.0%. The method is simple, sensitive and suitable for batch analysis of Tl in water samples.

  17. Thermal Characterization of Lauric-Stearic Acid/Expanded Graphite Eutectic Mixture as Phase Change Materials.

    Science.gov (United States)

    Zhu, Hua; Zhang, Peng; Meng, Zhaonan; Li, Ming

    2015-04-01

    The eutectic mixture of lauric acid (LA) and stearic acid (SA) is a desirable phase change material (PCM) due to the constant melting temperature and large latent heat. However, its poor thermal conductivity has hampered its broad utilization. In the present study, pure LA, SA and the mixtures with various mass fractions of LA-SA were used as the basic PCMs, and 10 wt% expanded graphite (EG) was added to enhance the thermal conductivities. The phase change behaviors, microstructural analysis, thermal conductivities and thermal stabilities of the mixtures of PCMs were investigated by differential scanning calorimetry (DSC), scanning electronic microscope (SEM), transient plane source (TPS) and thermogravimetric analysis (TGA), respectively. The results show that the LA-SA binary mixture of mixture ratio of 76.3 wt%: 23.7 wt% forms an eutectic mixture, which melts at 38.99 °C and has a latent heat of 159.94 J/g. The melted fatty acids are well absorbed by the porous network of EG and they have a good thermal stability. Furthermore, poor thermal conductivities can be well enhanced by the addition of EG.

  18. High performance liquid chromatographic separation of eight drugs collected in Chinese Pharmacopoeia 2010 on amylose ramification chiral stationary phase

    Directory of Open Access Journals (Sweden)

    Yan Wang

    2012-10-01

    Full Text Available The enantiomers separation of eight pharmaceutical racemates collected in Chinese Pharmacopoeia 2010 (Ch.P2010, including nitrendipine, felodipine, omeprazole, praziquantel, sulpiride, clenbuterol hydrochloride, verapamil hydrochloride and chlorphenamine maleate, was performed on chiral stationary phase of amylose ramification by high performance liquid chromatography (HPLC on Chiralpak AD-H column and Chiralpak AS-H column with the mobile phase consisted of isopropanol and n-hexane. The detection wavelength and the flow rate were set at 254 nm and 0.7 mL/min, respectively. The effects of proportion of organic additives, alcohol displacer and temperature on the separation were investigated. The results indicated that eight chiral drugs were separated on chiral stationary phase of amylase ramification in normal phase chromatographic system. The chromatographic retention and resolution of enantiomers were adjusted by factors, including the changes of the concentration of alcohol displacer in mobile phase, organic alkaline modifier and column temperature. It was shown that the resolution was improved with reducing concentration of alcohol displacer. When the concentration of organic alkaline modifier was 0.2%, the resolution and the peak shape were fairly good. Most racemates mentioned above had the best resolution at column temperature of 25 °C. The best temperature should be kept unchanged in the process of separation so as to obtain stable separation results.

  19. A phase angle based diagnostic scheme to planetary gear faults diagnostics under non-stationary operational conditions

    Science.gov (United States)

    Feng, Ke; Wang, Kesheng; Ni, Qing; Zuo, Ming J.; Wei, Dongdong

    2017-11-01

    Planetary gearbox is a critical component for rotating machinery. It is widely used in wind turbines, aerospace and transmission systems in heavy industry. Thus, it is important to monitor planetary gearboxes, especially for fault diagnostics, during its operational conditions. However, in practice, operational conditions of planetary gearbox are often characterized by variations of rotational speeds and loads, which may bring difficulties for fault diagnosis through the measured vibrations. In this paper, phase angle data extracted from measured planetary gearbox vibrations is used for fault detection under non-stationary operational conditions. Together with sample entropy, fault diagnosis on planetary gearbox is implemented. The proposed scheme is explained and demonstrated in both simulation and experimental studies. The scheme proves to be effective and features advantages on fault diagnosis of planetary gearboxes under non-stationary operational conditions.

  20. Two dimensional reversed-phase-reversed-phase separations isomeric separations incorporating C18 and carbon clad zirconia stationary phases.

    Science.gov (United States)

    Gray, Michael; Dennis, Gary R; Wormell, Paul; Shalliker, R Andrew; Slonecker, Patrick

    2002-11-01

    Informational theory and a geometric approach to factor analysis were employed to evaluate the degree of orthogonality of a two-dimensional reversed-phase-reversed-phase chromatographic system. The system incorporated a C18 column as one dimension and a carbon clad zirconia column as the second dimension. In order to study the resolving power of this system, the separation of a sample matrix containing an artificial mix of 32 isomers (structural and diastereoisomers) was evaluated. Using this system, between 25 and 28 of the 32 isomers could be separated, depending on the mobile phase combinations--with resolution that could not possibly be achieved in a single one dimensional separation. The results from this study indicate that in order to fully evaluate the resolving power of a 2D system multiple methods of analysis are most appropriate. This becomes increasingly important when the sample contains components that are very closely related and the retention of solutes is clustered in one quadrant of the 2D space. Ultimately, the usefulness of the 2D separation is determined by the goals of analyst.

  1. Increased lignocellulosic inhibitor tolerance of Saccharomyces cerevisiae cell populations in early stationary phase.

    Science.gov (United States)

    Narayanan, Venkatachalam; Schelin, Jenny; Gorwa-Grauslund, Marie; van Niel, Ed Wj; Carlquist, Magnus

    2017-01-01

    Production of second-generation bioethanol and other bulk chemicals by yeast fermentation requires cells that tolerate inhibitory lignocellulosic compounds at low pH. Saccharomyces cerevisiae displays high plasticity with regard to inhibitor tolerance, and adaptation of cell populations to process conditions is essential for reaching efficient and robust fermentations. In this study, we assessed responses of isogenic yeast cell populations in different physiological states to combinations of acetic acid, vanillin and furfural at low pH. We found that cells in early stationary phase (ESP) exhibited significantly increased tolerance compared to cells in logarithmic phase, and had a similar ability to initiate growth in the presence of inhibitors as pre-adapted cells. The ESP cultures consisted of subpopulations with different buoyant cell densities which were isolated with flotation and analysed separately. These so-called quiescent (Q) and non-quiescent (NQ) cells were found to possess similar abilities to initiate growth in the presence of lignocellulosic inhibitors at pH 3.7, and had similar viabilities under static conditions. Therefore, differentiation into Q-cells was not the cause for increased tolerance of ESP cultures. Flow cytometry analysis of cell viability, intracellular pH and reactive oxygen species levels revealed that tolerant cell populations had a characteristic response upon inhibitor perturbations. Growth in the presence of a combination of inhibitors at low pH correlated with pre-cultures having a high frequency of cells with low pH i and low ROS levels. Furthermore, only a subpopulation of ESP cultures was able to tolerate lignocellulosic inhibitors at low pH, while pre-adapted cell populations displayed an almost uniform high tolerance to the adverse condition. This was in stark contrast to cell populations growing exponentially in non-inhibitory medium that were uniformly sensitive to the inhibitors at low pH. ESP cultures of S. cerevisiae

  2. [Preparation of 1 µm non-porous C18 silica gel stationary phase for chiral-pressurized capillary electrochromatography].

    Science.gov (United States)

    Lu, Yangfang; Wang, Hui; Wang, Guiming; Wang, Yan; Gu, Xue; Yan, Chao

    2015-03-01

    Non-porous C18 silica gel stationary phase (1 µm) was prepared and applied to chiral separation in pressurized capillary electrochromatography (pCEC) for the enantioseparation of various basic compounds. The non-porous silica particles (1 µm) were synthesized using modified St6ber method. C18 stationary phase (1 µm) was prepared by immobilization of chloro-dimethyl-octadecylsilane. Using carboxymethyl-β-cyclodextrin (CM-β-CD) as the chiral additive, the pCEC conditions including the content of acetonitrile (ACN), concentration of buffer, pH, the concentration of chiral additive and flow rate as well as applied voltage were investigated to obtain the optimal pCEC conditions for the separation of four basic chiral compounds. The column provided an efficiency of up to 190,000 plates/m. Bupropion hydrochloride, clenbuterol hydrochloride, metoprolol tartrate, and esmolol hydrochloride were baseline separated under the conditions of 5 mmol/L ammonium acetate buffer at pH 4. 0 with 20% (v/ v) acetonitrile, and 15 mmol/L CM-β-CD as the chiral additive. The applied voltage was 2 kV and flow rate was 0.03 mL/min with splitting ratio of 300:1. The resolution were 1.55, 2.82, 1. 69, 1. 70 for bupropion hydrochloride, clenbuterol hydrochloride, metoprolol tartrate, esmolol hydrochloride, respectively. The C18 coverage was improved by repeating silylation method. The synthesized 1 µm C18 packings have better mechanical strength and longer service life because of the special, non-porous structure. The column used in pCEC mode showed better separation of the racemates and a higher rate compared with those used in the capillary liquid chromatography (cLC) mode. This study provided an alternative way for the method of pCEC enantioseparation with chiral additives in the mobile phase and demonstrated the feasibility of micron particle stationary phase in chiral separation.

  3. Exploring the enantiorecognition mechanism of Cinchona alkaloid-based zwitterionic chiral stationary phases and the basic trans-paroxetine enantiomers.

    Science.gov (United States)

    Sardella, Roccaldo; Macchiarulo, Antonio; Urbinati, Fabrizio; Ianni, Federica; Carotti, Andrea; Kohout, Michal; Lindner, Wolfgang; Péter, Antal; Ilisz, István

    2017-11-21

    The enantiomers of trans-paroxetine (the selectand) were separated on four chiral stationary phases incorporating either quinine [ZWIX(+), ZWIX(+A)] or quinidine [ZWIX(-), ZWIX(-A)] and (R,R)-aminocyclohexanesulfonic acid [in ZWIX(-), and ZWIX(+A)] or (S,S)-aminocyclohexanesulfonic acid [in ZWIX(+), and ZWIX(-A)] chiral selectors. The zwitterion nature of the phases is due to the presence of either (R,R)- or (S,S)-aminocyclohexanesulfonic acid in the selector structure bearing the quinuclidine moiety. ZWIX(+) and ZWIX(-) phases are available on the market with the commercial names CHIRALPAK ZWIX(+) and CHIRALPAK ZWIX(-), respectively. With the aim of rationalizing the enantiomer elution order with the above chiral stationary phases, a molecular dynamic protocol was applied and two energetic parameters were initially measured: selectand conformational energy and selectand interaction energy. In the search for other descriptors allowing a better fitting with the experimental evidences, in the present work we consider an energetic parameter, defined as the selector conformational energy, which resulted to be relevant in the explanation of the experimental elution order in most of the cases. Very importantly, the computational data produced by the present study strongly support the outstanding role of the conformational energy of the chiral selector as it interacts with the analytes. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Preparation and evaluation of surface-bonded tricationic ionic liquid silica as stationary phases for high-performance liquid chromatography.

    Science.gov (United States)

    Qiao, Lizhen; Shi, Xianzhe; Lu, Xin; Xu, Guowang

    2015-05-29

    Two tricationic ionic liquids were prepared and then bonded onto the surface of supporting silica materials through "thiol-ene" click chemistry as new stationary phases for high-performance liquid chromatography. The obtained columns of tricationic ionic liquids were evaluated respectively in the reversed-phase liquid chromatography (RPLC) mode and hydrophilic interaction liquid chromatography (HILIC) mode, and possess ideal column efficiency of 80,000 plates/m in the RPLC mode with naphthalene as the test solute. The tricationic ionic liquid stationary phases exhibit good hydrophobic and shape selectivity to hydrophobic compounds, and RPLC retention behavior with multiple interactions. In the HILIC mode, the retention and selectivity were evaluated through the efficient separation of nucleosides and bases as well as flavonoids, and the typical HILIC retention behavior was demonstrated by investigating retention changes of hydrophilic solutes with water volume fraction in mobile phase. The results show that the tricationic ionic liquid columns possess great prospect for applications in analysis of hydrophobic and hydrophilic samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Preparation and characterization of mesoporous silicas modified with chiral selectors as stationary phase for high-performance liquid chromatography.

    Science.gov (United States)

    Pérez-Quintanilla, Damián; Morante-Zarcero, Sonia; Sierra, Isabel

    2014-01-15

    New hybrid materials were prepared as novel chiral stationary phases (CSPs) for high-performance liquid chromatography (HPLC). Pure mesoporous silica (SM) and ethylene-bridged periodic mesostructured organosilica (PMO) were functionalized, by a post-synthesis method, with derivates of erythromycin and vancomycin. N2 adsorption-desorption measurements, XRD, FT-IR, MAS NMR, SEM, TEM and elemental analysis were used to characterize the physico-chemical properties of these mesostructured materials, before and after the modification process. The synthesized particles had non-symmetrical 3-D wormhole-like mesostructure, spherical morphology, and a mean pore diameter between 53 and 59 Å. CSPs prepared were tested for the separation of four chiral β-blockers (atenolol, metoprolol, pindolol and propranolol) in normal phase (NP) and polar organic phase (PO) elution modes. Much stronger chiral interaction was observed in vancomycin-modified silicas. Results obtained in these preliminary studies will permit in future works to improve the synthesis route in order to design mesoporous materials with better performance as a chiral stationary phase for HPLC. Copyright © 2013 Elsevier Inc. All rights reserved.

  6. Preparation and chromatographic evaluation of a newly designed steviol glycoside modified-silica stationary phase in hydrophilic interaction liquid chromatography and reversed phase liquid chromatography.

    Science.gov (United States)

    Liang, Tu; Fu, Qing; Shen, Aijin; Wang, Hui; Jin, Yu; Xin, Huaxia; Ke, Yanxiong; Guo, Zhimou; Liang, Xinmiao

    2015-04-03

    A diterpene glycoside compound, rebaudioside A (commonly abbreviated as RA), was immobilized onto porous silica surface through "thiol-ene" click chemistry strategy. The successful immobilization of the RA on the silica support was confirmed by FT-IR and elemental analysis. Chromatographic characteristics of the new stationary phase, named Click TE-RA, were evaluated by a set of diverse analytes such as carbohydrates, nucleosides, and organic acids in hydrophilic interaction liquid chromatography (HILIC) mode. The effects of water content, buffer pH and concentration were investigated and a typical HILIC retention feature of Click TE-RA was observed at high organic modifier content. The Click TE-RA stationary phase was further studied by a series of glycoside compounds. Tunable retention mechanisms from hydrophilic to hydrophobic interactions were observed. Separation of very polar compounds including oligosaccharides, nucleic acid bases and nucleosides using Click TE-RA in HILIC mode was successfully accomplished. In addition, separation of saponins both in HILIC and reversed-phase liquid chromatography (RPLC) modes was performed, demonstrating the presence of orthogonality between two different modes on Click TE-RA column. The multiple interactions induced by polar sugar group and hydrophobic aglycone group allowed this Click TE-RA to serve as a multi-mode stationary phase in two-dimensional liquid chromatography. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Preparation and thermal energy storage properties of paraffin/expanded graphite composite phase change material

    International Nuclear Information System (INIS)

    Zhang, Zhengguo; Zhang, Ni; Peng, Jing; Fang, Xiaoming; Gao, Xuenong; Fang, Yutang

    2012-01-01

    Highlights: ► EG was obtained by microwave irradiation to prepare the paraffin/EG composite PCM. ► Composite PCM was characterized by XRD to investigate the chemical compatibility. ► Temperature profiles of the composite PCM were obtained during thermal energy storage. -- Abstract: The paraffin/expanded graphite (EG) composite phase change material (PCM) was prepared by absorbing liquid paraffin into EG, in which paraffin was chosen as the PCM. EG was produced by microwave irradiation performed at room temperature. It was found that the EG prepared at 800 W irradiation power for 10 s exhibited the maximum sorption capacity of 92 wt% for paraffin. Scanning electron microscopy images showed that paraffin was uniformly dispersed in the pores of EG. Differential scanning calorimeter analysis indicated that the melting temperature of the composite PCM was close to that of paraffin, and its latent heat was equivalent to the calculated value based on the mass fraction of paraffin in the composite. X-ray diffraction analysis showed that the composite PCM was just a combination of paraffin with EG, and no new substance was produced. Thermal energy storage performance of the composite PCM was tested in a latent thermal energy storage (LTES) system. Transients of axial and radial temperature profiles were obtained in the LTES for the composite PCM and paraffin. The thermal energy storage charging duration for the composite PCM was reduced obviously compared to paraffin.

  8. Selective Essential Oils from Spice or Culinary Herbs Have High Activity against Stationary Phase and Biofilm Borrelia burgdorferi.

    Science.gov (United States)

    Feng, Jie; Zhang, Shuo; Shi, Wanliang; Zubcevik, Nevena; Miklossy, Judith; Zhang, Ying

    2017-01-01

    Although the majority of patients with acute Lyme disease can be cured with the standard 2-4 week antibiotic treatment, about 10-20% of patients continue suffering from chronic symptoms described as posttreatment Lyme disease syndrome. While the cause for this is debated, one possibility is that persister bacteria are not killed by the current Lyme antibiotics and remain active in the system. It has been reported that essential oils have antimicrobial activities and some have been used by patients with persisting Lyme disease symptoms. However, the activity of essential oils against the causative agent Borrelia burgdorferi ( B. burgdorferi ) has not been well studied. Here, we evaluated the activity of 34 essential oils against B. burgdorferi stationary phase culture as a model for persister bacteria. We found that not all essential oils had activity against the B. burgdorferi stationary phase culture, with top five essential oils (oregano, cinnamon bark, clove bud, citronella, and wintergreen) at a low concentration of 0.25% showing high anti-persister activity that is more active than the known persister drug daptomycin. Interestingly, some highly active essential oils were found to have excellent anti-biofilm ability as shown by their ability to dissolve the aggregated biofilm-like structures. The top three hits, oregano, cinnamon bark, and clove bud completely eradicated all viable cells without any regrowth in subculture in fresh medium, whereas but not citronella and wintergreen did not have this effect. Carvacrol was found to be the most active ingredient of oregano oil showing excellent activity against B. burgdorferi stationary phase cells, while other ingredients of oregano oil p-cymene and α-terpinene had no apparent activity. Future studies are needed to characterize and optimize the active essential oils in drug combination studies in vitro and in vivo and to address their safety and pharmacokinetic properties before they can be considered as a

  9. Selective Essential Oils from Spice or Culinary Herbs Have High Activity against Stationary Phase and Biofilm Borrelia burgdorferi

    Science.gov (United States)

    Feng, Jie; Zhang, Shuo; Shi, Wanliang; Zubcevik, Nevena; Miklossy, Judith; Zhang, Ying

    2017-01-01

    Although the majority of patients with acute Lyme disease can be cured with the standard 2–4 week antibiotic treatment, about 10–20% of patients continue suffering from chronic symptoms described as posttreatment Lyme disease syndrome. While the cause for this is debated, one possibility is that persister bacteria are not killed by the current Lyme antibiotics and remain active in the system. It has been reported that essential oils have antimicrobial activities and some have been used by patients with persisting Lyme disease symptoms. However, the activity of essential oils against the causative agent Borrelia burgdorferi (B. burgdorferi) has not been well studied. Here, we evaluated the activity of 34 essential oils against B. burgdorferi stationary phase culture as a model for persister bacteria. We found that not all essential oils had activity against the B. burgdorferi stationary phase culture, with top five essential oils (oregano, cinnamon bark, clove bud, citronella, and wintergreen) at a low concentration of 0.25% showing high anti-persister activity that is more active than the known persister drug daptomycin. Interestingly, some highly active essential oils were found to have excellent anti-biofilm ability as shown by their ability to dissolve the aggregated biofilm-like structures. The top three hits, oregano, cinnamon bark, and clove bud completely eradicated all viable cells without any regrowth in subculture in fresh medium, whereas but not citronella and wintergreen did not have this effect. Carvacrol was found to be the most active ingredient of oregano oil showing excellent activity against B. burgdorferi stationary phase cells, while other ingredients of oregano oil p-cymene and α-terpinene had no apparent activity. Future studies are needed to characterize and optimize the active essential oils in drug combination studies in vitro and in vivo and to address their safety and pharmacokinetic properties before they can be considered as a

  10. Ionic liquids as water-compatible GC stationary phases for the analysis of fragrances and essential oils.

    Science.gov (United States)

    Cagliero, Cecilia; Bicchi, Carlo; Cordero, Chiara; Liberto, Erica; Rubiolo, Patrizia; Sgorbini, Barbara

    2018-02-13

    Fragrances and products deriving from essential oils are often formulated or diluted in aqueous media, usually ethanol/water. Gas chromatography (GC) is the technique of choice to analyze volatiles. However, when using columns coated with conventional stationary phases, its application to aqueous samples often requires time-consuming and/or discriminative sample preparation techniques to extract the target analytes from the aqueous medium, so as to avoid its direct injection. In GC with conventional columns, water produces peak asymmetry, poor sensitivity and efficiency, strong adsorption, stationary phase degradation, and, last but not least, it is not easy to detect reliably when present in high amounts. In 2012, Armstrong's group introduced new fully water-compatible ionic-liquid (IL)-based GC capillary columns based on phosphonium and imidazolium derivative cations combined with trifluoromethanesulphonate. These columns were recently made available commercially by Supelco, under the trade name Watercol™. These derivatives maintain IL's unique selectivity and chromatographic properties, and enable water to be used as injection solvent, thus avoiding the sample preparation procedures required by conventional columns. This study reports and critically discusses the results of commercially available water-compatible IL columns for direct analysis of aqueous samples in the fragrance and essential oil fields by GC with thermal conductivity (TCD) and/or flame ionization detectors (FID). The results showed that water-compatible IL-based stationary phases can successfully be adopted for qualitative and quantitative analysis of fragrances and essential oils directly diluted in aqueous solvents. On the other hand, the study also shows that their inertness needs to be further increased and (possibly) the range of operative temperature extended when water is the main solvent of the sample.

  11. Selective Essential Oils from Spice or Culinary Herbs Have High Activity against Stationary Phase and Biofilm Borrelia burgdorferi

    Directory of Open Access Journals (Sweden)

    Jie Feng

    2017-10-01

    Full Text Available Although the majority of patients with acute Lyme disease can be cured with the standard 2–4 week antibiotic treatment, about 10–20% of patients continue suffering from chronic symptoms described as posttreatment Lyme disease syndrome. While the cause for this is debated, one possibility is that persister bacteria are not killed by the current Lyme antibiotics and remain active in the system. It has been reported that essential oils have antimicrobial activities and some have been used by patients with persisting Lyme disease symptoms. However, the activity of essential oils against the causative agent Borrelia burgdorferi (B. burgdorferi has not been well studied. Here, we evaluated the activity of 34 essential oils against B. burgdorferi stationary phase culture as a model for persister bacteria. We found that not all essential oils had activity against the B. burgdorferi stationary phase culture, with top five essential oils (oregano, cinnamon bark, clove bud, citronella, and wintergreen at a low concentration of 0.25% showing high anti-persister activity that is more active than the known persister drug daptomycin. Interestingly, some highly active essential oils were found to have excellent anti-biofilm ability as shown by their ability to dissolve the aggregated biofilm-like structures. The top three hits, oregano, cinnamon bark, and clove bud completely eradicated all viable cells without any regrowth in subculture in fresh medium, whereas but not citronella and wintergreen did not have this effect. Carvacrol was found to be the most active ingredient of oregano oil showing excellent activity against B. burgdorferi stationary phase cells, while other ingredients of oregano oil p-cymene and α-terpinene had no apparent activity. Future studies are needed to characterize and optimize the active essential oils in drug combination studies in vitro and in vivo and to address their safety and pharmacokinetic properties before they can be

  12. Modeling, analysis, and design of stationary reference frame droop controlled parallel three-phase voltage source inverters

    DEFF Research Database (Denmark)

    Vasquez, Juan Carlos; Guerrero, Josep M.; Savaghebi, Mehdi

    2011-01-01

    Power electronics based microgrids consist of a number of voltage source inverters (VSIs) operating in parallel. In this paper, the modeling, control design, and stability analysis of three-phase VSIs are derived. The proposed voltage and current inner control loops and the mathematical models...... of the VSIs were based on the stationary reference frame. A hierarchical control for the paralleled VSI system was developed based on three levels. The primary control includes the droop method and the virtual impedance loops, in order to share active and reactive power. The secondary control restores...

  13. Resolution and determination of enantiomeric purity of new chiral derivatives of xanthones using polysaccharide-based stationary phases.

    Science.gov (United States)

    Fernandes, Carla; Brandão, Pedro; Santos, Alexandre; Tiritan, Maria Elizabeth; Afonso, Carlos; Cass, Quezia B; Pinto, Madalena M

    2012-12-21

    The enantioresolution and determination of the enantiomeric purity of 24 new chiral derivatives of xanthones (CDXs) were investigated on polysaccharide-based chiral stationary phases (CSPs). The tris-3,5-dimethylphenylcarbamates of cellulose and amylose and tris-3,5-dimethoxyphenylcarbamate of amylose were selected as CSPs for this work. The separation of enantiomeric mixtures of CDXs was explored under multimodal elution conditions. All the enantiomeric mixtures of CDXs were enantioseparated with very high enantioselectivity and resolution with α and R(S) ranging from 1.43 to 12.41 and from 1.48 to 10.29, respectively. The best performances were achieved on amylose tris-3,5-dimethylphenylcarbamate stationary phase under polar organic elution conditions. Furthermore the enantiomeric purity for all the CDXs was measured, achieving values higher than 99%. Based on the obtained results, the influence of the mobile phases and structural features of the CSPs and CDXs on chiral discrimination are also discussed. Copyright © 2012 Elsevier B.V. All rights reserved.

  14. Effects of supercritical fluid chromatography conditions on enantioselectivity and performance of polyproline-derived chiral stationary phases.

    Science.gov (United States)

    Novell, Arnau; Méndez, Alberto; Minguillón, Cristina

    2015-07-17

    The chromatographic behaviour and performance of four polyproline-derived chiral stationary phases (CSPs) were tested using supercritical fluid chromatography (SFC). A series of structurally related racemic compounds, whose enantioseparation was proved to be sensitive to the type of mobile phase used in NP-HPLC, were chosen to be tested in the SFC conditions. Good enantioselection ability was shown by the CSPs for the analytes tested in the new conditions. Resolution, efficiency and analysis time, were considerably improved with respect to NP-HPLC when CO2/alcohol mobile phases were used. Monolithic columns clearly show enhanced chromatographic parameters and improved performance respect to their bead-based counterparts. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Preparative separation of the polar part from the rhizomes of Anemarrhena asphodeloides using a hydrophilic C18 stationary phase.

    Science.gov (United States)

    Cai, Jianfeng; Xin, Huaxia; Cheng, Lingping; Fu, YanHui; Jiang, Dasen; Feng, Jiatao; Fu, Qing; Jin, Yu; Liang, Xinmiao

    2017-09-15

    The goal of this study was to develop a method that utilized a hydrophilic C18 stationary phase in the preparative high performance liquid chromatography to isolate the polar part from the rhizomes of Anemarrhena asphodeloides. The results showed that an initial mobile phase of pure water for the separation could greatly increase the retention and solubility of the polar compounds at the preparative scale. Introducing polar groups on the surface of the hydrophilic C18 column together with the use of optimized mobile phase compositions improved the column separation selectivity for polar compounds. Eleven previously undescribed compounds in Anemarrhena asphodeloides were obtained, indicating that the method developed in this study would facilitate the purification and separation of the polar part of traditional Chinese medicines. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Graphite/salt composites for high temperature energy storage: a study of the effects of the graphite and of the microstructure of the composites on the phase change properties of the salts; Composites graphite/sel pour le stockage d'energie a haute temperature: etude des effets du graphite et de la microstructure des composites sur les proprietes de changement de phase des sels

    Energy Technology Data Exchange (ETDEWEB)

    Lopez, J.; Palomo del Barrio, E. [TREFLE UMR 8508, 33 - Talence (France); Dumas, J.P. [Universite de Pau et des Pays de l' Adour, LaTEP, 64 - Pau (France)

    2008-07-15

    Thermal energy storage at high temperature is an efficient way for energy saving in the industrial sector, as well as a key component for power generation based on renewable energy resources. Thermal energy storage technology based on phase change materials (mainly salts) has been identified to meet the requirements of investment costs and compactness. However, the low thermal conductivity of salts (1 W/m/K) could be a limiting factor concerning power. To overcome such a drawback, new materials combining salts with graphite have been developed. Nevertheless, it is important to verify that no degradation of the salts storage properties is induced by their thermal conductivity enhancement. In this Note, the effects of the graphite and the composites graphite/salt microstructure on the phase change properties of salts are analysed. It appears that the thermo chemical stability of salts is not disturbed by graphite and that graphite does not modify the latent heat of salts. It is shown that graphite usually promotes heterogeneous nucleation and that it can reduce melting temperature.

  17. New graphite/salt materials for high temperature energy storage. Phase change properties study; Nouveaux materiaux graphite/sel pour le stockage d'energie a haute temperature. Etude des proprietes de changement de phase

    Energy Technology Data Exchange (ETDEWEB)

    Lopez, J

    2007-07-15

    This work is a contribution to the study of new graphite/salt composites dedicated to high temperature energy storage ({>=}200 C). The aim is to analyse and to understand the influence of both graphite and composite microstructure on the phase change properties of salts. This PhD is carried out within the framework of two projects: DISTOR (European) and HTPSTOCK (French). The major contributions of this work are threefold: 1) An important database (solid-liquid phase change properties) is provided from the DSC analysis of six salts and the corresponding composites. 2) Rigorous modeling of salts melting in confined media in several geometries are proposed to understand why, during the first melting of the compression elaborated composites, problems of salt leakage are observed. These models show that the materials morphology is responsible for these phenomena: the graphite matrix restrains the volume expansion due to salt melting: salt melts under pressure, which leads to a melting on a large temperature range and to a loss of energy density. Sensitivity analysis of parameters (geometric and physic) shows that matrix rigidity modulus is the parameter on which it is necessary to act during the composites elaboration to blur this phenomenon. 3) Finally, this work proposes a thermodynamic formulation of both surface/interface phenomena and the presence of dissolved impurities being able to explain a melting point lowering. It seems that the melting point lowering observed ({approx} 5 C) are mainly due to the presence of dissolved impurities (brought by graphite) in the liquid, along with an additional Gibbs-Thomson effect ({approx} 1 C, related to the size of the clusters crystals). (author)

  18. Determination of nitrosamines and caffeine metabolites in wastewaters using gas chromatography mass spectrometry and ionic liquid stationary phases.

    Science.gov (United States)

    Reyes-Contreras, Carolina; Domínguez, Carmen; Bayona, Josep M

    2012-10-26

    Recently, the interest to assess the environmental and human health effects of a wide group of emerging contaminants is growing worldwide. However, one of the main problems associated to their exposure is their determination in environmental matrices. It is hindered by the high polarity of most of these analytes, the poor selectivity obtained with low polarity stationary phases and the high background obtained with polar columns commonly used in GC-MS. Accordingly, this study examines the suitability of ionic liquid (IL) (e.g. SLB-IL59, SLB-IL61, SLB-IL82 and SLB-IL111) as stationary phases for GC-MS and their application to the determination of nitrosamines and caffeine metabolites in wastewater samples. Different chromatographic conditions were evaluated and results discussed in terms of resolution and peak symmetry. The SLB-IL111 column enabled the baseline separation and quantification of 7 nitrosamines in a shorter analysis time compared with cyanopropylphenyl polysiloxane commonly used. On the other hand, the SLB-IL59 column provided the best results for caffeine metabolites. Copyright © 2012 Elsevier B.V. All rights reserved.

  19. Quantitative analysis of molecular interaction potentials of ionic liquid anions using multi-functionalized stationary phases in HPLC.

    Science.gov (United States)

    Cho, Chul-Woong; Stolte, Stefan; Ranke, Johannes; Preiss, Ulrich; Krossing, Ingo; Thöming, Jorg

    2014-08-04

    The molecular interaction potentials, including S (dipolarity/polarizability), A (hydrogen bonding acidity), and B (hydrogen bonding basicity), of anions are experimentally determined using multi-functionalized stationary phases in high-performance liquid chromatography (HPLC) systems. We employ three different multi-functionalized stationary phase columns (Obelisc R, Obelisc N, and Acclaim Trinity-P1) combined with two ingredients, namely, acetonitrile (ACN) and methanol (MeOH). These conditions can cause neutral, cationic, and anionic compounds to be retained. By using the retention characteristics of calibration compounds, including cations, anions, and neutral compounds, system parameters including the ionic interaction terms (zc Zc , za Za ) are evaluated using multiple linear regression, resulting in a standard deviation (SD) of 0.090-0.158 log units. Based on the system parameters and retention characteristics of the anions of interest, their molecular interaction potentials are characterized on the same scale for neutral and cationic molecules. Furthermore, to verify the determined molecular interaction potentials, we predict anion hydrophobicity. The results show that the determined S, A, and B, together with the computable descriptors E (excess molar refraction) and V (McGowan volume), can predict anion hydrophobicity with R(2) =0.982 and SD=0.167 (dimensionless). © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Purification of Monoclonal Antibodies Using a Fiber Based Cation-Exchange Stationary Phase: Parameter Determination and Modeling

    Directory of Open Access Journals (Sweden)

    Jan Schwellenbach

    2016-10-01

    Full Text Available Monoclonal antibodies (mAb currently dominate the market for protein therapeutics. Because chromatography unit operations are critical for the purification of therapeutic proteins, the process integration of novel chromatographic stationary phases, driven by the demand for more economic process schemes, is a field of ongoing research. Within this study it was demonstrated that the description and prediction of mAb purification on a novel fiber based cation-exchange stationary phase can be achieved using a physico-chemical model. All relevant mass-transport phenomena during a bind and elute chromatographic cycle, namely convection, axial dispersion, boundary layer mass-transfer, and the salt dependent binding behavior in the fiber bed were described. This work highlights the combination of model adaption, simulation, and experimental parameter determination through separate measurements, correlations, or geometric considerations, independent from the chromatographic cycle. The salt dependent binding behavior of a purified mAb was determined by the measurement of adsorption isotherms using batch adsorption experiments. Utilizing a combination of size exclusion and protein A chromatography as analytic techniques, this approach can be extended to a cell culture broth, describing the salt dependent binding behavior of multiple components. Model testing and validation was performed with experimental bind and elute cycles using purified mAb as well as a clarified cell culture broth. A comparison between model calculations and experimental data showed a good agreement. The influence of the model parameters is discussed in detail.

  1. Quinine-Based Zwitterionic Chiral Stationary Phase as a Complementary Tool for Peptide Analysis: Mobile Phase Effects on Enantio- and Stereoselectivity of Underivatized Oligopeptides.

    Science.gov (United States)

    Ianni, Federica; Sardella, Roccaldo; Carotti, Andrea; Natalini, Benedetto; Lindner, Wolfgang; Lämmerhofer, Michael

    2016-01-01

    Peptide stereoisomer analysis is of importance for quality control of therapeutic peptides, the analysis of stereochemical integrity of bioactive peptides in food, and the elucidation of the stereochemistry of peptides from a natural chiral pool which often contains one or more D-amino acid residues. In this work, a series of model peptide stereoisomers (enantiomers and diastereomers) were analyzed on a zwitterionic ion-exchanger chiral stationary phase (Chiralpak ZWIX(+) 5 µm), in order to investigate the retention and separation performance for such compounds on this chiral stationary phase and elucidate its utility for this purpose. The goal of the study focused on 1) investigations of the effects of the sample matrix used to dissolve the peptide samples; 2) optimization of the mobile phase (enabling deriving information on factors of relevance for retention and separation); and 3) derivation of structure-selectivity relationships. It turned out that small di- and tripeptides can be well resolved under optimized conditions, typically with resolutions larger than 1.5. The optimized mobile phase often consisted of methanol-tetrahydrofuran-water (49:49:2; v/v/v) with 25 mM formic acid and 12.5 mM diethylamine. This work proposes some guidance on which mobile phases can be most efficiently used for peptide stereoisomer separations on Chiralpak ZWIX. Chirality 28:5-16, 2016. © 2015 Wiley Periodicals, Inc. © 2015 Wiley Periodicals, Inc.

  2. Effect of Secondary Equilibria on the Adsorption of Ibuprofen Enantiomers on a Chiral Stationary Phase with a Grafted Antibiotic Eremomycin

    Science.gov (United States)

    Reshetova, E. N.; Asnin, L. D.; Kachmarsky, K.

    2018-02-01

    The chromatographic separation of ibuprofen enantiomers on a Nautilus-E chiral stationary phase with a grafted eremomycin antibiotic at high column loading is accompanied by distortion of the shape of chromatographic peaks. A model is proposed to explain this phenomenon. A number of factors are considered in the model: the ionization of ibuprofen in the mobile phase, the pH change in the mass transfer zone caused by ionization, and competitive adsorption involving buffer components. Simulations performed using this model within the theory of nonequilibrium chromatography allow the shape of chromatograms for large amounts of S- and R-ibuprofen samples to be predicted. The adsorption mechanism is found to be mainly ion-exchange. The contribution from the molecular adsorption of ibuprofen to the total retention is shown to be several percent.

  3. Bromine intercalated graphite for lightweight composite conductors

    KAUST Repository

    Amassian, Aram

    2017-07-20

    A method of fabricating a bromine-graphite/metal composite includes intercalating bromine within layers of graphite via liquid-phase bromination to create brominated-graphite and consolidating the brominated-graphite with a metal nanopowder via a mechanical pressing operation to generate a bromine-graphite/metal composite material.

  4. Characterizing the selectivity of stationary phases and organic modifiers in reversed-phase high-performance liquid chromatographic systems by a general solvation equation using gradient elution.

    Science.gov (United States)

    Du, C M; Valko, K; Bevan, C; Reynolds, D; Abraham, M H

    2000-11-01

    Retention data for a set of 69 compounds using rapid gradient elution are obtained on a wide range of reversed-phase stationary phases and organic modifiers. The chromatographic stationary phases studied are Inertsil (IN)-ODS, pentafluorophenyl, fluoro-octyl, n-propylcyano, Polymer (PLRP-S 100), and hexylphenyl. The organic solvent modifiers are 2,2,2-trifluoroethanol (TFE); 1,1,1,3,3,3-hexafluoropropan-2-ol (HFIP); isopropanol; methanol (MeOH); acetonitrile (AcN); tetrahydrofuran; 1,4-dioxane; N,N-dimethylformamide; and mixed solvents of dimethylsulfoxide (DMSO) with AcN and DMSO with MeOH (1:1). A total of 25 chromatographic systems are analyzed using a solvation equation. In general, most of the systems give reasonable statistics. The selectivity of the reversed phase-high-performance liquid chromatographic (HPLC) systems with respect to the solute's dipolarity-polarity, hydrogen-bond acidity, and basicity are reflected in correspondingly large coefficients in the solvation equation. We wanted to find the most orthogonal HPLC systems, showing the highest possible selectivity difference in order to derive molecular descriptors using the gradient retention times of a compound. We selected eight chromatographic systems that have a large range of coefficients of interest (s, a, and b) similar to those found in water-solvent partitions used previously to derive molecular descriptors. The systems selected are IN-ODS phases with AcN, MeOH, TFE, and HFIP as mobile phase, PLRP-S 100 phase with AcN, propylcyano phase with AcN and MeOH, and fluorooctyl phase with TFE. Using the retention data obtained for a compound in the selected chromatographic systems, we can estimate the molecular descriptors with the faster and simpler gradient elution method.

  5. A Model for Solving the Maxwell Quasi Stationary Equations in a 3-Phase Electric Reduction Furnace

    Directory of Open Access Journals (Sweden)

    S. Ekrann

    1982-10-01

    Full Text Available A computer code has been developed for the approximate computation of electric and magnetic fields within an electric reduction furnace. The paper describes the numerical methods used to solve Maxwell's quasi-stationary equations, which are the governing equations for this problem. The equations are discretized by a staggered grid finite difference technique. The resulting algebraic equations are solved by iterating between computations of electric and magnetic quantities. This 'outer' iteration converges only when the skin depth is larger or of about the same magnitude as the linear dimensions of the computational domain. In solving for electric quantities with magnetic quantities being regarded as known, and vice versa, the central computational task is the solution of a Poisson equation for a scalar potential. These equations are solved by line successive overrelaxation combined with a rebalancing technique.

  6. A weak cation-exchange monolith as stationary phase for the separation of peptide diastereomers by CEC.

    Science.gov (United States)

    Ludewig, Ronny; Nietzsche, Sandor; Scriba, Gerhard K E

    2011-01-01

    A CEC weak cation-exchange monolith has been prepared by in situ polymerization of acrylamide, methylenebisacrylamide and 4-acrylamidobutyric acid in a decanol-dimethylsulfoxide mixture as porogen. The columns were evaluated by SEM and characterized with regard to the separation of diastereomers and α/β-isomers of aspartyl peptides. Column preparation was reproducible as evidenced by comparison of the analyte retention times of several columns prepared simultaneously. Analyte separation was achieved using mobile phases consisting of acidic phosphate buffer and ACN. Under these conditions the peptides migrated due to their electrophoretic mobility but the EOF also contributed as driving force as a function of the pH of the mobile phase due to increasing dissociation of the carboxyl groups of the polymer. Raising the pH of the mobile phase also resulted in deprotonation of the peptides reducing analyte mobility. Due to these mechanisms each pair of diastereomeric peptides displayed the highest resolution at a different pH of the buffer component of the mobile phase. Comparing the weak-cation exchange monolith to an RP monolith and a strong cation-exchange monolith different elution order of some peptide diastereomers was observed, clearly illustrating that interactions with the stationary phase contribute to the CEC separations. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Resistive anomalies and phase transitions in potassium-intercalated benzene-derived graphite fibers

    Science.gov (United States)

    Olsen, Randall B.; McQuillan, Barry W.; Chin, Jack; Woolf, Lawrence D.

    1986-04-01

    The resistivity of substantially single-stage potassium-intercalated benzene-derived graphite fibers (BDF's) between 6 and 300 K is presented. Single resistive anomalies are found in second-, third-, fifth-, and sixth-stage fibers but are not found in first-stage fibers. The temperatures of the observed anomalies show some correlation with those previously seen in highly oriented pyrolytic graphite (HOPG). However, the pairs of resistive anomalies typically seen in HOPG are not observed in BDF's except for the fourth stage.

  8. Direct enantioseparation of underivatized aliphatic 3-hydroxyalkanoic acids with a quinine-based zwitterionic chiral stationary phase.

    Science.gov (United States)

    Ianni, Federica; Pataj, Zoltán; Gross, Harald; Sardella, Roccaldo; Natalini, Benedetto; Lindner, Wolfgang; Lämmerhofer, Michael

    2014-10-10

    While aliphatic 2-hydroxyalkanoic acids have been more or less successfully enantioseparated with various chiral stationary phases by HPLC and GC, analogous applications on underivatized aliphatic 3-hydroxyalkanoic acids are completely absent in the scientific literature. With the aim of closing this gap, the enantioseparation of 3-hydroxybutyric acid, 3-hydroxydecanoic acid and 3-hydroxymyristic acid has been performed with two ion-exchange type chiral stationary phases (CSPs): one containing the anion-exchange type tert-butyl carbamoyl quinine chiral selector motif (Chiralpak QN-AX), and the other carrying the new zwitterionic variant based on trans-(S,S)-2-aminocyclohexanesulfonic acid-derivatized quinine carbamate (Chiralpak ZWIX(+)) as the chiral selector and enantiodiscriminating element, respectively. The zwitterionic enantiorecognition material provided better results in terms of enantioselectivity and resolution compared to the anion-exchanger CSP at reduced retention times due to the intramolecular counterion effect imposed by the sulfonic acid moiety and its competition with the 3-hydroxyalkanoic acid analyte for ionic interaction at the quininium-anion exchanger site. It is thus recommended as the CSP of first choice for enantioseparations of the class of aliphatic 3-hydroxyalkanoic acids. With use of polar organic eluent composed of ACN/MeOH/AcOH - 95/5/0.05 (v/v/v), a good compromise in terms of analysis time and enantioresolution quality was accomplished. The major experimental variables have been investigated for optimization of the resolution and allowed to derive information on the enantiorecognition mechanism. Corresponding Chiralpak ZWIX(-), based on pseudo-enantiomeric selector derived from quinidine and trans-(R,R)-2-aminocyclohexanesulfonic acid with opposite configurations provided reversed enantiomer elution orders. It has further to be stressed that these separations can be obtained with mass spectrometry compatible mobile phases

  9. Preparation, characterization and application of N-methylene phosphonic acid chitosan grafted magnesia–zirconia stationary phase

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Qing; Chen, Jie; Huang, Kun; Zhang, Xin; Xu, Li [Tongji School of Pharmacy, Huazhong University of Science and Technology, Wuhan 430030 (China); Shi, Zhi-guo, E-mail: shizg@whu.edu.cn [Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2015-01-07

    Highlights: • N-methylene phosphonic acid chitosan grafted MgO–ZrO{sub 2} was prepared. • It exhibited superior HILIC chromatographic performance to the bare MgO–ZrO{sub 2}. • Monosaccharides, phospholipids and peptides were successfully separated. • It was a promising HILIC stationary phase. - Abstract: A hydrophilic stationary phase (SP) was prepared through grafting N-methylene phosphonic acid chitosan on magnesia–zirconia particles (P-CTS-MgO–ZrO{sub 2}) via Lewis acid–base interaction. The resulting material was characterized by thermogravimetric analysis, Fourier transform infrared spectroscopy, scanning electron microscope and nitrogen adsorption analysis. The chromatographic performance of P-CTS-MgO–ZrO{sub 2} was systemically evaluated by studying effect of acetonitrile content, pH and buffer concentration in the mobile phase. The results demonstrated that the novel SP provided hydrophilic, electrostatic-repulsion and ion-exchange interactions. Compared to the bare MgO–ZrO{sub 2}, P-CTS-MgO–ZrO{sub 2} exhibited superior peak shape, reasonable resolution and reduced analysis time in separation of basic analytes. Besides, remarkable resolving power of acids, i.e. six non-steroidal anti-inflammatory drugs which failed to be eluted from the bare MgO–ZrO{sub 2}, was obtained with the theoretical plate number (N/m) of 4653–31313, asymmetry factor <1.21 and the resolution of 1.6–3.4. Finally, P-CTS-MgO–ZrO{sub 2} SP was applied to separate monosaccharides, phospholipids and peptides. P-CTS-MgO–ZrO{sub 2} was a promising hydrophilic SP for wide applications.

  10. Preparation by low-temperature nonthermal plasma of graphite fiber and its characteristics for solid-phase microextraction.

    Science.gov (United States)

    Luo, Fan; Wu, Zucheng; Tao, Ping; Cong, Yanqing

    2009-01-05

    Low-temperature nonthermal plasma has been used to prepare solid-phase microextraction (SPME) fibers with high adsorbability, long-term serviceability, and high reproducibility. Graphite rods serving as fiber precursors were treated by an air plasma discharged at 15.2-15.5 kV for a duration of 8 min. Sampling results revealed that the adsorptive capacity of the homemade fiber was 2.5-34.6 times that of a polyacrylate (PA) fiber for alcohols (methanol, ethanol, isopropyl alcohol, n-butyl alcohol), and about 1.4-1.6 times and 2.5-5.1 times that of an activated carbon fiber (ACF) for alcohols and BTEX (benzene, toluene, ethylbenzene, and xylenes), respectively. It is confirmed from FTIR (Fourier transform infrared spectrophotometer) and SEM (scanning electron microscope) analyses that the improvement in the adsorptive performance attributed to increased surface energy and roughness of the graphite fiber. Using gas chromatography (GC)-flame-ionization detector (FID), the limits of detection (LODs) of the alcohols and BTEX ranged between 0.19 and 3.75 microg L(-1), the linear ranges were between 0.6 and 35,619 microg L(-1) with good linearity (R(2)=0.9964-0.9997). It was demonstrated that nonthermal plasma offers a fast and simple method for preparing an efficient graphite SPME fiber, and that SPME using the homemade fiber represents a sensitive and selective extraction method for the analysis of a wide range of organic compounds.

  11. Preparation by low-temperature nonthermal plasma of graphite fiber and its characteristics for solid-phase microextraction

    International Nuclear Information System (INIS)

    Luo Fan; Wu Zucheng; Tao Ping; Cong Yanqing

    2009-01-01

    Low-temperature nonthermal plasma has been used to prepare solid-phase microextraction (SPME) fibers with high adsorbability, long-term serviceability, and high reproducibility. Graphite rods serving as fiber precursors were treated by an air plasma discharged at 15.2-15.5 kV for a duration of 8 min. Sampling results revealed that the adsorptive capacity of the homemade fiber was 2.5-34.6 times that of a polyacrylate (PA) fiber for alcohols (methanol, ethanol, isopropyl alcohol, n-butyl alcohol), and about 1.4-1.6 times and 2.5-5.1 times that of an activated carbon fiber (ACF) for alcohols and BTEX (benzene, toluene, ethylbenzene, and xylenes), respectively. It is confirmed from FTIR (Fourier transform infrared spectrophotometer) and SEM (scanning electron microscope) analyses that the improvement in the adsorptive performance attributed to increased surface energy and roughness of the graphite fiber. Using gas chromatography (GC)-flame-ionization detector (FID), the limits of detection (LODs) of the alcohols and BTEX ranged between 0.19 and 3.75 μg L -1 , the linear ranges were between 0.6 and 35619 μg L -1 with good linearity (R 2 = 0.9964-0.9997). It was demonstrated that nonthermal plasma offers a fast and simple method for preparing an efficient graphite SPME fiber, and that SPME using the homemade fiber represents a sensitive and selective extraction method for the analysis of a wide range of organic compounds

  12. Kinetic modeling of sporulation and product formation in stationary phase by Bacillus coagulans RK-02 vis-à-vis other Bacilli.

    Science.gov (United States)

    Das, Subhasish; Sen, Ramkrishna

    2011-10-01

    A logistic kinetic model was derived and validated to characterize the dynamics of a sporogenous bacterium in stationary phase with respect to sporulation and product formation. The kinetic constants as determined using this model are particularly important for describing intrinsic properties of a sporogenous bacterial culture in stationary phase. Non-linear curve fitting of the experimental data into the mathematical model showed very good correlation with the predicted values for sporulation and lipase production by Bacillus coagulans RK-02 culture in minimal media. Model fitting of literature data of sporulation and product (protease and amylase) formation in the stationary phase by some other Bacilli and comparison of the results of model fitting with those of Bacillus coagulans helped validate the significance and robustness of the developed kinetic model. Copyright © 2011 Elsevier Ltd. All rights reserved.

  13. Optimising reversed-phase liquid chromatographic separation of an acidic mixture on a monolithic stationary phase with the aid of response surface methodology and experimental design.

    Science.gov (United States)

    Wang, Y; Harrison, M; Clark, B J

    2006-02-10

    An optimization strategy for the separation of an acidic mixture by employing a monolithic stationary phase is presented, with the aid of experimental design and response surface methodology (RSM). An orthogonal array design (OAD) OA(16) (2(15)) was used to choose the significant parameters for the optimization. The significant factors were optimized by using a central composite design (CCD) and the quadratic models between the dependent and the independent parameters were built. The mathematical models were tested on a number of simulated data set and had a coefficient of R(2) > 0.97 (n = 16). On applying the optimization strategy, the factor effects were visualized as three-dimensional (3D) response surfaces and contour plots. The optimal condition was achieved in less than 40 min by using the monolithic packing with the mobile phase of methanol/20 mM phosphate buffer pH 2.7 (25.5/74.5, v/v). The method showed good agreement between the experimental data and predictive value throughout the studied parameter space and were suitable for optimization studies on the monolithic stationary phase for acidic compounds.

  14. Two-dimensional high-performance thin-layer chromatography of tryptic bovine albumin digest using normal- and reverse-phase systems with silanized silica stationary phase.

    Science.gov (United States)

    Gwarda, Radosław Łukasz; Dzido, Tadeusz Henryk

    2013-10-18

    Among many advantages of planar techniques, two-dimensional (2D) separation seems to be the most important for analysis of complex samples. Here we present quick, simple and efficient two-dimensional high-performance thin-layer chromatography (2D HPTLC) of bovine albumin digest using commercial HPTLC RP-18W plates (silica based stationary phase with chemically bonded octadecyl ligands of coverage density 0.5μmol/m(2) from Merck, Darmstadt). We show, that at low or high concentration of water in the mobile phase comprised methanol and some additives the chromatographic systems with the plates mentioned demonstrate normal- or reversed-phase liquid chromatography properties, respectively, for separation of peptides obtained. These two systems show quite different separation selectivity and their combination into 2D HPTLC process provides excellent separation of peptides of the bovine albumin digest. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. Clean synthesis of molecular recognition polymeric materials with chiral sensing capability using supercritical fluid technology. Application as HPLC stationary phases.

    Science.gov (United States)

    da Silva, Mara Soares; Vão, Eva R; Temtem, Márcio; Mafra, Luís; Caldeira, Jorge; Aguiar-Ricardo, Ana; Casimiro, Teresa

    2010-03-15

    Molecularly imprinted polymers (MIPs) of poly(ethylene glycol dimethacrylate) and poly(N-isopropylacrylamide-co-ethylene glycol dimethacrylate) were synthesized for the first time in supercritical carbon dioxide (scCO(2)), using Boc-L-tryptophan as template. Supercritical fluid technology provides a clean and one-step synthetic route for the preparation of affinity polymeric materials with sensing capability for specific molecules. The polymeric materials were tested as stationary HPLC phases for the enantiomeric separation of L- and D-tryptophan. HPLC results prove that the synthesized MIPs are able to recognize the template molecule towards its enantiomer which opens up potential applications in chromatographic chiral separation. (c) 2009 Elsevier B.V. All rights reserved.

  16. A Nutrient-Regulated Cyclic Diguanylate Phosphodiesterase Controls Clostridium difficile Biofilm and Toxin Production during Stationary Phase.

    Science.gov (United States)

    Purcell, Erin B; McKee, Robert W; Courson, David S; Garrett, Elizabeth M; McBride, Shonna M; Cheney, Richard E; Tamayo, Rita

    2017-09-01

    The signaling molecule cyclic diguanylate (c-di-GMP) mediates physiological adaptation to extracellular stimuli in a wide range of bacteria. The complex metabolic pathways governing c-di-GMP synthesis and degradation are highly regulated, but the specific cues that impact c-di-GMP signaling are largely unknown. In the intestinal pathogen Clostridium difficile , c-di-GMP inhibits flagellar motility and toxin production and promotes pilus-dependent biofilm formation, but no specific biological functions have been ascribed to any of the individual c-di-GMP synthases or phosphodiesterases (PDEs). Here, we report the functional and biochemical characterization of a c-di-GMP PDE, PdcA, 1 of 37 confirmed or putative c-di-GMP metabolism proteins in C. difficile 630. Our studies reveal that pdcA transcription is controlled by the nutrient-regulated transcriptional regulator CodY and accordingly increases during stationary phase. In addition, PdcA PDE activity is allosterically regulated by GTP, further linking c-di-GMP levels to nutrient availability. Mutation of pdcA increased biofilm formation and reduced toxin biosynthesis without affecting swimming motility or global intracellular c-di-GMP. Analysis of the transcriptional response to pdcA mutation indicates that PdcA-dependent phenotypes manifest during stationary phase, consistent with regulation by CodY. These results demonstrate that inactivation of this single PDE gene is sufficient to impact multiple c-di-GMP-dependent phenotypes, including the production of major virulence factors, and suggest a link between c-di-GMP signaling and nutrient availability. Copyright © 2017 American Society for Microbiology.

  17. Membrane chromatography: protein purification from E. coli lysate using newly designed and commercial anion-exchange stationary phases.

    Science.gov (United States)

    Bhut, Bharat V; Christensen, Kenneth A; Husson, Scott M

    2010-07-23

    This contribution describes the purification of anthrax protective antigen (PA) protein from Escherichia coli lysate using bind-and-elute chromatography with newly designed weak anion-exchange membranes. Protein separation performance of the new AEX membrane adsorber was compared with the commercial Sartobind D membrane adsorber and HiTrap DEAE FF resin column under preparative scale conditions. Dynamic protein binding capacities of all three stationary phases were determined using breakthrough curve analysis. The AEX membrane showed higher binding capacities than the Sartobind D membrane at equivalent volumetric throughput and higher capacities than the HiTrap DEAE FF resin column at 15 times higher volumetric throughput. Anion-exchange chromatography was performed using all three stationary phases to purify PA protein. Quantitative SDS-PAGE analysis of effluent fractions showed that the purity of PA protein was higher for membrane adsorbers than the HiTrap DEAE FF resin column and was the same for the new AEX membrane and Sartobind D membrane adsorbers. The effects of E. coli lysate load volume and volumetric flow rate on PA protein separation resolution using the membrane adsorbers were minor, and the peak elution profile remained un-changed even under conditions where >75% of the total protein dynamic binding capacity of the membranes had been utilized. PA protein peak resolution was higher using pH-gradient elution than with ionic strength gradient elution. Overall, the results clearly demonstrate that membrane chromatography is a high-capacity, high-throughput, high-resolution separation technique, and that resolution in membrane chromatography can be higher than resin column chromatography under preparative conditions and at much higher volumetric throughput. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  18. Proline accumulation protects Saccharomyces cerevisiae cells in stationary phase from ethanol stress by reducing reactive oxygen species levels.

    Science.gov (United States)

    Takagi, Hiroshi; Taguchi, Junpei; Kaino, Tomohiro

    2016-08-01

    During fermentation processes, Saccharomyces cerevisiae cells are exposed to multiple stresses, including a high concentration of ethanol that represents toxicity through intracellular reactive oxygen species (ROS) generation. We previously reported that proline protected yeast cells from damage caused by various stresses, such as freezing and ethanol. As an anti-oxidant, proline is suggested to scavenge intracellular ROS. In this study, we examined the role of intracellular proline during ethanol treatment in S. cerevisiae strains that accumulate different concentrations of proline. When cultured in YPD medium, there was a significant accumulation of proline in the put1 mutant strain, which is deficient in proline oxidase, in the stationary phase. Expression of the mutant PRO1 gene, which encodes the γ-glutamyl kinase variant (Asp154Asn or Ile150Thr) with desensitization to feedback inhibition by proline in the put1 mutant strain, showed a prominent increase in proline content as compared with that of the wild-type strain. The oxidation level was clearly increased in wild-type cells after exposure to ethanol, indicating that the generation of ROS occurred. Interestingly, proline accumulation significantly reduces the ROS level and increases the survival rate of yeast cells in the stationary phase under ethanol stress conditions. However, there was not a clear correlation between proline content and survival rate in yeast cells. An appropriate level of intracellular proline in yeast might be important for its stress-protective effect. Hence, the engineering of proline metabolism could be promising for breeding stress-tolerant industrial yeast strains. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  19. HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC SEPARATION OF THE ENANTIOMERS OF ORGANOPHOSPHORUS PESTICIDES ON POLYSACCHARIDE CHIRAL STATIONARY PHASES

    Science.gov (United States)

    High-performance liquid chromatographic separation of the individual enantiomers of 12 organophosphorus pesticides (OPs) was obtained on polysaccharide enantioselective HPLC columns using alkane-alcohol mobile phase. The OP pesticides were crotoxyphos, dialifor, fonofos, fenamiph...

  20. HPLC SEPARATION OF CHIRAL ORGANOPHOSPHORUS PESTICIDES ON POLYSACCHARIDE CHIRAL STATIONARY PHASES

    Science.gov (United States)

    High-performance liquid chromatographic separation of the individual enantiomers of 12 organophosphorus pesticides (OPs) were obtained on polysaccharide chiral HPLC columns using an alkane-alcohol mobile phase. The OP pesticides were crotoxyphos, dialifor, dyfonate, fenamiphos, ...

  1. Preparation, characterization and thermal properties of binary nitrate salts/expanded graphite as composite phase change material

    International Nuclear Information System (INIS)

    Xiao, Junbing; Huang, Jin; Zhu, Panpan; Wang, Changhong; Li, Xinxi

    2014-01-01

    Highlights: • The expanded graphite enhanced thermal conductivity coefficient greatly. • The aqueous solution method adopting ultrasonic was utilized to disperse EG. • The combination of composite was physical without chemical reaction. • The reduction on total latent heat was slight after the adding EG. - Abstract: The binary nitrate salts/expanded graphite (EG) composite phase change material (PCM) were prepared via adding different mass rate of EG to binary nitrate salts consisting of NaNO 3 and KNO 3 (6:4) by aqueous solution method adopting ultrasonic. The morphology and chemical composition of EG and the composite PCM were characterized and investigated by X-ray diffraction (XRD), scan electron microscope (SEM), energy dispersive spectrometer (EDS), transmission electron microscope (TEM), respectively. Laser thermal conductivity instrument and differential scanning calorimeter (DSC) were employed to measure thermo physical properties. Drawing the conclusion from investigation, that EG had enhanced thermal conductivity coefficient which largely increased to 4.884 W/(m K) and reduced total latent heat by mostly 11.0%. The morphology and phase structure results indicated that EG were well dispersed into and physically combined with molten salts. In general, the prepared composite PCM could be a suitable phase change material for thermal energy storage

  2. Preparation of a silica stationary phase co-functionalized with Wulff-type phenylboronate and C12 for mixed-mode liquid chromatography.

    Science.gov (United States)

    Li, Hengye; Zhang, Xuemeng; Zhang, Lin; Wang, Xiaojin; Kong, Fenying; Fan, Dahe; Li, Lei; Wang, Wei

    2017-04-15

    A silica stationary phase was designed and synthesized through the co-functionalization of silica with Wulff-type phenylboronate and C12 for mixed-mode liquid chromatography applications. The as-synthesized stationary phase was characterized by elemental analysis and Fourier Transform-InfraRed Spectroscopy (FT-IR). Retention mechanisms, including boronate affinity (BA), reversed-phase (RP) and anion-exchange (AE), were involved. Retention mechanism switching was easily realized by adjustment of the mobile phase constitution. Cis-diol compounds could be selectively captured under neutral conditions in BA mode and off-line separated in RP mode. Neutral, basic, acidic and amphiprotic compounds were chromatographed on the column in RP chromatography, while inorganic anions were chromatographed in AE chromatography to characterize the mixed-mode nature of the prepared stationary phase. In addition, the RP performance was compared with an octadecyl silica column in terms of column efficiency (N/m), asymmetry factor (A f ), retention factor (k) and resolution (Rs). The prepared stationary phase offered multiple interactions with analytes in addition to hydrophobic interactions under RP elution conditions. Based on the mixed-mode properties, off-line 2D-LC, for selective capture and separation of urinary nucleosides, was successfully realized on a single column, demonstrating its powerful application potential for complex samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Antimicrobial efficacy of chlorine dioxide against Candida albicans in stationary and starvation phases in human root canal: An in-vitro study

    Directory of Open Access Journals (Sweden)

    Shirur Krishnaraj Somayaji

    2014-01-01

    Full Text Available Introduction: Candida albicans (C. albicans is the most commonly isolated fungal pathogen from dental root canal. C. albicans forms biofilm and develops resistance against root canal irrigants . This study determines the fungicidal efficacy of 13.8% chlorine dioxide in extracted human teeth at stationary and starvation phases of C. albicans. Materials and Methods: Teeth were decoronated and coronal portion of the roots were prepared into blocks, which were incubated at 37°C with C. albicans for five days. The samples were treated with chlorine dioxide for 12 and 20 minutes. Total of fifty blocks were taken in the study. Colony-forming units were counted in Sabourauds dextrose agar and scanning electron microscopic observation was done. Data were analyzed by one-way ANOVA and Bonferoni′s post hoc test. Results: Teeth at stationary phase (12 min showed mean colony count of 28,000 ± 1814 which is significantly (P < 0.001 less than control group. Teeth at starvation phase (12 min showed colony count of 65,600 ± 1912 which is also significantly (P < 0.001 less than control group. Teeth irrigated at stationary phase (20 min showed mean colony count of 23,400 ± 1776 (P < 0.001. Teeth irrigated at starvation phase (20 min showed mean colony count of 48,100 ± 1663 which is also significantly (P < 0.001 less than that of control group. Conclusion: Treatment of chlorine dioxide reduces the C. albicans count in root canals of extracted human teeth at stationary and starvation phases. Efficacy of chlorine dioxide against C. albicans is relatively higher in stationary phase than that of starvation phase.

  4. Growth potential of exponential- and stationary-phase Salmonella Typhimurium during sausage fermentation

    DEFF Research Database (Denmark)

    Birk, Tina; Henriksen, Sidsel; Müller, K.

    2016-01-01

    Raw meat for sausage production can be contaminated with Salmonella. For technical reasons, meat is often frozen prior to mincing but it is unknown how growth of Salmonella in meat prior to freezing affects its growth potential during sausage fermentation. We investigated survival of exponential-...... fermentation, sporadic growth of exponential-phase cells of S. Typhimurium was observed drawing attention to the handling and storage of sausage meat.......Raw meat for sausage production can be contaminated with Salmonella. For technical reasons, meat is often frozen prior to mincing but it is unknown how growth of Salmonella in meat prior to freezing affects its growth potential during sausage fermentation. We investigated survival of exponential...... starter culture. With no starter culture, both strains grew in both growth phases. In general, a functional starter culture abolished S. Typhimurium growth independent of growth phase and we concluded that ensuring correct fermentation is important for sausage safety. However, despite efficient...

  5. Thermal conductivity of an organic phase change material/expanded graphite composite across the phase change temperature range and a novel thermal conductivity model

    International Nuclear Information System (INIS)

    Ling, Ziye; Chen, Jiajie; Xu, Tao; Fang, Xiaoming; Gao, Xuenong; Zhang, Zhengguo

    2015-01-01

    Highlights: • Expanded graphite can improve thermal conductivity of RT44HC by 20–60 times. • Thermal conductivity of PCM/EG composites keeps constant before/after melting. • Thermal conductivity of PCMs nearly doubled during phase changing. • Thermal conductivity of composite PCM increases with density and percentage of EG. • The simple model predicts thermal conductivity of EG-based composites accurately. - Abstract: This work studies factors that affect the thermal conductivity of an organic phase change material (PCM), RT44HC/expanded graphite (EG) composite, which include: EG mass fraction, composite PCM density and temperature. The increase of EG mass fraction and bulk density will both enhance thermal conductivity of composite PCMs, by up to 60 times. Thermal conductivity of RT44HC/EG composites remains independent on temperature outside the phase change range (40–45 °C), but nearly doubles during the phase change. The narrow temperature change during the phase change allows the maximum heat flux or minimum temperature for heat source if attaching PCMs to a first (constant temperature) or second (constant heat flux) thermal boundary. At last, a simple thermal conductivity model for EG-based composites is put forward, based on only two parameters: mass fraction of EG and bulk density of the composite. This model is validated with experiment data presented in this paper and in literature, showing this model has general applicability to any composite of EG and poor thermal conductive materials

  6. Contaminants migration in the soil: the influence of transfer between the mobile and stationary phases

    International Nuclear Information System (INIS)

    Moreira, R.M.; Sabino, C.S.V.; Macedo, W.A.

    1996-01-01

    Three transport mechanisms control the contaminant migration in saturated soils: advection, diffusion and interchanges between liquid and solid phases. These interchanges define the retention by the soil and the contaminant delay related to the liquid phase flow. Therefore, the knowledge of the adsorption/desorption characteristics of the solute in solid surfaces is fundamental for the evaluation of toxic agent releases to the compartment soil. This communication reports the study which is being performed by the Centro de Desenvolvimento da Tecnologia Nuclear (CDTN) in this area, particularly with cesium and mercury by using X-ray absorption spectroscopy for contaminants migration

  7. Thermal properties improvement of Lithium nitrate/Graphite composite phase change materials

    International Nuclear Information System (INIS)

    Lachheb, Mohamed; Adili, Ali; Albouchi, Fethi; Mzali, Foued; Ben Nasrallah, Sassi

    2016-01-01

    Highlights: • Preparation of new Lithium nitrate/Graphite PCM-composites. • Experimental investigation of the thermo-physical properties of PCM-composites. • Prediction of theoretical thermo-physical properties by using different analytical models. - Abstract: This paper addresses the development and the thermal investigation of new composite materials with improved thermo-physical properties destined for solar thermal energy storage at high temperature. The thermo-physical properties of composites are characterized by using several techniques based on the temperature measurement and the obtained results are compared to the theoretical values calculated by different analytical models. The results of these experiments revealed a clear improvement in the different thermal properties when integrating graphite particles in the composite. In the other hand, a good agreement between experimental and theoretical values was obtained.

  8. GROPPER, an output program for results from BERSAFE. Phase 3 for graphite

    International Nuclear Information System (INIS)

    Harper, P.G.

    1980-05-01

    BERSAFE, the CEGB's Finite Element Stress Analysis System has been extended to enable analyses to be performed on structures made from irradiated graphite. As with all non-linear analyses there is a considerable amount of output data produced which needs to be selectively processed. GROPPER reads the tape file produced by such an analysis and outputs selected results to the line printer as well as preparing tapes for plotting of results. (author)

  9. Noteworthy ekectroanalytical features of the stage 4 to stage 3 phase transition in lithiated graphite

    Czech Academy of Sciences Publication Activity Database

    Levi, M. D.; Wang, C.; Markevich, E.; Aurbach, D.; Chvoj, Zdeněk

    2003-01-01

    Roč. 8, - (2003), s. 40-43 ISSN 1432-8488. [International Meeting on Advanced Batteries and Accumulators. Brno, 16.06.2002-20.06.2002] R&D Projects: GA AV ČR IAA1010207 Institutional research plan: CEZ:AV0Z1010914 Keywords : electrochemical lithiation * graphite electrode * potentiostatic intermittent titration Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.195, year: 2003

  10. Resistivity features in intercalated graphite compounds with bromine and iodine chloride in the region of structural phase transitions in the layer of intercalate

    International Nuclear Information System (INIS)

    Ovsyijenko, Yi.V.; Lazarenko, O.A.; Matsuj, L.Yu.; Prokopov, O.Yi.

    2013-01-01

    In the paper anomalous changes of resistivity in graphite intercalated compounds with iodine chloride and bromine are investigated in the phase transition temperature interval. It is shown that these anomalies are caused by the change of carriers mobility in the phase transitional interval as well as by the origin of ''mobile ions liquids''

  11. Laboratory-Scale Preparative Enantioseparations of Pharmaceutically Relevant Compounds on Commercially Available Chiral Stationary Phases for HPLC.

    Science.gov (United States)

    Sardella, Roccaldo; Ianni, Federica; Marinozzi, Maura; Macchiarulo, Antonio; Natalini, Benedetto

    2017-01-01

    In response to the outburst of research in the field of synthetic medicinal chemistry, enantioselective chromatography methods based on the use of chiral stationary phases (CSPs) found immediate acceptance as the elective choice for the analytical determinations of the enantiomeric purity of synthetic compounds. In contrast to an initial scepticism, also the preparative-scale applications are gaining increasing recognition as a powerful alternative to enantioselective synthesis for the supply of pure enantiomers of bioactive compounds. The increasing success of liquid chromatography methods has been made possible thanks to the development of highly efficient CSPs allowing the enantioresolution of practically all the chemical classes of chiral compounds. However, only few CSPs are really suitable for preparative- scale applications, being the loading capacity is the major concern for preparativescale enantioseparations. The cellulose- and amylose-based CSPs present the highest loading capacity and enantiodiscrimination power, which makes these CSPs the most versatile and applicable for preparative-scale applications in all the applicable elution modes (reversedphase, normal-phase, and with polar-organic or polar-ionic eluents). However, also other types of CSPs have been successfully employed at this regard (brush-type phases, polyacrylamide and cross-linked di-allyltartardiamide phases as well as cyclodextrin, and glycopeptide containing phases). Several instrumental methods exist for the determination of the absolute configuration of organic compounds in absence of known enantiopure reference standards. The most widely known are X-ray crystallography, followed by chirooptical methods [e.g., electronic and vibrational circular dichroism (ECD and VCD, respectively)] and nuclear magnetic resonance (NMR) spectroscopy. All these aspects will be treated in the review. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  12. The chiral separation of triazole pesticides enantiomers by amylose-tris (3,5-dimethylphenylcarbamate) chiral stationary phase.

    Science.gov (United States)

    Wang, Peng; Liu, Donghui; Jiang, Shuren; Xu, Yangguang; Zhou, Zhiqiang

    2008-10-01

    The amylose-tris(3,5-dimethylphenylcarbamate) chiral stationary phase was synthesized and used to separate the enantiomers of triazole pesticides by high-performance liquid chromatography. The mobile phase was n-hexane-isopropanol applying a flow rate of 1.0 mL/min. Six triazole pesticides were enantioselectively separated. Myclobutanil, paclobutrazol, tebuconazole, and uniconazole obtained complete separation with the resolution factors of 5.73, 2.99, 1.72, and 2.07, respectively, and imazalil and diniconazole obtained partial separation with the resolution factors of 0.79 and 0.77 under the optimized conditions. The effect of the content of isopropanol as well as column temperature on the separation was investigated. A circular dichroism detector was used to identify the enantiomers and determine the elution orders. The results showed the low temperature was good for the chiral separation except for diniconazole. The thermodynamic parameters calculated based on linear Van't Hoff plots showed the chiral separations were controlled by enthalpy.

  13. Separation of adrenergic amines in Citrus aurantium L. var. amara by capillary electrochromatography using a novel monolithic stationary phase.

    Science.gov (United States)

    Chizzali, Evelyn; Nischang, Ivo; Ganzera, Markus

    2011-08-01

    This manuscript reports on the use of capillary electrochromatography for the determination of tyramine, (±) synephrine, and (±) octopamine, the major alkaloids in bitter orange peel. A novel methacrylate-based monolithic stationary phase was prepared by UV-photopolymerization in 100 μm id fused-silica capillaries. It facilitated the quantitative assessment of alkaloids with a mobile phase comprising aqueous 10 mM ammonium acetate in ACN and isopropanol. Applied voltage and temperature were 25 kV and 25°C, and samples were injected in electrokinetic mode. The method reported herein revealed adequate sensitivity (LOD ≤0.6 μg/mL), repeatability (σrel ≤4.1%), accuracy (recovery rates between 95.2 and 102.2%), and precision (intra-day variation ≤5.7%, inter-day variation ≤4.1%). The application of the CEC assay on C. aurantium var. amara plant material and dietary supplements, which usually are advertised for slimming properties, indicated that synephrine (0.17-0.82%) is the dominant alkaloid. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Ion chromatography of transition metals: specific alteration of retention by complexation reactions in the mobile and on the stationary phase

    International Nuclear Information System (INIS)

    Baumgartner, S.

    1992-05-01

    Ion chromatography of mono- and bivalent cations was performed on a conventional cation exchanger. The pH influence of an ethylene-diamine/citrate eluent was significant for the retention of alkaline earth and transition metals, but negligible for alkali ions. This was dealt with from a mechanistic point of view. Mobile phase optimization allowed fast isocratic analysis of mono- and bivalent cations and the separation of the radionuclides Cs-137 and Sr-90. A newly synthesized stationary phase containing iminodiacetate (IDA) function was investigated for cation chromatography using ethylenediamine/citrate eluents, polyhydroxy acid and dipicolinic acid. The column's high selectivity for transition metal ions in comparison to alkali and alkaline earth metals may be governed by the choice of complexing ability and pH of the eluent. Applications verified by atomic absorption spectroscopy include alkaline earth metals in beverages and the determination of Co, Cd and Zn in solutions containing more than 10 14 -fold excess of Na and Mg, such as sea water

  15. Special graphites

    International Nuclear Information System (INIS)

    Leveque, P.

    1964-01-01

    A large fraction of the work undertaken jointly by the Commissariat a l'Energie Atomique (CEA) and the Pechiney Company has been the improvement of the properties of nuclear pile graphite and the opening up of new fields of graphite application. New processes for the manufacture of carbons and special graphites have been developed: forged graphite, pyro-carbons, high density graphite agglomeration of graphite powders by cracking of natural gas, impervious graphites. The physical properties of these products and their reaction with various oxidising gases are described. The first irradiation results are also given. (authors) [fr

  16. Use of serially coupled capillary columns with different polarity of stationary phases for the separation of the natural complex volatile mixture of the marine red alga Corallina elongata.

    Science.gov (United States)

    Dembitsky, V M; Srebnik, M

    2002-09-01

    Separation of a complex of natural volatile compounds using serially coupled capillary columns with different polarity of stationary phases by gas chromatography-mass spectrometry from the medicinal marine red alga Corallina elongata is reported. Nearly 200 hydrocarbons, halogen compounds, fatty acids, and other metabolites were found. Using this gas chromatography procedure we demonstrate the successful separation of different volatile organic compounds.

  17. Increments to chiral recognition facilitating enantiomer separations of chiral acids, bases, and ampholytes using Cinchona-based zwitterion exchanger chiral stationary phases.

    Science.gov (United States)

    Wernisch, Stefanie; Pell, Reinhard; Lindner, Wolfgang

    2012-07-01

    The intramolecular distances of anion and cation exchanger sites of zwitterionic chiral stationary phases represent potential tuning sites for enantiomer selectivity. In this contribution, we investigate the influence of alkanesulfonic acid chain length and flexibility on enantiomer separations of chiral acids, bases, and amphoteric molecules for six Cinchona alkaloid-based chiral stationary phases in comparison with structurally related anion and cation exchangers. Employing polar-organic elution conditions, we observed an intramolecular counterion effect for acidic analytes which led to reduced retention times but did not impair enantiomer selectivities. Retention of amphoteric analytes is based on simultaneous double ion pairing of their charged functional groups with the acidic and basic sites of the zwitterionic selectors. A chiral center in the vicinity of the strong cation exchanger site is vital for chiral separations of bases. Sterically demanding side chains are beneficial for separations of free amino acids. Enantioseparations of free (un-derivatized) peptides were particularly successful in stationary phases with straight-chain alkanesulfonic acid sites, pointing to a beneficial influence of more flexible moieties. In addition, we observed pseudo-enantiomeric behavior of quinine and quinidine-derived chiral stationary phases facilitating reversal of elution orders for all analytes. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. An inverse voter model for co-evolutionary networks: Stationary efficiency and phase transitions

    International Nuclear Information System (INIS)

    Zhu Chenping; Kong Hui; Li Li; Gu Zhiming; Xiong Shijie

    2011-01-01

    In some co-evolutionary networks, the nodes always flip their states between two opposite ones, changing the types of the links to others correspondingly. Meanwhile, the link-rewiring and state-flipping processes feed back each other, and only the links between the nodes in the opposite states are productive in generating flow for the network. We propose an inverse voter model to depict the basic features of them. New phase transitions from full efficiency to deficiency state are found by both the analysis and simulations starting from the random graphs and small-world networks. We suggest a new way to measure the efficiency of networks.

  19. Preparation by low-temperature nonthermal plasma of graphite fiber and its characteristics for solid-phase microextraction

    Energy Technology Data Exchange (ETDEWEB)

    Luo Fan [Department of Environmental Engineering, State Key Laboratory of Clean Energy Utilization, Key Laboratory of Polluted Environment Remediation and Ecological Health, MOE, Zhejiang University, Hangzhou 310027 (China); Wu Zucheng [Department of Environmental Engineering, State Key Laboratory of Clean Energy Utilization, Key Laboratory of Polluted Environment Remediation and Ecological Health, MOE, Zhejiang University, Hangzhou 310027 (China)], E-mail: wuzc@zju.edu.cn; Tao Ping [Institute of Structural Mechanics, China Academy of Engineering Physics, Mianyang 621900 (China); Cong Yanqing [College of Environmental Science and Engineering, Zhejiang Gongshang University, Hangzhou 310012 (China)

    2009-01-05

    Low-temperature nonthermal plasma has been used to prepare solid-phase microextraction (SPME) fibers with high adsorbability, long-term serviceability, and high reproducibility. Graphite rods serving as fiber precursors were treated by an air plasma discharged at 15.2-15.5 kV for a duration of 8 min. Sampling results revealed that the adsorptive capacity of the homemade fiber was 2.5-34.6 times that of a polyacrylate (PA) fiber for alcohols (methanol, ethanol, isopropyl alcohol, n-butyl alcohol), and about 1.4-1.6 times and 2.5-5.1 times that of an activated carbon fiber (ACF) for alcohols and BTEX (benzene, toluene, ethylbenzene, and xylenes), respectively. It is confirmed from FTIR (Fourier transform infrared spectrophotometer) and SEM (scanning electron microscope) analyses that the improvement in the adsorptive performance attributed to increased surface energy and roughness of the graphite fiber. Using gas chromatography (GC)-flame-ionization detector (FID), the limits of detection (LODs) of the alcohols and BTEX ranged between 0.19 and 3.75 {mu}g L{sup -1}, the linear ranges were between 0.6 and 35619 {mu}g L{sup -1} with good linearity (R{sup 2} = 0.9964-0.9997). It was demonstrated that nonthermal plasma offers a fast and simple method for preparing an efficient graphite SPME fiber, and that SPME using the homemade fiber represents a sensitive and selective extraction method for the analysis of a wide range of organic compounds.

  20. Non-stationary filtration mode during chemical reactions with the gas phase

    Science.gov (United States)

    Zavialov, Ivan; Konyukhov, Andrey; Negodyaev, Sergey

    2015-04-01

    An experimental and numerical study of filtration accompanied by chemical reactions between displacing fluid and solid skeleton is considered. Glass balls (400-500 μm in diameter) were placed in 1 cm gap between two glass sheets and were used as model porous medium. The baking soda was added to the glass balls. The 70% solution of acetic acid was used as the displacer. The modeling porous medium was saturated with a mineral oil, and then 70% solution of colored acetic acid was pumped through the medium. The glass balls and a mineral oil have a similar refractive index, so the model porous medium was optically transparent. During the filtration, the gas phase was generated by the chemical reactions between the baking soda and acetic acid, and time-dependent displacement of the chemical reaction front was observed. The front of the chemical reaction was associated with the most intensive gas separation. The front moved, stopped, and then moved again to the area where it had been already. We called this process a secondary oxidation wave. To describe this effect, we added to the balance equations a term associated with the formation and disappearance of phases due to chemical reactions. The equations were supplemented by Darcy's law for multiphase filtration. Nonstationarity front propagation of the chemical reaction in the numerical experiment was observed at Damköhler numbers greater than 100. The mathematical modelling was agreed well with the experimental results.

  1. Synchrotron X-ray diffraction studies of phase transitions in physisorbed monolayers of rare gases on graphite

    International Nuclear Information System (INIS)

    Bohr, J.

    1984-01-01

    This study is an investigation of phase transition in monoatomic layers adsorbed on graphite. Such effects can be considered physical realizations of two-dimensional systems. The experimental technique used is synchrotron X-ray diffraction. Systems which have been investigated include the commensurate-incommensurate phase transition in krypton monolayer. By adjusting the spreading pressure in the krypton layer by means of a coadsorbent deuterium gas it has been unambiguously demonstrated that at low temperatures the phase transition is of first order. A melting study of incommensurate argon monolayers demonstrates an experimental verification of the possibility for having a continuous melting transition in two-dimensions. Mixtures of two-components have been investigated for their phases. No (chemical) order-disorder transition is seen. A discussion is given on this lack of a chemical order. This lack is utilized to study the commensurate-incommensurate phase transition driven by average particle size. Finally, a special low-temperature phase is identified in a xenon monlayer which is diluted with freon. (Auth.)

  2. Sinorhizobium meliloti sigma factors RpoE1 and RpoE4 are activated in stationary phase in response to sulfite.

    Directory of Open Access Journals (Sweden)

    Bénédicte Bastiat

    Full Text Available Rhizobia are soil bacteria able to establish a nitrogen-fixing symbiosis with legume plants. Both in soil and in planta, rhizobia spend non-growing periods resembling the stationary phase of in vitro-cultured bacteria. The primary objective of this work was to better characterize gene regulation in this biologically relevant growth stage in Sinorhizobium meliloti. By a tap-tag/mass spectrometry approach, we identified five sigma factors co-purifying with the RNA polymerase in stationary phase: the general stress response regulator RpoE2, the heat shock sigma factor RpoH2, and three extra-cytoplasmic function sigma factors (RpoE1, RpoE3 and RpoE4 belonging to the poorly characterized ECF26 subgroup. We then showed that RpoE1 and RpoE4 i are activated upon metabolism of sulfite-generating compounds (thiosulfate and taurine, ii display overlapping regulatory activities, iii govern a dedicated sulfite response by controlling expression of the sulfite dehydrogenase SorT, iv are activated in stationary phase, likely as a result of endogenous sulfite generation during bacterial growth. We showed that SorT is required for optimal growth of S. meliloti in the presence of sulfite, suggesting that the response governed by RpoE1 and RpoE4 may be advantageous for bacteria in stationary phase either by providing a sulfite detoxification function or by contributing to energy production through sulfite respiration. This paper therefore reports the first characterization of ECF26 sigma factors, the first description of sigma factors involved in control of sulphur metabolism, and the first indication that endogenous sulfite may act as a signal for regulation of gene expression upon entry of bacteria in stationary phase.

  3. Nano-electrospray tandem mass spectrometric analysis of the acetylation state of histones H3 and H4 in stationary phase in Saccharomyces cerevisiae

    Directory of Open Access Journals (Sweden)

    Patterton Hugh G

    2011-07-01

    Full Text Available Abstract Background The involvement of histone acetylation in facilitating gene expression is well-established, particularly in the case of histones H3 and H4. It was previously shown in Saccharomyces cerevisiae that gene expression was significantly down-regulated and chromatin more condensed in stationary phase compared to exponential phase. We were therefore interested in establishing the acetylation state of histone H3 and H4 in stationary and in exponential phase, since the regulation of this modification could contribute to transcriptional shut-down and chromatin compaction during semi-quiescence. Results We made use of nano-spray tandem mass spectrometry to perform a precursor ion scan to detect an m/z 126 immonium ion, diagnostic of an Nε-acetylated lysine residue that allowed unambiguous identification of acetylated as opposed to tri-methylated lysine. The fragmentation spectra of peptides thus identified were searched with Mascot against the Swiss-Prot database, and the y-ion and b-ion fragmentation series subsequently analyzed for mass shifts compatible with acetylated lysine residues. We found that K9, K14 and K36 of histone H3 and K12 and K16 of histone H4 were acetylated in exponential phase (bulk histones, but could not detect these modifications in histones isolated from stationary phase cells at the sensitivity level of the mass spectrometer. The corresponding un-acetylated peptides were, however, observed. A significantly higher level of acetylation of these residues in exponential phase was confirmed by immuno-blotting. Conclusion H4K16 acetylation was previously shown to disrupt formation of condensed chromatin in vitro. We propose that de-acetylation of H4K16 allowed formation of condensed chromatin in stationary phase, and that acetylation of H3K9, H3K14, H3K36, and H4K12 reflected the active transcriptional state of the yeast genome in exponential phase.

  4. Thermal characterization of nitrates and nitrates/expanded graphite mixture phase change materials for solar energy storage

    International Nuclear Information System (INIS)

    Xiao, X.; Zhang, P.; Li, M.

    2013-01-01

    Highlights: • The addition of expanded graphite improved apparent thermal conductivity significantly. • The quadratic parallel model was used to predict the effective thermal conductivity. • The melting/freezing temperatures of mixture PCMs shifted slightly with adding of EG. - Abstract: Solar energy storage has become more attractive in recent years. In particular, latent thermal energy storage (LTES) with large energy storage density and isothermal heat storage/retrieval characteristics is a hot research topic. In the present study, sodium nitrate, potassium nitrate and their mixture were used as the base materials, and expanded graphite (EG) with high thermal conductivity and thermo-chemical stability was used as an additive to enhance the thermal conductivity. EG with various mass fractions was added to the base materials to form mixture phase change materials (PCMs), and the thermal characteristics of the mixtures were studied extensively. The transient hot-wire tests showed that the addition of EG enhanced the apparent thermal conductivity significantly, e.g. the apparent thermal conductivity of the nitrates/10 wt.% EG mixture PCM was increased by about 30–40%. The test results showed good agreement with theoretical calculations of the quadratic parallel model. Tests with differential scanning calorimeter (DSC) revealed that the melting/freezing temperatures of the mixture PCMs shifted slightly, compared with those of pure nitrates

  5. Application of magnetic graphitic carbon nitride nanocomposites for the solid-phase extraction of phthalate esters in water samples.

    Science.gov (United States)

    Wang, Man; Yang, Xiaodi; Bi, Wentao

    2015-02-01

    Magnetic graphitic carbon nitride nanocomposites were successfully prepared in situ and used to develop a highly sensitive magnetic solid-phase extraction method for the preconcentration of phthalate esters such as di-n-butyl phthalate, butyl phthalate, dihexyl phthalate, and di-(2-ethyl hexyl) phthalate from water. The adsorption and desorption of the phthalate esters on magnetic graphitic carbon nitride nanocomposites were investigated and the parameters affecting the partition of the phthalate esters, such as adsorption, desorption, recovery, were assessed. Under the optimized conditions, the proposed method showed excellent sensitivity with limits of detection (S/N = 3) in the range of 0.05-0.1 μg/L and precision in the range of 1.1-2.6% (n = 5). This method was successfully applied to the analysis of real water samples, and good spiked recoveries over the range of 79.4-99.4% were obtained. This research provides a possibility to apply this nanocomposite for adsorption, preconcentration, or even removal of various carbon-based ring or hydrophobic pollutants. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Synthesis and characterization of nanometric zinc oxide for a stationary phase in liquid chromatography

    Science.gov (United States)

    Gordillo-Delgado, F.; Soto-Barrera, C. C.; Plazas-Saldaña, J.

    2017-01-01

    The increasing demand for equipment to remove organic compounds in industry and research activity has led to evaluate nanometric zinc oxide (ZnO). In this work, we present the ZnO nanoparticles synthesis for reusing of discarded columns, as a low-cost alternative. The compound was obtained by sol-gel technique using zinc chloride and sodium hydroxide as precursors and a drying temperature of 169°C. An X-ray diffractometer was used to estimate the average particle size at 20.3±0.2nm the adsorption capacity was 0.0144L/g and the chemical resistance was tested with HCl and NaOH. The ZnO nanopowder was packed with 100psi pressure in an empty C-18 column cavity. The column packing resolution was evaluated using a high performance liquid chromatographer (HPLC-Thermo Scientific Dionex UltiMate 3000); using a caffeine standard, the following parameters were established: solvent flow: 1.2mL/min, average column temperature: 40°C, running time: 10 minutes, mobile phase acetonitrile-water composition (9:1). These results validate the potential of ZnO nanopowder as a column packing material in HPLC technique.

  7. Electrochromatographic performance of conventional and polar-embedded C16 silica monolithic stationary phases.

    Science.gov (United States)

    Ye, Fanggui; Huang, Baojun; Wang, Shun; Zhao, Shulin

    2010-11-01

    A novel monolithic silica column that has a polar-embedded amide-secondary amine group linking with C16 functionality for RP-CEC is described. The amide-secondary aminealkyloxysilane was synthesized by the reaction of 3-(2-aminoethylamino) propyltrimethoxysilane with hexadecanoyl chloride. Then, the silylant agent was bonded to the silica monolith matrix to produce hexadecanamide-secondary amine bonded silica (HDAIS) monolithic column. The electrochromatographic performance of HDAIS monolithic column for the separation of neutral, basic and polar solutes was studied, which was compared to that using the hexadecyl bonded silica monolithic column. The HDAIS monolithic column displayed reduced hydrophobic retention characteristics in the separation of five hydrophobic n-alkylbenzenes and four polar phenols when compared to the hexadecyl bonded silica monolithic column. A very much reduced silanol activity of HDAIS monolithic column was observed in the separation of test basic mixture including four aromatic amines, atenolol and metoprolol with 10 mM borate buffer (pH 7.5) containing 30% v/v ACN as the mobile phase. The comparison results indicate good performance for both polar and basic mixtures on HDAIS monolithic column in RP-CEC, and also show promising results for further applications.

  8. A reversed-phase/hydrophilic interaction mixed-mode C18-Diol stationary phase for multiple applications.

    Science.gov (United States)

    Wang, Qing; Ye, Mao; Xu, Li; Shi, Zhi-guo

    2015-08-12

    A mixed-mode chromatographic packing material, C18 and diol groups modified silica (C18-Diol), was prepared with controllable hydrophobicity and hydrophilicity. It demonstrated excellent aqueous compatibility and stability in aqueous mobile phase; compared to the traditional C18 column, improved peak shape of basic analytes was also obtained. Additionally, it exhibited both reversed-phase liquid chromatographic (RPLC) and hydrophilic interaction chromatographic (HILIC) performance; the analyte separation scope was thus enlarged, demonstrated by simultaneous separation of twenty acids, bases and neutrals. More interestingly, a novel on-line two-dimensional liquid chromatography on the single column (2D-LC-1C) was established by modifying the high performance liquid chromatographic instrument only with the addition of an extra six-port two-position valve. The early co-eluted components of the extract of Lonicera japonica on the 1st-dimension (RPLC) were collected for the online re-injection to the 2nd-dimension (HILIC) by conveniently varying the mobile phase components. Six more peaks were obtained. The established system was simple, easy operation and low cost, which had advantages in analyzing complicated samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Evaluation of mesoporous silicas functionalized with C18 groups as stationary phases for the solid-phase extraction of steroid hormones in milk.

    Science.gov (United States)

    Pérez-Fernández, Virginia; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; García, María Ángeles; Marina, María Luisa; Alonso, Isabel Sierra

    2014-06-01

    In this work, two mesoporous silicas functionalized with C18 groups (SM-C18 and SBA-15-C18) have been synthesized for their evaluation as stationary phases in SPE for the extraction and preconcentration of seven steroid hormones (estrone, estradiol, estriol, ethinyl estradiol, diethylstilbestrol, testosterone, and progesterone ) from milk. The characterization of both materials by diverse techniques such as transmission electron microscopy, SEM, thermogravimetric analysis, X-ray diffraction, and adsorption-desorption isotherms showed that the mesoporous silicas had a high surface area, high pore volume, and a homogeneous distribution of the pores and that both silicas presented a similar degree of functionalization. An analytical methodology for the simultaneous separation of the seven selected steroids by HPLC-DAD was developed. Both silicas were evaluated as stationary phases in SPE for the extraction of the steroid hormones from milk. This HPLC-DAD method was applied to the analysis of all extracts obtained in the SPE experiments, showing that from the two synthesized mesoporus silicas, SBA-15-C18 silica enabled the extraction of the seven compounds with recoveries between 88 and 108% for all except for estriol, for which a recovery of 62% was obtained. The analytical characteristics of this methodology were evaluated, showing good precision and linearity (R2 > 0.994) for all analytes. The comparison of the results obtained with this silica and those obtained with commercial C18 particles and with some other commercial cartridges usually employed in the extraction of steroids showed that SBA-15-C18 silica was able to extract the seven steroids with higher recovery values. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Preparation of chitosan-graft-(β-cyclodextrin) based sol-gel stationary phase for open-tubular capillary electrochromatography.

    Science.gov (United States)

    Lü, Haixia; Li, Qingyin; Yu, Xiaowei; Yi, Jiaojiao; Xie, Zenghong

    2013-07-01

    A novel open-tubular CEC column coated with chitosan-graft-(β-CD) (CDCS) was prepared using sol-gel technique. In the sol-gel approach, owing to the 3D network of sol-gel and the strong chemical bond between the stationary phase and the surface of capillary columns, good chromatographic characteristics and unique selectivity in separating isomers were shown. The column efficiencies of 55,000∼163,000 plates/m for the isomeric xanthopterin and phenoxy acid herbicides using the sol-gel-derived CDCS columns were achieved. Good stabilities were demonstrated that the RSD values for the retention time of thiourea and isoxanthopterin were 1.3 and 1.4% (run to run, n = 5), 1.6 and 2.0% (day to day, n = 3), 2.9 and 3.1% (column to column, n = 3), respectively. The sol-gel-coated CDCS columns have shown improved separations of isomeric xanthopterin in comparison with CDCS-bonded capillary column. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Enantiomeric Separation of 1-(Benzofuran-2-yl)alkylamines on Chiral Stationary Phases Based on Chiral Crown Ethers

    Energy Technology Data Exchange (ETDEWEB)

    Park, Soohyun; Kim, Sang Jun; Hyun, Myung Ho [Pusan National Univ., Busan (Korea, Republic of)

    2012-10-15

    Optically active chiral amines are important as building blocks for pharmaceuticals and as scaffolds for chiral ligands and, consequently, many efforts have been devoted to the development of efficient methods for their preparation. For example, reduction of amine precursors with chiral catalysts, enzymatic kinetic resolution or dynamic kinetic resolution of racemic amines and the direct amination of ketones with transaminases have been developed as the efficient methods for the preparation of optically active chiral amines. During the process of developing or utilizing optically active chiral amines, the methods for the determination of their enantiomeric composition are essential. Among various methods, liquid chromatographic resolution of enantiomers on chiral stationary phases (CSPs) have been known to be one of the most accurate and economic means for the determination of the enantiomeric composition of optically active chiral compounds. Especially, CSPs based on chiral crown ethers have been successfully used for the resolution of racemic primary amines. For example, CSPs based on (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid (CSP 1, Figure 1) or (3,3'-diphenyl-1,1'-binaphthyl)-20-crown-6 (CSP 2 and CSP 3, Figure 1) have been known to be quite effective for the resolution of cyclic and non-cyclic amines, various fluoroquinolone antibacterials containing a primary amino group, tocainide (antiarrhythmic agent) and its analogues, aryl-a-amino ketones and 3-amino-1,4-benzodiazepin-2-ones.

  12. Preparation and characterization of tentacle-type polymer stationary phase modified with graphene oxide for open-tubular capillary electrochromatography.

    Science.gov (United States)

    Gao, Xing; Mo, Rongzhen; Ji, Yibing

    2015-06-26

    In this research, a novel organic polymer coated stationary phase modified with inorganic nanomaterial was prepared for open-tubular capillary electrochromatography (OT-CEC). The capillary was developed by covalent attaching graphene oxide (GO) onto the tentacle-type polymer chains grafted capillary which was derivatized with ammonium hydroxide. Scanning electron microscopy (SEM) and Raman spectroscopy provided evidences that the tentacle-type polymer and GO were coated to the capillary inner wall. This novel GO-polymer modified capillary column generated a strong and stable electroosmotic flow (EOF) from anode to cathode with the running electrolytes of pH ranging from 4.0 to 9.0, and showed excellent separation ability toward neutral small molecules, amino acids and ephedrine-pseudoephedrine isomers with resolution higher than 2.30 and column efficiency up to over 170,000 plates/m. The repeatabilities of the GO-GMA@capillary were satisfying with relative standard deviations for intra-day and inter-day runs less than 3.27%, and column-to-column runs less than 7.49%. Additionally, the separation performance of GO-polymer modified capillary was compared with that of the polymer coated capillary and GO coated capillary. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Synergistic effects on enantioselectivity of zwitterionic chiral stationary phases for separations of chiral acids, bases, and amino acids by HPLC.

    Science.gov (United States)

    Hoffmann, Christian V; Pell, Reinhard; Lämmerhofer, Michael; Lindner, Wolfgang

    2008-11-15

    In an attempt to overcome the limited applicability scope of earlier proposed Cinchona alkaloid-based chiral weak anion exchangers (WAX) and recently reported aminosulfonic acid-based chiral strong cation exchangers (SCX), which are conceptionally restricted to oppositely charged solutes, their individual chiral selector (SO) subunits have been fused in a combinatorial synthesis approach into single, now zwitterionic, chiral SO motifs. The corresponding zwitterionic ion-exchange-type chiral stationary phases (CSPs) in fact combined the applicability spectra of the parent chiral ion exchangers allowing for enantioseparations of chiral acids and amine-type solutes in liquid chromatography using polar organic mode with largely rivaling separation factors as compared to the parent WAX and SCX CSPs. Furthermore, the application spectrum could be remarkably expanded to various zwitterionic analytes such as alpha- and beta-amino acids and peptides. A set of structurally related yet different CSPs consisting of either a quinine or quinidine alkaloid moiety as anion-exchange subunit and various chiral or achiral amino acids as cation-exchange subunits enabled us to derive structure-enantioselectivity relationships, which clearly provided strong unequivocal evidence for synergistic effects of the two oppositely charged ion-exchange subunits being involved in molecular recognition of zwitterionic analytes by zwitterionic SOs driven by double ionic coordination.

  14. Synthesis and characterization of a novel stationary phase, Si-Zr/Ti(PMTDS), based upon ternary oxide support for high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Amparo, Maura R.; Marques, Fabiana A.; Faria, Anizio M., E-mail: anizio@pontal.ufu.br [Universidade Federal de Uberlandia (FACIP/UFU), Ituiutaba, MG (Brazil). Faculdade de Ciencias Integradas do Pontal

    2013-09-15

    A new stationary phase based on the thermal immobilization of poly(methyltetradecylsiloxane) (PMTDS) on silica particles coated with a mixture of zirconia and titania was prepared and evaluated for the chromatographic separation of test mixtures. The spherical particles were characterized by elemental analysis, SEM, FTIR and {sup 29}Si NMR. The physicochemical properties of PMTDS phase supported on Si-Zr/Ti were intermediate between PMTDS phases supported on titanized silica and zirconized silica. The chromatographic performance of Si-Zr/Ti(PMTDS) phase was similar to PMTDS phases based on metal oxide coated silica having only one metal oxide and the preparation of a Si-Zr/Ti(PMTDS) phase allowed evaluation of the effect of each oxide, zirconia and titania, on the separation process and on the stability of the immobilized polymer phase. The hydrolytic stability of Si-Zr/Ti(PMTDS) stationary phase was similar to the Si-Ti(PMTDS) phase, improving the chemical stability of the silica-based PMTDS phase by about 100%. (author)

  15. An innovative monolithic zwitterionic stationary phase for the separation of phenolic acids in coffee bean extracts by capillary electrochromatography.

    Science.gov (United States)

    Murauer, Adele; Bakry, Rania; Schottenberger, Herwig; Huck, Christian; Ganzera, Markus

    2017-04-22

    A methacrylate based monolith, containing the innovative zwitterionic monomer (3-allyl-1-imidazol)propane sulfonate, was prepared in 100 μm I.D. silica capillaries by UV initiated photo-polymerization. Composition of the porogen, i.e. a mixture of 1-propanol, 1,4 butanediol and water, was of great importance to obtain a homogeneous monolith with satisfactory permeability and good electrochromatographic performance. Morphology of the stationary phase was studied in Scanning Electron Microscopy and IR experiments, which revealed a good attachment to the capillary wall, flowthrough-pores in the range of 0.5-2 μm, and a continuous monolithic structure. The developed material was well suited for the analysis of six common phenolic acids (salicylic, cinnamic, syringic, rosmarinic, caffeic and chlorogenic acid) by CEC. Their separation was possible in less than 8 min with a mobile phase comprising a 12 mM aqueous ammonium acetate solution with pH 8.5 and acetonitrile, at an applied voltage of - 20 kV. The developed method was validated (R 2  ≥ 0.995; LOD ≤ 3.9 μg mL -1 , except for salicylic acid; recovery rates from 94 to 104%) and successfully used for the determination of phenolic acids in Coffea arabica samples. All of them contained cinnamic, syringic and caffeic acid, however only in unroasted coffee beans chlorogenic acid (0.06%) was found. The quantitative results were in good agreement to reported literature data. Copyright © 2017 The Author(s). Published by Elsevier B.V. All rights reserved.

  16. Temperature-dependent thermal properties of a paraffin phase change material embedded with herringbone style graphite nanofibers

    International Nuclear Information System (INIS)

    Warzoha, Ronald J.; Weigand, Rebecca M.; Fleischer, Amy S.

    2015-01-01

    Highlights: • The thermal properties of a PCM with nanofibers are determined. • The solid-phase thermal conductivity scales exponentially with volume fraction. • The liquid-phase thermal conductivity is only enhanced beyond a critical percolation threshold. • The nanoscale interface resistance depends on the nanoparticle’s dimensionality. • The thermal diffusivity and volumetric heat capacity of the nanoenhanced PCMs are found. - Abstract: In many studies, carbon nanoparticles with high values of thermal conductivity (10–3000 W/m K) have been embedded into phase change thermal energy storage materials (PCMs) in order to enhance their bulk thermal properties. While a great deal of work to date has focused on determining the effect of these nanoparticles on a PCM’s solid phase thermal properties, little is known about their effect on its liquid phase thermal properties. Thus, in this study, the effect of implanting randomly oriented herringbone style graphite nanofibers (HGNF, average diameter = 100 nm, average length = 20 μm) on the bulk thermal properties of an organic paraffin PCM (IGI 1230A, T melt = 329.15 K) in both the solid and liquid phase is quantified. The bulk thermal conductivity, volumetric heat capacity and thermal diffusivity of HGNF/PCM nanocomposites are obtained as a function of temperature and HGNF volume loading level. It is found that the property enhancement varies significantly depending on the material phase. In order to explain the difference between solid and liquid phase thermal properties, heat flow at the nanoparticle–PCM and nanoparticle–nanoparticle interfaces is examined as a function of HGNF loading level and temperature. To do this, the solid and liquid phase thermal boundary resistances (TBRs) between the nanoparticles and the surrounding PCM and/or between contacting nanoparticles are found. Results suggest that the TBR at the HGNF–PCM interface is nearly double the TBR across the HGNF–HGNF interface in

  17. Construction of a hydrazone-linked chiral covalent organic framework-silica composite as the stationary phase for high performance liquid chromatography.

    Science.gov (United States)

    Zhang, Kai; Cai, Song-Liang; Yan, Yi-Lun; He, Zi-Hao; Lin, Hui-Mei; Huang, Xiao-Ling; Zheng, Sheng-Run; Fan, Jun; Zhang, Wei-Guang

    2017-10-13

    Covalent organic frameworks (COFs), as an emerging class of crystalline porous organic polymers, have great potential for applications in chromatographic separation owning to their fascinating crystalline structures and outstanding properties. However, development of COF materials as novel stationary phases in high performance liquid chromatography (HPLC) is just in its infancy. Herein, we report the design and construction of a new hydrazone-linked chiral COF, termed BtaMth COF, from a chiral hydrazide building block (Mth) and present a one-pot synthetic method for the fabrication of BtaMth@SiO 2 composite for HPLC separation of isomers. The as-synthesized BtaMth chiral COF displays good crystallinity, high porosity, as well as excellent chemical stability. Meanwhile, the fabricated HPLC column by using BtaMth@SiO 2 composite as the new stationary phase exhibits high resolution performances for the separation of positional isomers including nitrotoluene and nitrochlorobenzene, as well as cis-trans isomers including beta-cypermethrin and metconazole. Additionally, some effects such as the composition of the mobile phase and column temperature for HPLC separations on the BtaMth@SiO 2 packed column also have been studied in detail. The successful applications indicate the great potentials of hydrazone-linked chiral COF-silica composite as novel stationary phase for the efficient HPLC separation. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. The rye mutants identify a role for Ssn/Srb proteins of the RNA polymerase II holoenzyme during stationary phase entry in Saccharomyces cerevisiae.

    Science.gov (United States)

    Chang, Y W; Howard, S C; Budovskaya, Y V; Rine, J; Herman, P K

    2001-01-01

    Saccharomyces cerevisiae cells enter into a distinct resting state, known as stationary phase, in response to specific types of nutrient deprivation. We have identified a collection of mutants that exhibited a defective transcriptional response to nutrient limitation and failed to enter into a normal stationary phase. These rye mutants were isolated on the basis of defects in the regulation of YGP1 expression. In wild-type cells, YGP1 levels increased during the growth arrest caused by nutrient deprivation or inactivation of the Ras signaling pathway. In contrast, the levels of YGP1 and related genes were significantly elevated in the rye mutants during log phase growth. The rye defects were not specific to this YGP1 response as these mutants also exhibited multiple defects in stationary phase properties, including an inability to survive periods of prolonged starvation. These data indicated that the RYE genes might encode important regulators of yeast cell growth. Interestingly, three of the RYE genes encoded the Ssn/Srb proteins, Srb9p, Srb10p, and Srb11p, which are associated with the RNA polymerase II holoenzyme. Thus, the RNA polymerase II holoenzyme may be a target of the signaling pathways responsible for coordinating yeast cell growth with nutrient availability.

  19. Continuous beds (monoliths): stationary phases for liquid chromatography formed using the hydrophobic interaction-based phase separation mechanism.

    Science.gov (United States)

    Maruska, Audrius; Kornysova, Olga

    2004-04-30

    The pioneering research work published by Hjertén et al. [J. Chromatogr. 473 (1989) 273] in 1989 dealing with development and application of the continuous bed (monolithic) technique as an attractive alternative for the classical packed columns in chromatography, stimulated further investigations in this direction. The research data published since that time on the development and application of the continuous beds formed using hydrophobic interaction-based phase separation mechanism are reviewed. Some innovative species of the beds, such as polyrotaxane beds or nonparticulate restricted-access materials for direct analysis of the biological fluids in the capillary format are also discussed. Characteristic features and practical details of the continuous bed technique are revealed. Due to many advantages, the continuous bed technique became a competitor with the traditional packings in capillary or chip-based microanalysis. The importance of the continuous bed morphology on the chromatographic characteristics is shown. The applicability of modern microscopic analysis to evaluate the morphology of the continuous beds is demonstrated.

  20. Distinction of synthetic dl-α-tocopherol from natural vitamin E (d-α-tocopherol) by reversed-phase liquid chromatography. Enhanced selectivity of a polymeric C18 stationary phase at low temperature and/or at high pressure.

    Science.gov (United States)

    Yui, Yuko; Miyazaki, Shota; Ma, Yan; Ohira, Masayoshi; Fiehn, Oliver; Ikegami, Tohru; McCalley, David V; Tanaka, Nobuo

    2016-06-10

    Separation of diastereomers of dl-α-tocopherol was studied by reversed-phase liquid chromatography using three types of stationary phases, polymeric ODS, polymeric C30, and monomeric ODS. Polymeric ODS stationary phase (Inertsil ODS-P, 3mmID, 20cm) was effective for the separation of the isomers created by the presence of three chiral centers on the alkyl chain of synthetic dl-α-tocopherol. Considerable improvement of the separation of isomers was observed on ODS-P phase at high pressure and at low temperature. Complete separation of four pairs of diastereomers was achieved at 12.0°C, 536bar, while three peaks were observed when the separation was carried out either at 12.0°C at low pressure or at 20°C at 488bar. Higher temperature (30.0°C) with the ODS-P phase resulted in only partial separation of the diastereomers even at high pressure. Only slight resolution was observed for the mixture of diastereomers with the C30 stationary phase (Inertsil C30) at 12.0°C and 441bar, although the stationary phase afforded greater resolution for β- and γ-tocopherol than ODS-P. A monomeric C18 stationary phase did not show any separation at 12.0°C and 463bar. The results suggest that the binding site of the polymeric ODS-P phase is selective for flexible alkyl chains that provided the longest retention for the natural form, (R,R,R) form, and the enantiomer, (S,S,S) form, of dl-α-tocopherol. Copyright © 2016. Published by Elsevier B.V.

  1. Two Synthetic Methods for Preparation of Chiral Stationary Phases Using Crystalline Degradation Products of Vancomycin: Column Performance for Enantioseparation of Acidic and Basic Drugs.

    Science.gov (United States)

    Abdollahpour, Assem; Heydari, Rouhollah; Shamsipur, Mojtaba

    2017-07-01

    Two chiral stationary phases (CSPs) based on crystalline degradation products (CDPs) of vancomycin by using different synthetic methods were prepared and compared. Crystalline degradation products of vancomycin were produced by hydrolytic loss of ammonia from vancomycin molecules. Performances of two chiral columns prepared with these degradation products were investigated using several acidic and basic drugs as model analytes. Retention and resolution of these analytes on the prepared columns, as two main parameters, in enantioseparation were studied. The results demonstrated that the stationary phase preparation procedure has a significant effect on the column performance. The resolving powers of prepared columns for enantiomers resolution were changed with the variation in vancomycin-CDP coverage on the silica support. Elemental analysis was used to monitor the surface coverage of silica support by vancomycin-CDP. The results showed that both columns can be successfully applied to chiral separation studies.

  2. A facile liquid phase exfoliation method to prepare graphene sheets with different sizes expandable graphite

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Keqing; Shi, Yongqian [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei, Anhui 230026 (China); Jiang, Saihua [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei, Anhui 230026 (China); Suzhou Key Laboratory of Urban Public Safety, Suzhou Institute of University of Science and Technology of China, Suzhou, Jiangsu 215123 (China); Song, Lei [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei, Anhui 230026 (China); Hu, Yuan, E-mail: yuanhu@ustc.edu.cn [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei, Anhui 230026 (China); Suzhou Key Laboratory of Urban Public Safety, Suzhou Institute of University of Science and Technology of China, Suzhou, Jiangsu 215123 (China); Gui, Zhou, E-mail: zgui@ustc.edu.cn [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei, Anhui 230026 (China)

    2013-09-01

    Graphical abstract: - Highlights: • This study presented a novel method for the production of high-quality graphene sheets through the exfoliation of Li-intercalated EG with sonication. • The quality of the graphene sheets produced from different sizes EG was compared for the first time and the formation mechanism was discussed. • The graphene sheets obtained from the small size EG have less layers than the large size EG. - Abstract: In this work, graphene sheets suspension were synthesized directly from expandable graphite (EG) via an intercalation and exfoliation pathway using n-butyl lithium as the intercalating agent, water and N,N-dimethylformamide (DMF) as the exfoliating agent. The quality of the graphene sheets produced from different sizes EG was compared and the formation mechanism was discussed. The formation of the graphene sheets and its formation mechanism were confirmed by transmission electron microscopy (TEM), high-resolution TEM (HRTEM), selected area electron diffraction (SAED), Raman spectroscopy measurement, inductively coupled plasma atomic emission spectrometry (ICP-AES) and thermogravimetric analysis (TGA). The graphene sheets obtained from the small size EG have less layers than the large size EG.

  3. Involvement of GDH3-encoded NADP+-dependent glutamate dehydrogenase in yeast cell resistance to stress-induced apoptosis in stationary phase cells.

    Science.gov (United States)

    Lee, Yong Joo; Kim, Kyung Jin; Kang, Hong Yong; Kim, Hye-Rim; Maeng, Pil Jae

    2012-12-28

    Glutamate metabolism is linked to a number of fundamental metabolic pathways such as amino acid metabolism, the TCA cycle, and glutathione (GSH) synthesis. In the yeast Saccharomyces cerevisiae, glutamate is synthesized from α-ketoglutarate by two NADP(+)-dependent glutamate dehydrogenases (NADP-GDH) encoded by GDH1 and GDH3. Here, we report the relationship between the function of the NADP-GDH and stress-induced apoptosis. Gdh3-null cells showed accelerated chronological aging and hypersusceptibility to thermal and oxidative stress during stationary phase. Upon exposure to oxidative stress, Gdh3-null strains displayed a rapid loss in viability associated with typical apoptotic hallmarks, i.e. reactive oxygen species accumulation, nuclear fragmentation, DNA breakage, and phosphatidylserine translocation. In addition, Gdh3-null cells, but not Gdh1-null cells, had a higher tendency toward GSH depletion and subsequent reactive oxygen species accumulation than did WT cells. GSH depletion was rescued by exogenous GSH or glutamate. The hypersusceptibility of stationary phase Gdh3-null cells to stress-induced apoptosis was suppressed by deletion of GDH2. Promoter swapping and site-directed mutagenesis of GDH1 and GDH3 indicated that the necessity of GDH3 for the resistance to stress-induced apoptosis and chronological aging is due to the stationary phase-specific expression of GDH3 and concurrent degradation of Gdh1 in which the Lys-426 residue plays an essential role.

  4. Branched polyethyleneimine-bonded tentacle-type polymer stationary phase for peptides and proteins separations by open-tubular capillary electrochromatography.

    Science.gov (United States)

    Zhang, Xiaowei; Yang, Juan; Liu, Shaofeng; Lin, Xucong; Xie, Zenghong

    2011-12-01

    A novel tentacle-type polymer stationary phase covalently modified with branched polyethyleneimine (PEI) was developed for peptides and proteins separations by open-tubular CEC (OT-CEC). The preparation procedure included the silanization of capillary inner wall, in situ graft polymerization and PEI functionalization. A wrinkly polymer surface of multitudinous steric amine groups was evenly formed on the capillary inner wall, and anodic EOF could be gained within a wide pH range of 2.5-7.5. The electroosmotic mobility was examined for its dependence on pH as well as PEI concentrations. Good repeatability was gained with RSD for the migration time of EOF marker within 4.8% and satisfactory chemical stability was validated. Due to the existence of amine groups on the surface of tentacle-type polymer stationary phase, the silanol effect that occurs between the positively charged biomolecules and the silanols of the capillary column was greatly suppressed. Compared with a monolayer-coating capillary, seven enkephalin-related peptides were well resolved on the PEI-bonded column with high efficiencies. Favorable separations of peptides and proteins with high column efficiencies were obtained in 144,000-189,000 and 97,000-170,000 plates/m. Branched PEI-bonded tentacle-type polymer stationary phase has been proven to afford satisfactory retention and resolution of peptides and proteins. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Solid-phase extraction of polar pesticides from environmental water samples on graphitized carbon and Empore-activated carbon disks and on-line coupling to octadecyl-bonded silica analytical columns.

    NARCIS (Netherlands)

    Slobodník, J.; Oztekizan, O.; Lingeman, H.; Brinkman, U.A.T.

    1996-01-01

    The suitability of Empore-activated carbon disks (EACD), Envi-Carb graphitized carbon black (GCB) and CPP-50 graphitized carbon for the trace enrichment of polar pesticides from water samples was studied by means of off-line and on-line solid-phase extraction (SPE). In the off-line procedure, 0.5-2

  6. High performance liquid chromatographic separation of thirteen drugs collected in Chinese Pharmacopoeia 2010(Ch.P2010 on cellulose ramification chiral stationary phase

    Directory of Open Access Journals (Sweden)

    Ying Zhou

    2012-02-01

    Full Text Available The enantiomers separation of thirteen drugs collected in Ch.P2010 was performed on chiral stationary phase of cellulose ramification (chiralpak OD and chiralpak OJ by high performance liquid chromatographic (HPLC methods, which included ibuprofen (C1, ketoprofen (C2, nitrendipine (C3, nimodipine (C4, felodipine (C5, omeprazole (C6, praziquantel (C7, propranolol hydrochloride (C8, atenolol (C9, sulpiride (C10, clenbuterol hydrochloride (C11, verapamil hydrochloride (C12, and chlorphenamine maleate (C13. The mobile phase consisted of isopropanol and n-hexane. The detection wavelength was set at 254 nm and the flow rate was 0.7 mL/min. The enantiomers separation of these thirteen racemates on chiralpak OD column and chiralpak OJ column was studied, while the effects of proportion of organic additives, alcohol displacer and temperature on the separation were studied. And the mechanism of some of racemates was discussed. The results indicated that thirteen chiral drugs could be separated on chiral stationary phase of cellulose ramification in normal phase chromatographic system. The chromatographic retention and resolution of enantiomers could be adjusted by factors including column temperature and the concentration of alcohol displacer and organic alkaline modifier in mobile phase. It was shown that the resolution was improved with reducing concentration of alcohol displacer. When concentration of organic alkaline modifier was 0.2% (v/v, the resolution and the peak shape were fairly good. Most racemates mentioned above had better resolution at column temperature of 25 °C. When racemates were separated, the temperature should be kept so as to obtain stable separation results. Keywords: HPLC, Chiral stationary phase, Optical enantiomers, Cellulose ramification

  7. Comparison of Various Types of Stationary Phases in Non-Aqueous Reversed-Phase High-Performance Liquid Chromatography–Mass Spectrometry of Glycerolipids in Blackcurrant Oil and Its Enzymatic Hydrolysis Mixture

    Czech Academy of Sciences Publication Activity Database

    Lísa, M.; Holčapek, M.; Sovová, Helena

    2009-01-01

    Roč. 1216, č. 47 (2009), s. 8371-8378 ISSN 0021-9673 Institutional research plan: CEZ:AV0Z40720504 Keywords : ultra high-performance liquid chromatography * C30 stationary phase * triacylglycerols Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.101, year: 2009

  8. Liquid chromatographic resolution of racemic rasagiline and its analogues on a chiral stationary phase based on (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid.

    Science.gov (United States)

    Tak, Kyung Mi; Park, Eun Ju; Hyun, Myung Ho

    2013-12-01

    A liquid chromatographic chiral stationary phase based on (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid was applied to the resolution of 15 analytes, including racemic rasagiline, a chiral drug for the treatment of Parkinson's disease, and its analogues. The composition of mobile phase was optimized to be ethanol/acetonitrile/acetic acid/triethylamine (80:20:0.2:0.3, v/v/v/v) by evaluating the chromatographic results for the resolution of five selected analytes under various mobile phase conditions. Under the optimized mobile phase conditions, racemic rasagiline was resolved quite well with a separation factor of 1.48 and resolution of 2.71 and its 14 analogues were also resolved reasonably well with separation factors of 1.06-1.54 and resolutions of 0.54-2.11. Among 15 analytes, racemic rasagiline was resolved best except for just one analyte. The analyte structure-enantioselectivity relationship indicated that racemic rasagiline has the most appropriate structural characteristics for resolution on the chiral stationary phase. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Application of a cholesterol stationary phase in the analysis of phosphorothioate oligonucleotides by means of ion pair chromatography coupled with tandem mass spectrometry.

    Science.gov (United States)

    Studzińska, Sylwia; Krzemińska, Katarzyna; Szumski, Michał; Buszewski, Bogusław

    2016-07-01

    The main aim of this study was the investigation of the influence of several ion pair reagents towards both the retention and the mass spectrometry sensitivity of phosphorothioate oligonucleotides. A cholesterol stationary phase was applied for the first time in the analysis of this group of compounds. The mobile phase composition was modified by changing the concentration and the type of amines and acetates or 1,1,1,3,3,3-hexafluoroisopropanol. It has been shown that the increase of amines concentration results in the retention factor increase for each oligonucleotide, on each adsorbent. The only exception was the mobile phase composed of triethylamine and 1,1,1,3,3,3-hexafluoroisopropanol. This is a consequence of interactions taking place between a cholesterol molecule and an alcohol. This effect was convenient when the mass spectrometry detection was applied, since it allowed an increase in the sensitivity. Moreover, optimization of the mobile phase composition and its impact on the efficiency of ionization process and on the sensitivity in mass spectrometry were also presented. The optimization of this new method, based on cholesterol stationary phase coupled with mass spectrometry detection, was finally applied for the determination of phosphorothioate oligonucleotides impurity in a real sample. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Experimental Investigation on Thermal Management of Electric Vehicle Battery Module with Paraffin/Expanded Graphite Composite Phase Change Material

    Directory of Open Access Journals (Sweden)

    Jiangyun Zhang

    2017-01-01

    Full Text Available The temperature has to be controlled adequately to maintain the electric vehicles (EVs within a safety range. Using paraffin as the heat dissipation source to control the temperature rise is developed. And the expanded graphite (EG is applied to improve the thermal conductivity. In this study, the paraffin and EG composite phase change material (PCM was prepared and characterized. And then, the composite PCM have been applied in the 42110 LiFePO4 battery module (48 V/10 Ah for experimental research. Different discharge rate and pulse experiments were carried out at various working conditions, including room temperature (25°C, high temperature (35°C, and low temperature (−20°C. Furthermore, in order to obtain the practical loading test data, a battery pack with the similar specifications by 2S∗2P with PCM-based modules were installed in the EVs for various practical road experiments including the flat ground, 5°, 10°, and 20° slope. Testing results indicated that the PCM cooling system can control the peak temperature under 42°C and balance the maximum temperature difference within 5°C. Even in extreme high-discharge pulse current process, peak temperature can be controlled within 50°C. The aforementioned results exhibit that PCM cooling in battery thermal management has promising advantages over traditional air cooling.

  11. 2-DE based proteomic analysis of Saccharomyces cerevisiae wild and K+ transport-affected mutant (trk1,2) strains at the growth exponential and stationary phases.

    Science.gov (United States)

    Curto, Miguel; Valledor, Luis; Navarrete, Clara; Gutiérrez, Dolores; Sychrova, Hana; Ramos, José; Jorrin, Jesús

    2010-11-10

    By using a 2-DE based workflow, the proteome of wild and potassium transport mutant trk1,2 under optimal growth potassium concentration (50mM) has been analyzed. At the exponential and stationary phases, both strains showed similar growth, morphology potassium content, and Vmax of rubidium transport, the only difference found being the Km values for this potassium analogue transport, higher for the mutant (20mM) than for the wild (3-6mM) cells. Proteins were buffer-extracted, precipitated, solubilized, quantified, and subjected to 2-DE analysis in the 5-8 pH range. More differences in protein content (37-64mgg(-1) cell dry weight) and number of resolved spots (178-307) were found between growth phases than between strains. In all, 164 spots showed no differences between samples and a total of 105 were considered to be differential after ANOVA test. 171 proteins, corresponding to 71 unique gene products have been identified, this set being dominated by cytosolic species and glycolitic enzymes. The ranking of the more abundant spots revealed no differences between samples and indicated fermentative metabolism, and active cell wall biosynthesis, redox homeostasis, biosynthesis of amino acids, coenzymes, nucleotides, and RNA, and protein turnover, apart from cell division and growth. PCA analysis allowed the separation of growth phases (PC1 and 2) and strains at the stationary phase (PC3 and 4), but not at the exponential one. These results are also supported by clustering analysis. As a general tendency, a number of spots newly appeared at the stationary phase in wild type, and to a lesser extent, in the mutant. These up-accumulated spots corresponded to glycolitic enzymes, indicating a more active glucose catabolism, accompanied by an accumulation of methylglyoxal detoxification, and redox-homeostasis enzymes. Also, more extensive proteolysis was observed at the stationary phase with this resulting in an accumulation of low Mr protein species. Copyright © 2010

  12. Effect of pressure on the selectivity of polymeric C18 and C30 stationary phases in reversed-phase liquid chromatography. Increased separation of isomeric fatty acid methyl esters, triacylglycerols, and tocopherols at high pressure.

    Science.gov (United States)

    Okusa, Kensuke; Iwasaki, Yuki; Kuroda, Ikuma; Miwa, Shohei; Ohira, Masayoshi; Nagai, Toshiharu; Mizobe, Hoyo; Gotoh, Naohiro; Ikegami, Tohru; McCalley, David V; Tanaka, Nobuo

    2014-04-25

    A high-density, polymeric C18 stationary phase (Inertsil ODS-P) or a polymeric C30 phase (Inertsil C30) provided improved resolution of the isomeric fatty acids (FAs), FA methyl esters (FAMEs), triacylglycerols (TAGs), and tocopherols with an increase in pressure of 20-70MPa in reversed-phase HPLC. With respect to isomeric C18 FAMEs with one cis-double bond, ODS-P phase was effective for recognizing the position of a double bond among petroselinic (methyl 6Z-octadecenoate), oleic (methyl 9Z-octadecenoate), and cis-vaccenic (methyl 11Z-octadecenoate), especially at high pressure, but the differentiation between oleic and cis-vaccenic was not achieved by C30 phase regardless of the pressure. A monomeric C18 phase (InertSustain C18) was not effective for recognizing the position of the double bond in monounsaturated FAME, while the separation of cis- and trans-isomers was achieved by any of the stationary phases. The ODS-P and C30 phases provided increased separation for TAGs and β- and γ-tocopherols at high pressure. The transfer of FA, FAME, or TAG molecules from the mobile phase to the ODS-P stationary phase was accompanied by large volume reduction (-30∼-90mL/mol) resulting in a large increase in retention (up to 100% for an increase of 50MPa) and improved isomer separation at high pressure. For some isomer pairs, the ODS-P and C30 provided the opposite elution order, and in each case higher pressure improved the separation. The two stationary phases showed selectivity for the isomers having rigid structures, but only the ODS-P was effective for differentiating the position of a double bond in monounsaturated FAMEs. The results indicate that the improved isomer separation was provided by the increased dispersion interactions between the solute and the binding site of the stationary phase at high pressure. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Novel bis(5-methyltetrazolium)amine ligand-bonded stationary phase with reduced leakage of metal ions in immobilized metal affinity chromatography of proteins.

    Science.gov (United States)

    Bo, Chunmiao; Wang, Chaozhan; Wei, Yinmao

    2016-11-01

    Immobilized metal affinity chromatography (IMAC) has been widely used for the specific separation of biopolymers. However, leakage of metal ions from IMAC adsorbents is of concern in IMAC. In this study, we designed a novel tridenate bis(5-methyltetrazolium)amine (BMTA) to reduce the leakage of metal ions by improving the affinity to immobilized metal ions. The ligand was bonded onto silica via three-step reaction to prepare a high-performance IMAC stationary phase. The chromatographic behaviors of ribonuclease A, cytochrome c, and lysozyme on the Cu(II)-, Ni(II)-, and Zn(II)-chelated stationary phase were investigated with respect to pH effect and elution with an imidazole gradient. The retention times of these three proteins increased by increasing the pH of the mobile phase but decreased by increasing the concentration of the competitive displacer. The retaining strength of the three proteins on the chelated stationary phase were in the order Cu(II) > Ni(II) > Zn(II). The behavior of these three proteins was consistent with the properties of a typical IMAC. The BMTA ligand exhibited a much stronger affinity for Cu(II) and Ni(II) than iminodiacetic acid (IDA), which is often regarded as a standard tridentate IMAC ligand. Quantum mechanical calculations at the B3LYP/6-31G level were used to image the coordination mode of the protein-metal ions-BMTA complex. In addition, a fused histidine-tagged cecropin b-human epidermal growth factor (CB-EGF) from Escherichia coli crude extract was purified by the Ni(II)-chelated stationary phase, and the purity of the CB-EGF was determined to be at least 90 %. These results suggest that the BMTA ligand may have potential applications in the preparation of therapeutics. Graphical Abstract A novel ligand of tridenate bis(5-methyltetrazolium)amine (BMTA) was designed to reduce the leakage of metal ions from the column in immobolized metal affinity chromatography (IMAC).

  14. Graphites for nuclear applications; Les graphites pour les applications nucleaires

    Energy Technology Data Exchange (ETDEWEB)

    Bonal, J.P.; Gosmain, L. [CEA Saclay, Dept. des Materiaux pour le Nucleaire (DMN), Lab. de Microscopie et d' Etudes de l' Endommagement, 91 - Gif-sur-Yvette (France)

    2006-03-15

    Being an excellent neutron moderator, graphite is used as a structural material in many nuclear reactor types. By the end of the 50's, the French gas-cooled reactor development needed manufacturing of a nuclear-grade graphite. Graphite irradiation can lead to in-lattice energy accumulation, dimensional changes and physical properties modification. Moreover, the radiolytic corrosion induced by the coolant (CO{sub 2}) may generate mechanical properties degradation. Today, French gas-cooled reactors are all in their decommissioning phase that requires the knowledge of the radiological inventory of the irradiated graphites. At present time, graphite is still foreseen as a future material for hydrogen production by high temperature gas cooled nuclear plants. In the future, graphite will be the necessary moderator material for high temperature reactors with thermal neutron spectrum dedicated to hydrogen and electricity production. (authors)

  15. Solvation molar enthalpies and heat capacities of n-alkanes and n-alkylbenzenes on stationary phases of wide-ranging polarity.

    Science.gov (United States)

    Lebrón-Aguilar, Rosa; Quintanilla-López, Jesús Eduardo; Santiuste, José María

    2010-12-03

    A comparison of the most usual gas chromatographic methods for the calculation of partial molar enthalpies of solvation (Δ(sol)H(o)) has been carried out. Those methods based on the fitting of lnV(g) or ln(k/T) vs. 1/T and ln(k/T) vs. (1/T and the temperature arrangement, T(a)) are the most adequate ones for obtaining Δ(sol)H(o) values. However, the latter is the only reliable option for Δ(sol)H(o) estimation when commercial WCOT capillary columns are used, since in this case the estimation of some variables involved in the V(g) determination is less accurate or even impossible. Consequently, in this paper, Δ(sol)H(o) obtained from ln(k/T) vs. (1/T+T(a)) fitting at 373.15 and 298.15K for n-alkanes and n-alkylbenzenes on 12 commercial capillary columns coated with stationary phases covering the 203-3608 McReynolds polarity range are reported. Moreover, molar heat capacities of solvation at constant pressure (Δ(sol)C(p)(o)) have also been calculated using this method. A clear influence on Δ(sol)H(o) of the type and content of the substitution group in the stationary phase was observed. In addition, a linear relationship of Δ(sol)C(p)(o) with the van der Waals volume of the n-alkanes and the temperature gradient of density of the stationary phase was found. The effect of the size of the hydrocarbon on both thermodynamic variables was also investigated. Copyright © 2010 Elsevier B.V. All rights reserved.

  16. Stationary Frame Current Control Evaluations for Three-Phase Grid-Connected Inverters with PVR-based Active Damped LCL Filters

    DEFF Research Database (Denmark)

    Han, Yang; Shen, Pan; Guerrero, Josep M.

    2016-01-01

    Grid-connected inverters (GCIs) with LCL output filter have the ability of attenuating high-frequency (HF) switching ripples. However, by using only grid-current control, the system is prone to resonances if it is not properly damped, and the current distortion would be amplified significantly...... to suppress the LCL resonance is proposed. Although both proportional-resonant (PR) controller in αβ stationary frame and PI controller in dq synchronous frame achieve zero steady-state error, the amplitude- and phase-frequency characteristics differ greatly from each other except for the reference tracking...

  17. Artificial graphites

    International Nuclear Information System (INIS)

    Maire, J.

    1984-01-01

    Artificial graphites are obtained by agglomeration of carbon powders with an organic binder, then by carbonisation at 1000 0 C and graphitization at 2800 0 C. After description of the processes and products, we show how the properties of the various materials lead to the various uses. Using graphite enables us to solve some problems, but it is not sufficient to satisfy all the need of the application. New carbonaceous material open application range. Finally, if some products are becoming obsolete, other ones are being developed in new applications [fr

  18. The use of Stationary Phase Optimized Selectivity Liquid Chromatography for the development of herbal fingerprints to detect targeted plants in plant food supplements.

    Science.gov (United States)

    Deconinck, E; Djiogo, C A Sokeng; Kamugisha, A; Courselle, P

    2017-08-01

    The consumption of plant food supplements is increasing steadily and more and more, these products are bought through internet. Often the products sold through internet are not registered or declared with a national authority, meaning that no or minimal quality control is performed and that they could contain herbs or plants that are regulated. Stationary Phase Optimized Selectivity Liquid Chromatography (SOS-LC) was evaluated for the development of specific fingerprints, to be used for the detection of targeted plants in plant food supplements. Three commonly used plants in plant food supplements and two regulated plants were used to develop fingerprints with SOS-LC. It was shown that for all plants specific fingerprints could be obtained, allowing the detection of these targeted plants in triturations with different herbal matrices as well as in real samples of suspicious supplements seized by the authorities. For three of the five plants a more specific fingerprint was obtained, compared to the ones developed on traditional columns described in literature. It could therefore be concluded that the combination of segments of different types of stationary phases, as used in SOS-LC, has the potential of becoming a valuable tool in the quality control and the identification of crude herbal or plant material and in the detection of regulated plants in plant food supplements or other herbal preparations. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Novel tentacle-type polymer stationary phase grafted with anion exchange polymer chains for open tubular CEC of nucleosides and proteins.

    Science.gov (United States)

    Aydoğan, Cemil; Çetin, Kemal; Denizli, Adil

    2014-08-07

    A novel and simple method for preparation of a tentacle-type polymer stationary phase grafted with polyethyleneimine (PEI) anion exchanger was developed for open tubular capillary electrochromatography (OT-CEC) of nucleosides and proteins. The polymeric stationary phase was prepared using 3-chloro-2-hydroxypropyl methacrylate (HPMA-Cl)-based reactive monomer. The preparation procedure included pretreatment of the capillary inner wall, silanization, in situ graft polymerization with HPMA-Cl and PEI modification. To compare with the tentacle-type capillary column with PEI functionalization, a monolayer capillary column without PEI functionalization was also prepared. The electrochromatographic characterization of the prepared open tubular column was performed using alkylbenzenes. The electroosmotic flow (EOF) with regard to PEI concentrations and the running buffer pH was investigated. The separation conditions of the nucleosides and the proteins were optimized. The modified tentacle-type column with high anion exchange capacity has proven to afford better retention and resolution for the separation of nucleosides and proteins. The PEI functionalization column can also provide long-term stable use for biomolecule separation using a single capillary with relative standard deviation values of retention times of less than 2%. The results indicate that the present method for open tubular capillary preparation with a HPMA-Cl-based reactive monomer is promising for OT-CEC biomolecule separation.

  20. Characterization of polyaniline-coated stationary phases by using the linear solvation energy relationship in the hydrophilic interaction liquid chromatography mode using capillary liquid chromatography.

    Science.gov (United States)

    Taraba, Lukáš; Křížek, Tomáš; Hodek, Ondřej; Kalíková, Květa; Coufal, Pavel

    2017-02-01

    A polyaniline coating was used to modify the surface of bare silica gel and octadecyl silica stationary phases to characterize the properties of altered materials. It was assumed that the mixed-mode retention was established on the basis of the polyaniline chemical structure and its combination with the original sorbents. Polyaniline was deposited onto the original surfaces during the chemical polymerization of aniline hydrochloride. The prepared materials were slurry packed into capillary columns and systematic chromatographic characterization was performed using the linear solvation energy relationship, also employing descriptors that allow inclusion of ionic interactions in the proposed retention mechanism. The retention times of 80 solutes with various chemical structures were measured in the hydrophilic interaction liquid chromatography mode. The obtained results demonstrated the significant contribution of the polyaniline coating to the retention mechanism under the given conditions; the assumed mixed-mode retention was confirmed. The dominant retention interaction for both modified stationary phases was based on the protonation of nitrogen atoms in the polyaniline structure, leading to suitable retention and selectivity for the hydrophilic analytes, especially anionic and zwitterionic species. Thus, especially, the polyaniline-coated bare silica gel sorbent seems to be promising for potential applications related to the separation of polar compounds. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Comparison of the peak resolution and the stationary phase retention between the satellite and the planetary motions using the coil satellite centrifuge with counter-current chromatographic separation of 4-methylumbelliferyl sugar derivatives

    Science.gov (United States)

    Shinomiya, Kazufusa; Zaima, Kazumasa; Harada, Yukina; Yasue, Miho; Harikai, Naoki; Tokura, Koji; Ito, Yoichiro

    2016-01-01

    Coil satellite centrifuge (CSC) produces the complex satellite motion consisting of the triplicate rotation of the coiled column around three axes including the sun axis (the angular velocity, ω1), the planet axis (ω2) and the satellite axis (the central axis of the column) (ω3) according to the following formula: ω1 = ω2 + ω3. Improved peak resolution in the separation of 4-methylumbelliferyl sugar derivatives was achieved using the conventional multilayer coiled columns with ethyl acetate/1-butanol/water (3 : 2 : 5, v/v) for the lower mobile phase at the combination of the rotation speeds (ω1, ω2, ω3) = (300, 150, 150 rpm), and (1 : 4 : 5, v/v) for the upper mobile phase at (300 : 100 : 200 rpm). The effect of the satellite motion on the peak resolution and the stationary phase retention was evaluated by each CSC separation with the different rotation speeds of ω2 and ω3 under the constant revolution speed at ω1 = 300 rpm. With the lower mobile phase, almost constant peak resolution and stationary phase retention were yielded regardless of the change of ω2 and ω3, while with the upper mobile phase these two values were sensitively varied according to the different combination of ω2 and ω3. For example, when ω2 = 147 or 200 rpm is used, no stationary phase was retained in the coiled column while ω2 = 150 rpm could retain enough volume of stationary phase for separation. On the other hand, the combined rotation speeds at (ω1, ω2, ω3) = (300, 300, 0 rpm) or (300, 0, 300 rpm) produced insufficient peak resolution regardless of the choice of the mobile phase apparently due to the lack of rotation speed except at (300, 0, 300 rpm) with the upper mobile phase. At lower rotation speed of ω1 = 300 rpm, better peak resolution and stationary phase retention were obtained by the satellite motion (ω3) than by the planetary motion (ω2), or ω3 > ω2. The effect of the hydrophobicity of the two-phase solvent systems on the stationary phase retention was

  2. Dynamic high performance liquid chromatography on chiral stationary phases. Low temperature separation of the interconverting enantiomers of diazepam, flunitrazepam, prazepam and tetrazepam.

    Science.gov (United States)

    Sabia, Rocchina; Ciogli, Alessia; Pierini, Marco; Gasparrini, Francesco; Villani, Claudio

    2014-10-10

    Diazepam and the structurally related 1,4-benzodiazepin-2-ones tetrazepam, prazepam and flunitrazepam are chiral molecules because they adopt a ground state conformation featuring a non-planar seven membered ring devoid of any reflection-symmetry element. The two conformational enantiomers of this class of benzodiazepines interconvert rapidly at room temperature by a simple ring flipping process. Low temperature HPLC on the Whelk-O1 chiral stationary phase allowed us to separate the conformational enantiomers of diazepam and of the related 1,4-benzodiazepin-2-ones, under conditions where the interconversion rate is sufficiently low, compared to the chromatographic separation rate. Diazepam, tetrazepam and prazepam showed temperature dependent dynamic HPLC profiles with interconversion plateaus indicative of on-column enantiomer interconversion (enantiomerization) in the temperature range between -10 °C and -35 °C, whereas for flunitrazepam on-column interconversion was observed at temperatures between -40 °C and -66 °C. Simulation of exchange-deformed HPLC profiles using a computer program based on the stochastic model yielded the apparent rate constants for the on-column enantiomerization and the corresponding free energy activation barriers. At -20 °C the enantiomerization barriers, ΔG(≠), for diazepam, prazepam and tetrazepam were determined to be in the range 17.6-18.7 kcal/mol. At -55 °C ΔG(≠) for flunitrazepam was determined to be in the 15.6-15.7 kcal/mol range. The experimental dynamic chromatograms and the corresponding interconversion barriers reported in this paper call for a reinterpretation of previously published results on the HPLC behavior of diazepam on chiral stationary phases. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Response surface methodology for the determination of the design space of enantiomeric separations on cinchona-based zwitterionic chiral stationary phases by high performance liquid chromatography.

    Science.gov (United States)

    Hanafi, Rasha Sayed; Lämmerhofer, Michael

    2018-01-26

    Quality-by-Design approach for enantioselective HPLC method development surpasses Quality-by-Testing in offering the optimal separation conditions with the least number of experiments and in its ability to describe the method's Design Space visually which helps to determine enantiorecognition to a significant extent. Although some schemes exist for enantiomeric separations on Cinchona-based zwitterionic stationary phases, the exact design space and the weights by which each of the chromatographic parameters influences the separation have not yet been statistically studied. In the current work, a screening design followed by a Response Surface Methodology optimization design were adopted for enantioseparation optimization of 3 model drugs namely the acidic Fmoc leucine, the amphoteric tryptophan and the basic salbutamol. The screening design proved that the acid/base additives are of utmost importance for the 3 chiral drugs, and that among 3 different pairs of acids and bases, acetic acid and diethylamine is the couple able to provide acceptable resolution at variable conditions. Visualization of the response surface of the retention factor, separation factor and resolution helped describe accurately the magnitude by which each chromatographic factor (% MeOH, concentration and ratio of acid base modifiers) affects the separation while interacting with other parameters. The global optima compromising highest enantioresolution with the least run time for the 3 chiral model drugs varied extremely, where it was best to set low % methanol with equal ratio of acid-base modifiers for the acidic drug, very high % methanol and 10-fold higher concentration of the acid for the amphoteric drug while 20 folds of the base modifier with moderate %methanol were needed for the basic drug. Considering the selected drugs as models for many series of structurally related compounds, the design space defined and the optimum conditions computed are the key for method development on

  4. Diastereo- and enantioseparation of a Nα-Boc amino acid with a zwitterionic quinine-based stationary phase: Focus on the stereorecognition mechanism

    International Nuclear Information System (INIS)

    Ianni, Federica; Carotti, Andrea; Marinozzi, Maura; Marcelli, Gloria; Di Michele, Alessandro; Sardella, Roccaldo; Lindner, Wolfgang; Natalini, Benedetto

    2015-01-01

    Highlights: • The ZWIX(+) column allowed getting the Boc-Aph(Hor)-OH (1) isomeric peaks resolved. • ECD studies and molecular dynamic simulations allowed to assign the elution order. • Molecular descriptors revealed the active role of achiral elements of the CSP. - Abstract: A chiral chromatography method enabling the simultaneous diastereo- and enantioseparation of N α -Boc-N 4 -(hydroorotyl)-4-aminophenylalanine [Boc-Aph(Hor)-OH, 1] was optimized with a quinine-based zwitterionic stationary phase. The polar-ionic eluent system consisting of ACN:MeOH:water—49.7:49.7:0.6 (v/v/v) with formic acid (4.0 mM) and diethylamine (2.5 mM), allowed the successful separation of the four acid stereoisomers: α D,D-/D,L-1 = 1.08; α D,L-/L,D-1 = 1.08; α L,D-/L,L-1 = 1.40. According to the in-house developed synthetic procedure and the recorded electronic circular dichroism spectra, the following stereoisomeric elution order was readily established in the optimal chromatographic conditions: D,D-1 < D,L-1 < L,D-1 < L,L-1. With the aim of better understanding the molecular basis of the retention behaviour of the four stereoisomers in the employed chromatographic system and conditions, a computational protocol consisting in molecular dynamics simulations was applied. The use of the three descriptors INTER (in kcal mol −1 , encoding for the interaction energy between the selector SO unit and the whole system), INTER-SA (in kcal mol −1 , encoding for the interaction energy between SO and the sole selectand SA), and SELF (in kcal mol −1 , encoding for the conformational energy of SA relative to its minimum energy registered by the collected snapshots) revealed the active role of achiral sub-structural elements of the chiral stationary phase and eluent components in the overall stereorecognition mechanism

  5. Diastereo- and enantioseparation of a N(α)-Boc amino acid with a zwitterionic quinine-based stationary phase: focus on the stereorecognition mechanism.

    Science.gov (United States)

    Ianni, Federica; Carotti, Andrea; Marinozzi, Maura; Marcelli, Gloria; Di Michele, Alessandro; Sardella, Roccaldo; Lindner, Wolfgang; Natalini, Benedetto

    2015-07-23

    A chiral chromatography method enabling the simultaneous diastereo- and enantioseparation of N(α)-Boc-N(4)-(hydroorotyl)-4-aminophenylalanine [Boc-Aph(Hor)-OH, 1] was optimized with a quinine-based zwitterionic stationary phase. The polar-ionic eluent system consisting of ACN:MeOH:water-49.7:49.7:0.6 (v/v/v) with formic acid (4.0mM) and diethylamine (2.5mM), allowed the successful separation of the four acid stereoisomers: αd,d-/d,l-1=1.08; αd,l-/l,d-1=1.08; αl,d-/l,l-1=1.40. According to the in-house developed synthetic procedure and the recorded electronic circular dichroism spectra, the following stereoisomeric elution order was readily established in the optimal chromatographic conditions: d,d-1stationary phase and eluent components in the overall stereorecognition mechanism. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Paraffin/expanded graphite phase change composites with enhanced thermal conductivity prepared by implanted β-SiC nanowires with chemical vapor deposition method

    Science.gov (United States)

    Yin, Zhaoyu; Zhang, Xiaoguang; Huang, Zhaohui; Liu, Silin; Zhang, Weiyi; Liu, Yan'gai; Wu, Xiaowen; Fang, Minghao; Min, Xin

    2018-02-01

    Expanded graphite/β-SiC nanowires composites (ESNC) were prepared through chemical vapor deposition, and paraffin/expanded graphite/β-SiC nanowires composites (PESNC) were made through vacuum impregnation to overcome liquid leakage during phase transition and enhance the thermal conductivity of paraffin. Fourier transform infrared spectroscopy showed no chemical interactions between the paraffin and ESNC. Differential scanning calorimetry estimated the temperature and latent heat of PESNC during melting to 45.73 °C and 124.31 J g-1, respectively. The respective values of these quantities during freezing were recorded as 48.93 °C and 124.14 J g-1. The thermal conductivity of PESNC was estimated to 0.75 W mK-1, which was 3.26-folds that of pure paraffin (0.23 W mK-1). PESNC perfectly maintained its phase transition after 200 melting-freezing cycles. The resulting ideal thermal conductivity, good chemical stability, thermal properties and thermal reliability of PESNC are promising for use in energy efficient buildings and solar energy systems.

  7. Novas fases estacionárias à base de sílica para cromatografia líquida de alta eficiência New stationary phases based on silica for high performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    César R. Silva

    2004-04-01

    Full Text Available The present work reviews recent advances in the preparation of new reversed phase packing materials such as sterically protected, bidentate, hybrid organic-inorganic and monolithic phases and phases containing embedded polar groups. The bonding chemistry involved in the preparation of these phases as well as their advantages over conventional C8 and C18 reversed phases are discussed. Understanding the reasons behind the development of these newer column packings helps analysts select the best stationary phase for a given application.

  8. A 2H nuclear magnetic resonance study of the state of water in neat silica and zwitterionic stationary phases and its influence on the chromatographic retention characteristics in hydrophilic interaction high-performance liquid chromatography.

    Science.gov (United States)

    Wikberg, Erika; Sparrman, Tobias; Viklund, Camilla; Jonsson, Tobias; Irgum, Knut

    2011-09-23

    2H NMR has been used as a tool for probing the state of water in hydrophilic stationary phases for liquid chromatography at temperatures between -80 and +4 °C. The fraction of water that remained unfrozen in four different neat silicas with nominal pore sizes between 60 and 300 Å, and in silicas with polymeric sulfobetaine zwitterionic functionalities prepared in different ways, could be determined by measurements of the line widths and temperature-corrected integrals of the 2H signals. The phase transitions detected during thawing made it possible to estimate the amount of non-freezable water in each phase. A distinct difference was seen between the neat and modified silicas tested. For the neat silicas, the relationship between the freezing point depression and their pore size followed the expected Gibbs-Thomson relationship. The polymeric stationary phases were found to contain considerably higher amounts of non-freezable water compared to the neat silica, which is attributed to the structural effect that the sulfobetaine polymers have on the water layer close to the stationary phase surface. The sulfobetaine stationary phases were used alongside the 100 Å silica to separate a number of polar compounds in hydrophilic interaction (HILIC) mode, and the retention characteristics could be explained in terms of the surface water structure, as well as by the porous properties of the stationary phases. This provides solid evidence supporting a partitioning mechanism, or at least of the existence of an immobilized layer of water into which partitioning could be occurring. Copyright © 2011 Elsevier B.V. All rights reserved.

  9. Modeling, analysis, and design of stationary reference frame droop controlled parallel three-phase voltage source inverters

    DEFF Research Database (Denmark)

    Vasquez, Juan Carlos; Guerrero, Josep M.; Savaghebi, Mehdi

    2013-01-01

    Power electronics based MicroGrids consist of a number of voltage source inverters (VSIs) operating in parallel. In this paper, the modeling, control design, and stability analysis of parallel connected three-phase VSIs are derived. The proposed voltage and current inner control loops and the mat......Power electronics based MicroGrids consist of a number of voltage source inverters (VSIs) operating in parallel. In this paper, the modeling, control design, and stability analysis of parallel connected three-phase VSIs are derived. The proposed voltage and current inner control loops...... control restores the frequency and amplitude deviations produced by the primary control. Also, a synchronization algorithm is presented in order to connect the MicroGrid to the grid. Experimental results are provided to validate the performance and robustness of the parallel VSI system control...

  10. Evaluation of different hydrophilic stationary phases for the simultaneous determination of iminosugars and other low molecular weight carbohydrates in vegetable extracts by liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Rodríguez-Sánchez, S; Quintanilla-López, J E; Soria, A C; Sanz, M L

    2014-11-01

    Iminosugars are considered potential drug candidates for the treatment of several diseases, mainly as a result of their α-glycosidase inhibition properties. A method by hydrophilic interaction liquid chromatography tandem mass spectrometry has been optimized for the first time for the simultaneous determination of complex mixtures of bioactive iminosugars and other low molecular weight carbohydrates (LMWC) in vegetable extracts. Three hydrophilic stationary phases (sulfoalkylbetaine zwitterionic, polyhydroxyethyl aspartamide and ethylene bridge hybrid (BEH) with trifunctionally bonded amide) were compared under both basic and acidic conditions. The best sensitivity (limits of detection between 0.025 and 0.28ngmL -1 ) and overall chromatographic performance in terms of resolution, peak width and analysis time were obtained with the BEH amide column using 0.1% ammonium hydroxide as a mobile phase additive. The optimized method was applied to the analysis of extracts of hyacinth bulbs, buckwheat seeds and mulberry leaves. Iminosugar and other LMWC structures were tentatively assigned by their high resolution daughter ions mass spectra. Several iminosugars such as glycosyl-fagomine in mulberry extract were also described for the first time. Among the extracts analysed, mulberry showed the widest diversity of iminosugars, whereas the highest content of them was found in hyacinth bulb (2.5mgg -1 ) followed by mulberry (1.95 mgg -1 ). Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Design, preparation and application of a Pirkle-type chiral stationary phase for enantioseparation of some racemic organic acids and molecular dynamics studies

    Directory of Open Access Journals (Sweden)

    Reşit Çakmak

    2017-08-01

    Full Text Available This study consists of two parts. In the first part of the study; a Pirkle-type chiral stationary phase was prepared by synthesizing an aromatic amine derivative of (R-2-amino-1-butanol as a chiral selectorand binding to L- tyrosine -modified cyanogen bromide (CNBr-activated Sepharose 4B and then, packed into the separation column. T he chromatographic performance of the separation column was evaluated w ith racemic mandelic acid and 2-phenylpropionic acid by using phosphate buffers at three different pHs as mobile phase. In the resolution processes, t he prepared solutions were loaded onto the separation column at two different concentrations and at three different pHs for each racemic organic acid, separately. Enantiomeric excess (ee % of the eluates was determined on CHIRALPAK AD-H chiral analytical column by HPLC. The maximum ee% for mandelic acid and 2-phenylpropionic acid was determined to be 60.84 and 27.4, respectively. Separation factors (k 1 ’, k 2 ’, α, and Rs were calculated for each acid. The structures of the obtained compounds were characterized using the spectroscopic methods (NMR, and elemental analysis. In the second part of the study; enantioselective interactions between the prepared CSP and the analytes have been widely studied by docking, molecular dynamics simulation and quantum mechanical computation methods. The reason of column eluation of rac-2-phenylpropionic acid with lower enantiomeric yield was explained by these techniques.

  12. Experiment and simulation of a LiFePO4 battery pack with a passive thermal management system using composite phase change material and graphite sheets

    Science.gov (United States)

    Lin, Chunjing; Xu, Sichuan; Chang, Guofeng; Liu, Jinling

    2015-02-01

    A passive thermal management system (TMS) for LiFePO4 battery modules using phase change material (PCM) as the heat dissipation source to control battery temperature rise is developed. Expanded graphite matrix and graphite sheets are applied to compensate low thermal conductivity of PCM and improve temperature uniformity of the batteries. Constant current discharge and mixed charge-discharge duties were applied on battery modules with and without PCM on a battery thermal characteristics test platform. Experimental results show that PCM cooling significantly reduces the battery temperature rise during short-time intense use. It is also found that temperature uniformity across the module deteriorates with the increasing of both discharge time and current rates. The maximum temperature differences at the end of 1C and 2C-rate discharges are both less than 5 °C, indicating a good performance in battery thermal uniformity of the passive TMS. Experiments on warm-keeping performance show that the passive TMS can effectively keep the battery within its optimum operating temperature for a long time during cold weather uses. A three dimensional numerical model of the battery pack with the passive TMS was conducted using ANSYS Fluent. Temperature profiles with respect to discharging time reveal that simulation shows good agreement with experiment at 1C-discharge rate.

  13. Correlations between retention indices and molecular structure of their benzoyl derivatives on phenyl substituted polysiloxane stationary phases

    International Nuclear Information System (INIS)

    Pias, J.B.; Gasco, L.

    1976-01-01

    The retention indices of aliphaticalcohols of carbon number up to Csub(g), and of their benzoyl derivatives up to C 7 , were determined in columns packed with Chromosorb G (AW-DMCS-HP) coated previously with 5% methyl, and methyl phenyl polysiloxanes with increasing polarity (SE-30, OV-3, OV-7; OV-11, OV-17 and OV-25). Correlations between retention indices and chain length for 1-alcohols, 2-alcohols, 3-alcohols, 1, on -3-alcohols, 2-methyl-1-alcohols and for their corresponding benzoyl derivatives were calculated at 100, 120 and 140 0 C. In alcohols, a -CH 2 - group increases I approximately 100 units, and in their benzoyl derivatives from 80 to 100 units. Dispersion indices ΔI, and positional and structural increments of I were evaluated for -OH and benzoyl groups in terms for phase polarity and chain length. Effects of chain length, chain branching and double bond location on retention parameters were also studied. (author)

  14. Diastereo- and enantioseparation of a N{sup α}-Boc amino acid with a zwitterionic quinine-based stationary phase: Focus on the stereorecognition mechanism

    Energy Technology Data Exchange (ETDEWEB)

    Ianni, Federica; Carotti, Andrea; Marinozzi, Maura; Marcelli, Gloria [Department of Pharmaceutical Sciences, University of Perugia, Via Fabretti 48, 06123 Perugia (Italy); Di Michele, Alessandro [Department of Physics and Geology, University of Perugia, Via Pascoli 1, 06123 Perugia (Italy); Sardella, Roccaldo, E-mail: roccaldo.sardella@unipg.it [Department of Pharmaceutical Sciences, University of Perugia, Via Fabretti 48, 06123 Perugia (Italy); Lindner, Wolfgang [Department of Analytical Chemistry, University of Vienna, Währinger Strasse 38, 1090 Vienna (Austria); Natalini, Benedetto [Department of Pharmaceutical Sciences, University of Perugia, Via Fabretti 48, 06123 Perugia (Italy)

    2015-07-23

    Highlights: • The ZWIX(+) column allowed getting the Boc-Aph(Hor)-OH (1) isomeric peaks resolved. • ECD studies and molecular dynamic simulations allowed to assign the elution order. • Molecular descriptors revealed the active role of achiral elements of the CSP. - Abstract: A chiral chromatography method enabling the simultaneous diastereo- and enantioseparation of N{sup α}-Boc-N{sup 4}-(hydroorotyl)-4-aminophenylalanine [Boc-Aph(Hor)-OH, 1] was optimized with a quinine-based zwitterionic stationary phase. The polar-ionic eluent system consisting of ACN:MeOH:water—49.7:49.7:0.6 (v/v/v) with formic acid (4.0 mM) and diethylamine (2.5 mM), allowed the successful separation of the four acid stereoisomers: α{sub D,D-/D,L-1} = 1.08; α{sub D,L-/L,D-1} = 1.08; α{sub L,D-/L,L-1} = 1.40. According to the in-house developed synthetic procedure and the recorded electronic circular dichroism spectra, the following stereoisomeric elution order was readily established in the optimal chromatographic conditions: D,D-1 < D,L-1 < L,D-1 < L,L-1. With the aim of better understanding the molecular basis of the retention behaviour of the four stereoisomers in the employed chromatographic system and conditions, a computational protocol consisting in molecular dynamics simulations was applied. The use of the three descriptors INTER (in kcal mol{sup −1}, encoding for the interaction energy between the selector SO unit and the whole system), INTER-SA (in kcal mol{sup −1}, encoding for the interaction energy between SO and the sole selectand SA), and SELF (in kcal mol{sup −1}, encoding for the conformational energy of SA relative to its minimum energy registered by the collected snapshots) revealed the active role of achiral sub-structural elements of the chiral stationary phase and eluent components in the overall stereorecognition mechanism.

  15. Separation of biomolecules by micro-high-performance anion-exchange chromatography using a tentacle-like stationary phase.

    Science.gov (United States)

    Marlin, Nicola Dawn; Smith, Norman William

    2005-05-01

    A variety of biomolecules and their variants, which have previously been problematic to separate, have been analysed using a novel anion-exchange resin based on a non-porous polystyrene polymeric support with a hydrophilic coating and grafted tentacular quaternary ammonium functional groups. The hydrophilic coating results in minimal interaction between the support and the biomolecule, while the highly flexible tentacular-like anion-exchange groups increase the ionic interaction potential and act as an umbrella to hold the proteins away from the surface. Because of the removal of silanophilic interactions, minimisation of hydrophobic interactions, and the highly flexible nature of the tentacle-like ion exchangers, ionic interactions can therefore dominate the separation. As such this phase is highly suited to the separation of highly charged biomolecules and their variants. This polymeric strong anion-exchange (SAX) support was packed into a fused-silica capillary column and, using a salt concentration gradient, various recombinant proteins were analysed by micro-HPLC resulting in baseline resolution.

  16. Properties of form-stable paraffin/silicon dioxide/expanded graphite phase change composites prepared by sol–gel method

    International Nuclear Information System (INIS)

    Li, Min; Wu, Zhishen; Tan, Jinmiao

    2012-01-01

    Highlights: ► Paraffin/SiO 2 /EG composite PCM was prepared with sol–gel method. ► The thermal conductivity of SiO 2 /paraffin/EG is 94.7% higher than paraffin. ► The latent heat of paraffin/SiO 2 /EG composite is 104.4 J/g. -- Abstract: A form-stable paraffin/silicon dioxide (SiO 2 )/expanded graphite (EG) composite phase change material (PCM) was prepared by sol–gel method. Silica gel acts as the supporting material and EG is used to increase the thermal conductivity. The mass fractions of silicon oxide and graphite are 20.8% and 7.2%, respectively. The composite PCM was characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Fourier transformation infrared spectroscopy (FTIR) method. Thermal properties and thermal stability of the composite PCM were studied using differential scanning calorimetry (DSC). The result shows that paraffin was well dispersed in the network of silica gel and there is no chemical reaction between them. The phase change temperature of the paraffin/SiO 2 composite and the paraffin/SiO 2 /EG composite are 27.53 °C and 27.72 °C, respectively. The latent heat of the paraffin/SiO 2 composite and the paraffin/SiO 2 /EG composite are 112.8 J/g and 104.4 J/g, respectively. The thermal conductivity of the SiO 2 /paraffin composite and the SiO 2 /paraffin/EG composite are 28.2% and 94.7% higher than that of paraffin.

  17. Thermal and electrical conductivity enhancement of graphite nanoplatelets on form-stable polyethylene glycol/polymethyl methacrylate composite phase change materials

    International Nuclear Information System (INIS)

    Zhang, Lei; Zhu, Jiaoqun; Zhou, Weibing; Wang, Jun; Wang, Yan

    2012-01-01

    Graphite nanoplatelets (GnPs), obtained by sonicating the expanded graphite, were employed to simultaneously enhance the thermal (k) and electrical (σ) conductivity of organic form-stable phase change materials (FSPCMs). Using the method of in situ polymerization upon ultrasonic irradiation, GnPs serving as the conductive fillers and polyethylene glycol (PEG) acting as the phase change material (PCM) were uniformly dispersed and embedded inside the network structure of polymethyl methacrylate (PMMA), which contributed to the well package and self-supporting properties of composite FSPCMs. X-ray diffraction and Fourier transform infrared spectroscopy results indicated that the GnPs were physically combined with PEG/PMMA matrix and did not participate in the polymerization. The GnPs additives were able to effectively enhance the k and σ of organic FSPCM. When the mass ratio of GnP was 8%, the k and σ of FSPCM changed up to 9 times and 8 orders of magnitude over that of PEG/PMMA matrix, respectively. The improvements in both k and σ were mainly attributed to the well dispersion and large aspect ratio of GnPs, which were endowed with benefit of forming conducting network in polymer matrix. It was also confirmed that all the prepared specimens possessed available thermal storage density and thermal stability. -- Highlights: ► GnPs were employed to simultaneously enhance the k and σ of organic FSPCMs. ► PEG/PMMA/GnPs composite FSPCMs were prepared by in situ polymerization method. ► The composite FSPCMs exhibited well package and self-supporting properties. ► GnPs additives effectively enhanced the k and σ of composite FSPCMs. ► All the composites possessed available thermal storage density and thermal stability.

  18. Modeling and predicting chiral stationary phase enantioselectivity: An efficient random forest classifier using an optimally balanced training dataset and an aggregation strategy.

    Science.gov (United States)

    Piras, Patrick; Sheridan, Robert; Sherer, Edward C; Schafer, Wes; Welch, Christopher J; Roussel, Christian

    2018-03-01

    Predicting whether a chiral column will be effective is a daily task for many analysts. Moreover, finding the best chiral column for separating a particular racemic compound is mostly a matter of trial and error that may take up to a week in some cases. In this study we have developed a novel prediction approach based on combining a random forest classifier and an optimized discretization method for dealing with enantioselectivity as a continuous variable. Using the optimization results, models were trained on data sets divided into four enantioselectivity classes. The best model performances were achieved by over-sampling the minority classes (α ≤ 1.10 and α ≥ 2.00), down-sampling the majority class (1.2 ≤ α < 2.0), and aggregating multicategory predictions into binary classifications. We tested our method on 41 chiral stationary phases using layered fingerprints as descriptors. Experimental results show that this learning methodology was successful in terms of average area under the Receiver Operating Characteristic curve, Kappa indices and F-measure for structure-based prediction of the enantioselective behavior of 34 chiral columns. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Chiral recognition of N-phthaloyl, N-tetrachlorophthaloyl, and N-naphthaloyl α-amino acids and their esters on polysaccharide-derived chiral stationary phases.

    Science.gov (United States)

    Kim, Byoung-Hyoun; Lee, Sang Uck; Moon, Dong Cheul

    2012-12-01

    Enantiomeric separations of N-phthaloyl (N-PHT), N-tetrachlorophthaloyl (N-TCPHT), and N-naphthaloyl (N-NPHT) α-amino acids and their esters were examined on several kinds of polysaccharide-derived chiral stationary phases (CSPs). Resolution capability of CSPs was greater Chiralcel OF than the others for N-PHT and N-NPHT α-amino acids and their esters. In N-TCPHT α-amino acids and their esters, good enantioselectivities showed Chiralcel OG for N-TCPHT α-amino acids, Chiralpak AD for N-TCPHT α-amino acid methyl esters, and Chiralcel OD for N-TCPHT α-amino acid ethyl esters, respectively. From the results of liquid chromatography and computational chemistry, it is concluded that l-form is preferred and more retained with electrostatic interaction in case of interaction between N-PHT α-amino acid derivatives and Chiralcel OF, N-TCPHT α-amino acid derivatives and Chiralcel OD, and N-NPHT α-amino acid derivatives and Chiracel OF. On the other hand, d-form is preferred and more retained with van der Waals interaction in case of interaction between N-TCPHT α-amino acid ester derivatives and Chiralcel OG and Chiralpak AD. Copyright © 2012 Wiley Periodicals, Inc.

  20. Enantioseparation of α-Hydroxyallylphosphonates and Phosphonoallylic Carbonate Derivatives on Chiral Stationary Phases Using Sequential UV, Polarimetric, and Refractive Index Detection.

    Science.gov (United States)

    Hamper, Bruce C; Mannino, Michael P; Mueller, Melissa E; Harrison, Liam T; Spilling, Christopher D

    2016-09-01

    Chromatographic separation of the enantiomers of parent compounds dimethyl α-hydroxyallyl phosphonate and 1-(dimethoxyphosphoryl) allyl methyl carbonate was demonstrated by high-performance liquid chromatography (HPLC) using Chiralpak AS-H and ad-H chiral stationary phases (CSP), respectively, using a combination of UV, polarimetric, and refractive index detectors. A comparison was made of the separation efficiency and elution order of enantiomeric α-hydroxyallyl phosphonates and their carbonate derivatives on commercially available polysaccharide AS, ad, OD, IC-3, and Whelk-O 1 CSPs. In general, the α-hydroxyallyl phosphonates were resolved on the AS-H CSP, whereas the carbonate derivatives and were preferentially resolved on the ad-H CSP. The impact of aryl substitution on the resolution of analytes and was evaluated. Thermodynamic parameters determined for enantioselective adsorption hydroxyphosphonates and on the AS-H CSP and carbonate on the ad-H CSP demonstrated enthalpic control for separation of the enantiomers. Chirality 28:656-662, 2016. © 2016 Wiley Periodicals, Inc. © 2016 Wiley Periodicals, Inc.

  1. Sensitive immunoassay-based detection of Vibrio parahaemolyticus using capture and labeling particles in a stationary liquid phase lab-on-a-chip.

    Science.gov (United States)

    Park, Byunghee; Choi, Suk-Jung

    2017-04-15

    In the present study, a method was developed for detection of Vibrio parahaemolyticus based on a stationary liquid phase lab-on-a-chip (SLP LOC). The present SLP LOC comprises a sample chamber, washing chamber, and detection chamber connected by two channels. The method utilizes two types of particles: capture particles (CPs), which are magnetic nanoparticles functionalized with antibody; and labeling particles (LPs), which are silica nanoparticles functionalized with horseradish peroxidase and antibody. Samples were added to the sample chamber with CPs and LPs, forming a CP-bacteria-LP complex, and the complex was transported to the detection chamber containing chromogenic substrate solution. The method allowed the detection of V. parahaemolyticus in the range of 10 1 -10 5 cfu within 45min. Additionally, contamination of oyster samples with V. parahaemolyticus was detected within 2.5h, including 2h of culturing. The present method has the advantage of being highly rapid and facile, and enabling the detection of bacteria with high sensitivity. Moreover, the LOC and LOC processing device used in this method possess simple structures, making the detection process economical and allowing miniaturization. Therefore, the present SLP LOC detection method is potentially useful for in situ determination of food safety. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Retention and effective diffusion of model metabolites on porous graphitic carbon.

    Science.gov (United States)

    Lunn, Daniel B; Yun, Young J; Jorgenson, James W

    2017-12-29

    The study of metabolites in biological samples is of high interest for a wide range of biological and pharmaceutical applications. Reversed phase liquid chromatography is a common technique used for the separation of metabolites, but it provides little retention for polar metabolites. An alternative to C18 bonded phases, porous graphitic carbon has the ability to provide significant retention for both non-polar and polar analytes. The goal of this work is to study the retention and effective diffusion properties of porous graphitic carbon, to see if it is suitable for the wide injection bands and long run times associated with long, packed capillary-scale separations. The retention of a set of standard metabolites was studied for both stationary phases over a wide range of mobile phase conditions. This data showed that porous graphitic carbon benefits from significantly increased retention (often >100 fold) under initial gradient conditions for these metabolites, suggesting much improved ability to focus a wide injection band at the column inlet. The effective diffusion properties of these columns were studied using peak-parking experiments with the standard metabolites under a wide range of retention conditions. Under the high retention conditions, which can be associated with retention after injection loading for gradient separations, D eff /D m ∼0.1 for both the C18-bonded and porous graphitic carbon columns. As C18 bonded particles are widely, and successfully utilized for long gradient separations without issue of increasing peak width from longitudinal diffusion, this suggests that porous graphitic carbon should be amenable for long runtime gradient separations as well. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Synthesis and evaluation of a maltose-bonded silica gel stationary phase for hydrophilic interaction chromatography and its application in Ginkgo Biloba extract separation in two-dimensional systems.

    Science.gov (United States)

    Sheng, Qianying; Yang, Kaiya; Ke, Yanxiong; Liang, Xinmiao; Lan, Minbo

    2016-09-01

    Maltose covalently bonded to silica was prepared by using carbonyl diimidazole as a cross-linker and employed as a stationary phase for hydrophilic interaction liquid chromatography. The column efficiency and the effect of water content, buffer concentration, and pH value influenced on retention were investigated. The separation or enrichment selectivity was also studied with nucleosides, saccharides, amino acids, peptides, and glycopeptides. The results indicated that the stationary phase processed good separation efficiency and separation selectivity in hydrophilic interaction liquid chromatography mode. Moreover, a two-dimensional hydrophilic interaction liquid chromatography× reversed-phase liquid chromatography method with high orthogonality was developed to analyze the Ginkgo Biloba extract fractions. The development of this two-dimensional chromatographic system would be an effective tool for the separation of complex samples of different polarities and contents. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Enantioseparation of 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate tagged amino acids and other zwitterionic compounds on cinchona-based chiral stationary phases.

    Science.gov (United States)

    Hellinger, Roland; Horak, Jeannie; Lindner, Wolfgang

    2013-10-01

    The fluorescent tag 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC; AccQ Fluor reagent kit from Waters) is a commercial N-terminal label for proteinogenic amino acids (AAs), designed for reversed-phase separation and quantification of the AA racemates. The applicability of AQC-tagged AAs and AA-type zwitterionic compounds was tested for enantiomer separation on the tert-butyl carbamate modified quinine and quinidine based chiral stationary phases, QN-AX and QD-AX employing polar-organic elution conditions. The investigated test analytes included the enantiomers of the positional isomers of isoleucine (Ile), threonine, homoserine, and 4-hydroxyproline. Furthermore, β-AAs, cyclic, and heterocyclic AAs including trans-2-amino-cyclohexane carboxylic acid and trans-2-aminocyclohexyl sulfonic acid, phenylalanine derivatives substituted with halides with increasing electronegativity and 3,4-dihydroxyphenylalanine, cysteine-related derivatives including homocysteic acid, methionine sulfone, cysteine-S-acetic acid, and cysteine-S-acetamide as well as a small range of aminophosphonic acids were enantioseparated. A mechanistic interaction study of AQC-AAs in comparison with fluoresceine isothiocyanate-labeled AAs was performed. The chiral and chemoselective recognition processes involved in enantiomer separation and retention was systematically discussed. Special emphasis was set on the influential factors exhibited by the chemistry, branching position, and spatial properties of the investigated zwitterionic analytes. The general interest to separate and distinguish between different types of branched-chained AAs and metabolic side products thereof lies in the toxicity of some of these compounds, which makes for instance allo-Ile an attractive candidate in disease-related biomarker research.

  5. C₁₈-bound porous silica monolith particles as a low-cost high-performance liquid chromatography stationary phase with an excellent chromatographic performance.

    Science.gov (United States)

    Ali, Faiz; Cheong, Won Jo

    2014-12-01

    Ground porous silica monolith particles with an average particle size of 2.34 μm and large pores (363 Å) exhibiting excellent chromatographic performance have been synthesized on a relatively large scale by a sophisticated sol-gel procedure. The particle size distribution was rather broad, and the d(0.1)/d(0.9) ratio was 0.14. The resultant silica monolith particles were chemically modified with chlorodimethyloctadecylsilane and end-capped with a mixture of hexamethyldisilazane and chlorotrimethylsilane. Very good separation efficiency (185,000/m) and chromatographic resolution were achieved when the C18 -bound phase was evaluated for a test mixture of five benzene derivatives after packing in a stainless-steel column (1.0 mm × 150 mm). The optimized elution conditions were found to be 70:30 v/v acetonitrile/water with 0.1% trifluoroacetic acid at a flow rate of 25 μL/min. The column was also evaluated for fast analysis at a flow rate of 100 μL/min, and all the five analytes were eluted within 3.5 min with reasonable efficiency (ca. 60,000/m) and resolution. The strategy of using particles with reduced particle size and large pores (363 Å) combined with C18 modification in addition to partial-monolithic architecture has resulted in a useful stationary phase (C18 -bound silica monolith particles) of low production cost showing excellent chromatographic performance. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Comparison of high-accuracy numerical simulations of black-hole binaries with stationary-phase post-Newtonian template waveforms for initial and advanced LIGO

    International Nuclear Information System (INIS)

    Boyle, Michael; Brown, Duncan A; Pekowsky, Larne

    2009-01-01

    We study the effectiveness of stationary-phase approximated post-Newtonian waveforms currently used by ground-based gravitational-wave detectors to search for the coalescence of binary black holes by comparing them to an accurate waveform obtained from numerical simulation of an equal-mass non-spinning binary black hole inspiral, merger and ringdown. We perform this study for the initial- and advanced-LIGO detectors. We find that overlaps between the templates and signal can be improved by integrating the match filter to higher frequencies than used currently. We propose simple analytic frequency cutoffs for both initial and advanced LIGO, which achieve nearly optimal matches, and can easily be extended to unequal-mass, spinning systems. We also find that templates that include terms in the phase evolution up to 3.5 post-Newtonian (pN) order are nearly always better, and rarely significantly worse, than 2.0 pN templates currently in use. For initial LIGO we recommend a strategy using templates that include a recently introduced pseudo-4.0 pN term in the low-mass (M ≤ 35 M o-dot ) region, and 3.5 pN templates allowing unphysical values of the symmetric reduced mass η above this. This strategy always achieves overlaps within 0.3% of the optimum, for the data used here. For advanced LIGO we recommend a strategy using 3.5 pN templates up to M = 12 M o-dot , 2.0 pN templates up to M = 21 M o-dot , pseudo-4.0 pN templates up to 65 M o-dot , and 3.5 pN templates with unphysical η for higher masses. This strategy always achieves overlaps within 0.7% of the optimum for advanced LIGO.

  7. Microstructural Characterization of Next Generation Nuclear Graphites

    Energy Technology Data Exchange (ETDEWEB)

    Karthik Chinnathambi; Joshua Kane; Darryl P. Butt; William E. Windes; Rick Ubic

    2012-04-01

    This article reports the microstructural characteristics of various petroleum and pitch based nuclear graphites (IG-110, NBG-18, and PCEA) that are of interest to the next generation nuclear plant program. Bright-field transmission electron microscopy imaging was used to identify and understand the different features constituting the microstructure of nuclear graphite such as the filler particles, microcracks, binder phase, rosette-shaped quinoline insoluble (QI) particles, chaotic structures, and turbostratic graphite phase. The dimensions of microcracks were found to vary from a few nanometers to tens of microns. Furthermore, the microcracks were found to be filled with amorphous carbon of unknown origin. The pitch coke based graphite (NBG-18) was found to contain higher concentration of binder phase constituting QI particles as well as chaotic structures. The turbostratic graphite, present in all of the grades, was identified through their elliptical diffraction patterns. The difference in the microstructure has been analyzed in view of their processing conditions.

  8. Preparation and properties of palmitic-stearic acid eutectic mixture/expanded graphite composite as phase change material for energy storage

    International Nuclear Information System (INIS)

    Zhang, Nan; Yuan, Yanping; Du, Yanxia; Cao, Xiaoling; Yuan, Yaguang

    2014-01-01

    A novel composite PCM (phase change material) with PA-SA (palmitic-stearic acid) eutectic mixture as PCM and EG (expanded graphite) as supporting material was prepared. The optimum absorption ratio of PA-SA/EG (Palmitic-stearic acid/expanded graphite) composite PCM was determined as PA-SA:EG = 13:1 (by mass). Scanning electron microscope and Fourier transformation infrared spectroscopy results show that PA-SA was uniformly distributed in the porous network structure of EG due to the physical action. Thermal property and thermal stability of the PA-SA/EG composite PCM were characterized by DSC (differential scanning calorimetry) and TGA (thermogravimetric analysis). DSC results indicated that the melting and freezing temperatures and latent heats of PA-SA/EG were measured as 53.89 °C and 54.37 °C, and 166.27 J/g and 166.13 J/g. TGA test results revealed that PA-SA/EG had a good thermal stability in working temperature range. Thermal cycling test results showed PA-SA/EG had a good thermal reliability after 720 thermal cycles. Thermal conductivity of the composite PCM was measured as 2.51 W/m K, much higher than that of PA-SA. The thermal energy storage and release rates of PA-SA/EG were also increased due to the high thermal conductivity of EG. In conclusion, the prepared PA-SA/EG composite PCM can be acted as a potential material for thermal energy storage due to the acceptable thermal properties, good thermal reliability and stability, high thermal conductivity. - Highlights: • PA-SA/EG (Palmitic-stearic acid/expanded graphite) composite PCM was prepared. • Optimum absorption ratio of PA-SA in EG was obtained as 13:1 (by mass). • Thermal conductivity and performance of PA-SA/EG have been significate improved. • PA-SA/EG has a good thermal reliability and thermal stability

  9. [[Chiral separation of five arylpropionic acid drugs and determination of their enantiomers in pharmaceutical preparations by reversed-phase high performance liquid chromatography with cellulose-tris-(4-methylbenzoate) stationary phase

    Science.gov (United States)

    Luo, An; Wan, Qiang; Fan, Huajun; Chen, Zhi; Wu, Xuehao; Huang, Xiaowen; Zang, Linquan

    2014-09-01

    Chromatographic behaviors for enantiomeric separation of arylpropionic acid drugs were systematically developed by reversed phase-high performance liquid chromatography (RP-HPLC) using cellulose-tris-(4-methylbenzoate) (CTMB) as chiral stationary phase (CSP). The effects of the composition of the mobile phase, additives and temperature on chiral separation of flurbiprofen, pranoprofen, naproxen, ibuprofen and loxoprofen were further investigated. The enantiomers had been successfully separated on CSP of CTMB by the mobile phase of methanol-0.1% (v/v) formic acid except naproxen by acetonitrile-0.1% (v/v) formic acid at 25 °C. The mechanisms of the racemic resolution for the above mentioned five drugs are discussed thermodynamically and structurally. The resolutions between respective enantiomers for arylpropionic acid drugs on CTMB had significant differences due to their chromatographic behaviors. The order of resolutions ranked pranoprofen, loxoprofen, flurbiprofen, ibuprofen and naproxen. The method established has been successfully applied to the determination of the enantiomers of the five drugs in commercial preparations under the optimized conditions. It proved that the method is simple, reliable and accurate.

  10. Wide-range high-resolution transmission electron microscopy reveals morphological and distributional changes of endomembrane compartments during log to stationary transition of growth phase in tobacco BY-2 cells.

    Science.gov (United States)

    Toyooka, Kiminori; Sato, Mayuko; Kutsuna, Natsumaro; Higaki, Takumi; Sawaki, Fumie; Wakazaki, Mayumi; Goto, Yumi; Hasezawa, Seiichiro; Nagata, Noriko; Matsuoka, Ken

    2014-09-01

    Rapid growth of plant cells by cell division and expansion requires an endomembrane trafficking system. The endomembrane compartments, such as the Golgi stacks, endosome and vesicles, are important in the synthesis and trafficking of cell wall materials during cell elongation. However, changes in the morphology, distribution and number of these compartments during the different stages of cell proliferation and differentiation have not yet been clarified. In this study, we examined these changes at the ultrastructural level in tobacco Bright yellow 2 (BY-2) cells during the log and stationary phases of growth. We analyzed images of the BY-2 cells prepared by the high-pressure freezing/freeze substitution technique with the aid of an auto-acquisition transmission electron microscope system. We quantified the distribution of secretory and endosomal compartments in longitudinal sections of whole cells by using wide-range gigapixel-class images obtained by merging thousands of transmission electron micrographs. During the log phase, all Golgi stacks were composed of several thick cisternae. Approximately 20 vesicle clusters (VCs), including the trans-Golgi network and secretory vesicle cluster, were observed throughout the cell. In the stationary-phase cells, Golgi stacks were thin with small cisternae, and only a few VCs were observed. Nearly the same number of multivesicular body and small high-density vesicles were observed in both the stationary and log phases. Results from electron microscopy and live fluorescence imaging indicate that the morphology and distribution of secretory-related compartments dramatically change when cells transition from log to stationary phases of growth. © The Author 2014. Published by Oxford University Press on behalf of Japanese Society of Plant Physiologists. All rights reserved. For permissions, please email: journals.permissions@oup.com.

  11. Temperature dependences of the retention indices of mono- and polyethylene glycol acetals and ethers on stationary phase DB-1 and enthalpies of their sorption from the gas phase

    Science.gov (United States)

    Zhabina, A. A.; Krasnykh, E. L.

    2017-12-01

    Gas chromatography is used to study the sorption characteristics and retention of a series of mono-, di-, and triethylene glycol ethers on nonpolar phase DB-1 in the temperature range of 70-180°C. Temperature dependences of the retention indices of the compounds are obtained and their linear character in the investigated range of temperatures is demonstrated. The enthalpies of sorption of the investigated compounds are calculated and analyzed, based on the temperature dependences of the retention factors.

  12. TLC-MS versus TLC-LC-MS fingerprints of herbal extracts. Part III. Application of the reversed-phase liquid chromatography systems with C18 stationary phase.

    Science.gov (United States)

    Sajewicz, Mieczysław; Staszek, Dorota; Natic, Maja; Waksmundzka-Hajnos, Monika; Kowalska, Teresa

    2011-08-01

    In the previous paper from this series, we proposed mass spectrometric fingerprinting of complex botanical samples upon the examples of the pharmacologically important phenolic acids and flavonoids selectively extracted from Salvia lavandulifolia. In this study, we explore fingerprinting efficiency with a novel two-dimensional analytical system composed of the reversed-phase thin-layer chromatography and the reversed-phase high performance liquid chromatography with mass spectrometric detection (2D RP-TLC-RP-LC-MS). We also compare its efficiency with that of the one-dimensional analytical system (the reversed-phase thin-layer chromatography with mass spectrometric detection; 1D RP-TLC-MS). As our present study is basically focused on the method development, we considered it as justified to carry out our comparison with the phenolic acid extracts selectively derived from the Salvia lavandulifolia species, similar as it was done in Part II from this series. Upon the results obtained, it was established that the 1D RP-TLC-MS mode and the 2D RP-TLC-RP-LC-MS mode can be applied to fingerprinting of herbal extracts, and that the 2D RP-TLC-RP-LC mode can provide a more abundant information than that originating from the 1D RP-TLC mode.

  13. Gene encoding gamma-carbonic anhydrase is cotranscribed with argC and induced in response to stationary phase and high CO2 in Azospirillum brasilense Sp7.

    Science.gov (United States)

    Kaur, Simarjot; Mishra, Mukti N; Tripathi, Anil K

    2010-07-04

    Carbonic anhydrase (CA) is a ubiquitous enzyme catalyzing the reversible hydration of CO2 to bicarbonate, a reaction underlying diverse biochemical and physiological processes. Gamma class carbonic anhydrases (gamma-CAs) are widespread in prokaryotes but their physiological roles remain elusive. At present, only gamma-CA of Methanosarcina thermophila (Cam) has been shown to have CA activity. Genome analysis of a rhizobacterium Azospirillum brasilense, revealed occurrence of ORFs encoding one beta-CA and two gamma-CAs. One of the putative gamma-CA encoding genes of A. brasilense was cloned and overexpressed in E. coli. Electrometric assays for CA activity of the whole cell extracts overexpressing recombinant GCA1 did not show CO2 hydration activity. Reverse transcription-PCR analysis indicated that gca1 in A. brasilense is co-transcribed with its upstream gene annotated as argC, which encodes a putative N-acetyl-gamma-glutamate-phosphate reductase. 5'-RACE also demonstrated that there was no transcription start site between argC and gca1, and the transcription start site located upstream of argC transcribed both the genes (argC-gca1). Using transcriptional fusions of argC-gca1 upstream region with promoterless lacZ, we further demonstrated that gca1 upstream region did not have any promoter and its transcription occurred from a promoter located in the argC upstream region. The transcription of argC-gca1 operon was upregulated in stationary phase and at elevated CO2 atmosphere. This study shows lack of CO2 hydration activity in a recombinant protein expressed from a gene predicted to encode a gamma-carbonic anhydrase in A. brasilense although it cross reacts with anti-Cam antibody raised against a well characterized gamma-CA. The organization and regulation of this gene along with the putative argC gene suggests its involvement in arginine biosynthetic pathway instead of the predicted CO2 hydration.

  14. Synthesis of Optically Active Poly(diphenylacetylenes Using Polymer Reactions and an Evaluation of Their Chiral Recognition Abilities as Chiral Stationary Phases for HPLC

    Directory of Open Access Journals (Sweden)

    Katsuhiro Maeda

    2016-11-01

    Full Text Available A series of optically active poly(diphenylacetylene derivatives bearing a chiral substituent (poly-2S or chiral and achiral substituents (poly-(2Sx-co-31−x on all of their pendant phenyl rings were synthesized by the reaction of poly(bis(4-carboxyphenylacetylene with (S-1-phenylethylamine ((S-2 or benzylamine (3 in the presence of a condensing reagent. Their chiroptical properties and chiral recognition abilities as chiral stationary phases (CSPs for high-performance liquid chromatography (HPLC were investigated. Poly-2S and poly-(2Sx-co-31−x (0.06 < x < 0.71 formed a preferred-handed helical conformation with opposite helical senses after thermal annealing despite possessing the same chiral pendant (h-poly-2S and h-poly-(2Sx-co-31−x. Furthermore, h-poly-2S and h-poly-(2S0.36-co-30.64 emitted circularly polarized luminescence with opposite signs. h-Poly-2S showed higher chiral recognition abilities toward a larger number of racemates than poly-2S without a preferred-handed helicity and the previously reported preferred-handed poly(diphenylacetylene derivative bearing the same chiral substituent on half of its pendant phenyl rings. h-Poly-(2S0.36-co-30.64 also exhibited good chiral recognition abilities toward several racemates, though the elution order of some enantiomers was reversed compared with h-poly-2S.

  15. PlcRa, a new quorum-sensing regulator from Bacillus cereus, plays a role in oxidative stress responses and cysteine metabolism in stationary phase.

    Science.gov (United States)

    Huillet, Eugénie; Tempelaars, Marcel H; André-Leroux, Gwenaëlle; Wanapaisan, Pagakrong; Bridoux, Ludovic; Makhzami, Samira; Panbangred, Watanalai; Martin-Verstraete, Isabelle; Abee, Tjakko; Lereclus, Didier

    2012-01-01

    We characterized a new quorum-sensing regulator, PlcRa, which is present in various members of the B. cereus group and identified a signaling heptapeptide for PlcRa activity: PapRa(7). We demonstrated that PlcRa is a 3D structural paralog of PlcR using sequence analysis and homology modeling. A comparison of the transcriptomes at the onset of stationary phase of a ΔplcRa mutant and the wild-type B. cereus ATCC 14579 strain showed that 68 genes were upregulated and 49 genes were downregulated in the ΔplcRa mutant strain (>3-fold change). Genes involved in the cysteine metabolism (putative CymR regulon) were downregulated in the ΔplcRa mutant strain. We focused on the gene with the largest difference in expression level between the two conditions, which encoded -AbrB2- a new regulator of the AbrB family. We demonstrated that purified PlcRa bound specifically to the abrB2 promoter in the presence of synthetic PapRa(7), in an electrophoretic mobility shift assay. We further showed that the AbrB2 regulator controlled the expression of the yrrT operon involved in methionine to cysteine conversion. We found that the ΔplcRa mutant strain was more sensitive to hydrogen peroxide- and disulfide-induced stresses than the wild type. When cystine was added to the culture of the ΔplcRa mutant, challenged with hydrogen peroxide, growth inhibition was abolished. In conclusion, we identified a new RNPP transcriptional regulator in B. cereus that activated the oxidative stress response and cysteine metabolism in transition state cells.

  16. PlcRa, a new quorum-sensing regulator from Bacillus cereus, plays a role in oxidative stress responses and cysteine metabolism in stationary phase.

    Directory of Open Access Journals (Sweden)

    Eugénie Huillet

    Full Text Available We characterized a new quorum-sensing regulator, PlcRa, which is present in various members of the B. cereus group and identified a signaling heptapeptide for PlcRa activity: PapRa(7. We demonstrated that PlcRa is a 3D structural paralog of PlcR using sequence analysis and homology modeling. A comparison of the transcriptomes at the onset of stationary phase of a ΔplcRa mutant and the wild-type B. cereus ATCC 14579 strain showed that 68 genes were upregulated and 49 genes were downregulated in the ΔplcRa mutant strain (>3-fold change. Genes involved in the cysteine metabolism (putative CymR regulon were downregulated in the ΔplcRa mutant strain. We focused on the gene with the largest difference in expression level between the two conditions, which encoded -AbrB2- a new regulator of the AbrB family. We demonstrated that purified PlcRa bound specifically to the abrB2 promoter in the presence of synthetic PapRa(7, in an electrophoretic mobility shift assay. We further showed that the AbrB2 regulator controlled the expression of the yrrT operon involved in methionine to cysteine conversion. We found that the ΔplcRa mutant strain was more sensitive to hydrogen peroxide- and disulfide-induced stresses than the wild type. When cystine was added to the culture of the ΔplcRa mutant, challenged with hydrogen peroxide, growth inhibition was abolished. In conclusion, we identified a new RNPP transcriptional regulator in B. cereus that activated the oxidative stress response and cysteine metabolism in transition state cells.

  17. Determination of pore size distributions in capillary-channeled polymer fiber stationary phases by inverse size-exclusion chromatography and implications for fast protein separations.

    Science.gov (United States)

    Wang, Zhengxin; Marcus, R Kenneth

    2014-07-18

    Capillary-channeled polymer (C-CP) fibers have been utilized as liquid chromatography stationary phases, primarily for biomacromolecule separations on the analytical and preparative scales. The collinear packing of the eight-channeled C-CP fibers provides for very efficient flow, allowing operation at high linear velocity (u>100mm s(-1)) and low backpressure (chromatography (iSEC) has been employed to determine the pore size distribution (PSD) within C-CP fibers. A diversity of test species (from metal ions to large proteins) was used as probes under non-retaining conditions to obtain a response curve reflecting the apparent partition coefficient (Kd) versus hydrodynamic radii (rm). A mean pore radius (rp) of 4.2nm with standard deviation (sp) of ±1.1nm was calculated by fitting the Kd versus rm data to model equations with a Gaussian pore size distribution, and a pore radius of 4.0±0.1nm was calculated based on a log-normal distribution. The derived mean pore radius is much smaller than traditional support materials, with the standard deviation showing a relatively uniform pore distribution. van Deemter plots were analyzed to provide practical confirmation of the structural implications. Large molecules (e.g., proteins) that are fully excluded from pores have no significant C-terms in the van Deemter plots whereas small molecules that can access the pore volumes display appreciable C-terms, as expected. Fitting of retention data to the Knox equation suggests that the columns operate with a characteristic particle diameter (dp) of ∼53μm. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. A chemometric approach to determine the phenolic compounds in different barley samples by two different stationary phases: a comparison between C18 and pentafluorophenyl core shell columns.

    Science.gov (United States)

    Gómez-Caravaca, Ana María; Verardo, Vito; Berardinelli, Annachiara; Marconi, Emanuele; Caboni, Maria Fiorenza

    2014-08-15

    Barley (Hordeum vulgare L.) is a cereal crop that has been cultivated since ancient times. However, its interest as nutritional food and as food ingredient is relatively new. Thus, in this study, the phenolic compounds of eighteen different varieties of barley (4 waxy and 14 non-waxy) grown under the same agronomic conditions in the same experimental field have been determined by HPLC-DAD-MS. Two new methodologies were developed using new generation superficially porous HPLC columns with different stationary phases: C18 and pentafluorophenyl (PFP). Twelve free phenolic compounds and eight bound phenolic compounds could be identified in barley samples in less than 22min. The study of different method parameters showed that C18 column was more suitable for the analysis of phenolic compounds of barley. Hierarchical cluster analysis (HCA) was conducted in order to assess the different ability of the two different core shell HPLC columns in the discrimination between "waxy" and "non-waxy" varieties, and only HCA of C18 column could separate waxy and non-waxy genotypes. Significant differences in the content of phenolic compounds between waxy and non-waxy samples were found, being waxy barley samples the ones which presented higher content of free and bound phenolic compounds. Once the best discriminant HPLC column was established, principal component analysis (PCA) was applied and it was able to discriminate between "waxy" and "non-waxy" varieties; however it discriminated the barley samples based only in free phenolic compounds. Because of that, partial least squares discriminant analysis (PLS-DA) and Artificial Neural Networks (ANN) were carried out. PLS-DA and ANN permitted the classification of waxy and non-waxy genotypes from both free and bound phenolic compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Group separation of transplutonium and rare earth elements by liquid chromatography with free stationary phase using 2,4,6-tris[ditolylphosphoryl] - 1,3,5 - triazine as extractant

    International Nuclear Information System (INIS)

    Chmutova, M.K.; Ivanova, L.A.; Bodrin, G.B.; Polikarpov, Yu.M.; Myasoedov, B.F.

    1994-01-01

    Methods of group separation of trace amounts of transplutonium elements (TPE) and weight amounts of rare earth elements (REE) in the systems on the basis of bifunctional neutral organophosphoric compounds by the method of liquid chromatography with a free stationary phase have been developed. When solution of 2,4,6 - tris[ditolylphosphoryl] - 1,3,5 - triazine in chloroform was used as stationary phase, REE were the first to be washed out by 0.5 mol/l NH 4 SCN-1 mol/l HCl solution, then TPE - by 0.025 mol/l of oxyethylidenediphosphonic acid in water. the fractions contained about 100% of one of the groups without impurity of the other. 7 refs.; 6 figs

  20. iTRAQ quantitative analysis of Francisella tularensis ssp. holarctica live vaccine strain and Francisella tularensis ssp. tularensis SCHU S4 response to different temperatures and stationary phases of growth.

    Science.gov (United States)

    Lenco, Juraj; Link, Marek; Tambor, Vojtech; Zaková, Jitka; Cerveny, Lukas; Stulik, And Jiri

    2009-05-01

    Proteomics has been shown to significantly contribute to the investigation of the pathogenicity of the extremely infectious bacteria Francisella tularensis. In this study, the authors employed iTRAQ quantitative proteomic analysis in order to monitor alterations in proteomes of F. tularensis ssp. holarctica live vaccine strain and F. tularensis ssp. tularensis SCHU S4 associated with the cultivation at different temperatures or in the stationary phase. Correlated production of the identified proteins studied by the exploratory statistical analysis revealed novel candidates for virulence factors that were regulated in a similar manner to the genes encoded in the Francisella Pathogenicity Island. Moreover, the assessment of the adaptation of live vaccine strain and SCHU S4 strain to the examined stimuli uncovered differences in their physiological responses to the stationary phase of growth.

  1. Differences in stationary-phase cells of a commercial Saccharomyces cerevisiae wine yeast grown in aerobic and microaerophilic batch cultures assessed by electric particle analysis, light diffraction and flow cytometry.

    Science.gov (United States)

    Portell, X; Ginovart, M; Carbó, R; Vives-Rego, J

    2011-01-01

    We applied electric particle analysis, light diffraction and flow cytometry to obtain information on the morphological changes during the stationary phase of Saccharomyces cerevisiae. The reported analyses of S. cerevisiae populations were obtained under two different conditions, aerobic and microaerophilic, at 27°C. The samples analysed were taken at between 20 and 50 h from the beginning of culture. To assist in the interpretation of the observed distributions a complexity index was used. The aerobically grown culture reached significantly greater cell density. Under these conditions, the cell density experienced a much lower reduction (3%) compared with the microaerophilic conditions (30%). Under aerobic conditions, the mean cell size determined by both electric particle analysis and light diffraction was lower and remained similar throughout the experiment. Under microaerophilic conditions, the mean cell size determined by electric particle analysis decreased slightly as the culture progressed through the stationary phase. Forward and side scatter distributions revealed two cell subpopulations under both growth conditions. However, in the aerobic growing culture the two subpopulations were more separated and hence easier to distinguish. The distributions obtained with the three experimental techniques were analysed using the complexity index. This analysis suggested that a complexity index is a good descriptor of the changes that take place in a yeast population in the stationary phase, and that it aids in the discussion and understanding of the implications of these distributions obtained by these experimental techniques.

  2. Advanced risk assessment of the effects of graphite fibers on electronic and electric equipment, phase 1. [simulating vulnerability to airports and communities from fibers released during aircraft fires

    Science.gov (United States)

    Pocinki, L. S.; Kaplan, L. D.; Cornell, M. E.; Greenstone, R.

    1979-01-01

    A model was developed to generate quantitative estimates of the risk associated with the release of graphite fibers during fires involving commercial aircraft constructed with graphite fiber composite materials. The model was used to estimate the risk associated with accidents at several U.S. airports. These results were then combined to provide an estimate of the total risk to the nation.

  3. Characterization of commercial expandable graphite fire retardants

    Energy Technology Data Exchange (ETDEWEB)

    Focke, Walter Wilhelm, E-mail: walter.focke@up.ac.za; Badenhorst, Heinrich; Mhike, Washington; Kruger, Hermanus Joachim; Lombaard, Dewan

    2014-05-01

    Highlights: • Expandable graphite is less well-ordered than its graphite bisulfate progenitor. • It includes graphite oxide as a randomly interstratified phase. • CO{sub 2}, CO and SO{sub 2} are released during thermal-driven exfoliation. - Abstract: Thermal analysis and other techniques were employed to characterize two expandable graphite samples. The expansion onset temperatures of the expandable graphite's were ca. 220 °C and 300 °C respectively. The key finding is that the commercial products are not just pure graphite intercalation compounds with sulfuric acid species intercalated as guest ions and molecules in between intact graphene layers. A more realistic model is proposed where graphite oxide-like layers are also randomly interstratified in the graphite flakes. These graphite oxide-like layers comprise highly oxidized graphene sheets which contain many different oxygen-containing functional groups. This model explains the high oxygen to sulfur atomic ratios found in both elemental analysis of the neat materials and in the gas generated during the main exfoliation event.

  4. Radiation behaviour of graphite for HTGR

    International Nuclear Information System (INIS)

    Shtrombakh, Ya.I.; Platonov, P.A.; Gurovich, B.A.; Alekseev, V.M.

    1996-01-01

    The paper presents the results of investigations of different graphite materials, among with the standard reactor graphite manufacturing by electrode technology and a number of advanced graphites of new generation. During the investigation of radiation stability of standard reactor graphite the basic mechanisms of radiation damage of its structure were studied. With the help of transmission electron microscopy deformations and cracking of filler and binder were detected in the vicinity of the boundaries, separating these two components. Cracking begins with crystallite splitting and ends in full fracture of boundary layers. Such process of degradation can be explained by disjoint deformations resulting from difference in growth rate of filler and binder crystallites, in its turn caused by considerable difference between their sizes. It has been concluded that radiation stability of graphite may be improved by creating such graphite materials, in which the difference in sizes of crystallites of different structure components would be the minimal possible. When developing production technology of isotropic graphite for high temperature reactors, some progress was made towards the solution of this problem. Despite considerable swelling at high temperature this type of graphite appeared to be substantially less susceptible to the degradation of the structure and to deterioration of physico-mechanical properties. In addition to graphites manufactured by tradition technology, the graphite was investigated, in which pyrocarbon precipitated from gas phase under 1000 deg. C was used as binder. Carbon precipitated in such a way was non-graphitized at high temperatures and therefore it demonstrated sharp shrinkage under irradiation at high temperature, and shrinkage rate correlated with pyrocarbon quota in graphite structure. (author). 5 refs, 18 figs, 1 tab

  5. Surfactant-coated graphitized multiwalled carbon nanotubes as the pseudostationary phase in electrokinetic chromatography for the analysis of phytochemical compounds in biological fluids.

    Science.gov (United States)

    Cao, Wan; Hu, Shuai-Shuai; Ying, Xue-Zhen; Ye, Li-Hong; Cao, Jun

    2015-04-01

    This report describes the use of surfactant-coated graphitized multiwalled carbon nanotubes (SC-GMWNTs) as a novel pseudostationary phase in CE with diode array detection for the determination of phenolic acids and tanshinones in herbal and urine samples. Several parameters influencing the separation were studied, such as the concentrations of SDS, GMWNTs, and isopropanol; choice of carbon nanotubes; sodium borate content; and buffer pH. The results revealed that the presence of SC-GMWNTs in buffer enhanced the separation efficiency for the target analytes relative to conventional micelles due to the strong interaction between the surface of the GMWNTs and the target compounds. Under the optimum conditions, the method showed good linearity, with correlation coefficients higher than 0.9950. LODs were in the range of 0.71-3.10 μg/mL. Furthermore, satisfactory separations were achieved with good recovery values in the range of 89.97 and 103.30% when 10 mM borate, 30 mM SDS, 10% isopropanol, and 6 μg/mL SC-GMWNTs were introduced into the buffer solution. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Modified carbon nanotubes as a sorbent for solid-phase extraction of gold, and its determination by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Moghaddam, Firouzeh Hassani; Behzadi, Mansoureh; Naghizadeh, Matin; Taher, Mohammad Ali

    2015-01-01

    A simple, sensitive and accurate method was developed for solid-phase extraction and preconcentration of trace levels of gold in various samples. It is based on the adsorption of gold on modified oxidized multi-walled carbon nanotubes prior to its determination by graphite furnace atomic absorption spectrometry. The type and volume of eluent solution, sample pH value, flow rates of sample and eluent, sorption capacity and breakthrough volume were optimized. Under these conditions, the method showed linearity in the range of 0.2–6.0 ng L −1 with coefficients of determination of >0.99 in the sample. The relative standard deviation for seven replicate determinations of gold (at a level of 0.6 ng L −1 ) is ±3.8 %, the detection limit is 31 pg L −1 (in the initial solution and at an S/N ratio of 3; for n = 8), and the enrichment factor is 200. The sorption capacity of the modified MWCNTs for gold(III) is 4.15 mg g −1 . The procedure was successfully applied to the determination of gold in (spiked) water samples, human hair, human urine and standard reference material with recoveries ranging from 97.0 to 104.2 %. (author)

  7. Determination of Tetracycline Antibiotic Residues in Honey and Milk by Miniaturized Solid Phase Extraction Using Chitosan-Modified Graphitized Multiwalled Carbon Nanotubes.

    Science.gov (United States)

    Xu, Jing-Jing; An, Mingrui; Yang, Rui; Tan, Zhijing; Hao, Jie; Cao, Jun; Peng, Li-Qing; Cao, Wan

    2016-03-30

    A rapid, simple, and strongly selective miniaturized solid phase extraction (SPE) technique, requiring only small amounts of sorbent (24 mg) and elution solvent (600 μL), coupled with ultrahigh-performance liquid chromatography and quadrupole time-of-flight mass spectrometry was developed for detecting tetracycline antibiotics. These analytes were extracted from honey and milk using chitosan-modified graphitized multiwalled carbon nanotubes (G-MWNTs) as the solid sorbent and acetonitrile/acetic acid (8:2, v/v) as the eluent in miniaturized SPE. Under the optimum experimental conditions, a satisfactory linearity (r(2) > 0.992) was obtained, and the limits of detection were in the range of 0.61-10.34 μg/kg for the analytes. The mean recoveries of the five tetracycline antibiotic residues in the real samples were between 81.5 and 101.4%. The results demonstrated that chitosan-modified G-MWNTs comprise a promising material for the enrichment of tetracycline antibiotics from complex food matrices.

  8. The influence of expanded graphite on thermal properties for paraffin/high density polyethylene/chlorinated paraffin/antimony trioxide as a flame retardant phase change material

    International Nuclear Information System (INIS)

    Zhang Ping; Song Lei; Lu Hongdian; Wang Jian; Hu Yuan

    2010-01-01

    The influences of expanded graphite (EG) on the thermal properties of chlorinated paraffin (CP) and antimony trioxide (AT) on phase change material which bases on paraffin/high density polyethylene (HDPE) are studied. Differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), thermogravimetric analysis-Fourier transform infrared spectrometry (TGA-FTIR), microscale combustion calorimeter (MCC) and cone calorimeter (CONE) were used to evaluate the influence of EG on paraffin/HDPE/CP/AT system. The DSC results indicated that the latent heat value of PCM could be increased when the mass fraction of HDPE was decreased in the PCM, and EG could confine the molecular heat movement of paraffin. EG could improve the thermal stability and increase the char residue at high temperature for paraffin/HDPE/CP/AT hybrid. The volatilized products formed on thermal degradation of paraffin/HDPE/CP/AT with EG showed the release of CO 2 gas was hastened and increased, and the amount of combustible gases were decreased by TGA-FTIR analysis. The MCC and CONE results presented that the flame retardant efficiency of CP/AT could be improved by adding EG in paraffin/HDPE/CP/AT system.

  9. Gene encoding γ-carbonic anhydrase is cotranscribed with argC and induced in response to stationary phase and high CO2 in Azospirillum brasilense Sp7

    Science.gov (United States)

    2010-01-01

    Background Carbonic anhydrase (CA) is a ubiquitous enzyme catalyzing the reversible hydration of CO2 to bicarbonate, a reaction underlying diverse biochemical and physiological processes. Gamma class carbonic anhydrases (γ-CAs) are widespread in prokaryotes but their physiological roles remain elusive. At present, only γ-CA of Methanosarcina thermophila (Cam) has been shown to have CA activity. Genome analysis of a rhizobacterium Azospirillum brasilense, revealed occurrence of ORFs encoding one β-CA and two γ-CAs. Results One of the putative γ-CA encoding genes of A. brasilense was cloned and overexpressed in E. coli. Electrometric assays for CA activity of the whole cell extracts overexpressing recombinant GCA1 did not show CO2 hydration activity. Reverse transcription-PCR analysis indicated that gca1 in A. brasilense is co-transcribed with its upstream gene annotated as argC, which encodes a putative N-acetyl-γ-glutamate-phosphate reductase. 5'-RACE also demonstrated that there was no transcription start site between argC and gca1, and the transcription start site located upstream of argC transcribed both the genes (argC-gca1). Using transcriptional fusions of argC-gca1 upstream region with promoterless lacZ, we further demonstrated that gca1 upstream region did not have any promoter and its transcription occurred from a promoter located in the argC upstream region. The transcription of argC-gca1 operon was upregulated in stationary phase and at elevated CO2 atmosphere. Conclusions This study shows lack of CO2 hydration activity in a recombinant protein expressed from a gene predicted to encode a γ-carbonic anhydrase in A. brasilense although it cross reacts with anti-Cam antibody raised against a well characterized γ-CA. The organization and regulation of this gene along with the putative argC gene suggests its involvement in arginine biosynthetic pathway instead of the predicted CO2 hydration. PMID:20598158

  10. Gene encoding γ-carbonic anhydrase is cotranscribed with argC and induced in response to stationary phase and high CO2 in Azospirillum brasilense Sp7

    Directory of Open Access Journals (Sweden)

    Mishra Mukti N

    2010-07-01

    Full Text Available Abstract Background Carbonic anhydrase (CA is a ubiquitous enzyme catalyzing the reversible hydration of CO2 to bicarbonate, a reaction underlying diverse biochemical and physiological processes. Gamma class carbonic anhydrases (γ-CAs are widespread in prokaryotes but their physiological roles remain elusive. At present, only γ-CA of Methanosarcina thermophila (Cam has been shown to have CA activity. Genome analysis of a rhizobacterium Azospirillum brasilense, revealed occurrence of ORFs encoding one β-CA and two γ-CAs. Results One of the putative γ-CA encoding genes of A. brasilense was cloned and overexpressed in E. coli. Electrometric assays for CA activity of the whole cell extracts overexpressing recombinant GCA1 did not show CO2 hydration activity. Reverse transcription-PCR analysis indicated that gca1 in A. brasilense is co-transcribed with its upstream gene annotated as argC, which encodes a putative N-acetyl-γ-glutamate-phosphate reductase. 5'-RACE also demonstrated that there was no transcription start site between argC and gca1, and the transcription start site located upstream of argC transcribed both the genes (argC-gca1. Using transcriptional fusions of argC-gca1 upstream region with promoterless lacZ, we further demonstrated that gca1 upstream region did not have any promoter and its transcription occurred from a promoter located in the argC upstream region. The transcription of argC-gca1 operon was upregulated in stationary phase and at elevated CO2 atmosphere. Conclusions This study shows lack of CO2 hydration activity in a recombinant protein expressed from a gene predicted to encode a γ-carbonic anhydrase in A. brasilense although it cross reacts with anti-Cam antibody raised against a well characterized γ-CA. The organization and regulation of this gene along with the putative argC gene suggests its involvement in arginine biosynthetic pathway instead of the predicted CO2 hydration.

  11. Graphite Formation in Cast Iron

    Science.gov (United States)

    Stefanescu, D. M.

    1985-01-01

    In the first phase of the project it was proven that by changing the ratio between the thermal gradient and the growth rate for commercial cast iron samples solidifying in a Bridgman type furnace, it is possible to produce all types of graphite structures, from flake to spheroidal, and all types of matrices, from ferritic to white at a certain given level of cerium. KC-135 flight experiments have shown that in a low-gravity environment, no flotation occurs even in spheroidal graphite cast irons with carbon equivalent as high as 5%, while extensive graphite flotation occurred in both flake and spheroidal graphite cast irons, in high carbon samples solidified in a high gravity environment. This opens the way for production of iron-carbon composite materials, with high carbon content (e.g., 10%) in a low gravity environment. By using KC-135 flights, the influence of some basic elements on the solidification of cast iron will be studied. The mechanism of flake to spheroidal graphite transition will be studied, by using quenching experiments at both low and one gravity for different G/R ratios.

  12. Simultaneous determination of clobutinol hydrochloride and doxylamine succinate from syrups by RP HPLC using a new stationary phase containing embedded urea polar groups

    Directory of Open Access Journals (Sweden)

    Paulo Cesar Pires Rosa

    2012-06-01

    Full Text Available A new, simple, fast, reproducible and sensitive reversed phase HPLC method, using a new stationary phase containing embedded urea polar groups, has been developed and validated for the simultaneous determination of clobutinol hydrochloride (CLO and doxylamine succinate (DOX in syrups. The determination was carried out on a C8 urea column (125 mm x 3.9 mm i.d., 5 µm particle size synthetized at the Liquid Chomatography Laboratory (LabCrom of the Chemistry Institute of Unicamp. The mobile phase consisted of a mixture of acetonitrile:methanol:phosphate buffer (pH 2.5 in the gradient mode. The diode array detector (DAD was operated at 230 nm for CLO and 262 nm for DOX. The method showed adequate precision, with relative standard deviations (RSD less than 1%. The presence of the excipients did not interfere in the results of the analysis. Accuracy was determined by adding standards of the drugs to a placebo and good recovery values were obtained. The analytical curves were linear (r² 0.9999 for CLO and 0.9998 for DOX over a wide concentration range (2.4-336 µg mL-1 for CLO and 2.3-63 µg mL-1 for DOX. The solutions were stable for at least 72 hours at room temperature. The criteria for validation using the ICH guidelines were fulfilled.Um novo método simples, fácil e reprodutível, de fase reversa para CLAE, usando uma fase estacionária contendo um grupo polar, uréia, embutido, foi desenvolvido e validado para determinação simultânea de cloridrato de clobutinol (CLO e succinato de doxilamina (DOX em xarope. A determinação foi realizada em uma coluna C8 uréia (125 mm x 3,9 mm d.i., 5 µm tamanho de partícula sintetizada em nosso laboratório (LabCrom. A fase móvel consistiu de mistura de acetonitrila:metanol:tampão fosfato pH 2,5, em eluição por gradiente. O detector por arranjos de diodo (DAD foi utilizado a 230 nm para CLO e a 262 nm para DOX. O método apresentou precisão adequada, com desvio padrão relativo menor que 1%. A

  13. Graphite Technology Development Plan

    Energy Technology Data Exchange (ETDEWEB)

    W. Windes; T. Burchell; M.Carroll

    2010-10-01

    The Next Generation Nuclear Plant (NGNP) will be a helium-cooled High Temperature Gas Reactor (HTGR) with a large graphite core. Graphite physically contains the fuel and comprises the majority of the core volume. Graphite has been used effectively as a structural and moderator material in both research and commercial high-temperature gas-cooled reactors. This development has resulted in graphite being established as a viable structural material for HTGRs. While the general characteristics necessary for producing nuclear grade graphite are understood, historical “nuclear” grades no longer exist. New grades must be fabricated, characterized, and irradiated to demonstrate that current grades of graphite exhibit acceptable non-irradiated and irradiated properties upon which the thermomechanical design of the structural graphite in NGNP is based. This Technology Development Plan outlines the research and development (R&D) activities and associated rationale necessary to qualify nuclear grade graphite for use within the NGNP reactor.

  14. Graphitic carbon nitrides modified hollow fiber solid phase microextraction for extraction and determination of uric acid in urine and serum coupled with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Sun, Ying-pei; Chen, Juan; Qi, Huan-yang; Shi, Yan-ping

    2015-11-01

    An elevated uric acid (UA) in urine or serum can affect renal function and blood pressure, which is an indicator of gout, cardiovascular and renal diseases, hypertension, etc. In this work, a new type of mixed matrix membrane (MMM), based on graphitic carbon nitrides (g-CNs) and hollow fiber (HF), was prepared and combined with solid phase microextraction (SPME) mode to determine UA in urine and serum followed by gas chromatography-mass spectrometry (GC/MS). The porous g-CNs were dispersed in ammonia, and then the exfoliated g-CNs nanosheets were held in the pores of HF by capillary forces and sonification. The prepared g-CNs modified HF (g-CNs-HF) was immersed in biofluid directly to extract UA with SPME mode and the solvent-free mode is convenient for further derivatization and analysis. To achieve the highest extraction efficiency (EF), main extraction and derivatization parameters, such as g-CNs-HF immobilizing time, sonification power and time of extraction, derivatization and desorption time, were optimized. Under the optimum extraction conditions, a favorable linearity of UA was obtained in the range 0.1-200μgmL(-1) with correlation coefficients higher than 0.9990, and the average recoveries at three spiked levels of UA in urine and serum ranged from 80.7% to 121.6%, from 84.7% to 101.1%, respectively. The obtained results demonstrated the developed g-CNs-HF-SPME is a simple, rapid, cost-effective, solvent-free method for the analysis of UA in biofluid. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Online coupling of hydrophilic interaction/strong cation exchange/reversed-phase liquid chromatography with porous graphitic carbon liquid chromatography for simultaneous proteomics and N-glycomics analysis.

    Science.gov (United States)

    Zhao, Yun; Law, Henry C H; Zhang, Zaijun; Lam, Herman C; Quan, Quan; Li, Guohui; Chu, Ivan K

    2015-10-09

    In this study we developed a fully automated three-dimensional (3D) liquid chromatography methodology-comprising hydrophilic interaction separation as the first dimension, strong cation exchange fractionation as the second dimension, and low-pH reversed-phase (RP) separation as the third dimension-in conjunction downstream with additional complementary porous graphitic carbon separation, to capture non-retained hydrophilic analytes, for both shotgun proteomics and N-glycomics analyses. The performance of the 3D system alone was benchmarked through the analysis of the total lysate of Saccharomyces cerevisiae, leading to improved hydrophilic peptide coverage, from which we identified 19% and 24% more proteins and peptides, respectively, relative to those identified from a two-dimensional hydrophilic interaction liquid chromatography and low-pH RP chromatography (HILIC-RP) system over the same mass spectrometric acquisition time; consequently, the 3D platform also provided enhanced proteome and protein coverage. When we applied the integrated technology to analyses of the total lysate of primary cerebellar granule neurons, we characterized a total of 2201 proteins and 16,937 unique peptides for this primary cell line, providing one of its most comprehensive datasets. Our new integrated technology also exhibited excellent performance in the first N-glycomics analysis of cynomolgus monkey plasma; we successfully identified 122 proposed N-glycans and 135 N-glycosylation sites from 122 N-glycoproteins, and confirmed the presence of 38 N-glycolylneuraminic acid-containing N-glycans, a rare occurrence in human plasma, through tandem mass spectrometry for the first time. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Facile and fast preparation of low-cost silica-supported graphitic carbon nitride for solid-phase extraction of fluoroquinolone drugs from environmental waters.

    Science.gov (United States)

    Speltini, Andrea; Maraschi, Federica; Govoni, Roberta; Milanese, Chiara; Profumo, Antonella; Malavasi, Lorenzo; Sturini, Michela

    2017-03-17

    The analytical application of silica-supported graphitic carbon nitride (g-C 3 N 4 @silica) for solid-phase extraction (SPE) of fluoroquinolone (FQ) pollutants from water is presented for the first time. g-C 3 N 4 @silica was easily and quickly prepared by one-pot thermal condensation of dicyandiamide and characterized by powder X-ray diffraction, thermogravimetric analysis, scanning electron microscopy, Fourier transform infrared spectroscopy and surface area measurements. The novel composite was applied as sorbent for SPE of FQs from water prior high-performance liquid chromatography with fluorescence detection. The extraction efficiency of g-C 3 N 4 was tested in tap and surface waters at actual concentrations (10-100ngL -1 ). Quantitative adsorption was achieved using 100mg sorbent (20wt% g-C 3 N 4 ) for pre-concentration of 50-500mL sample, at the native pH (∼7.5-8). Elution was performed with 25mM H 3 PO 4 aqueous solution-acetonitrile (80:20), obtaining recoveries in the range 70-114%, enrichment factors up to 500 and inter-day RSDs≤12%. The batch-to-batch reproducibility was assessed on three independently synthesized g-C 3 N 4 @silica preparations (RSD 6-12%). g-C 3 N 4 supported on silica microparticles proved to be of easy preparation, inexpensive, reusable for at least 4 extractions of raw surface waters, and suitable for determination in real matrices. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Radiation damage in graphite

    CERN Document Server

    Simmons, John Harry Walrond

    1965-01-01

    Nuclear Energy, Volume 102: Radiation Damage in Graphite provides a general account of the effects of irradiation on graphite. This book presents valuable work on the structure of the defects produced in graphite crystals by irradiation. Organized into eight chapters, this volume begins with an overview of the description of the methods of manufacturing graphite and of its physical properties. This text then presents details of the method of setting up a scale of irradiation dose. Other chapters consider the effect of irradiation at a given temperature on a physical property of graphite. This

  18. New potential humic acid stationary phase toward drug components: Development of a chemometric-assisted RP-HPLC method for the determination of paracetamol and caffeine in tablet formulations.

    Science.gov (United States)

    Topkafa, Mustafa; Ayyildiz, Hamide Filiz; Memon, Fakhar N; Kara, Huseyin

    2016-07-01

    A new humic acid based stationary phase has been used, for the first time, to achieve the separation and quantification of paracetamol and caffeine in pharmaceutical preparations under reversed-phase high-performance liquid chromatography conditions. Central composite design was applied as a powerful tool to optimize the most dominant parameters that influence the resolution of reversed-phase high-performance liquid chromatography, that is, mobile phase composition (acetonitrile percentage in water), flow rate, and column temperature. The optimum conditions were obtained as 21.69%, 1.5 mL/min, and 15°C, respectively, with the aid of a second-order quadratic model and desirability function. Under the optimum conditions, the peaks could be baseline separated within 10 min. For the developed reversed-phase high-performance liquid chromatography method, the linearity was investigated in the concentration ranges of 2-160 mg/mL (R(2) = 0.999) for paracetamol and 2-9.9 mg/mL (R(2) = 0.991) for caffeine. Mean recoveries for paracetamol and caffeine were 95.90 and 95.68%, respectively. The limits of detection and quantification were 4.1 × 10(-4) and 1.3 × 10(-3) mg/mL for paracetamol and 1.6 × 10(-4) and 5.0 × 10(-4) mg/mL for caffeine. The results showed that the new humic acid based stationary phase is very suitable for the separation of paracetamol and caffeine in pharmaceutical preparations and, thus it can be used effectively in the pharmaceutical industry. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Modeling Fission Product Sorption in Graphite Structures

    International Nuclear Information System (INIS)

    Szlufarska, Izabela; Morgan, Dane; Allen, Todd

    2013-01-01

    The goal of this project is to determine changes in adsorption and desorption of fission products to/from nuclear-grade graphite in response to a changing chemical environment. First, the project team will employ principle calculations and thermodynamic analysis to predict stability of fission products on graphite in the presence of structural defects commonly observed in very high-temperature reactor (VHTR) graphites. Desorption rates will be determined as a function of partial pressure of oxygen and iodine, relative humidity, and temperature. They will then carry out experimental characterization to determine the statistical distribution of structural features. This structural information will yield distributions of binding sites to be used as an input for a sorption model. Sorption isotherms calculated under this project will contribute to understanding of the physical bases of the source terms that are used in higher-level codes that model fission product transport and retention in graphite. The project will include the following tasks: Perform structural characterization of the VHTR graphite to determine crystallographic phases, defect structures and their distribution, volume fraction of coke, and amount of sp2 versus sp3 bonding. This information will be used as guidance for ab initio modeling and as input for sorptivity models; Perform ab initio calculations of binding energies to determine stability of fission products on the different sorption sites present in nuclear graphite microstructures. The project will use density functional theory (DFT) methods to calculate binding energies in vacuum and in oxidizing environments. The team will also calculate stability of iodine complexes with fission products on graphite sorption sites; Model graphite sorption isotherms to quantify concentration of fission products in graphite. The binding energies will be combined with a Langmuir isotherm statistical model to predict the sorbed concentration of fission products

  20. Modeling Fission Product Sorption in Graphite Structures

    Energy Technology Data Exchange (ETDEWEB)

    Szlufarska, Izabela [University of Wisconsin, Madison, WI (United States); Morgan, Dane [University of Wisconsin, Madison, WI (United States); Allen, Todd [University of Wisconsin, Madison, WI (United States)

    2013-04-08

    The goal of this project is to determine changes in adsorption and desorption of fission products to/from nuclear-grade graphite in response to a changing chemical environment. First, the project team will employ principle calculations and thermodynamic analysis to predict stability of fission products on graphite in the presence of structural defects commonly observed in very high- temperature reactor (VHTR) graphites. Desorption rates will be determined as a function of partial pressure of oxygen and iodine, relative humidity, and temperature. They will then carry out experimental characterization to determine the statistical distribution of structural features. This structural information will yield distributions of binding sites to be used as an input for a sorption model. Sorption isotherms calculated under this project will contribute to understanding of the physical bases of the source terms that are used in higher-level codes that model fission product transport and retention in graphite. The project will include the following tasks: Perform structural characterization of the VHTR graphite to determine crystallographic phases, defect structures and their distribution, volume fraction of coke, and amount of sp2 versus sp3 bonding. This information will be used as guidance for ab initio modeling and as input for sorptivity models; Perform ab initio calculations of binding energies to determine stability of fission products on the different sorption sites present in nuclear graphite microstructures. The project will use density functional theory (DFT) methods to calculate binding energies in vacuum and in oxidizing environments. The team will also calculate stability of iodine complexes with fission products on graphite sorption sites; Model graphite sorption isotherms to quantify concentration of fission products in graphite. The binding energies will be combined with a Langmuir isotherm statistical model to predict the sorbed concentration of fission

  1. Stationary nonlinear Airy beams

    International Nuclear Information System (INIS)

    Lotti, A.; Faccio, D.; Couairon, A.; Papazoglou, D. G.; Panagiotopoulos, P.; Tzortzakis, S.; Abdollahpour, D.

    2011-01-01

    We demonstrate the existence of an additional class of stationary accelerating Airy wave forms that exist in the presence of third-order (Kerr) nonlinearity and nonlinear losses. Numerical simulations and experiments, in agreement with the analytical model, highlight how these stationary solutions sustain the nonlinear evolution of Airy beams. The generic nature of the Airy solution allows extension of these results to other settings, and a variety of applications are suggested.

  2. Tentacle-type zwitterionic stationary phase prepared by surface-initiated graft polymerization of 3-[N,N-dimethyl-N-(methacryloyloxyethyl)-ammonium] propanesulfonate through peroxide groups tethered on porous silica.

    Science.gov (United States)

    Jiang, Wen; Irgum, Knut

    2002-09-15

    A novel stationary phase with tentacle-type zwitterionic interaction layer was synthesized by free radical graft polymerization of 3-[N,N-dimethyl-N-(methacryloyloxyethyl)ammonium]propanesulfonate (SPE) from the surface of Kromasil porous silica particles. The polymerization was initiated by thermal cleavage of tert-butylperoxy groups covalently attached to the particle surface, and the material therefore carries a tentacle-type polymeric interaction layer with 3-sulfopropylbetaine functional moieties. The composition of the surface graft was determined by elemental analysis, and the surface charge was measured using photon correlation spectroscopy. The measured zeta-potentials were close to 0 and nearly independent of pH, and the tentacle character of the interactive layers were evident from the lack of colloidal stability in the absence of salt (antipolyelectrolytic behavior) and a marked increase in column back-pressure when the concentration of perchloric acid or perchlorate salt was increased. The chromatographic properties were evaluated on columns packed with the functionalized material, and it was shown that this zwitterionic stationary phase could simultaneously and independently separate inorganic anions and cations using aqueous solutions of perchloric acid or perchlorate salts as eluents. The material was also capable of separating two acidic and three basic proteins in a single run, using gradient salt elution at constant pH.

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

    Science.gov (United States)

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

    2016-07-01

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

  4. Magnetic solid-phase extraction combined with graphite furnace atomic absorption spectrometry for speciation of Cr(III) and Cr(VI) in environmental waters.

    Science.gov (United States)

    Jiang, Hong-mei; Yang, Ting; Wang, Yan-hong; Lian, Hong-zhen; Hu, Xin

    2013-11-15

    A new approach of magnetic solid phase extraction (MSPE) coupled with graphite furnace atomic absorption spectrometry (GFAAS) has been developed for the speciation of Cr(III) and Cr(VI) using zincon-immobilized silica-coated magnetic Fe3O4 nanoparticles (Zincon-Si-MNPs) as the MSPE absorbent. Cr(III) was quantitatively reserved on the absorbent at pH 9.1 while total Cr was reserved at pH 6.5. The absorbed Cr species were eluted by using 2 mol/L HCl and detected by GFAAS. The concentration of Cr(VI) could be calculated by subtracting Cr(III) from total Cr. All the parameters affecting the separation and extraction efficiency of Cr species such as pH, extraction time, concentration and volume of eluent, sample volume and influence of co-existing ions were systematically examined and the optimized conditions were established accordingly. The detection limit (LOD) of the method was 0.016 and 0.011 ng mL(-1) for Cr(III) and Cr(VI), respectively, with the enrichment factor of 100 and 150. The precisions of this method (Relative standard deviation, RSD, n=7) for Cr(III) and Cr(VI) at 0.1 ng mL(-1) were 6.0% and 6.2%, respectively. In order to validate the proposed method, a certified reference material of environmental water was analyzed, and the result of Cr speciation was in good agreement with the certified value. This MSPE-GFAAS method has been successfully applied for the speciation of Cr(III) and Cr(VI) in lake and tap waters with the recoveries of 88-109% for the spiked samples. Moreover, the MSPE separation mechanism of Cr(III) and Cr(VI) based on their adsorption-desorption on Zincon-Si-MNPs has been explained through various spectroscopic characterization. © 2013 Elsevier B.V. All rights reserved.

  5. Theoretical analysis of the graphitization of a nanodiamond

    Energy Technology Data Exchange (ETDEWEB)

    Kwon, S Joon; Park, Jae-Gwan [Nano Science and Technology Division, Korea Institute of Science and Technology (KIST), PO Box 131, Cheongryang, Seoul, 130-650 (Korea, Republic of)

    2007-09-26

    We report on a theoretical analysis of the graphitization of a nanosize diamond (nanodiamond) in the metastable state. A nanodiamond annealed at a relatively lower temperature suffers morphological transition into a nanodiamond-graphite core-shell structure. Thermodynamic stability analysis of the nanodiamond showed that the phase diagram (relationship between the annealing temperature and radius) of the nanodiamond-graphite has three regimes: smaller nanodiamond, nanodiamond-graphite, and larger nanodiamond. These regimes of nanodiamond-graphite are due to an additional phase boundary from finding the maximum size of the nanodiamond which can be graphitized. In the theoretical analysis, the most probable and the maximum volume fractions of graphite in the nanodiamond were 0.76 and 0.84 respectively, which were independent of the annealing temperature and the initial radius of the nanodiamond. Therefore, the nanodiamond is not completely transformed into graphite by simple annealing at relatively lower process temperature and pressure. The highest graphitization probability decreased with increasing annealing temperature. Raman spectra for the F{sub 2g} vibration mode of nanodiamond were also calculated, and we found that the variation in properties of the spectral line was strongly dependent on the graphitization temperature and the initial size of the nanodiamond.

  6. Theoretical analysis of the graphitization of a nanodiamond

    International Nuclear Information System (INIS)

    Kwon, S Joon; Park, Jae-Gwan

    2007-01-01

    We report on a theoretical analysis of the graphitization of a nanosize diamond (nanodiamond) in the metastable state. A nanodiamond annealed at a relatively lower temperature suffers morphological transition into a nanodiamond-graphite core-shell structure. Thermodynamic stability analysis of the nanodiamond showed that the phase diagram (relationship between the annealing temperature and radius) of the nanodiamond-graphite has three regimes: smaller nanodiamond, nanodiamond-graphite, and larger nanodiamond. These regimes of nanodiamond-graphite are due to an additional phase boundary from finding the maximum size of the nanodiamond which can be graphitized. In the theoretical analysis, the most probable and the maximum volume fractions of graphite in the nanodiamond were 0.76 and 0.84 respectively, which were independent of the annealing temperature and the initial radius of the nanodiamond. Therefore, the nanodiamond is not completely transformed into graphite by simple annealing at relatively lower process temperature and pressure. The highest graphitization probability decreased with increasing annealing temperature. Raman spectra for the F 2g vibration mode of nanodiamond were also calculated, and we found that the variation in properties of the spectral line was strongly dependent on the graphitization temperature and the initial size of the nanodiamond

  7. Oxidation Resistant Graphite Studies

    Energy Technology Data Exchange (ETDEWEB)

    W. Windes; R. Smith

    2014-07-01

    The Very High Temperature Reactor (VHTR) Graphite Research and Development Program is investigating doped nuclear graphite grades exhibiting oxidation resistance. During a oxygen ingress accident the oxidation rates of the high temperature graphite core region would be extremely high resulting in significant structural damage to the core. Reducing the oxidation rate of the graphite core material would reduce the structural effects and keep the core integrity intact during any air-ingress accident. Oxidation testing of graphite doped with oxidation resistant material is being conducted to determine the extent of oxidation rate reduction. Nuclear grade graphite doped with varying levels of Boron-Carbide (B4C) was oxidized in air at nominal 740°C at 10/90% (air/He) and 100% air. The oxidation rates of the boronated and unboronated graphite grade were compared. With increasing boron-carbide content (up to 6 vol%) the oxidation rate was observed to have a 20 fold reduction from unboronated graphite. Visual inspection and uniformity of oxidation across the surface of the specimens were conducted. Future work to determine the remaining mechanical strength as well as graphite grades with SiC doped material are discussed.

  8. Stationary-State Mutagenesis in Escherichia coli

    Indian Academy of Sciences (India)

    Stationary-phase mutagenesis in nondividing E. coli cells exposed to a nonlethal stress was, a few years ago, claimed to be a likely case of a Lamarckian mechanism capable of producing exclusively useful mutations in a directed manner. After a heated debate over the last decade it now appears to involve a Darwinian ...

  9. Method for producing dustless graphite spheres from waste graphite fines

    Science.gov (United States)

    Pappano, Peter J [Oak Ridge, TN; Rogers, Michael R [Clinton, TN

    2012-05-08

    A method for producing graphite spheres from graphite fines by charging a quantity of spherical media into a rotatable cylindrical overcoater, charging a quantity of graphite fines into the overcoater thereby forming a first mixture of spherical media and graphite fines, rotating the overcoater at a speed such that the first mixture climbs the wall of the overcoater before rolling back down to the bottom thereby forming a second mixture of spherical media, graphite fines, and graphite spheres, removing the second mixture from the overcoater, sieving the second mixture to separate graphite spheres, charging the first mixture back into the overcoater, charging an additional quantity of graphite fines into the overcoater, adjusting processing parameters like overcoater dimensions, graphite fines charge, overcoater rotation speed, overcoater angle of rotation, and overcoater time of rotation, before repeating the steps until graphite fines are converted to graphite spheres.

  10. A graphite nanoeraser

    DEFF Research Database (Denmark)

    Liu, Ze; Bøggild, Peter; Yang, Jia-rui

    2011-01-01

    We present here a method for cleaning intermediate-size (up to 50 nm) contamination from highly oriented pyrolytic graphite and graphene. Electron-beam-induced deposition of carbonaceous material on graphene and graphite surfaces inside a scanning electron microscope, which is difficult to remove...

  11. Electrochemical treatment of graphite

    International Nuclear Information System (INIS)

    Podlovilin, V.I.; Egorov, I.M.; Zhernovoj, A.I.

    1983-01-01

    In the course of investigating various modes of electroche-- mical treatment (ECT) it has been found that graphite anode treatment begins under the ''glow mode''. A behaviour of some marks of graphite with the purpose of ECT technique development in different electrolytes has been tested. Electrolytes have been chosen of three types: highly alkaline (pH 13-14), neutral (pH-Z) and highly acidic (pH 1-2). For the first time parallel to mechanical electroerosion treatment ECT graphite and carbon graphite materials previously considered chemically neutral is proposed. ECT of carbon graphite materials has a number of advantages as compared with electroerrosion and mechanical ones this is treatment rate and purity (ronghness) of the surface. A sMall quantity of sludge (6-8%) under ECT is in highly alkali electrolytes

  12. Conformational variability of the stationary phase survival protein E from Xylella fastidiosa revealed by X-ray crystallography, small-angle X-ray scattering studies, and normal mode analysis.

    Science.gov (United States)

    Machado, Agnes Thiane Pereira; Fonseca, Emanuella Maria Barreto; Reis, Marcelo Augusto Dos; Saraiva, Antonio Marcos; Santos, Clelton Aparecido Dos; de Toledo, Marcelo Augusto Szymanski; Polikarpov, Igor; de Souza, Anete Pereira; Aparicio, Ricardo; Iulek, Jorge

    2017-10-01

    Xylella fastidiosa is a xylem-limited bacterium that infects a wide variety of plants. Stationary phase survival protein E is classified as a nucleotidase, which is expressed when bacterial cells are in the stationary growth phase and subjected to environmental stresses. Here, we report four refined X-ray structures of this protein from X. fastidiosa in four different crystal forms in the presence and/or absence of the substrate 3'-AMP. In all chains, the conserved loop verified in family members assumes a closed conformation in either condition. Therefore, the enzymatic mechanism for the target protein might be different of its homologs. Two crystal forms exhibit two monomers whereas the other two show four monomers in the asymmetric unit. While the biological unit has been characterized as a tetramer, differences of their sizes and symmetry are remarkable. Four conformers identified by Small-Angle X-ray Scattering (SAXS) in a ligand-free solution are related to the low frequency normal modes of the crystallographic structures associated with rigid body-like protomer arrangements responsible for the longitudinal and symmetric adjustments between tetramers. When the substrate is present in solution, only two conformers are selected. The most prominent conformer for each case is associated to a normal mode able to elongate the protein by moving apart two dimers. To our knowledge, this work was the first investigation based on the normal modes that analyzed the quaternary structure variability for an enzyme of the SurE family followed by crystallography and SAXS validation. The combined results raise new directions to study allosteric features of XfSurE protein. © 2017 Wiley Periodicals, Inc.

  13. Properties of graphite composites based on natural and synthetic graphite powders and a phenolic novolac binder

    Science.gov (United States)

    Magampa, P. P.; Manyala, N.; Focke, W. W.

    2013-05-01

    Model graphite composites, similar to those used in nuclear applications as encasement material in fuel pebbles, were prepared by uniaxial cold compression moulding. They contained natural flake graphite, synthetic graphite and 20 wt.% phenolic novolac resin binder. The materials were carbonised at 900 °C in a nitrogen atmosphere and then annealed at 1800 °C in helium atmosphere. The X-ray diffraction studies showed that the graphite in these composites had hexagonal crystal structure after annealing. Raman spectroscopy revealed the presence of the structurally disordered phase derived from the carbonised resin. Optical microscopy revealed a flake-like microstructure for composites containing mainly natural graphite and needle-coke like particles for composites containing mainly synthetic graphite. The composites featured anisotropic property behaviour as the particles were partially aligned in a direction perpendicular to the compression direction. Thermogravimetric analysis studies showed that the annealed graphite composites were stable in air to 650 °C. The linear thermal expansion coefficients measured by thermomechanical analysis (20-600 °C) in the direction of pressing were in the range 5-9 × 10-6 K-1 and in the range 1.2-2 × 10-6 K-1 in the direction normal to pressing. The thermal conductivity of the composites were measured using Xenon flash method from 100 to 1000 °C and the values ranged from 19 to 30 W m-1 K-1.

  14. Irradiation creep of graphite

    International Nuclear Information System (INIS)

    Kennedy, C.R.

    1990-01-01

    Displacement damage of graphite by neutron irradiation causes graphite to change dimensions. This dimensional instability requires careful attention when graphite is used as as moderator and reflector material in nuclear devices. Natural gradients in flux and temperature result in time-varying differential growth generating stresses similar to thermal stresses with an ever increasing temperature gradient. Graphite, however, does have the ability to creep under irradiation, allowing the stress intensity to relax below the fracture strength of the material. Creep strain also serves to average the radiation-induced strains, thus contributing to the stability of the core. As the dimensional instability is a function of temperature, so are the creep characteristics of graphite, and it is of interest to generalize the available data for extension to more extreme conditions of fluence and temperature. Irradiation creep of graphite is characterized by two stages of creep; a primary stage that saturates with time and a secondary stage that is generally assumed to be linear and constant with time. Virtually all past studies have not considered primary creep in detail primarily because there is limited available data at the very low fluences required to saturate primary creep. It is the purpose of this study to carefully examine primary creep in detail over the irradiation temperature range of 150 to 1000 degree C. These studies also include the combined effects of creep, differential growth, and structural changes in graphite by irradiation. 3 refs., 5 figs

  15. Evaluation of the chiral recognition properties and the column performances of three chiral stationary phases based on cellulose for the enantioseparation of six dihydropyridines by high-performance liquid chromatography.

    Science.gov (United States)

    Yu, Jia; Tang, Jing; Yuan, Xiaowei; Guo, Xingjie; Zhao, Longshan

    2017-03-01

    Separations of six dihydropyridine enantiomers on three commercially available cellulose-based chiral stationary phases (Chiralcel OD-RH, Chiralpak IB, and Chiralpak IC) were evaluated with high-performance liquid chromatography (HPLC). The best enantioseparation of the six chiral drugs was obtained with a Chiralpak IC (250 × 4.6 mm i.d., 5 μm) column. Then the influence of the mobile phase including an alcohol-modifying agent and alkaline additive on the enantioseparation were investigated and optimized. The optimal mobile phase conditions and maximum resolution for every analyte were as follows respectively: n-hexane/isopropanol (85:15, v/v) for nimodipine (R = 5.80) and cinildilpine (R = 5.65); n-hexane/isopropanol (92:8, v/v) for nicardipine (R = 1.76) and nisoldipine (R = 1.92); and n-hexane/isopropanol/ethanol (97:2:1, v/v/v) for felodipine (R = 1.84) and lercanidipine (R = 1.47). Relative separation mechanisms are discussed based on the separation results, and indicate that the achiral parts in the analytes' structure showed an important influence on the separation of the chiral column. © 2017 Wiley Periodicals, Inc.

  16. The staphylococcal accessory regulator, SarA, is an RNA-binding protein that modulates the mRNA turnover properties of late-exponential and stationary phase Staphylococcus aureus cells

    Directory of Open Access Journals (Sweden)

    John M Morrison

    2012-03-01

    Full Text Available The modulation of mRNA turnover is gaining recognition as a mechanism by which Staphylococcus aureus regulates gene expression, but the factors that orchestrate alterations in transcript degradation are poorly understood. In that regard, we previously found that 138 mRNA species, including the virulence factors protein A (spa and collagen binding protein (cna, are stabilized in a sarA-dependent manner during exponential phase growth, suggesting that SarA protein may directly or indirectly effect the RNA turnover properties of these transcripts. Herein, we expanded our characterization of the effects of sarA on mRNA turnover during late exponential and stationary phases of growth. Results revealed that the locus affects the RNA degradation properties of cells during both growth phases. Further, using gel mobility shift assays and RIP-ChIP, it was found that SarA protein is capable of binding mRNA species that it stabilizes both in vitro and within bacterial cells. Taken together, these results suggest that SarA post-transcriptionally regulates S. aureus gene expression in a manner that involves binding to and consequently altering the mRNA turnover properties of target transcripts.

  17. Thermodynamic and structural study of two-dimensional phase transitions within films of molecules physi-sorbed on graphite; the role of orientational order in wetting and roughening phenomena

    International Nuclear Information System (INIS)

    Angerand, Francois

    1987-01-01

    Two-dimensional phase transitions within films physi-sorbed upon the basal face of graphite have been investigated using two experimental methods: volumetric measurements of adsorption isotherms and neutron diffraction. Our main objective was to study the role played by orientational order in these films, its influence on their thermodynamic and structural properties, and its significance in wetting and roughening phenomena, which are indirectly accessible from adsorption studies. A comparative study of the adsorption isotherms of two molecules having comparable dipole moments, NH 3 and C 2 H 3 F, discloses very dissimilar behaviours, due to the fact that hydrogen bonding is involved in the interaction between NH 3 , but not C 2 H 3 F, molecules. The impossibility of such a bond for the interaction of the adsorbate with the substrate results in a poor cohesion energy of the NH 3 ad-film in comparison with those of its bulk condensed phases. The situation is opposite for the film of C 2 H 3 F which behaves almost as a rare gas film. From multilayer adsorption isotherms of CO it is shown that graphite (0001) is perfectly wet by the plastic (orientationally disordered) crystal phase, β-CO, whereas it is incompletely wet by the low-temperature crystal phase α-CO, in which the molecules are orientationally ordered. The critical temperatures of two-dimensional condensation have been measured for the successive ad-layers, up to the fifth. They seem to converge towards a value of 65 K, which we consider as representing the temperature of the roughening transition of the (0001) face of β-CO. A neutron diffraction study of the monolayers of N 2 O and C(CD 3 ) 4 adsorbed on graphite has been carried out. For N 2 O our results suggest a structure more involved than conjectured. For C(CD 3 ) 4 we have evidence for a triple point at 178 K. The crystal monolayer has a compact hexagonal structure. (author) [fr

  18. Graphite for fusion energy applications

    International Nuclear Information System (INIS)

    Eatherly, W.P.; Clausing, R.E.; Strehlow, R.A.; Kennedy, C.R.; Mioduszewski, P.K.

    1987-03-01

    Graphite is in widespread and beneficial use in present fusion energy devices. This report reflects the view of graphite materials scientists on using graphite in fusion devices. Graphite properties are discussed with emphasis on application to fusion reactors. This report is intended to be introductory and descriptive and is not intended to serve as a definitive information source

  19. Recent developments in graphite

    International Nuclear Information System (INIS)

    Cunningham, J.E.

    1983-01-01

    Overall, the HTGR graphite situation is in excellent shape. In both of the critical requirements, fuel blocks and support structures, adequate graphites are at hand and improved grades are sufficiently far along in truncation. In the aerospace field, GraphNOL N3M permits vehicle performance with confidence in trajectories unobtainable with any other existing material. For fusion energy applications, no other graphite can simultaneously withstand both extreme thermal shock and neutron damage. Hence, the material promises to create new markets as well as to offer a better candidate material for existing applications

  20. Carbon-14 Graphitization Chemistry

    Science.gov (United States)

    Miller, James; Collon, Philippe; Laverne, Jay

    2014-09-01

    Accelerator Mass Spectrometry (AMS) is a process that allows for the analysis of mass of certain materials. It is a powerful process because it results in the ability to separate rare isotopes with very low abundances from a large background, which was previously impossible. Another advantage of AMS is that it only requires very small amounts of material for measurements. An important application of this process is radiocarbon dating because the rare 14C isotopes can be separated from the stable 14N background that is 10 to 13 orders of magnitude larger, and only small amounts of the old and fragile organic samples are necessary for measurement. Our group focuses on this radiocarbon dating through AMS. When performing AMS, the sample needs to be loaded into a cathode at the back of an ion source in order to produce a beam from the material to be analyzed. For carbon samples, the material must first be converted into graphite in order to be loaded into the cathode. My role in the group is to convert the organic substances into graphite. In order to graphitize the samples, a sample is first combusted to form carbon dioxide gas and then purified and reduced into the graphite form. After a couple weeks of research and with the help of various Physics professors, I developed a plan and began to construct the setup necessary to perform the graphitization. Once the apparatus is fully completed, the carbon samples will be graphitized and loaded into the AMS machine for analysis.

  1. Graphite Technology Development Plan

    Energy Technology Data Exchange (ETDEWEB)

    W. Windes; T. Burchell; R. Bratton

    2007-09-01

    This technology development plan is designed to provide a clear understanding of the research and development direction necessary for the qualification of nuclear grade graphite for use within the Next Generation Nuclear Plant (NGNP) reactor. The NGNP will be a helium gas cooled Very High Temperature Reactor (VHTR) with a large graphite core. Graphite physically contains the fuel and comprises the majority of the core volume. Considerable effort will be required to ensure that the graphite performance is not compromised during operation. Based upon the perceived requirements the major data needs are outlined and justified from the perspective of reactor design, reatcor performance, or the reactor safety case. The path forward for technology development can then be easily determined for each data need. How the data will be obtained and the inter-relationships between the experimental and modeling activities will define the technology development for graphite R&D. Finally, the variables affecting this R&D program are discussed from a general perspective. Factors that can significantly affect the R&D program such as funding, schedules, available resources, multiple reactor designs, and graphite acquisition are analyzed.

  2. Melting temperature of graphite

    International Nuclear Information System (INIS)

    Korobenko, V.N.; Savvatimskiy, A.I.

    2001-01-01

    Full Text: Pulse of electrical current is used for fast heating (∼ 1 μs) of metal and graphite specimens placed in dielectric solid media. Specimen consists of two strips (90 μm in thick) placed together with small gap so they form a black body model. Quasy-monocrystal graphite specimens were used for uniform heating of graphite. Temperature measurements were fulfilled with fast pyrometer and with composite 2-strip black body model up to melting temperature. There were fulfilled experiments with zirconium and tungsten of the same black body construction. Additional temperature measurements of liquid zirconium and liquid tungsten are made. Specific heat capacity (c P ) of liquid zirconium and of liquid tungsten has a common feature in c P diminishing just after melting. It reveals c P diminishing after melting in both cases over the narrow temperature range up to usual values known from steady state measurements. Over the next wide temperature range heat capacity for W (up to 5000 K) and Zr (up to 4100 K) show different dependencies of heat capacity on temperature in liquid state. The experiments confirmed a high quality of 2-strip black body model used for graphite temperature measurements. Melting temperature plateau of tungsten (3690 K) was used for pyrometer calibration area for graphite temperature measurement. As a result, a preliminary value of graphite melting temperature of 4800 K was obtained. (author)

  3. Evaluation of the chiral recognition properties as well as the column performance of four chiral stationary phases based on cellulose (3,5-dimethylphenylcarbamate) by parallel HPLC and SFC.

    Science.gov (United States)

    Nelander, Hanna; Andersson, Shalini; Ohlén, Kristina

    2011-12-30

    The performance of four commercially available cellulose tris(3,5-dimethylphenylcarbamate) based chiral stationary phases (CSPs) was evaluated with parallel high performance liquid chromatography (HPLC) and super critical fluid chromatography (SFC). Retention, enantioselectivity, resolution and efficiency were compared for a set of neutral, basic and acidic compounds having different physico-chemical properties by using different mobile phase conditions. Although the chiral selector is the same in all the four CSPs, a large difference in the ability to retain and resolve enantiomers was observed under the same chromatographic conditions. We believe that this is mainly due to differences in the silica matrix and immobilization techniques used by the different vendors. An extended study of metoprolol and structure analogues gave a deeper understanding of the accessibility of the chiral discriminating interactions and its impact on the resolution of the racemic compounds on the four CSPs studied. Also, a clear difference in enantioselectivity is observed between SFC and LC mode, hydrogen bonding was found to play an important role in the differential binding of the enantiomers to the CSPs. Copyright © 2011 Elsevier B.V. All rights reserved.

  4. Comparative study on the liquid chromatographic enantioseparation of cyclic β-amino acids and the related cyclic β-aminohydroxamic acids on Cinchona alkaloid-based zwitterionic chiral stationary phases.

    Science.gov (United States)

    Bajtai, Attila; Fekete, Beáta; Palkó, Márta; Fülöp, Ferenc; Lindner, Wolfgang; Kohout, Michal; Ilisz, István; Péter, Antal

    2018-03-01

    The enantiomeric pairs of cis and trans stereoisomers of cyclic β-aminohydroxamic acids and their related cis and trans cyclic β-amino acids containing two chiral centers were directly separated on four structurally related chiral stationary phases derived from quinine and quinidine modified with (R,R)- and (S,S)-aminocyclohexanesulfonic acids. Applying these zwitterionic ion-exchangers as chiral selectors, the effects of the composition of the bulk solvent, the acid and base additives, the structures of the analytes, and temperature on the enantioresolution were investigated. To study the effects of temperature and obtain thermodynamic parameters, experiments were carried out at constant mobile phase compositions in the temperature range 5-50°C. The differences in the changes in standard enthalpy Δ(ΔH°), entropy Δ(ΔS°), and free energy Δ(ΔG°) were calculated from the linear van't Hoff plots derived from the ln α versus 1/T curves in the studied temperature range. Results thus obtained indicated enthalpy-driven separations in all cases. The sequence of elution of the enantiomers was determined and found to be reversed when ZWIX(-)™ was changed to ZWIX(+)™ or ZWIX(-A) to ZWIX(+A). © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Capillary-channeled polymer (C-CP) fibers as a stationary phase for sample clean-up of protein solutions for matrix-assisted laser/desorption ionization mass spectrometry.

    Science.gov (United States)

    Manard, Benjamin T; Marcus, R Kenneth

    2012-08-01

    Capillary-channeled polymer (C-CP) fibers are employed in a micropipette tip format to affect a stationary phase for the solid phase extraction (SPE) of proteins from buffer solutions prior to MALDI-MS analysis. Proteins readily adsorb to the polypropylene (PP) C-CP fibers while buffer species are easily washed off the tips using DI-H(2)O. Elution of the solutes is achieved with an aliquot of 50:50 ACN:H(2)O, which is compatible with the subsequent spotting on the MALDI target with the matrix solution. Lysozyme and cytochrome c are used as test species, with a primary buffer composition of 100 mM Tris-HCl. In this case, direct MALDI-MS produces no discernible protein signals. SPE on the C-CP fibers yields high fidelity mass spectra for 1 μL sample volumes. Limits of detection for cytochrome c in 100 mM Tris-HCl are on the order of 40 nM. Extraction of cytochrome c from buffer concentrations of up to 1 M Tris-HCl, provides signal recoveries that are suppressed by only ~50% versus neat protein solutions. Finally, extraction of 3.1 μM cytochrome c from a synthetic urine matrix exhibits excellent recovery.

  6. Capillary-Channeled Polymer (C-CP) Fibers as a Stationary Phase for Sample Clean-Up of Protein Solutions for Matrix-Assisted Laser/Desorption Ionization Mass Spectrometry

    Science.gov (United States)

    Manard, Benjamin T.; Marcus, R. Kenneth

    2012-08-01

    Capillary-channeled polymer (C-CP) fibers are employed in a micropipette tip format to affect a stationary phase for the solid phase extraction (SPE) of proteins from buffer solutions prior to MALDI-MS analysis. Proteins readily adsorb to the polypropylene (PP) C-CP fibers while buffer species are easily washed off the tips using DI-H2O. Elution of the solutes is achieved with an aliquot of 50:50 ACN:H2O, which is compatible with the subsequent spotting on the MALDI target with the matrix solution. Lysozyme and cytochrome c are used as test species, with a primary buffer composition of 100 mM Tris-HCl. In this case, direct MALDI-MS produces no discernible protein signals. SPE on the C-CP fibers yields high fidelity mass spectra for 1 μL sample volumes. Limits of detection for cytochrome c in 100 mM Tris-HCl are on the order of 40 nM. Extraction of cytochrome c from buffer concentrations of up to 1 M Tris-HCl, provides signal recoveries that are suppressed by only ~50 % versus neat protein solutions. Finally, extraction of 3.1 μM cytochrome c from a synthetic urine matrix exhibits excellent recovery.

  7. Adsorption behaviors of neutral and ionizable compounds on hybrid stationary phases in the absence (BEH-C18) and the presence (CSH-C18) of immobile surface charges.

    Science.gov (United States)

    Gritti, Fabrice; Guiochon, Georges

    2013-03-22

    The adsorption behaviors of a neutral (caffeine) and a positively charged compound (nortriptylinium) are investigated on two RPLC/hybrid stationary phases, eluted with a low ionic strength buffer (phosphate buffer, W(S)pH 2.63, I=10mM). The first phase, bridge ethylene hybrid (BEH), is neutral at all pHs whereas the second, charged surface hybrid (CSH), contains a protonated ligand at W(W)pH C18 at 20mV and by the subsequent decrease of the equilibrium constant of weak adsorption sites (C18 environment) and removal of the strong adsorption sites (accessible silanols). At the highest sample loadings (5 and 20μL, C=30g/L), the EML and the bi-EML isotherms failed because some adsorbate-adsorbate interactions take place when bulk concentrations exceed 0.2g/L. The experimental data were then successively fitted to an empirical heterogeneous Langmuir-Moreau (LM) explicit isotherm. The best saturation capacities of the empirical heterogeneous LM isotherm is consistent with the manufacturer's estimate of the surface concentration of residual silanols onto the BEH- and CSH-C18 endcapped adsorbent (<0.1μmol/m(2)). Copyright © 2013 Elsevier B.V. All rights reserved.

  8. Ortho-substituent correlated retention of polychlorinated biphenyls on a 50% n-octyl-methylpolysiloxane stationary phase by HRGC/MSD

    Energy Technology Data Exchange (ETDEWEB)

    Fischer, R.; Ballschmiter, K.

    1988-11-01

    Polychlorinated biphenyls (PCB) have been known as ubiquitous environmental pollutants since the late 60s. They are found partitioned between all environmental compartments according to their physico-chemical properties. Investigation of their partitioning, degradation, and transport behaviour demands sensitive and selective analytical methods for this complex mixture of up to 209 theoretically possible compounds. Congener-specific separation by high-resolution gas chromatography coupled with mass-selective detection would be a suitable approach to this multi-compound problem. In this paper, the separation of PCB congeners by capillary gas chromatography (HRGC) on a 50% n-octyl-methylpolysiloxane phase is presented.

  9. Nuclear graphite ageing and turnaround

    International Nuclear Information System (INIS)

    Marsden, B.J.; Hall, G.N.; Smart, J.

    2001-01-01

    Graphite moderated reactors are being operated in many countries including, the UK, Russia, Lithuania, Ukraine and Japan. Many of these reactors will operate well into the next century. New designs of High Temperature Graphite Moderated Reactors (HTRS) are being built in China and Japan. The design life of these graphite-moderated reactors is governed by the ageing of the graphite core due to fast neutron damage, and also, in the case of carbon dioxide cooled reactors by the rate of oxidation of the graphite. Nuclear graphites are polycrystalline in nature and it is the irradiation-induced damage to the individual graphite crystals that determines the material property changes with age. The life of a graphite component in a nuclear reactor can be related to the graphite irradiation induced dimensional changes. Graphites typically shrink with age, until a point is reached where the shrinkage stops and the graphite starts to swell. This change from shrinkage to swelling is known as ''turnaround''. It is well known that pre-oxidising graphite specimens caused ''turnaround'' to be delayed, thus extending the life of the graphite, and hence the life of the reactor. However, there was no satisfactory explanation of this behaviour. This paper presents a numerical crystal based model of dimensional change in graphite, which explains the delay in ''turnaround'' in the pre-oxidised specimens irradiated in a fast neutron flux, in terms of crystal accommodation and orientation and change in compliance due to radiolytic oxidation. (author)

  10. Study on solid phase extraction and graphite furnace atomic absorption spectrometry for the determination of nickel, silver, cobalt, copper, cadmium and lead with MCI GEL CHP 20Y as sorbent

    International Nuclear Information System (INIS)

    Yang Guangyu; Fen Weibo; Lei Chun; Xiao Weilie; Sun Handong

    2009-01-01

    A solid phase extraction and graphite furnace atomic absorption spectrometry (GFAAS) for the determination of nickel, silver, cobalt, copper, cadmium and lead with MCI GEL CHP 20Y as sorbent was studied. Trace amounts of chromium, nickel, silver, cobalt, copper, cadmium and lead were reacted with 2-(2-quinolinil-azo)-4-methyl-1,3-dihydroxidobenzene (QAMDHB) followed by adsorption onto MCI GEL CHP 20Y solid phase extraction column, and 1.0 mol L -1 HNO 3 was used as eluent. The metal ions in 300 mL solution can be concentrated to 1.0 mL, representing an enrichment factor of 300 was achieved. The recoveries of analytes at pH 8.0 with 1.0 g of resin were greater than 95% without interference from alkaline, earth alkaline and some metal ions. When detected with graphite furnace atomic absorption spectrometry, the detection limits in the original samples were 1.4 ng L -1 for Cr(III), 1.0 ng L -1 for Ni(II), 0.85 ng L -1 for Ag(I), 1.2 ng L -1 for Co(II), 1.0 ng L -1 for Cu(II), 1.2 ng L -1 for Cd(II) and 1.3 ng L -1 for Pb(II). The validation of the procedure was performed by the analysis of the certified standard reference materials, and the presented procedure was applied to the determination of analytes in biological, water and soil samples with good results (recoveries range from 89 to 104%, and R.S.D.% lower than 3.2%. The results agreed with the standard value or reference method)

  11. I. Diamino telechelic polybutadienes: Synthesis, characterization and melt coupling. II. Poly(epsilon-caprolactone-beta-poly(ethylene glycol) polymeric nanoparticles for drug delivery. III. Zirconia based cellulosic HPLC chiral stationary phase for enantioseparations

    Science.gov (United States)

    Ji, Shengxiang

    This thesis is comprised of three parts under the theme of functional specialty polymers. The first project involves the synthesis, characterization, and melt coupling of diamino telechelic polybutadienes. The second part describes the preparation of PCL-PEG polymeric nanoparticles for drug delivery. The third project focuses on the preparation of cellulosic HPLC chiral stationary phases for enantioseparations. Styrene-butadiene-styrene (SBS) block copolymers (BCPs) are difficult to process due to high order-disorder transition temperature and high viscosity. An attractive strategy for approaching this problem is the use of reactive coupling between diamino telechelic PB (TPB) and anhydride-terminated polystyrene (PS-anh) to generate SBS BCPs during melt processing. Diamino TPBs were synthesized by ring-opening metathesis polymerization of 1,5-cyclooctadiene using 1,8-dicyano-4-octene as a chain transfer agent, followed by lithium aluminum hydride reduction. A 19F NMR method was developed to quantify the primary amine functionality for TPBs. Melt coupling of diamino TPB and PS-anh at 180 °C resulted in formation of SBS triblock copolymers, which was confirmed by SAXS. Maleimide terminated poly(epsilon-caprolactone)- b-poly(ethylene glycol) (PCL-PEG-MAL) nanoparticles are of special interest in biomedical applications. However, the synthesis of PCL-PEG-MAL with high maleimide functionality is difficult. Carboxylic acid functionalized poly(epsilon-caprolactone)s (PCL-COOHs) with narrow polydispersity were prepared by ring-opening polymerization of epsilon-caprolactone. Three PCL-PEG-OHs were, synthesized by coupling of excess HO-PEG-OH with different molecular weight PCL-COCls, The hydroxyl end-groups were transferred to maleimide groups to give PCL-PEG-MALs. Nanoparticles with maleimide functionality were prepared by impingement mixing. Particle sizes and size distributions were determined by dynamic light scattering. The amount of accessible maleimide on the

  12. Enantiomer separation of a powerful chiral auxiliary, 2-methoxy-2-(1-naphthyl)propionic acid by liquid chromatography using chiral anion exchanger-type stationary phases in polar-organic mode; investigation of molecular recognition aspects.

    Science.gov (United States)

    Gyimesi-Forrás, Krisztina; Akasaka, Kazuaki; Lämmerhofer, Michael; Maier, Norbert M; Fujita, Takuma; Watanabe, Masataka; Harada, Nobuyuki; Lindner, Wolfgang

    2005-01-01

    The enantiodiscriminating potential of the weak anion exchange-type quinine-based chiral stationary phases (CSPs) for direct enantiomer separation of racemic 2-methoxy-2-(1-naphthyl)propionic acid (selectand, SA) was studied. The influence of structure variations of the selector (SO) in the carbamate functional group and/or in the C6' position of quinoline moiety on retention and enantioselectivity was investigated. Systematic chromatographic studies were made to gain more insight into the overall chiral recognition mechanism for a given mobile phase. In this context, the tert-butylcarbamoyl quinine and the corresponding diisopropylphenyl-derived selector provided the highest resolution and enantioselectivity under polar-organic conditions with the elution order of (R) before the (S) enantiomer. When the bulkiness of the substituents in the C6' position of the SO was increased, the selectivity was decreased in all cases. Alkylation of the nitrogen atom in the carbamate functionality of the SO resulted in the complete loss of enantiomer separation, confirming the crucial importance of the hydrogen-bond formation involved in the stereodiscriminating events. In addition, ten different mono-, bi-, or trivalent acids, necessary as competitor molecules (counter-ions) of the mobile phase, were screened to judge their influence on retention and overall enantioselectivity. Among them, acetic acid, formic acid, N-acetylglycine, and glycolic acid proved to be the most promising counter-ions with R(S) values of 6.35, 6.81, 8.19, and 7.34, respectively. On the basis of chromatographic data, a tentative molecular recognition model was proposed. Simultaneous ion-pairing and hydrogen bonding, in concert with pi-pi stacking and steric interactions, were expected to be responsible for chiral recognition mechanism. This was partially corroborated by structural and/or conformational analysis of the tert-butylcarbamoyl quinine-2-methoxy-2-(1-naphthyl)propionic acid (SO-SA) complex

  13. High pressure size exclusion chromatography (HPSEC) determination of dissolved organic matter molecular weight revisited: Accounting for changes in stationary phases, analytical standards, and isolation methods

    Science.gov (United States)

    McAdams, Brandon C.; Aiken, George R.; McKnight, Diane M.; Arnold, William A.; Chin, Yu-Ping

    2018-01-01

    We reassessed the molecular weight of dissolved organic matter (DOM) determined by high pressure size exclusion chromatography (HPSEC) using measurements made with different columns and various generations of polystyrenesulfonate (PSS) molecular weight standards. Molecular weight measurements made with a newer generation HPSEC column and PSS standards from more recent lots are roughly 200 to 400 Da lower than initial measurements made in the early 1990s. These updated numbers match DOM molecular weights measured by colligative methods and fall within a range of values calculated from hydroxyl radical kinetics. These changes suggest improved accuracy of HPSEC molecular weight measurements that we attribute to improved accuracy of PSS standards and changes in the column packing. We also isolated DOM from wetlands in the Prairie Pothole Region (PPR) using XAD-8, a cation exchange resin, and PPL, a styrene-divinylbenzene media, and observed little difference in molecular weight and specific UV absorbance at 280 nm (SUVA280) between the two solid phase extraction resins, suggesting they capture similar DOM moieties. PPR DOM also showed lower SUVA280 at similar weights compared to DOM isolates from a global range of environments, which we attribute to oxidized sulfur in PPR DOM that would increase molecular weight without affecting SUVA280.

  14. High Pressure Size Exclusion Chromatography (HPSEC) Determination of Dissolved Organic Matter Molecular Weight Revisited: Accounting for Changes in Stationary Phases, Analytical Standards, and Isolation Methods.

    Science.gov (United States)

    McAdams, Brandon C; Aiken, George R; McKnight, Diane M; Arnold, William A; Chin, Yu-Ping

    2018-01-16

    We reassessed the molecular weight of dissolved organic matter (DOM) determined by high pressure size exclusion chromatography (HPSEC) using measurements made with different columns and various generations of polystyrenesulfonate (PSS) molecular weight standards. Molecular weight measurements made with a newer generation HPSEC column and PSS standards from more recent lots are roughly 200 to 400 Da lower than initial measurements made in the early 1990s. These updated numbers match DOM molecular weights measured by colligative methods and fall within a range of values calculated from hydroxyl radical kinetics. These changes suggest improved accuracy of HPSEC molecular weight measurements that we attribute to improved accuracy of PSS standards and changes in the column packing. We also isolated DOM from wetlands in the Prairie Pothole Region (PPR) using XAD-8, a cation exchange resin, and PPL, a styrene-divinylbenzene media, and observed little difference in molecular weight and specific UV absorbance at 280 nm (SUVA 280 ) between the two solid phase extraction resins, suggesting they capture similar DOM moieties. PPR DOM also showed lower SUVA 280 at similar weights compared to DOM isolates from a global range of environments, which we attribute to oxidized sulfur in PPR DOM that would increase molecular weight without affecting SUVA 280 .

  15. Correlations Between retention indices and molecular structure of aliphatic alcohols and of their benzoyl derivatives on phenyl substituted polysiloxane stationary phases

    International Nuclear Information System (INIS)

    Pias, J. B.; Gasco, L.

    1976-01-01

    The retention indices of aliphatic alcohols of carbon number up to C g , and of their benzoyl derivatives up to C 7 , were determined in columns packed with Chromo sorb G (AW-DMCS-HP) coated previously with 5% methyl, and methyl phenyl polysiloxanes with increasing polarity (SE-30, 0V-3, 0V-7, 0V-11, 0V-17 and OV-25). Correlations between retention indices and chain length for 1-alcohols, 2-alcohols, 3-alcohols, 1 , on -3-alcohols, 2-methyl-1-alcohols and for their corresponding benzoyl derivatives were calculated at 100, 120 and 140 degree centigree. In alcohols, a -CH 2 - group increases I approximately 100 units, and in their benzoyl derivatives from 80 to 100 units. Dispersion indices Δl , and positional and structural increments δI, were evaluated for -OH and benzoyl groups in terms of phase polarity and chain length. Effects of chain length, chain branching and double bond location on retention parameters were also studied. (Author) 23 refs

  16. Variation of the properties of siliconized graphite during neutron irradiation

    International Nuclear Information System (INIS)

    Virgil'ev, Y.S.; Chugunova, T.K.; Pikulik, R.G.

    1986-01-01

    The authors evaluate the radiation-induced property changes in siliconized graphite of the industrial grades SG-P and SG-M. The authors simultaneously tested the reference (control) specimens of graphite that are used as the base for obtaining the SG-M siliconized graphite by impregnating with silicon. The suggested scheme (model) atributes the dimensional changes of the siliconized graphite specimens to the effect of the quantitative ratio of the carbide phase and carbon under different conditions of irradiation. If silicon is insufficient for the formation of a dense skeleton, graphite plays a devisive role, and it may be assumed that at an irradiation temperature greater than 600 K, the material shrinks. The presence of isolated carbide inclusions also affects the physicomechanical properties (including the anitfriction properties)

  17. Irradiation Creep in Graphite

    Energy Technology Data Exchange (ETDEWEB)

    Ubic, Rick; Butt, Darryl; Windes, William

    2014-03-13

    An understanding of the underlying mechanisms of irradiation creep in graphite material is required to correctly interpret experimental data, explain micromechanical modeling results, and predict whole-core behavior. This project will focus on experimental microscopic data to demonstrate the mechanism of irradiation creep. High-resolution transmission electron microscopy should be able to image both the dislocations in graphite and the irradiation-induced interstitial clusters that pin those dislocations. The team will first prepare and characterize nanoscale samples of virgin nuclear graphite in a transmission electron microscope. Additional samples will be irradiated to varying degrees at the Advanced Test Reactor (ATR) facility and similarly characterized. Researchers will record microstructures and crystal defects and suggest a mechanism for irradiation creep based on the results. In addition, the purchase of a tensile holder for a transmission electron microscope will allow, for the first time, in situ observation of creep behavior on the microstructure and crystallographic defects.

  18. Cesium diffusion in graphite

    International Nuclear Information System (INIS)

    Evans, R.B. III; Davis, W. Jr.; Sutton, A.L. Jr.

    1980-05-01

    Experiments on diffusion of 137 Cs in five types of graphite were performed. The document provides a completion of the report that was started and includes a presentation of all of the diffusion data, previously unpublished. Except for data on mass transfer of 137 Cs in the Hawker-Siddeley graphite, analyses of experimental results were initiated but not completed. The mass transfer process of cesium in HS-1-1 graphite at 600 to 1000 0 C in a helium atmosphere is essentially pure diffusion wherein values of (E/epsilon) and ΔE of the equation D/epsilon = (D/epsilon) 0 exp [-ΔE/RT] are about 4 x 10 -2 cm 2 /s and 30 kcal/mole, respectively

  19. A Novel Two-Step Liquid-Liquid Extraction Procedure Combined with Stationary Phase Immobilized Human Serum Albumin for the Chiral Separation of Cetirizine Enantiomers along with M and P Parabens

    Directory of Open Access Journals (Sweden)

    Aleksandra Chmielewska

    2016-12-01

    Full Text Available The research into the separation of drug enantiomers is closely related to the safety and efficiency of the drugs. The aim of this study was to develop a simple and validated HPLC method to analyze cetirizine enantiomers. In the case of liquid dosage forms, besides the active substance in large amounts there are usually also inactive ingredients such as methyl- and propylparaben. Unfortunately, these compounds can interfere with the analyte, inter alia during chiral separation of the analyte enantiomers. The proposed innovative two-step liquid-liquid extraction procedure allowed for the determination of cetirizine enantiomers (along with M and P parabens also in liquid dosage forms. The main focus of this study was the chromatographic activity of cetirizine dihydrochloride on the proteinate-based chiral stationary phase. The chromatographic separation of cetirizine enantiomers was performed on an immobilized human serum albumin (HSA column for the first time. Measurements were performed at a wavelength of 227 nm. Under optimal conditions, baseline separation of two enantiomers was obtained with 1.43 enantioseparation factor (α and 1.82 resolution (Rs. Finally, the proposed method was successfully applied to the selected pharmaceutical formulations.

  20. A Novel Two-Step Liquid-Liquid Extraction Procedure Combined with Stationary Phase Immobilized Human Serum Albumin for the Chiral Separation of Cetirizine Enantiomers along with M and P Parabens.

    Science.gov (United States)

    Chmielewska, Aleksandra; Konieczna, Lucyna; Bączek, Tomasz

    2016-12-07

    The research into the separation of drug enantiomers is closely related to the safety and efficiency of the drugs. The aim of this study was to develop a simple and validated HPLC method to analyze cetirizine enantiomers. In the case of liquid dosage forms, besides the active substance in large amounts there are usually also inactive ingredients such as methyl- and propylparaben. Unfortunately, these compounds can interfere with the analyte, inter alia during chiral separation of the analyte enantiomers. The proposed innovative two-step liquid-liquid extraction procedure allowed for the determination of cetirizine enantiomers (along with M and P parabens) also in liquid dosage forms. The main focus of this study was the chromatographic activity of cetirizine dihydrochloride on the proteinate-based chiral stationary phase. The chromatographic separation of cetirizine enantiomers was performed on an immobilized human serum albumin (HSA) column for the first time. Measurements were performed at a wavelength of 227 nm. Under optimal conditions, baseline separation of two enantiomers was obtained with 1.43 enantioseparation factor (α) and 1.82 resolution ( R s ). Finally, the proposed method was successfully applied to the selected pharmaceutical formulations.

  1. Graphite-based photovoltaic cells

    Science.gov (United States)

    Lagally, Max; Liu, Feng

    2010-12-28

    The present invention uses lithographically patterned graphite stacks as the basic building elements of an efficient and economical photovoltaic cell. The basic design of the graphite-based photovoltaic cells includes a plurality of spatially separated graphite stacks, each comprising a plurality of vertically stacked, semiconducting graphene sheets (carbon nanoribbons) bridging electrically conductive contacts.

  2. Graphite technology development plan

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1986-07-01

    This document presents the plan for the graphite technology development required to support the design of the 350 MW(t) Modular HTGR within the US National Gas-Cooled Reactor Program. Besides descriptions of the required technology development, cost estimates, and schedules, the plan also includes the associated design functions and design requirements.

  3. (Irradiation creep of graphite)

    Energy Technology Data Exchange (ETDEWEB)

    Kennedy, C.R.

    1990-12-21

    The traveler attended the Conference, International Symposium on Carbon, to present an invited paper, Irradiation Creep of Graphite,'' and chair one of the technical sessions. There were many papers of particular interest to ORNL and HTGR technology presented by the Japanese since they do not have a particular technology embargo and are quite open in describing their work and results. In particular, a paper describing the failure of Minor's law to predict the fatigue life of graphite was presented. Although the conference had an international flavor, it was dominated by the Japanese. This was primarily a result of geography; however, the work presented by the Japanese illustrated an internal program that is very comprehensive. This conference, a result of this program, was better than all other carbon conferences attended by the traveler. This conference emphasizes the need for US participation in international conferences in order to stay abreast of the rapidly expanding HTGR and graphite technology throughout the world. The United States is no longer a leader in some emerging technologies. The traveler was surprised by the Japanese position in their HTGR development. Their reactor is licensed and the major problem in their graphite program is how to eliminate it with the least perturbation now that most of the work has been done.

  4. PROPRIÉTÉS ÉLECTRONIQUES DU GRAPHITE

    OpenAIRE

    Schneider, Johannes M.

    2010-01-01

    In this thesis, low-temperature magnetotransport (T = 10 mK) and the de Haas-van Alphen effect of both natural graphite and highly oriented pyrolytic graphite (HOPG) are examined. In the first part, low field magnetotransport up to B = 11 T is discussed. A Fourier analysis of the background removed signal shows that the electric transport in graphite is governed by two types of charge carriers, electrons and holes. Their phase and frequency values are in agreement with the predictions of the ...

  5. Determination of tellurium at ultra-trace levels in drinking water by on-line solid phase extraction coupled to graphite furnace atomic absorption spectrometer

    International Nuclear Information System (INIS)

    Pedro, Juana; Stripekis, Jorge; Bonivardi, Adrian; Tudino, Mabel

    2008-01-01

    In this paper, two time-based flow injection (FI) separation pre-concentration systems coupled to graphite furnace atomic absorption spectrometry (GFAAS) for tellurium determination are studied and compared. The first alternative involves the pre-concentration of the analyte onto Dowex 1X8 employed as packaging material of a micro-column inserted in the flow system. The second set-up is based on the co-precipitation of tellurium with La(OH) 3 followed by retention onto XAD resins. Both systems are compared in terms of limit of detection, linear range, RSD%, sample throughput, micro-columns lifetime and aptitude for fully automatic operation. The features of the Dowex system are: 37% efficiency of retention and an enhancement factor of 42 for a pre-concentration time of 180 seconds (sample flow rate = 3 ml min -1 ) with acetic acid elution volumes of 80 μl. The detection limit (3 s) is 7 ng l -1 and the relative standard deviation (n = 7200 ng l -1 ) is 5.8%. The analytical performance of the XAD system is: 72% efficiency of retention and an enhancement factor of 25 for a pre-concentration time of 180 s (sample flow rate = 3 ml min -1 ) with nitric acid elution volumes of 300 μl. The detection limit is 66 ng l -1 and the relative standard deviation (n = 7200 ng l -1 ) is 8.3%. Applications to the determination of tellurium in tap water and the validation of the analytical methodology employing SRM 1643e as certified reference material are shown

  6. INCREASING OF MECHANICAL PROPERTIES OF CAST GRAPHITIZED STEEL

    Directory of Open Access Journals (Sweden)

    I. V. Akimov

    2015-06-01

    Full Text Available Purpose. Due to the presence of many essential properties (low prime cost, high manufacturability and damping ability, heat conductivity, fluidity and others,the graphitized cast irons are widely applied for parts operating under the conditions of static and cyclic loads, wear at dry friction and aggressive media at elevated temperatures. At the same time because of significant content of the graphite phase in the structure, the cast irons possess relatively low mechanical properties. Thereby the attention is drawn to graphitized steels, the peculiarity of which consists in the presence of graphite inclusions in the structure, which appoints specific cast iron's properties to these materials. But unlike cast irons, the graphite content in them is in 2…3 times lower and it affects positively on mechanical and service properties indices. This work deals with the optimization of the composition of cast graphitized steel, which has high mechanical properties indices. Methodology. The experimental design technique was used in this work. Alloys prototypes were smelted and their mechanical properties were investigated on the basis of these techniques. Findings were exposed to regression processing, and the dependences of the alloys components influence on its properties were obtained. By means of graphical optimization the optimal composition of steel with high mechanical properties indices has been determined. Findings.Ithasbeenestablishedthat carbon and silicon have the most significant influence on the strength and cyclic endurance of graphitized steels. The chemical composition of the cast graphitized steel with high static and cyclic strength indices was suggested in this work. Originality. With the use of mathematical experimental design techniques the dependences describing the influence of carbon, silicon and copper on the static and cyclic strength indices were obtained. They allow optimizing compositions of graphitized steels. Practical

  7. Gas transport in graphitic materials

    International Nuclear Information System (INIS)

    Hoinkis, E.

    1995-02-01

    The characterization of the gas transport properties of porous solids is of interest in several fields of science and technology. Many catalysts, adsorbents, soils, graphites and carbons are porous. The gas transport through most porous solids can be well described by the dusty gas model invented by Evans, Watson and Mason. This model includes all modes of gas tranport under steady-state conditions, which are Knudsen diffusion, combined Knudsen/continuum diffusion and continuum diffusion, both for gas pairs with equal and different molecular weights. In the absence of a pressure difference gas transport in a pore system can be described by the combined Knudsen/continuum diffusion coefficient D 1 for component 1 in the pores, the Knudsen diffusion coefficient D 1K in the pores, and the continuum diffusion coefficient D 12 for a binary mixture in the pores. The resistance to stationary continuum diffusion of the pores is characterized by a geometrical factor (ε/τ) 12 = (ε/τ)D 12 , were D 12 is the continuum diffusion coefficient for a binary mixture in free space. The Wicke-Kallenbach method was often used to measure D 1 as function of pressure. D 12 and D 1K can be derived from a plot 1/D 1 νs P, and ε/τcan be calculated since D 12 is known. D 1K and the volume of dead end pores can be derived from transient measurements of the diffusional flux at low pressures. From D 1K the expression (ε/τ c ) anti l por may be calculated, which characterizes the pore system for molecular diffusion, where collisions with the pore walls are predominant. (orig.)

  8. Ultrafast Multiphoton Thermionic Photoemission from Graphite

    Directory of Open Access Journals (Sweden)

    Shijing Tan

    2017-01-01

    Full Text Available Electronic heating of cold crystal lattices in nonlinear multiphoton excitation can transiently alter their physical and chemical properties. In metals where free electron densities are high and the relative fraction of photoexcited hot electrons is low, the effects are small, but in semimetals, where the free electron densities are low and the photoexcited densities can overwhelm them, the intense femtosecond laser excitation can induce profound changes. In semimetal graphite and its derivatives, strong optical absorption, weak screening of the Coulomb potential, and high cohesive energy enable extreme hot electron generation and thermalization to be realized under femtosecond laser excitation. We investigate the nonlinear interactions within a hot electron gas in graphite through multiphoton-induced thermionic emission. Unlike the conventional photoelectric effect, within about 25 fs, the memory of the excitation process, where resonant dipole transitions absorb up to eight quanta of light, is erased to produce statistical Boltzmann electron distributions with temperatures exceeding 5000 K; this ultrafast electronic heating causes thermionic emission to occur from the interlayer band of graphite. The nearly instantaneous thermalization of the photoexcited carriers through Coulomb scattering to extreme electronic temperatures characterized by separate electron and hole chemical potentials can enhance hot electron surface femtochemistry, photovoltaic energy conversion, and incandescence, and drive graphite-to-diamond electronic phase transition.

  9. Identification of IbeR as a Stationary-Phase Regulator in Meningitic Escherichia coli K1 that Carries a Loss-of-Function Mutation in rpoS

    Directory of Open Access Journals (Sweden)

    Feng Chi

    2009-01-01

    Full Text Available IbeR is a regulator present in meningitic Escherichia coli strain E44 that carries a loss-of-function mutation in the stationary-phase (SP regulatory gene rpoS. In order to determine whether IbeR is an SP regulator in E44, two-dimensional gel electrophoresis and LC-MS were used to compare the proteomes of a noninvasive ibeR deletion mutant BR2 and its parent strain E44 in the SP. Four up-regulated (TufB, GapA, OmpA, AhpC and three down-regulated (LpdA, TnaA, OpmC proteins in BR2 were identified when compared to E44. All these proteins contribute to energy metabolism or stress resistance, which is related to SP regulation. One of the down-regulated proteins, tryptophanase (TnaA, which is regulated by RpoS in other E. coli strains, is associated with SP regulation via production of a signal molecule indole. Our studies demonstrated that TnaA was required for E44 invasion, and that indole was able to restore the noninvasive phenotype of the tnaA mutant. The production of indole was significantly reduced in BR2, indicating that ibeR is required for the indole production via tnaA. Survival studies under different stress conditions indicated that IbeR contributed to bacteria stress resistance in the SP. Taken together, IbeR is a novel regulator contributing to the SP regulation.

  10. Harwell Graphite Calorimeter

    International Nuclear Information System (INIS)

    Linacre, J.K.

    1970-01-01

    The calorimeter is of the steady state temperature difference type. It contains a graphite sample supported axially in a graphite outer jacket, the assembly being contained in a thin stainless steel outer can. The temperature of the jacket and the temperature difference between sample and jacket are measured by chromel-alumel thermocouples. The instrument is calibrated by means of an electric heater of low mass positioned on the axis of the sample. The resistance of the heater is known and both current through the heater and the potential across it may be measured. The instrument is filled with nitrogen at a pressure of one half atmosphere at room temperature. The calorimeter has been designed for prolonged operation at temperatures up to 600°C, and dose rates up to 1 Wg -1 , and instruments have been in use for periods in excess of one year

  11. Structural disorder of graphite and implications for graphite thermometry

    Directory of Open Access Journals (Sweden)

    M. Kirilova

    2018-02-01

    Full Text Available Graphitization, or the progressive maturation of carbonaceous material, is considered an irreversible process. Thus, the degree of graphite crystallinity, or its structural order, has been calibrated as an indicator of the peak metamorphic temperatures experienced by the host rocks. However, discrepancies between temperatures indicated by graphite crystallinity versus other thermometers have been documented in deformed rocks. To examine the possibility of mechanical modifications of graphite structure and the potential impacts on graphite thermometry, we performed laboratory deformation experiments. We sheared highly crystalline graphite powder at normal stresses of 5 and 25  megapascal (MPa and aseismic velocities of 1, 10 and 100 µm s−1. The degree of structural order both in the starting and resulting materials was analyzed by Raman microspectroscopy. Our results demonstrate structural disorder of graphite, manifested as changes in the Raman spectra. Microstructural observations show that brittle processes caused the documented mechanical modifications of the aggregate graphite crystallinity. We conclude that the calibrated graphite thermometer is ambiguous in active tectonic settings.

  12. Chemical stabilization of graphite surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Bistrika, Alexander A.; Lerner, Michael M.

    2018-04-03

    Embodiments of a device, or a component of a device, including a stabilized graphite surface, methods of stabilizing graphite surfaces, and uses for the devices or components are disclosed. The device or component includes a surface comprising graphite, and a plurality of haloaryl ions and/or haloalkyl ions bound to at least a portion of the graphite. The ions may be perhaloaryl ions and/or perhaloalkyl ions. In certain embodiments, the ions are perfluorobenzenesulfonate anions. Embodiments of the device or component including stabilized graphite surfaces may maintain a steady-state oxidation or reduction surface current density after being exposed to continuous oxidation conditions for a period of at least 1-100 hours. The device or component is prepared by exposing a graphite-containing surface to an acidic aqueous solution of the ions under oxidizing conditions. The device or component can be exposed in situ to the solution.

  13. Impedance of electrochemically modified graphite.

    Science.gov (United States)

    Magdić, Katja; Kvastek, Krešimir; Horvat-Radošević, Višnja

    2014-01-01

    Electrochemical impedance spectroscopy, EIS, has been applied for characterization of electrochemically modified graphite electrodes in the sulphuric acid solution. Graphite modifications were performed by potential cyclization between potentials of graphite oxide formation/reduction, different number of cycles, and prolonged reduction steps after cyclization. Impedance spectra measured at two potential points within double-layer region of graphite have been successfully modeled using the concept of porous electrodes involving two different electrolyte diffusion paths, indicating existence of two classes of pores. The evaluated impedance parameter values show continuous changes with stages of graphite modification, indicating continuous structural changes of pores by number of potential cycles applied. Differences of impedance parameter values at two potential values indicate the potential induced changes of solution properties within the pores of modified graphite.

  14. Heat exchanger using graphite foam

    Science.gov (United States)

    Campagna, Michael Joseph; Callas, James John

    2012-09-25

    A heat exchanger is disclosed. The heat exchanger may have an inlet configured to receive a first fluid and an outlet configured to discharge the first fluid. The heat exchanger may further have at least one passageway configured to conduct the first fluid from the inlet to the outlet. The at least one passageway may be composed of a graphite foam and a layer of graphite material on the exterior of the graphite foam. The layer of graphite material may form at least a partial barrier between the first fluid and a second fluid external to the at least one passageway.

  15. Blunt indentation of core graphite

    International Nuclear Information System (INIS)

    Hartley, M.; McEnaney, B.

    1996-01-01

    Blunt indentation experiments were carried out on unoxidized and thermally oxidised IM1-24 graphite as a model to simulate local point stresses acting on graphite moderator bricks. Blunt indentation of unoxidized graphite initiates cracks close to the region of maximum tensile stress at the edge of the indentation. Cracks propagate and converge to form a cone of material. Failure is catastrophic, typically forming three pieces of graphite and ejecting the cone referred to above. The failure mode under indentation loading for highly oxidised graphite (weigh loss > 40%) is different from that for the unoxidized graphite. There is no longer a distinct crack path, the indentation is much deeper than in the case of the unoxidized graphite, and there is a region of crushed debris beneath the indentation, producing a crater-like structure. The reduction in the compressive fracture stress, σ cf , under indentation loading with increasing fractional weight loss on oxidation, x, can be fitted to σ cf /σ 0 = exp-[5.2x] where σ 0 is the compressive fracture stress of the unoxidized graphite. This indicates that the effect of thermal oxidation on indentation fracture stress is more severe than the effects of radiolytic oxidation on conventional strengths of nuclear graphites. (author). 8 refs, 12 figs

  16. Speciation of As(III) and As(V) in water samples by graphite furnace atomic absorption spectrometry after solid phase extraction combined with dispersive liquid-liquid microextraction based on the solidification of floating organic drop.

    Science.gov (United States)

    Shamsipur, Mojtaba; Fattahi, Nazir; Assadi, Yaghoub; Sadeghi, Marzieh; Sharafi, Kiomars

    2014-12-01

    A solid phase extraction (SPE) coupled with dispersive liquid-liquid microextraction based on the solidification of floating organic drop (DLLME-SFO) method, using diethyldithiphosphate (DDTP) as a proper chelating agent, has been developed as an ultra preconcentration technique for the determination of inorganic arsenic in water samples prior to graphite furnace atomic absorption spectrometry (GFAAS). Variables affecting the performance of both steps were thoroughly investigated. Under optimized conditions, 100mL of As(ΙΙΙ) solution was first concentrated using a solid phase sorbent. The extract was collected in 2.0 mL of acetone and 60.0 µL of 1-undecanol was added into the collecting solvent. The mixture was then injected rapidly into 5.0 mL of pure water for further DLLME-SFO. Total inorganic As(III, V) was extracted similarly after reduction of As(V) to As(III) with potassium iodide and sodium thiosulfate and As(V) concentration was calculated by difference. A mixture of Pd(NO3)2 and Mg(NO3)2 was used as a chemical modifier in GFAAS. The analytical characteristics of the method were determined. The calibration graph was linear in the rage of 10-100 ng L(-1) with detection limit of 2.5 ng L(-1). Repeatability (intra-day) and reproducibility (inter-day) of method based on seven replicate measurements of 80 ng L(-1) of As(ΙΙΙ) were 6.8% and 7.5%, respectively. The method was successfully applied to speciation of As(III), As(V) and determination of the total amount of As in water samples and in a certified reference material (NIST RSM 1643e). Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Graphitic packing removal tool

    Science.gov (United States)

    Meyers, Kurt Edward; Kolsun, George J.

    1997-01-01

    Graphitic packing removal tools for removal of the seal rings in one piece. he packing removal tool has a cylindrical base ring the same size as the packing ring with a surface finish, perforations, knurling or threads for adhesion to the seal ring. Elongated leg shanks are mounted axially along the circumferential center. A slit or slits permit insertion around shafts. A removal tool follower stabilizes the upper portion of the legs to allow a spanner wrench to be used for insertion and removal.

  18. Study of high dose nitrogen implantation into graphite

    International Nuclear Information System (INIS)

    Romanovskij, E.A.; Bespalova, O.V.; Borisov, A.M.; Goryaga, N.G.; Zatekin, V.V.; Kulikauskas, V.S.; Sukharev, V.G.

    1997-01-01

    Rutherford backscattering spectroscopy was used for the study of high dose (35 keV)N + ions implantation into graphites and glassy carbon. Quantitative date on depth profiles and its dependences on irradiation fluence and ion beam flux were obtained for all elements. The stationary cupola-shaped depth profile with maximum nitrogen concentration 22-27% (at.) is reached at sufficiently large fluence. The obtained results are discussed in the frame of high dose implantation models and compared with results of another methods of carbon nitride synthesis

  19. Glass-Graphite Composite Materials

    International Nuclear Information System (INIS)

    Mayzan, M.Z.H.; Lloyd, J.W.; Heath, P.G.; Stennett, M.C.; Hyatt, N.C.; Hand, R.J.

    2016-01-01

    A summary is presented of investigations into the potential of producing glass-composite materials for the immobilisation of graphite or other carbonaceous materials arising from nuclear power generation. The methods are primarily based on the production of base glasses which are subsequently sintered with powdered graphite or simulant TRISO particles. Consideration is also given to the direct preparation of glass-graphite composite materials using microwave technology. Production of dense composite wasteforms with TRISO particles was more successful than with powdered graphite, as wasteforms containing larger amounts of graphite were resistant to densification and the glasses tried did not penetrate the pores under the pressureless conditions used. Based on the results obtained it is concluded that the production of dense glassgraphite composite wasteforms will require the application of pressure. (author)

  20. High-performance liquid chromatography separation of cis-trans anthocyanin isomers from wild Lycium ruthenicum Murr. employing a mixed-mode reversed-phase/strong anion-exchange stationary phase.

    Science.gov (United States)

    Jin, Hongli; Liu, Yanfang; Guo, Zhimou; Yang, Fan; Wang, Jixia; Li, Xiaolong; Peng, Xiaojun; Liang, Xinmiao

    2015-01-21

    The cis-trans isomerism is a common phenomenon for acylated anthocyanins. Nevertheless, few studies reported effective methods for the preparation of isomeric anthocyanins from natural products. In this work, a high-performance liquid chromatography (HPLC) method was developed to efficiently purify anthocyanin isomers from Lycium ruthenicum Murr. based on a mixed-mode reversed-phase/strong anion-exchange column (named XCharge C8SAX). Four commercially available columns were evaluated with a pair of isomeric anthocyanins, and the results demonstrated that the XCharge C8SAX column exhibited improved selectivity and column efficiency for the isomers. The chromatographic parameters, including pH, organic content, and ionic strength, were investigated. Optimal separation quality for the anthocyanin isomers was achieved on the XCharge C8SAX column. Six pure anthocyanins, including two pairs of cis-trans isomeric anthocyanins with one new anthocyanin, were purified from L. ruthenicum and identified. All of the results indicated that this method is an effective way to separate anthocyanins, especially for cis-trans isomers.

  1. Macroscopic Properties of Restacked, Redox-Liquid Exfoliated Graphite and Graphite Mimics Produced in Bulk Quantities

    Energy Technology Data Exchange (ETDEWEB)

    Srivastava, Vikram K [ORNL; Quinlan, Ronald [ORNL; Agapov, Alexander L [ORNL; Dunlap, John R [ORNL; Nelson, Kimberly M [ORNL; Duranty, Edward R [ORNL; Sokolov, Alexei P [ORNL; Bhat, Gajanan [ORNL; Mays, Jimmy [ORNL

    2014-01-01

    The excellent properties exhibited by monolayer graphene have spurred the development of exfoliation techniques using bulk graphite to produce large quantities of pristine monolayer sheets. Development of simple chemistry to exfoliate and intercalate graphite and graphite mimics in large quantities is required for numerous applications. To determine the macroscopic behavior of restacked, exfoliated bulk materials, a systematic approach is presented using a simple, redox-liquid sonication process along to obtain large quantities of 2D and 3D hexagonally layered graphite, molybdenum disulfi de, and boron nitride, which are subsequently characterized to observe chemical and structural changes. For MoS 2 sonicated with the antioxidant sodium bisulfi te, results from Raman spectroscopy, X-ray diffraction, and electron microscopy indicate the presence of distorted phases from different polymorphs, and apparent nanotube structures in the bulk, restacked powder. Furthermore, using thermograviemtric analysis, the antioxidant enhances the resistance to oxidative degradation of MoS 2 , upon thermal treatment up to 900 C. The addition of the ionic antioxidant decreased dispersion stability in non-polar solvent, suggesting decreased compatibility with non-polar systems. Using simple chemical methods, the ability to generate tailored multidimensional layered materials with unique macroscopic properties is critical for numerous applications, including electrical devices, reinforced polymer composites, lithium ion capacitors, and chemical sensing.

  2. Determination of diphenylarsinic acid, phenylarsonic acid and inorganic arsenic in drinking water by graphite-furnace atomic-absorption spectrometry after simultaneous separation and preconcentration with solid-phase extraction disks.

    Science.gov (United States)

    Hagiwara, Kenta; Inui, Tetsuo; Koike, Yuya; Nakamura, Toshihiro

    2013-01-01

    A simple method of graphite-furnace atomic-absorption spectrometry (GFAAS) after solid-phase extraction (SPE) was developed for the determination of diphenylarsinic acid (DPAA), phenylarsonic acid (PAA), and inorganic arsenic (iAs) in drinking water. This method involves the simultaneous collection of DPAA, PAA, and iAs using three stacked SPE disks, i.e., an Empore SDB-XD disk (the upper layer), an activated carbon disk (the middle layer), and a Cation-SR disk loaded with Zr and Ca (ZrCa-CED; the lower layer). A 200-mL aqueous sample was adjusted to pH 3 with nitric acid and passed through the SPE disks at a flow rate of 15 mL min(-1), to concentrate DPAA on the SDB-XD disk, PAA on the activated carbon disk, and iAs on the ZrCa-CED. The As compounds were eluted from the disks with 10 mL of ethanol containing 0.5 mol L(-1) ammonia solution for DPAA, 20 mL of 1 mol L(-1) ammonia solution for PAA, and 20 mL of 6 mol L(-1) hydrochloric acid for iAs. The eluates of DPAA, PAA, and iAs were diluted to 20, 25, and 25 mL, respectively, with deionized water, and then analyzed by GFAAS. The detection limits of As (three-times the standard deviation (n = 3) of the blank values) were 0.13 and 0.16 μg L(-1) at enrichment factors of 10 and 8, respectively, using a 200-mL water sample. Spike tests with 2 μg (10 μg L(-1)) of DPAA, PAA, and iAs in 200 mL of tap water and bottled drinking water showed good recoveries (96.1-103.8%).

  3. Stationary wave patterns in deep water | Doyle | Quaestiones ...

    African Journals Online (AJOL)

    ship" or an obstacle in a stream, is revisited. The wave patterns are calculated using the results of the method of stationary phase. This allows for an elegant geometrical construction in which the reciprocal polar of the wave normal diagram ...

  4. Ceramic Stationary Gas Turbine Development. Technical progress report, April 1, 1993--October 31, 1994

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1994-12-01

    This report summarizes work performed by Solar Technologies Inc. and its subcontractors, during the period April 1, 1993 through October 31, 1994 under Phase II of the DOE Ceramic Stationary Gas Turbine Development program. The objective of the program is to improve the performance of stationary gas turbines in cogeneration through the implementation of selected ceramic components.

  5. Acoustic emission from polycrystalline graphites

    International Nuclear Information System (INIS)

    Ioka, I.; Yoda, S.; Oku, T.; Miyamoto, Y.

    1987-01-01

    Acoustic emission was monitored from polycrystalline graphites with different microstructure (pore size and pore volume) subjected to compressive loading. The graphites used in this study comprised five brands, that is, PGX, ISEM-1, IG-11, IG-15, and ISO-88. A root mean square (RMS) voltage and event counts of acoustic emission for graphites were measured during compressive loading. The acoustic emission was measured using a computed-based data acquisition and analysis system. The graphites were first deformed up to 80 % of the average fracture stress, then unloaded and reloaded again until the fracture occured. During the first loading, the change in RMS voltage for acoustic emission was detected from the initial stage. During the unloading, the RMS voltage became zero level as soon as the applied stress was released and then gradually rose to a peak and declined. The behavior indicated that the reversed plastic deformation occured in graphites. During the second loading, the RMS voltage gently increased until the applied stress exceeded the maximum stress of the first loading; there is no Kaiser effect in the graphites. A bicrystal model could give a reasonable explanation of this results. The empirical equation between the ratio of σ AE to σ f and σ f was obtained. It is considered that the detection of microfracture by the acoustic emission technique is effective in macrofracture prediction of polycrystalline graphites. (author)

  6. Hypervelocity impacts into graphite

    Science.gov (United States)

    Latunde-Dada, S.; Cheesman, C.; Day, D.; Harrison, W.; Price, S.

    2011-03-01

    Studies have been conducted into the characterisation of the behaviour of commercial graphite (brittle) when subjected to hypervelocity impacts by a range of projectiles. The experiments were conducted with a two-stage gas gun capable of launching projectiles of differing density and strength to speeds of about 6kms-1 at right angles into target plates. The damage caused is quantified by measurements of the crater depth and diameters. From the experimental data collected, scaling laws were derived which correlate the crater dimensions to the velocity and the density of the projectile. It was found that for moderate projectile densities the crater dimensions obey the '2/3 power law' which applies to ductile materials.

  7. Radiolytic graphite oxidation revisited

    International Nuclear Information System (INIS)

    Minshall, P.C.; Sadler, I.A.; Wickham, A.J.

    1996-01-01

    The importance of radiolytic oxidation in graphite-moderated CO 2 -cooled reactors has long been recognised, especially in the Advanced Gas-Cooled Reactors where potential rates are higher because of the higher gas pressure and ratings than the earlier Magnox designs. In all such reactors, the rate of oxidation is partly inhibited by the CO produced in the reaction and, in the AGR, further reduced by the deliberate addition of CH 4 . Significant roles are also played by H 2 and H 2 O. This paper reviews briefly the mechanisms of these processes and the data on which they are based. However, operational experience has demonstrated that these basic principles are unsatisfactory in a number of respects. Gilsocarbon graphites produced by different manufacturers have demonstrated a significant difference in oxidation rate despite a similar specification and apparent equivalence in their pore size and distribution, considered to be the dominant influence on oxidation rate for a given coolant-gas composition. Separately, the inhibiting influence of CH 4 , which for many years had been considered to arise from the formation of a sacrificial deposit on the pore walls, cannot adequately be explained by the actual quantities of such deposits found in monitoring samples which frequently contain far less deposited carbon than do samples from Magnox reactors where the only source of such deposits is the CO. The paper also describes the current status of moderator weight-loss predictions for Magnox and AGR Moderators and the validation of the POGO and DIFFUSE6 codes respectively. 2 refs, 5 figs

  8. Graphite reactor physics

    International Nuclear Information System (INIS)

    Bacher, P.; Cogne, F.

    1964-01-01

    The study of graphite-natural uranium power reactor physics, undertaken ten years ago when the Marcoule piles were built, has continued to keep in step with the development of this type of pile. From 1960 onwards the critical facility Marius has been available for a systematic study of the properties of lattices as a function of their pitch, of fuel geometry and of the diameter of cooling channels. This study has covered a very wide field: lattice pitch varying from 19 to 38 cm. uranium rods and tubes of cross-sections from 6 to 35 cm 2 , channels with diameters between 70 and 140 mm. The lattice calculation methods could thus be checked and where necessary adapted. The running of the Marcoule piles and the experiments carried out on them during the last few years have supplied valuable information on the overall evolution of the neutronic properties of the fuel as a function of irradiation. More detailed experiments have also been performed in Marius with plutonium-containing fuels (irradiated or synthetic fuels), and will be undertaken at the beginning of 1965 at high temperature in the critical facility Cesar, which is just being completed at Cadarache. Spent fuel analyses complement these results and help in their interpretation. The thermalization and spectra theories developed in France can thus be verified over the whole valid temperature range. The efficiency of control rods as a function of their dimensions, the materials of which they are made and the lattices surrounding them has been measured in Marius, and the results compared with calculation on the one hand and with the measurements carried out in EDF 1 on the other. Studies on the control proper of graphite piles were concerned essentially with the risks of spatial instability and the means of detecting and controlling them, and with flux distortions caused by the control rods. (authors) [fr

  9. Graphite structure and magnetic parameters of flake graphite cast iron

    Science.gov (United States)

    Vértesy, G.; Uchimoto, T.; Takagi, T.; Tomáš, I.; Kage, H.

    2017-11-01

    Different matrix and graphite morphologies were generated by a special heat treatment in three chemically different series of flake graphite cast iron samples. As cast, furnace cooled and air cooled samples were investigated. The length of graphite particles and the pearlite volume of samples were determined by metallographic examination and these parameters were compared with the nondestructively measured magnetic parameters. Magnetic measurements were performed by the method of Magnetic Adaptive Testing, which is based on systematic measurement and evaluation of minor magnetic hysteresis loops. It was shown that linear correlation existed between the magnetic quantities and the graphite length, and also between the magnetic quantities and the relative pearlite content in the investigated cast iron. A numerical expression was also determined between magnetic descriptors and relative pearlite content, which does not depend on the detailed experimental conditions.

  10. Eutectic solidification mode of spheroidal graphite cast iron and graphitization

    Directory of Open Access Journals (Sweden)

    Hideo Nakae

    2007-02-01

    Full Text Available The shrinkage and chilling tendency of spheroidal graphite (abbreviated SG cast iron is much greater than that of the flake graphite cast iron in spite of its higher amount of C and Si contents. Why? The main reason should be the difference in their graphitization during the eutectic solidification. In this paper, we discuss the difference in the solidification mechanism of both cast irons for solving these problems using unidirectional solidification and the cooling curves of the spheroidal graphite cast iron. The eutectic solidification rate of the SG cast iron is controlled by the diffusion of carbon through the austenite shell, and the final thickness is 1.4 times the radius of the SG, therefore, the reduction of the SG size, namely, the increase in the number, is the main solution of these problems.

  11. Obtention of nuclear grade graphite

    International Nuclear Information System (INIS)

    Ferreira, M.L.

    1984-01-01

    The impurity level of natural graphite found in some of the most important mines of the State of Minas Gerais - Brasil is determined. It is also concerned with the development and use of natural graphite in nuclear reactors. Standard methods for chemical and instrumentsal analysis such as Spectrografic Determination by Emission, Spectrografic Determination by X-Rays, Spectrografic Determination by Atomic Asorption, Photometric Determination, and also chemical and physical methods for separation of impurities as well standard method for Estimating the Thermal Neutron Absorption Cross Section of graphite were employed. Some aditionals methods of purification to the ordinary treatment such as the use of metanol and halogens are also described. (Author) [pt

  12. Production test IP-725, increased graphite temperature limit, F Reactor. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Russell, A.

    1965-12-10

    This report presents the results of a high graphite temperature test conducted at F Reactor from January, through June, 1965. Since the reactor was soon to be permanently shut down, this was believed to be a good opportunity to investigate the effect of increased graphite temperature on graphite stack oxidation with CO{sub 2}, During the first phase of the test, the graphite temperature limit was increased, from 650 C to 700 C for a period of approximately 3 1/2 months. During this phase of the test the actual maximum operating graphite temperature was maintained near the 700 C limit. During the second phase of the test the temperature limit was further increased to 750 C for approximately 2 months. Unfortunately,, the actual graphite operating temperature was maintained at the desired temperature level for only several weeks and thus complicated interpretation of the test results. Throughout the 6 month test period, stack oxidation was monitored with graphite samples inserted in 2 bare process tube channels and by measurement of CO (reaction product of graphite and CO{sub 2}) in the reactor gas atmosphere.

  13. Construção de câmara de luz ultravioleta para fotopolimerização de fases estacionárias monolíticas Coinstruction of ultraviolet-light chamber for monolithic stationary phases photo-polymerization

    Directory of Open Access Journals (Sweden)

    Fernando Antonio Simas Vaz

    2008-01-01

    Full Text Available The assembly of a photochemical reactor with six fluorescent lamps, used for photopolymerizations is described. This chamber presents a mobile support, allowing the placement of samples at different heights and a safety lock that interrupts the radiation, if it is opened during operation. The mirrored internal walls avoid the dispersion and non-uniform distribution of light. There is no high heating because the own character of the used lamps. All parts could be purchased in commerce with less than U$ 150,00. This reactor was successfully used for monolithic stationary phase photopolymerization.

  14. Virtual Stationary Automata for Mobile Networks

    National Research Council Canada - National Science Library

    Dolev, Shlomi; Gilbert, Seth; Lahiani, Limor; Lynch, Nancy; Nolte, Tina

    2005-01-01

    We define a programming abstraction for mobile networks called the Virtual Stationary Automata programming layer, consisting of real mobile clients, virtual timed I/O automata called virtual stationary automata (VSAs...

  15. Metallic Coatings for Graphite/Epoxy Composites

    Science.gov (United States)

    1980-08-01

    Perforated Foil-Coated Graphite/ Epoxy Panel .............. ........................... 4-6 4-4 Two-In. -Diameter 5052 Aluminum Alloy Repair Patch...The Phase I L i4-1 I1 evaluation indicated a need for a more corrosion-resistant aluminum alloy . The coating system selected was 0.0019-in. -thick 5052 ...application techniques on moisture resistance. The selected foil was 0.0025 in.-thick, 5052 aluminum alloy perforated with 0.010-in.-dlameter holes at a

  16. Stationary measure in the multiverse

    Energy Technology Data Exchange (ETDEWEB)

    Linde, Andrei [Department of Physics, Stanford University, Stanford, CA 94305 (United States); Vanchurin, Vitaly; Winitzki, Sergei, E-mail: alinde@stanford.edu, E-mail: vitaly@cosmos2.phy.tufts.edu, E-mail: winitzki@physik.uni-muenchen.de [Department of Physics, Ludwig-Maximilians University, Munich (Germany)

    2009-01-15

    We study the recently proposed ''stationary measure'' in the context of the string landscape scenario. We show that it suffers neither from the ''Boltzmann brain'' problem nor from the ''youngness'' paradox that makes some other measures predict a high CMB temperature at present. We also demonstrate a good performance of this measure in predicting the results of local experiments, such as proton decay.

  17. A stationary q-metric

    Science.gov (United States)

    Toktarbay, S.; Quevedo, H.

    2014-10-01

    We present a stationary generalization of the static $q-$metric, the simplest generalization of the Schwarzschild solution that contains a quadrupole parameter. It possesses three independent parameters that are related to the mass, quadrupole moment and angular momentum. We investigate the geometric and physical properties of this exact solution of Einstein's vacuum equations, and show that it can be used to describe the exterior gravitational field of rotating, axially symmetric, compact objects.

  18. CALANDRIA TYPE SODIUM GRAPHITE REACTOR

    Science.gov (United States)

    Peterson, R.M.; Mahlmeister, J.E.; Vaughn, N.E.; Sanders, W.J.; Williams, A.C.

    1964-02-11

    A sodium graphite power reactor in which the unclad graphite moderator and fuel elements are contained within a core tank is described. The core tank is submersed in sodium within the reactor vessel. Extending longitudinally through the core thnk are process tubes with fuel elements positioned therein. A bellows sealing means allows axial expansion and construction of the tubes. Within the core tank, a leakage plenum is located below the graphite, and above the graphite is a gas space. A vent line regulates the gas pressure in the space, and another line removes sodium from the plenum. The sodium coolant flows from the lower reactor vessel through the annular space between the fuel elements and process tubes and out into the reactor vessel space above the core tank. From there, the heated coolant is drawn off through an outlet line and sent to the heat exchange. (AEC)

  19. Graphite oxidation in HTGR atmosphere

    International Nuclear Information System (INIS)

    Growcock, F.B.; Barry, J.J.; Finfrock, C.C.; Rivera, E.; Heiser, J.H. III

    1982-01-01

    On-going and recently completed studies of the effect of thermal oxidation on the structural integrity of HTGR candidate graphites are described, and some results are presented and discussed. This work includes the study of graphite properties which may play decisive roles in the graphites' resistance to oxidation and fracture: pore size distribution, specific surface area and impurity distribution. Studies of strength loss mechanisms in addition to normal oxidation are described. Emphasis is placed on investigations of the gas permeability of HTGR graphites and the surface burnoff phenomenon observed during recent density profile measurements. The recently completed studies of catalytic pitting and the effects of prestress and stress on reactivity and ultimate strength are also discussed

  20. Graphite surveillance in N Reactor

    International Nuclear Information System (INIS)

    Woodruff, E.M.

    1991-09-01

    Graphite dimensional changes in N Reactor during its 24 yr operating history are reviewed. Test irradiation results, block measurements, stack profiles, top of reflector motion monitors, and visual observations of distortion are described. 18 refs., 14 figs., 1 tab

  1. Graphite materials for nuclear reactors

    International Nuclear Information System (INIS)

    Oku, Tatsuo

    1991-01-01

    Graphite materials have been used in the nuclear fission reactors from the beginning of the reactor development for the speed reduction and reflection of neutron. Graphite materials are used both as a moderator and as a reflector in the core of high temperature gas-cooled reactors, and both as a radiation shielding material and as a reflector in the surrounding of the core for the fast breeder reactor. On the other hand, graphite materials are being positively used as a first wall of plasma as it is known that low Z materials are useful for holding high temperature plasma in the nuclear fusion devices. In this paper the present status of the application of graphite materials to the nuclear fission reactors and fusion devices (reactors) is presented. In addition, a part of results on the related properties to the structural design and safety evaluation and results examined on the subjects that should be done in the future are also described. (author)

  2. Measurement of thermal stress in graphite intercalated with bromine

    Energy Technology Data Exchange (ETDEWEB)

    Chung, D.D.L.; Wong, L.W.

    1988-03-01

    The thermal stress of graphite intercalated with bromine was found to increase from zero at about 100/degree/C to about 1.3 MPa at 200/degree/C. The effect was reversible with hysteresis. The thermal stress increase had a sharp temperature dependence due to its association with the exfoliation phase transition.

  3. Graphite formation in cast iron, phase 2

    Science.gov (United States)

    Stefanescu, D. M.; Fiske, M. R.

    1985-01-01

    Several types of cast irons are directionally solidified aboard the KC-135 aircraft. Also, control samples are run on Earth for comparison. Some of these samples are unusable because of various mechanical problems; the analysis and the interpretation of results on the samples that are run successfully is discussed.

  4. Graphite oral tattoo: case report

    OpenAIRE

    Moraes, Renata Mendonça; Gouvêa Lima, Gabriela de Morais; Guilhermino, Marinaldo; Vieira, Mayana Soares; Carvalho, Yasmin Rodarte; Anbinder, Ana Lia

    2015-01-01

    Pigmented oral lesions compose a large number of pathological entities, including exogenous pigmentat oral tattoos, such as amalgam and graphite tattoos. We report a rare case of a graphite tattoo on the palate of a 62-year-old patient with a history of pencil injury, compare it with amalgam tattoos, and determine the prevalence of oral tattoos in our Oral Pathology Service. We also compare the clinical and histological findings of grafite and amalgam tattoos. Oral tattoos affect women more f...

  5. Graphitic carbon nitride nanofibers in seaweed-like architecture for gas chromatographic separations.

    Science.gov (United States)

    Zheng, Yunzhong; Han, Qing; Qi, Meiling; Qu, Liangti

    2017-05-05

    Seaweed-like graphitic carbon nitride (g-C 3 N 4 ) has a unique porous architecture composed of interlocking g-C 3 N 4 nanofibers (NF-C 3 N 4 ) with much higher surface area than bulk g-C 3 N 4 and shows good potential in separation science. This work investigated the separation performance of NF-C 3 N 4 as stationary phase for capillary gas chromatographic (GC) separations. The NF-C 3 N 4 column exhibits weak polarity and high column efficiency of 4728 plates/m for n-dodecane. Importantly, it displays good separation performance for a wide range of analytes and shows different retention behaviors from the bulk g-C 3 N 4 column and commercial HP-5MS column with 5% phenylpolysiloxane. Particularly, it shows high resolving capability for both aliphatic and aromatic isomers. In addition, NF-C 3 N 4 column has high thermal stability up to 280°C and good separation repeatability with relative standard deviation (RSD) values in the range of 0.29-0.61% for intra-day, 0.56-1.1% for inter-day and 2.0-4.9% for between-column, respectively. Moreover, it was applied for the determination of isomer impurities in real samples, showing good potential in GC applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Experience with graphite in JET

    International Nuclear Information System (INIS)

    Pick, M.A.; Celentano, G.; Deksnis, E.; Dietz, K.J.; Shaw, R.; Sonnenberg, K.; Walravens, M.

    1987-01-01

    During the current operational period of JET more than 50% of the internal area of the machine is covered in graphite tiles. This includes the 15 m 2 of carbon tiles installed in the new toroidal limiter, the 40 poloidal belts of graphite tiles covering the U-joints and bellows as well as a two metre high ring (-- 20 m 2 ) or carbon tiles on the inner wall of the Torus. A ring of tiles in the equatorial plane (3 tiles high) consists of carbon-carbon fibre tiles. Test bed results indicated that the fine grained graphite tiles cracked at ∼ 1 kW/cm 2 for 2s of irradiation whereas the carbon-carbon fibre tiles were able to sustain a flux, limited by the irradiation facility, of 3.5 kW for 3s without any damage. The authors report on the generally positive experience they have had had with the installed graphite during the present and previous in-vessel configurations. This includes the physical integrity of the tiles under severe conditions such as high energy run-away electron beams, plasma disruptions and high heat fluxes. They report on the importance of the precise positioning of the inner wall and x-point tiles at the very high power fluxes of JET and the effect of deviations on both graphite and carbon-fibre tiles

  7. Computer simulation of the steam--graphite reaction under isothermal and steady-state conditions

    International Nuclear Information System (INIS)

    Joy, D.S.; Stem, S.C.

    1975-05-01

    A mathematical model was formulated to describe the isothermal, steady-state diffusion and reaction of steam in a graphite matrix. A generalized Langmuir-Hinshelwood equation is used to represent the steam-graphite reaction rate. The model also includes diffusion in the gas phase adjacent to the graphite matrix. A computer program, written to numerically integrate the resulting differential equations, is described. The coupled nonlinear differential equations in the graphite phase are solved using the IBM Continuous System Modeling Program. Classical finite difference techniques are used for the gas-phase calculations. An iterative procedure is required to couple the two sets of calculations. Several sample problems are presented to demonstrate the utility of the model. (U.S.)

  8. Anatomy of successive helium-shell flashes: Stationary shell burning

    International Nuclear Information System (INIS)

    Sackmann, I.

    1980-01-01

    For successive helium-shell flashes, the amounts of helium and hydrogen burned were computed over the peak flash phase, over the total flash cycle, and over the quiet, interflash phase. It was found that the frequently made assumption of stationary shell burning is violated by the helium-shell flash for the first few flashes; here, over a total flash cycle, the helium-burning shell always progresses considerably faster outward than the hydrogen-burning shell. However, after about 15 flashes, coincident with the leveling out of the peaks of the helium shell, agreement with stationary shell burning is attained, both for the 3 M/sub sun/ and 6 M/sub sun/ cases

  9. Stationary analysis of signals and ratio decay determination in BWR type reactors by neuronal network

    International Nuclear Information System (INIS)

    Sanchis, R.; Palomo, M. J.; Munoz-Cobo, J. L.

    1998-01-01

    The signals registered in the nuclear plants have non stationary characteristics, in numerous times. This made difficult the application of the methods of analysis. There are determinate temporal intervals in that the signal is stationary with determinate mean, value together of zones with corrupt registers, and other zones with mean value distinct, but stationary during a temporal interval. The methodology consist in a stationary analysis to the signal received of the nuclear plant. With the Gabor Transformation are determined the temporal intervals of the stationary signals, synthesised it, as previous phase to the application of the methods of the analysis of stability parameters with methods ARMA, SVD, Neural Net,... to the reconstructed signal. 4 refs. (Author)

  10. Mechanical properties of graphites and carbon materials

    International Nuclear Information System (INIS)

    Jouquet, Gilbert.

    1977-01-01

    The mechanical behavior of graphites and artificial carbons is related to the structure of these materials. The influence of structural modifications in a graphite monocrystal on the deformation and fracture properties is studied [fr

  11. One-sided asymptotically mean stationary channels

    OpenAIRE

    Simon, Francois

    2014-01-01

    This paper proposes an analysis of asymptotically mean stationary (AMS) communication channels. A hierarchy based on stability properties (stationarity, quasi-stationarity, recurrence and asymptotically mean stationarity) of channels is identified. Stationary channels are a subclass of quasi-stationary channels which are a subclass of recurrent AMS channels which are a subclass of AMS channels. These classes are proved to be stable under Markovian composition of channels (e.g., the cascade of...

  12. RECOVERY OF VALUABLE MATERIAL FROM GRAPHITE BODIES

    Science.gov (United States)

    Fromm, L.W. Jr.

    1959-09-01

    An electrolytic process for recovering uranium from a graphite fuel element is described. The uraniumcontaining graphite body is disposed as the anode of a cell containing a nitric acid electrolyte and a 5 amp/cm/sup 2/ current passed to induce a progressive disintegration of the graphite body. The dissolved uranium is quickly and easily separated from the resulting graphite particles by simple mechanical means, such as centrifugation, filtration, and decontamination.

  13. On the ''memory'' effect and its relation to the mechanism of formation of mercury-graphite electrode in inversion voltammetry

    International Nuclear Information System (INIS)

    Nejman, E.Ya.; Petrova, L.G.; Dolgopolova, G.M.; Ignatov, V.I.

    1977-01-01

    Simultaneous discharge ionization of lead-copper and cadmium-copper systems on the surface of mercury-plated graphite and graphite electrodes has been studied. A model is suggested of the preparation process of a mercury-plated graphite electrode obtained in simultaneous electroposition of mercury and elements determined as microimpurities. Processes, which occur on the electrode during relaxation time between electrolysis beginning and formation of the mercury phase, may be probable reasons for mutual effects of elements of the mercury-plated graphite electrode

  14. Condensational theory of stationary tornadoes

    International Nuclear Information System (INIS)

    Makarieva, A.M.; Gorshkov, V.G.; Nefiodov, A.V.

    2011-01-01

    Using the Bernoulli integral for air streamline with condensing water vapor a stationary axisymmetric tornado circulation is described. The obtained profiles of vertical, radial and tangential velocities are in agreement with observations for the Mulhall tornado, world's largest on record and longest-lived among the three tornadoes for which 3D velocity data are available. Maximum possible vortex velocities are estimated. -- Highlights: → Water vapor condensation causes a logarithmic drop of air pressure towards tornado center. → The first ever theoretical description of tornado velocities is obtained. → The maximum vortex velocity grows logarithmically with decreasing tornado eye radius. → Air motion with high velocities can only develop in sufficiently large condensation areas.

  15. Residual stress measurements in polycrystalline graphite with micro-Raman spectroscopy

    International Nuclear Information System (INIS)

    Krishna, Ram; Jones, Abbie N.; Edge, Ruth; Marsden, Barry J.

    2015-01-01

    Micro-Raman microscopy technique is applied to evaluate unevenly distributed residual stresses in the various constituents of polygranular reactor grades graphite. The wavenumber based Raman shift (cm −1 ) corresponds to the local residual stress and measurements of stress dependent first order Raman spectra in graphite have enabled localized residual stress values to be determined. The bulk polygranular graphite of reactor grades – Gilsocarbon, NBG-18 and PGA – are examined to illustrate the residual stress variations in their constituents. Binder phase and filler particles have shown to be under compressive and tensile stresses, respectively. Among the studied graphite grades, the binder phase in Gilsocarbon has the highest residual stress and NBG-18 has the lowest value. Filler particles in Gilsocarbon have the highest residual stress and PGA showed the lowest, this is most likely due to the morphology of the coke particles used in the manufacturing and applied processing techniques for fabrications. Stresses have also been evaluated along the peripheral of pores and at the tips of the cracks. Cracks in filler and binder phases have shown mixed behaviour, compressive as well as tensile, whereas pores in binder and filler particles have shown compressive behaviour. The stresses in these graphitic constituents are of the order of MPa. Non-destructive analyses presented in this study make the current state-of-the-art technique a powerful method for the study of stress variations near the graphite surface and are expected to increase its use further in property determination analysis of low to highly fluence irradiated graphite samples from the material test reactors. - Highlights: • Micro-Raman spectroscopy can measure significantly small residual stresses. • Gilsocarbon, NBG-18 and PGA graphite were evaluated for residual stresses. • Residual stresses in the constituents of graphite were evaluated. • Binder and filler particles are often found under

  16. Superconductivity in graphite intercalation compounds

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Robert P. [Cavendish Laboratory, University of Cambridge, Madingley Road, Cambridge CB3 0HE (United Kingdom); Weller, Thomas E.; Howard, Christopher A. [Department of Physics & Astronomy, University College of London, Gower Street, London WCIE 6BT (United Kingdom); Dean, Mark P.M. [Department of Condensed Matter Physics and Materials Science, Brookhaven National Laboratory, Upton, NY 11973 (United States); Rahnejat, Kaveh C. [Department of Physics & Astronomy, University College of London, Gower Street, London WCIE 6BT (United Kingdom); Saxena, Siddharth S. [Cavendish Laboratory, University of Cambridge, Madingley Road, Cambridge CB3 0HE (United Kingdom); Ellerby, Mark, E-mail: mark.ellerby@ucl.ac.uk [Department of Physics & Astronomy, University College of London, Gower Street, London WCIE 6BT (United Kingdom)

    2015-07-15

    Highlights: • Historical background of graphite intercalates. • Superconductivity in graphite intercalates and its place in the field of superconductivity. • Recent developments. • Relevant modeling of superconductivity in graphite intercalates. • Interpretations that pertain and questions that remain. - Abstract: The field of superconductivity in the class of materials known as graphite intercalation compounds has a history dating back to the 1960s (Dresselhaus and Dresselhaus, 1981; Enoki et al., 2003). This paper recontextualizes the field in light of the discovery of superconductivity in CaC{sub 6} and YbC{sub 6} in 2005. In what follows, we outline the crystal structure and electronic structure of these and related compounds. We go on to experiments addressing the superconducting energy gap, lattice dynamics, pressure dependence, and how these relate to theoretical studies. The bulk of the evidence strongly supports a BCS superconducting state. However, important questions remain regarding which electronic states and phonon modes are most important for superconductivity, and whether current theoretical techniques can fully describe the dependence of the superconducting transition temperature on pressure and chemical composition.

  17. Thermodynamic Simulation of Equilibrium Composition of Reaction Products at Dehydration of a Technological Channel in a Uranium-Graphite Reactor

    Science.gov (United States)

    Pavliuk, A. O.; Zagumennov, V. S.; Kotlyarevskiy, S. G.; Bespala, E. V.

    2018-01-01

    The problems of accumulation of nuclear fuel spills in the graphite stack in the course of operation of uranium-graphite nuclear reactors are considered. The results of thermodynamic analysis of the processes in the graphite stack at dehydration of a technological channel, fuel element shell unsealing and migration of fission products, and activation of stable nuclides in structural elements of the reactor and actinides inside the graphite moderator are given. The main chemical reactions and compounds that are produced in these modes in the reactor channel during its operation and that may be hazardous after its shutdown and decommissioning are presented. Thermodynamic simulation of the equilibrium composition is performed using the specialized code TERRA. The results of thermodynamic simulation of the equilibrium composition in different cases of technological channel dehydration in the course of the reactor operation show that, if the temperature inside the active core of the nuclear reactor increases to the melting temperature of the fuel element, oxides and carbides of nuclear fuel are produced. The mathematical model of the nonstationary heat transfer in a graphite stack of a uranium-graphite reactor in the case of the technological channel dehydration is presented. The results of calculated temperature evolution at the center of the fuel element, the replaceable graphite element, the air gap, and in the surface layer of the block graphite are given. The numerical results show that, in the case of dehydration of the technological channel in the uranium-graphite reactor with metallic uranium, the main reaction product is uranium dioxide UO2 in the condensed phase. Low probability of production of pyrophoric uranium compounds (UH3) in the graphite stack is proven, which allows one to disassemble the graphite stack without the risk of spontaneous graphite ignition in the course of decommissioning of the uranium-graphite nuclear reactor.

  18. Investigation of carbon near the graphite-diamond-liquid triple point

    International Nuclear Information System (INIS)

    Prawer, S.; Jamieson, D.N.

    1992-01-01

    Pulsed laser irradiation is used to heat deeply buried damage layers in diamond. Over a small range of laser powers, damage annealing, formation of buried graphitic layers, and melting of diamond followed by its conversion upon cooling into graphite are observed. The diagnostics employed are Channeling Contrast Microscopy, optical absorption, surface profilometry, and scanning and optical microscopies. The results are explained in terms of the behaviour of carbon under high internal pressures close to the diamond-graphite-liquid carbon triple point in the phase diagram. 17 refs., 3 figs

  19. Graphite nanoreinforcements in polymer nanocomposites

    Science.gov (United States)

    Fukushima, Hiroyuki

    Nanocomposites composed of polymer matrices with clay reinforcements of less than 100 nm in size, are being considered for applications such as interior and exterior accessories for automobiles, structural components for portable electronic devices, and films for food packaging. While most nanocomposite research has focused on exfoliated clay platelets, the same nanoreinforcement concept can be applied to another layered material, graphite, to produce nanoplatelets and nanocomposites. Graphite is the stiffest material found in nature (Young's Modulus = 1060 GPa), having a modulus several times that of clay, but also with excellent electrical and thermal conductivity. The key to utilizing graphite as a platelet nanoreinforcement is in the ability to exfoliate this material. Also, if the appropriate surface treatment can be found for graphite, its exfoliation and dispersion in a polymer matrix will result in a composite with not only excellent mechanical properties but electrical properties as well, opening up many new structural applications as well as non-structural ones where electromagnetic shielding and high thermal conductivity are requirements. In this research, a new process to fabricate exfoliated nano-scale graphite platelets was established (Patent pending). The size of the resulted graphite platelets was less than 1 um in diameter and 10 nm in thickness, and the surface area of the material was around 100 m2/g. The reduction of size showed positive effect on mechanical properties of composites because of the increased edge area and more functional groups attached with it. Also various surface treatment techniques were applied to the graphite nanoplatelets to improve the surface condition. As a result, acrylamide grafting treatment was found to enhance the dispersion and adhesion of graphite flakes in epoxy matrices. The resulted composites showed better mechanical properties than those with commercially available carbon fibers, vapor grown carbon fibers

  20. Seismic Study of TMSR Graphite Core Structure

    International Nuclear Information System (INIS)

    Tsang, Derek; Huang Chao Chao

    2014-01-01

    Graphite plays an important role in the thorium based molten salt reactor (TMSR) nuclear energy system. The graphite core acts as reflector, moderator and structural material in the TMSR core. The graphite core assembly has hundreds of graphite bricks interconnected with graphite keys and dowels. In other words, the graphite core is a kind of discrete stack structure with highly nonlinear dynamic behaviour, and it will show totally different dynamics responses comparing with welded structure or bolted structure when subjected to the seismic loading. Hence it is important to investigate the dynamics characteristics of the TMSR graphite core assembly and to meet the seismic design requirement. The most popular way to investigate the nonlinearity of graphite core is to do finite element analyses. Due to the large number of nonlinear behaviour caused by contacts, collisions and impacts between the graphite bricks and keys, the computational costs on seismic analysis of the whole core would be very high. Many methods have been developed in the past 20 years to conquer this difficulty. In this work substructure method and finite element method have been used to study the dynamic behaviour of a stack of graphite bricks under seismic loading. The numerical results of these two methods will be compared. The results show that the super element method is an efficient method for graphite core seismic analyses. (author)

  1. AGC-2 Graphite Preirradiation Data Package

    Energy Technology Data Exchange (ETDEWEB)

    David Swank; Joseph Lord; David Rohrbaugh; William Windes

    2012-10-01

    The NGNP Graphite R&D program is currently establishing the safe operating envelope of graphite core components for a Very High Temperature Reactor (VHTR) design. The program is generating quantitative data necessary for predicting the behavior and operating performance of the new nuclear graphite grades. To determine the in-service behavior of the graphite for pebble bed and prismatic designs, the Advanced Graphite Creep (AGC) experiment is underway. This experiment is examining the properties and behavior of nuclear grade graphite over a large spectrum of temperatures, neutron fluences and compressive loads. Each experiment consists of over 400 graphite specimens that are characterized prior to irradiation and following irradiation. Six experiments are planned with the first, AGC-1, currently being irradiated in the Advanced Test Reactor (ATR) and pre-irradiation characterization of the second, AGC-2, completed. This data package establishes the readiness of 512 specimens for assembly into the AGC-2 capsule.

  2. Voronoi-Tessellated Graphite Produced by Low-Temperature Catalytic Graphitization from Renewable Resources.

    Science.gov (United States)

    Zhao, Leyi; Zhao, Xiuyun; Burke, Luke T; Bennett, J Craig; Dunlap, Richard A; Obrovac, Mark N

    2017-09-11

    A highly crystalline graphite powder was prepared from the low temperature (800-1000 °C) graphitization of renewable hard carbon precursors using a magnesium catalyst. The resulting graphite particles are composed of Voronoi-tessellated regions comprising irregular sheets; each Voronoi-tessellated region having a small "seed" particle located near their centroid on the surface. This suggests nucleated outward growth of graphitic carbon, which has not been previously observed. Each seed particle consists of a spheroidal graphite shell on the inside of which hexagonal graphite platelets are perpendicularly affixed. This results in a unique high surface area graphite with a high degree of graphitization that is made with renewable feedstocks at temperatures far below that conventionally used for artificial graphites. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Progress in radioactive graphite waste management

    International Nuclear Information System (INIS)

    2010-07-01

    Radioactive graphite constitutes a major waste stream which arises during the decommissioning of certain types of nuclear installations. Worldwide, a total of around 250 000 tonnes of radioactive graphite, comprising graphite moderators and reflectors, will require management solutions in the coming years. 14 C is the radionuclide of greatest concern in nuclear graphite; it arises principally through the interaction of reactor neutrons with nitrogen, which is present in graphite as an impurity or in the reactor coolant or cover gas. 3 H is created by the reactions of neutrons with 6 Li impurities in graphite as well as in fission of the fuel. 36 Cl is generated in the neutron activation of chlorine impurities in graphite. Problems in the radioactive waste management of graphite arise mainly because of the large volumes requiring disposal, the long half-lives of the main radionuclides involved and the specific properties of graphite - such as stored Wigner energy, graphite dust explosibility and the potential for radioactive gases to be released. Various options for the management of radioactive graphite have been studied but a generally accepted approach for its conditioning and disposal does not yet exist. Different solutions may be appropriate in different cases. In most of the countries with radioactive graphite to manage, little progress has been made to date in respect of the disposal of this material. Only in France has there been specific thinking about a dedicated graphite waste-disposal facility (within ANDRA): other major producers of graphite waste (UK and the countries of the former Soviet Union) are either thinking in terms of repository disposal or have no developed plans. A conference entitled 'Solutions for Graphite Waste: a Contribution to the Accelerated Decommissioning of Graphite Moderated Nuclear Reactors' was held at the University of Manchester 21-23 March 2007 in order to stimulate progress in radioactive graphite waste management

  4. Graphite structure and magnetic parameters of flake graphite cast iron

    Czech Academy of Sciences Publication Activity Database

    Vértesy, G.; Uchimoto, T.; Takagi, T.; Tomáš, Ivan; Kage, H.

    2017-01-01

    Roč. 442, Nov (2017), s. 397-402 ISSN 0304-8853 R&D Projects: GA ČR GB14-36566G Institutional support: RVO:68378271 Keywords : magnetic NDE * magnetic adaptive testing * cast iron * graphite structure * pearlite content Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 2.630, year: 2016

  5. Bainitic high-strength cast iron with globular graphite

    Science.gov (United States)

    Silman, G. I.; Makarenko, K. V.; Kamynin, V. V.; Zentsova, E. A.

    2013-07-01

    Special features of formation of bainitic structures in grayed cast irons are considered. The influence of the graphite phase and of the special features of chemical composition of the iron on the intermediate transformation in high-carbon alloys is allowed for. The range of application of high-strength cast irons with bainitic structure is determined. The paper is the last and unfinished work of G. I. Silman completed by his disciples as a tribute to their teacher.

  6. Graphite moderated 252Cf source

    International Nuclear Information System (INIS)

    Sajo B, L.; Barros, H.; Greaves, E. D.; Vega C, H. R.

    2014-08-01

    The thorium molten salt reactor is an attractive and affordable nuclear power option for developing countries with insufficient infrastructure and limited technological capability. In the aim of personnel training and experience gathering at the Universidad Simon Bolivar there is in progress a project of developing a subcritical thorium liquid fuel reactor. The neutron source to run this subcritical reactor is a 252 Cf source and the reactor will use high-purity graphite as moderator. Using the MCNP5 code the neutron spectra of the 252 Cf in the center of the graphite moderator has been estimated along the channel where the liquid thorium salt will be inserted; also the ambient dose equivalent due to the source has been determined around the moderator. (Author)

  7. Investigation of porous graphitic carbon for triterpenoids and natural resinous materials analysis by high performance liquid chromatography hyphenated to mass spectrometry.

    Science.gov (United States)

    Rhourri-Frih, B; Chaimbault, P; Dequeral, D; André, P; Lafosse, M

    2012-06-01

    Natural resinous materials are mainly composed of pentacyclic triterpenes which exhibit a large number of interesting medicinal activities. However, the presence of numerous isomers within the active substances makes their screening by HPLC very challenging. Porous graphitic carbon was investigated as stationary phase to achieve triterpenes isomers separation. The influence of various parameters (temperature, formic acid concentration and mobile phase composition) on the retention was considered. A usual decrease of the retention of triterpenes was observed with the increase of the temperature. Therefore, separation in resinous materials was performed at 25°C. Acetonitrile-isopropanol mixture was chosen as mobile phase in gradient elution and leads to the best compromise between efficiency and high resolution. The lack of chromophore groups in the pentacyclic triterpenes structures required the use of mass spectrometry detection. Moreover, atmospheric pressure photo-ionisation mass spectrometry prevents compounds fragmentation which was helpful for spectra interpretation and compounds identification. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. AGC-3 Graphite Preirradiation Data Analysis Report

    Energy Technology Data Exchange (ETDEWEB)

    William Windes; David Swank; David Rohrbaugh; Joseph Lord

    2013-09-01

    This report describes the specimen loading order and documents all pre-irradiation examination material property measurement data for the graphite specimens contained within the third Advanced Graphite Capsule (AGC-3) irradiation capsule. The AGC-3 capsule is third in six planned irradiation capsules comprising the Advanced Graphite Creep (AGC) test series. The AGC test series is used to irradiate graphite specimens allowing quantitative data necessary for predicting the irradiation behavior and operating performance of new nuclear graphite grades to be generated which will ascertain the in-service behavior of the graphite for pebble bed and prismatic Very High Temperature Reactor (VHTR) designs. The general design of AGC-3 test capsule is similar to the AGC-2 test capsule, material property tests were conducted on graphite specimens prior to loading into the AGC-3 irradiation assembly. However the 6 major nuclear graphite grades in AGC-2 were modified; two previous graphite grades (IG-430 and H-451) were eliminated and one was added (Mersen’s 2114 was added). Specimen testing from three graphite grades (PCEA, 2114, and NBG-17) was conducted at Idaho National Laboratory (INL) and specimen testing for two grades (IG-110 and NBG-18) were conducted at Oak Ridge National Laboratory (ORNL) from May 2011 to July 2013. This report also details the specimen loading methodology for the graphite specimens inside the AGC-3 irradiation capsule. The AGC-3 capsule design requires "matched pair" creep specimens that have similar dose levels above and below the neutron flux profile mid-plane to provide similar specimens with and without an applied load. This document utilized the neutron flux profile calculated for the AGC-3 capsule design, the capsule dimensions, and the size (length) of the selected graphite and silicon carbide samples to create a stacking order that can produce "matched pairs" of graphite samples above and below the AGC-3 capsule elevation mid-point to

  9. Preparation and characterization of dense graphite/glassy carbon composite coating for sealing application

    Science.gov (United States)

    Wang, Yang; Chen, Zhaofeng; Yu, Shengjie; Pan, Ning; Liao, Jiahao

    2017-09-01

    Glassy carbon (GC), characterized by a homogeneous structure and glass-like fracture surface once broken, has attracted increasing attention because of its excellent performance. In this paper, a dense graphite/glassy carbon composite coating with low gas permeability was introduced. In this composite coating, small graphite particles acting as second phase were wrapped by glassy carbon matrix. The composite coatings with different mass fractions of graphite particles were prepared. The mass loss of phenolic resin was determined by TG (thermogravimetry) analysis to determine the pyrolysis process. Raman spectrum analysis indicates that graphite content in composite coatings affected the G/D ratio significantly. The permeability of composite coatings with 50% and 100% graphite particles was almost same, which was ranged from 6  ×  10-13 m3 · µm/m2 · s · Pa to 3  ×  10-13 m3 · µm/m2 · s · Pa within the differential pressure from 100 kPa to 70 kPa. While the composite coating with 150% graphite particles had higher gas permeability due to the tiny micro-cracks and micro-pores produced. What was more, the densification mechanism of graphite/glassy carbon composite coating was also discussed in detail.

  10. Quenchable compressed graphite synthesized from neutron-irradiated highly oriented pyrolytic graphite in high pressure treatment at 1500 °C

    Science.gov (United States)

    Niwase, Keisuke; Terasawa, Mititaka; Honda, Shin-ichi; Niibe, Masahito; Hisakuni, Tomohiko; Iwata, Tadao; Higo, Yuji; Hirai, Takeshi; Shinmei, Toru; Ohfuji, Hiroaki; Irifune, Tetsuo

    2018-04-01

    The super hard material of "compressed graphite" (CG) has been reported to be formed under compression of graphite at room temperature. However, it returns to graphite under decompression. Neutron-irradiated graphite, on the other hand, is a unique material for the synthesis of a new carbon phase, as reported by the formation of an amorphous diamond by shock compression. Here, we investigate the change of structure of highly oriented pyrolytic graphite (HOPG) irradiated with neutrons to a fluence of 1.4 × 1024 n/m2 under static pressure. The neutron-irradiated HOPG sample was compressed to 15 GPa at room temperature and then the temperature was increased up to 1500 °C. X-ray diffraction, high-resolution transmission electron microscopy on the recovered sample clearly showed the formation of a significant amount of quenchable-CG with ordinary graphite. Formation of hexagonal and cubic diamonds was also confirmed. The effect of irradiation-induced defects on the synthesis of quenchable-CG under high pressure and high temperature treatment was discussed.

  11. Environmentally benign graphite intercalation compound composition for exfoliated graphite, flexible graphite, and nano-scaled graphene platelets

    Energy Technology Data Exchange (ETDEWEB)

    Zhamu, Aruna; Jang, Bor Z.

    2014-06-17

    A carboxylic-intercalated graphite compound composition for the production of exfoliated graphite, flexible graphite, or nano-scaled graphene platelets. The composition comprises a layered graphite with interlayer spaces or interstices and a carboxylic acid residing in at least one of the interstices, wherein the composition is prepared by a chemical oxidation reaction which uses a combination of a carboxylic acid and hydrogen peroxide as an intercalate source. Alternatively, the composition may be prepared by an electrochemical reaction, which uses a carboxylic acid as both an electrolyte and an intercalate source. Exfoliation of the invented composition does not release undesirable chemical contaminants into air or drainage.

  12. Pyrolytic graphite gauge for measuring heat flux

    Science.gov (United States)

    Bunker, Robert C. (Inventor); Ewing, Mark E. (Inventor); Shipley, John L. (Inventor)

    2002-01-01

    A gauge for measuring heat flux, especially heat flux encountered in a high temperature environment, is provided. The gauge includes at least one thermocouple and an anisotropic pyrolytic graphite body that covers at least part of, and optionally encases the thermocouple. Heat flux is incident on the anisotropic pyrolytic graphite body by arranging the gauge so that the gauge surface on which convective and radiative fluxes are incident is perpendicular to the basal planes of the pyrolytic graphite. The conductivity of the pyrolytic graphite permits energy, transferred into the pyrolytic graphite body in the form of heat flux on the incident (or facing) surface, to be quickly distributed through the entire pyrolytic graphite body, resulting in small substantially instantaneous temperature gradients. Temperature changes to the body can thereby be measured by the thermocouple, and reduced to quantify the heat flux incident to the body.

  13. Uranium Oxide Aerosol Transport in Porous Graphite

    Energy Technology Data Exchange (ETDEWEB)

    Blanchard, Jeremy; Gerlach, David C.; Scheele, Randall D.; Stewart, Mark L.; Reid, Bruce D.; Gauglitz, Phillip A.; Bagaasen, Larry M.; Brown, Charles C.; Iovin, Cristian; Delegard, Calvin H.; Zelenyuk, Alla; Buck, Edgar C.; Riley, Brian J.; Burns, Carolyn A.

    2012-01-23

    The objective of this paper is to investigate the transport of uranium oxide particles that may be present in carbon dioxide (CO2) gas coolant, into the graphite blocks of gas-cooled, graphite moderated reactors. The transport of uranium oxide in the coolant system, and subsequent deposition of this material in the graphite, of such reactors is of interest because it has the potential to influence the application of the Graphite Isotope Ratio Method (GIRM). The GIRM is a technology that has been developed to validate the declared operation of graphite moderated reactors. GIRM exploits isotopic ratio changes that occur in the impurity elements present in the graphite to infer cumulative exposure and hence the reactor’s lifetime cumulative plutonium production. Reference Gesh, et. al., for a more complete discussion on the GIRM technology.

  14. ISX-A graphite limiter experiment

    International Nuclear Information System (INIS)

    Langley, R.A.; Colchin, R.J.; Isler, R.C.; Murakami, M.; Simpkins, J.E.; Cecchi, J.L.; Corso, V.L.; Dylla, H.F.; Ellis, R.A. Jr.; Nishi, M.

    1979-01-01

    Graphite limiters were installed and tested in the ISX-A tokamak as part of the ISX-A surface physics program and the TFTR materials research program. The puropse of the experiment was to compare plasma performance using graphite limiters as opposed to the standard ISX-A stainless steel limiters. Heaters were installed in the graphite limiters so that the effects of operation at elevated temperatures could be evaluated

  15. Sealing nuclear graphite with pyrolytic carbon

    International Nuclear Information System (INIS)

    Feng, Shanglei; Xu, Li; Li, Li; Bai, Shuo; Yang, Xinmei; Zhou, Xingtai

    2013-01-01

    Pyrolytic carbon (PyC) coatings were deposited on IG-110 nuclear graphite by thermal decomposition of methane at ∼1830 °C. The PyC coatings are anisotropic and airtight enough to protect IG-110 nuclear graphite against the permeation of molten fluoride salts and the diffusion of gases. The investigations indicate that the sealing nuclear graphite with PyC coating is a promising method for its application in Molten Salt Reactor (MSR)

  16. Graphitic Carbon Nitride Materials for Energy Applications

    OpenAIRE

    Belen Jorge, A.; Dedigama, I.; Mansor, N.; Jervis, R.; Corà, F.; McMillan, P. F.; Brett, D.

    2015-01-01

    Polymeric layered carbon nitrides were investigated for use as catalyst support materials for proton exchange membrane fuel cells (PEMFCs) and water electrolyzers (PEMWEs). Three different carbon nitride materials were prepared: a heptazine-based graphitic carbon nitride material (gCNM), poly (triazine) imide carbon nitride intercalated with LiCl component (PTI-Li+Cl-) and boron-doped graphitic carbon nitride (B-gCNM). Following accelerated corrosion testing, all graphitic carbon nitride mate...

  17. Dynamics of graphite flake on a liquid

    Science.gov (United States)

    Miura, K.; Tsuda, D.; Kaneta, Y.; Harada, R.; Ishikawa, M.; Sasaki, N.

    2006-11-01

    One-directional motion, where graphite flakes are driven by a nanotip on an octamethylcyclotetrasiloxane (OMCTS) liquid surface, is presented. A transition from quasiperiodic to chaotic motions occurs in the dynamics of a graphite flake when its velocity is increased. The dynamics of graphite flakes pulled by the nanotip on an OMCTS liquid surface can be treated as that of a nanobody on a liquid.

  18. Graphite-to-metal bonding techniques

    International Nuclear Information System (INIS)

    Lindquist, L.O.; Mah, R.

    1977-11-01

    The results of various bonding methods to join graphite to different metals are reported. Graphite/metal bonds were tested for thermal flux limits and thermal flux cycling lifetimes. The most successful bond transferred a heat flux of 6.50 MW/m 2 in more than 500 thermal cycles. This bond was between pyrolytic graphite and copper with Ti-Cu-Sil as the bonding agent

  19. Stationary infinitely divisible processes

    DEFF Research Database (Denmark)

    Barndorff-Nielsen, Ole E.

    Several recent strands of work has led to the consideration of various types of continuous time stationary and infinitely divisible processes. A review of these types, with some new results, is presented.......Several recent strands of work has led to the consideration of various types of continuous time stationary and infinitely divisible processes. A review of these types, with some new results, is presented....

  20. Laboratory Investigations of Stationary Methane Anemometer

    Science.gov (United States)

    Kruczkowski, Janusz; Krawczyk, Jerzy; Ostrogórski, Piotr

    2017-12-01

    This paper presents a new stationary device that can perform simultaneous measurements of air flow velocity and methane concentration in a mine heading (stationary methane anemometer). The test station is designed to use the instrument to test the effect of various parameters on the air-methane stream. The air velocities and methane concentrations were fed to the measuring area via an injector and recorded. The results present numerical simulations of flow phenomena that occurred during measurement experiments.

  1. Dampers for Stationary Labyrinth Seals

    Science.gov (United States)

    El-Aini, Yehia; Mitchell, William; Roberts, Lawrence; Montgomery, Stuart; Davis, Gary

    2011-01-01

    Vibration dampers have been invented that are incorporated as components within the stationary labyrinth seal assembly. These dampers are intended to supplement other vibration-suppressing features of labyrinth seals in order to reduce the incidence of high-cycle-fatigue failures, which have been known to occur in the severe vibratory environments of jet engines and turbopumps in which labyrinth seals are typically used. A vibration damper of this type includes several leaf springs and/or a number of metallic particles (shot) all held in an annular seal cavity by a retaining ring. The leaf springs are made of a spring steel alloy chosen, in conjunction with design parameters, to maintain sufficient preload to ensure effectiveness of damping at desired operating temperatures. The cavity is vented via a small radial gap between the retaining ring and seal housing. The damping mechanism is complex. In the case of leaf springs, the mechanism is mainly friction in the slippage between the seal housing and individual dampers. In the case of a damper that contains shot, the damping mechanism includes contributions from friction between individual particles, friction between particles and cavity walls, and dissipation of kinetic energy of impact. The basic concept of particle/shot vibration dampers has been published previously; what is new here is the use of such dampers to suppress traveling-wave vibrations in labyrinth seals. Damping effectiveness depends on many parameters, including, but not limited to, coefficient of friction, mode shape, and frequency and amplitude of vibrational modes. In tests, preloads of the order of 6 to 15 lb (2.72 to 6.8 kilograms) per spring damper were demonstrated to provide adequate damping levels. Effectiveness of shot damping of vibrations having amplitudes from 20 to 200 times normal terrestrial gravitational acceleration (196 to 1,960 meters per square second) and frequencies up to 12 kHz was demonstrated for shot sizes from 0.032 to

  2. A new damage diagnosis approach for NC machine tools based on hybrid Stationary subspace analysis

    Science.gov (United States)

    Gao, Chen; Zhou, Yuqing; Ren, Yan

    2017-05-01

    This paper focused on the damage diagnosis for NC machine tools and put forward a damage diagnosis method based on hybrid Stationary subspace analysis (SSA), for improving the accuracy and visibility of damage identification. First, the observed single sensor signal was reconstructed to multi-dimensional signals by the phase space reconstruction technique, as the inputs of SSA. SSA method was introduced to separate the reconstructed data into stationary components and non-stationary components without the need for independency and prior information of the origin signals. Subsequently, the selected non-stationary components were analysed for training LS-SVM (Least Squares Support Vector Machine) classifier model, in which several statistic parameters in the time and frequency domains were exacted as the sample of LS-SVM. An empirical analysis in NC milling machine tools is developed, and the result shows high accuracy of the proposed approach.

  3. The Fracture Toughness of Nuclear Graphites Grades

    Energy Technology Data Exchange (ETDEWEB)

    Burchell, Timothy D. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Erdman, III, Donald L. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Lowden, Rick R. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Hunter, James A. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Hannel, Cara C. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2017-04-01

    New measurements of graphite mode I critical stress intensity factor, KIc (commonly referred to as the fracture toughness) and the mode II critical shear stress intensity, KIIc, are reported and compared with prior data for KIc and KIIc. The new data are for graphite grades PCEA, IG-110 and 2114. Variations of KIc and acoustic emission (AE) data with graphite texture are reported and discussed. The Codes and Standards applications of fracture toughness, KIc, data are also discussed. A specified minimum value for nuclear graphite KIc is recommended.

  4. AC induction field heating of graphite foam

    Science.gov (United States)

    Klett, James W.; Rios, Orlando; Kisner, Roger

    2017-08-22

    A magneto-energy apparatus includes an electromagnetic field source for generating a time-varying electromagnetic field. A graphite foam conductor is disposed within the electromagnetic field. The graphite foam when exposed to the time-varying electromagnetic field conducts an induced electric current, the electric current heating the graphite foam. An energy conversion device utilizes heat energy from the heated graphite foam to perform a heat energy consuming function. A device for heating a fluid and a method of converting energy are also disclosed.

  5. Production of nuclear graphite in France

    International Nuclear Information System (INIS)

    Legendre, P.; Mondet, L.; Arragon, Ph.; Cornuault, P.; Gueron, J.; Hering, H.

    1955-01-01

    The graphite intended for the construction of the reactors is obtained by the usual process: confection of a cake from coke of oil and tar, cooked (in a electric oven) then the product of cook is graphitized, also by electric heating. The use of the air transportation and the control of conditions cooking and graphitization have permitted to increase the nuclear graphite production as well as to better control their physical and mechanical properties and to reduce to the minimum the unwanted stains. (M.B.) [fr

  6. Study of corrosion resistance graphite in oxygen

    International Nuclear Information System (INIS)

    Zelenskij, V.F.; Odejchuk, N.P.; Petel'guzov, I.A.; Ryzhov, V.P.; Yakovlev, V.K.

    2011-01-01

    The paper presents the results of the corrosion resistance of MPG, ARV and GSP graphite grades in oxygen at temperatures of 400, 600 and 800 o C. The oxidation kinetics of graphites is defined. It is shown, that interaction process of graphites with oxygen is characterized by a decrease of sample weights. The description of installation for carrying out of tests and a technique of carrying out of tests and researches is resulted. It is shown that the best corrosion resistance in the investigated temperature range has GSP graphite with density of 1.8-1.9 g/cm 3 of NSC KIPT production.

  7. NGNP Graphite Selection and Acquisition Strategy

    Energy Technology Data Exchange (ETDEWEB)

    Burchell, T.; Bratton, R.; Windes, W.

    2007-09-30

    The nuclear graphite (H-451) previously used in the United States for High-Temperature Reactors (HTRs) is no longer available. New graphites have been developed and are considered suitable candidates for the Next-Generation Nuclear Plant (NGNP). A complete properties database for these new, available, candidate grades of graphite must be developed to support the design and licensing of NGNP core components. Data are required for the physical, mechanical (including radiation-induced creep), and oxidation properties of graphites. Moreover, the data must be statistically sound and take account of in-billet, between billets, and lot-to-lot variations of properties. These data are needed to support the ongoing development1 of the risk-derived American Society of Mechanical Engineers (ASME) graphite design code (a consensus code being prepared under the jurisdiction of the ASME by gas-cooled reactor and NGNP stakeholders including the vendors). The earlier Fort St. Vrain design of High-Temperature Reactor (HTRs) used deterministic performance models for H-451, while the NGNP will use new graphite grades and risk-derived (probabilistic) performance models and design codes, such as that being developed by the ASME. A radiation effects database must be developed for the currently available graphite materials, and this requires a substantial graphite irradiation program. The graphite Technology Development Plan (TDP)2 describes the data needed and the experiments planned to acquire these data in a timely fashion to support NGNP design, construction, and licensing. The strategy for the selection of appropriate grades of graphite for the NGNP is discussed here. The final selection of graphite grades depends upon the chosen reactor type and vendor because the reactor type (pebble bed or prismatic block) has a major influence on the graphite chosen by the designer. However, the time required to obtain the needed irradiation data for the selected NGNP graphite is sufficiently

  8. Nuclear graphite for high temperature reactors

    International Nuclear Information System (INIS)

    Marsden, B.J.

    2001-01-01

    The cores and reflectors in modern High Temperature Gas Cooled Reactors (HTRs) are constructed from graphite components. There are two main designs; the Pebble Bed design and the Prism design. In both of these designs the graphite not only acts as a moderator, but is also a major structural component that may provide channels for the fuel and coolant gas, channels for control and safety shut off devices and provide thermal and neutron shielding. In addition, graphite components may act as a heat sink or conduction path during reactor trips and transients. During reactor operation, many of the graphite component physical properties are significantly changed by irradiation. These changes lead to the generation of significant internal shrinkage stresses and thermal shut down stresses that could lead to component failure. In addition, if the graphite is irradiated to a very high irradiation dose, irradiation swelling can lead to a rapid reduction in modulus and strength, making the component friable.The irradiation behaviour of graphite is strongly dependent on its virgin microstructure, which is determined by the manufacturing route. Nevertheless, there are available, irradiation data on many obsolete graphites of known microstructures. There is also a well-developed physical understanding of the process of irradiation damage in graphite. This paper proposes a specification for graphite suitable for modern HTRs. (author)

  9. Stationary Liquid Fuel Fast Reactor

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Won Sik [Purdue Univ., West Lafayette, IN (United States); Grandy, Andrew [Argonne National Lab. (ANL), Argonne, IL (United States); Boroski, Andrew [Argonne National Lab. (ANL), Argonne, IL (United States); Krajtl, Lubomir [Argonne National Lab. (ANL), Argonne, IL (United States); Johnson, Terry [Argonne National Lab. (ANL), Argonne, IL (United States)

    2015-09-30

    For effective burning of hazardous transuranic (TRU) elements of used nuclear fuel, a transformational advanced reactor concept named SLFFR (Stationary Liquid Fuel Fast Reactor) was proposed based on stationary molten metallic fuel. The fuel enters the reactor vessel in a solid form, and then it is heated to molten temperature in a small melting heater. The fuel is contained within a closed, thick container with penetrating coolant channels, and thus it is not mixed with coolant nor flow through the primary heat transfer circuit. The makeup fuel is semi- continuously added to the system, and thus a very small excess reactivity is required. Gaseous fission products are also removed continuously, and a fraction of the fuel is periodically drawn off from the fuel container to a processing facility where non-gaseous mixed fission products and other impurities are removed and then the cleaned fuel is recycled into the fuel container. A reference core design and a preliminary plant system design of a 1000 MWt TRU- burning SLFFR concept were developed using TRU-Ce-Co fuel, Ta-10W fuel container, and sodium coolant. Conservative design approaches were adopted to stay within the current material performance database. Detailed neutronics and thermal-fluidic analyses were performed to develop a reference core design. Region-dependent 33-group cross sections were generated based on the ENDF/B-VII.0 data using the MC2-3 code. Core and fuel cycle analyses were performed in theta-r-z geometries using the DIF3D and REBUS-3 codes. Reactivity coefficients and kinetics parameters were calculated using the VARI3D perturbation theory code. Thermo-fluidic analyses were performed using the ANSYS FLUENT computational fluid dynamics (CFD) code. Figure 0.1 shows a schematic radial layout of the reference 1000 MWt SLFFR core, and Table 0.1 summarizes the main design parameters of SLFFR-1000 loop plant. The fuel container is a 2.5 cm thick cylinder with an inner radius of 87.5 cm. The fuel

  10. Microstructure, elastic and inelastic properties of partially graphitized biomorphic carbons

    Science.gov (United States)

    Orlova, T. S.; Kardashev, B. K.; Smirnov, B. I.; Gutierrez-Pardo, A.; Ramirez-Rico, J.; Martinez-Fernandez, J.

    2015-03-01

    The microstructural characteristics and amplitude dependences of the Young's modulus E and internal friction (logarithmic decrement δ) of biocarbon matrices prepared by beech wood carbonization at temperatures T carb = 850-1600°C in the presence of a nickel-containing catalyst have been studied. Using X-ray diffraction and electron microscopy, it has been shown that the use of a nickel catalyst during carbonization results in a partial graphitization of biocarbons at T carb ≥ 1000°C: the graphite phase is formed as 50- to 100-nm globules at T carb = 1000°C and as 0.5- to 3.0-μm globules at T carb = 1600°C. It has been found that the measured dependences E( T carb) and δ( T carb) contain three characteristic ranges of variations in the Young's modulus and logarithmic decrement with a change in the carbonization temperature: E increases and δ decreases in the ranges T carb 1300°C; in the range 1000 biocarbons carbonized in the presence of nickel correlates with the evolution of their microstructure. The largest values of E are obtained for samples with T carb = 1000 and 1600°C. However, the samples with T carb = 1600°C exhibit a higher susceptibility to microplasticity due to the presence of a globular graphite phase that is significantly larger in size and total volume.

  11. Characterisation of austempered spheroidal graphite aluminium cast iron

    Energy Technology Data Exchange (ETDEWEB)

    Boutorabi, S.M.A. [Iran Univ. of Science and Technology, Tehran (Iran, Islamic Republic of). Dept. of Metallurgy and Materials

    1997-06-01

    The micro constituents of austempered spheroidal graphite aluminium cast iron were investigated. The heat tinting, special etching and microhardness measurement techniques were used. The results showed that the colour of each micro constituents and the hardness values in austempered ductile iron depend on the carbon content of each phase. The above techniques were supported by using an special etching which showed similar differences in each phase. It was shown that the heat tinting and special etching are reliable tools to characterise the complex matrix of ADI. The microhardness data supported interestingly the colour changes in above technique. (orig.)

  12. Preparation of graphene by electrical explosion of graphite sticks.

    Science.gov (United States)

    Gao, Xin; Xu, Chunxiao; Yin, Hao; Wang, Xiaoguang; Song, Qiuzhi; Chen, Pengwan

    2017-08-03

    Graphene nanosheets were produced by electrical explosion of high-purity graphite sticks in distilled water at room temperature. The as-prepared samples were characterized by various techniques to find different forms of carbon phases, including graphite nanosheets, few-layer graphene, and especially, mono-layer graphene with good crystallinity. Delicate control of energy injection is critical for graphene nanosheet formation, whereas mono-layer graphene was produced under the charging voltage of 22.5-23.5 kV. On the basis of electrical wire explosion and our experimental results, the underlying mechanism that governs the graphene generation was carefully illustrated. This work provides a simple but innovative route for producing graphene nanosheets.

  13. Influence of stationary and non-stationary conditions on drying time and mechanical properties of a porcelain slab

    Science.gov (United States)

    Hammouda, Imen; Mihoubi, Daoued

    2017-12-01

    This work deals with a numerical study of the response of a porcelain slab when subjected to convective drying in stationary and non-stationary conditions. The used model describes heat, mass, and momentum transfers is applied to an unsaturated viscoelastic medium described by a Maxwell model. The numerical code allows us to determine the effect of the surrounding air temperature on drying kinetics and on mechanical stress intensities. Von Mises stresses are analysed in order to foresee an eventual damage that may occur during drying. Simulation results for several temperatures in the range of [30 °C, 90 °C] shows that for the temperature from 30 °C to 60 °C, Von Mises stresses are always lower than the yield strength. But above 70 °C, Von Mises stresses are higher than the ultimate strength, and consequently there is a risk of crack at the end of the constant drying rate period. The idea proposed in this work is to integrate a reducing temperature phase when the predicted Von Mises stress intensity exceeds the admissible stress. Simulation results shows that a non-stationary convective drying (90-60 °C) allows us to optimize costs and quality by reducing the drying time and maintaining Von Mises stress values under the admissible stress.

  14. Stationary radiation of objects with scattering media

    International Nuclear Information System (INIS)

    Vasil'eva, Inna A

    2001-01-01

    The radiation observed inside or outside a stationary radiator with a scattering medium is a sum of components, each being determined by, first, the primary radiation from some part of the radiator and, second, the probability of this radiation reaching the region where it is observed. In this review, general and rather simple relations between these components are discussed. These relations, unlike the components themselves, are independent of the specific optical characteristics of the object as well as of its geometry, inhomogeneity, etc. In deriving the relations, the situations in which geometrical optics is either applicable or inapplicable to radiation in a scattering medium are considered. For the case where geometrical optics does apply, stationary relations are derived from the probabilistic stationarity condition for radiation passing through the medium, i.e., from the fact that all radiation emitted in a stationary regime disappears with probability unity. Equilibrium relations are derived from the stationary relations in the particular case of a thermal radiator in an isothermal cavity. To derive the stationary relations in the geometrical optics approximation, we obtain general solutions of the linear equation of transfer using the Green function approach. If geometrical optics cannot be applied to a scattering and radiating medium, only relations for the components of outgoing thermal radiation are obtained, and the generalized Kirchhoff law, obtained by Levin and Rytov using statistical radio-physics methods, is employed. In this case, stationary relations are also derived from a probabilistic stationarity condition; the equilibrium relations follow from the stationary ones as well as from the equilibrium condition for radiation in the isothermal cavity. The quantities involved in all the relations obtained are a subject of experimental and computational spectroscopic studies. Examples of current and potential applications are given. The relations

  15. Analyzing Non Stationary Processes in Radiometers

    Science.gov (United States)

    Racette, Paul

    2010-01-01

    The lack of well-developed techniques for modeling changing statistical moments in our observations has stymied the application of stochastic process theory for many scientific and engineering applications. Non linear effects of the observation methodology is one of the most perplexing aspects to modeling non stationary processes. This perplexing problem was encountered when modeling the effect of non stationary receiver fluctuations on the performance of radiometer calibration architectures. Existing modeling approaches were found not applicable; particularly problematic is modeling processes across scales over which they begin to exhibit non stationary behavior within the time interval of the calibration algorithm. Alternatively, the radiometer output is modeled as samples from a sequence random variables; the random variables are treated using a conditional probability distribution function conditioned on the use of the variable in the calibration algorithm. This approach of treating a process as a sequence of random variables with non stationary stochastic moments produce sensible predictions of temporal effects of calibration algorithms. To test these model predictions, an experiment using the Millimeter wave Imaging Radiometer (MIR) was conducted. The MIR with its two black body calibration references was configured in a laboratory setting to observe a third ultra-stable reference (CryoTarget). The MIR was programmed to sequentially sample each of the three references in approximately a 1 second cycle. Data were collected over a six-hour interval. The sequence of reference measurements form an ensemble sample set comprised of a series of three reference measurements. Two references are required to estimate the receiver response. A third reference is used to estimate the uncertainty in the estimate. Typically, calibration algorithms are designed to suppress the non stationary effects of receiver fluctuations. By treating the data sequence as an ensemble

  16. Correlations Between retention indices and molecular structure of aliphatic alcohols and of their benzoyl derivatives on phenyl substituted polysiloxane stationary phases; Cromatografia en fase gaseosa sobre metilfenilpolisiloxanos. Estructura molecular y parametros de retencion para alcoholes y sus derivados benzoilados

    Energy Technology Data Exchange (ETDEWEB)

    Pias, J. B.; Gasco, L.

    1976-07-01

    The retention indices of aliphatic alcohols of carbon number up to C{sub g}, and of their benzoyl derivatives up to C{sub 7}, were determined in columns packed with Chromo sorb G (AW-DMCS-HP) coated previously with 5% methyl, and methyl phenyl polysiloxanes with increasing polarity (SE-30, 0V-3, 0V-7, 0V-11, 0V-17 and OV-25). Correlations between retention indices and chain length for 1-alcohols, 2-alcohols, 3-alcohols, 1 , on -3-alcohols, 2-methyl-1-alcohols and for their corresponding benzoyl derivatives were calculated at 100, 120 and 140 degree centigree. In alcohols, a -CH{sub 2}- group increases I approximately 100 units, and in their benzoyl derivatives from 80 to 100 units. Dispersion indices {delta}l , and positional and structural increments {delta}I, were evaluated for -OH and benzoyl groups in terms of phase polarity and chain length. Effects of chain length, chain branching and double bond location on retention parameters were also studied. (Author) 23 refs.

  17. Effect of graphite target power density on tribological properties of graphite-like carbon films

    Science.gov (United States)

    Dong, Dan; Jiang, Bailing; Li, Hongtao; Du, Yuzhou; Yang, Chao

    2018-05-01

    In order to improve the tribological performance, a series of graphite-like carbon (GLC) films with different graphite target power densities were prepared by magnetron sputtering. The valence bond and microstructure of films were characterized by AFM, TEM, XPS and Raman spectra. The variation of mechanical and tribological properties with graphite target power density was analyzed. The results showed that with the increase of graphite target power density, the deposition rate and the ratio of sp2 bond increased obviously. The hardness firstly increased and then decreased with the increase of graphite target power density, whilst the friction coefficient and the specific wear rate increased slightly after a decrease with the increasing graphite target power density. The friction coefficient and the specific wear rate were the lowest when the graphite target power density was 23.3 W/cm2.

  18. Flexible PVC flame retarded with expandable graphite

    CSIR Research Space (South Africa)

    Focke, WW

    2014-02-01

    Full Text Available The utility of expandable graphite as a flame retardant for PVC, plasticized with 60 phr of a phosphate ester, was investigated. Cone calorimeter results, at a radiant flux of 35 kW m 2, revealed that adding only 5 wt.% expandable graphite lowered...

  19. Mechanical properties of graphite and carbon materials

    International Nuclear Information System (INIS)

    Jouquet, G.

    1976-01-01

    The elastic properties of the graphite monocrystal, the role of internal characteristics (texture, porosity) on the mechanical behavior of carbons, effects caused by the gaseous environment and neutron irradiation, and the resistance of graphites to cyclic mechanical stresses are discussed [fr

  20. Significance of primary irradiation creep in graphite

    CSIR Research Space (South Africa)

    Erasmus, C

    2013-05-01

    Full Text Available Traditionally primary irradiation creep is introduced into graphite analysis by applying the appropriate amount of creep strain to the model at the initial time-step. This is valid for graphite components that are subjected to high fast neutron flux...

  1. Electrochemical Capacitor Development for Pulsed Power Communications, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — This SBIR Phase I addresses the development of electrochemical ultracapacitors (ECs) using graphitic nanosheets as the electrode material. The advantages Eltron's...

  2. Methane generated from graphite--tritium interaction

    International Nuclear Information System (INIS)

    Coffin, D.O.; Walthers, C.R.

    1979-01-01

    When hydrogen isotopes are separated by cryogenic distillation, as little as 1 ppM of methane will eventually plug the still as frost accumulates on the column packings. Elemental carbon exposed to tritium generates methane spontaneously, and yet some dry transfer pumps, otherwise compatible with tritium, convey the gas with graphite rotors. This study was to determine the methane production rate for graphite in tritium. A pump manufacturer supplied graphite samples that we exposed to tritium gas at 0.8 atm. After 137 days we measured a methane synthesis rate of 6 ng/h per cm 2 of graphite exposed. At this rate methane might grow to a concentration of 0.01 ppM when pure tritium is transferred once through a typical graphite--rotor transfer pump. Such a low methane level will not cause column blockage, even if the cryogenic still is operated continuously for many years

  3. Stability and instability of stationary solutions for sublinear parabolic equations

    Science.gov (United States)

    Kajikiya, Ryuji

    2018-01-01

    In the present paper, we study the initial boundary value problem of the sublinear parabolic equation. We prove the existence of solutions and investigate the stability and instability of stationary solutions. We show that a unique positive and a unique negative stationary solutions are exponentially stable and give the exact exponent. We prove that small stationary solutions are unstable. For one space dimensional autonomous equations, we elucidate the structure of stationary solutions and study the stability of all stationary solutions.

  4. AGC-2 Graphite Preirradiation Data Analysis Report

    Energy Technology Data Exchange (ETDEWEB)

    William Windes; W. David Swank; David Rohrbaugh; Joseph Lord

    2013-08-01

    This report described the specimen loading order and documents all pre-irradiation examination material property measurement data for the graphite specimens contained within the second Advanced Graphite Capsule (AGC-2) irradiation capsule. The AGC-2 capsule is the second in six planned irradiation capsules comprising the Advanced Graphite Creep (AGC) test series. The AGC test series is used to irradiate graphite specimens allowing quantitative data necessary for predicting the irradiation behavior and operating performance of new nuclear graphite grades to be generated which will ascertain the in-service behavior of the graphite for pebble bed and prismatic Very High Temperature Reactor (VHTR) designs. Similar to the AGC-1 specimen pre-irradiation examination report, material property tests were conducted on specimens from 18 nuclear graphite types but on an increased number of specimens (512) prior to loading into the AGC-2 irradiation assembly. All AGC-2 specimen testing was conducted at Idaho National Laboratory (INL) from October 2009 to August 2010. This report also details the specimen loading methodology for the graphite specimens inside the AGC-2 irradiation capsule. The AGC-2 capsule design requires “matched pair” creep specimens that have similar dose levels above and below the neutron flux profile mid-plane to provide similar specimens with and without an applied load. This document utilized the neutron flux profile calculated for the AGC-2 capsule design, the capsule dimensions, and the size (length) of the selected graphite and silicon carbide samples to create a stacking order that can produce “matched pairs” of graphite samples above and below the AGC-2 capsule elevation mid-point to provide specimens with similar neutron dose levels.

  5. The fracture of graphite; La rupture des graphites

    Energy Technology Data Exchange (ETDEWEB)

    Rouby, D. [Institut National des Sciences Appliquees (INSA), Groupe d' Etudes de Metallurgie Physique et de Physique des Materiaux, UMR CNRS 5510, 69 - Villeurbanne (France); Monchaux, St. [Institut National des Sciences Appliquees (INSA), Dept. Science et Genie des Materiaux, 69 - Villeurbanne (France); Tahon, B. [Laboratoire SGL Carbon SAS, 74 - Passy (France)

    2006-03-15

    By mechanical loading, the behaviour of poly-granular graphites for industrial uses is globally brittle: when a pre-existing flaw becomes critical a crack initiates and then propagates more or less catastrophically. This scheme implies several features which are described in the present paper. First, as the crack will be initiated at a critical flaw, the ultimate stress appears as largely dispersed and the strength is not an intrinsic material's parameter. Secondly, the processing route introduces in the material some microstructure anisotropy, largely influencing the strength dispersion. Finally, the crack propagation is controlled by a bridging mechanism of the lips which depends on the microstructure. This effect can be described by the so-called crack growth resistance curve: the R-curve. (authors)

  6. Investigation on the formation of lonsdaleite from graphite

    Energy Technology Data Exchange (ETDEWEB)

    Greshnyakov, V. A.; Belenkov, E. A., E-mail: belenkov@csu.ru [Chelyabinsk State University (Russian Federation)

    2017-02-15

    Structural stability and the possible pathways to experimental formation of lonsdaleite—a hexagonal 2H polytype of diamond—have been studied in the framework of the density functional theory (DFT). It is established that the structural transformation of orthorhombic Cmmm graphite to 2H polytype of diamond must take place at a pressure of 61 GPa, while the formation of lonsdaleite from hexagonal P6/mmm graphite must take place at 56 GPa. The minimum potential barrier height separating the 2H polytype state from graphite is only 0.003 eV/atom smaller than that for the cubic diamond. The high potential barrier is indicative of the possibility of stable existence of the hexagonal diamond under normal conditions. In this work, we have also analyzed the X-ray diffraction and electron-microscopic data available for nanodiamonds found in meteorite impact craters in search for the presence of hexagonal diamond. Results of this analysis showed that pure 3C and 2H polytypes are not contained in the carbon materials of impact origin, the structure of nanocrystals found representing diamonds with randomly packed layers. The term “lonsdaleite,” used to denote carbon materials found in meteorite impact craters and diamond crystals with 2H polytype structure, is rather ambiguous, since no pure hexagonal diamond has been identified in carbon phases found at meteorite fall sites.

  7. Stationary Double Layers in a Collisionless Magnetoplasma

    DEFF Research Database (Denmark)

    Noriyoshi, Sato; Mieno, Tetsu; Hatakeyama, Rikizo

    1983-01-01

    Stationary double layers are generated in a magnetoplasma by applying potential differences between two heated plates on which the plasma is produced by surface ionization. By measuring the double-layer formation process, a localized potential drop is found to be formed initially in front...... of the plate on the low-potential side, being accompanied with current limitation. This localized potential drop moves along the plasma column, but finally stops and results in the formation of the stationary double layer in the presence of sufficient plasma supply from the plate on the high-potential side....

  8. Enhancement of optical nonlinearities with stationary light

    DEFF Research Database (Denmark)

    Iakoupov, Ivan

    Stationary light arises in atomic ensembles with certain energy level configurations, when two counter-propagating classical drives (lasers) are applied. Probe light coupled to a different energy level transition than the classical drives can be completely stopped, while still retaining its light...... character. We will be interested in the regime of stationary light, where the probe light still propagates through the atomic ensemble, but extremely slowly. In other words, probe field has a very low group velocity, which increases its interaction time with any optical nonlinearity. The enhancement...

  9. PLASTIC FLOW OF CEMENTITE AND GRAPHITE IMPURITIES AT PROCESSING BY CAST IRON PRESSURE

    Directory of Open Access Journals (Sweden)

    A. I. Pokrovskiy

    2013-01-01

    Full Text Available It is shown that the plastic deformation of cast irons with impurities of fragile phases of cement and graphite is an example of the general case of deformation of heterogeneous materials, in which fragile phase is located inside of the plastic base. It is confirmed that the most important factor is application of the deformation schemes close to uniform compression, what enables to deform plastically the fragile phases in the cast iron structure.

  10. 4. Workshop - Measurement techniques of stationary and transient multiphase flow

    Energy Technology Data Exchange (ETDEWEB)

    Prasser, H.M. (ed.)

    2001-05-01

    In November 2000, the 4th Workshop on Measurement Techniques for Stationary and Transient Multiphase Flows took place in Rossendorf. Three previous workshops of this series were national meetings; this time participants from different countries took part. The programme comprised 14 oral presentations, 9 of which are included in these proceedings in full length. A special highlight of the meeting was the main lecture ''Ultrasonic doppler method for bubbly flow measurement'' of Professor Masanori Aritomi, Dr. Hiroshige Kikura and Dr. Yumiko Suzuki. The workshop again dealt with high-resolution phase distribution and phase velocity measurement techniques based on electrical conductivity, ultrasound, laser light and high-speed cinematography. A number of presentations were dedicated to the application of wire-mesh sensors developed by FZR for different applications used by the Technical Universities of Delft and Munich and the Tokyo Institute of Technology. (orig.)

  11. 4. Workshop - Measurement techniques of stationary and transient multiphase flow

    International Nuclear Information System (INIS)

    Prasser, H.M.

    2001-05-01

    In November 2000, the 4th Workshop on Measurement Techniques for Stationary and Transient Multiphase Flows took place in Rossendorf. Three previous workshops of this series were national meetings; this time participants from different countries took part. The programme comprised 14 oral presentations, 9 of which are included in these proceedings in full length. A special highlight of the meeting was the main lecture ''Ultrasonic doppler method for bubbly flow measurement'' of Professor Masanori Aritomi, Dr. Hiroshige Kikura and Dr. Yumiko Suzuki. The workshop again dealt with high-resolution phase distribution and phase velocity measurement techniques based on electrical conductivity, ultrasound, laser light and high-speed cinematography. A number of presentations were dedicated to the application of wire-mesh sensors developed by FZR for different applications used by the Technical Universities of Delft and Munich and the Tokyo Institute of Technology. (orig.)

  12. Graphite Oxidation Thermodynamics/Reactions

    International Nuclear Information System (INIS)

    Propp, W.A.

    1998-01-01

    The vulnerability of graphite-matrix spent nuclear fuel to oxidation by the ambient atmosphere if the fuel canister is breached was evaluated. Thermochemical and kinetic data over the anticipated range of storage temperatures (200 to 400 C) were used to calculate the times required for a total carbon mass loss of 1 mgcm-2 from a fuel specimen. At 200 C, the time required to produce even this small loss is large, 900,000 yr. However, at 400 C the time required is only 1.9 yr. The rate of oxidation at 200 C is negligible, and the rate even at 400 C is so small as to be of no practical consequence. Therefore, oxidation of the spent nuclear fuel upon a loss of canister integrity is not anticipated to be a concern based upon the results of this study

  13. Stationary Cycling and Children with Cerebral Palsy: Case Reports for Two Participants

    Science.gov (United States)

    Siebert, Kara L.; DeMuth, Sharon K.; Knutson, Loretta M.; Fowler, Eileen G.

    2010-01-01

    These case reports describe a stationary cycling intervention and outcomes for two child participants (P1 and P2) with spastic diplegic cerebral palsy. Each child completed a 12-week, 30-session cycling intervention consisting of strengthening and cardiorespiratory fitness phases. P1 exhibited higher training intensities, particularly during the…

  14. Relativistic elasticity of stationary fluid branes

    DEFF Research Database (Denmark)

    Armas, J.; Obers, N.A.

    2013-01-01

    Fluid mechanics can be formulated on dynamical surfaces of arbitrary codimension embedded in a background space-time. This has been the main object of study of the blackfold approach in which the emphasis has primarily been on stationary fluid configurations. Motivated by this approach we show un...

  15. Polarization fluctuations in stationary light beams

    International Nuclear Information System (INIS)

    Shevchenko, A.; Setaelae, T.; Kaivola, M.; Friberg, A.T.; Royal Institute of Technology , Department of Microelectronics and Applied Physics; Sweden)

    2009-01-01

    For stationary beams the degree of polarization contains only limited information on time dependent polarization. Two approaches towards assessing a beams polarization dynamics, one based on Poincare and the other on Jones vector formalism, are described leading to the notion of polarization time. Specific examples of partially temporally coherent electromagnetic beams are discussed. (Author)

  16. Stationary Double Layers in a Collisionless Magnetoplasma

    DEFF Research Database (Denmark)

    Noriyoshi, Sato; Mieno, Tetsu; Hatakeyama, Rikizo

    1983-01-01

    Stationary double layers are generated in a magnetoplasma by applying potential differences between two heated plates on which the plasma is produced by surface ionization. By measuring the double-layer formation process, a localized potential drop is found to be formed initially in front of the ...

  17. New interval forecast for stationary autoregressive models ...

    African Journals Online (AJOL)

    In this paper, we proposed a new forecasting interval for stationary Autoregressive, AR(p) models using the Akaike information criterion (AIC) function. Ordinarily, the AIC function is used to determine the order of an AR(p) process. In this study however, AIC forecast interval compared favorably with the theoretical forecast ...

  18. Stone Stability under Stationary Nonuniform Flows

    NARCIS (Netherlands)

    Steenstra, Remco; Hofland, B.; Paarlberg, Andries; Smale, Alfons; Huthoff, Fredrik; Uijttewaal, W.S.J.

    2016-01-01

    A stability parameter for rock in bed protections under nonuniform stationary flow is derived. The influence of the mean flow velocity, turbulence, and mean acceleration of the flow are included explicitly in the parameter. The relatively new notion of explicitly incorporating the mean acceleration

  19. What is "stationary" deformation of pure Cu?

    Czech Academy of Sciences Publication Activity Database

    Blum, W.; Dvořák, Jiří; Král, Petr; Eisenlohr, P.; Sklenička, Václav

    2014-01-01

    Roč. 49, č. 8 (2014), s. 2987-2997 ISSN 0022-2461 R&D Projects: GA ČR(CZ) GAP108/11/2260 Institutional support: RVO:68081723 Keywords : creep * Cu * recrystallization * stationary deformation resistances Subject RIV: JJ - Other Materials Impact factor: 2.371, year: 2014

  20. Simulation of stationary sheet metal cutting processes

    NARCIS (Netherlands)

    Wisselink, H.H.; Huetink, Han

    1998-01-01

    In stationary sheet metal cutting processes, like guillotining and slitting, the sheet is cut progressively from one end to the other. This in contrary with transient processes (blanking) where the sheet is cut at once. Where transient shearing processes can be modelled in 2-D (plain strain or

  1. Learning Markov models for stationary system behaviors

    DEFF Research Database (Denmark)

    Chen, Yingke; Mao, Hua; Jaeger, Manfred

    2012-01-01

    to a single long observation sequence, and in these situations existing automatic learning methods cannot be applied. In this paper, we adapt algorithms for learning variable order Markov chains from a single observation sequence of a target system, so that stationary system properties can be verified using...

  2. The stationary states of interacting fields

    NARCIS (Netherlands)

    Frazer, W.R.; Hove, Léon van

    1958-01-01

    As an application of a time-independent perturbation formalism developed earlier for systems with many degrees of freedom, we give in terms of diagrams the general perturbation expressions for the exact stationary states of interacting fields. The physical vacuum is obtained by applying to the bare

  3. An experimental stationary quadrotor with variable DOF

    Indian Academy of Sciences (India)

    Unmanned air vehicles (UAV) and especially quadrotors have drawn great attention in recent years because of their maneuverability, ease of design and control. Most of the works concentrate mostly on control; yet, design and communication are also some sub-topics. In this research, a stationary, four rotor air vehicle with ...

  4. Calendar Year 2016 Stationary Source Emissions Inventory

    Energy Technology Data Exchange (ETDEWEB)

    Evelo, Stacie [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2017-01-01

    The City of Albuquerque (COA) Environmental Health Department Air Quality Program has issued stationary source permits and registrations the Department of Energy/Sandia Field Office for operations at the Sandia National Laboratories/New Mexico. This emission inventory report meets the annual reporting compliance requirements for calendar year (CY) 2016 as required by the COA.

  5. Stationary thermal convection in a viscoelastic ferrofluid

    Energy Technology Data Exchange (ETDEWEB)

    Laroze, D., E-mail: david.laroze@gmail.co [Max Planck Institute for Polymer Research, D 55021 Mainz (Germany); Instituto de Alta Investigacion, Universidad de Tarapaca, Casilla 7D, Arica (Chile); Martinez-Mardones, J. [Instituto de Fisica, Pontificia Universidad Catolica de Valparaiso, Casilla 4059, Valparaiso (Chile); Perez, L.M. [Departamento de Ingenieria Metalurgica, Universidad de Santiago de Chile, Av. Bernardo OHiggins 3363, Santiago (Chile); Rojas, R.G. [Instituto de Fisica, Pontificia Universidad Catolica de Valparaiso, Casilla 4059, Valparaiso (Chile)

    2010-11-15

    We report theoretical and numerical results on convection for a magnetic fluid in a viscoelastic carrier liquid. We focus in the stationary convection for idealized boundary conditions. We obtain explicit expressions of convective thresholds in terms of the control parameters of the system. Close to bifurcation, the coefficients of the corresponding amplitude equation are determined analytically. Finally, the secondary instabilities are performed.

  6. Graphite Fluoride Fiber Composites For Heat Sinking

    Science.gov (United States)

    Hung, Ching-Cheh; Long, Martin; Stahl, Mark

    1989-01-01

    Graphite fluoride fiber/polymer composite materials consist of graphite fluoride fibers in epoxy, polytetrafluoroethylene, or polyimide resin. Combines high electrical resistivity with high thermal conductivity and solves heat-transfer problems of many electrical systems. Commercially available in powder form, for use as dry lubricant or cathode material in lithium batteries. Produced by direct fluorination of graphite powder at temperature of 400 to 650 degree C. Applications include printed-circuit boards for high-density power electronics, insulators for magnetic-field cores like those found in alternators and transformers, substrates for thin-film resistors, and electrical-protection layers in aircraft de-icers.

  7. Synthesis of soluble graphite and graphene.

    Science.gov (United States)

    Kelly, K F; Billups, W E

    2013-01-15

    Because of graphene's anticipated applications in electronics and its thermal, mechanical, and optical properties, many scientists and engineers are interested in this material. Graphene is an isolated layer of the π-stacked hexagonal allotrope of carbon known as graphite. The interlayer cohesive energy of graphite, or exfoliation energy, that results from van der Waals attractions over the interlayer spacing distance of 3.34 Å (61 meV/C atom) is many times weaker than the intralayer covalent bonding. Since graphene itself does not occur naturally, scientists and engineers are still learning how to isolate and manipulate individual layers of graphene. Some researchers have relied on the physical separation of the sheets, a process that can sometimes be as simple as peeling of sheets from crystalline graphite using Scotch tape. Other researchers have taken an ensemble approach, where they exploit the chemical conversion of graphite to the individual layers. The typical intermediary state is graphite oxide, which is often produced using strong oxidants under acidic conditions. Structurally, researchers hypothesize that acidic functional groups functionalize the oxidized material at the edges and a network of epoxy groups cover the sp(2)-bonded carbon network. The exfoliated material formed under these conditions can be used to form dispersions that are usually unstable. However, more importantly, irreversible defects form in the basal plane during oxidation and remain even after reduction of graphite oxide back to graphene-like material. As part of our interest in the dissolution of carbon nanomaterials, we have explored the derivatization of graphite following the same procedures that preserve the sp(2) bonding and the associated unique physical and electronic properties in the chemical processing of single-walled carbon nanotubes. In this Account, we describe efficient routes to exfoliate graphite either into graphitic nanoparticles or into graphene without

  8. Status of Chronic Oxidation Studies of Graphite

    Energy Technology Data Exchange (ETDEWEB)

    Contescu, Cristian I. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Mee, Robert W. [Univ. of Tennessee, Knoxville, TN (United States)

    2016-05-01

    Graphite will undergo extremely slow, but continuous oxidation by traces of moisture that will be present, albeit at very low levels, in the helium coolant of HTGR. This chronic oxidation may cause degradation of mechanical strength and thermal properties of graphite components if a porous oxidation layer penetrates deep enough in the bulk of graphite components during the lifetime of the reactor. The current research on graphite chronic oxidation is motivated by the acute need to understand the behavior of each graphite grade during prolonged exposure to high temperature chemical attack by moisture. The goal is to provide the elements needed to develop predictive models for long-time oxidation behavior of graphite components in the cooling helium of HTGR. The tasks derived from this goal are: (1) Oxidation rate measurements in order to determine and validate a comprehensive kinetic model suitable for prediction of intrinsic oxidation rates as a function of temperature and oxidant gas composition; (2) Characterization of effective diffusivity of water vapor in the graphite pore system in order to account for the in-pore transport of moisture; and (3) Development and validation of a predictive model for the penetration depth of the oxidized layer, in order to assess the risk of oxidation caused damage of particular graphite grades after prolonged exposure to the environment of helium coolant in HTGR. The most important and most time consuming of these tasks is the measurement of oxidation rates in accelerated oxidation tests (but still under kinetic control) and the development of a reliable kinetic model. This report summarizes the status of chronic oxidation studies on graphite, and then focuses on model development activities, progress of kinetic measurements, validation of results, and improvement of the kinetic models. Analysis of current and past results obtained with three grades of showed that the classical Langmuir-Hinshelwood model cannot reproduce all

  9. Stable dispersions of polymer-coated graphitic nanoplatelets

    Science.gov (United States)

    Stankovich, Sasha (Inventor); Nguyen, Sonbinh T. (Inventor); Ruoff, Rodney S. (Inventor)

    2011-01-01

    A method of making a dispersion of reduced graphite oxide nanoplatelets involves providing a dispersion of graphite oxide nanoplatelets and reducing the graphite oxide nanoplatelets in the dispersion in the presence of a reducing agent and a polymer. The reduced graphite oxide nanoplatelets are reduced to an extent to provide a higher C/O ratio than graphite oxide. A stable dispersion having polymer-treated reduced graphite oxide nanoplatelets dispersed in a dispersing medium, such as water or organic liquid is provided. The polymer-treated, reduced graphite oxide nanoplatelets can be distributed in a polymer matrix to provide a composite material.

  10. Synthesis of graphene nanoplatelets from peroxosulfate graphite intercalation compounds

    OpenAIRE

    MELEZHYK A.V.; TKACHEV A.G.

    2014-01-01

    Ultrasonic exfoliation of expanded graphite compound obtained by cold expansion of graphite intercalated with peroxodisulfuric acid was shown to allow the creation of graphene nanoplatelets with thickness of about 5-10 nm. The resulting graphene material contained surface oxide groups. The expanded graphite intercalation compound was exfoliated by ultrasound much easier than thermally expanded graphite. A mechanism for the cleavage of graphite to graphene nanoplatelets is proposed. It include...

  11. Characterization of polymer monolithic stationary phases for capillary HPLC

    Czech Academy of Sciences Publication Activity Database

    Moravcová, D.; Jandera, P.; Urban, J.; Planeta, Josef

    2003-01-01

    Roč. 26, č. 11 (2003), s. 1005-1016 ISSN 1615-9306 R&D Projects: GA ČR GA203/02/0023 Institutional research plan: CEZ:AV0Z4031919; CEZ:MSM 253100002 Keywords : monolithic column s * capillary HPLC * column testing Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.108, year: 2003

  12. Carbon nanotube based stationary phases for microchip chromatography

    DEFF Research Database (Denmark)

    Mogensen, Klaus Bo; Kutter, Jörg Peter

    2012-01-01

    The objective of this article is to provide an overview and critical evaluation of the use of carbon nanotubes and related carbon-based nanomaterials for microchip chromatography. The unique properties of carbon nanotubes, such as a very high surface area and intriguing adsorptive behaviour, have...... integrated, tailor-made nanotube columns by means of catalytic growth of the nanotubes inside the fluidic channels. An evaluation of the different implementations of carbon nanotubes and related carbon-based nanomaterials for microfluidic chromatography devices is given in terms of separation performance...

  13. Large volume monolithic stationary phases: preparation, properties, and applications.

    Science.gov (United States)

    Podgornik, Aleš; Jančar, Janez; Mihelič, Igor; Barut, Miloš; Strancar, Aleš

    2010-03-01

    Monoliths represents the 4th generation of chromatographic supports. They consist of a single piece of highly porous material with interconnected flow through pores. Because of that transport is based on convection what results in a flow unaffected separation and dynamic binding capacity. This is especially important when large molecular weight molecules such as proteins, DNA or viruses have to be purified. For this purpose large volume monolithic columns are needed. In this article preparation of such columns is described together with their main applications. The article is dedicated to Prof. Tine Koloini who substantially contributed to this topic.

  14. Different Stationary Phase Selectivities and Morphologies for Intact Protein Separations

    NARCIS (Netherlands)

    Astefanei, A.; Dapic, I.; Camenzuli, M.

    The central dogma of biology proposed that one gene encodes for one protein. We now know that this does not reflect reality. The human body has approximately 20,000 protein-encoding genes; each of these genes can encode more than one protein. Proteins expressed from a single gene can vary in terms

  15. Translational misreading in Mycobacterium smegmatis increases in stationary phase.

    Science.gov (United States)

    Leng, Tianqi; Pan, Miaomiao; Xu, Xin; Javid, Babak

    2015-12-01

    The study of errors in gene translation has largely been confined to a small number of model organisms. We have examined all possible misreading errors at a defined codon in Mycobacterium smegmatis. Using a dual-luciferase gain of function reporter system that employs a mutated essential lysine in firefly luciferase, we accurately quantified mistranslation errors. Overall, accuracy of gene translation was comparable with Escherichia coli at streptomycin increased misreading errors at several codons associated in particular with U·U, G·U and C·U codon·anti-codon mismatches, but oxidative stress did not change translational fidelity. Our study is the first comprehensive examination of misreading errors for a defined codon in mycobacteria. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. Chelating agents as stationary phase in extraction chromatography, ch. 11

    International Nuclear Information System (INIS)

    Sebesta, F.

    1975-01-01

    Chelating agents have been used largely in extraction chromatography for separations related to activation analysis, for concentration of metals from dilute solutions, and for preparation of radiochemically pure or carrier-free radionuclides. This review deals with the theory of extraction by chelating agents, the experimental technique, and the chelating agents and systems used (β-diketones, oximes, hydroxamic acid, dithizone and diethyldithiocarbamic acid)

  17. Optical motion control of maglev graphite.

    Science.gov (United States)

    Kobayashi, Masayuki; Abe, Jiro

    2012-12-26

    Graphite has been known as a typical diamagnetic material and can be levitated in the strong magnetic field. Here we show that the magnetically levitating pyrolytic graphite can be moved in the arbitrary place by simple photoirradiation. It is notable that the optical motion control system described in this paper requires only NdFeB permanent magnets and light source. The optical movement is driven by photothermally induced changes in the magnetic susceptibility of the graphite. Moreover, we demonstrate that light energy can be converted into rotational kinetic energy by means of the photothermal property. We find that the levitating graphite disk rotates at over 200 rpm under the sunlight, making it possible to develop a new class of light energy conversion system.

  18. Large Scale Reduction of Graphite Oxide

    Data.gov (United States)

    National Aeronautics and Space Administration — This project seeks to develop an optical method to reduce graphite oxide into graphene efficiently and in larger formats than currently available. Current reduction...

  19. Graphite Oxide and Aromatic Amines : Size Matters

    NARCIS (Netherlands)

    Spyrou, Konstantinos; Calvaresi, Matteo; Diamanti, Evmorfi A. K.; Tsoufis, Theodoros; Gournis, Dimitrios; Rudolf, Petra; Zerbetto, Francesco

    2015-01-01

    Experimental and theoretical studies are performed in order to illuminate, for first time, the intercalation mechanism of polycyclic aromatic molecules into graphite oxide. Two representative molecules of this family, aniline and naphthalene amine are investigated. After intercalation, aniline

  20. Review: BNL Tokamak graphite blanket design concepts

    International Nuclear Information System (INIS)

    Fillo, J.A.; Powell, J.R.

    1976-01-01

    The BNL minimum activity graphite blanket designs are reviewed, and three are discussed in the context of an experimental power reactor (EPR) and commercial power reactor. Basically, the three designs employ a 30 cm or thicker graphite screen. Bremsstrahlung energy is deposited on the graphite surface and re-radiated away as thermal radiation. Fast neutrons are slowed down in the graphite, depositing most of their energy, which is then radiated to a secondary blanket with coolant tubes, as in types A and B, or removed by intermittent direct gas cooling (type C). In types A and B, radiation damage to the coolant tubes in the secondary blanket is reduced by one or two orders of magnitude, while in type C, the blanket is only cooled when the reactor is shut down, so that coolant cannot quench the plasma. (Auth.)

  1. Analysis of Picosecond Pulsed Laser Melted Graphite

    Science.gov (United States)

    Steinbeck, J.; Braunstein, G.; Speck, J.; Dresselhaus, M. S.; Huang, C. Y.; Malvezzi, A. M.; Bloembergen, N.

    1986-12-01

    A Raman microprobe and high resolution TEM have been used to analyze the resolidified region of liquid carbon generated by picosecond pulse laser radiation. From the relative intensities of the zone center Raman-allowed mode for graphite at 1582 cm{sup -1} and the disorder-induced mode at 1360 cm{sup -1}, the average graphite crystallite size in the resolidified region is determined as a function of position. By comparison with Rutherford backscattering spectra and Raman spectra from nanosecond pulsed laser melting experiments, the disorder depth for picosecond pulsed laser melted graphite is determined as a function of irradiating energy density. Comparisons of TEM micrographs for nanosecond and picosecond pulsed laser melting experiments show that the structure of the laser disordered regions in graphite are similar and exhibit similar behavior with increasing laser pulse fluence.

  2. Analysis of picosecond pulsed laser melted graphite

    Energy Technology Data Exchange (ETDEWEB)

    Steinbeck, J.; Braunstein, G.; Speck, J.; Dresselhaus, M.S.; Huang, C.Y.; Malvezzi, A.M.; Bloembergen, N.

    1986-01-01

    A Raman microprobe and high resolution TEM have been used to analyze the resolidified region of liquid carbon generated by picosecond pulse laser radiation. From the relative intensities of the zone center Raman-allowed mode for graphite at 1582 cm/sup -1/ and the disorder-induced mode at 1360 cm/sup -1/, the average graphite crystallite size in the resolidified region is determined as a function of position. By comparison with Rutherford backscattering spectra and Raman spectra from nonosecond pulsed laser melting experiments, the disorder depth for picosecond pulsed laser melted graphite is determined as a function of irradiating energy density. Comparisons of TEM micrographs for nanosecond and picosecond pulsed laser melting experiments show that the structure of the laser disordered regions in graphite are similar and exhibit similar behavior with increasing laser pulse fluence.

  3. Analysis of picosecond pulsed laser melted graphite

    International Nuclear Information System (INIS)

    Steinbeck, J.; Braunstein, G.; Speck, J.; Dresselhaus, M.S.; Huang, C.Y.; Malvezzi, A.M.; Bloembergen, N.

    1986-01-01

    A Raman microprobe and high resolution TEM have been used to analyze the resolidified region of liquid carbon generated by picosecond pulse laser radiation. From the relative intensities of the zone center Raman-allowed mode for graphite at 1582 cm -1 and the disorder-induced mode at 1360 cm -1 , the average graphite crystallite size in the resolidified region is determined as a function of position. By comparison with Rutherford backscattering spectra and Raman spectra from nonosecond pulsed laser melting experiments, the disorder depth for picosecond pulsed laser melted graphite is determined as a function of irradiating energy density. Comparisons of TEM micrographs for nanosecond and picosecond pulsed laser melting experiments show that the structure of the laser disordered regions in graphite are similar and exhibit similar behavior with increasing laser pulse fluence

  4. Immobilization of Rocky Flats Graphite Fines Residue

    International Nuclear Information System (INIS)

    Rudisill, T.S.

    1999-01-01

    The development of the immobilization process for graphite fines has proceeded through a series of experimental programs. The experimental procedures and results from each series of experiments are discussed in this report

  5. Poly (propylene carbonate)/exfoliated graphite nanocomposites ...

    Indian Academy of Sciences (India)

    propylene carbonate)/exfoliated graphite nanocomposites: selective adsorbent for the extraction and detection of gold(III). Sher Bahadar Khan Hadi M Marwani Jongchul Seo Esraa M Bakhsh Kalsoom Akhtar Dowan Kim Abdullah M Asiri. Volume 38 ...

  6. Seismic research on graphite reactor core

    International Nuclear Information System (INIS)

    Lai Shigang; Sun Libin; Zhang Zhengming

    2013-01-01

    Background: Reactors with graphite core structure include production reactor, water-cooled graphite reactor, gas-cooled reactor, high-temperature gas-cooled reactor and so on. Multi-body graphite core structure has nonlinear response under seismic excitation, which is different from the response of general civil structure, metal connection structure or bolted structure. Purpose: In order to provide references for the designing and construction of HTR-PM. This paper reviews the history of reactor seismic research evaluation from certain countries, and summarizes the research methods and research results. Methods: By comparing the methods adopted in different gas-cooled reactor cores, inspiration for our own HTR seismic research was achieved. Results and Conclusions: In this paper, the research ideas of graphite core seismic during the process of designing, constructing and operating HTR-10 are expounded. Also the project progress of HTR-PM and the research on side reflection with the theory of similarity is introduced. (authors)

  7. Investigation on the Effect of Sulfur and Titanium on the Microstructure of Lamellar Graphite Iron

    DEFF Research Database (Denmark)

    Moumeni, Elham; Stefanescu, Doru Michael; Tiedje, Niels Skat

    2013-01-01

    The goal of this work was to identify the inclusions in lamellar graphite cast iron in an effort to explain the nucleation of the phases of interest. Four samples of approximately the same carbon equivalent but different levels of sulfur and titanium were studied. The Ti/S ratios were from 0.15 t...

  8. Neutron Diffraction from the Second Layer of 4He on Graphite

    DEFF Research Database (Denmark)

    da Costa Carneiro, Kim; Passell, L.; Thomlinson, W.

    1981-01-01

    Neutron diffraction has been used to study the second atomic layer of **4He adsorbed on graphite. As the **4He-coverage exceeds the first layer, the second initially forms a fluid phase. But when there is enough **4He in the third layer to compress the second, this layer solidifies. The structure...

  9. Energy evaluations, graphite corrosion in Bugey I

    International Nuclear Information System (INIS)

    Brisbois, J.; Fiche, C.

    1967-01-01

    Bugey I presents a problem of radiolytic corrosion of the graphite by the CO 2 under pressure at high temperature. This report aims to evaluate the energy transferred to the gas by a Bugey I core cell, in normal operating conditions. The water, the carbon oxides and the hydrogen formed quantities are deduced as the consumed graphite and methane. Experimental studies are realized in parallel to validate the presented results. (A.L.B.)

  10. Elastic properties of graphite and interstitial defects

    International Nuclear Information System (INIS)

    Ayasse, J.-B.

    1977-01-01

    The graphite elastic constants C 33 and C 44 , reflecting the interaction of the graphitic planes, were experimentally measured as a function of irradiation and temperature. A model of non-central strength atomic interaction was established to explain the experimental results obtained. This model is valid at zero temperature. The temperature dependence of the elastic properties was analyzed. The influence of the elastic property variations on the specific heat of the lattice at very low temperature was investigated [fr

  11. Analysis of carbohydrates in Lupinus albus stems on imposition of water deficit, using porous graphitic carbon liquid chromatography-electrospray ionization mass spectrometry.

    Science.gov (United States)

    Antonio, Carla; Pinheiro, Carla; Chaves, Maria Manuela; Ricardo, Cândido Pinto; Ortuño, Maria Fernanda; Thomas-Oates, Jane

    2008-04-11

    This work reports the development and application of a negative ion mode online LC-ESI-MS method for studying the effect of water deficit on the carbohydrate content of Lupinus albus stems, using a porous graphitic carbon (PGC) stationary phase and an ion trap mass spectrometer. Using this method, separation and detection of several water soluble carbohydrates, ranging from mono-, di-, and oligosaccharides (raffinose, stachyose, and verbascose) to sugar alcohols was achieved in approximately 10 min. This on-line PGC-LC-ESI-MS method shows good linearity with correlation coefficients R(2)>0.99, selectivity, short analysis time, and limits of detection (LOD) ranging from 0.4 to 9 pmol for sugars and 4-20 pmol for sugar alcohols. This PGC-LC-ESI-MS method is sensitive and allowed us to detect even small alterations in carbohydrate levels in L. albus stems that resulted from a mild/early water deficit (nmol g(-1)DW). This paper describes details of our method and its application to the quantitative analysis of water soluble underivatised carbohydrates extracted from L. albus stem tissues that have been subjected to early and severe water deficit conditions, followed by a rewatering period.

  12. Solving the stationary Liouville equation via a boundary element method

    Science.gov (United States)

    Chappell, David J.; Tanner, Gregor

    2013-02-01

    Energy distributions of linear wave fields are, in the high frequency limit, often approximated in terms of flow or transport equations in phase space. Common techniques for solving the flow equations in both time dependent and stationary problems are ray tracing and level set methods. In the context of predicting the vibro-acoustic response of complex engineering structures, related methods such as Statistical Energy Analysis or variants thereof have found widespread applications. We present a new method for solving the transport equations for complex multi-component structures based on a boundary element formulation of the stationary Liouville equation. The method is an improved version of the Dynamical Energy Analysis technique introduced recently by the authors. It interpolates between standard statistical energy analysis and full ray tracing, containing both of these methods as limiting cases. We demonstrate that the method can be used to efficiently deal with complex large scale problems giving good approximations of the energy distribution when compared to exact solutions of the underlying wave equation.

  13. Oxidizability and explosibility of pure graphite powder

    International Nuclear Information System (INIS)

    L Rahmani; D Roubineau; S Cornet

    2005-01-01

    Full text of publication follows: While graphite is widely considered a heat-resistant material, e.g. able to screen metallic shielding from thermal damage, and graphite powder is used as a fire extinguisher agent where water or carbon dioxide should not, it still can react with air and - being carbon - give forth a significant amount of heat. Whether this makes it a hazard in operations such as dismantling nuclear reactors that contain hundreds of tons of graphite, including a small percentage of powder, is a question that has to be answered, considering that dismantling implies the use of such potential fire initiators as thermal cutters and electrical equipment. For this reason EDF commissioned the Centre National de Prevention et Protection (CNPP) to carry out explosibility tests on unirradiated, nuclear grade (i.e. with about 100 ppm of impurities) graphite powder. CNPP tests were so designed as to simulate realistic conditions that might result from a severe mishap during a dismantling operation, such as the crash of heavy equipment on graphite blocks coupled with the bruise of a high power electrical cable. EDF-CNPP tests complement others, done either in Italy most notably on irradiated graphite dust contaminated with various pollutants, or in the UK where the ability of settled graphite dust to propagate an initial gas explosion into an adjacent volume was assessed. EDF-CNPP tests comprise two steps. Step one was intended to produce a qualitative understanding of how nuclear grade graphite behaves while heated in air. In a first series of experiments graphite samples were heated up to 900 C during two and a half hours and their mass loss measured: it was found that while fine powder is wholly oxidised, coarser powder and chunks retained about two thirds of their initial mass. Oxidation kinetics, as assessed by oven temperature shoot-up, begins at 580 C and is quite low, compared with that of iron powder. In a second series of experiments a graphite piece

  14. Oxidizability and explosibility of pure graphite powder

    International Nuclear Information System (INIS)

    Rahmani, L.; Roubineau, D.; Cornet, S.

    2005-01-01

    Full text of publication follows: While graphite is widely considered a heat-resistant material, e.g. able to screen metallic shielding from thermal damage, and graphite powder is used as a fire extinguisher agent where water or carbon dioxide should not, it still can react with air and - being carbon - give forth a significant amount of heat. Whether this makes it a hazard in operations such as dismantling nuclear reactors that contain hundreds of tons of graphite, including a small percentage of powder, is a question that has to be answered, considering that dismantling implies the use of such potential fire initiators as thermal cutters and electrical equipment. For this reason EDF commissioned the Centre National de Prevention et Protection (CNPP) to carry out explosibility tests on unirradiated, nuclear grade (i.e. with about 100 ppm of impurities) graphite powder. CNPP tests were so designed as to simulate realistic conditions that might result from a severe mishap during a dismantling operation, such as the crash of heavy equipment on graphite blocks coupled with the bruise of a high power electrical cable. EDF-CNPP tests complement others, done either in Italy most notably on irradiated graphite dust contaminated with various pollutants, or in the UK where the ability of settled graphite dust to propagate an initial gas explosion into an adjacent volume was assessed. EDF-CNPP tests comprise two steps. Step one was intended to produce a qualitative understanding of how nuclear grade graphite behaves while heated in air. In a first series of experiments graphite samples were heated up to 900 C during two and a half hours and their mass loss measured: it was found that while fine powder is wholly oxidised, coarser powder and chunks retained about two thirds of their initial mass. Oxidation kinetics, as assessed by oven temperature shoot-up, begins at 580 C and is quite low, compared with that of iron powder. In a second series of experiments a graphite piece

  15. Measurement of the cleavage energy of graphite.

    Science.gov (United States)

    Wang, Wen; Dai, Shuyang; Li, Xide; Yang, Jiarui; Srolovitz, David J; Zheng, Quanshui

    2015-08-28

    The basal plane cleavage energy (CE) of graphite is a key material parameter for understanding many of the unusual properties of graphite, graphene and carbon nanotubes. Nonetheless, a wide range of values for the CE has been reported and no consensus has yet emerged. Here we report the first direct, accurate experimental measurement of the CE of graphite using a novel method based on the self-retraction phenomenon in graphite. The measured value, 0.37±0.01 J m(-2) for the incommensurate state of bicrystal graphite, is nearly invariant with respect to temperature (22 °C≤T≤198 °C) and bicrystal twist angle, and insensitive to impurities from the atmosphere. The CE for the ideal ABAB graphite stacking, 0.39±0.02 J m(-2), is calculated based on a combination of the measured CE and a theoretical calculation. These experimental measurements are also ideal for use in evaluating the efficacy of competing theoretical approaches.

  16. Pressure and graphite effects on electrical conductivity in pyroxene

    Science.gov (United States)

    Wang, D.; Liu, T.; Shen, K.; Li, B.

    2017-12-01

    The geophysical observations including magnetotelluric (MT) and geomagnetic deep sounding show the distribution of electrical conductivity in the Earth's interior. The laboratory-based conductivity measurements of minerals and rocks are usually used to interpret the geophysical observations. Pyroxene is the second most abundant components in the upper mantle, and the electrical conductivity of pyroxene is important to understanding the bulk electrical conductivity. The electrical conductivity of a mineral is affected by many factors, such as its chemical composition, temperature, pressure. Here we report the effects of pressure and graphite on the electrical conductivity of pyroxene and applied to interpretation of MT observation. The starting materials are natural of orthopyroxene and clinopyroxe crystals. A powder sample with grain size 10 um was packed in a Mo capsule and hot-pressed at high pressures and temperatures using a 1000-ton Walker-type uniaxial split-cylinder apparatus. A mixture of pyroxene and a few percent of diamond was annealed at high pressure and temperature. All the hot-pressed samples before and after electrical conductivity measurements, were characterized by scanning electron microscopy, Fourier-Transform Infrared and Raman spectroscopy. High pressure conductivity experiments were carried out in a Walker-type multi-anvil apparatus using a 14/8 assembly. We use a Solartron 1260 Impedance/Gain -phase analyzer with 1V applied voltage within a frequency range of 1M-0.1 Hz to collect data. Complex impedance data on were collected in several heating and cooling cycles The electrical conductivity of pyroxene was made at 4,7,10 GPa, and electrical conductivity of the graphite-bearing pyroxene was measured at 4GPa. The results show the electrical conductivity decrease with the increasing of pressure, which may correspond to the transform from orthopyroxene to clinopyroxene. The results can be used to explain a drop of the electrical conductivity in

  17. Stability of stationary and periodic solutions equations in Banach space

    Directory of Open Access Journals (Sweden)

    A. Ya. Dorogovtsev

    1997-01-01

    Full Text Available Linear difference and differential equations with operator coefficients and random stationary (periodic input are considered. Conditions are presented for the mean stability of stationary (periodic solutions under small perturbation of the coefficients.

  18. Framework for Assessing Biogenic CO2 Emissions from Stationary Sources

    Science.gov (United States)

    This revision of the 2011 report, Accounting Framework for Biogenic CO2 Emissions from Stationary Sources, evaluates biogenic CO2 emissions from stationary sources, including a detailed study of the scientific and technical issues associated with assessing biogenic carbon dioxide...

  19. One-Pot Exfoliation of Graphite and Synthesis of Nanographene/Dimesitylporphyrin Hybrids

    Directory of Open Access Journals (Sweden)

    M. Mar Bernal

    2015-05-01

    Full Text Available A simple one-pot process to exfoliate graphite and synthesize nanographene-dimesitylporphyrin hybrids has been developed. Despite the bulky mesityl groups, which are expected to hinder the efficient π–π stacking between the porphyrin core and graphene, the liquid-phase exfoliation of graphite is significantly favored by the presence of the porphyrins. Metallation of the porphyrin further enhances this effect. The resulting graphene/porphyrin hybrids were characterized by spectroscopy (UV-visible, fluorescence, and Raman and microscopy (STEM, scanning transmission electron microscopy.

  20. Entropy production and thermodynamics of nonequilibrium stationary states: a point of view.

    Science.gov (United States)

    Gallavotti, Giovanni

    2004-09-01

    Entropy might be a not well defined concept if the system can undergo transformations involving stationary nonequilibria. It might be analogous to the heat content (once called "caloric") in transformations that are not isochoric (i.e., which involve mechanical work): it could be just a quantity that can be transferred or created, like heat in equilibrium. The text first reviews the philosophy behind a recently proposed definition of entropy production in nonequilibrium stationary systems. A detailed technical attempt at defining the entropy of a stationary states via their variational properties follows: the unsatisfactory aspects of the results add arguments in favor of the nonexistence of a function of state to be identified with entropy; at the same time new aspects and properties of the phase space contraction emerge. Copyright 2004 American Institute of Physics